ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

ฌ‫ޫࣹ์ݝݿ‬φϊςΫ‫ॴڀݚ‬ɹ໨ɹɹɹ࣍
ʮฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռूʯ૑‫ץ‬Λॕͯ͠ . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

1ʢཧ‫ݚ‬ʣੴ઒఩໵

ॕɹࣙ . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

3

ʢJASRIʣന઒఩‫ٱ‬‫ר‬಄‫ ݴ‬. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

5ʢφϊςΫ‫ݚ‬ʣদҪ७࣐೥ɹɹɹใ . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

7

ฌ‫ݝݿ‬ϏʔϜϥΠϯ BL08B2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

9ฌ‫ݝݿ‬ϏʔϜϥΠϯ BL24XU. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

13. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

17੒ɹՌɹू . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

21

XAFS ࣮‫ݧ‬εςʔγϣϯͷ‫ݱ‬ঢ় . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

23

ࢪઃӡ༻͓Αͼར༻ঢ়‫گ‬ʢφϊςΫ‫ݚ‬ʣཥɹཕ

BL08B2 খ̭֯ઢࢄཚଌఆͷ‫ݱ‬ঢ়ͱ XAFS/SAXS ಉ࣌ଌఆͷ੔උʹ͍ͭͯ . . . . . . . . . . . . .

26

ʢφϊςΫ‫ݚ‬ʣ‫܂‬ຊ࣎ੜ

BL08B2 ̭ઢΠϝʔδϯάεςʔγϣϯͷ੔උ. . . . . . . . . . . . . . . . . . . . . . . . . . . . .

30খ̭֯ઢࢄཚ (SAXS) ʹΑΔΞΫϦϧ‫ܥ‬ΤϚϧγϣϯཻࢠ͓Αͼൽບͷߏ଄ղੳ . . . . . . . . . . .

33

ʢφϊςΫ‫ݚ‬ʣ࣫‫ྑݪ‬ণʢ೔ຊ߹੒Խֶʣࢁຊ༑೭ɼҪ্ढ़ຬɼ໦ా ཁɼ੢‫ݪ‬༏ࢠɼాଜ௚‫ٱ‬ɼླ໦‫ܙ‬ଠɼଜ্ ਖ਼τϙάϥϑΟʔʹΑΔ 4H-SiC ΤϐλΩγϟϧບதͷਕঢ়సҐͷධՁ . . . . . . . . . . . . . . . . . .

37

ʢిத‫ݚ‬ʣ‫ึޭాח‬ɼ௕໺ਖ਼༟, ౔ాलҰɼʢిΧςΫϊʣ໺‫ޱ‬ਅҰɼࢁຊ݈Ұɼখ໺‫ت‬๕ɼࣉా‫ܓ‬հ༗‫ػ‬൒ಋମࡐྉͷ̭ઢࢄཚߏ଄ղੳ

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

39ʢࡾඛԽֶʣླ໦୓໵ɼҏଜ޺೭ɼখౡ༏ࢠ

̭ઢ CT ʹΑΔϙϦϚʔϑΥʔϜͷηϧߏ଄‫ ࡯؍‬. . . . . . . . . . . . . . . . . . . . . . . . . . . . .
ʢΞγοΫεʣཱੴ७Ұ࿠ɼ๺ࢁ༟‫ڭ‬ɼࢁాՂ༞

i41φϊϑΟϥʔίϯϙδοτࡐͷߏ଄ͱ෺ཧಛੑͱͷ૬ؔղ໌ . . . . . . . . . . . . . . . . . . . . . . .

44

ʢॅ༑ϕʔΫʣट౻༃޾ɼࡾ୐ຑ୅ɼࠤ౻݈ଠɼຓඌ੓એɼ
ʢφϊςΫ‫ݚ‬ʣ‫܂‬ຊ࣎ੜ์ࣹޫΛར༻ͨ͠ΰϜࡐྉதͷ֊૚ߏ଄௥੻

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

48

ʢ౦༸ΰϜʣେߐ༟জɼখౡਖ਼ষɼ্ྛ ޺ɼᐩຊ༤‫و‬ɼञҪल೭

XAFS ʹΑΔΤωϧΪʔσόΠεࡐྉͷ‫ߏॴہ‬଄ղੳ . . . . . . . . . . . . . . . . . . . . . . . . . .

51

ʢॅԽ෼ੳηʣߴ‫ڮ‬রԝɼ෱ຬਔࢤɼ໦ଜ޺ɼ຤޿ল‫ޗ‬ɼౡాਅҰɼத௡࿨߂

ߗ̭ઢφϊूޫ༻ԁ‫ܗ‬ଟ૚ບκʔϯϓϨʔτͷ੡࡞ͱੑೳධՁ . . . . . . . . . . . . . . . . . . . . . .

54

ʢฌ‫ཱݝݿ‬େӃʣ࿜ౡ ༃, খࢁ‫ٱو‬, ߴ໺ल࿨, খ੢ൟथ, ௰ ୎໵, ʢNTTATʣ஛த‫وٱ‬, ࢢ‫ ؙ‬ஐ, େ஌ব೭ߴฏߦ౓̭ઢϚΠΫϩϏʔϜͷ‫ܗ‬੒ͱͦͷԠ༻‫ ڀݚ‬. . . . . . . . . . . . . . . . . . . . . . . . . . . .

57

ʢฌ‫ཱݝݿ‬େӃʣ௡ࡔՂ޾ɼҥּཅ‫ش‬ɼߥҪඒஐࢠɼᖒాࠫ‫ر‬ɼԼాຑ༝ɼඌ্‫و‬༸ɼഷ ࿨ًɼߴ໺ल࿨ɼ࿜ౡ ༃ɼʢφϊςΫ‫ݚ‬ʣদҪ७࣐ɼʢ౦େʣੴ઒ ༃ɼ࿨ాҰ࣮BL24XU ʹ͓͚ΔϚΠΫϩϏʔϜɼϚΠΫϩΠϝʔδϯάͷߴ౓Խ . . . . . . . . . . . . . . . . . .

61

ʢฌ‫ཱݝݿ‬େӃʣߴ໺ल࿨

ඍখ֯ೖࣹ̭ઢճં๏ʹΑΔϙϦ-α-ΦϨϑΟϯ/઀ணࡎք໘ͷඍࡉߏ଄ . . . . . . . . . . . . . . . . .

67ʢਆ‫ށ‬େӃʣখࣉ ‫ݡ‬ɼۨాΊ͙Έɼ੢໺ ޹ɼʢφϊςΫ‫ݚ‬ʣԣࢁ࿨࢘ɼদҪ७࣐ɼ
ʢSESʣ஛ా৾‫ޗ‬޿֯ࢄཚޫֶ‫ܥ‬ͷߏஙͱ೪ணࡎͷണ཭աఔʹ͓͚Δߏ଄มԽͷͦͷ৔‫ ࡯؍‬. . . . . . . . . . . . . . .

71

ʢSESʣ஛ా৾‫ޗ‬ɼੴా ੒ɼ໺੉૜ࢢɼ
ʢφϊςΫ‫ݚ‬ʣதલউ඙ɼཥ ཕɼ‫܂‬ຊ࣎ੜɼ࣫‫ྑݪ‬ণɼ೔ࢁ͓͞Γɼԣࢁ࿨࢘ɼদҪ७࣐ϚΠΫϩ XAFS ޫֶ‫૷ݧ࣮ͱܥ‬ஔͷελσΟ . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

75

ʢฌ‫ཱݝݿ‬େӃʣഷ ࿨ًɼඌ্‫و‬༸ɼ௡ࡔՂ޾ɼ
ʢφϊςΫ‫ݚ‬ʣԣࢁ࿨࢘ɼদҪ७࣐ɼ
ʢSESʣ஛ా৾‫ޗ‬

̭ઢ 3D τϙάϥϑΟʔʹΑΔ 4H-SiC ‫ج‬ఈ໘సҐ͓Αͼ؏௨ਕঢ়సҐͷΠϝʔδϯά . . . . . . . .

83

ʢిத‫ݚ‬ʣాপྑฏɼ‫ึޭాח‬ɼ౔ాलҰɼʢ෋࢜ి‫ػ‬ʣ৿ େี‫ࢠݪ‬೩ྉඃ෴؅ࡐͷࢎԽൽບɾۚଐք໘෦ͷαϒϚΠΫϩϏʔϜʹΑΔඍࡉߏ଄ղੳ . . . . . . . . .

86ʢిத‫ݚ‬ʣᖒ෦޹࢙ɼԂా݈ɼ‫ݹ‬୩ਖ਼༟ɼ๺ౡঙҰ

Real-time Synchrotoron Radiation X-Ray Diffraction from Erbium Silicate Formations
on SiO2 /Si Substrates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

91(NTT Basic Res. Lab.) H. Omi์ࣹޫ̭ઢࢄཚ๏Λ༻͍ͨໟ൅ͷઢҡ഑޲ղੳ . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

95ʢՖԦʣ‫ٱ‬ถ୎ࢤɼಙ‫ึࢤݪ‬ඒɼ୮࣏ൣจ

Ϧν΢ϜΠΦϯೋ࣍ి஑ͷෛ‫͚͓ʹۃ‬Δ Mn ෼෍ͷϚΠΫϩϏʔϜ XRF ๏ʹΑΔධՁ . . . . . . . .
ʢNECʣ‫ాށ‬ত෉ii98߹੒ΰϜͷߏ଄ͱಛੑͱͷ૬ؔੑ – ̭ઢࢄཚղੳʹΑΔҰ࣠৳௕݁থԽ‫ڍ‬ಈͷ‫ – ࡯؍‬. . . . . . . . 102
ʢѴԽ੒ʣ‫੉ؠ‬উ߂ɺࠓઘެ෉ɺদԼ࢙஧ɺࡔຊ௚‫ل‬Ϧν΢ϜΠΦϯి஑ਖ਼‫ࡐۃ‬ͷ์ిաఔʹ͓͚Δ‫ॴہ‬తߏ଄มԽ . . . . . . . . . . . . . . . . . . . . . . 105
ʢTRCʣத઒෢ࢤɼ੨໦༃ਔɼԬాҰ޾ฌ‫ݝݿ‬ϏʔϜϥΠϯ੒ՌൃදҰཡ . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109

iii

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ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

「兵庫県ビームライン年報・成果集」
創刊を祝して（独）理化学研究所播磨研究所所長
石川 哲也
兵庫県ビームライン年報・成果集のご創刊おめでとうございます．
兵庫県 ID (BL24XU)および兵庫県 BM (BL08B2)の二本のビームラインを擁する兵庫県は，SPring-8 供用開始後の比較的早い時期から当時の姫路工業大学理学部（現兵庫県立大学理学部）を通じての人材育成や，地元を中心とした放射光産業利用の振興に大きな役割を担ってきました．このような兵庫県のご努力は，国や産業界からの後押しとともに，SPring-8 の産業利用を順調に発展させ，全利用課題の 20%超を産業界からの課題が占めるという，世界的にも極めて高水準を達成し，他国の放射光施設の目標とされるまでになっております．
このたび，SPring-8 での成果非占有課題における成果公開の促進に対応すべく，「兵
庫県ビームライン年報・成果集」を創刊されますことに，心からお祝い申し上げるとともに，兵庫県ビームラインの利用から創出された重要かつ先進的な情報が，広く放射光利用者に公開されることによって，我が国の放射光利用の質的向上に寄与していただけますことは，関係者の一人としてこれに勝る喜びはございません．
現今の先進技術の多くが，ナノレベルやより小さなレベルで物質の構造，組成，電子状態の制御を必要とし，また既存技術であってもナノレベルでの理解を進めること
によって大幅な改良・改善の余地を見出しうる場合が少なくないことを考えますと，ナノを観る光としての放射光の重要性と需要は益々高まっていくものと考えております．
（独）理化学研究所は今後とも量的・質的に高まっていく高輝度放射光への要求に対応すべく，（公財）高輝度光科学研究センターと協力し，SPring-8 を世界最高水準の放射光施設として維持・発展させて参りますが，引き続き兵庫県のご支援とご理解を要請する次第です．
昨年度から SACLA の供用が開始され，また今年度には神戸の京コンピュータの供用も開始されました．兵庫県の東と西の二つの最先端科学技術基盤施設利用への地元の皆様の積極的な参加をお願いし，そこからの皆様の飛躍的な発展を祈念いたしまして，お祝いの結びとさせていただきます．

提供: RIKEN/JASRI

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祝辞（公財）高輝度光科学研究センター
理事長
白川 哲久

「兵庫県ビームライン年報・成果集」創刊号の刊行にあたり，一言ご挨拶申し上げます．
SPring-8 は供用開始後 16 年目に入りました．その間に利用可能なビームラインは
10 本から 57 本まで整備され，学術利用・産業利用等多くの先端的なあるいは波及効
果の大きな成果が報告されました．その中で，兵庫県ビームラインは SPring-8 を誘致された兵庫県が産業利用振興のために先頭を切って整備されたビームラインでサンビーム（産業用専用ビームライン建設協同体）とともに，SPring-8 の産業利用を牽引する多くの利用成果を挙げて来られました．
SPring-8 は施設の運営に多額の国費が必要であり，その意義や有用性について国民の理解を得るためには，生み出した成果を広く社会に情報発信していくことが求められます．JASRI では，利用者の皆様からより多くの利用成果を報告頂けるように，利用実験終了後 3 年以内に査読付論文あるいは SPring-8 利用研究成果集などによる公開をお願いしています．兵庫県ビームラインでは従来の産業利用報告会や論文発表に加えて，新たに「兵庫県ビームライン年報・成果集」を創刊されることになり，SPring-8の利用成果をわかりやすい形で社会にＰＲして頂けるものと大きな期待をしております．
国 内 産業 の競 争 力強 化の た めに は， SPring-8 の 単独 利 用だ けで なく ， PF ，
NewSUBARU をはじめとする放射光施設や中性子施設 J ｰ PARC，スーパーコンピュ
ータ京などと相補的に利用することによって，さらに短期間に大きな成果が期待できると考えております．JASRI ではこれらの施設との連携をはかり，産業界をはじめ
SPring-8 利用者の皆様の利便性をさらに向上させるべき，利用者本位の視点に立って，具体的な施策を進めているところです．さらに，JASRI は SPring-8 に加えてＸ線自由電子レーザー（SACLA）についても特定放射光施設の登録施設利用促進機関として位置づけられており，（独）理化学研究所と連携しながら利用者選定や利用支援など具体的な利用制度を整備し，昨年 3 月から共用を開始しました．強力で位相のそろった
短パルスの新しいレーザー光の活用についてもよろしくお願い致します．
「兵庫県ビームライン年報・成果集」の創刊を機に，兵庫県ビームラインの活動がさらに発展されますことを心から祈念して，祝辞とさせて頂きます．

提供: RIKEN/JASRI

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巻

頭

言

（公財）ひょうご科学技術協会
放射光ナノテク研究所
所長
松井 純爾
理研・原研の共同チームによる次世代放射光施設の設置プロジェクトに筆者が参画
し，巣鴨の理研分室を頻繁に出入りしたのは，まだフォトンファクトリの企業専用ビームラインを活用している最中でした．
平成４年に，当時の県庁兵庫県知事公室で「県ビームライン構想」が，県下のみならず関西，全国産業利用を意識して企画立案されました．筆者がこちらに異動した平成 8 年末に輸送部，分光器，ハッチ，安全設備などの仕様作成を開始し，平成 10 年３月に工事が完了，光学調整を経て同年５月に放射光を初めて確認しました．早速，初期成果が求められ，思案のあげく，Si 単結晶の非対称反射を活用してＸ線の平行度を上げ，屈折イメージング実験を昆虫やカエル等で行ないました．結果，通常よりはるかに解像度の良いＸ線像が得られて，SPring-8 の威力をあらためて感じた訳です．
その後兵庫県は，この世界最高性能の高輝度放射光と，地域の産業が有する高性能
ナノ粒子コンポジット材料技術を直結して，県内企業の国際競争力を高めた産業の振興および集積を図るために，JST（科学技術振興機構）ファンドによる地域結集型共同研究事業「ナノ粒子コンポジット材料の基盤開発」を平成 16 年 1 月に開始しました．このプロジェクトには県内 24 企業を含む総勢 36 機関が参画しました．ナノ粒子の分散と凝集構造の評価のためには放射光による小角Ｘ線散乱技術が必須であることから，偏向電磁石光源による二本目のビームラインが必要となり，平成 17 年 4 月に設置工事に着工して，翌年 3 月にここでも放射光を確認しました．そして，この JST
プロジェクトによる地域 COE 構築の証しとして，SPring-8 敷地内に「兵庫県放射光
ナノテク研究所」を建設することを理研より認めていただきました．
上記のプロジェクト参加企業も含めて，今日まで実に多くの企業各社に利用いただ
きましたが，本成果集は，プロジェクト後の最近の利用課題について結果を纏めた最初の冊子です．兵庫県ビームラインの産業利用がここに至りましたのも，理研ならびに JASRI の温かいご支援の賜物と厚く感謝申し上げます．

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೥ɹɹɹใ

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ฌ‫ݝݿ‬ϏʔϜϥΠϯ BL08B2
BL08B2ʢਤ 1ʣ͸ɼฌ‫͕ݝݿ‬؅ཧӡӦ͢Δ࢈‫༻ۀ‬ͲʹऔΓࠐΈɼࣄ‫ۀ‬తഎ‫ܠ‬ɼ͢ͳΘͪਝ଎ͳࢼྉॲཧ

ϏʔϜϥΠϯͰ͋ΓɼBL24XU ͱͱ΋ʹɼ࢈‫ۀ‬ք΍େͱଌఆσʔλͷϑΟʔυόοΫΛҕୗͰ͖Δ‫࡞ڥ؀‬ΓֶͳͲͷ‫ʹؔػڀݚ‬ରͯ͠์ࣹޫͷར༻‫ػ‬ձΛఏ‫͠ڙ‬

Λߦͬͨɽ

͍ͯΔɽ
ͭ·ΓɼBL24XU ʹ͓͍ͯϏʔϜ‫༻ڙ‬Λ։࢝ͯ͠Ҏདྷɼࡐྉར༻ٕज़ͷߴ౓Խʹͱ΋ͳͬͯɼଟ͘ͷෳࡶ

1. ϏʔϜϥΠϯɾ࣮‫૷ݧ‬ஔͷ֓ཁ
1. 1 XAFSͳ‫ܥ‬ͷ߹ۚɼߴ෼ࢠϙϦϚʔɼଟ‫ݩ‬ૉ૊੒ͷ࣓ੑࡐྉͱࢎԽ෺ɼͳΒͼʹͦΕΒͷ෺࣭͕ଟ૚Խ͋Δ͍͸ࠞ࢈‫ۀ‬քʹ͓͍ͯͦͷར༻ൺ཰ͷߴ͍ XAFS ଌఆ૷߹͞ΕΔ͜ͱͰɼ͞Βʹ৽͍͠ಛੑΛ࣋ͬͨෳ߹ࡐྉ

ஔΛɼຊϏʔϜϥΠϯʹ͓͍ͯ΋੔උ͢Δ͜ͱͱͨ͠ɽΛ։ൃ͢Δ܏޲͕‫ͨͬ·ڧ‬ɽ͜ͱʹɼϙϦϚʔ΍ۚଐ͜ΕʹΑΓɼ෯޿͍࢈‫ۀ‬෼໺ͷϢʔβʔར༻͕ల։Ͱ

ࡐྉʹ௒ඍཻࢠΛ෼ࢄ͢Δ͜ͱͰɼ଱ຏ໣ੑɼਟੑɼ

͖ΔΑ͏ʹͳͬͨɽ

ૄਫੑɼ཭‫ܕ‬ੑɼ५‫׈‬ੑɼ෼ղੑɼ‫ٵ‬ணੑɼߗ౓ɼృ

۩ମతʹ౰εςʔγϣϯͰ͸ɼQuick-XAFS ΋‫ؚ‬Ίɼ෍೉қ౓ͱ͍ͬͨ෺ཧతੑ࣭͕มΘΔ͜ͱ͕෼͔Γɼඪ४తͳ XAFS ଌఆ‫ػ‬ೳΛఏ‫͍ͯ͠ڙ‬Δɽ2011 ೥౓৽͍͠‫ػ‬ೳΛ༗͢Δࡐྉͷ։ൃ͕੝Μͱͳͬͨ͜ͱΛʹ͓͍ͯ͸ɼ஝ి஑ࡐྉ΍৮ഔࡐྉͷ։ൃʹؔ͢Δར

ड͚ͯɼภ޲ి࣓ੴʢBMʣʹΑΔ৽͍͠ϏʔϜϥΠ༻՝୊͕ଟ͋ͬͨ͘ɽ஝ి஑ͷςʔϚͰ͸ɼి஑ͷߴϯ BL08B2 ͷ‫ݐ‬ઃʹΑΓ͜ΕΒͷχʔζʹରԠ͢Δ

༰ྔԽ΍௕ण໋ԽͷऔΓ૊Έͱͯ͠ਖ਼‫ࡐۃ‬ͷߏ଄ධՁ͜ͱͱͨ͠ɽͱΓΘ͚ɼখ̭֯ઢࢄཚ๏ʹΑΔඍཻࢠ

Λ໨తͱͨ͠՝୊Ͱ͋ͬͨɽ

෼ࢄ‫ܥ‬ϙϦϚʔࡐྉ΁ͷରԠͱɼϧʔνϯతղੳख๏

ਖ਼‫ࡐۃ‬ྉͷ‫༹ݻ‬ମߏ଄Λߏ੒͢Δ‫ݩ‬ૉछͷ૊Έ߹ΘΛ XAFSɼค຤̭ઢճં͋Δ͍͸Πϝʔδϯά෼໺ͳͤํ΍ɼఴՃ‫ݩ‬ૉͷޮՌɼ͋Δ͍͸ম݁৚݅౳Λม͑

ਤ 1. BL08B2 ϋονߏ੒–9–

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)ͨࡐྉͳͲͰߏ଄ධՁ͕ߦΘΕɼࡐྉ͕ࣔ͢ಛੑͱͷΑΓɼ֤छసҐʢΒͤΜసҐɼਕঢ়సҐɼ‫ج‬ఈ໘಺స૬ؔੑͷղ໌΍ɼੜ੒ϓϩηε΁ͷϑΟʔυόοΫͷ

ҐʣΛ޿ࢹ໺ʹ౉Γɼ઱໌͔ͭߴ෼ղೳͷίϯτϥε

औΓ૊Έʹ‫͞༻׆‬Εͨɽτ૾ͱͯ͠‫͞࡯؍‬Ε͓ͯΓɼϫΠυΪϟοϓ൒ಋମσࠓ‫ޙ‬͸ॆ์ిաఔʹ͓͚Δߏ଄มԽΛͦͷ৔‫Ͱ࡯؍‬
࣮ߦ͢Δͱ͍ͬͨμΠφϛΫεʹ஫໨͢Δར༻՝୊͕

όΠεͷϓϩηεվྑͷͨΊʹɼ‫و‬ॏͳ৘ใखஈͱ͠
ͯ‫͞༻׆‬Ε͍ͯΔɽ

૿͑Δ΋ͷͱ༧૝͞ΕΔɽ
·ͨ 2011 ೥౓‫ޙ‬൒Ͱ͸ɼߏ଄෺ͷࡐྉʹར༻͞Ε

1. 3 CT Πϝʔδϯά

Δమ߯εϥάࡐʹؔ͢Δ‫ڀݚ‬՝୊͕ελʔτͨ͠ɽమΠϝʔδϯά͓Αͼ CT Ͱ͸ɼτϙάϥϑΟಉ༷ʹ߯εϥάʹ‫·ؚ‬ΕΔ༗֐෺࣭Ͱ͋Δ࿡ՁΫϩϜʹؔ͠޿ࢹ໺ɼߴ෼ղೳͰͷࢼྉ಺෦ͷඇഁյ‫͕࡯؍‬ՄೳͰͯɼಛఆͷ߭෺૬தʹ‫ݻ‬ఆԽɼ҆ఆԽͤ͞Δٕज़Λ֬͋Δɽબ୒ՄೳͳޫࢠΤωϧΪʔ͸ɼ5ʙ30 keV ͷൣཱ͢Δ͜ͱͰɼ‫ʹڥ؀‬༏͍҆͠શͳεϥάࡐͱ͢Δऔ

ғͱ޿͘ɼࡐྉʹԠͨ͡࠷దͳ৚݅Ͱͷ࣮‫͕ݧ‬ՄೳͰΓ૊ΈͰ͋Δɽ͋Δɽࠓ‫ظ‬͸ਫ਼ີΰχΦεςʔδ΍ޫֶ‫ثػ‬ͷ੔උΛ͜ͷ‫ڀݚ‬։ൃͰ͸‫ࢠݪ‬Ϩϕϧͷߏ଄ධՁٕज़͕ඞཁ

ਐΊɼCT ଌఆ‫ػ‬ೳ΋ར༻Մೳͱͳ͍ͬͯΔɽ

ͱ͞ΕɼXAFS ͷ‫ޙࠓ͕༻׆‬΋‫ظ‬଴͞Ε͍ͯΔɽϋʔυߏ੒ͱͯ͠ɼࡱ૾෦ʹ͸Մࢹޫม‫ܕ׵‬ͷ X ઢΠϝʔδϯάΧϝϥγεςϜΛॆ࣮͍ͤͯ͞Δɽ‫ޫܬ‬ମ෦͸ɼൃޫྔΛՔ͙͜ͱ͕Ͱ͖Δ P43ʢGd2 O2 S:Tbʣ΍ɼ࢒ޫ‫ݮ‬ਰ࣌ؒͷ୹͍ YAGʢY3 Al5 O12 :CeʣΛඋ͍͑ͯΔɽ֦େഒ཰͸Ϩϯζ‫ܥ‬ͷ૊Έ߹ΘͤʹΑΓɼ౳ഒ͔Β໿ 5 ഒͷൣғͰબ୒ՄೳͰ͋ΔɽΧϝϥຊମͱͯ͠͸ɼେ໘ੵࡱ૾࢓༷ʢϐΫηϧαΠζ 9 µmɼ
ϐΫηϧ਺ 4008 × 2672ʣɼൺֱతߴ෼ղೳ࢓༷ʢϐΫηϧαΠζ 3.63 µmɼϐΫηϧ਺ 1920 × 1440ʣΛඋ͍͑ͯΔɽࡱ૾෦ʹ͍ͭͯ΋࣮‫ݧ‬໨తʹରͨ͠૊Έ߹Θͤߏ੒͕બ୒ՄೳͰ͋Δɽࠓ‫ظ‬ͷར༻՝୊ʹ͍ͭͯ͸ɼߴ෼ࢠࡐྉͱ݈߁৯඼

ͷ͕̎݅͋ͬͨɽ͍ͣΕ΋ɼCT ख๏Λಈత‫ʹ࡯؍‬Ԡ༻͢Δ಺༰Ͱ͋Γɼ݁Ռͱͯ͠઱໌ͳࡾ࣍‫ݩ‬ը૾৘ใਤ 2. ࣮‫ݧ‬ϋον 1 ಺ͷঢ়‫گ‬Λಘ͍ͯΔɽ
݈߁৯඼΁ͷԠ༻Ͱ͸ɼࣃͷΤφϝϧ࣭૚ʹ‫ܗ‬੒͞

1. 2 τϙάϥϑΟ

ΕΔॳ‫ظ‬ᴭৰ͕ɼΧϧγ΢Ϝ੒෼Λਁಁͤ͞Δ͜ͱͰ෯޿͍ϏʔϜΛ‫͖Ͱڅڙ‬Δภ޲ి࣓ੴޫ‫ͱݯ‬ਫ਼ີ Xઢ෼ޫޫֶ‫ܥ‬ͷ૊Έ߹Θͤɼ͓Αͼਫ਼ີΰχΦϝʔλͷར༻ʹΑΓɼ୯৭ X ઢτϙάϥϑΟ͕ՄೳͰ͋Δɽ

2011 ೥౓΋Ҿ͖ଓ͖ɼ൒ಋମ‫ج‬൘ࡐྉͷ݁থܽؕ΁ͷԠ༻‫͞ߦ࣮͕ڀݚ‬Εͨɽओʹ୸Խ‫ܔ‬ૉʢSiCʣʹؔ͢Δར༻՝୊Ͱ͋ΔɽSiC ݁থ͸ɼγϦίϯʹൺ΂ͯߴ଱ѹɼ௿ଛࣦɼߴԹಈ࡞ͳͲͷ఺Ͱ༏ΕͨσόΠεΛ࣮‫͢ݱ‬Δࡐྉͱͯ͠‫ظ‬଴͞Ε͍ͯΔɽ
͜ͷ࣮༻Խʹ͸ɼSiC ‫ج‬൘΍ΤϐλΩγϟϧບதʹ͓͍ͯߴີ౓ʹଘࡏ͢Δ݁থܽؕΛ཈੍ɼ੍‫͢ޚ‬Δ͜
ͱ͕՝୊ͱͳ͍ͬͯΔɽ͜ͷ‫ڀݚ‬։ൃʹ͓͍ͯɼ݁থ
ܽؕΛՄࢹԽՄೳͱ͢Δ์ࣹޫτϙάϥϑΟ͕‫͞༻׆‬Ε͍ͯΔɽBL08B2 ͷ୯৭ X ઢτϙάϥϑΟར༻ʹ࠶ੴփԽ͢ΔաఔΛɼಈ෺ͷࣃยࢼྉΛ༻͍ͯ‫͞࡯؍‬ΕΔࢼΈ͕ͳ͞Εͨɽ࠶ੴփԽ൓Ԡͷਐߦաఔ͕࣌ؒ
୯ҐͰ‫͞࡯؍‬Εɼճ෮ͷޮՌΛ೺Ѳ͢Δ͜ͱ͕Ͱ͖ͨɽ
ߴ෼ࢠࡐྉ΁ͷԠ༻Ͱ͸ɼγϡʔζιʔϧʹ࠾༻͞
ΕΔथࢷࡐྉʹ͍ͭͯɼม‫ܗ‬աఔΛಈతʹ‫͠࡯؍‬ɼྗֶతͳಛੑΛ೺Ѳ͢Δ͜ͱΛ໨తͱ࣮ͨ͠‫ߦ͕ݧ‬ΘΕͨɽ࣮ࡍͷ࢖༻৚݅ʹ૬౰͢ΔԠྗҹՃʹର͠ɼ‫ٵ‬ऩίϯτϥετ๏ʹΑΔ CT ‫ߦ͕࡯؍‬ΘΕͨɽ͍ͣΕͷ՝୊ʹ͍ͭͯ΋ɼCT ͰಘΒΕΔࡾ࣍‫ཱݩ‬ମߏ଄ͷ࣮ۭؒΠϝʔδϯά͸ɼࡐྉߏ଄ઃ‫ܭ‬ͷ৘ใͱͯ͠‫༻׆‬͞ΕΔ΋ͷͱ‫ظ‬଴͞Ε͓ͯΓɼ·ͨɼϑʔϦΤม‫׵‬Λඞཁͱ͠ͳ͍ࡐྉ಺෦ͷը૾ԽΛߦ͏͜ͱʹΑΓɼඞͣ͠΋์ࣹޫʹೃછΈͷͳ͍࢈‫ۀ‬քٕज़ऀʹ΋์ࣹޫͷ༗༻ੑΛΞϐʔϧͰ͖ΔΑ͏ʹͳͬͨɽ– 10 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

1. 4 খ֯ X ઢࢄཚʢSAXSʣ

1. 5 ค຤ճં

ඍཻࢠ෼ࢄ‫ܥ‬ϙϦϚʔࡐྉʢφϊཻࢠίϯϙδοτʣࠓ‫ظ‬͸ɼ৮ഔࡐྉͷಈత‫ؔ͢ʹ࡯؍‬Δར༻՝୊͕࣮

౳ͷ௕प‫ߏظ‬଄΍ɼඍཻࢠͷີ౓෼෍΍ू߹ʢΫϥεߦ͞Εͨɽ৮ഔ։ൃͰ͸ɼ‫׆‬ੑ͕ߴ͘ɼण໋ͷ௕͍ࡐλϦϯάʣঢ়ଶɼۭಎ෼෍ͳͲΛখ̭֯ઢࢄཚ๏Ͱଌ

ྉ͕‫ٻ‬ΊΒΕΔɽੴ༉Խֶ੡඼ͷ੡଄༻৮ഔͷΑ͏ʹఆͰ͖ΔϋʔυͷߏஙΛߦ͏͜ͱͱͨ͠ɽͦͷࡍɼඍଟ‫ݩ‬ૉͰߏ੒͞ΕΔࢎԽ෺৮ഔͷ৔߹ɼ࠷ऴతʹ‫ܗ‬੒ཻࢠ‫ܗ‬੒աఔ΍෼ࢄ‫ܥ‬ϙϦϚʔࡐྉͷৼಈɼԠྗҹՃ͞ΕΔෳ߹ࢎԽ෺ʹର֤ͯ͠ʑͷఴՃ‫ݩ‬ૉ͕༩͑ΔӨ౳ͷ֎෦༳ཚ৚݅Լʹ͓͚Δࡐྉߏ଄ͷʮͦͷ৔ʯଌ‫ڹ‬Λ໌֬ʹ͢Δ͜ͱ͕ॏཁͱͳΔɽ͜ͷ࠷ॳͷऔΓ૊ఆ͢Δ͜ͱΛ໨ࢦͨ͠ɽ·ͨɼখ̭֯ઢࢄཚʹՃ͑ͯΈͱͯ͠ɼ৮ഔࡐྉதʹమΛఴՃ͢Δ͜ͱͰ‫ܗ‬੒͞Ε޿̭֯ઢࢄཚͷճંσʔλͷऔಘΛಉ࣌ʹՄೳͱ͢Δ

Δ݁থ૬ͷධՁ͕ࢼΈΒΕͨɽߴԹॲཧ৚݅ʢ400ʙ600 ˆʣͰͷ݁থ૬ͷมԽΛ͜ͱͰɼ෯޿͍஌‫ݟ‬ΛಘΔ͜ͱͱͨ͠ɽ

௥੻͢Δ໨తͰɼBL08B2 ͷେ‫ܕ‬ճં૷ஔʹߴԹՃ೤࿍ͱ PILATUS ‫ݕ‬ग़‫ث‬Λ௥Ճ౥ࡌ͢Δվ଄ΛߦͬͨɽϢʔβʔ͕ඞཁͱ͢Δ֯౓෼ղೳੑೳͱ֯౓૸ࠪ৚݅
ͱΛߟྀͨ͠Χϝϥ௕ͷઃ‫ܭ‬΍ɼ࣌෼ׂଌఆ‫ػ‬ೳΛ࣮‫͢ݱ‬ΔͨΊͷଌఆγεςϜͷ։ൃΛߦ͍ɼ2011 ೥౓‫ޙ‬൒ΑΓ‫༻ڙ‬Λ։࢝ͨ͠ɽ
ͦͷ৔‫࡯؍‬ͷ࣮‫ʹݧ‬ΑΓɼ৮ഔࡐྉͷম݁৚݅૬౰
ͷ৚݅ʹରͯ͠ɼߏ଄૬సҠʹΑΔ΋ͷͱߟ͑ΒΕΔ
݁থ૬ͷมԽΛճંϓϩϑΝΠϧ্Ͱଊ͑Δ͜ͱʹ੒ޭͨ͠ɽಉ༷ʹɼՃ೤৚݅ԼͰͷ݁থߏ଄มԽΛ࣌෼ׂͰ௥
੻͢Δ಺༰ͱͯ͠ɼ೪ɾ઀ணࡐྉ΁ͷར༻՝୊͕࣮ߦ
͞ΕͨɽҎ্ͷར༻՝୊Λ௨ͯ͡ɼBL08B2 ͕༗͢Δ
ਤ 3. ࣮‫ݧ‬ϋον 2 ಺ͷঢ়‫گ‬ճંଌఆ‫ػ‬ೳ͕ಈత‫ʹ࡯؍‬ରͯ͠༗ޮͳπʔϧͱͳΓ

SAXS Χϝϥ௕ͷ෯޿͍બ୒ੑʢ500ʙ6000 mm ͓Αͼ 15600 mmʣͱਝ଎ͳΧϝϥ௕੾Γସ͑ɼͳΒ

͏Δ͜ͱΛ࣮ূͰ͖ͨɽ

2. ར༻ঢ়‫گ‬ͼʹɼछʑͷଌఆख๏ʢSAXS/WAXS ಉ࣌ଌఆɼGI-

2011 ೥౓͸ɼ஝ి஑ࡐྉ΍৮ഔ౳ɼΫϦʔϯΤωϧ

SAXSɼRheo-SAXSɼAnomalous-SAXSɼXAFS/WAXS ಉ࣌ଌఆʣΛఏ‫͢ڙ‬Δ͜ͱͰɼ࢈‫ۀ‬քͷ༷ʑͳଌఆχʔζʹରԠ͍ͯ͠Δɽࠓ‫ظ‬͸ɼϏʔϜΞϥΠϝϯτͱࢼྉަ‫׵‬ΛࣗಈԽ
͢Διϑτ΢ΣΞΛ੔උͨ͜͠ͱʹΑΓɼϢʔβʔͷϏʔϜλΠϜར༻ͷޮ཰Խͱૢ࡞ͷ؆қԽΛ࣮‫͠ݱ‬
ͨɽ·ͨۙ೥ɼి஑ࡐྉΛ͸͡Ίͱͨ͠ΤωϧΪʔࡐྉ։ൃͷχʔζ͕ߴ·͍ͬͯΔ͜ͱ͔Βɼ͜ΕΒͷ෺ੑɾߏ଄ධՁΛͦͷ৔‫Ͱ࡯؍‬Մೳͱ͢Δ Quick-

XANES/SAXS/WAXS ಉ࣌ଌఆΛ੔උͨ͠ɽར༻Մ
ೳͳΤωϧΪʔൣғ͸ 8ʙ25.5 keVɼಁա๏͋Δ͍͸‫ޫܬ‬๏ʹΑΔ 10 ඵ࣌෼ׂଌఆ͕ՄೳͰ͋Δɽࠓ‫ޙ‬͸ɼར༻ՄೳͳΤωϧΪʔൣғͷ֦ுͱ Quick ଌఆͷߴ଎ԽΛ‫ݕ‬౼͍ͯ͠ΔɽΪʔ࢈‫͚͓ʹۀ‬Δར༻՝୊͕૿͑ͭͭ͋Δ܏޲Ͱ͋ͬ
ͨɽϚγϯλΠϜͷ಺༁͸ɼ࢈‫ۀ‬քϢʔβʔʹΑΔར
༻՝୊ͱͱ΋ʹɼ࣮‫ݧ‬४උͷͨΊͷελσΟɼϢʔβʔχʔζΛຬͨͨ͢Ίͷ৽‫ػ‬ೳ։ൃΛ໨తͱͨ͠ར
༻՝୊ɼ‫ͱۀا‬ͷ‫ڞ‬ಉ‫ڀݚ‬՝୊Λର৅ͱ͍ͯ͠Δɽ

2011 ೥౓ͷશར༻೔਺ͷ͏ͪɼ໿ 50 %ΛϢʔβʔར༻՝୊ʹఏ‫ͨ͠ڙ‬ɽϢʔβʔར༻՝୊ͷ෦෼͸ɼXAFS
͕ 32 %ɼখ֯ X ઢࢄཚͰ 30 %ɼτϙάϥϑΟͰ 15%ɼค຤ճંͰ 16 %ɼΠϝʔδϯάͰ 7 %ͷ಺༁Ͱ͋ͬͨɽ͜ͷ͏ͪ੒Ռઐ༗՝୊͸ɼ18 %Λ઎Ί͍ͯΔɽ
·ͨଌఆ୅ߦͷར༻͸ɼར༻՝୊ͷ 9 %૬౰Ͱ͋ͬ
ͨɽଌఆ୅ߦར༻ʹ͸ɼฌ‫͕ݝݿ‬ओ࠵͢Δิॿࣄ‫੍ۀ‬౓Λར༻ͨ͠தখ‫͔ۀا‬ΒͷఏҊ՝୊΋‫ؚ‬Ήɽຊࣄ‫ۀ‬͸ɼ஍Ҭ࢈‫͚͓ʹۀ‬Δ์ࣹޫར༻ͷ‫׆‬ੑԽɼ৽ͨͳར
༻‫ۀا‬ͷൃ۷ɼ์ࣹޫΛར༻͢Δ‫ऀڀݚ‬ҭ੒Λ໨తͱͨ͠΋ͷͰ͋Δɽ

– 11 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)͓͍ͯϛΫϩϯΦʔμʔͷҐஔ෼ղೳͰͷߏ଄ධՁ๏

3. ࠓ‫ޙ‬ͷ‫ܭ‬ը
2012 ೥౓ʹ͓͍ͯ΋ɼ࢈‫ۀ‬քʹ͓͚Δ์ࣹޫར༻Λࢧԉ͢Δ‫׆‬ಈΛ‫ܧ‬ଓ͢Δɽͦͷ۩ମతͳྫͱͯ͠ɼϢʔβʔ͕‫ٻ‬ΊΔ৽‫ػ‬ೳͷ੔උ‫׆‬ಈ͕͋Δɽখ̭֯ઢࢄཚ
Ͱ͸ɼଞͷϏʔϜϥΠϯͰ‫ʹط‬ར༻։͍࢝ͯ͠Δࣔࠩ
૸ࠪ೤ྔ෼ੳ (DSC) ͱͷಉ࣌ଌఆʢDSC/SAXS/WAXSಉ࣌ଌఆʣͷ੔උཁ๬͕ଟ͋͘ΔͨΊɼฌ‫ݝݿ‬ϏʔϜϥΠϯͰ΋ߴ෼ࢠ‫ࡐܥ‬ྉ։ൃΛߦ͏‫ۀا‬Λλʔήοτʹ੔උΛߦ͏༧ఆͰ͋ΔɽXAFS Ͱ͸ɼΠϝʔδϯάଌఆ๏ͱ೾௕૸ࠪͱΛ૊Έ߹Θͤͨɼೋ࣍‫ݩ‬ΠϝʔδΛ࣮‫͢ݱ‬Δ͜ͱΛ໨తͱ͍ͯ͠Δɽ·ͨɼϙϦΩϟϐ
ϥϦूޫϨϯζΛ༻͍ͨूޫޫֶ‫ܥ‬Λ੔උ͢Δ༧ఆͰ
͋Δɽ10ʙ20 µm αΠζͷूޫʹΑΓɼࢼྉ্Ͱͷτʔλϧ‫౓ڧ‬΋ൺֱతେ͖͍ϏʔϜΛ‫ܗ‬੒͢Δɽ‫ޫܬ‬̭ઢϚοϐϯάଌఆ΍ߴҐஔ෼ղೳ XAFS ͷ‫ػ‬ೳΛॆ࣮ͤ͞Δ༧ఆͰ͋Δɽฌ‫ޫࣹ์ݝݿ‬φϊςΫ‫ॴڀݚ‬ԣࢁ࿨࢘ɼཥɹཕɼ‫܂‬ຊ࣎ੜɼ࣫‫ྑݪ‬ণɼদҪ७࣐

ϯά XAFS ‫ػ‬ೳΛ੔උ͢Δ༧ఆͰ͋Δɽ޿͍ྖҬʹ– 12 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

ฌ‫ݝݿ‬ϏʔϜϥΠϯ BL24XUฌ‫Ͱݝݿ‬͸ɼฏ੒ 8 ೥ 10 ݄ʹ SPring-8 ʹ͓͚Δ‫ڞ‬

A2ɼޫֶϋον B2ɼ࣮‫ݧ‬ϋον B1ʣɼඍখྖҬ෼ੳ༻ϏʔϜϥΠϯ͔Βͷ์ࣹޫ‫͕༻ڙ‬։࢝͞Εͨ௚‫ޙ‬ͷʹॏ఺Λஔ͍ͨΤϯυεςʔγϣϯΛӡ༻͍ͯ͠Δɽ

ฏ੒ 9 ೥౓ʹɼ࠷ॳͷઐ༻ϏʔϜϥΠϯͰ͋Δʮฌ‫ݿ‬

2011 ೥౓Ͱ͸ɼ࣮‫ݧ‬ϋον A1 ʹ͓͚Δ Bonse-Hart‫ݝ‬ϏʔϜϥΠϯʢBL24XUʣʯΛ‫ݐ‬ઃͨ͠ɽ̔ͷࣈ‫ܕ‬‫ۃܕ‬খ֯ࢄཚޫֶ‫ܥ‬ɼޫֶϋον B2 ʹ͓͚ΔϚΠΫΞϯδϡϨʔλͱμΠϠϞϯυ݁থʹΑΔτϩΠΧํϩϏʔϜ XAFS ޫֶ‫ܥ‬ͷຊ֨ӡ༻͕։࢝͞ΕɼϚΠࣜΛ࠾༻͢Δ͜ͱʹΑΓɼҟͳͬͨ̏छͷ࣮‫ݧ‬Λ̏ͭΫϩϏʔϜޫֶ‫ܥ‬Λར༻ͨ͠डୗ෼ੳ΋։࢝͞Εͯͷ࣮‫ݧ‬ϋονʹ͓͍ͯಉ࣌ฒߦͰ࣮ࢪͰ͖ΔγεςϜ͍Δɽ

Λߏங͢Δ͜ͱͰɼ࢈‫ۀ‬քϢʔβʔΛத৺ʹଟ͘ͷ‫ݚ‬

1. ϏʔϜϥΠϯɾ࣮‫૷ݧ‬ஔͷ֓ཁ‫ڀ‬՝୊࣮‫͞ࢪ࣮͕ݧ‬ΕͨɽϚΠΫϩϏʔϜΛ༻͍ͨ‫ॴہ‬෼ੳٕज़ͷҰ૚ͷߴ౓Խͱɼখ֯ɾ‫ۃ‬খ֯ࢄཚଌఆ΁ͷରԠʹॏ఺తʹऔΓ

1. 1 A ϒϥϯν૊Ή͜ͱΛ໨తʹɼ̏ϋονߏ੒Λऴྃ͠ɼA ϒϥϯ্ड़ͷ෼ޫ‫ث‬վྑͷ݁ՌɼϒϥϯνͷϏʔϜ‫౓ڧ‬͸νͱ B ϒϥϯνͷೋͭͷλϯσϜϋονߏ੒ʹมߋ͢

2.5 × 1011 ޫࢠ/ඵఔ౓ͱͳΓɼ໿ 30 %ͷ޲্͕ୡ੒

ΔϏʔϜϥΠϯվ଄Λߦͬͨʢਤ 1ʣɽA ϒϥϯνʹ͓͞Ε͍ͯΔɽ·ͨɼ݁থϗϧμʔͷվྑʹΑΓϏʔϜ͍ͯ͸Ж-SAXS ౳ʹΑΓബບࡐྉதͷφϊཻࢠͷ෼ͷ҆ఆੑ͕޲্͠ɼ1 ೔͋ͨΓͷมಈྔ͸ɼҐஔɼ‫ڧ‬෍ɼཻ‫ܘ‬ɼφϊϙΞɼ഑޲ੑ౳ͷධՁΛల։͢Δ͜ͱ౓‫ ਺ʹڞ‬%Ҏ಺ʹऩ·͍ͬͯΔɽ

ͱ͠ɼB ϒϥϯνʹ͓͍ͯ͸࣮༻ϨϕϧͷφϊϏʔϜA ϒϥϯνͷ࣮‫ݧ‬ϋον͸఻ൖ௕ͷ௕͍λϯσϜγεςϜΛߏங͠ɼ͞·͟·ͳࡐྉʹ͍ͭͯαϒ 100ϋονΛߏ੒͓ͯ͠Γɼ࣮‫ݧ‬ϋονؒ͸ஈ֊తʹଠ͘nm ྖҬͷ݁থੑධՁɼԠྗղੳɼඍྔ‫ݩ‬ૉ෼ੳ౳Λͨ͠ਅۭ༌ૹύΠϓͰ઀ଓ͞Ε͍ͯΔɽ͜ͷಛ௃Λརల։͢Δ͜ͱͱͨ͠ɽ͢ͳΘͪɼಉ࣌ʹ์ࣹޫ‫څڙ‬Λ༻͠ɼ࣮‫ݧ‬ϋον A1 Ͱ͸ค຤ճં૷ஔɼ‫ۃ‬খ֯ࢄཚՄೳͱ͍ͯ͠Δ֤ϒϥϯνʹ͸ɼͦΕͧΕೋͭͷ࣮‫ݧ‬૷ஔͷӡ༻Λߦ͓ͬͯΓɼBonse-Hart ‫ܥֶޫܕ‬Λརϋον͕λϯσϜʹ഑ஔ͞Ε͓ͯΓʢ࣮‫ݧ‬ϋον A1ɼ

ਤ 1. BL24XU ϋονߏ੒– 13 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)༻ͨ͠‫ۃ‬খ֯ࢄཚ૷ஔͰ͸ɼ໿ 0.2 µm−1 ͷ෼ղೳ͕ϯδϡϨʔλͷߴௐ೾Λ 5 keV ຖͰΤωϧΪʔΛબಘΒΕ͓ͯΓɼϢʔβʔར༻͕։࢝͞Ε͍ͯΔɽ

୒ͯ͠ӡ༻͍ͯ͠Δʢ1 ࣍ޫ͕ 10 keVʣɽ

·ͨɼA2 ϋον͸௕͍఻ൖ௕Λ࣋ͭͨΊɼϚΠΫ࣮‫ݧ‬ϋον͸̎ͭͷλϯσϜ഑ஔͰߏ੒͞Ε͓ͯΓɼϩϏʔϜ‫ܗ‬੒ʹ༗རͰ͋Δɽ͜͜Ͱ͸ࣼೖࣹճં૷

্ྲྀଆͷޫֶϋον*1 B2 Ͱ͸ɼߴۭؒ෼ղೳɼߴ࣌ؒ

ஔɼϚΠΫϩϏʔϜར༻ޫֶ‫ܥ‬Λӡ༻͍ͯ͠ΔɽϚΠ෼ղೳʹಛԽͨ͠ར༻ͷଞɼ࠷্ྲྀʹઃஔͨ͠ XAFSΫϩϏʔϜར༻ޫֶ‫Ͱܥ‬͸ɼαΠζ໿ 15 µm ͷϚΠεςʔγϣϯͷӡ༻Λߦ͍ͬͯΔɽԼྲྀଆͷ࣮‫ݧ‬ϋοΫϩϏʔϜ‫ܗ‬੒͕Մೳͱͳ͓ͬͯΓɼैདྷͰ͸ෆՄೳν B1 Ͱ͸ɼߴ֯౓෼ղೳʹಛԽͨ͠ϚΠΫϩϏʔϜͰ͋ͬͨඍখྖҬ෼ੳ΁ͷల։͕Մೳͱͳ͍ͬͯΔɽར༻ΛՄೳͱ͍ͯ͠Δɽ࣮ࡍʹ WAXD ଌఆͷϢʔβʔར༻͕ߦΘΕ͓ͯΓɼ؅ཧ͸ओʹฌ‫ཱݝݿ‬େֶ X ઢޫֶߨ࠲͕୲౰ͯ͠

B ϒϥϯνͱͷ༗‫ػ‬తɾ૬ิతͳ‫͕༻׆‬Մೳͱͳͬͯ

͓ΓɼϢʔβʔར༻͚ͩͰͳ͘ɼߨ࠲ʹΑΔֶज़‫ڀݚ‬͍Δɽ΋ߦͳΘΕ͍ͯΔɽ1) ޫֶϋον B2 ɹ XAFS εςʔγϣϯ஝ి஑൓ԠͷϝΧχζϜղ໌ɼಛʹ 3d ભҠۚଐΛ‫ؚ‬Ήਖ਼‫ࡐۃ‬ͷԽֶঢ়ଶʹؔ͢ΔධՁΛ໨తͱͨ͠ϚΠΫϩ XAFS ͷ੔උΛਐΊͨɽޫֶ‫ܥ‬෦෼Ͱ͸ɼߴً౓์ࣹޫͱϛϥʔूޫૉࢠʹΑΓɼࢼྉ໘಺ʹ͓͚Δ
Ґஔ෼ղೳͱͯ͠ 1ʙ3 µmɼ‫ ͯ͠ͱ౓ڧ‬109 ʙ1010 ޫࢠ/ඵͷ̭ઢϚΠΫϩϏʔϜΛ࣮‫ͨ͠ݱ‬ɽ͞Βʹࢼྉͷਂ͞ํ޲ʹ͓͚Δ෼ղೳ΋ߟྀͨ͠ଌఆ‫ܥ‬Λ‫ݕ‬౼தͰ͋Δɽ͜ΕΒΛར༻͠ɼਖ਼‫Ͱ্ࡐۃ‬ͷ෦ҐΛ۠ผͨ͠ධՁͱͱ΋ʹɼߏ੒ཻࢠͷৄࡉͳධՁʹԠ༻Λߦ͍ͬͯ͘ɽຊ࣮‫ݧ‬γεςϜʹΑͬͯɼి‫ؾ‬༰ྔ΍αΠΫϧར༻ʹର͢Δి஑ण໋ͳͲͷॹಛੑΛɼ‫ࢠݪ‬Ϩϕϧͷߏ଄΍ిࢠ‫ܥ‬ͷঢ়ଶ͔Βཧղ͠ɼ͞Βʹࡐྉઃ‫ʹܭ‬

ਤ 2. ࣮‫ݧ‬ϋον A1 ಺ͷঢ়‫گ‬͓͚Δࢦ਑͕ಘΒΕΔ͜ͱΛ‫ظ‬଴͍ͯ͠Δɽ·ͨ‫ࢠݪ‬഑Ґߏ଄ͷมԽΛৄࡉʹௐ΂Δ໨తͰɼۭؒ෼ղೳͱ
‫͍ߴʹڞ‬ΤωϧΪʔ෼ղೳ΋ซͤ࣋ͭ XAFS ‫ػ‬ೳͷ੔උ΋‫ܭ‬ը͍ͯ͠ΔɽϚΠΫϩ XAFS ͷຊ֨తͳ‫ڙ‬༻։࢝͸ 2012 ೥Լ‫͋Ͱظ‬Δɽ2) ޫֶϋον B2 ɹϚΠΫϩϏʔϜεςʔγϣϯϚΠΫϩϏʔϜεςʔγϣϯͰ͸ɼ্ྲྀଆʹଟ໨తޫֶϕϯνɼԼྲྀଆʹ൚༻‫ܕ‬ϚΠΫϩϏʔϜ෼ੳ૷ஔΛ഑͓ͯ͠Γɼ্ྲྀଆͰ͸ओʹֶज़‫ڀݚ‬ͷͨΊͷޫֶ‫ܥ‬΍ɼϚΠΫϩΠϝʔδϯάޫֶ‫ܥ‬Λ༻͍ͨϢʔβʔར༻͕ల։͞Ε͍ͯΔɽ
ֶज़‫Ͱڀݚ‬͸ɼX ઢ‫ݦ‬ඍޫֶ‫ܥ‬ͷ‫ڀݚ‬΍ɼ৽‫ֶޫن‬ૉࢠͷ։ൃ౳Λߦ͓ͬͯΓɼಛʹԁ‫ܗ‬ଟ૚ບκʔϯϓ
ਤ 3. ࣮‫ݧ‬ϋον A2 ಺ͷঢ়‫گ‬Ϩʔτͷ։ൃʹ͓͍ͯ͸ɼߴޮ཰͔ͭճં‫ݶ‬քʹ͍ۙੑೳΛ࣋ͭूޫੑೳΛୡ੒ͨ͜͠ͱΛ֬ೝͨ͠ɽ·ͨɼϚΠΫϩΠϝʔδϯάޫֶ‫Ͱܥ‬͸ɼߴ෼ղೳ CT ‫ͼٴ‬ɼ

1. 2 B ϒϥϯνߴ଎౓ CT ͷ੔උΛߦ͍ɼߴ଎౓ CT Ͱ͸ɼϦΞϧλ

B ϒϥϯνͷ෼ޫ‫ث‬͸ਫฏΦϑηοτͷγϦίϯ̎݁থ෼ޫ‫͋Ͱث‬Γɼ௨ৗ͸ 10 keVʙ30 keV ͷؒͰΞ– 14 –∗1 ෼ޫ‫ث‬ͷ࢓্༷ɼന৭ϏʔϜͷར༻΋ՄೳͰ͋Δ͜ͱ͔Βʮޫֶϋονʯͱ‫ݺ‬শ͢Δ͜ͱͱͳ͍ͬͯΔɽฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

ਤ 4. ޫֶϋον B2 ಺ͷঢ়‫گ‬

ਤ 5. ࣮‫ݧ‬ϋον B1 ಺ͷঢ়‫گ‬ΠϜͰͷ಺෦ߏ଄‫͕࡯؍‬Մೳͳ̐࣍‫ ݩ‬CT ͷϢʔβʔʢ൒ಋମɼۚଐɾແ‫ػ‬ɼ༗‫ػ‬ɾߴ෼ࢠɼઌ୺ෳ߹ࡐྉ

ར༻Λ։࢝ͨ͠ɽ

౳ʣʹ͍ͭͯɼαϒ 100 nm ྖҬͷ݁থੑධՁɼԠྗղ

൚༻ X ઢϚΠΫϩϏʔϜ෼ੳ૷ஔͰ͸ɼ࢖༻͢Δ

ੳɼඍྔ‫ݩ‬ૉ෼ੳ౳Λల։͢Δ͜ͱͱͨ͠ɽ·ͨɼϋοX ઢϚΠΫϩϏʔϜ͸ɼαΠζɼ‫౓ڧ‬ɼൃࢄ֯Λ༻్ν A1ɼA2 Ͱ͸ɼµ-SAXSɼGrazing Incidence SAXSʹԠͯ͡બ୒͢Δ͜ͱ͕Ͱ͖ɼ࠷খαΠζ 120 nm ͷ

(GI-SAXS)ɼUltra-SAXS (USAXS) ౳ʹΑΓബບࡐϏʔϜ͕࢖༻ՄೳͰ͋Δɽख๏ͱͯ͠͸ɼ޿֯ X ઢճྉதͷφϊཻࢠͷ෼෍ɼཻ‫ܘ‬ɼφϊϙΞɼ഑޲ੑ౳ͷંɼ‫ޫܬ‬෼ੳͷಉ࣌ଌఆΛՄೳͱ͓ͯ͠Γɼ2011 ೥ධՁΛల։͢Δ͜ͱͱͨ͠ɽ
ୈ̍‫ܭظ‬ըͰ͸ɼߴً౓์ࣹޫར༻‫ڀݚ‬ͷ࢈‫ۀ‬ք΁౓Ͱ͸ಉ࣌Ϛοϐϯάଌఆ͕ՄೳͳγεςϜͷ੔උΛͷී‫ٴ‬Λ‫׆‬ಈ໨తͷओ‫ʹ؟‬ਾ͍͕͑ͯͨɼୈ̎‫ܭظ‬ըߦͬͨɽ3) ࣮‫ݧ‬ϋον B1 ɹ४ฏߦϚΠΫϩϏʔϜεςʔγϣϯओʹ൒ಋମ݁থͷඍখྖҬߴ‫౓ײ‬࿪Έ‫ܭ‬ଌΛ໨తʹɼ४ฏߦ X ઢϚΠΫϩϏʔϜճં࣮‫ݧ‬Λߦ͍ͬͯΔɽϚΠΫϩϏʔϜ͸ɼ
ʢ+, −, −, +ʣ഑ஔͷ̎ͭͷνϟϯωϧΧοτ݁থͱϕϯτγϦϯυϦΧϧϛϥʔΛ૊Έ߹Θͤͯ‫ܗ‬੒͍ͯ͠ΔɽϢʔβʔ͸γϦϯυϦ
Χϧϛϥʔͷަ‫׵‬΍ୀආͰɼҎԼͷ̏छͷϏʔϜ͔Βબ୒࣮ͯ͠‫͖Ͱݧ‬Δɽޫֶ‫ ܥ‬1 ͸ɼϏʔϜαΠζ 0.8µm × 1.7 µmɼൃࢄ֯ 25 radɼޫֶ‫ ܥ‬2 ͸ɼϏʔϜαΠζ 0.4 µm × 1.0 µmɼൃࢄ֯ 50 radɼޫֶ‫ ܥ‬3͸ɼϏʔϜαΠζ 35 µm × 35 µmɼൃࢄ֯ 3.5 rad Ͱ

͋Δɽয఺ʹ͸ߴਫ਼౓ θ−2θ ճં‫͕ܭ‬ઃஔ͞ΕɼϩοΩϯάΧʔϒ΍‫ۭؒࢠ֨ٯ‬ϚοϐϯάͷҐஔґଘੑΛଌఆͰ͖ΔɽϑϥοΫε͸͢΂ͯ 107 ޫࢠ/ඵఔ౓Ͱ͋ΔɽͰ͸ɼBL08B2 ͱͷ૬‫ޓ‬ར༻ʹΑΓࣾձతʹΠϯύΫ
τͷߴ͍੒ՌΛ૑ग़͢ΔͨΊɼࢀըऀ਺Λదਖ਼‫ن‬໛ʹ཈͑ɼςʔϚΛಛԽͨ͠ઌ୺త‫ڀݚ‬ͷਪਐʹ࣠଍ΛҠ͢͜ͱͱͨ͠ɽ

BL24XU ͷಛ௕Λ࠷େ‫ʹݶ‬ੜ͔͠ɼ࢈‫ۀ‬քͷଟ༷ͳࡐྉධՁͷཁ੥ʹରԠͰ͖Δ̭ઢϏʔϜΛఏ‫͢ڙ‬Δ
͜ͱʹΑΓɼ࢈‫ۀ‬քͷχʔζʹਝ଎ɾॊೈʹରԠͰ͖Δ࢓૊ΈΛཱ֬͠ɼ์ࣹޫͷ࢈‫ۀ‬ར༻ଅਐΛ໨ࢦ͠ਚྗ͖ͯͨ͠ɽ
·ͨɼ֤छ‫ݚ‬मձɾٕज़૬ஊɾडୗ‫౓੍ڀݚ‬ͷ࣮ࢪ౳Λ௨ͯ͡ɼ‫ཱʹ಺ݝ‬஍͢Δಛ௕͋Δଟ਺ͷத‫ݎ‬ɾதখ‫ۀا‬΍஍৔࢈‫΁ۀ‬ͷ์ࣹޫར༻Λଅਐ͠ɼ์ࣹޫར
༻ͷ੄໺ͷ֦େʹऔΓ૊Ήͱͱ΋ʹɼؔ੢஍Ҭɼ͞Βʹ͸શࠃͷઌ୺తٕज़։ൃΛਐΊΔ‫ʹۀا‬΋‫ݝ‬ϏʔϜϥΠϯΛੵ‫ۃ‬తʹఏ‫͠ڙ‬ɼ৽ࡐྉͷධՁɾ։ൃ౳ʹଟ͘ͷ஌‫ݟ‬Λ஝ੵ͍ͯ͠Δɽ

3. ࠓ‫ޙ‬ͷ‫ܭ‬ը

2. ར༻ঢ়‫گ‬ࠓ‫ޙ‬΋֤छͷଌఆ૷ஔΛϚΠφʔνΣϯδ͠ɺଌఆ‫ڀݚ‬ख๏ͱͯ͠͸ɼϋον B1ɼB2 ʹ͓͍࣮ͯ༻Ϩ‫ثػ‬ͷॆ࣮ΛਤΓ͍ͨɽ্‫ه‬ͷΑ͏ͳऔΓ૊ΈΛ͞ΒϕϧͷφϊϏʔϜγεςϜΛߏங͠ɼ͞·͟·ͳࡐྉ– 15 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)ʹ‫ܧ‬ଓ͢Δ͜ͱͰɼSPring-8 Λத֩ͱ͢Δ೻ຏՊֶฌ‫ཱݝݿ‬େֶେֶӃ ෺࣭ཧֶ‫ڀݚ‬ՊެԂ౎ࢢΛࠃࡍతͳޫՊֶٕज़‫͢ʹ఺ڌڀݚ‬Δ͜ͱ΁ߴ໺ल࿨ɼ௡ࡔՂ޾ɼ࿜ౡɹ༃

ͷߩ‫ݙ‬Λ໨తͱ͍ͯ͠Δɽ

SPring-8 ͱ͍͏‫و‬ॏͳ‫ཱ͕ݯࢿڀݚ‬஍͢Δ஍ํࣗฌ‫ޫࣹ์ݝݿ‬φϊςΫ‫ॴڀݚ‬࣏ମͱͯ͠ɼͦͷ໾ׂͱ੹೚ͷେ͖͞Λೝࣝ͠ɼ‫ݝ‬ͷԣࢁ࿨࢘ɼཥɹཕɼ‫܂‬ຊ࣎ੜɼ࣫‫ྑݪ‬ণɼ஛ా৾‫ޗ‬ɼՊֶٕज़੓ࡦͱ΋࿈ಈͤ͞ͳ͕Βɼฌ‫ݝݿ‬ϏʔϜϥΠদҪ७࣐ϯͷӡӦʹࠓ‫ޙ‬΋౒ྗΛ܏஫ͯ͠Ώ͘ɽ– 16 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

ࢪઃӡ༻͓Αͼར༻ঢ়‫گ‬ฌ‫Ͱݝݿ‬͸ɼ์ࣹޫ‫͚͓ʹڀݚ‬Δ࢈‫ۀ‬ར༻Λଅਐͨ͢͠ɽ౰‫ॴڀݚ‬͸ɼ‫ݝ‬ઐ༻ϏʔϜϥΠϯʹΑΔଟछଟ

ΔͨΊɼ1998 ೥౓ʹ̍ຊ໨ͷ‫ݝ‬ઐ༻ϏʔϜϥΠϯͰ༷͋ͳ෼ੳख๏Λิ‫͢׬‬Δ֤छ̭ઢճં૷ஔɼిք์ग़

Δ BL24XU ͷ‫༻ڙ‬Λ։࢝͠ɼϚΠΫϩϏʔϜΛ࢖ͬ‫ݦࢠిࠪ૸ܕ‬ඍ‫ڸ‬ɼ૸ࠪϓϩʔϒ‫ݦ‬ඍ‫ڸ‬ɼ‫ڞ‬য఺Ϩʔ֤ͨछΠϝʔδϯάɼճં૷ஔ౳Λ‫ͯ͠༻׆‬ɼ൒ಋମβʔϥϚϯ‫ݦ‬ඍ‫Ͳͳڸ‬ͷ෼ੳ૷ஔ΍ࢼྉ४උࣨɼେ

ࡐྉɼੜମࡐྉɼߴ෼ࢠࡐྉ౳෯޿͍ࡐྉ෼໺Ͱͷ‫ہ‬ֶ΍‫ͱۀا‬ͷ‫ڞ‬ಉ‫ڀݚ‬Λߦ͏ͨΊͷ‫ڞ‬ಉ‫ࣨڀݚ‬ɼձٞॴ෼ੳʹରԠ͠ɼ۩ମతͳ‫ڀݚ‬੒ՌΛ‫͖ͨͯ͛ڍ‬ɽࣨͳͲΛඋ͑ͨଟ‫ػ‬ೳࢪઃͰ͋ΓɼίʔσΟωʔλʔͦͷ‫ޙ‬ɼ࢈‫ۀ‬քʹ͓͍ͯ͸ɼΑΓ੡඼Խʹ௚݁͢Δ

΍‫ڀݚ‬һ͕഑ஔ͞Εɼར༻‫ۀا‬౳͔Βͷ͞·͟·ͳ૬ٕज़։ൃஈ֊Ͱͷࡐྉ෼ੳχʔζ͕૿Ճɼ·ͨࡐྉརஊɾཁ੥ʹରԠ͢Δͱͱ΋ʹɼ‫ݝ‬ઐ༻ϏʔϜϥΠϯͷ

༻ٕज़ͷߴ౓Խʹ൐ͬͯɼ৽͍͠‫ػ‬ೳΛ༗͢Δࡐྉͷར༻‫ۀا‬౳ʹର͠ɼ֤छਃ੥ɼ࣮‫ݧ‬४උɼ෼ੳΞυό։ൃ౳͕੝Μʹͳ͖ͬͯͨ͜ͱͳͲ͔ΒɼBL24XU ͕Πε౳Λߦ͍ͬͯΔɽ·ͨɼ์ࣹޫར༻͕ະ‫͋Ͱݧܦ‬༗͢Δख๏ʹՃ͑ɼখ̭֯ઢࢄཚʢSAXSʣɼ޿Ҭ̭Δ‫ʹۀا‬ରͯ͠΋ɼ‫ݚ‬मɾٕज़૬ஊɾτϥΠΞϧతͳઢ‫ٵ‬ऩඍࡉߏ଄ղੳʢXAFSʣɼߴਫ਼౓ค຤̭ઢճંɼ

ར༻‫ػ‬ձͷఏ‫ڙ‬Λ௨ٕͯ͡ज़తࢧԉΛߦ͍ͬͯΔɽ

୯৭̭ઢτϙάϥϑΟ౳ͷख๏ʹ͍ͭͯ΋ରԠ͢΂͘ɼެӹࡒஂ๏ਓͻΐ͏͝Պֶٕज़‫ڠ‬ձͰ͸ɼ̎ຊͷ‫ݝ‬̎ຊ໨ͷ‫ݝ‬ઐ༻ϏʔϜϥΠϯͰ͋Δ BL08B2 Λ‫ݐ‬ઃઐ༻ϏʔϜϥΠϯͱฌ‫ޫࣹ์ݝݿ‬φϊςΫ‫ॴڀݚ‬ΛҰ͠ɼ2005 ೥౓ΑΓ‫༻ڙ‬Λ։࢝ͨ͠ɽ

‫ݩ‬తʹ؅ཧ͠ɼ༗ޮ͔ͭޮ཰తʹӡӦ͢Δ͜ͱʹΑΓɼ͜ΕΒͷࢪઃ؅ཧɾӡӦʹ͍ͭͯ͸ɼ̍ຊ໨ͷ‫ݝ‬ઐར༻‫ۀا‬౳ʹͱͬͯ࢖͍উखͷྑ͍‫ڥ؀‬Λ੔͑ɼ࢈‫ۀ‬༻ϏʔϜϥΠϯͷ‫༻ڙ‬։࢝౰ॳ͔Βެӹࡒஂ๏ਓͻΐ෼໺ʹ͓͚Δ์ࣹޫͷར༻͕ԁ‫ʹ׈‬ਐΉΑ͏౒ΊΔͱ͏͝Պֶٕज़‫ڠ‬ձ͕ɼฌ‫͔ݝݿ‬ΒͷҕୗΛड͚࣮ͯࢪ

ͱ΋ʹɼ֤छ‫ݚ‬मձɾٕज़૬ஊɾडୗ‫౓੍ڀݚ‬౳ͷ࣮͍ͯ͠ΔɽࢪΛ௨ͯ͡ɼ‫ཱʹ಺ݝ‬஍͢Δಛ௕͋Δଟ਺ͷத‫ݎ‬ɾத

2008 ೥ 1 ݄ʹ͸ɼެӹࡒஂ๏ਓͻΐ͏͝Պֶٕज़

খ‫ۀا‬΍஍৔࢈‫΁ۀ‬ͷ์ࣹޫར༻Λଅਐ͠ɼ์ࣹޫར

‫ڠ‬ձ͕ฌ‫͔ݝݿ‬Βͷࢦఆ؅ཧऀͱͳΓɼSPring-8 ͷ༻ͷ੄໺ͷ֦େʹऔΓ૊ΜͰ͍Δɽಛʹɼ‫಺ݝ‬த‫ݎ‬ɾར༻‫ۀا‬౳Λࢧԉ͠ɼଟ༷ͳ‫ڞ‬ಉ‫ڀݚ‬ϓϩδΣΫτͷ

தখ‫͚͓ʹۀا‬Δ‫ݝ‬ઐ༻ϏʔϜϥΠϯΛར༻ͨ͠‫ڀݚ‬‫ͳͱ఺ڌ‬Δฌ‫ޫࣹ์ݝݿ‬φϊςΫ‫ॴڀݚ‬ͷ‫༻ڙ‬Λ։࢝։ൃͷ͏ͪɼ৽෺࣭ɾࡐྉɼઌਐόΠΦ౳ͷ෼໺Ͱ༏ਤ 1. ฌ‫ݝݿ‬ϏʔϜϥΠϯͷར༻ମ੍– 17 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)ਤ 2. ฌ‫ݝݿ‬ϏʔϜϥΠϯͷར༻ମ੍Εͨ੒Ռͷ૑ग़͕‫ظ‬଴͞ΕΔ‫ۀا‬ͷडୗ‫ܦڀݚ‬අʹର๬Λ౿·͑ɼ̭ઢΠϝʔδϯάɼτϞάϥϑΟͳͲɼͯ͠ɼฌ‫͢ࢪ࣮͕ݝݿ‬Δॿ੒੍౓Λ‫͠༻׆‬ɼ์ࣹޫརॱ࣍෼ੳαʔϏεͷଌఆ๏Λॆ࣮͍ͤͯ͞Δɽ

༻ͷΞυόΠε΍ٕज़ࢦಋͳͲɼ੡඼։ൃͷͨΊͷࢼ࡞඼։ൃ΍࣮ূࢼ‫ࢸʹݧ‬ΔҰ࿈ͷࢧԉΛߦ͍ɼ์ࣹޫ

ҡ࣋؅ཧɾ‫ܦ‬අෛ୲ར༻‫ۀا‬ͷൃ۷ΛਐΊ͍ͯΔɽฌ‫ݝݿ‬ઐ༻ϏʔϜϥΠϯ͓Αͼฌ‫ޫࣹ์ݝݿ‬φϊςࠓ‫ޙ‬΋ɼؔ੢஍Ҭɼ͞Βʹ͸શࠃͷઌ୺తٕज़։ൃ
ΛਐΊΔ‫ʹۀا‬΋‫ݝ‬ઐ༻ϏʔϜϥΠϯΛੵ‫ۃ‬తʹఏ‫ڙ‬͠ɼ৽ࡐྉͷධՁɾ։ൃ౳ʹଟ͘ͷ஌‫ݟ‬Λ஝ੵ͢Δ͜Ϋ‫ॴڀݚ‬ͷҡ࣋؅ཧɾ‫৽ߋثػ‬ɼϢʔβʔαϙʔτʹ͍ͭͯ͸ɼެӹࡒஂ๏ਓͻΐ͏͝Պֶٕज़‫ڠ‬ձ͕࣮‫ݧ‬ͱͰɼར༻‫ۀا‬౳ͷχʔζʹԠͨ͡ߴ౓ͳٕज़త՝୊

ϋον಺ͷ‫ͱثػ‬Ұ‫ݩ‬తͳ؅ཧΛߦ͍ͬͯΔɽͳ͓ɼʹରԠͰ͖ΔΑ͏౒Ί͍ͯ͘ɽBL24XU ͷٕज़తͳ؅ཧɾӡӦ෦෼ʹؔͯ͠͸ɼಉ‫ڠ‬ձΑΓ٬һ‫ڀݚ‬һʹҕ৤͍ͯ͠Δฌ‫ཱݝݿ‬େֶେֶӃར༻ମ੍෺࣭ཧֶ‫ڀݚ‬Պ̭ઢޫֶߨ࠲ͷ‫ڭ‬һ͕ɼฌ‫ޫࣹ์ݝݿ‬ฌ‫ݝݿ‬ϏʔϜϥΠϯͷར༻ʹࢸΔաఔΛਤ 1 ʹࣔ͢ɽφϊςΫ‫ͱͱॴڀݚ‬΋ʹ୲͍ͬͯΔɽ‫ݝ‬ઐ༻ϏʔϜϥΠϯͷҡ࣋؅ཧʹ͔͔Δඅ༻ʹ͍ͭͯ͸ɼઃஔऀͰ͋Δฌ‫͕ݝݿ‬ෛ୲͍ͯ͠Δ͕ɼฌ‫ݿ‬ӡӦମ੍‫ݝ‬ͷෛ୲Ͱ࿫͏ઃඋҎ֎ͷ͏ͪɼ࣮‫ʹݧ‬ඞཁͱͳΔओฌ‫ݝݿ‬ϏʔϜϥΠϯͷར༻ʹؔΘΔӡӦମ੍Λਤ 2ʹࣔ͢ɽཁ‫ثػ‬౳ͷ੔උඅɼਓ݅අɼ‫ڀݚ‬අʹ͍ͭͯ͸ར༻‫ا‬‫ۀ‬౳͔Βෛ୲͍͍͓ͨͩͯΓɼ͜ͷඅ༻ʹ͍ͭͯ͸ɼϢʔβʔλΠϜͷ഑෼ʹԠֹͨۚ͡ʢ50 ສԁ/೔ʣΛɼडୗ‫ڀݚ‬ʢ෼ੳαʔϏεʣ֤ར༻‫ۀا‬౳͕ެӹࡒஂ๏ਓͻΐ͏͝Պֶٕज़‫ڠ‬ձʹฌ‫ݝݿ‬ઐ༻ϏʔϜϥΠϯ͕උ͑Δ൚༻తͳ෼ੳπʔࢧ෷͍ͬͯΔɽϧΛ‫͠༻׆‬ɼ࢈‫ۀ‬ք͕์ࣹޫΛར༻͠΍͍͢γεςϜΛఏ‫͢ڙ‬Δͱͱ΋ʹɼ࢈‫ۀ‬քʹ͓͚Δજࡏతχʔζͷར༻ঢ়‫گ‬

։୓ΛਐΊΔͨΊɼ2009 ೥౓ΑΓɼ‫ۀا‬౳͔ΒͷҕୗΛड͚ͯฌ‫ޫࣹ์ݝݿ‬φϊςΫ‫ॴڀݚ‬ͷ‫ڀݚ‬һ͕ɼࢼྉͷଌఆɾղੳΛߦ͏डୗ‫ڀݚ‬Λ࣮ࢪ͍ͯ͠Δɽ෼ੳͷ಺༰ͱͯ͠͸ɼ౰ॳɼXAFS ͱখ̭֯ઢࢄཚ
ͷ྆ଌఆ๏Λର৅ͱͯ͠ελʔτ͕ͨ͠ɼ࢈‫ۀ‬քͷཁฌ‫ ݝݿ‬BL ͷར༻ʹ౰ͨͬͯɼར༻ਃ੥͸ਵ࣌ड෇͚͓ͯΓɼར༻࣌‫͍ͯͭʹظ‬΋ɼຖ݄࣮ࢪ͍ͯ͠Δεέδϡʔϧձٞʹ͓͍ͯɼ‫ݝ‬ઐ༻ϏʔϜϥΠϯͷޮ཰తͳӡ༻Λߟྀͭͭ͠ɼ‫ۀا‬ͷҙ޲ΛͳΔ΂͘ଚॏ͢– 18 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू
Δ‫Ͱܗ‬೔ఔௐ੔Λߦ͓ͬͯΓɼSPring-8 ͷશϏʔϜλΠϜʹର͢Δ‫ݝ‬ઐ༻ϏʔϜϥΠϯͷՔಇ཰͸ɼ΄΅100 ˋͱͳ͍ͬͯΔɽฌ‫ ݝݿ‬BL ʹ͓͚Δɼ࠷ۙ̏Χ೥ͷ૷ஔผར༻ׂ߹
Λਤ 3 ʹ͕ࣔ͢ɼϚΠΫϩϏʔϜΛ༻͍ͨ‫ॴہ‬෼ੳ΍খ̭֯ઢࢄཚʢSAXSʣͷར༻͕ߴׂ͍߹ͰਪҠͯ͠
͍Δɽར༻෼໺ʹ͍ͭͯ͸ਤ 4 ͷͱ͓ΓͰ͋Δ͕ɼฌ‫ݝݿ‬ͷओͨΔ࢈‫͋Ͱۀ‬Δమ߯΍ۚଐؔ܎ͷར༻ׂ߹͸೥ʑ‫ݮ‬গ͠ɼ࠷ۙ͸ಛʹ‫ؔͼٴ಺ݝ‬੢‫ۀا‬ͷχʔζ͕ߴ͍ి஑΍൒ಋମͱ͍ͬͨলΤωɼ࣍ੈ୅ΤωϧΪʔؔ࿈ࡐྉͷར༻͕૿Ճ͍ͯ͠Δɽ

ਤ 3. ฌ‫ݝݿ‬ϏʔϜϥΠϯͷ૷ஔผར༻ׂ߹
ฌ‫Ͱݝݿ‬͸ɼ2011 ೥ 12 ݄ʹؔ੢ͷ 6 ࣏ࣗମ͕‫ڞ‬ಉͰࣄ‫ۀ‬Λ։࢝͠ɺฌ‫ཱݝݿ‬େֶɺਆ‫ށ‬େֶɺཧԽֶ‫ݚ‬‫ॴڀ‬ɼJASRIɼؔ܎‫ۀا‬౳ʹࢀը͍͍͍ͨͩͯΔʮؔ੢Πϊϕʔγϣϯࠃࡍઓུ૯߹ಛ۠ʯʹ͓͍ͯɼ์ࣹ
ޫͱγϛϡϨʔγϣϯٕज़Λ૬ิతʹ૊Έ߹Θͤͨ࣍ੈ୅ΤωϧΪʔؔ࿈ࡐྉͷ։ൃΛ࠷ॏ఺՝୊ͱͯ͠औ
Γ૊ΜͰ͍Δ͜ͱ͔ΒɼҾ͖ଓ͖౰֘෼໺ͷར༻͸ߴׂ͍߹ͰਪҠ͢Δ΋ͷͱࢥΘΕΔɽ
ฌ‫ޫࣹ์ݝݿ‬φϊςΫ‫ॴڀݚ‬ਤ 4. ฌ‫ݝݿ‬ϏʔϜϥΠϯͷ෼໺ผར༻ׂ߹

ӬҪ݈Ұ

– 19 –

ɹ੒ɹՌɹू

– 21 –

ɹฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

BL08B2

2011A3302, 2011B3302

XAFS ࣮‫ݧ‬εςʔγϣϯͷ‫ݱ‬ঢ়
Current Status of XAFS Station at BL08B2
ཥɹཕLei Liʢެࡒʣͻΐ͏͝Պֶٕज़‫ڠ‬ձɹ์ࣹޫφϊςΫ‫ॴڀݚ‬

Synchrotron Radiation Nanotechnology Laboratory, Hyogo Science and Technology Association֓ཁɿɹ BL08B2 ͷ XAFS εςʔγϣϯ͸ɼಁա๏ɼ‫ޫܬ‬๏ɼస‫ࢠి׵‬ऩྔ๏ͱશ൓ࣹ XAFS Λඋ͍͑ͯΔɽ
ར༻ՄೳͳޫࢠΤωϧΪʔͷൣғ͸ 4.0–72 KeV Ͱ͋Δɽߴਫ਼౓ͳଌఆΛ࣮‫͖Ͱݱ‬ΔΑ͏ɼޫֶ‫ʹܥ‬͸ඪ४‫ܕ‬γϦίϯೋ݁থ෼ޫ‫ͱث‬લ‫ޙ‬ͷϛϥʔͱΛ૊Έ߹Θͤͨ΋ͷΛ࠾༻͍ͯ͠Δɽ‫ޫܬ‬๏Ͱ͸ɼLytle ‫ܕ‬ͷ‫ݕ‬ग़‫ث‬
ͱ 19 ૉࢠήϧϚχ΢Ϝ൒ಋମ‫ݕ‬ग़‫ث‬Λ੔උ͍ͯ͠Δɽ·ͨΫϥΠΦελοτʹΑΔࢼྉͷԹ౓ௐ੔΍ɼin-situ൓ԠੑΨε΍ɼࣗಈࢼྉަ‫ث׵‬Λར༻ͨ͠࿈ଓଌఆ΋ՄೳͰ͋ΔɽΩʔϫʔυɿɹ XAFSɼΫΠοΫ XAFSɼin-situ ‫࡯؍‬എ‫ڀݚͱܠ‬໨తޫֶ‫͓ܥ‬Αͼଌఆ༻ϏʔϜͷಛ࣭ࡐྉͷੑೳߴ౓Խʹͱ΋ͳͬͯɼ৽͍͠‫ػ‬ೳΛ༗͢

BL08B2 Ͱ͸ɼภ޲ి࣓ੴΛޫ‫ͯ͠ͱݯ‬ɼओʹલஔΔࡐྉͷ։ൃ౳͕੝Μʹͳ͖͍ͬͯͯΔɽ࢈‫ۀ‬քʹϛϥʔɼSPring-8 ඪ४‫ܕ‬γϦίϯೋ݁থ෼ޫ‫ث‬ɼ‫ޙ‬͓͍ͯ͸ɼΑΓ੡඼Խʹ௚݁͢Δٕज़։ൃஈ֊Ͱͷஔूޫϛϥʔ͔Β੒Δ༌ૹ෦Λ੔උͨ͠ɽBL08B2 ͷࡐྉ෼ੳχʔζ͕૿Ճ͓ͯ͠Γɼ͜ΕΒʹԠ͑ΔΑ͏ϨΠΞ΢τͰ͸ɼXAFS ϏʔϜϥΠϯͷ୅දͰ͋ΔʹɼϏʔϜϥΠϯ BL08B2 ʹ͓͍̭ͯઢ‫ٵ‬ऩඍࡉߏ

BL01B1 Λࢀߟͱͨ͠ [1, 2]ɽ
෼ޫ‫ث‬͸Մม܏ࣼ‫ػܕ‬ೳͷߏ଄Λ࠾༻͠ɼSi 111 ൓

଄ʢXAFSʣଌఆ૷ஔΛ੔උ͖ͯͨ͠ɽ

BL08B2 ͷ XAFS ଌఆ૷ஔͰ͸ɼSPring-8 ʹ͓͍ࣹͱ Si 311 ൓ࣹΛ੾Γସ͑ͯར༻Մೳͱ͢Δ͜ͱͰͯ BL01B1 ΍ BL14B2ɼ͋Δ͍͸αϯϏʔϜ BL16B2

ߴ͍ΤωϧΪʔબ୒ੑΛՄೳͱͨ͠ɽͦͷͨΊɼϏʔΛซ༻͢ΔϢʔβʔͷ࢖͍қ͞Λߟྀͯ͠ɼ͜ΕΒϜϥΠϯ BL08B2 ͷ XAFS ૷ஔ͸ɼ4.0∼72 keV ͷ޿ϏʔϜϥΠϯ‫ڞ‬௨ͷ‫ߏثػ‬੒Ͱ੔උΛߦͬͨɽXAFS

͍ΤωϧΪʔྖҬͰ൚༻తͳ XAFS Λߦ͏͜ͱ͕Մ

੔උͰ͸ JASRI ͔Βͷࢦಋ΍ଌఆ༻ιϑτ΢ΣΞͷ

ೳͰ͋Δɽ݁থ໘ Si(111) ͸ 4.0∼37 keV ΤωϧΪʔఏ‫ڙ‬౳ͷαϙʔτΛ௖͖ͳ͕Βӡసͷ҆ఆԽΛਤΔ͜ྖҬΛɼ݁থ໘ Si(311) ͸ 7.6∼72 keV ΤωϧΪʔྖͱ͕Ͱ͖ͨɽ

ҬΛΧόʔͰ͖ΔɽΤωϧΪʔ෼ղೳɼϏʔϜϑΥτ৮ഔ΍ి஑ࡐྉ౳ͷ൓Ԡաఔʹ͓͚Δߏ଄มԽΛ࣌ϯ਺͸݁থ໘ʹΑͬͯҟͳΔͷͰɺଌఆ໨తʹ߹Θͤ෼ׂଌఆͰ͖ΔΑ͏ɼΫΠοΫ XAFS(Quick XAFS)ͯબ୒͢Δ͜ͱʹͳΔɽલஔ͓Αͼ‫ޙ‬ஔϛϥʔ͸ϏʔͷͨΊͷ‫ثػ‬੔උΛߦ͍ɼଌఆ࣌ؒͷ୹ॖԽ͕ਤΒΕϜΛίϦϝʔτ͓Αͼूޫ͢Δͱಉ࣌ʹɼߴௐޫͷͨɽ·ͨɼి஑‫ͼٴ‬৮ഔ։ൃʹ͓͚Δར༻χʔζͷ૿আ‫͏͍ͱڈ‬ॏཁͳ໾ׂ͕͋Δɽϛϥʔͷ܏͖֯͸֤ΤେԽΛਪଌ͠ɼXAFS ʹΑΔ in situ ‫ʹ࡯؍‬ରԠ͢Δ

ωϧΪʔྖҬʹ͓͚Δɼ1 ࣍ޫ൓ࣹ཰ͱ 3 ࣍ޫͷࠞೖͨΊɼϏʔϜϥΠϯ‫ݐ‬ઃ౰ॳʹ͓͍ͯ൓ԠੑΨεͷઃൺΛߟྀͯ͠ɼ0∼8 mrad ͷؒͰઃఆ͞ΕΔɽϏʔϜඋΛ੔උͨ͠ɽҎ্ͷ੔උʹΑΓɼଌఆͷߴޮ཰ԽΛϑΥτϯ਺͸໿ 109 ∼1011 photons/sec ͕ಘΒΕ͍ͯਤͬͨɽΔɽΤωϧΪʔ෼ղೳ͸෼ޫ‫ث‬ͷ݁থ໘ʹґଘ͢Δɽ

Si 111 ൓ࣹΛ࢖༻ͨ͠ͱ͖ͷϏʔϜͷΤωϧΪʔ෼ղೳ͸࠷খ ∆E/E ͸ 10−4 ୆ͰɼSi 311 ൓ࣹͷ৔߹ͷ

– 23 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)∆E/E ͸ 10−5 ୆Ͱ͋ΔɽϏʔϜαΠζ͸ɼ্Լํ޲
Λूޫ৚͓݅ΑͼࢼྉલεϦοτͰɼ·ͨɼਫฏํ޲
ͷαΠζ͸ࢼྉલεϦοτͰܾఆ͞ΕɼΑ͘࢖ΘΕΔαΠζ͸ 2 mm ఔ౓Ͱ͋ΔɽଌఆϞʔυ͓Αͼ‫ݕ‬ग़‫Ͳͳܥ‬

Fig. 1 ʹࣔ͢Α͏ʹ࣮‫ݧ‬ϋον಺ 1 ʹ͸ɼঢ߱Ս୆
෇ఆ൫্ʹɼ‫ج‬ຊతͳ XAFS ‫ܭ‬ଌγεςϜͰ͋Δࢼྉपล‫͓ثػ‬Αͼ‫ݕ‬ग़‫͕ܥث‬ઃஔ͞Ε͍ͯΔɽ্ྲྀ͔Βೖࣹ̭ઢΛ੔‫͢ܗ‬ΔεϦοτɼI0 ଌఆ༻ͷΠΦϯνΣ
ϯόʔɼࢼྉ‫ݻ‬ఆ͓ΑͼҐஔௐ੔༻ XZ εςʔδͱɼશ൓ࣹ഑ஔ༻ଟ࣠ߏ੒Ͱ͋Δਫ਼ີΰχΦεςʔδɼI1
ଌఆ༻ͷΠΦϯνΣϯόʔͱϏʔϜҐஔ༻Ϩʔβʔ͕ॱ൪ʹઃஔ͞Ε͍ͯΔɽ·ͨࢼྉԹ౓ௐ੔༻ΫϥΠΦελοτͱ‫ر‬ബࢼྉΛଌఆ͢Δ 19 ૉࢠ SSD ΋ಉఆ൫্ʹઃஔ͞Ε͍ͯΔɽ

Fig. 2. (a) Experimental K-edge XAFS spectrumand (b) k 3 χ(k) EXAFS spectra of CeO2 .
Ͱ͖ΔγεςϜͱͯ͠ XIA ࣾ੡ XMAP Λಋೖͨ͠ɽ
Ξφϩά‫ܭ‬ଌγεςϜʹ͓͚ΔΞϯϓௐ੔΍ɼSCA
ͷબ୒ɼΧ΢ϯλͷ‫ܭ‬ଌΛ XMAP ͷଌఆ୆্ʹඋ͑
͍ͯΔɽXMAP γεςϜΛ༻͍Δ͜ͱʹΑΓɼ͜Ε

Fig. 1. XAFS experimental set-up.

·Ͱ࣌ؒΛཁ͍ͯͨ͠ 19 ૉࢠ SSD ͷௐ੔͕ɼશͯύಁա๏͸̭ઢ‫ٵ‬ऩ෼ޫʹ͓͚Δ௚઀๏Ͱ͋Δɽ‫ݕ‬ग़‫ͯ͠ͱث‬͸μΠφϛοΫϨϯδ͕େ͖͘ɼి‫ۃ‬௕͞ 14

cmɼ28 cm ͷΠΦϯνΣϯόʔ͕༻ҙ͞Ε͓ͯΓɼΠΦϯνΣϯόʔ༻ͷΨε͸ɼHe, N2 , Ar, Kr Ψε͓Αͼࠞ߹Ψε͕༻ҙ͞Ε͍ͯΔɽଌఆྫͱͯ͠ CeO2
ͷ XAFS ‫ٵ‬ऩεϖΫτϧΛ Fig. 2 ʹࣔ͢ɽXAFS ৼಈ͕໌ྎʹ‫ݕ‬ग़Ͱ͖Δ͜ͱ͕֬ೝ͞Εͨɽ‫ ޫܬ‬XAFS ଌఆ༻ʹ͸ Lytle ‫ݕ‬ग़‫ ͱث‬19 ૉࢠ SSD‫ݕ‬ग़‫༻͕ث‬ҙ͞Ε͍ͯΔɽ·֤ͨछͷࢄཚޫ‫ٵ‬ऩ༻ιίϯ͔Βߦ͏͜ͱ͕Ͱ͖ΔΑ͏ʹͳΓɼͦͷͨΊௐ੔͕‫ۃ‬Ίͯ༰қʹߦ͑ΔΑ͏ʹͳͬͨɽ

Quick XAFS ๏͸ɼ෼ޫ‫ث‬Λ࿈ଓతʹ૸Ҿ͠ͳ͕Βɼ̭ઢ‫౓ڧ‬σʔλʢI0 , I1 ͱ I2 ʣͱ෼ޫ‫౓֯ث‬σʔλʢΤωϧΪʔʣΛಉ࣌ʹଌఆ͢Δ XAFS ଌఆํࣜͰ͋ΔɽQuick XAFS ๏Λ༻͍Δ͜ͱʹΑΓɼ௨ৗʹൺ΂୹࣌ؒͰ XAFS ଌఆ͕࣮‫͞ݱ‬Ε in situ ‫͕࡯؍‬Մೳʹͳͬͨɽͭ·Γɼे਺ඵ͔Β਺෼ͷ࣌ؒʹ͓͍ͯे෼ʹղੳʹͰ͖Δ XAFS εϖΫτϧ͕औಘͰ͖Δɽ
ଌఆ໨తͰ͋Δ‫ݩ‬ૉͷೱ౓͕ߴ͍ബບࢼྉ΍մঢ়ۚϑΟϧλʔ͕༻ҙ͞Ε͍ͯΔɽബບࢼྉ΍‫ر‬ബࢼྉͷ‫ ޫܬ‬XAFS ଌఆʹ͸ 19 ૉࢠ SSD Λ༻͍Δ͜ͱ͕ෆՄܽͱͳͬͯ͘Δɽ·ͨ୹࣌ؒͰ؆୯ͳσʔλॲཧ͕ଐࢼྉ͸ɼ൚༻తʹ࢖༻͞Ε͍ͯΔಁա๏ XAFS Ͱ͸ѻ͍೉͍ࢼྉͰ͋Δɽ͜ΕΒͷࢼྉʹରͯ͠ɼ༰қʹ

XAFS ଌఆΛՄೳʹ͢Δͷ͕స‫ࢠి׵‬ऩྔ‫ݕ‬ग़‫Ͱث‬– 24 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू
͋Δɽ̭ઢΛ‫ٵ‬ऩͨ͠ࢼྉද໘͔ΒΦʵδΣిࢠ͕์

BL08B2 Ͱ੔උͨ͠൓ԠੑΨεγεςϜͱ૊Έ߹Θग़͞ΕΔ͕ɼͦͷΦʵδΣిࢠ‫౓ڧ‬͸̭ઢ‫ٵ‬ऩྔʹൺͤͨར༻‫ػ‬ձͷ૿Ճ͕‫ظ‬଴͞ΕΔɽి஑ͳͲͷ։ൃʹྫ͢ΔͷͰɼΦʵδΣిࢠΛ‫ݕ‬ग़͢Δ͜ͱΑΓ XAFS͓͍ͯ͸ɺߴҐஔ෼ղೳ XAFS ͷඞཁੑ͕ߴ͘ɼ‫ॴہ‬εϖΫτϧΛଌఆ͢Δ͢Δ͜ͱΛՄೳʹ͢Δͷ͕స‫׵‬తͳ৘ใΛಘΔ͜ͱΛ໨తʹɼBL08B2 Ͱ͸ EXAFS

ిࢠऩྔʢCEYʣ๏Ͱ͋ΔɽCEY ๏͸‫ޫܬ‬๏ʹൺ΂ɼྖҬ·Ͱͷߴ࣭ͳσʔλ‫ܭ‬ଌ͕Ͱ͖ΔϚΠΫϩϏʔද໘හ‫Ͱײ‬ɼ͔ͭ‫ݕ‬ग़ޮ཰͕ߴ͍ͱ͍͏ར఺͕͋ΔɽϜ XAFS ๏Λ‫ݕ‬౼͍ͯ͠Δɽ·ͨଞͷख๏ʢSAXS,CTɼXRDʣΛ૊Έ߹ΘͤΔ͜ͱͰɼΑΓߴਫ਼౓ʹ͠ࠓ‫ޙ‬ͷ՝୊

ͯɼΑΓଟ͘ͷ৘ใऔಘɺΑΓศརͳଌఆख๏ͷཱ֬

XAFS ๏Ͱ͸ɼin situ ‫࡯؍‬ͷଌఆ๏͕ओཁͳར༻
ํ๏ͷͻͱͭͰ͋Δɽ͜ͷͨΊɼ৮ഔ΍ࡐྉ։ൃ΁ͷXAFS Ԡ༻ͷ‫͔ظૣ͕ڀݚ‬ΒऔΓ্͛ΒΕ͖ͯͨɽͦ
ͷཧ༝͸‫ڥ؀‬໰୊΍ΤωϧΪʔ໰୊͕ਂࠁԽ͢ΔதͰߴ‫ػ‬ೳࡐྉ͕‫ٻ‬ΊΒΕ͍ͯΔ͔ΒͰ͋Δɽ
͜ͷΑ͏ͳ৮ഔ΍ࡐྉΛ։ൃ͢Δ্Ͱɼͦͷ৔‫࡯؍‬ʹΑΔߏ଄‫࡯؍‬Λߦ͏͜ͱ͸ɼ൓Ԡ࣌ͷߏ଄มԽΛղ
໌͢Δ༗༻ͳखஈͱͳ͍ͬͯΔɽ൚༻λΠϓߴԹ൓Ԡ༻ XAFS ࣮‫ݧ‬ηϧͳͲͷࢼྉपล‫ثػ‬ઃඋΛ੔උ͢ͱ੔උΛߦ͍ͬͯΔɽࢀߟจ‫ݙ‬[1] ߐଜमҰɼӉཹլ๎࠸ɼ୩ా ഹ: ೔ຊ݁থֶձࢽ
42, 5-11 (2000).
[2] T. Uruga, H. Tanida, Y. Yoneda, K. Takeshita, S.
Emura, M. Takahashi, M. Harada, Y.Nishihata,
Y. Kubozono, T. Tanaka, T.Yamamoto, H.
Maeda, O. Kamishima, Y.Takabayashi, Y.
Nakata, H. Kimura, S. Goto, and T. Ishikawa:
J. Synchrotron Rad. 6, 143-145 (1999).

Δ͜ͱͰɼ࢈‫ۀ‬ར༻Λ͞Βʹ֦େͰ͖Δ΋ͷͱߟ͑Δɽ

– 25 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

BL08B2

2009B3300, 2010A3300

BL08B2 খ̭֯ઢࢄཚଌఆͷ‫ݱ‬ঢ়ͱ
XAFS/SAXS ಉ࣌ଌఆͷ੔උʹ͍ͭͯ
Combined XAFS/SAXS measurement at BL08B2‫܂‬ຊ ࣎ੜ
Shigeo Kuwamotoʢެࡒʣͻΐ͏͝Պֶٕज़‫ڠ‬ձɹ์ࣹޫφϊςΫ‫ॴڀݚ‬

Synchrotron Radiation Nanotechnology Laboratory, Hyogo Science and Technology Association֓ཁɿɹฌ‫ݝݿ‬ϏʔϜϥΠϯ BL08B2 Ͱ͸ɼ‫ۀ࢈ࡏݱ‬քʹͯ੝Μʹ‫ڀݚ‬։ൃ͕ߦΘΕ͍ͯΔۚଐ৮ഔɾి஑
ࡐྉɾۚଐφϊཻࢠίϯϙδοτࡐྉΛର৅ʹɼిࢠɾԽֶঢ়ଶͱߏ଄ͱͷ૬ؔੑධՁΛ໨తͱ̭ͨ͠ઢ‫ٵ‬ऩඍࡉߏ଄ (XAFS) ଌఆͱখ̭֯ઢࢄཚ (SAXS) ଌఆͷಉ࣌ଌఆγεςϜͷ੔උΛਐΊ͍ͯΔɽຊใࠂͰ͸ɼ

BL08B2 ͷ SAXS ଌఆͷ‫ݱ‬ঢ়ͱ XAFS/SAXS ಉ࣌ଌఆͷ੔උঢ়‫͍ͯͭʹگ‬ใࠂ͢ΔɽΩʔϫʔυɿɹ SAXSɼXAFSɼQuick-XANES͕ࣼੜ͡ͳ͍͜ͱ͔Β SAXS ෼ղೳΛࠨӈ͢ΔΧϝഎ‫ܠ‬‫ػ‬ೳੑࡐྉ͕༗͢Δ௕प‫ߏظ‬଄΍‫ूڽ‬ମߏ଄ͷφϊϝʔτϧΦʔμʔͷߏ଄৘ใΛߴਫ਼౓ʹऔಘɾධՁ
͢Δ͜ͱΛ໨తͱͯ͠ɼฌ‫ݝݿ‬ϏʔϜϥΠϯ BL08B2
Ͱ͸ SAXS ଌఆ૷ஔΛઃஔ͍ͯ͠ΔɽSAXS ࣮‫࣌ݧ‬ͷޫֶ‫ܥ‬͸ɼ෼ޫ‫ث‬લ‫ʹޙ‬ίϦϝʔγϣϯ༻ϑϥοτϛϥʔͱूޫ༻ϕϯτγϦϯυϦΧϧϛϥʔΛ഑ஔͨ͠ूޫޫֶ‫ܥ‬Λ࠾༻͍ͯ͠ΔʢFig. 1ʣɽ͜ͷޫֶ‫ܥ‬͸ɼSPring-8 ಺ͷ XAFS ϏʔϜϥΠϯʢBL01B1ʣ[1]΍ւ֎ͷҟৗ෼ࢄଌఆΛ໨తͱͨ͠ϏʔϜϥΠϯ [2]Ͱ࠾༻͞Ε͓ͯΓɼߴ͍ΤωϧΪʔ෼ղೳͱ෯޿͍ΤωϧΪʔબ୒ੑ͕ಘΒΕΔɽ·ͨɼ̭ઢϏʔϜͷ܏ϥ௕ʢଌఆࢼྉ͔Β‫ݕ‬ग़‫Ͱ·ث‬ͷ‫཭ڑ‬ʣͷมߋ͕༰қʹͳΔͱͱ΋ʹɼ௕͍ਅۭύΠϓΛཁ͢ΔΧϝϥ௕ͷηοςΟϯά͕ՄೳͱͳΔɽ͜ΕʹΑΓ BL08B2 Ͱ͸ɼ਺ඦφϊϝʔτϧΦʔμʔͷߏ଄ධՁ͕Մೳͳ 6,000mm ͷΧϝϥ௕΍ɼೋͭͷ࣮‫ݧ‬ϋονΛ࿈݁ͯ͠ߏங
͢Δ 15,600 mm ͷΧϝϥ௕Λ༻͍ͨ‫ۃ‬খ̭֯ઢࢄཚ

(Ultra-SAXS) ଌఆ͕ՄೳͰ͋Δɽ‫ࡏݱ‬ͷ SAXS ଌఆͷಛੑΛ Table 1 ʹࣔ͢ɽ্‫ه‬ͷΑ͏ͳΧϝϥ௕ͱΤωϧΪʔͷ޿͍બ୒ੑΛ
༗͢Δ SAXS ޫֶ‫ ͱܥ‬BL08B2 ‫ط‬ଘͷ XAFS ଌఆ‫ܥ‬Λ૊Έ߹ΘͤΔ͜ͱͰɼBL08B2 Ͱ͸ XAFS/SAXS ಉ࣌ଌఆ͕ՄೳͱͳΔɽ͜ͷ XAFS/SAXS ಉ࣌ଌఆ͸ɼ

Fig. 1. Beamline layout and SAXS optics.

– 26 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

Table 1. Characteristics of SAXS optics and apparatus.
Energy range
Mirror angle
Photon flux
Beam size
SAXS camera length
SAXS detectors
Measurement methods

8 ∼ 15 keV (5.3 ∼ 25 keV)∗
4 mrad ∼ 7 mrad
1.0 × 1010 photons/sec (12.4 keV)

0.15(H) × 0.25(W) mm at detector position
500 ∼ 6,200 mm, 15,600 mm

Imaging plate (R-AXIS4++), PILATUS, XRII-CCD, Flat panel sensor
SAXS/WAXS, GI-SAXS, A-SAXS, Rheo-SAXS, XAFS/SAXS∗

Preparation of mirror angle is required.

‫ۀ࢈ࡏݱ‬քͰ੝Μʹ‫ڀݚ‬ɾ։ൃ͕ߦΘΕ͍ͯΔۚଐ৮
ഔɾి஑ࡐྉ෼໺ʹ͓͍ͯɼిࢠɾԽֶঢ়ଶͱߏ଄ͱͷ૬ؔੑΛධՁ͢Δ৽ͨͳ෼ੳπʔϧͱͳΔͱߟ͑Δɽຊ՝୊Ͱ͸ɼඪ४ࢼྉΛ༻͍ͨ XAFS/SAXS ಉ࣌ଌఆͳ
Βͼʹ in-situ ࣮‫ݧ‬Λ૝ఆͨ͠ Quick-XANES/SAXSಉ࣌ଌఆͷ༧උ࣮‫ݧ‬ΛߦͬͨͷͰɼͦͷ݁Ռʹ͍ͭͯ
ใࠂ͢Δɽ
࣮‫ݧ‬

SAXS ଌఆ͸ɼΧϝϥ௕ 1,800 mmɼ೾௕ 0.139 nm(8.94 keV)ɼ‫ݕ‬ग़‫ʹث‬ೋ࣍‫ݩ‬൒ಋମ‫ݕ‬ग़‫ ث‬PILATUS
Λ࢖༻ͨ͠ɽXAFS ଌఆ͸ɼಁաଌఆ༻ʹ I0 ɼI1 ‫ܭ‬ଌ༻ΠΦϯνϟϯόʔΛ SAXS ࢼྉ୆લ‫ʹޙ‬഑ஔͯ͠ߦͬͨɽଌఆࢼྉ͸ EXAFS ଌఆ༻ʹඪ४ࢼྉͱ͠

Fig. 2. Time frame diagram for combined quickXANES/SAXS measurements.

ͯനۚബບΛɼQuick-XANES/SAXS ಉ࣌ଌఆʹ͸ిࢠ഑ઢ౳Ͱ࢖༻͞ΕΔಔφϊཻࢠϖʔετʢʢ‫ג‬ʣφϊɾΩϡʔϒɾδϟύϯ੡ʣΛ༻͍ɼՃ೤࿍Λར༻͠40 ◦ C∼200 ◦ C ͷՃ೤ʹΑΔมԽΛ‫ͨ͠࡯؍‬ɽQuickXANES/SAXS ಉ࣌ଌఆ͸ɼSAXS ଌఆ࣌ؒΛ 5 ඵɼ
Cu-K ‫ٵ‬ऩ୺෇ۙͷΤωϧΪʔൣғ 8.94∼9.06 keV ͷ
Quick-XANES ଌఆΛ 10 ඵɼΤωϧΪʔ͕ 8.94 keVʹ໭Δ࣌ؒʢ෼ޫ‫ ث‬θ ࣠ͷҠಈ࣌ؒʣͱଌఆ଴‫࣌ػ‬ؒΛ߹ΘͤͨσουλΠϜΛ 5 ඵͱͨ͠ 20 ඵ࣌෼ׂଌఆͱͳΔΑ͏ʹௐ੔ͨ͠ [3]ɽ͜ͷ in-situ ଌఆͷϑϨʔϜμΠΞάϥϜΛ Fig. 2 ʹࣔͨ͠ɽଌఆִؒ͸ɼΒʹ୹࣌ؒԽ͢Δ͜ͱ΋ՄೳͰ͋Δɽ

Fig. 3. XAFS spectrum of standard sample obtained
by XAFS/SAXS measurement.

݁ՌmmʀࢼྉҐஔʣͰ΋ EXAFS ྖҬ·Ͱղੳʹे෼ͳ

Quick-XANES ଌఆͷΤωϧΪʔൣғͷௐઅʹΑΓ͞εϖΫτϧΛಘΔ͜ͱ͕Ͱ͖ͨɽ

Fig. 3 ͸ɼSAXS ࢼྉ୆Ґஔʹͯଌఆͨ͠നۚബ
ບͷ XAFS εϖΫτϧͰ͋ΔɽSAXS ଌఆ༻ʹ‫د‬ੜࢄཚআ‫ڈ‬Λे෼ʹߦͬͨࡉ͍̭ઢϏʔϜʢ0.3 × 0.4

Fig. 4, 5 ͸ɼಔφϊཻࢠϖʔετΛ 40 ◦ C ͔Β200 ◦ C ʹՃ೤ͨ͠ࡍͷ 20 ඵ࣌෼ׂ Quick-XANES/– 27 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)
SAXS ಉ࣌ଌఆͷ݁ՌͰ͋ΔɽՃ೤ɾ࣌ؒ‫ܦ‬աʹΑΓ
SAXS ϓϩϑΝΠϧʹେ͖ͳมԽ͕‫͞࡯؍‬ΕͨɽՃ೤ॳ‫ࢼʹظ‬ྉதʹ‫·ؚ‬ΕΔߴ෼ࢠ෼ࢄࡎ༝དྷͷϐʔΫ͕খ͘͞ͳΓɼͦͷ‫ޙ‬ɼখ֯ྖҬͷࢄཚ‫౓ڧ‬ͷ্ঢ͕‫؍‬࡯͞Εͨɽ͜ͷ͜ͱ͔Βɼߴ෼ࢠ෼ࢄࡎ͕Ճ೤ʹΑΓম٫͞Εͨ‫ʹޙ‬φϊཻࢠͷձ߹ɾ༥ண͕ੜ͍ͯ͡Δͱ
ߟ͑ΒΕΔɽ·ͨɼಉ࣌ʹଌఆͨ͠ Quick-XANES Ͱ΋Ճ೤ɾ࣌ؒ‫ܦ‬աʹ൐͏ XANES εϖΫτϧͷΤωϧ
Ϊʔγϑτ͕‫͞࡯؍‬Εͨɽ

Fig. 5. Time-resolved SAXS profiles collected during
the heating of copper nanoparticles.
ಉ࣌ଌఆ΋ՄೳͰ͋Δɽ‫ ޫܬ‬XAFS ଌఆͱͷ૊Έ߹ΘͤʹΑΓɼର৅‫ݩ‬ૉͷೱ౓͕௿͍ࢼྉʹରͯ͠΋

XAFS/SAXS ಉ࣌ଌఆ͕ՄೳͰ͋Δɽࠓ‫ޙ‬ͷ՝୊
ࠓճͷ࣮‫ʹݧ‬ΑΓɼBL08B2 ‫ط‬ଘͷ XAFS ଌఆ‫ܥ‬ͱ SAXS ଌఆΛ૊Έ߹Θͤͨ XAFS/SAXS ಉ࣌ଌఆɼͳΒͼʹɼin-situ ଌఆΛ໨తͱͨ͠ 20 ඵ࣌෼

Fig. 4. Quick-XANES spectra collected during theheating of copper nanoparticles.
ඪ४ࢼྉʢCu, CuO, Cu2 OʣͷεϖΫτϧͱൺֱ
͢Δͱɼಔφϊཻࢠϖʔετ͸Ճ೤ॳ‫ࢎʹطͰظ‬Խ͕ਐΜͩ Cu2 O ঢ়ଶͰ͋ΓɼՃ೤ɾ࣌ؒ‫ܦ‬աʹΑΓࢼྉͷిࢠঢ়ଶ͕ Cu2 O ͔Β CuO ΁γϑτ͍ͯ͠Δ͜ͱ
͕෼͔ͬͨʢFig. 4 தͷ໼ҹ෦ͷΤωϧΪʔγϑτʣɽ͜ΕΒͷ͜ͱ͔ΒɼՃ೤ʹΑΓಔφϊཻࢠͷ༥ணͱಉ࣌ʹࢎԽ൓Ԡ΋ਐߦ͍ͯ͠Δ͜ͱ͕෼͔ͬͨɽࠓ‫ޙ‬͸ɼ

XANES εϖΫτϧͷมԽͱ SAXS ϓϩϑΝΠϧͷมԽͷৄࡉͳؔ࿈෇͚Λߦ͍૬ؔతͳධՁΛߦ͏༧ఆͰ
͋Δɽ
ຊใࠂͰ͸ಁա XAFS ଌఆͷ݁Ռʹ͍ͭͯใࠂ͠
͕ͨɼLytle ‫ݕ‬ग़‫ث‬Λ༻͍ͨ‫ ޫܬ‬XAFS ଌఆͰͷଌఆ‫ܥ‬ͷ੔උ΋‫͍ͯྃ͠׬‬ΔɽSAXS ଌఆͰ͸ɼଌఆࢼྉ
Լྲྀଆͷ I1 ‫ܭ‬ଌ༻ΠΦϯνϟϯόʔ΍Ψε૚͕ࢄཚσʔλʹେ͖͘Ө‫͢ڹ‬ΔͨΊɼI1 ‫ݕ‬ग़‫ͯ͠ͱث‬ΠΦϯνϟϯόʔΛ࢖༻͢Δ͜ͱ͕Ͱ͖ͳ͍৔߹͸ɼLytle‫ݕ‬ग़‫ث‬Λར༻ͨ͠‫ ޫܬ‬XAFS ଌఆͱ SAXS ଌఆͱͷׂͷ Quick-XANES/SAXS ಉ࣌ଌఆΛ࣮‫͖ͨͰݱ‬ɽ

BL08B2 ͷޫֶ‫ܥ‬ͷಛ௃Λ‫͔ͨ͠׆‬෯޿͍ΤωϧΪʔൣғʹΑΔଟछ‫ݩ‬ૉ΁ͷରԠͱ SAXS ෼ղೳͷ޿͍બ୒ੑ͔Βɼ͞·͟·ͳ‫ػ‬ೳੑࡐྉʹରԠՄೳͳ XAFS/SAXS ಉ࣌ଌఆ‫ܥ‬Λ੔උ͢Δ͜ͱ͕Ͱ͖ͨɽۚଐ৮ഔ
ࡐྉ΍ి஑ࡐྉɼφϊཻࢠίϯϙδοτࡐྉ։ൃ෼໺
ʹ͓͍ͯɼର৅‫ݩ‬ૉͷిࢠɾԽֶঢ়ଶͱߏ଄ͱͷ૬ؔੑΛධՁ͢ΔޮՌతͳπʔϧʹͳΔͱߟ͑Δɽࠓ‫ޙ‬͸ɼ޿֯ࢄཚΛ૊Έ߹Θͤͨ XAFS/WAXS/SAXS ಉ࣌ଌఆ‫ܥ‬ͷ੔උΛਐΊΔͱͱ΋ʹɼ͞·͟·ͳΤωϧΪʔʢಛʹ 5∼6 keV ͷ௿ΤωϧΪʔྖҬͱ

20∼25 keV ͷߴΤωϧΪʔྖҬʣͰͷ‫ૅج‬σʔλͷऔಘɼQuick ଌఆͷߴ଎ԽΛਐΊΔɽ·ͨɼෳࡶͳଌ
ఆγεςϜͷιϑτ΢ΣΞʹΑΔ؆қԽɾϢʔβʔϑϨϯυϦΟԽΛߦ͍ɼϢʔβʔར༻Λల։͍ͯ͘͠༧
ఆͰ͋Δɽ
ࢀߟจ‫ݙ‬[1] T. Uruga et al.: J. Synchrotron Rad. 6, 143-145(1999).

– 28 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

[2] J. Ferrer et al.: J. Synchrotron Rad. 5, 1346-1356(1998).

[3] S. Nikitenko et al.: J. Synchrotron Rad. 15, 632640 (2008).

– 29 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

BL08B2

2010A3344, 2010B3344, 2011A3344

BL08B2 ̭ઢΠϝʔδϯάεςʔγϣϯͷ੔උ
Tuning of BL08B2 X-ray Imaging Station࣫‫ྑ ݪ‬ণ
Yoshimasa Urushiharaʢެࡒʣͻΐ͏͝Պֶٕज़‫ڠ‬ձɹ์ࣹޫφϊςΫ‫ॴڀݚ‬

Synchrotron Radiation Nanotechnology Laboratory, Hyogo Science and Technology Association֓ཁɿɹ BL08B2 ͷ̭ઢΠϝʔδϯάεςʔγϣϯͰ͸ɼภ޲ి࣓ੴޫ‫͔ݯ‬ΒͷϫΠυϏʔϜͷಛ௃Λੜ͔ͨ͠޿ࢹ໺ɾߴ෼ղೳΠϝʔδϯάɾCT ࣮‫ݧ‬Λߦ͍ͬͯΔɽ̭ઢΠϝʔδϯάɾCT ૷ஔ͸େ‫ܕ‬ఆ൫্ʹߏங͞Ε͍ͯΔͨΊɼࢼྉεςʔδ༻ͷ޿͍εϖʔε͕֬อ͞Ε͓ͯΓɼϢʔβʔ࣋ࠐͷ૷ஔΛ༻͍ͨ in situ ‫࡯؍‬͕ՄೳͰ͋ΔɽຊεςʔγϣϯͰ͸ɼࢼྉʵը૾‫ݕ‬ग़‫཭ڑؒث‬Λ 30–1000 mm ·Ͱมߋ͢Δ͜ͱ͕Ͱ͖ɼ߹
ۚ಺ཻք, ϙϦϚʔ಺ཻࢠք໘౳ͷ൓Ԡ΍ۭಎͳͲͷ಺෦‫ʹ࡯؍‬దͨ͠۶ંίϯτϥετΠϝʔδϯάΛߦ͏͜ͱ͕Ͱ͖ΔɽΩʔϫʔυɿɹ޿ࢹ໺ X ઢΠϝʔδϯάɼ̭ઢϚΠΫϩ CTɼ۶ંίϯτϥετΠϝʔδϯάഎ‫ܠ‬̭ઢΠϝʔδϯά͸, ෺࣭಺෦ͷঢ়ଶΛը૾Խ͢Δ‫ܭ‬ଌखஈͱͯ͠஌ΒΕ͍ͯΔɽ̭ઢը૾‫ݕ‬ग़‫͓ث‬Αͼ‫ثػࢉܭ‬ͷൃୡʹ൐͍ɼ̭ઢίϯϐϡʔςουτϞ
άϥϑΟʢCTʣʹΑΔ 3 ࣍‫ݩ‬ՄࢹԽٕज़ͷར༻͕ਐΈɼҩྍ෼໺͚ͩͰͳ͘࢈‫ۀ‬෼໺ͷ޻‫ࡐۀ‬ྉͳͲʹରͯ͠΋޿͘༻͍ΒΕΔΑ͏ʹͳͬͨɽBL08B2 Ͱ͸ɼ

2010A ‫ݧ࣮ʹظ‬ϋον̍Լྲྀଆʹ X ઢΠϝʔδϯάɾCT εςʔγϣϯ (Fig. 1) Λ੔උ͠ɼภ޲ి࣓ੴޫ
‫͔ݯ‬ΒͷϫΠυϏʔϜͷಛ௃Λੜ͔ͨ͠޿ࢹ໺ΠϝʔδϯάɾCT ࣮‫ݧ‬Λ։࢝ͨ͠ [1]ɽ͜ΕʹΑΓɼฌ‫ݝݿ‬ϏʔϜϥΠϯͱͯ͠ɼBL24XU ͰͷφϊΠϝʔδϯ
άɾCT ͱซͤͯɼ෯޿͍εέʔϧͰͷࡐྉ‫࡯؍‬ख๏Λఏ‫͖Ͱڙ‬ΔΑ͏ʹͳͬͨɽຊख๏ͷΑ͏ͳ࣮ۭؒΠϝʔδϯά͸ɼϑʔϦΤม‫׵‬Λඞཁͱ͠ͳ͍ࡐྉ಺෦

Fig. 1. Overview of X-ray imaging and CT station.
ଌఆ‫͓ܥ‬Αͼ‫ྫ࡯؍‬ߏ଄ධՁ͕ՄೳͰ͋ΔͨΊɼඞͣ͠΋์ࣹޫʹೃછΈ࣮‫ʹݧ‬͸, γϦίϯೋ݁থ෼ޫ‫ʹث‬ΑΓ୯৭Խ͞Εͷͳ͍࢈‫ۀ‬քٕज़ऀʹ΋์ࣹޫͷ༗༻ੑΛΞϐʔϧͰͨ 5–30 keV ͷ̭ઢ͕ར༻Ͱ͖Δɽߴ࣍ޫ͸ɼ෼ޫ‫ث‬

͖Δɽͦ͜Ͱར༻։࢝ʹ౰ͨΓɼ࢈‫ۀ‬քٕज़ऀʹର͠ͷೋͭͷ݁থͷฏߦੑΛΘ͔ͣʹͣΒ͢σνϡʔϯʹͯ CT ར༻ͷ࣮༻ੑͷ‫ۃݟ‬ΊΛ໨తͱͨ͠ CT ‫ݚ‬मձΑΓআ‫͍ͯ͠ڈ‬Δ͕ɼΑΓޮՌతʹআ‫͢ڈ‬ΔͨΊʹɼ

(2010 ೥ 4 ݄ 20 ೔) Λઃ͚ͨɽ‫ݚ‬मձʹ͸ 11 ࣾʹਆޫֶϋον಺ʹઃஔ͞Εͨೋͭͷશ൓ࣹϛϥʔΛར༻‫ށ‬େֶΛՃ͑ͨ‫ ܭ‬15 ໊͕ࢀՃ͠ɼ֤͕ࣾ࣋ࢀͨ͠ࢼ

͢Δ͜ͱ΋Ͱ͖Δɽ͜ͷΑ͏ʹ୯৭ੑͷߴ͍̭ઢϏʔྉΛଌఆ͢Δ͜ͱͰɼCT ར༻ͷՄೳੑΛ֬ೝ͢Δ͜

ϜΛ༻͍Δ͜ͱͰɼఆྔੑʹ༏Ε̭ͨઢ‫ٵ‬ऩ܎਺෼෍

ͱ͕Ͱ͖ͨɽ

ͷՄࢹԽΛߦ͏͜ͱ͕Ͱ͖Δɽ

– 30 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

Table 1. Properties of X-ray imaging detector at BL08B2.
Scintillator

P43 fine powder :YAG;Ce single crystal :diameter = 25 mm, thickness = 10 µm
diameter = 10 mm, thickness = 15 µm

Relay lens

Nikon F mount lens :f = 35 mm (F1.4), f = 50 mm (F1.2),

Kenko teleconverter :f = 105 mm (F2), f = 180 mm (F2.8)
×1.4, ×2

Digital Camera

BU-53LN (Bitran Co.) :CCD image sensor

4008×2672 pixel, 9 µm/pixel
16 bit A/D, 1.0 frame/sec
Orca-Flash2.8 (Hamamatsu photonics) :CMOS image sensor
1920×1440 pixel, 3.63 µm/pixel
12 bit A/D, 45 frame/secඪ४ͷࢼྉεςʔδ͸ɼਫ਼ີʹҐஔௐ੔Մೳͳࣗಈ

‫ͯ͠ͱྫ࡯؍‬ɼ෯ 6 mm ͓Αͼ 10 mm ͷ 2 छྨͷεςʔδͰߏ੒͞Ε͍ͯΔɽಛʹࢼྉճసεςʔδࢢൢҩༀ඼ৣࡎͷ CT ૾Λ Fig. 2 ʹࣔͨ͠ɽCT ࡱӨ͸ɼ180 ౓૸ࠪʹ͓͚Δճస࣠ͷภ৺͸ 1 µm Ҏ಺ʹʹΑΓɼৣࡎதʹ෼ࢄ͍ͯ͠Δༀޮ੒෼ɼො‫ࡎܗ‬ɼ͓

ऩ·͓ͬͯΓɼߴਫ਼౓ͷ CT ը૾࠶ߏ੒͕ՄೳͰ͋Δɽ·ͨɼϢʔβʔ࣋ࠐͷ૷ஔ͕ઃஔՄೳͳεϖʔε΋֬อ͞Ε͓ͯΓɼཁ๬ʹԠͨ͡ in situ ‫࡯؍‬Λߦ͏͜ͱ
͕Ͱ͖Δɽͦͷଞʹ΋Πϝʔδϯά࣮‫Ͱݧ‬͸ɼϏʔϜϥΠϯอ༗ͷ൚༻Ճ೤࿍͓ΑͼϨΦϝʔλʔηϧΛར
༻͢Δ͜ͱ΋Ͱ͖Δɽ౤Ө૾ͷࡱӨʹ͸ɼ̭ઢ–Մࢹޫม‫׵‬γϯνϨʔλɼϦϨʔϨϯζ (λϯσϜϨϯζ)ɼߴղ૾౓ɾߴ‫౓ײ‬σδλϧΧϝϥͰߏ੒͞ΕΔؒ઀‫̭ܕ‬ઢը૾‫ݕ‬ग़‫ث‬Λ࢖༻͓ͯ͠Γɼ‫࡯؍‬ର৅ʹ߹Θͤͯࢹ໺ɾۭؒ෼ղೳΛௐઅ͢ΔɽTable 1 ʹ͸ɼը૾‫ݕ‬ग़‫ث‬ͷ࢓༷Λࣔͨ͠ɽ௨ৗɼγϯνϨʔλ͸ P43ʢGd2 O2 S;Tbʣค຤εΫϦʔϯΛ༻͍͍ͯΔ͕ɼߴۭؒ෼ղೳࡱӨ࣌ʹ͸ɼ

YAG;Ce ୯݁থεΫϦʔϯΛར༻͢Δ͜ͱ͕Ͱ͖Δɽ౤Ө૾͸γϯνϨʔλʹΑΓՄࢹޫʹม‫͞׵‬Εͨ‫ޙ‬ɼϦϨʔϨϯζʹΑΓ 1–10 ഒʹ֦େ͞ΕɼσδλϧΧ
ϝϥͰ‫ه‬࿥͞ΕΔɽBL08B2 Ͱ͸ɼ޿ࢹ໺ࡱӨ༻ʹ 10ϝΨϐΫηϧ CCD Χϝϥɼ͓Αͼߴ଎ࡱӨ༻ʹ࠷େ

45 ϑϨʔϜ/ඵͷ CMOS ΧϝϥΛ੔උ͓ͯ͠Γɼ࣮‫ݧ‬৚݅ʹΑΓ࢖͍෼͚͍ͯΔɽը૾‫ݕ‬ग़‫ث‬͸ޫ࣠ͱฏߦͳฒਐϨʔϧ্ʹઃஔ͞Ε͓ͯΓɼޫͷ఻೻ʹΑΔ
۶ંίϯτϥετͷޮՌΛಘΔͨΊʹɼࢼྉ–ը૾‫ݕ‬ग़‫཭ڑؒث‬Λ 30–1000 mm ·Ͱ༰қʹมߋ͢Δ͜ͱ
͕Ͱ͖ΔɽຊγεςϜͰར༻Ͱ͖Δ࠷େࢹ໺͸͓Αͦԣ 20 mm × ॎ 10 mm Ͱ͋Γɼ10 mm Λ௒͑ΔαΠζͷ޻‫ۀ‬੡඼ʹରͯ͠΋ 2 ࣍Ճ޻͢Δ͜ͱͳ͘ɼͦͷ··ͷঢ়ଶͰ CT ࡱӨ͢Δ͜ͱ͕ՄೳͰ͋Δɽ

– 31 –

Fig. 2. Volume rendering images of drug tablets.

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)ΑͼίʔςΟϯά૚ΛՄࢹԽ͢Δ͜ͱ͕Ͱ͖ɼৣࡎͷͱΛ༥߹ͨ͠ଌఆγεςϜΛߏங͢ΔɽXAFS ͷ‫ݕ‬ग़඼࣭Λࠨӈ͢Δༀޮ੒෼ͷαΠζɾ෼෍ͷ‫ۉ‬Ұੑɼ͋‫ʹܥ‬ը૾‫ݕ‬ग़‫ث‬Λ༻͍Δ͜ͱͰɼ޿ྖҬ͔ͭ਺ µm ͷΔ͍͸ίʔςΟϯά૚ͷް͞ͳͲͷॏཁͳ৘ใΛಘΔ

Ґஔ෼ղೳͰͷ XAFS ଌఆ͕ՄೳʹͳΔɽຊख๏͸ɼ͜ͱ͕Ͱ͖ΔɽϚΠΫϩϏʔϜΛར༻ͨ͠૸ࠪ‫ܕ‬ख๏ʹൺֱͯ͠ɼ୹
࣌ؒͰ޿ྖҬͷ 2 ࣍‫ ݩ‬XAFS ϚοϓΛಘΔ͜ͱ͕Ͱࠓ‫ޙ‬ͷ‫ܭ‬ը͖ɼి஑෼໺Ͱͷి‫ۃ‬पลͷ‫ߏॴہ‬଄ղੳ౳΁ͷ༗ޮ‫ࡏݱ‬ɼߴۭؒ෼ղೳࡱӨΛ‫ر‬๬͢ΔϢʔβʔʹରͯ͠ɼYAG;Ce ୯݁থεΫϦʔϯΛ༻͍ͨߏ੒ͷը૾‫ݕ‬ग़‫ث‬Λఏ‫͍ͯ͠ڙ‬Δɽ͔͠͠ͳ͕Β P43 ค຤εΫϦʔϯΛ༻͍ͨ৔߹ʹൺֱͯ͠ɼຊߏ੒Ͱ͸ɼ1 ຕͷ౤Ө૾ΛࡱӨ͢ΔͨΊʹ 30 ഒҎ্ͷ࿐ޫ͕࣌ؒඞཁͰ͋
ΔͨΊɼଟ਺ͷ౤Ө૾ΛࡱӨ͢Δ CT ͷεϧʔϓοτੑ͸ඇৗʹѱ͍ɽͦ͜Ͱɼը૾‫ݕ‬ग़‫ث‬ͷߴޮ཰ԽΛਤ
Δɽ۩ମతʹ͸ɼ୯݁থγϯνϨʔλͷࡐ࣭ɼް͓͞
ΑͼϦϨʔϨϯζΛ‫ݟ‬௚͠ɼۭؒ෼ղೳΛམͱͣ͞ɼ
࿐ޫ࣌ؒΛ 1/2 ҎԼ΁୹ॖ͢Δ͜ͱΛ໨ඪͱ͍ͨ͠ɽ

BL08B2 ͸ɼ̭ઢ‫ٵ‬ऩ୺ඍࡉߏ଄ (XAFS) ෼ੳʹదͨ͠ޫֶ‫ܥ‬Λ༗͢Δɽͦ͜ͰɼXAFS ͱΠϝʔδϯάར༻͕‫ظ‬଴Ͱ͖Δɽ͔͠͠ͳ͕Β XAFS Πϝʔδϯάଌఆ͸ɼ্‫ه‬ͷར఺ͷ൒໘ɼ̍ճͷଌఆͰऩू͞ΕΔσʔλ͕๲େͳྔͱͳΔͨΊɼଌఆ‫ޙ‬ͷσʔλॲཧ͕໰୊ʹͳΔ͜ͱ͕‫ݒ‬೦͞ΕΔɽͦ͜Ͱ࢈‫ۀ‬ར༻ల։
͢Δʹ౰ͨΓɼϋʔυ΢ΣΞͷ੔උ͚ͩͰͳ͘ɼσʔλॲཧ౳ͷιϑτ໘ͰɼϢʔβʔ͕ϧʔνϯతʹར༻Ͱ͖ΔγεςϜͷߏஙΛ໨ࢦ͢ɽ·ͨຊख๏Λ 2 ࣍‫ݩ‬Πϝʔδϯά͔Β CT ๏ʹΑΔ 3 ࣍‫ݩ‬Πϝʔδϯά΁ͷ֦ு΋‫ݕ‬౼͍ͨ͠ɽ
ࢀߟจ‫ݙ‬[1] H. Takano, Y. Urushihara and J. Matsui:
SPring-8 Research Frontiers 2010, 140 (2011).

– 32 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

BL08B2

2010B3331, 2011B3331

খ̭֯ઢࢄཚ (SAXS) ʹΑΔΞΫϦϧ‫ܥ‬ΤϚϧγϣϯཻࢠ͓Αͼൽບͷߏ଄ղੳ

Structure Analysis of Acrylic Emulsion Particles and Films
by Small Angle X-ray Scattering (SAXS)ࢁຊ ༑೭ɼҪ্ ढ़ຬɼ໦ా ཁɼ੢‫ ݪ‬༏ࢠɼాଜ ௚‫ٱ‬ɼླ໦ ‫ܙ‬ଠɼଜ্ ਖ਼
Tomoyuki Yamamoto, Kaname Kida, Yuko Nishihara, Naohisa Tamura, Keita Suzuki,
Tadashi Murakami೔ຊ߹੒Խֶ޻‫ࣜגۀ‬ձࣾ தԝ‫ॴڀݚ‬Central Research Laboratory, The Nippon Synthetic Chemical Industry Co., Ltd.

֓ཁɿ খ֯ X ઢࢄཚ (SAXS) Λ༻͍ͯϙϦϚʔΤϚϧγϣϯཻࢠͷߏ଄͔Βൽບͷ‫ܗ‬੒աఔ͓Αͼߏ଄ͷղੳΛߦͬͨɽಈతޫࢄཚ (DLS) ͔Βͷཻࢠ‫( ܘ‬dDLS ) ͱ SAXS ͔Βͷཻ‫( ܘ‬dSAXS ) Λ༻͍ͯɼਫதͰͷք໘‫׆‬ੑࡎͷ޿͕ΓͰ͋ΔίϩφαΠζ (Cs ) ΛධՁͨ͠ɽCs ͸ք໘‫׆‬ੑࡎ෼ࢠ࠯௕ͱ‫૿ʹڞ‬Ճ͕ͨ͠ɼ࠯௕͕௕
͘ͳΔʹैͬͯ๞࿨܏޲Λࣔͨ͠ɽൽບ‫ܗ‬੒աఔͰ͸ɼཻ‫ܘ‬͸มԽͤͣʹཻࢠؒ‫ͳ͘୹͕཭ڑ‬Δ͜ͱʹΑͬͯϑΟϧϜ͕‫ܗ‬੒͞ΕΔ͜ͱ͕໌Β͔ͱͳͬͨɽ࠷ऴతʹͰ͖ͨൽບதͰ͸ɼཻࢠ͸࿡ํ࠷ີॆరߏ଄Λͱ͍ͬͯͨɽ੡ບ௚‫ޙ‬ͷϑΟϧϜͰ͸ཻࢠࠟ͸໌ྎ͕ͩɼ‫࣌ܦ‬తʹ༥ண͕ਐߦཻ͠ࢠ͕ࠟෆ઱໌ʹͳ͍ͬͯ͘͜ͱ΋֬ೝ͞Εͨɽ
ΩʔϫʔυɿɹΤϚϧγϣϯɼք໘‫׆‬ੑࡎɼখ֯ X ઢࢄཚɼಈతޫࢄཚɼίϩφɼ࿡ํ࠷ີॆర

എ‫ڀݚͱܠ‬໨త·ͨɼDLS ͸ଌఆର৅༹͕ӷʹ‫ݶ‬ఆ͞ΕΔ͜ͱ΍ίۙ೥ɼ‫ڥ؀‬໰୊΁ͷؔ৺ͷߴ·Γ͔Β༗‫͔ܥࡎ༹ػ‬Βਫ‫΁ܥ‬Ҡߦ͕‫ٸ‬଎ʹਐߦ͍ͯ͠ΔɽຊใͰѻ͏ϙϦϚʔΤϚϧγϣϯͱ͸ 50 – 500 nm ͷߴ෼ࢠඍཻࢠ
͕ք໘‫׆‬ੑࡎʹΑͬͯਫதʹ෼ࢄͨ͠΋ͷͷ͜ͱͰ͋Γɼ༗‫ࡎ༹ػ‬Λ࢖༻͠ͳ͍‫ʹڥ؀‬΍͍͞͠ૉࡐͰ͋Δɽ͜ͷಛ௃Λ‫͔ͯ͠׆‬ίʔςΟϯάࡎ΍ృྉɼ೪ணࡎͳ
Ͳɼͦͷ༻్ͱधཁ͸೥ʑ֦େ͍ͯ͠ΔɽΤϚϧγϣ
ϯͷେ͖ͳಛ௃͸ɼίʔςΟϯάաఔͰ͸ӷମͰ͋Δ
ͷʹର͠ɼ࠷ऴ༻్Ͱ͸‫ݻ‬ମʹมԽ͢Δ͜ͱͰ͋ΔɽͦΕ‫ނ‬ɼߴ‫ػ‬ೳੑΤϚϧγϣϯͷ։ൃʹ౰ͨͬͯ͸೪౓҆ఆੑɼృ޻ੑͷΑ͏ͳ༹ӷ෺ੑ͔Βൽບ‫౓ڧ‬ͷΑ͏ͳ‫ݻ‬ମ෺ੑ·Ͱͷ೺Ѳ͕ඞཁͰ͋Δɽ
ΤϚϧγϣϯͷߏ଄ղੳͷख๏ͱͯ͠Ϩʔβʔ‫ݦ‬ඍ‫[ ڸ‬1] ΍૸ࠪ‫͋ܕ‬Δ͍͸ಁա‫ݦࢠిܕ‬ඍ‫࡯؍ڸ‬౳ [2] ͕͋ΔɽͦΕΒͷख๏͸࣮ۭؒ‫͋Ͱ࡯؍‬Γͦͷղऍ͸༰ΞɾγΣϧͱཻ͍ͬͨࢠ಺ߏ଄ʹؔ͢Δ஌‫͕ݟ‬ಘΒΕͳ͍ͱ͍͏໰୊͕͋Δɽ
ۙ೥ɼ์ࣹޫར༻͕੝ΜʹͳΓ SAXS ΋ൺֱతར༻͠΍͘͢ͳ͖ͬͯͨ͜ͱ͔ΒɼΤϚϧγϣϯͷධՁʹ‫͞༻׆‬Ε͍ͯΔ [3]ɽͨͩ͠ɼSAXS ͷ৘ใ͸‫ۭٯ‬ؒͷ΋ͷʹͳΔͷͰղऍ͸ଟগ೉͘͠͸ͳΔ͕ɼฏ‫ۉ‬తͳ৘ใ͕ಘΒΕΔ͜ͱɼཻࢠ‫ܗ‬ঢ়΍ཻࢠ಺ߏ଄͋Δ͍͸༹ӷ/‫ݻ‬ମͷ૬Λ໰ΘͣʹଌఆՄೳͰ͋Δͱ͍ͬ
ͨಛ௃͕͋Δɽ·ͨɼ࣌෼ׂଌఆΛߦ͑͹ಈతͳաఔ
ͷ৘ใ΋ಘΒΕΔ [4, 5]ɽ͜͜Ͱ͸ SAXS Λ༻͍ͯΤϚϧγϣϯͷཻࢠߏ଄ɼൽບͷ‫ܗ‬੒աఔ͓Αͼߏ଄ͱ༹͍ͬͨӷ͔Β‫ݻ‬ମʹࢸΔ·Ͱͷߏ଄ͷղੳ݁Ռʹ͍ͭͯใࠂ͢Δɽ࣮‫ݧ‬қͰ͋Δɽ͔͠͠‫ྖ࡯؍‬Ҭ͕‫ॴہ‬తͰ͋Δ͜ͱɼม‫ܗ‬ք໘‫׆‬ੑࡎ෼ࢠ࠯௕ͱίϩφαΠζ Cs ͱͷؔ܎ΛௐԼͰͷଌఆʹࠔ೉͞Λ൐͏ͳͲͱ͍ͬͨ՝୊͕͋Δɽ΂ΔͨΊʹ༻͍ͨࢼྉΛ Table 1 ʹࣔ͢ɽSAXS ଌఆ͸– 33 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)
Table 1. Emulsion specimens having the surfactants with various molecular lengthcode

polymersurfactant

extended molecular length/ nm

2EHA-ANR

2EHA

anionic non-reactive

6.3

2EHA-AR
2EHA-NR↑↑

anionic reactive
nonionic reactive

7.5
17.7

anionic polyvinyl alcohol

31.5

2EHA-PVOH↑

2EHA: 2-ethylhexyl acrylate
Table 2. A specimen for monitoring drying processcode

surfactant

Tg
/ oC

dSAXS
/ nm

dDLS
/ nm

2EHA/AA-AR

anionic reactive

-70

153.7

174.0

AA: acrylic acid
Table 3. Specimens for structure analysis of the films
code

surfactant

dSAXS

dDLS

/ nm

/ nm

2EHA/AA-AR
BA/AA-ARanionic reactive
anionic reactive

153.7
135.9

174.0
143.8

2EHA/MAA-ANR

anionic non-reactive

89.4

111.1

BA: butyl acrylate, MAA: methacrylic acid
SPring-8 ͷ BL08B2 Λ࢖༻͠ɼ໿ 6 m ͷΧϝϥ௕Ͱߦͬͨɽଌఆͨ͠ΤϚϧγϣϯೱ౓͸ 5 mass% Ͱ͋Δɽ·ͨɼΤϚϧγϣϯ‫ر‬ബ༹ӷΛ༻͍ͯ DLS(NICOMPTM

380 ZLS, Particle Sizing Systems) ଌఆ΋ߦ͍ɼdDLSΛධՁͨ͠ɽ
ൽບ‫ܗ‬੒աఔͷ௥੻ʹ͸ Table 2 ͷࢼྉΛ༻͍ɼछʑ
ͷೱ౓ʹௐ੡ͨ͠ࢼྉΛ༻͍ͨɽ͞Βʹɼ੡ບ‫ ޙ‬7 ͔݄‫ܦ‬աͨ͠ࢼྉͷଌఆ΋ߦ͍ɼ‫࣌ܦ‬తͳൽບߏ଄มԽ
΋ධՁͨ͠ɽTable 3 ʹࣔ͢ࢼྉΛ༻͍ɼࣨԹͰ෩‫ס‬ʹΑΓ੡ບͨ͠ࢼྉͷ SAXS ଌఆ͔Βൽບߏ଄ͷղੳΛߦͬͨɽ
݁Ռ͓Αͼߟ࡯
ΤϚϧγϣϯཻࢠߏ଄ ಘΒΕͨࢄཚ‫ۂ‬ઢΛΨ΢ε෼෍ʹ͕ͨ͠͏‫ٿ‬ϞσϧͰղੳͯ͠ dSAXS Λࢉग़͠
ͨɽFig. 1 ͸ dSAXS ɼdDLS ɼCs ͔ΒಘΒΕͨΤϚϧ

Fig. 1.

γϣϯཻࢠߏ଄Λ໛ࣜతʹࣔͨ͠΋ͷͰ͋Δɽࣼࣈ͕cles having the surfactants with various molecularlength. Deep and light blue areas indicate the sizes

dSAXS Λɼଠࣈ͕ dDLS Λ͍ࣔͯ͠Δɽ
Fig. 2 ͸ɼք໘‫׆‬ੑࡎͷ৳ͼ͖Γ෼ࢠ࠯௕ͱ Cs ͷؔ܎Λࣔͨ͠΋ͷͰ͋Δɽ2EHA-ANRɼ2EHA-AR ͷ

Schematic models of the emulsion parti-of the core and the corona of the emulsion particles,
respectively.

– 34 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू
Α͏ʹք໘‫׆‬ੑࡎͷ෼ࢠ࠯௕͕୹͍ͱ Cs ͸ͦͷ৳ͼͯ‫࣌ܦ‬తʹཻࢠؒͷ༥ண͕‫͜ى‬Γɼք໘ͷίϯτϥε

͖Γ෼ࢠ࠯௕ͱ΄΅ରԠ͍ͯͨ͠ɽҰํɼք໘‫׆‬ੑτ͕ෆ઱໌ʹͳΓ SAXS ϐʔΫ͕ग़೉͘ͳͬͨͨΊࡎͷ෼ࢠ࠯௕͕௕͘ͳΔʹैͬͯ Cs ͸૿େ͍ͯ͘͠

Ͱ͋Δͱߟ͑ΒΕΔɽ

͕ɼൺྫతʹ૿େ͢ΔͷͰ͸ͳ͘๞࿨܏޲Λࣔͨ͠ɽ͜ͷ‫ڍ‬ಈ͔Βք໘‫׆‬ੑࡎ෼ࢠ࠯௕͕ൺֱత୹͍৔߹ɼ
຤୺ΠΦϯͷ੩ి൓ൃʹΑΓൺֱత৳ͼ͖ͬͨߏ଄Λ
ͱ͍ͬͯΔͷʹର͠ɼͦͷ෼ࢠ࠯௕͕௕͘ͳΔͱΤϯτϩϐʔޮՌͷ‫د‬༩ͷͨΊ۶‫ߏͨ͠ۂ‬଄Λͱ͍ͬͯΔ
ͱਪఆ͞ΕΔɽैདྷɼίΞཻࢠ͔Βք໘‫׆‬ੑࡎ͕௕͍
ໟͷΑ͏ʹੜ͍͑ͯΔϞσϧ͕ଟࣔ͘͞Ε͍ͯΔ͕ɼ

2EHA-ANRɼ2EHA-AR ͷք໘‫׆‬ੑࡎ͸ίΞཻࢠ͔Β୹͍ࢗͷΑ͏ʹੜ͍͑ͯΔ࣮ଶ͕໌Β͔ͱͳͬͨɽ

Fig. 3. SAXS profiles at various sample concentrations during dry process. Numerical values in theFig. 2. Relationship between corona size and extended molecular length of surfactants.
‫ס‬૩աఔ ೱ౓ͷҟͳΔΤϚϧγϣϯͷࢄཚ‫ۂ‬ઢΛfigure represent nonvolatile content of the polymer
emulsions. Dark gray broken line and light graychain line represent the shift of the peaks upon close
packing and the position of the peaks by scattering
due to the particles themselves, respectively. Curves

Fig. 3 ʹࣔ͢ (ϐʔΫҐஔͷมԽΛ‫ݟ‬΍͘͢͢ΔͨΊ

are vertically shifted. “After 7 months” in the figure represents the sample stored for 7 months afterʹɼॎ࣠ʹؔͯ͠͸γϑτͯ͠ϓϩοτ)ɽೱ౓ 99.7

casting a film at room temperature.

mass% ͷ΋ͷ͸‫ס‬૩ൽບʹ૬౰͢Δɽೱ౓͕ 6.25 mass%ൽບߏ଄ Fig. 4 ͸ Table 3 ͷࢼྉͷ Iq 2 − q ϓϩοͰ q = 0.03 nm−1 ෇ۙʹཻࢠؒ‫ׯ‬বޮՌʹΑΓϐʔΫ͕ग़‫͠ݱ‬ɼೱ౓͕ߴ͘ͳΔʹैͬͯ͜ͷϐʔΫ͸τͰ͋ΔɽҰ൪େ͖ͳϐʔΫͷҐஔʹର͢Δߴ࣍ϐʔߴ q ଆ΁γϑτ͍ͯͬͨ͠ (ਤதͷ఺ઢ)ɽͦͯ͠ɼ࠷

ΫͷҐஔͷൺ΋ਤதʹࣔͨ͠ɽϐʔΫൺ͕
√√
1: 3: 2: 7: 3 · · · ͷ৔߹ɼ࿡ํ࠷ີॆరߏ଄Λҙຯ͢ऴతʹൽບͷཻࢠؒ‫ʹ཭ڑ‬૬౰͢Δ q = 0.048 nm−1ʹͳͬͨɽҰํɼΤϚϧγϣϯཻࢠࣗ਎͔Βͷࢄཚ͸

Δɽࠓճͷࢄཚ‫ۂ౓ڧ‬ઢͰ͸ϐʔΫ͕ϒϩʔυͰ͋Γ෇ۙʹग़‫͢ݱ‬Δ͕ɼೱ౓͕૿Ճͯ͠

શͯͷϐʔΫ͕‫͞࡯؍‬Ε͍ͯͳ͍͕ɼϐʔΫҐஔൺ͕΋ͦͷҐஔ͸΄ͱΜͲมԽ͠ͳ͔ͬͨ (ਤதͷೋ఺࠯࿡ํ࠷ີॆరͷͦΕʹ͍ۙͷͰɼൽບதͰཻࢠ͸࿡ํઢ)ɽ͜ͷ͜ͱ͔ΒΤϚϧγϣϯൽບͷ‫ܗ‬੒աఔͰ͸࠷ີॆరߏ଄Λͱ͍ͬͯΔ΋ͷͱਪ࡯͞Εͨ [6]ɽq = 0.078 nm−1ཻࢠαΠζ͸มԽͤͣʹɼཻࢠؒ‫͢઀͕ۙ཭ڑ‬Δ͜ͱʹΑΓൽບ͕‫ܗ‬੒͞ΕΔ͜ͱ͕෼͔ͬͨɽ੡ບ‫ ޙ‬7 ͔·ͱΊͱࠓ‫ޙ‬ͷ՝୊݄‫ܦ‬ա (ࣨԹอ؅) ͨ͠΋ͷ͸ q = 0.048 nm−1 ͷϐʔ

SAXS Λ༻͍ͯΤϚϧγϣϯཻࢠͷߏ଄ɼൽບͷ‫ܗ‬Ϋ͕ফࣦͨ͠ɽ͜Ε͸ࢼྉͷΨϥεసҠԹ౓ (Tg) ͕੒աఔ͓Αͼߏ଄Λղੳͨ͠ɽͦͷ݁Ռɼք໘‫׆‬ੑࡎࣨԹҎԼͰ͋ΔͨΊɼϙϦϚʔ෼ࢠ࠯͕‫͠ࢄ֦ʹ͍ޓ‬͸෼ࢠ࠯௕͕୹͍ͱ৳ͼ͖ͬͨߏ଄ɼ௕͍ͱ΍΍۶‫ۂ‬– 35 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)ࠓ‫ޙ‬͸ߴً౓ͳ์ࣹޫͷಛ௃Λ‫͔ͯ͠׆‬ɼ ࣌෼ׂଌఆʹΑΔม‫ܗ‬ԼͰͷൽບͷߏ଄มԽΛ௥੻͢Δ͜ͱ
Ͱɼൽບߏ଄ͱ෺ੑͱͷ૬͕ؔΑΓ໌Β͔ʹͰ͖Δͱ
‫ظ‬଴͍ͯ͠ΔɽँࣙSAXS ଌఆΛߦ͏ʹ౰ͨΓɼͻΐ͏͝Պֶٕज़‫ڠ‬ձͷ‫܂‬ຊ࣎ੜࢯΛ͸͡Ίଟ͘ͷํʑʹ͓ੈ࿩ʹͳΓ·ͨ͠ɽ͜ͷ৔ΛआΓ͓ͯྱΛਃ͋͛͠·͢ɽࢀߟจ‫ݙ‬

Fig. 4. Iq 2 − q plot for emulsion films. Ratios of theposition of higher order peaks or shoulders to thatof the first peak are also indicated.

ͨ͠ߏ଄Λͱ͍ͬͯΔͱߟ͑ΒΕͨɽൽບ‫ܗ‬੒աఔͰ͸ཻ‫ܘ‬͸มԽͤͣʹɼཻࢠؒ‫ͯͬͳ͘୹͕཭ڑ‬ൽບ͕‫ܗ‬੒͞ΕΔ͜ͱ͕෼͔ͬͨɽ࠷ऴతʹ‫ܗ‬੒͞Εͨൽບதͷཻࢠ͸࿡ํ࠷ີॆరߏ଄Λͱ͍ͬͯͨɽͦͯ࣌͠
ؒ‫ܦ‬աͱͱ΋ʹ༥ண͕ਐߦ͠ɼཻࢠ‫ڥ‬ք͕ෆ઱໌ʹ[1] G. Balakrishnan, T. Nicolai, L. Benyahia, and D.
Durand: Langmuir, 28, 5921-5926 (2012).
[2] ྛ༝‫ࢠل‬ɼత৔ઍࡀɼ໼෦੓࣮: ృྉͷ‫ڀݚ‬ɼ147ɼ
7-11 (2007).
[3] F. C. Giacomelli, I. C. Riegel, P. Stepánek, C.
L. Petzhold, M. D. Ninago, Á. J. Satti, A.
E. Ciolino, M. A. Villar, V. Schmidt, and C.
Giacomelli: Langmuir, 26, 14494-14501 (2010).
[4] S. Hu, J. Rieger, Y. Lai,.S. V. Roth, R. Gehrke,
and Y. Men: Macromolecules, 41, 5073-5076(2008).
[5] X. Chen, S. Fischer, and Y. Men: Langmuir, 27,
12807-12814 (2011).
[6] ࣨҪ फҰ: ߴ෼ࢠϥςοΫεͷԽֶɼߴ෼ࢠ‫ߦץ‬ձɼp235 (1970).

ͳ͍ͬͯ͘͜ͱ΋໌Β͔ͱͳͬͨɽ

– 36 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

2008A3321, 200863321, 2009A3321, 200963321

BL08B2τϙάϥϑΟʔʹΑΔ 4H-SiC ΤϐλΩγϟϧບதͷਕঢ়సҐͷධՁInvestigation of Threading Edge Dislocationin 4H-SiC Epitaxal Layers by X-Ray Topography‫ ึޭ ాח‬1 ɼ௕໺ ਖ਼༟ 1 ɼ໺‫ ޱ‬ਅҰ 2 ɼࢁຊ ݈Ұ 2 ɼখ໺ ‫ت‬๕ 2 ɼࣉా ‫ܓ‬հ 2 ɼ౔ా लҰ 1
Isaho Kamata1 , Masahiro Nagano1 , Shininchi Noguchi2 ,Ken-ichi Yamamoto2 , Kiyoshi Ono2 , Keisuke Terada2 , Hidekazu Tsuchida111(Ұࡒ) ిྗதԝ‫ॴڀݚ‬ɼ2 (‫ి )ג‬ΧςΫϊγεςϜζ

CRIEPI, 2 Electric Power Engineering Systems Co., Ltd.

֓ཁɿɹ̭ઢτϙάϥϑΟʔଌఆΛ༻͍ͯ, 4H-SiC ΤϐλΩγϟϧບதʹ‫·ؚ‬ΕΔਕঢ়సҐ (Threading Edge

Dislocation : TED) ͷసҐ૾‫ܗ‬ঢ়ʹ͍ͭͯௐࠪΛߦͬͨɽτϙάϥϑΟʔଌఆͰಘΒΕΔ 6 छྨͷҟͳͬͨ
TED ૾͸ɼTED ͷόʔΨʔεϕΫτϧͱճંϕΫτϧͷͳ֯͢౓ʹΑͬͯੜ͡Δ͜ͱ͕ɼγϛϡϨʔγϣϯͱ࣮ࡍͷసҐ૾ͱͷর߹݁Ռ͔Β໌Β͔ʹͳͬͨɽΩʔϫʔυɿɹ̭ઢτϙάϥϑΟʔ, 4H-SiCɼਕঢ়సҐɼTEDɼόʔΨʔεϕΫτϧ

എ‫ڀݚͱܠ‬໨త࣮‫ݧ‬զʑ͸ɼকདྷͷిྗ҆ఆ‫ٕڅڙ‬ज़ͷߴ౓Խ͓ΑͼΤ࣮‫ݧ‬͸ BLO8B2 ʹ͓͍ͯɼϏʔϜΛࢼྉද໘͢Ε͢ωϧΪʔߴޮ཰ར༻ͷਪਐͨΊɼߴੑೳύϫʔΤϨΫΕʹೖࣹͤ͞Δ (grazing incident beam topography)τϩχΫε‫ʹثػ‬ద༻Մೳͳߴ଱ѹɾ௿ଛࣦ SiC ύख๏Λ༻͍ͯߦͬͨɽଌఆ͸ 1128 ൓ࣹΛ༻͍ͯɼද

ϫʔ൒ಋମૉࢠͷ‫ڀݚ‬։ൃΛߦ͍ͬͯΔ.

໘΁ͷϏʔϜೖࣹ֯͸໿ 5◦ ͱͯ͠ߦͳͬͨɽ

SiC ͸ɼ޿͍όϯυΪϟοϓɼߴ͍೤఻ಋ཰ɼߴ͍

ϏʔϜ͸ɺSi(111) ϞϊΫϩϝʔλʹΑͬͯ୯৭Խ

ઈԑഁյిѹ‫Ͳͳ౓ڧ‬༏Εͨ෺ੑ஋Λ࣋ͬ͜ͱ͔Βɼ͠ɼ೾௕ 1.541 Å Λ༻͍ͨɽ2θ-θ ΰχΦϝʔλத৺଱ߴԹɼ௿ଛࣦ൒ಋମύϫʔσόΠεࡐྉͱͯ͠஫໨

ʹࢼྉΛηοτ͠ɼ2θ ΞʔϜʹઃஔͨ͠ΠΦϯνϟ

͞Ε͍ͯΔ.

ϯόʹͯɼϩοΩϯάΧʔϒΛͱΓɼҐஔ߹ΘͤΛߦ͔͠͠ɼSiC ‫ج‬൘΍ΤϐλΩγϟϧບ (ΤϏບ) தͳͬͨɽʹ݁থܽؕ΍సҐ͕ߴີ౓ʹଘࡏ͢Δ͜ͱ͕ɼSiC ύࢼྉ͸ɼ᫔ࣹ೤Ճ೤ CVD Λ༻͍ͯɼ੒௕৚݅ɼ1545

ϫʔ൒ಋମૉࢠͷ࣮༻Խ֦େΛ્֐͢ΔҰͭͷཁҼ◦Cɼ42 Torr ʹͯɼSi ໘ 8◦ Φϑ‫ج‬൘্ʹΤϏ੒௕͞ͱͳ͍ͬͯΔ. SiC ‫ج‬൘΍ΤϏບதʹ͸ɼΒͤΜసҐͤͨް͞ 20 µm ͷ΋ͷΛ࢖༻ͨ͠ [1].

(TSD)ɼਕঢ়సҐ (TED)ɼ‫ج‬ఈ໘಺సҐ (BPD)ɼੵ
૚ܽؕͳͲଟ͘ͷసҐ΍͕ܽؕ‫·ؚ‬Ε͓ͯΓɼૉࢠྖ݁Ռ͓Αͼߟ࡯

Ҭʹଘࡏ͢ΔͱɼૉࢠಛੑΛѱԽͤ͞Δͱ‫ݴ‬ΘΕ͍ͯΔ. ͦͷͨΊɼసҐ΍ܽؕͷੑ࣭Λ໌Β͔ʹͯ͠ɼີ౓Λ‫ݮ‬গͤ͞ΔํࡦΛߨ͡Δ͜ͱ͕ॏཁͰ͋Δ.
ࠓճ͸ɼ̭ઢτϙάϥϑΟʔଌఆΛ༻͍ͯɼ4H-SiC
ΤϐλΩγϟϧບதʹ‫·ؚ‬ΕΔ TED ͷసҐ૾‫ܗ‬ঢ়ʹ͍ͭͯௐࠪΛߦͬͨ݁ՌΛใࠂ͢Δ.

4H-SiC ΤϏບද໘্ʹଘࡏ͢Δ TSD ͸ɼόʔΨʔεϕΫτϧͱͯ͠ɺ‫ج‬ఈ໘ʹਨ௚ͳํ޲ͷ 1c[0001] Λ࣋ͭɽࠓճͷࢼྉ͸ɺ(0001)Si ໘ 8◦ Φϑ‫ج‬൘Ͱ͋ΔͨΊ 8◦ ͚ͩ<1120>ํ޲ʹ܏͍ࣼͯ͠Δɽ

TED ͸όʔΨʔεϕΫτϧͱͯ͠ɼ 13 a <1120>ͷ
λΠϓΛ࣋ͭ͜ͱ͕஌ΒΕ͓ͯΓɼ4H-SiC ͷΑ͏ͳ– 37 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)࿡ํথͷ݁থதͰ͸ɼ6 ํ޲ͷόʔΨʔεϕΫτϧΛ
࣋ͭͱߟ͑ΒΕΔɽ

Fig. 1 ʹɼτϙάϥϑΟʔଌఆͰಘΒΕͨ 4H-Sic
ΤϏບද໘্ʹଘࡏ͢Δ TED(a – f) ͱ TSD(g) ͷసҐίϯτϥετ૾Λࣔ͢ɽFig. 1 ͷ 6 छྨͷ TED ͱ

TSD ͷτϙάϥϑΟʔ૾͸ɼશͯ 1 ճͷࡱӨͰಘΒΕͨಉҰͷτϙάϥϑΟʔࣸਅ্ʹ͓͍ͯ‫͞࡯؍‬Εͨ΋ͷͰ͋ΔɽసҐ૾ͷίϯτϥετ͔Βɼ6 छྨͷ TEDͷసҐ૾͕ࣝผՄೳͰ͋Δ͜ͱ͕Θ͔Δɽ

Fig. 2. Simulation result of topography images of
TED seach having an 13 a <1120> Burgers vector
with six different directions.
– f) ͸ɼFig. 1 ͷ‫( ߸ه‬a – f) ʹରԠ͍ͯ͠Δ͜ͱ͕෼͔Δ.
Ҏ্ͷ݁Ռ͔Β, ࣮‫Ͱݧ‬ಘΒΕͨ 6 छྨͷ TED ૾͕ɺόʔΨʔεϕΫτϧͷҧ͍ʹΑΔ૾Ͱ͋Δ͜ͱ͕֬ೝ͞Εͨ [2, 3].
ࠓ‫ޙ‬ͷ՝୊

Fig. 1. Synchrotron X-ray topography images of(a)-(f) TEDs and (g) TSD in 4H-SiC epilayer.

͜Ε·Ͱ൑ผෆՄೳͰ͋ͬͨ TED ͷόʔΨʔεϕΫτϧํ޲ΛɼసҐ૾ͷ‫ܗ‬ঢ়͔Β൑ผ͢Δ͜ͱʹ੒ޭ͜Ε·Ͱ KOH Τονϯά๏΍൚༻τϙάϥϑΟʔͨ͠ɽࠓ‫ޙ‬͸ɼTED Ҏ֎ͷ༷ʑͳܽؕʹ͍ͭͯ΋ଌఆΛਐΊ͍ͯ͘ɽ

Ͱ͸ɼ6 छྨͷ TED ͸ࣝผ͞Εͣɼ1 छྨͷΤονϐοτ΍τϙ૾͔͠‫͞࡯؍‬Ε͍ͯͳ͔ͬͨɽ͔͠͠ɼ
ࠓճͷτϙάϥϑΟʔख๏ʹΑͬͯɼ6 छྨͷࣝผ͕ՄೳͱͳΔ͜ͱ͕໌Β͔ʹͳͬͨɽ

Fig. 2 ʹɼγϛϡϨʔγϣϯʹΑͬͯಘΒΕͨ TEDసҐ૾Λࣔ͢ɽTED సҐͷόʔΨʔεϕΫτϧͱճંϕΫτϧͷͳ֯͢౓ʹΑΓɼ6 छྨͷసҐτϙάϥϑΟʔ૾͕ಘΒΕͨɽճંϕΫτϧ g ͱɼTED ͷόʔb ͷ૬ରతͳ֯౓͸ɼ֤ਤͷԼʹ‫ه‬ΨʔεϕΫτϧ ࢀߟจ‫ݙ‬[1] H. Tsuchida, I. Kamata, T. Jikimoto, and K.
Izumi: J. Cryst. Growth 237-239, 1206 (2002).
[2] I. Kamata, M. Nagano, H. Tsuchida, Y. Chen,
and M. Dudley: J. Cryst. Growth 311, 1416
(2009).
[3] I. Kamata, M. Nagano, H. Tsuchida, Y. Chen,
and M. Dudley: Mater. Sci. Forum 600-603, 305(2009).

ࡌͯ͋͠ΔɽFig. 1 ͱ Fig. 2 Λর߹͢Δͱɼ‫( ߸ه‬a– 38 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

BL08B2

2012A3326

༗‫ػ‬൒ಋମࡐྉͷ̭ઢࢄཚߏ଄ղੳ

Structural Analysis of Organic Semiconductor Materials
by X-ray Scatteringླ໦ ୓໵ɼҏଜ ޺೭ɼখౡ ༏ࢠ ∗Takuya Suzuki, Hiroyuki Imura, Yuko, Kojima∗ࡾඛԽֶՊֶٕज़‫ڀݚ‬ηϯλʔ

Mitsubishi Chemical Group Science and Technology Research Center, Inc.

֓ཁɿɹ༗‫ػ‬ബບଠཅి஑ʹ͓͍ͯɼ‫׆‬ੑ૚Ͱ͋ΔόϧΫϔςϩδϟϯΫγϣϯʢBHJʣͷφϊߏ଄͕ిՙൃ
ੜɼిՙ༌ૹ౳ͷ෺ੑΛେ͖͘ࠨӈ͍ͯ͠Δͱߟ͑ΒΕΔɽຊ‫Ͱڀݚ‬͸ɼp ‫ܕ‬൒ಋମ͕ P3HTɼn ‫ܕ‬൒ಋମͰ͋ΔϑϥʔϨϯ༠ಋମ͕ C60PCBM Ͱ͋Δ BHJ ബບͷߏ଄ΛɼΞχʔϧԹ౓ґଘੑʹண໨͠ɼඍখ֯ೖࣼখ
̭֯ઢࢄཚ๏ʢGI-SAXSʣʹΑΓධՁͨ͠ɽ
Ωʔϫʔυɿɹ GI-SAXSɼόϧΫϔςϩδϟϯΫγϣϯɼ༗‫ػ‬ബບഎ‫ڀݚͱܠ‬໨త࣮‫ݧ‬ۙ೥ɼγϦίϯ‫ܥ‬ଠཅి஑ʹ୅ΘΔ࣍ੈ୅ଠཅి஑

ࢼྉͷ༗ྗީิͱͯ͠ɼ༗‫ػ‬൒ಋମΛ༻͍ͨ༗‫ػ‬ബບଠཅಋిੑߴ෼ࢠʀPoly(3-hexylthiophene)ʢP3HTʣɼ

ి஑ʢOPVʣ͕ܰྔੑ΍ॊೈੑͱ͍ͬͨಛੑ͔Β஫໨ϑϥʔϨϯ༠ಋମʀphenyl C61-butyric acid methyl

͞Ε͍ͯΔɽಛʹɼిՙυφʔͰ͋Δ π ‫ڞ‬໾ߴ෼ࢠͱ

ester (PCBM) (P3HT:PCBM = 1:0.85 wt%)ʣɽΞిՙΞΫηϓλʔͰ͋ΔϑϥʔϨϯ༠ಋମΛࠞ߹ͨ͠χʔϧԹ౓ʀΞχʔϧͳ͠ɼ120◦ Cɼ150◦ Cɼ180◦ Cɽߏ଄͔Β੒ΔόϧΫϔςϩδϟϯΫγϣϯʢBHJʣߏ૷ஔ଄‫ܕ‬ബບͷग़‫ʹݱ‬ΑΓɼOPV ͷൃిޮ཰͸ඈ༂తʹ޲্ͨ͠ [1, 2]ɽߴಛੑΛ࣮‫͢ݱ‬ΔͨΊʹ࠷దͳ BHJ

BL08B2 (SPring-8ɼฌ‫ͭͨݝݿ‬ͷࢢ)ଌఆ৚݅ߏ଄ʹ͓͍ͯ͸ɼಋిੑߴ෼ࢠͱϑϥʔϨϯ༠ಋମ͕ࣗ‫ݾ‬૊৫తʹ૬෼཭͠ɼ૬‫ʹޓ‬໢໨ߏ଄Λ‫ܗ‬੒͢Δ͜೾௕ʀ1.5 Åɼ Χϝϥ௕ʀ6.187 mɼ ‫ݕ‬ग़‫ث‬ʀIPɼೖࣹ֯ʀ0.20◦ ɽͱͰޮ཰తʹ༌ૹύεΛ࡞Δঢ়‫͕گ‬๬·͍͠ͱߟ͑

γϦίϯ‫ج‬൘্ʹεϐϯίʔτ๏ʹΑΓ࡞੒ͨ͠ΒΕ͍ͯΔɽ·ͨ૬෼཭αΠζ͸ྭ‫ࢠى‬ͷ֦ࢄ௕Ͱ͋

ް͞໿ 200nm ͷബບࢼྉʹ̭ઢΛ͢Ε͢Εೖࣹͤ͞ɼ

Δ 10nm ఔ౓͕๬·͍͠ͱ͞Ε͍ͯΔɽͦͷΑ͏ͳೋ࣍‫ݕݩ‬ग़‫ ث‬IP ʹΑΓ X ઢͷࢄཚ૾ΛಘͨɽͦͷφϊεέʔϧྖҬͷ BHJ ߏ଄ΛఆྔతʹධՁ͢Δͨ‫ޙ‬ɼࢄཚ૾ͷ in-plane ํ޲ͷࢄཚϓϩϑΝΠϧΛධՁΊͷख๏ͱͯ͠ɼ̭ઢΛϓϩʔϒͱͯ͠༻͍ͨখ̭֯

ͨ͠ɽઢࢄཚज़͕༗༻Ͱ͋Δɽຊ‫Ͱڀݚ‬͸ɼOPV ബບதͷ

BHJ ߏ଄ͷఆྔղੳΛ໨తͱ͠ɼࣼೖࣹখ̭֯ઢࢄ

݁Ռ͓Αͼߟ࡯

ཚ๏ʢGI-SAXSʣΛ༻͍ͯ OPV ബບதͷφϊߏ଄ͷΞχʔϧԹ౓ґଘੑΛධՁͨ͠ɽ

Fig. 1 ʹɼP3HT:PCBM ബບͷࢄཚϓϩϑΝΠϧ
ͷԹ౓ґଘੑΛࣔ͢ɽ྆ର਺ϓϩοτͰσʔλͷॎ࣠∗ ‫ࡏݱ‬ͷॴଐ: ࡾඛԽֶՊֶٕज़‫ڀݚ‬ηϯλʔ෼ੳ෺ੑηϯλʔ

Present Address: Mitsubishi Chemical Group Scienceand Technology Research Center, Inc., Materials Analysis Center͸γϑτࡁΈͰ͋Δɽq = 0.2∼0.3 nm−1 ෇ۙʹɼ໌ྎͳ‫؍͕ݞ‬ଌ͞Εͨɽ͜Ε͸ BHJ ߏ଄ʹ͓͍ͯɼϑϥʔϨϯ༠ಋମ͕‫ͯ͠ूڽ‬ಛ௃తͳαΠζΛ࣋ͬͨυ– 39 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)
Fig. 2 ʹɼP3HT:PCBM ബບͷࢄཚϓϩϑΝΠϧ
ͷϑΟοςΟϯά݁ՌΛࣔ͢ɽ‫ܗ‬ঢ়Ҽࢠʹ‫ٿ‬ঢ়Ϟσϧɼ‫ٿ‬൒‫ܘ‬ͷଟ෼ࢄ౓ʹ Schultz ෼෍ɼߏ଄ҼࢠʹϑϥΫλϧϞσϧΛԾఆ͢Δ͜ͱͰɼྑ޷ͳϑΟοςΟϯά݁ՌΛಘͨɽ͜ͷ࣌ͷϑϥʔϨϯ‫ूڽ‬ମͷ൒‫ܘ‬͸ɼ25◦ Cʹ͓͍ͯ໿ 8 nm Ͱ͋Γɼ180◦ ʹ͓͍ͯ͸໿ 10 nm
ʹ૿େ͢Δ͜ͱ͕ࣔ͞ΕͨɽϑϥΫλϧ࣍‫ݩ‬͸ɼ25◦ Cʹ͓͍ͯ໿ 2.7 Ͱ͋Γɼ180◦ ʹ͓͍ͯ͸໿ 2.9 ʹ૿େ͢Δ͜ͱ͕ࣔ͞Εͨɽ͜Ε͸ɼঢԹʹΑΓɼBHJ ߏ଄தʹ͓͍ͯ nm εέʔϧͰϑϥʔϨϯ෼ࢠ͕‫͠ूڽ‬ͯ૬෼཭αΠζ͕େ͖͘ͳΔͱ‫ʹڞ‬ɼΑΓେ͖ͳαΠζྖҬʹ͓͍ͯ΋૬෼཭ͷਐల͕ੜ͍ͯ͡Δ͜ͱΛ͍ࣔࠦͯ͠Δɽ
ࠓ‫ޙ‬ͷ՝୊
ࠓճɼBHJ ߏ଄தͷ૬෼཭αΠζͷΞχʔϧԹ౓ґ

Fig. 1. GI-SAXS profiles of P3HT:PCBM films.

ଘੑͷධՁʹ੒ޭͨ͠ɽࠓ‫ޙ‬͸ɼ૬෼཭ߏ଄ͱߴ෼ࢠ

ϝΠϯΛ‫ܗ‬੒͍ͯ͠Δ͜ͱΛ͍ࣔࠦͯ͠Δ [2]ɽ·ͨͷ݁থੑͷมԽͷ૬ؔΛɼGI-SAXS/WAXS ಉ࣌ଌఆhigh-q ଆʹ͓͍ͯ͸ɼ܏͖͕ −4.0 ͷ΂͖৐ଇ͕‫؍‬ଌΛ‫ݕ‬౼͢Δ͜ͱͰղ໌͍ͯ͘͜͠ͱ͕՝୊ͱߟ͑Δɽ͞Εͨɽ͜Ε͸ϑϥʔϨϯͷ‫ूڽ‬ମ͕γϟʔϓͳք໘Λ࣋ͬͯ૬෼཭͍ͯ͠Δ͜ͱΛ͍ࣔࠦͯ͠Δɽlow-qྖҬʹ͓͍ͯ͸ɼ΂͖৐ଇΛ༗͢Δ্ཱ͕ͪΓ͕‫؍‬ଌ͞Εͨɽ͜Ε͸‫ͨ͠ूڽ‬ϑϥʔϨϯ෼ࢠ͕ϑϥΫλϧ
తͳߴ࣍‫ߏूڽ‬଄Λ‫ܗ‬੒͍ͯ͠Δ͜ͱʹ༝དྷ͢Δͱߟࢀߟจ‫ݙ‬[1] M. Y. Chiu et al.: Adv. Mater. 20, 2573-2578(2008).
[2] J. M. Szarko et al.: Adv. Mater. 22, 5468-5472(2010).

͑ΒΕΔɽ

Fig. 2. Model fitting results of GI-SAXS profiles of P3HT:PCBM films.

– 40 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

2009B3329, 2010A3329, 2010B3329, 2011B3329

BL08B2

̭ઢ CT ʹΑΔϙϦϚʔϑΥʔϜͷηϧߏ଄‫࡯؍‬Cell Structure Observation of Polymer Foam
by X-ray Computed-Tomographyཱੴ ७Ұ࿠ɼ๺ࢁ ༟‫ڭ‬ɼࢁా Ղ༞
Junichiro TateishiɼHironori KitayamaɼKeisuke Yamada‫ࣜג‬ձࣾΞγοΫεɹεϙʔπ޻ֶ‫ॴڀݚ‬

Asics Corporation, Institute of Sport Science֓ཁɿɹѹॖม‫ܗ‬Լʹ͓͚ΔϙϦϚʔϑΥʔϜͷηϧߏ଄Λ̭ઢ CT ʹΑΓ‫ͨ͠࡯؍‬ɽCT ૾͔ΒɼѹॖෛՙʹΑΓηϧߏ଄Λ‫ܗ‬੒͢ΔϙϦϚʔน͸࠲۶ม‫͢ܗ‬Δ͜ͱ͕෼͔ͬͨɽ·ͨɼߴͻͣΈҬʹ͓͍ͯηϧߏ଄͸ফ໓͠ɼϙϦϚʔϑΥʔϜ͸த࣮Խͨ͠ɽ͜ΕΒ‫݁࡯؍‬Ռͱѹॖม‫ܗ‬Լʹ͓͚ΔϙϦϚʔϑΥʔϜͷԠྗ-ͻͣΈಛੑͱͷରԠΛ‫ݕ‬౼ͨ݁͠Ռɼѹॖม‫ظॳܗ‬ͷԠྗ૿େ͸ηϧนͷѹॖม‫࠲ͱܗ‬۶ม‫ʹܗ‬ɼߴͻͣΈҬͰͷ‫ͳܹٸ‬Ԡྗ૿େ͸‫ؾ‬๐ͷফࣦʹΑΔத࣮Խʹ‫ى‬Ҽ͢Δ͜ͱ͕໌Β͔ͱͳͬͨɽ
Ωʔϫʔυɿɹ̭ઢ CTɼϙϦϚʔϑΥʔϜɼηϧߏ଄ɼԠྗ-ͻͣΈಛੑഎ‫ڀݚͱܠ‬໨త࣮‫ݧ‬γϡʔζιʔϧʹ͸ɼਓମอ‫ޢ‬΍‫ٕڝ‬ύϑΥʔϚϯ‫ࡐࢼڙ‬͸ΤνϨϯਣࢎϏχϧίϙϦϚʔʢEVAʣͷε޲্ͷͨΊɼিܸ؇িੑΛ͸͡Ίͱͯ͠଱‫ٱ‬ੑɼܰՍ‫ڮ‬ϑΥʔϜͱͨ͠ɽ‫ࡐࢼڙ‬ͷີ౓͸ 0.20 g/cm3 Ͱྔੑ౳ͷଟ༷ͳੑೳ͕‫ٻ‬ΊΒΕΔ [1, 2]ɽ‫ݱ‬ঢ়ɼ͜Ε͋Γɼγϡʔζιʔϧʹ൚༻͞ΕΔϙϦϚʔϑΥʔϜΒཁ‫ٻ‬ੑೳΛಉ࣌ʹຬͨͨ͢Ίɼιʔϧͷߏ੒ࡐྉʹͱಉ༷ͳ΋ͷͰ͋Δɽ‫ࢼڙ‬ମ‫ܗ‬ঢ়͸ॎ 5 mm × ԣ 5͸Ս‫ͨ͠ڮ‬ϙϦϚʔ͔Β੒ΔϑΥʔϜ͕൚༻͞ΕΔɽ
͜ͷϑΥʔϜ͸ɼՍ‫ͨ͠ڮ‬ϙϦϚʔΛนͱ͠ɼ‫ؾ‬ମΛ

mm × ߴ͞ 10 mm ͷ֯பͱ͠ɼ͋Β͔͡Ίγʔτঢ়ʹൃ๐੒‫ͨ͠ܗ‬ϑΥʔϜ͔Β੾Γग़ͨ͠ɽ̭ઢ CT ૷ஔͷ֓ཁΛ Fig. 1 ʹࣔ͢ [3]ɽϩʔςʔ಺แͨ͠‫ؾ‬๐ʢηϧʣ͕ࡾ࣍‫ݩ‬తʹ࿈݁͢Δ͜ͱͰ‫ܗ‬γϣϯεςʔδ্ʹ‫ݻ‬ఆͨ͠ΞΫϦϧνϡʔϒ಺ʹ‫ڙ‬੒͞ΕͨࡐྉͰ͋ΔɽϙϦϚʔϑΥʔϜʹ͓͍ͯɼ‫ط‬ड़ͷੑೳΛઃ‫͢ܭ‬Δ

ࢼମΛ੩ஔ͠ɼϘϧτͷͶ͡ࠐΈʹΑͬͯѹॖͻͣΈͨΊʹ͸ɼѹॖෛՙԼʹ͓͚ΔྗֶಛੑΛ೺Ѳ͢Δ͜
ͱ͕ॏཁͱͳΔɽ·ͨɼ‫ݦ‬ඍ‫ʹڸ‬ΑΔϙϦϚʔϑΥʔϜද໘ͷೋ࣍‫͔࡯؍ݩ‬Βɼͦͷྗֶಛੑ͸ηϧߏ଄ʹӨ‫͞ڹ‬ΕΔ͜ͱ͕஌ΒΕ͍ͯΔɽ͔͠͠ͳ͕Β‫ʹີݫ‬͸ɼද໘Ͱ͸ͳ͘಺෦ʹ͓͚Δࡾ࣍‫ݩ‬తͳηϧߏ଄ͷධՁͱɼͦΕΛ‫ֶྗͨ͠ʹݩ‬ಛੑͷཧղ͓Αͼࡐྉઃ‫͕ܭ‬๬·ΕΔͱ͜ΖͰ͋Δɽͦ͜Ͱຊ‫Ͱڀݚ‬͸ɼϙϦϚʔϑΥʔϜͷྗֶಛੑΛ੍‫͏͠ޚ‬Δࡐྉઃ‫ࢦܭ‬ඪΛ‫ݟ‬ग़͢΂͘ɼѹॖม‫ܗ‬Լʹ͓͚ΔϙϦϚʔϑΥʔϜ಺෦ͷηϧߏ଄Λ̭ઢ CT ʹΑΓ‫͠࡯؍‬ɼηϧߏ଄͕ྗֶಛੑʹ‫͢΅ٴ‬Ө‫ૅجͯؔ͠ʹڹ‬తͳ஌‫ݟ‬ΛಘΔ͜ͱ

Fig. 1. X-ray CT system for cell structure obser-Λ໨తͱͨ͠ɽ

vation.

– 41 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

Fig. 2. CT image of polymer foam, (a) tomogram and (b) volume-rendering view.

Λ෇༩ͨ͠ɽ͜ͷͱ͖ɼ‫ࢼڙ‬ମʹͶ͡Ε͸ੜ͍ͯ͡ͳ

Fig. 3 ʹ͸ɼϙϦϚʔϑΥʔϜͷѹॖม‫ܗ‬Լʹ͓͍ɽಁա૾͸ɼP43 ‫ޫܬ‬ମΛ༻͍ϦϨʔϨϯζΛհ͠

͚ΔԠྗ-ͻͣΈ‫ۂ‬ઢͱ CT ૾ (a-f) ΛͦΕͧΕࣔ͢ɽ

ͯྫྷ٫ CCDʢ4008 pix × 2672 pixʣʹΑΓࡱ૾ͨ͠ɽ

CT ૾͸ѹॖํ޲ͱฏߦ໘ͷ΋ͷͰ͋Δɽ·ͨɼԠྗ-̭ઢͷΤωϧΪʔ͸ 12.4 kevɼ࿐ޫ࣌ؒ͸ 0.1 ඵɼͻͣΈ‫ۂ‬ઢதͷ໼ҹ͸ɼCT Λ࣮ࢪͨ͠ͻͣΈΛࣔ͠౤Өຕ਺͸ 1000 ຕ/180◦ ͱͨ͠ɽ‫ࢼڙ‬ମ-‫ޫܬ‬ମؒͷ͍ͯΔɽԠྗ-ͻͣΈ‫ۂ‬ઢʹΑΕ͹ɼϙϦϚʔϑΥʔ‫཭ڑ‬͸ 100 mm Ͱ͋Δɽ1 ճͷ CT ଌఆʹཁͨ࣌ؒ͠

Ϝ͸ྗֶಛੑʹେ͖ͳඇઢ‫ܗ‬ੑΛ༗͠ɼͻͣΈʹԠ͡

͸ 90 ෼ఔ౓Ͱ͋ͬͨɽಁա૾Λ Back Projection ๏ͯಛ௃తͳ 3 ͭͷྖҬΛ༗͢Δ͜ͱ͕෼͔Δɽͭ·ʹΑΓ࠶ߏ੒͢Δ͜ͱͰஅ૚૾Λಘͨɽѹॖม‫ܗ‬ԼʹΓɼඍখม‫ܗ‬Ҭʹ͓͍ͯॳ‫߶ظ‬ੑΛൃ‫͢ݱ‬Δ Stage 1ɼ͓͚ΔϙϦϚʔϑΥʔϜͷྗֶಛੑ͸ɼCT ͱ͸ผ్ɼҰ࣠ѹॖࢼ‫ʹݧ‬ΑΓධՁͨ͠ɽ‫ࢼڙ‬ମ‫ܗ‬ঢ়͸௚‫ ܘ‬10mmɼߴ͞ 10 mm ͷԁபͱ͠ɼΫϩεϔου଎౓ 6
mm/min. ʹͯѹॖͻͣΈΛ෇༩͠ɼαϯϓϦϯάλ
ΠϜ 50 ms Ͱՙॏ‫ͼٴ‬มҐΛ‫ܭ‬ଌͨ͠ɽͦͷ‫ޙ‬ɼͻͣΈͷ૿େʹΑͬͯ΋Ԡྗͷ૿େ͕খ͍͞

Stage 2ɼߴͻͣΈҬͰ͸‫ʹܹٸ‬Ԡྗ͕૿େ͢Δ Stage
3 ͕ଘࡏ͢ΔɽҰํ CT ૾ʹΑΕ͹ɼ = 0.0 ʹ͓͍ͯɼηϧ͸΄΅౳ํతͳ‫ܗ‬ঢ়Λ༗͍ͯ͠Δ΋ͷͷɼ = 0.1 ͱͳΔͱɼബ͍ηϧน͔Β༏ઌతʹ࠲۶͍ͯ͠Δ༷ࢠ͕֬݁Ռ͓Αͼߟ࡯

ೝͰ͖ΔɽԠྗ-ͻͣΈಛੑʹ͓͍ͯ͸ɼ͜ͷͻͣΈ

Fig. 2 ʹɼແͻͣΈঢ়ଶʹ͓͚ΔϙϦϚʔϑΥʔʢ = 0.1ʣ෇ۙʹ͓͍ͯ Stage 1 ͔Β Stage 2 ΁ҠߦϜͷஅ૚૾͓Αͼࡾ࣍‫૾ݩ‬ΛͦΕͧΕࣔ͢ɽ͍ͣΕͷ

͢Δɽ͞ΒʹͻͣΈ͕૿େ͢Δͱʢ = 0.1 ∼ 0.6ʣɼਤʹ͓͍ͯ΋ന৭෦͸ϙϦϚʔɼࠇ৭෦͸ۭܺΛද͠ηϧนͷ࠲۶‫ݱ‬৅͸ଟ͘ͷηϧʹ͓͍ͯੜͨ͡ɽ͜ͷ͓ͯΓɼ࣮‫૷ݧ‬ஔ͸ηϧߏ଄‫ेʹ࡯؍‬෼ͳۭؒ෼ղೳ

݁ՌʹΑΕ͹ɼStage 2 ͸ηϧนͷ࠲۶‫ݱ‬৅ʹ‫ى‬Ҽ͢Λ༗͍ͯ͠Δ͜ͱ͕෼͔ΔɽFig. 2(a) ʹΑΕ͹ɼຊ‫ݕ‬౼Ͱ༻͍ͨϙϦϚʔϑΥʔϜ͸ɼηϧͷ௚‫ ͕ܘ‬100µm ఔ౓ɼηϧนͷް͕͞ 10 µm ఔ౓Ͱ͋Δ͜ͱ͕෼͔ͬͨɽՃ͑ͯɼ‫͍ޓ‬ͷηϧ͸؏௨͢Δ͜ͱͳ͘ɼ͍
ΘΏΔΫϩʔζυηϧߏ଄Λ‫ܗ‬੒͍ͯ͠Δ͜ͱ͕֬ೝ
Ͱ͖ͨɽ·ͨ Fig. 2(b) ʹΑΕ͹ɼηϧ͸ 3 ࣍‫ݩ‬తʹ࿈͍݁ͯ͠Δ༷ࢠ΋֬ೝͰ͖Δɽ

Δ΋ͷͰ͋Δ͜ͱ͕ਪ࡯Ͱ͖Δɽ‫͢ݴ׵‬Ε͹ɼStage2 ʹ͓͍ͯ͸ɼ࠲۶ͨ͠ηϧน͕ԠྗΛ఻ୡ͠ͳ͍ͨ
ΊɼͻͣΈͷ૿େʹΑͬͯ΋Ԡྗͷ૿େ͕খ͘͞ͳΔ
΋ͷͱࢥΘΕΔɽ = 0.8 ʹୡ͢Δͱɼ্Լͷηϧน͕઀৮͠ɼ‫Ͱ͚͔ݟ‬͸ηϧߏ଄͕ফ໓͠ɼத࣮ମʢඇ
ൃ๐ঢ়ଶʣͱͳΔ͜ͱ͕෼͔ͬͨɽͭ·ΓɼStage 3– 42 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

Fig. 3. Stress-strain curve of specimen and CT images of inner layer in parall to compressive direction.
Arrows positions denote strain values corresponding to CT images.

ʹ‫ݟ‬ΒΕΔԠྗͷ‫૿ͳܹٸ‬େ͸ɼத࣮ମͷѹॖʹରԠ• ࠲۶ͨ͠ηϧน͸Ԡྗ఻ୡΛ͠ͳ͍ͨΊɼͻͣΈͷ૿େʹΑͬͯ΋Ԡྗͷ૿େ͕খ͍͞ Stage 2 ͕ൃ‫ݱ‬͢Δ΋ͷͰ͋Δͱߟ͑ΒΕΔɽ͢Δɽ

͜ΕΒͷ݁Ռ͔ΒɼϙϦϚʔϑΥʔϜͷྗֶಛੑ͸ηϧนͷ࠲۶‫ڍ‬ಈʹӨ‫͞ڹ‬ΕΔ͜ͱ͕࣮‫ݧ‬తʹࣔ͞ΕͨɽϙϦϚʔϑΥʔϜͷྗֶಛੑΛ੍‫͢ޚ‬Δ্Ͱ͸ɼ• ߴͻͣΈҬʹ‫ݟ‬ΒΕΔԠྗͷ‫૿ͳܹٸ‬େʢStage 3ʣ͸ɼηϧߏ଄͕ফࣦͨ͠த࣮ମͷѹॖ‫ڍ‬ಈʹରԠηϧนͷ࠲۶ಛੑ͕ॏཁͳઃ‫ܭ‬ύϥϝʔλͷҰͭͱͳ

͢ΔɽΔ΋ͷͱߟ͑ΒΕΔɽࠓ‫ޙ‬ɼ͞ΒͳΔৄࡉ‫ݕ‬౼ͷͨΊʹ͸ɼ࣮༻தͷԠྗɼࠓ‫ޙ‬ͷ՝୊

଎౓ʹଈͨ͠৚݅Ͱͷ CT ଌఆ΍ɼಘΒΕͨ݁ՌΛຊ‫ݕ‬౼Ͱ͸ɼϙϦϚʔϑΥʔϜͷྗֶಛੑΛ੍‫͢ޚ‬ΔࢦඪΛ‫ݟ‬ग़͢΂͘ɼѹॖม‫ʹܗ‬ΑΔࡐྉ಺෦ͷηϧߏ଄มԽΛ̭ઢ CT ʹΑΓ‫͠࡯؍‬ɼྗֶಛੑͱͷରԠΛ‫ݕ‬౼ͨ͠ɽͦͷ݁ՌɼҎԼͷ஌‫͕ݟ‬ಘΒΕͨɽ• ѹॖม‫ܗ‬Լʹ͓͚ΔϙϦϚʔϑΥʔϜͷྗֶಛੑ͸ඇઢ‫ܗ‬ੑΛ༗͠ɼͻͣΈʹԠͯ͡ 3 ͭͷಛ௃తͳྖ

ҬΛ༗͢Δɽ• ѹॖෛՙʹΑΓϙϦϚʔϑΥʔϜΛߏ੒͢Δηϧนʹ࠲۶͕ੜ͡Δɽ‫ͨ͠ʹج‬ίϯϐϡʔλγϛϡϨʔγϣϯͷ࣮ࢪ౳͕‫ڍ‬͛ΒΕΔɽ·ͨɼ࣮༻্ॏཁͳ໰୊ͱͳΔϙϦϚʔϑΥʔϜͷ଱‫ٱ‬ੑΛཧղ͢Δ্Ͱ͸ɼຊख๏ʹΑΔηϧߏ଄‫࡯؍‬͸༗༻ͳ஌‫ͳͱݟ‬ΔͰ͋Ζ͏ɽࢀߟจ‫ݙ‬[1] T.Nishiwaki: Sports Technology 1, 76-82 (2008).
[2] ஥୩੓߶: όΠΦϝΧχζϜֶձࢽ 33, 187-192(2009).
[3] H. Takano, Y. Urushihara, and J. Matsui:
SPring-8 Research Frontiers 2010, 140-141(2011).

– 43 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

BL08B2

2011B3330

φϊϑΟϥʔίϯϙδοτࡐͷߏ଄ͱ෺ཧಛੑͱͷ૬ؔղ໌

Elucidation of Correlation Between Structure andPhysical Properties of Nano-Compositeट౻ ༃޾ 1 ɼࡾ୐ ຑ୅ 1 ɼࠤ౻ ݈ଠ 1 ɼຓඌ ੓એ 1 ɼ‫܂‬ຊ ࣎ੜ 2
Yasuyuki Shudo1 , Mayo Miyake1 , Kenta Sato1 , Kazunobu Senoo1 , Shigeo Kuwamoto2
1

ॅ༑ϕʔΫϥΠτ‫ࣜג‬ձࣾ, 2 ެӹࡒஂ๏ਓͻΐ͏͝Պֶٕज़‫ڠ‬ձ
1

2

Sumitomo Bakelite Co., Ltd.,
Hyogo Science and Technology Association

֓ཁɿɹφϊγϦΧཻࢠΛߴॆరͨ͠ߏ଄ൃ৭ಁ໌ෳ߹‫ج‬൘ͷߏ଄ͱޫֶಛੑͷؔ܎Λղ໌͢ΔͨΊɼෳ߹‫ج‬൘ͷখ֯ X ઢࢄཚ (SAXS) ଌఆΛߦͬͨɽSAXS ϓϩϑΝΠϧʹ͓͚Δ‫ܗ‬ঢ়Ҽࢠͱߏ଄ҼࢠΛղੳͨ݁͠Ռɼ
φϊγϦΧཻࢠͷ෼ࢄঢ়ଶ͸ɼ‫ݕ‬౼ͨ͠ॆరྔ 0.1–55 vol% ʹ͓͍ͯɼཻࢠಉ͕࢜‫཭ڑ୹ͣͤूڽ‬டংੑΛ༗͠ɼ͜ͷ෼ࢄߏ଄͕ߏ଄ൃ৭ੑͷൃ‫دʹݱ‬༩͍ͯ͠Δ͜ͱ͕໌Β͔ͱͳͬͨɽ
Ωʔϫʔυɿɹখ֯ X ઢࢄཚɼߏ଄ൃ৭ɼφϊίϯϙδοτ

എ‫ڀݚͱܠ‬໨తຊ‫Ͱڀݚ‬͸ߴ෼ࢠՍ‫ڮ‬ωοτϫʔΫதʹφϊγϦΧ

ΘΕΘΕ͸ߴ෼ࢠՍ‫ڮ‬ωοτϫʔΫதʹφϊγϦΧ
ཻࢠΛॆరͤ͞Δ͜ͱʹΑͬͯɼߴ଱೤ੑ͓Αͼ௿ઢ๲ு཰Λ༗͢Δಁ໌ϓϥενοΫෳ߹‫ج‬൘ͷ։ൃʹ੒ޭͨ͠ [1, 2]ɽ͜ͷಁ໌ෳ߹‫ج‬൘ͷޫֶಛੑ͸ɼφϊγϦΧཻࢠͷ෼ࢄঢ়ଶʹΑ੍ͬͯ‫ޚ‬ՄೳͰ͋Γɼෳ߹ཻࢠΛ෼ࢄͤͨ͞ෳ߹ϑΟϧϜʹ͓͚Δཻࢠ෼ࢄঢ়ଶ
ͱߏ଄ൃ৭ੑͷ૬ؔΛղ໌͢ΔͨΊɼSAXS ʹΑΔߏ଄ղੳΛߦͬͨɽ࣮‫ݧ‬‫ج‬൘ͷ͞ΒͳΔߴੑೳԽʹ͸ɼ෼ࢄঢ়ଶͷղ໌͕ॏཁ

ೋ‫׭‬ೳΞΫϦϨʔτϞϊϚʔɼϝνϧΤνϧέτϯ

Ͱ͋Δɽφϊཻࢠͷ෼ࢄঢ়ଶͷղੳ͸ SPring-8 ʹ͓෼ࢄίϩΠμϧγϦΧʢฏ‫ܘࢠཻۉ‬໿ 200 nmʣɼ͓͚Δߴً౓์ࣹޫΛ༻͍ͨখ֯ X ઢࢄཚ (SAXS) ͕Αͼޫॏ߹։࢝ࡎ͔ΒͳΔϫχεΛௐ੔͠ɼ༹ഔΛ‫ݮ‬ͱ͘ʹ༗ޮͰ͋Γɼφϊཻࢠؒͷ‫ׯ‬বޮՌʹ‫ى‬Ҽ͢ΔѹԼʹͯআ‫ͨ͠ڈ‬ɽγʔτঢ়ʹ੒‫ࢼͨ͠ܗ‬ྉʹɼࢵ֎ߏ଄Ҽࢠ͕ SAXS ϓϩϑΝΠϧ͔ΒಘΒΕΔɽ

ޫরࣹʢੵࢉޫྔ໿ 700 mJ/cm ʣ͠Ս‫ڮ‬൓ԠΛਐߦ

2ΘΕΘΕͷ։ൃͨ͠ಁ໌ෳ߹‫ج‬൘Ͱ͸φϊγϦΧཻࢠ͕ٖࣅతͳ݁থߏ଄Λ‫ܗ‬੒͠ɼ‫͢ूڽʹ͍ޓ‬Δ͜ͱ

ͤͨ͞‫ޙ‬ɼ230 ◦ C Ͱ 3 ࣌ؒͷ೤ॲཧΛ͢Δ͜ͱʹΑΓບް໿ 200 µm ͷෳ߹ϑΟϧϜΛಘͨɽͳ͘ϥϯμϜ෼ࢄ͍ͯ͠Δ͜ͱΛࣔࠦ͢Δ݁Ռ͕͜Ε্‫ه‬ͷΑ͏ʹಘΒΕͨϑΟϧϜͷ೾௕ґଘੑͷશޫ·Ͱͷ SAXS ଌఆʹΑͬͯಘΒΕ͍ͯΔɽ͞Βʹɼಛઢಁա཰͓Αͼ൓ࣹ཰͸ɼࢵ֎Մࢹ੺֎෼ޫޫ౓‫ܭ‬ఆͷཻࢠ‫͓ܘ‬Αͼཻࢠॆరྔʹ͓͍ͯɼ৭ૉ౳Λ‫ؚ‬༗ʢ೔ຊ෼ޫࣾ੡ V-670ʣΛ༻͍ͯଌఆͨ͠ɽ

͍ͯ͠ͳ͍ʹ΋ؔΘΒͣՄࢹޫͷಛఆ೾௕ͷΈΛ൓ࣹՄೳͳൃ৭ੑಁ໌ϑΟϧϜ͕ಘΒΕͨɽ͜ͷൃ৭‫ݱ‬৅͸ߏ଄ൃ৭ͱͯ͠஌ΒΕΔ΋ͷͰ͋ΓɼҰൠʹ͸ɼφϊཻࢠͷίϩΠυ݁থͷ‫ن‬ଇ഑ྻʹΑΔޫͷճં൓ࣹͳͲ͕஌ΒΕ͍ͯΔ [3]ɽ͔͠͠ͳ͕Βɼφϊཻࢠͷ഑ྻ‫ܗ‬੒΍ߏ଄ൃ৭ੑൃ‫ݱ‬ͷϝΧχζϜʹ͍ͭͯ͸ະ

SAXS ଌఆ͸ฌ‫ݝݿ‬ϏʔϜϥΠϯ BL08B2 ͷୈ 2 ϋονʹ࣮ͯࢪͨ͠ɽ‫ݕ‬ग़‫ʹث‬͸ 2 ࣍‫ݕݩ‬ग़‫ ث‬PILATUS
Λ༻͍ɼΧϝϥ௕͓Αͼ೾௕͸ 6.2 m, 1.5 Å ͱ 1.6 m,

1.0 Å ͷ 2 ৚݅Ͱߦͬͨɽ̭ઢͷ࿐ޫ࣌ؒ͸αϯϓϧ
ͷࢄཚ‫ʹ౓ڧ‬Αͬͯ 2–60 ඵͷൣғͰมԽ͓ͤͯ͜͞
ͳ͍ɼͦΕͧΕͷࢄཚϓϩϑΝΠϧΛ‫ͨ͛ܨ‬ɽͩʹղ໌͞Ε͍ͯͳ͍఺΋ଟ͍ɽ– 44 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू
݁Ռ͓Αͼߟ࡯

࣍ʹɼφϊγϦΧཻࢠΛ 10 vol% Ҏ্ॆరͨ͠ෳ

·ͣɼ༻͍ͨφϊγϦΧཻࢠͷฏ‫͓ܘࢠཻۉ‬Αͼͦͷཻ౓෼෍Λௐ΂ΔͨΊɼφϊγϦΧॆరྔ 0.1 vol%ʢମੵ෼཰ η = 0.001ʣͷϑΟϧϜͷ SAXS ϓϩϑΝΠϧΛҰ࣍‫ݩ‬Խ͠ɼཻࢠؒ‫ׯ‬বޮՌ͕ແ͍΋ͷͱԾఆ߹ϑΟϧϜͷ SAXS ϓϩϑΝΠϧͷղੳΛߦͬͨɽෳ
߹ϑΟϧϜʹ͓͍ͯɼφϊγϦΧཻࢠͷిࢠີ౓͕૬
ରతʹඇৗʹߴ͍ͨΊɼφϊγϦΧཻࢠʹ‫ى‬Ҽ͢ΔࢄཚҎ֎͸ແࢹͰ͖ΔͱԾఆ͢Δͱɼࢄཚؔ਺ I(q) ͸࣍ࣜͷΑ͏ʹ‫ه‬ड़͢Δ͜ͱ͕Ͱ͖Δ [4]ɽͯ࣍͠ʹࣔؔ͢਺ͰϑΟοςΟϯάΛߦͬͨɽ ∞P (q) =
p(R)|F (q, R)|2 dR

I(q) = KP (q)S(q)0͜͜Ͱ, p(R) ͸࣍ࣜͰࣔ͢ Gauss ෼෍ؔ਺Ͱ͋ΓɼR0

͜͜Ͱ K ͸ཻࢠ਺͓Αͼཻࢠମੵʹؔ͢Δఆ਺ɼP (q)͸ཻࢠͷฏ‫ۉ‬൒‫ܘ‬ɼσ ͸ཻࢠ൒‫ܘ‬ͷඪ४ภࠩͰ͋Δɽ
 
2 
1
R − R0√exp −p(R) = √2πσ2σ͸ཻࢠ‫ܗ‬ঢ়ҼࢠɼS(q) ͸ཻࢠؒ૬ؔΛද͢ߏ଄Ҽࢠ2·ͨɼ|F (q, R)| ͸൒‫ ܘ‬R ͷ߶ମ‫ٿ‬ͷ‫ܗ‬ঢ়ҼࢠͰ͋Γɼ࣍ࣜͰࣔ͞ΕΔɽ

F (q, R) = 3

sin(qR) − qR cos(qR)
(qR)3

Ͱ͋Δɽ

Fig. 2 ʹɼγϦΧཻࢠΛ 10–55 vol%༗͢Δෳ߹ϑΟϧϜͷ SAXS ϓϩϑΝΠϧΛࣔ͢ɽη ͸ମੵ෼཰Λࣔ
͢ɽq > 0.04 nm−1 Ͱ͸͍ͣΕͷॆరྔʹ͓͍ͯ΋γϦΧཻࢠͷ‫ܗ‬ঢ়Ҽࢠ P (q) ʹ‫ى‬Ҽͨ͠ಛ௃తͳࢄཚ

ϓϩϑΝΠϧ͕֬ೝ͞Εͨ͜ͱ͔ΒɼφϊγϦΧཻࢠΛߴॆరྔͨ͠ෳ߹ϑΟϧϜφϊγϦΧཻࢠʹ༝དྷ͢

Fig. 1 ʹφϊγϦΧཻࢠΛ 0.1 vol%‫ؚ‬༗͢Δෳ߹

Δ SAXS Λ‫؍‬ଌ͢Δ͜ͱ͕Ͱ͖͍ͯΔ͜ͱ͕֬ೝ͞

ϑΟϧϜͷ SAXS ϓϩϑΝΠϧ͓Αͼલड़ͷࣜʹΑΕͨɽҰํɼq < 0.04 nm−1 ͷྖҬʹ͓͍ͯ͸‫ۃ‬େΔϑΟοςΟϯάΧʔϒΛࣔ͢ɽq = 0.04–0.20 nm−1஋͕‫ݱ‬ΕɼͦͷϐʔΫҐஔ͸ཻࢠͷॆరྔ͕૿͢ʹͭͷൣғͰɼ࠷খೋ৐๏Λ༻͍ͯϑΟοςΟϯάΛߦͬΕͯ޿֯ଆ΁γϑτ͍ͯ͠Δ͜ͱ͕֬ೝͰ͖Δɽ͜Εͨ݁Ռɼཻࢠ‫ܘ‬ͷฏ‫ۉ‬஋͸ 2R0 ͸ 197 nmɼCV ஋

͸ P (q) Ͱ͸ද͢͜ͱ͕Ͱ͖ͳ͍ͨΊɼφϊγϦΧͷ

(2σ/2R0 × 100) ͸ 5.2 %ͱ΄΅୯෼ࢄͷཻ౓෼෍Ͱ

ཻࢠؒ૬ؔʹ༝དྷ͢Δ΋ͷͱਪఆ͞ΕɼφϊγϦΧͷ

͋Δ͜ͱ͕Θ͔ͬͨɽq < 0.03 nm−1 Ͱ͸ཧ࿦ؔ਺ͱ

ཻࢠ഑ྻ͕ॆరྔʹΑͬͯมԽ͍ͯ͠Δ͜ͱ͕ࣔࠦ͞

ͷဃ཭͕‫ݟ‬ΒΕΔ͕ɼ͜Ε͸ 0.1 vol%ͷ‫ك‬ബঢ়ଶʹ͓ΕΔɽ͍ͯ΋ཻࢠؒͷ‫ׯ‬বޮՌ͕࢒ଘ͍ͯ͠ΔͨΊͰ͋Δͱ
12ߟ͑ΒΕΔɽ

10

8

10

10

η=0.001
KP(q)8

I(q) / a.u.

7

10

6

I(q) / a.u.

10

5

10

4

10

3

10

6

10

4

10

2

10

10

2

10

0

10

1

10

–2

10

0

10

η=0.55
η=0.50η=0.40η=0.33
η=0.20η=0.10

10

–2

10

2

3

4

5 6 7 89

2

–1

10

−1

3

4

5 6 7 892

3

4

5 6 7 89

2

–1

10

3

4

5 6 7 89

−1

0

10

q / nm0

10

q / nmFig. 2. SAXS profiles of composite film containing
volume fractions (η) of nanosilica particles.

Fig. 1. SAXS profile of composite film that contains
0.1 volume percent (η = 0.001) nanosilica particlesཻࢠ഑ྻঢ়ଶΛΑΓৄࡉʹղੳ͢ΔͨΊɼ֤ࢄཚϓand its fitting curve assuming a Gaussian sphere.

ϩϑΝΠϧʹର͠ߏ଄Ҽࢠ S(q) ͷநग़Λߦͬͨɽຊ

– 45 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)‫ݕ‬౼Ͱ͸ɼ0.1 vol%ͷ‫ك‬ബঢ়ଶͰ͸ཻࢠؒ૬͕ؔແࢹ

ཻࢠ഑ஔʹ୹‫཭ڑ‬டংੑΛ༗͢ΔφϊγϦΧ෼ࢄߏ଄

Ͱ͖ΔͱΈͳ͠ɼφϊγϦΧཻࢠͷ‫ܗ‬ঢ়Ҽࢠ P (q) ͱ͕ߏ଄ൃ৭ੑͷൃ‫دʹݱ‬༩͍ͯ͠Δ͜ͱ͕Θ͔ͬͨɽͨ͠ɽ֤ࢄཚؔ਺ I(q) Λ 0.1 vol%ͷࢄཚؔ਺ͰׂΓɼq ͕े෼େ͖ͳԕํʹ͓͍ͯ S(q) ͕ 1 ʹऩଋ͢ΔΑ͏ʹ‫֨ن‬ԽΛߦͳ͏͜ͱʹΑͬͯߏ଄Ҽࢠ S(q) Λ‫ٻ‬ΊͨɽFig. 3 ʹ֤ॆరྔʹ͓͚Δߏ଄ҼࢠΛࣔ͢ɽq =0.02–0.04 nm−1 ʹ‫͍ڧ‬ϐʔΫ͕ଘࡏ͠ɼཻࢠॆరྔ
ͷ૿େͱͱ΋ʹ޿֯ଆ΁γϑτ͢Δ༷ࢠ͕֬ೝ͞Εͨɽ͜ͷ‫͍ڧ‬ϐʔΫཻ͕ࢠؒ૬ؔͷୈҰϐʔΫͰ͋Δͱਪ࡯͞Εɼཻࢠॆరྔͷ૿େͱͱ΋ʹཻࢠؒ‫ڑ‬཭͕খ͘͞ͳ͍ͬͯΔ͜ͱ͕ࣔࠦ͞ΕΔɽ͜ͷ܏޲͸

Percus–Yevick Ϟσϧ [5] Ͱද͞ΕΔϥϯμϜ෼ࢄ‫ܥ‬ͱ͸ҟͳΔ΋ͷͰ͋Γɼॆరྔ͕ߴ͘ͳͬͯ΋ཻࢠಉ͕࢜‫͢ूڽ‬Δ͜ͱͳ͋͘Δ‫཭ڑ‬Λอͬͨ··෼ࢄͨ͠ɼ
டংੑͷ͋Δߏ଄Λ‫ܗ‬੒͍ͯ͠Δ΋ͷͱਪ࡯͞ΕΔɽ

33 volume percent nanosilica particles.

4.0
η=0.55
η=0.50η=0.40η=0.33
η=0.20η=0.10

3.5
3.0

700

2.0
1.5
1.0
0.5
0.02

0.04

0.06

0.08

Λpeak (SAXS)
λpeak (Reflectance)

600

Λpeak, λpeak / nm

S(q)

2.5

0.0
0.00

Fig. 4. FE-SEM image of composite film containing

500
400
300
200
100

0.10

0

−1

q / nm

0

20

30

40

50

60

Silica content / vol%Fig. 3. Structrure factors of composite film containing various volume fractions nanosilica particles.

10

Fig. 5. Changes in Λpeak and λpeak that were ob-

Fig. 4 ʹॆరྔ 33 vol%ʢମੵ෼཰ η = 0.33ʣͷ

tained from S(q) and reflectance spectra in the visible light range, respectively.

ϑΟϧϜͷද໘Λ FE-SEM Ͱ‫݁ͨ͠࡯؍‬ՌΛࣔ͢ɽ͜ͷ‫ݟʹ૾࡯؍ॴہ‬ΒΕΔΑ͏ʹɼ͍ͣΕͷॆరྔͰ΋γϦΧ͕࠷ۙ઀ཻࢠؒͰҰఆͷ‫཭ڑ‬Λҡ࣋ͨ͠୹‫཭ڑ‬ࠓ‫ޙ‬ͷ՝୊

டংੑΛ༗͢Δ෼ࢄঢ়ଶΛ‫ܗ‬੒͍ͯ͠Δͱߟ͑ΒΕΔɽ

Fig. 5 ʹɼߏ଄ҼࢠͷୈҰϐʔΫ qpeak ʹ૬౰͢Δ
࣮ۭؒαΠζ Λpeak = 2π/qpeak ɼ͓Αͼࢵ֎Մࢹ੺֎
෼ޫޫ౓‫Ͱܭ‬ଌఆ֤ͨ͠αϯϓϧͷՄࢹޫྖҬͷ൓ࣹεϖΫτϧʹ͓͚Δ൓ࣹϐʔΫ೾௕ λpeak ͷॆరྔʹ
ΑΔมԽΛࣔ͢ɽॆరྔ͕૿Ճ͢ΔʹͭΕɼΛpeak ͓Αͼ λpeak ͕͍ͣΕ΋‫ݮ‬গ͢Δ܏޲Λࣔ͢͜ͱ͔ΒɼφϊγϦΧཻࢠΛՍ‫ڮ‬ϙϦϚʔωοτϫʔΫதʹౚ݁ͤ͞Δ͜ͱʹΑΓߏ଄ൃ৭ಁ໌‫ج‬൘Λ࡞੒͠ɼͦͷߏ଄ͱޫֶಛੑͷؔ܎Λղ໌͢ΔͨΊখ̭֯ઢࢄཚଌ
ఆʹΑΔߏ଄ղੳΛߦͬͨɽ‫ܗ‬ঢ়Ҽࢠͱߏ଄ҼࢠΛ෼཭͠ߏ଄ҼࢠΛղੳͨ݁͠ՌɼγϦΧ͸ߴॆరঢ়ଶʹ͓͍ͯ΋‫͢ूڽ‬Δ͜ͱͳ͘෼ࢄঢ়ଶΛอ͍ͬͯΔ͜ͱ

– 46 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू
͕Θ͔ΓɼγϦΧཻࢠؒͷ୹‫཭ڑ‬டংੑ͕ߏ଄ൃ৭ੑ

ࢀߟจ‫ݙ‬

ͷൃ‫دʹݱ‬༩͍ͯ͠ΔͱࢥΘΕΔ݁ՌΛಘͨɽ

[1] K. Senoo, T. Takeuchi, W. Oka, Y. Shimobe,
S. Kuwamoto, Y. Urushihara, J. Matsui, and
K. Nakamae: J. Network Polym., Jpn., 30, 16(2009).
[2] K. Senoo, T. Takeuchi, W. Oka, Y. Shimobe,
S. Kuwamoto, Y. Urushihara, J. Matsui, and
K. Nakamae: J. Network Polym., Jpn., 31, 19(2010).
[3] S. Kinoshita, S. Yoshioka, and J. Miyazaki: Rep.
Prog. Phys., 71, 076401 (2008).
[4] H. Matsuoka, T. Harada, K. Kago, and H.
Yamaoka: Langmuir, 12, 5588 (1996).
[5] J. K. Percus and G. J. Yevick: Phys. Rev., 110,
1 (1958).
[6] H. Matsuoka, H. Tanaka, T. Hashimoto, and N.
Ise: Phys. Rev. B, 36, 1754 (1987).

ࠓ‫ޙ‬͸ߏ଄டংੑΛߋʹৄࡉʹղੳ͢ΔͨΊɼࠓճߦͬͨߏ଄ҼࢠͷղੳʹՃ͑ɼࡾ࣍‫ݩ‬ύϥΫϦελ
ϧཧ࿦ [6] Λ༻͍ͨࢄཚؔ਺ͷղੳ΍‫ࢉܭ‬γϛϡϨʔγϣϯʹΑΔߏ଄ධՁʹΑͬͯɼߏ଄டংੑΛΑΓఆྔతʹղੳ͢Δ༧ఆͰ͋Δɽ
·ͨɼࠓճ͸ະ‫ݕ‬౼Ͱ͋Δෳ߹ϑΟϧϜͷಁ໌ੑʹ͍ͭͯ͸ɼՄࢹޫͷ೾௕Φʔμʔͷߏ଄ʹ૬͕ؔ͋Δ
΋ͷͱਪ࡯͞ΕΔ͜ͱ͔Βɼࠓ‫ޙ‬͸ߋͳΔ௒খ֯ྖҬͷߏ଄‫࡯؍‬Λ࣮ࢪ͠ɼφϊγϦΧ͕‫ܗ‬੒͢Δ֊૚ߏ଄΍‫ࢹڊ‬తͳෆ‫ۉ‬Ұੑͱޫֶಛੑͱͷ૬ؔΛ໌Β͔ʹ͍ͨ͠ɽ

– 47 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

2011A3352, 2011B3352, 2012A3256, 2012A3352

BL08B2, BL24XU์ࣹޫΛར༻ͨ͠ΰϜࡐྉதͷ֊૚ߏ଄௥੻

Analysis of Hierarchical Structure of Rubber
Using Ultra Small Angle X-ray Scatteringେߐ ༟জɼখౡ ਖ਼ষɼ্ྛ ޺ɼᐩຊ ༤‫و‬ɼञҪ ल೭
Hiroaki Oe, Masaaki Kojima, Hiroshi Uebayashi, Yuuki Masumoto, Hideyuki Sakai౦༸ΰϜ޻‫ࣜגۀ‬ձࣾ

TOYO TIRE & RUBBER CO., LTD.

֓ཁɿɹ์ࣹޫ X ઢখ֯ࢄཚ๏Λ༻͍ɼΰϜࡐྉதͷิ‫ࡎڧ‬഑ஔߏ଄Λ੩తɾಈత৚݅ԼͰධՁͨ͠ɽิ‫ࡎڧ‬ͷ෼ࢄɾ‫ूڽ‬Λ޿͘֊૚ผʹߏ଄‫͢࡯؍‬Δ͜ͱͰɼ۩ମతͳ૬ରධՁ͕ՄೳͱͳΓɼ෺ੑͱͷ૬ؔੑ΋֬ೝͰ
͖ͨɽ·ͨɼΰϜࡐྉධՁ࣌ʹࢄ‫͞ݟ‬ΕΔ഑޲ੑʹண໨͠‫ݕ‬౼ͨ݁͠Ռɼิ‫ࡎڧ‬༝དྷͷ഑޲ߏ଄‫ܗ‬੒͕ࣔࠦ͞
ΕɼΰϜͷ഑޲ํ޲Λબผ͢Δ͜ͱͰ‫ػ‬ցಛੑ੍͕‫͖Ͱޚ‬Δ͜ͱΛ‫ݟ‬ग़ͨ͠ɽΩʔϫʔυɿɹΰϜɼখ֯ࢄཚɼϑΟϥʔɼ‫ूڽ‬ɼ෼ࢄɼ֊૚ߏ଄ɼ഑޲

എ‫ڀݚͱܠ‬໨త

BL08B2 ʹ͓͚Δࢼ‫ݧ‬৚݅͸ɼ̭ઢͷ೾௕Λ 1.5 ÅɼΰϜࡐྉ͸ɼ֤छΰϜ੡඼ʹ‫ٻ‬ΊΒΕΔੑೳΛຬ଍Χϝϥ௕Λ 15930 mmɼ6094 mm ͷ 2 ਫ४ͱ͠ɼσΟͤ͞ΔͨΊʹଟ਺ͷҟͳΔఴՃࡎΛࠞ߹͢Δ͕Ώ͑ɼςΫλʔʹ͸ PILATUS Λ࢖༻ͨ͠ɽ·ͨαϯϓϧ΁

छʑͷ૬͔Β‫ܗ‬੒͞ΕΔߏ଄Λ࣋ͬͨෳࡶࡐྉͰ͋Δɽ

ͷ̭ઢরࣹ࣌ؒ͸ 15 sec ͱ͠ɼಘΒΕͨ 2 ࣍‫ࢄݩ‬ཚ૾ͦͷ͞·͟·ͳ‫ڍ‬ಈ΍‫ݱ‬৅͸ɼۙ೥ͷ෼ੳɾղੳٕज़

͔Β෯ 40◦ ͷൣғͰԁ‫؀‬ฏ‫ ͠ۉ‬1 ࣍‫ݩ‬σʔλʹม‫׵‬ɼͷਐาʹ΋͔͔ΘΒͣɼࡐྉ͕ෆ‫ۉ‬Ұ͔ͭ 3 ࣍‫ݩ‬ͷ֊ࢄཚ‫ۂ‬ઢΛಘͨɽຊ৚݅Ͱͷ q Ϩϯδ͸ɼ0.005∼0.5૚ߏ଄Λ༗͍ͯ͠ΔͨΊɼ͍·ͩϒϥοΫϘοΫεత

nm−1 Ͱ͋ͬͨɽ

ͳཁૉ͕ଟ͍ɽҰํͰΰϜ੡඼ͷ‫ڥ؀‬ɾ҆શʹର͢Δ

ΑΓখ֯ଆͷσʔλΛಘΔͨΊʹɼBonse-Hart ‫ܕ‬χʔζ͸ߴ·ΓɼࡐྉͷߴੑೳԽɾߴ‫ػ‬ೳԽʹ޲͚ͨͷޫֶ‫ܥ‬Λ༗͢Δ BL24XU ʹͯࢼ‫ݧ‬Λ࣮ࢪͨ͠ɽ̭ઢ

։ൃ͕‫ٸ‬຿Ͱ͋Δ͜ͱ͔ΒɼΑΓਫ਼ີͳ෼ੳɾղੳٕ

ΤωϧΪʔ͸ 10 keVɼσΟςΫλʔʹ͸ YAP γϯνज़͕ඞཁෆՄܽͰ͋ΔɽϨʔγϣϯΧ΢ϯλʔΛ࢖༻͠ɼଌఆதΞςωʔλΛͦ͜Ͱɼ์ࣹޫ̭ઢখ֯ࢄཚ๏Λར༻͢Δ͜ͱʹΑར༻͠ͳ͕Β֯౓ૢ࡞εςοϓΛൣғຖʹՄม͠σʔΓɼΰϜࡐྉதͷφϊ ∼ ϛΫϩεέʔϧʹΘͨΔ֊

λΛ࠾औͨ͠ɽαϯϓϧ΁ͷ̭ઢরࣹ࣌ؒ͸ 20 min૚ߏ଄ɼಛʹΰϜ෺ੑΛେ͖ܾ͘ఆ͢ΔҼࢠͷҰͭͰͰɼಘΒΕͨࢄཚσʔλͷ q Ϩϯδ͸ɼ0.0009∼0.13

͋Δิ‫ࡎڧ‬ʢΧʔϘϯϒϥοΫ΍γϦΧ౳ʣͷ෼ࢄɾ

nm−1 Ͱ͋ͬͨɽ

‫ڍूڽ‬ಈΛछʑͷ৚݅ͷԼͰଌఆɾղੳ͠ɼ௚઀‫࡯؍‬·ͨɼϦΨΫࣾ੡̭ઢখ֯ࢄཚ૷ஔ MicroMax-007ͳͲͷղੳσʔλɼ͓Αͼ‫ػ‬ցಛੑͱฒߦͯ͠ߟ࡯͢

ʹͯߴ q ϨϯδͷධՁΛ࣮ࢪͨ͠ɽ̭ઢ೾௕͸ 1.54 Åɼ

Δ͜ͱͰ৽ͨͳ஌‫ݟ‬Λ‫ݟ‬ग़͠ɼߴੑೳࡐྉ։ൃ΁ͱͭΧϝϥ௕ 1138 mm ͱ͠ɼ͜ͷࡍಘΒΕͨ q Ϩϯδ͸ͳ͍͛ͨɽ

0.04∼5.43 nm−1 Ͱ͋ͬͨɽαϯϓϧ͸ɼόϯόϦʔϛΩαʔʹΑͬͯΰϜͱ഑߹ࡎΛࠞ࿅͠ɼۚ‫ܕ‬Ϟʔϧ࣮‫ݧ‬υͰϓϨεՃ޻͢Δ͜ͱͰɼް͞ 1.0 mm ͷΰϜγʔΰϜࡐྉதͷ֊૚ߏ଄ΛΑΓ޿͍ൣғͰධՁ͢Δτʹ੒‫ͨ͠ܕ‬ɽ·ͨɼαϯϓϧͷ֎෦ܹࢗʹΑΔߏ଄ͨΊɼҟͳΔϨϯδσʔλΛ࠾औͰ͖ΔΑ͏࣍ʹࣔ͢มԽΛධՁ͢ΔͨΊɼαϯϓϧ৳௕࣌ͷখ֯ࢄཚ࣮‫ݧ‬छʑͷ৚݅ͷԼɼ̭ઢখ֯ࢄཚ࣮‫ݧ‬Λ࣮ࢪͨ͠ɽ

Λ࣮ࢪͨ͠ɽҾுࢼ‫ݧ‬͸ɼมҐΛ೚ҙͰઃఆͰ͖ΔҾ

– 48 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռूு૷ஔʹαϯϓϧΛηοτ͠ɼ྆୺ʹมҐΛ͔͚Δ͜
ͱͰ์ࣹޫরࣹҐஔ͕มҐʹΑΒͣαϯϓϧͷதԝͱͳΔΑ͏ʹͨ͠ɽ
݁Ռ͓Αͼߟ࡯

Fig. 1 ͸ɼενϨϯϒλδΤϯΰϜ (SBR)/γϦΧ഑߹‫͚͓ʹܥ‬ΔΰϜࡐྉͷࢄཚϓϩϑΝΠϧΛࣔͨ͠΋ͷͰ͋Δɽ࠾औͨ͠σʔλΛॏͶ߹Θͤɼ0.001 <q < 5 ͷ޿͍ൣғͰߏ଄ղੳΛ࣮ࢪͨ͠ɽγϦΧ෼ࢄʹΑΔࡐྉߏ଄ͱ෺ੑͷؔ܎ΛධՁ͢ΔͨΊɼਤதSample2 ʹγϦΧ෼ࢄॲཧΛࢪ͠ɼSample1 ͸ະॲཧͱͨ͠ɽղੳʹ͸ɼUnified function [1, 2] Λར༻͠ɼγϦΧཻࢠ ∼ ‫ूڽ‬ମ ∼ γϦΧωοτϫʔΫͷߏ଄৘

Fig. 1. Combined SAXS profiles for SBR/Silica.

ใΛ֊૚ຖʹධՁͨ͠ɽ݁ՌɼγϦΧҰཻ࣍ࢠ‫ىʹܘ‬Ҽͨ͠ϐʔΫʢq = 0.5 ෇ۙʣ͸ɼSample1, 2 Ͱࠩ͸‫ݟ‬ड͚ΒΕͣɼγϦΧ෼ࢄॲཧͷ༗ແʹӨ‫ڹ‬Λड͚ͳ͍͜ͱ͕֬ೝͰ͖ͨɽq < 0.1 Ͱ͸ɼγϦΧͷ‫ूڽ‬ମ༝དྷͷϐʔΫ͕‫؍‬ଌ͞ΕɼSample2 ͷํ͕γϦΧͷ෼ࢄޮՌʹΑΓ‫ूڽ‬ମαΠζ͕ࡉ͔͘ͳΔ܏޲ʹ͋ͬͨɽ͞ΒʹɼγϦΧωοτϫʔΫͷߏ଄৘ใΛ൓ө࣭ͨ͠ྔϑϥΫλϧ࣍‫[ ݩ‬3] ΋ Sample2 ͷํ͕େ͖͍͜ͱ
͔ΒɼγϦΧ෼ࢄॲཧʹΑΓ‫ۉ‬ҰԽ͕ਤΒΕͨ͜ͱΛ
ࢧ࣋͢Δ݁Ռͱͳͬͨɽ·ͨɼΰϜࡐྉͷಈత೪஄ੑ
ࢼ‫͚͓ʹݧ‬ΔώεςϦγεϩε΋ Sample2 ͷํ͕খ͘͞ͳΓɼࡐྉߏ଄ͱͷྑ޷ͳ૬ؔੑΛࣔͨ͠ɽಈత৚݅ԼͰͷࡐྉߏ଄ͷมԽΛΈΔͨΊʹɼ৳௕

Fig. 2. SAXS profiles under tensile test.

࣌ʹ͓͚ΔࢄཚଌఆΛ࣮ࢪͨ͠ɽFig. 2 ͸ɼSBR/γϦΧ഑߹‫͚͓ʹܥ‬ΔΰϜࡐྉͷ֤৳௕཰ʹ͓͚Δ 2 ࣍‫ࢄݩ‬ཚ૾ͱԁ‫؀‬ฏ‫ʹۉ‬ΑΓࢉग़ͨ͠ࢄཚ‫ۂ‬ઢͰ͋Δɽ
ࢄཚ૾͔Β͸ɼ৳௕཰ͷ૿େʹ൐͍όλϑϥΠύ
λʔϯ͕ΑΓ઱໌ʹ‫ݱ‬Εɼ͔ͭҾுํ޲ͱ͸ਨ௚ํ޲ʹ഑޲͕‫ܗ‬੒͞Ε͍ͯΔՄೳੑΛࣔࠦ͢Δ݁Ռͱ
ͳͬͨɽ·ͨࢄཚ‫ۂ‬ઢΑΓɼγϦΧ‫ूڽ‬ମ༝དྷͷγϣϧμʔϐʔΫ͕৳௕ͱͱ΋ʹγϑτ͍ͯ͠Δ͜ͱ͔
ΒɼࡐྉதͷγϦΧߏ଄ʹ༝དྷͨ͠ߏ଄มԽ͕‫ͬ͜ى‬
͍ͯΔͱߟ͑ΒΕΔɽҰൠతʹҾுํ޲ʹରͯ͠ϙϦϚʔ࠯͕഑޲͢Δͱߟ͑ΒΕ͍ͯΔ͕ɼ͋ΘͤͯγϦΧͷ഑޲ߏ଄Λߟྀ
͢Δ͜ͱͰɼΑΓৄࡉʹม‫࣌ܗ‬ͷߏ଄ܾఆΛߟ࡯Ͱ͖Δख͕͔ΓͷҰͭͱͳΔɽ·ͨɼ300 %৳௕࣌ͷࢄཚϓϩϑΝΠϧ͕ͦΕ·Ͱͷ΋ͷΑΓେ͖͘มԽ͍ͯ͠
Δ͜ͱ͔ΒɼഁஅʹࢸΔߏ଄มԽͷલ৮ΕΛͱΒ͑ͯ

Fig. 3. SAXS profiles analyzed by vertical and horizontal component in scattering image.

͍ΔՄೳੑ΋ߟ͑ΒΕେม‫ڵ‬ຯਂ͍݁Ռͱͳͬͨɽ

– 49 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

Fig. 4. (a) Correlation between oriented rubber and mold flow. (b) Scattering image of oriented rubber.

ࢄཚ૾ͷਫฏํ޲ͱਨ௚ํ޲ͷσʔλΛͦΕͧΕʹͱΛৄࡉʹ‫ݕ‬౼ͨ݁͠ՌɼMold Flow ͱ͸ਨ௚ͷํऔΓग़͠ɼࢄཚ‫ۂ‬ઢʹฦͨ݁͠ՌΛ Fig. 3 ʹࣔ͢ɽਨ޲ʹγϦΧ‫ूڽ‬ମ༝དྷͷ഑޲͕‫ܗ‬੒͞ΕΔͷΛ֬ೝͰ௚ɾਫฏํ޲ͷͦΕͧΕͷσʔλͰɼγϣϧμʔϐʔ͖ͨ (Fig. 4(b))ɽΰϜͷ‫ػ‬ցಛੑʹؔͯ͠΋ɼ഑޲ΫҐஔɼϐʔΫγϑτྔɼ࣭ྔϑϥΫλϧ࣍‫ݩ‬౳ʑϓํ޲ʹਫฏɼਨ௚ͷ 2 ਫ४Ͱ֤छࢼ‫ݧ‬Λ࣮ࢪͨ͠ͱ͜

ϩϑΝΠϧ͕େ͖͘ҟͳΔɽਨ௚ํ޲σʔλதͷγϣΖɼҾுಛੑɼ೪஄ಛੑʹ༗ӹͳ͕ࠩΈΒΕͨɽϧμʔϐʔΫ͸ɼ৳௕཰ʹԠͨ͡ϐʔΫγϑτ͕ΈΒΕɼ৳௕ʹ൐͏γϦΧ‫ूڽ‬ମؒ‫཭ڑ‬Λ൓ө͍ͯ͠Δࠓ‫ޙ‬ͷ՝୊

ͱߟ͑ΒΕΔɽରͯ͠ਫฏํ޲ͷσʔλ͸ɼγϦΧ‫ڽ‬ूମαΠζ༝དྷͷϓϩϑΝΠϧͰ͋ΔͱਪఆͰ͖Δͨ
Ίɼ૯ͯ͡ม‫͚͓ʹܗ‬Δࡐྉߏ଄ܾఆ͕۩ମతʹՄೳͱͳͬͨɽ·ͨɼFig. 4(a) ͸ɼSBR/γϦΧ‫ܥ‬ΰϜͷಉҰαϯϓϧγʔτ಺Λ෼ׂଌఆ͠ɼͦͷࡍಘΒΕͨ 2 ࣍‫ࢄݩ‬ཚ૾ΛଌఆՕॴຖʹ·ͱΊͨ΋ͷͰ͋Δɽࢄཚ૾ͷόλϑϥΠύλʔϯ͔Β഑޲ੑ͕ೝΊΒΕɼ͜Ε͕ q ஋ΑΓ 100∼200 nm εέʔϧͰ഑޲ߏ଄Λ‫ܗ‬੒͍ͯ͠Δͱਪ࡯Ͱ͖ΔͨΊɼγϦΧ‫ߏूڽ‬଄༝དྷͷ഑޲͕ࣔࠦ͞ΕΔɽ͞ΒʹଌఆՕॴʹΑΔ֯౓ґଘੑ͕‫ݟ‬ड͚ΒΕΔ
͜ͱ͔ΒɼՃེૢ࡞࣌ʹ͓͚Δۚ‫Ͱ಺ܕ‬ͷΰϜͷྲྀΕ
ʢMold Flowʣͱ૬͍ؔͯ͠ΔՄೳੑ͕͋Δɽ͜ͷ͜ࡐྉߏ଄ධՁʹରͯ͠‫ͳྗڧ‬πʔϧͰ͋Δ์ࣹޫ̭ઢখ֯ࢄཚΛ‫ͯ͠࢖ۦ‬ɼ෺ੑͱߏ଄ͷ૬ؔΛߟ࡯͠ɼ֤੡඼ʹର͢Δ࠷దߏ଄ΛεέʔϧຖʹఏҊɼల։Ͱ
͖ΔΑ͏ͳσʔλϕʔεΛߏங͍ͨ͠ɽ·ͨɼΰϜ੡଄࣌ʹ͓͚Δ഑޲ੑͷ੍‫ʹޚ‬ΑΓɼ͞ΒͳΔ੡඼ͷߴੑೳԽɼߴ‫ػ‬ೳԽ΁ͱ‫ظ‬଴Ͱ͖Δ͜ͱ͔Βɼࠓ‫ࡉৄޙ‬ʹղੳ͢Δ༧ఆͰ͋Δɽࢀߟจ‫ݙ‬[1] G. Beaucage: J.Appl.Cryst. 28, 717-728 (1995).
[2] T. Koga et al: Macromolecules 41, 453-464(2008).
[3] D. Yamaguchi et al: Eur.Phys.J.B, 63, 153-163(2008).

– 50 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

BL08B2, BL24XU

2011B3325, 2012A3325, 2012A3220

XAFS ʹΑΔΤωϧΪʔσόΠεࡐྉͷ‫ߏॴہ‬଄ղੳStructure Analysis of Energy Device Materials by XAFSߴ‫ ڮ‬রԝɼ෱ຬ ਔࢤɼ໦ଜ ޺ɼ຤޿ ল‫ޗ‬ɼౡా ਅҰɼத௡ ࿨߂
Teruo Takahashi, Hitoshi Fukumitsu, Hiroshi Kimura, Syougo Suehiro, Shin-ichi Shimada,Kazuhiro NakatsuॅԽ෼ੳηϯλʔɹٕज़։ൃηϯλʔ
Sumika Chemical Analysis Service Co. Ltd,Technology Innovation Center֓ཁɿɹΤωϧΪʔσόΠεͱͯ͠༻͍ΒΕ͍ͯΔϦν΢ϜΠΦϯ 2 ࣍ి஑ (LIB) ͷਖ਼‫ࡐۃ‬Λ XAFS(̭ઢ‫ٵ‬ऩඍࡉߏ଄ղੳ) ʹΑΓߦͬͨɽಁաྗͷߴ͍ߴً౓์ࣹޫΛར༻͢Δ͜ͱͰɼॆ์ి͠ͳ͕Βਖ਼‫׆ۃ‬෺࣭தͷભҠۚଐͷՁ਺ɼߏ଄มԽΛ in-situ Ͱ௥੻͢Δ͜ͱ͕Ͱ͖ͨɽ·ͨి஑໘಺ͷ‫ڍ‬ಈ͚ͩͰͳ͘ɼి‫ۃ‬அ໘ʹ͓͚Δ෼ੳʹ͍ͭͯ΋ϚΠΫϩϏʔϜΛར༻͢Δ͜ͱͰ࣮ࢪՄೳͰ͋Δ͜ͱ͕֬ೝͰ͖ͨɽ
Ωʔϫʔυɿɹฌ‫ ݝݿ‬BLɼϦν΢ϜΠΦϯి஑ɼXAFSɼϚΠΫϩϏʔϜʹͯ࡞੒Λߦͬͨɽਖ਼‫ʹۃ‬͸ NCA(χοέϧίόϧτ

എ‫ڀݚͱܠ‬໨త࠶ੜΤωϧΪʔʹର͢Δࣾձతཁ๬ʹΑΓɼΤωϧΪʔσόΠεͱͯ͠Ϧν΢ϜΠΦϯ 2 ࣍ి஑ (LIB) ʹର͢Δ‫ظ‬଴ɾཁ๬͕ߴ·͍ͬͯΔɽLIB ͷੑೳ޲্ʹ͸࡞੡ͨ͠ి஑ి‫ిͱۃ‬஑ੑೳͷ૬ؔΛཧղ͢Δ͜ͱ
͕ඞཁͰ͋Δɽి஑ి‫ۃ‬͸‫׆‬෺࣭ɼόΠϯμʔɼಋిॿࡎ͔ΒͳΔෳࡶͳߏ଄Λͱ͓ͬͯΓɼಛੑͷཧղʹ͸લॲཧΛ‫ؚ‬Ίͨద੾ͳ෼ੳख๏ͷద༻͕ॏཁͱͳΔɽ
ຊ՝୊Ͱ͸ಛʹ LIB ਖ਼‫ࡐۃ‬ྉʹண໨͠ɼՁ਺΍݁߹‫Ͳͳ཭ڑ‬ͷॏཁͳߏ଄৘ใΛಘΔ͜ͱ͕Ͱ͖Δ XAFSΞϧϛ) ਖ਼‫ࡐۃ‬ɼෛ‫ʹۃ‬͸ΧʔϘϯɼిղӷʹඇਫ‫ܥ‬ిղӷʢిղ࣭ 1M LiPF6 Λ‫ؚ‬ΉΤνϨϯΧʔϘωʔτͱδΤνϧΧʔϘωʔτͷମੵൺ 1ɿ1 ࠞ߹༹ӷʣΛ༻͍ͨϥϛωʔτηϧΛ੡࡞ͨ͠ɽ͜ΕΛ BL08B2
ʹ࣋ͪࠐΈɼॆ์ి૷ஔͱ઀ଓɼ0.2C ͷ৚݅Ͱॆ์
ి͠ͳ͕Βి‫ۃ‬ͷத৺෇ۙΛ XAFS ଌఆͨ͠ɽଌఆ
͸χοέϧɼίόϧτͷͦΕͧΕͷ‫ٵ‬ऩ୺Ͱಁա๏ʹͯߦͬͨɽ̎ʣϚΠΫϩϏʔϜΛར༻ͨ͠அ໘ XAFS ଌఆΛར༻࣮ͨ͠‫ݧ‬Λߦͳͬͨɽ์ࣹޫΛར༻͢Δ XAFS̍ʣͱಉ༷ʹਖ਼‫ʹۃ‬͸ NCA(χοέϧίόϧτΞϧ

Ͱ͸ಛʹి஑Քಈঢ়ଶͰͷ in-situ ෼ੳʹҖྗΛൃ‫ش‬ϛ) ਖ਼‫ࡐۃ‬ɼෛ‫ʹۃ‬͸ΧʔϘϯɼిղӷʹ̍ʣͱಉ͡

͢ΔɽΞϧϛϥϛωʔτ‫ిܕ‬஑Λ࡞੒͠ɼॆ์ి͠ͳ

ඇਫ‫ిܥ‬ղӷΛ༻͍ͨϥϛωʔτηϧΛ੡࡞ͨ͠ɽ͜

͕Βͷ in-situ XAFS ଌఆʹΑΔਖ਼‫ࡐۃ‬ͷ‫ߏॴہ‬଄ղΕΛॴఆͷॆిঢ়ଶ·Ͱॆి‫ޙ‬ɼి஑Λղମɼਖ਼‫ۃ‬ΛੳΛ࣮ࢪͨ͠ɽ·ͨ LIB ి‫ۃ‬͸ްΈํ޲ʹిࢠɼΠऔΓग़ͯ͠ిղӷͰચড়ͨ͠ɽి஑ͷղମ͸άϩʔϒΦϯ఻ಋ͢Δ͜ͱ͔Βɼ໘಺͚ͩͰͳ͘அ໘ํ޲ͷॆϘοΫε಺෦Ͱ࣮ࢪͨ͠ɽࢼྉ͸ະॆిɼ50 %ॆిɼ์ిঢ়‫گ‬ͷ೺Ѳ΋ॏཁͱߟ͑ΒΕΔɽͦ͜Ͱஅ໘ʹ͓

100 %ॆిͷ 3 छྨΛ४උͨ͠ɽ

͚ΔϚΠΫϩϏʔϜΛར༻ͨ͠ XAFS ଌఆ͕Մೳ͔
Ͳ͏͔ʹ͍ͭͯ΋‫ݕ‬౼Λ࣮ࢪͨ͠ɽ

ਖ਼‫ۃ‬γʔτΛथࢷͰ๊ຒ͠ɼΞϧΰϯΠΦϯΛར༻ͨ͠அ໘Ճ޻૷ஔʹͯి‫ۃ‬அ໘ࢼྉΛ࡞੒ͨ͠ɽ͜ͷࢼྉΛ BL24XU ʹ͓͍ͯϚΠΫϩ XAFS ࣮‫͠ڙʹݧ‬࣮‫ݧ‬ͨɽࢼྉ͸·ͣ͸χοέϧɼ͓Αͼίόϧτͷ‫̭ޫܬ‬̍ʣϥϛωʔτηϧΛར༻ͨ͠ in-situ XAFS ଌఆઢϚοϐϯάΛߦ͍ଌఆҐஔΛܾΊΔࢀߟσʔλͱ͠ଌఆʹར༻͢ΔϦν΢Ϝి஑ి‫ࢼۃ‬ྉ͸ҎԼͷखॱͨɽଌఆҐஔΛܾΊͨ‫ޙ‬ɼϚΠΫϩϏʔϜ̭ઢʢ3 µm– 51 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

Fig. 1. (a) Ni K-edge XANES spectra of NCA electrode (charge process). (b) Charging curve of NCA
electrode (red square; left axis) and XANES peak position (blue square; right axis).
× 1 µmʣΛར༻͠ɼ‫ޫܬ‬๏ʹͯ XAFS εϖΫτϧΛ
औಘͨ͠ɽ

1.5 Å ෇ۙʹ Ni-O ݁߹ɼ2.5 Å ෇ۙʹ Ni-Ni ݁߹ͷϐʔΫ͕֬ೝͰ͖ΔɽNi-O ݁߹ϐʔΫ͸ॆిʹ൐͍‫͕౓ڧ‬େ͖͘ͳ͍ͬͯΔ༷ࢠ͕‫ݟ‬ΒΕͨɽ͜Ε͸ Ni

݁Ռ͓Αͼߟ࡯

ΠΦϯ͸ϠʔϯςϥʔޮՌʹΑΓ࿪Μͩࢎૉ 6 ഑Ґߏ଄Ͱ͋Δ͕ɼॆిʹΑΓ͜ͷޮՌ͕ফࣦɼNi-O ݁߹̍ʣϥϛωʔτηϧΛར༻ͨ͠ in-situ XAFS ଌఆ

Fig. 1 ʹχοέϧ K ‫ٵ‬ऩ୺ʹ͓͚Δ XAFS ଌఆ݁ՌΛࣔͨ͠ɽॆిʹ൐͍‫ٵ‬ऩ୺͕࿈ଓతʹߴΤωϧΪʔଆʹγϑτ͍༷ͯ͘͠ࢠ͕֬ೝͰ͖ͨɽॆ์ి
Χʔϒͱ XANES εϖΫτϧͷϐʔΫτοϓҐஔΛϓϩοτ͢Δ͜ͱͰχοέϧͷՁ਺ͱͷ࿈ಈੑ΋֬ೝͰ‫͕ͦ཭ڑ‬Ζ͍ɼϐʔΫ‫͢ڧ૿͕౓ڧ‬Δ͜ͱ͕஌ΒΕͯ
͍Δ [1]ɽίόϧτͰ͸͜ͷΑ͏ͳޮՌ͕‫ݟ‬ΒΕͳ͍͜ͱ΋֬ೝͰ͖͍ͯΔɽ͜ͷΑ͏ʹ‫ݩ‬ૉ͝ͱͷ‫ߏॴہ‬଄ͷมԽΛ in-situ Ͱ௥੻͢Δ͜ͱ͕Ͱ͖ͨɽ
̎ʣϚΠΫϩϏʔϜΛར༻ͨ͠அ໘ XAFS ଌఆ

Fig. 3 ʹ 50 %ॆిࢼྉͷஅ໘ XAFS ଌఆ݁ՌΛࣔ

͖͍ͯΔɽFig. 2 ʹ͸ EXAFS ղੳͷ݁ՌΛࣔͨ͠ɽͨ͠ɽ‫̭ޫܬ‬ઢϚοϐϯάͰಛ௃తͳஅ໘ͷ 3 ՕॴͰͦΕͧΕϚΠΫϩϏʔϜΛར༻ͨ͠ XAFS εϖΫτϧΛऔಘͨ͠ɽ͜ͷࢼྉʹ͓͍ͯ͸அ໘Ͱͷ৔ॴґଘੑ͸‫ݟ‬ΒΕͳ͔ͬͨɽNCA ‫ܥ‬ਖ਼‫Ͱࡐۃ‬͸ॆిঢ়ଶͰ
ి஑Λ์ஔ͢ΔͱϦν΢Ϝ͕֦ࢄ͠ɼిҐ෼෍͕ฏ‫ۉ‬Խ͞Εͯ͠·͏ͱ͞Ε͍ͯΔɽࠓճͷ࣮‫Ͱݧ‬͸ɼॆి‫ޙ‬ɼղମ͢Δ·Ͱͷ͕࣌ؒ௕͔ͬͨͨΊʹి‫಺ۃ‬෦ͰϦν΢Ϝͷ֦ࢄ͕‫͍·ͯͬ͜͠ى‬ɼ৔ॴґଘੑ͕‫ݟ‬ΒΕͳ͔ͬͨՄೳੑ͕ߟ͑ΒΕΔɽ

Fig. 4 ʹࣔ͢Α͏ʹɼະॲཧɼ50 %ॆిɼ100 %ॆిͦΕͧΕͷࢼྉʹ͓͚Δ XAFS εϖΫτϧΛൺֱ
͢Δͱɼॆిʹͱ΋ͳ͍ߴΤωϧΪʔଆ΁γϑτ͍༷ͯ͘͠ࢠ͕֬ೝͰ͖͓ͯΓɼࢼྉؒͰͷൺֱ͸໰୊ͳ

Fig. 2. Fourier-transform of in-situ Ni K-edge EX-

͘Ͱ͖Δ͜ͱ͕֬ೝͰ͖ͨɽ

AFS spectra of NCA electrode.

– 52 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

Fig. 3. (a) Fluorescence X-ray mapping and (b) microbeam XANES spectra of NCA electrode (SOC 50 %).
Ͱ͖ͨɽࠓ‫ޙ‬ͷ՝୊ͱͯ͠Լ‫ه‬ͷ 2 ఺ʹ͍ͭͯ‫ݕ‬౼Λ࣮ࢪ͢Δɽ


1 2 ࣍‫ ݩ‬XAFS

ࣗಈं༻Λ͸͡Ίͱͯ͠ి‫ۃ‬໘ੵͷେ‫ܕ‬Խ͕ਐߦ͠

͍ͯΔɽి‫ۃ‬໘಺ʹ͓͚Δॆ์ిͷෆ‫ۉ‬Ұɼ͓Αͼͦͷ‫ݪ‬Ҽͷղ໌ʹ޲͚ͯ 2 ࣍‫Ͱݩ‬ͷॆ์ి਒౓ͷ೺Ѳ͕ඞཁʹͳΔɽͳ͓ɼ͜ͷ৔߹Ͱ΋ॆ์ి͠ͳ͕Βͷin-situ ෼ੳ͕๬·ΕΔɽ2 େ‫ؾ‬ඇ๫࿐Ͱͷஅ໘ XAFS ଌఆຊ՝୊Ͱ͸ి஑Λղମ‫ޙ‬ɼେ‫ؾ‬தͰϚΠΫϩϏʔϜΛར༻ͨ͠அ໘ XAFS ଌఆΛ࣮ࢪͨ͠ɽ࣮ࡍͷి஑

Fig. 4. Microbeam XANES spectra of NCA electrode.

ࡐྉ͸େ‫ͱؾ‬ͷ൓ԠʹΑΓม࣭͢ΔͨΊɼงғ‫ؾ‬ःஅηϧΛ࡞੡ͯ͠ଌఆΛߦͳ͏ඞཁ͕͋Δɽࢀߟจ‫ݙ‬·ͱΊͱࠓ‫ޙ‬ͷ՝୊Ҏ্ͷ݁Ռ͔ΒɼLIB Λॆ์ి͠ͳ͕Βͷ‫ڍ‬ಈɼ͓[1] ଠాढ़໌ɿ̭ઢ‫ٵ‬ऩ෼ޫɹ XAFS ͱͦͷԠ༻.

Αͼஅ໘ʹ͓͚ΔՁ਺มԽʹ͍ͭͯ஌‫ݟ‬ΛಘΔ͜ͱ͕

– 53 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

BL24XU

2009B3200, 2010A3200, 2010B3200

ߗ̭ઢφϊूޫ༻ԁ‫ܗ‬ଟ૚ບκʔϯϓϨʔτͷ੡࡞ͱੑೳධՁ

Circular Multilayer Zone Plate for High-energy X-ray
Nano-imaging
࿜ౡ ༃ 1 , খࢁ‫ ٱو‬1∗ , ߴ໺ल࿨ 1 , খ੢ൟथ 1† , ௰ ୎໵ 1∗ , ஛த‫ وٱ‬2‡ , ࢢ‫ ؙ‬ஐ 2 , େ஌ব೭ 2
Yasushi Kagoshima1 ,Takahisa Koyama1∗ , Hidekazu Takano1 , Shigeki Konishi1† , Takuya
Tsuji1∗ , Hisataka Takenaka2‡ , Satoshi Ichimaru2 , Tadayuki Ohchi,211ฌ‫ཱݝݿ‬େֶେֶӃ෺࣭ཧֶ‫ڀݚ‬Պଟॏ‫ݶۃ‬෺࣭Պֶηϯλʔ, 2 NTT ΞυόϯεςΫϊϩδ‫ࣜג‬ձࣾ

Center for Novel Material Science under Multi-Extreme Conditions, Graduate School of Material Science,
University of Hyogo,
2

NTT Advanced Technology Corporation֓ཁɿɹ̭ઢԁ‫ܗ‬ଟ૚ບκʔϯϓϨʔτʢMZPʣΛ੡࡞͠ɼ20 keV ͷ̭ઢΛ༻͍ͯͦͷूޫੑೳΛධՁͨ͠ɽ

MoSi2 ͱ Si Λଟ૚ບࡐͱ͠ɼDC ϚάωτϩϯεύολϦϯάʹΑΓਊઢ্ʹަ‫ʹޓ‬੒ບͨ͠ɽઢ૾ؔ਺Λଌఆ͠ɼτϞάϥϑΟʔͷख๏Λ༻͍ͯ఺૾ؔ਺ʹม‫ͨ͠׵‬ɽͦͷ݁Ռɼ੡࡞ͨ͠ MZP ͸ճં‫ݶ‬քੑೳʢճ
ંੵ෼ͰಘΒΕͨ஋Ͱ͋Δ 35 nmʣΛୡ੒Ͱ͖Δ͜ͱΛࣔͨ͠ɽ͞Βʹɼ૸ࠪ‫ݦܕ‬ඍ‫ʹڸ‬ద༻͠ɼ50 nm ͷline-&-space Λղ૾͢Δ͜ͱ͕Ͱ͖ͨɽঘɼຊใࠂॻ͸‫ݪ‬ஶ࿦จʢT. Koyama et al., Rev. Sci. Instrum. 83,
013705 (2012).ʣΛ೔ຊ‫ޠ‬Խ͠ɼվฤͨ͠΋ͷͰ͋ΔɽΩʔϫʔυɿɹߴۭؒ෼ղೳߗ̭ઢϨϯζɼ̭ઢ‫ݦ‬ඍ‫ڸ‬ɼϑϨωϧκʔϯϓϨʔτɼઢ૾෼෍ؔ਺ɼ఺૾෼෍
ؔ਺ʹΑͬͯఏҊ͞Εͨ [1]ɽզʑͷάϧʔϓ΋ɺಉ༷ͷഎ‫ڀݚͱܠ‬໨తϑϨωϧκʔϯϓϨʔτʢFZPʣ͸ɼ̭ઢ‫ݦ‬ඍ‫ڸ‬ͷ̭ઢϨϯζͱͯ͠޿͘༻͍ΒΕ͍ͯΔɽͦͷۭؒ෼ղೳ͸࠷΋֎ଆͷκʔϯ෯Ͱܾ·Γɼκʔϯ෯͕‫΄͍ڱ‬ํ๏Λ༻͍̭ͯઢԁ‫ܗ‬ଟ૚ບκʔϯϓϨʔτʢMZPʣͷ։ൃΛਐΊ͖ͯͨɻຊߘͰ͸ɼզʑ͕։ൃͨ͠ MZPͷ੡࡞๏ͱूޫಛੑධՁʹ͍ͭͯड़΂ΔɽͲߴ͍ۭؒ෼ղೳ͕ಘΒΕΔɽճંޮ཰͸κʔϯͷް͞Ͱܾ·Γɼߗ̭ઢྖҬͰ࣮༻తͳճંޮ཰ΛಘΔʹ

ଟ૚ບκʔϯϓϨʔτͷ੡࡞͸ॏۚଐΛ༻͍ͯ΋਺ेϚΠΫϩϝʔτϧͷް͕͞ଟ૚ບࡐʹ͸ MoSi2 ͱ Si Λબ୒ͨ͠ɽ͜ͷ૊Έ߹ඞཁͰ͋Δɽैͬͯɼߴ͍ۭؒ෼ղೳͱߴ͍ճંޮ཰

Θͤʹ͸ɼ଱೤ੑ͕ߴ͘ք໘ͷ֦ࢄ͕গͳ͍ͱ͍͏ಛ

Λಉ࣌ʹ࣮‫͢ݱ‬Δʹ͸ɼඇৗʹΞεϖΫτൺͷେ͖͍௕͕͋Δ [2]ɽFig. 1 ʹࣔ͢Α͏ʹɼMZP ͸Ψϥεඍκʔϯߏ଄͕ඞཁͱͳΔɽFZP ͸௨ৗిࢠϏʔϜϦࡉਊઢ্ʹ DC ϚάωτϩϯεύολϦϯάʹΑΓଟιάϥϑΟʔ๏Ͱ࡞ΒΕΔ͕ɼಉ๏Ͱ͸ΞεϖΫτൺ૚ບΛ੒ບ͠ɼͦͷ‫ޙ‬ɼ੾அɾ‫ݚ‬ຏɾബยԽ͠ɼॴ๬

ͷେ͖͍ඍࡉߏ଄ͷ࡞੡͕‫ۃ‬Ίͯࠔ೉Ͱ͋Δɽ͜ͷ໰ͷް͞ͱ͢Δɽਊઢͷ௚‫ܘ‬͸ɼࢢൢͷϨʔβʔଌఆ‫ث‬୊Λࠀ෰͢ΔͨΊʹɼࡉ͍ϫΠϠʔͷଆ໘ʹܰ‫ݩ‬ૉͱॏ‫ݩ‬ૉͷ૊Έ߹Θ͔ͤΒͳΔଟ૚ບΛৠணͯ͠ɼͦΕΛബບঢ়ʹ‫ݚ‬ຏ͢ΔεύολʔεϥΠεκʔϯϓϨʔΛ༻͍ͨ‫ܭ‬ଌʹΑΓ 50.192 µm ͱܾΊͨɽN ൪໨ͷκʔϯͷ൒‫ ܘ‬rn ͱয఺‫ ཭ڑ‬f ͸࣍ࣜͰ༩͑ΒΕΔɽ

τʢଟ૚ບκʔϯϓϨʔτͱ΋͍͏ʣ͕ Rudolph Β∗ ‫ࡏݱ‬ͷॴଐ: JASRI/SPring-8† ‫ࡏݱ‬ͷॴଐ: εϓϦϯάΤΠταʔϏε‫ࣜג‬ձࣾ‡ ‫ࡏݱ‬ͷॴଐ: ‫ࣜג‬ձࣾτϠϚ

rn =


√
r2
nf λ = nr1 , f = 1 .
λ͜͜Ͱɼr1 ͸ୈ 1 κʔϯͷ൒‫ܘ‬ɼλ ͸೾௕Ͱ͋Δɽ࠷಺൒‫ ܘ‬rim (im=251) ͸্ड़ͷਊઢ௚‫ܘ‬ͷ൒෼ͱͨ͠ɽ

– 54 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू
͜ΕʹΑΓɼr1 =1.584 µm ͱͳΔɽ࠷େʢ࠷಺ʣκʔ

Δ͚ͩߴ͘͢ΔͨΊͰ͋ΔɽMZP Λۭؒతʹίώʔϯ෯ ∆rim ɼ࠷খʢ࠷֎ʣκʔϯ෯ ∆rom (om=385)ɼ

Ϩϯτʹর໌͢ΔͨΊʹɼޫ‫͔ݯ‬Β໿ 30 m ͷҐஔશଟ૚ບް rom − rim ɼ‫ܗ‬੒κʔϯ਺ N ͸ͦΕͧΕɼʹ͋Δ̐৅‫ݶ‬εϦοτͷ։‫ޱ‬αΠζΛ໿ 10 µm ࢛ํ50.0 nmɼ40.4 nmɼ5.985 µmɼ134 (=385-251) Ͱ͋ͱͨ͠ɽ࠷Լྲྀͷ CCD ΧϝϥΛ༻͍ͯूޫϏʔϜͷ

Δɽޫ࣠ํ޲ͷް͞͸ɼκʔϯ෯͕ 40 nm Ͱ̭ઢͷ

Far-field beam pattern Λ‫͕ͳ͠࡯؍‬Βɼޫֶ‫ܥ‬ΛௐΤωϧΪʔ͕ 20 keV ͷͱ͖࠷େճંޮ཰Λ༩͑Δ੔ͨ͠ɽଞͷৄࡉ͸ Fig. 3 Λࢀর͞Ε͍ͨɽۭؒ෼ղ

32 µm ͱͨ͠ɽ͜ͷͱ͖ͷճંޮ཰͸ɼcoupled waveೳ͸ɼ௚‫ ܘ‬300 µm ͷനۚϫΠϠʔΛφΠϑΤοδʹ

theory [3, 4] ʹ‫ʹࢉܭͮ͘ج‬ΑΔͱ 35.6%Ͱ͋Δɽ20

༻͍ͨ҉ࢹ໺φΠϑΤοδ૸ࠪ๏ʹΑΓଌఆͨ͠ɽ͜

keV ʹ͓͚Δয఺‫཭ڑ‬͸ 40.5 mm Ͱ͋ΔɽFig. 2 ʹΕʹΑΓಘΒΕΔϏʔϜϓϩϑΝΠϧ͸ઢ૾෼෍ؔ਺

੡࡞ͨ͠ MZP ͷஅ໘ͷ૸ࠪిࢠ‫ݦ‬ඍ‫૾ڸ‬Λࣔ͢ɽ

ʢline spread function: LSFʣͰ͋ΔɽφΠϑΤοδ
ͷਫ਼ີ૸ࠪʹ͸෼ղೳ 2 nm ͷϐΤκεςʔδΛ༻͍ͨɽଌఆͰಘΒΕͨ LSF ͷ൒஋શ෯ʢFWHMʣ͸ 110

Wire
core
Multilayer
deposition(MoSi2/Si)

Sectioning,
polishing &thinning

Zone
width

Incidentbeam(20 keV)

Center stop
OSA
(Au 30 µmφ, 100 µmt) (Pt 20 µmφ)

CCD cameraor PIN diode

MZP
4D-slitZone
thickness

Fig. 3.

Blade
Knife edge
(Pt 300-µmφ wire)

Optical system for evaluating focusing

properties of the MZP constructed at the Hyogo
ID-BL (BL24XU) of SPring-8.

Fig. 1. Fabrication process of MZP.

nm Ͱ͋ͬͨɽԁ‫ܗ‬։‫ޱ‬Ϩϯζͷ৔߹ɼ఺૾෼෍ؔ਺

(a) Multilayer Overcoat layer (b)ʢpoint spread function: PSFʣͷಈ‫޲ํܘ‬ͷϏʔϜϓϩϑΝΠϧͱ LSF ͷ‫ܗ‬ঢ়͕΄΅Ұக͢ΔͨΊɼLSF
ͷ FWHM ΛूޫϏʔϜαΠζͱ͢Δ͜ͱ͕ଟ͍ɽ͠

Core

Core

͔͠ͳ͕Βຊ MZP ͷ৔߹ɼ࡞੡্ͷ੍໿͔Β‫ྠ͍ڱ‬ଳ։‫ޱ‬Λ࣋ͪɼLSF ͸‫͍ڧ‬αΠυϐʔΫʢ෭‫ۃ‬େʣͷ

10 μmӨ‫ڹ‬Λड͚ΔͨΊɼPSF ͱ͸େ͖͘ҟͳΔϏʔϜϓϩ~6 μm

ϑΝΠϧͱͳΔɽ͢ͳΘͪɼ LSF ͷ FWHM ͸ PSF

Fig. 2. Micrographs of the fabricated MZP ob-ͷͦΕΑΓ͔ͳΓେ͖͘ͳΔɽͦ͜Ͱίϯϐϡʔλτ

tained using a scanning electron microscope: (a)ϞάϥϑΟʔʢCTʣͷ࠶ߏ੒‫ݪ‬ཧΛԠ༻ͯ͠ɼLSF

whole structure and (b) enlarged image of themultilayer region (region indicated by the white
rectangle in (a)).

͔Β PSF Λ‫ٻ‬Ίͨɽͦͷ‫ݪ‬ཧͷ֓೦Λ Fig. 4 ʹࣔ͢ɽφΠϑΤοδʢNanoslitʣΛ X ํ޲ʹ૸ࠪͯ͠ಘΒ
ΕΔ‫౓ڧ‬෼෍͕ LSF Ͱ͋ΔɽφΠϑΤοδͷճస֯Λ θ ͱ͢Ε͹ɼφΠϑΤοδͷҐஔ X Ͱͷ LSF ͷ஋͸ɼয఺पΓͷ‫౓ڧ‬෼෍ʢPSFʣͷ Y ํ޲΁ͷੵ෼ूޫಛੑධՁ

஋ͳͷͰɼLSF(X, θ) ͸ X ઢτϞάϥϑΟʔʹ͓͚Δ

Fig. 3 ʹूޫಛੑධՁ࣮‫ݧ‬ͷޫֶ‫ܥ‬Λࣔ͢ɽ̭ઢ

ઢ‫ٵ‬ऩ܎਺ͷ౤ӨʹରԠ͢Δɽैͬͯɼয఺पΓͷ‫ڧ‬ͷΤωϧΪʔ͸γϦίϯ̎݁থ෼ޫ‫ث‬ʢ෼ޫ‫ ث‬BʣͰ౓෼෍Λઢ‫ٵ‬ऩ܎਺෼෍ͱΈͳͤ͹ɼCT ࠶ߏ੒ͷ‫ݪ‬

20 keV Λબ୒ͨ͠ɽ͜Ε͸ Mo ͷ K ‫ٵ‬ऩ୺௚ԼͷΤཧΛͦͷ··ద༻͢Δ͜ͱʹΑͬͯ PSF Λ‫͖Ͱࢉܭ‬ωϧΪʔͰ͋ΓɼMo ͷ‫ٵ‬ऩΛආ͚ͯճંޮ཰ΛͰ͖Δɽຊ‫Ͱڀݚ‬͸·ͣୈҰஈ֊ͱͯ͠ɼ̍ͭͷ LSF Λ– 55 –


Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)ฏํ޲Ͱ line-&-space (L&S) ͷίϯτϥετ͕ए‫ׯ‬Y
Back-projection

LSFҟͳΔ͕ɼ͜Ε͸ MZP ͷඇ఺ऩࠩͷͨΊͰ͸ͳ͘ɼXޫֶ‫ܥ‬ͷυϦϑτͷӨ‫ʹڹ‬ΑΓଌఆʹ௕࣌ؒΛཁ͢Δyํ޲ͷղ૾ྗ͕‫ྼ্͚͔ݟ‬Խͨͨ͠ΊͰ͋Δɽ૸ࠪํ

Projection

X

O

PSF

(a)

(b)

2.0

Intensity
distribution͕ղ૾Ͱ͖ͨ͜ͱ͕ͦͷূࠨͰ͋Δɽ

x

Z (μm)

1.5

Nanoslit
scan

0.5

Fig. 4. Diagram showing calculation of PSF from
LSF based on tomographic reconstruction.

50 nm L&S

1.0θ޲Λม͑Δ͜ͱͰɼԖ௚ɾਫฏ྆ํ޲Ͱ 50 nm ͷ L&S

0.0

50 nm L&Sશ౤Өํ޲Ͱ౳͍͠ͱͯ͠ CT ࠶ߏ੒‫ࢉܭ‬Λߦͬͨɽ0.0ͦͷ݁ՌΛ Fig. 5 ʹࣔ͢ɽಘΒΕͨ PSF ͷ FWHM

0.5

1.0

1.5

X (μm)

2.0 0.0

0.5

1.0

1.5

2.0

X (μm)

͸ 33 nm ͱͳΓɼFresnel-Kirchhoff ͷճંੵ෼ʹΑΓ‫ٻ‬Ίͨ஋ʢ35 nmʣͱ΄΅౳͍͜͠ͱΛ֬ೝͨ͠ɽ

Fig. 6. Scanning transmission images of a Siemens
star pattern. Yellow arrows indicate the scanningsequence.

110 nmँࣙ͜ͷ։ൃ͸ಠཱߦ੓๏ਓՊֶٕज़ৼ‫ߏػڵ‬ͷઌ୺‫ܭ‬33 nmଌ෼ੳٕज़ɾ‫ثػ‬։ൃࣄ‫ʹۀ‬ΑΔ੒ՌͰ͋Δɽຊ։ൃʹΑΔ੒Ռ͸ɼෳ਺ͷ࿦จͱͯ͠ެදࡁΈͰ͋Δ [5]ɽͦΕΒ͸ɼ՝୊൪߸ 2007B∼2010B3200 ͰߦΘΕ࣮ͨ‫ʹݧ‬ΑΔ੒ՌͰ͋Δɽࢀߟจ‫ݙ‬

Fig. 5. Measured LSF (black), tomographicallyreconstructed PSF (red), and PSF calculated using Fresnel-Kirchhoff diffraction integral (blue).

૸ࠪ‫ݦܕ‬ඍ‫ڸ‬੡࡞ͨ͠ MZP Λ૸ࠪ‫ݦܕ‬ඍ‫ʹڸ‬Ԡ༻ͨ͠ɽFig. 6͸ςετνϟʔτͷಁա‫͋Ͱ૾౓ڧ‬Δɽνϟʔτͷύλʔϯ͸ް͞ 500 nm ͷλϯλϧ੡Ͱɼ20 keV ʹ͓͚Δ‫ٵ‬ऩ཰͸Θ͔ͣ 5%Ͱ͋Δɽ̎࣍‫ࠪ૸ݩ‬ͷϐΫηϧ਺͸ 80×80 ͰɼϐΤκεςʔδͷεςοϓϐον
͕ 25 nmɼଌఆ࣌ؒ͸ 0.5 ඵ/ϐΫηϧͰ͋Δɽޫଋີ౓͸໿ 1.5×107 photons/s Ͱ͋ͬͨɽ૾͕࿪ΜͰΔ[1] D. Rudolph, B. Niemann, and G. Schmahl: Proc.
SPIE 316, 103 (1981).
[2] H. Takenaka, T. Kawamura, Y. Ishii, and S.
Asagiri: J. Appl. Phys. 78, 5227 (1995).
[3] J. Maser and G. Schmahl: Opt. Commun. 89,
355 (1992).
[4] G. Schneider: Appl. Phys. Lett. 71, 2242 (1997).
[5] T. Koyama et al., Rev. Sci. Instrum. 83, 013705(2012), T. Koyama et al., AIP Conf. Proc. 1365,
24-27 (2011), T. Koyama et al., AIP Conf.
Proc. 1365, 100-103 (2011), H. Takenaka etal., J. Phys.: Conf. Ser. 186, 012066 (2009),
T. Koyama et al., J. Phys.: Conf. Ser. 186,
012074 (2009), T. Koyama et al., Applied Physics
Express 1, 117003 (2008).

ͷ͸ɼଌఆதͷυϦϑτͷͨΊͰ͋ΔɽԖ௚ํ޲ͱਫ

– 56 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

2009A3202, 2009B3202, 2010A3202, 2010B3202,
2011A3202, 2011B3202

BL24XUߴฏߦ౓̭ઢϚΠΫϩϏʔϜͷ‫ܗ‬੒ͱͦͷԠ༻‫ڀݚ‬Formation and Application of Highly Parallel X-ray Microbeam௡ࡔ Ղ޾ 1 ɼҥּ ཅ‫ ش‬1 ɼߥҪ ඒஐࢠ 1 ɼᖒా ࠫ‫ ر‬1 ɼԼా ຑ༝ 1 ɼඌ্ ‫و‬༸ 1 ɼഷ ࿨ً 1 ɼ
ߴ໺ ल࿨ 1 ɼ࿜ౡ ༃ 1 ɼদҪ ७࣐ 2 ɼੴ઒ ༃ 3 ɼ࿨ా Ұ࣮ 3
Yoshiyuki Tsusaka1 , Haruki Kinugasa1 , Michiko Arai1 , Saki Sawada1 , Mayu Shimoda1 ,Takahiro Onoue1 , Kazuki Hazama1 , Hidekazu Takano1 , Yasushi Kagoshima1 ,Junji Matsui2 , Yasushi Ishikawa3 , Kazumi Wada3
1ฌ‫ཱݝݿ‬େֶେֶӃ෺࣭ཧֶ‫ڀݚ‬Պɼ2 ʢެࡒʣͻΐ͏͝Պֶٕज़‫ڠ‬ձɼ3 ౦‫ژ‬େֶେֶӃ޻ֶ‫ڀݚ‬Պ
1Graduate School of Material Science, University of Hyogo,
2
Hyogo Science and Technology Association,
3
Graduate School of Engineering, The University of Tokyo.

֓ཁɿɹ SPring-8 BL24XU ࣮‫ݧ‬ϋον B1 ʹ 3 छͷߴฏߦ౓̭ઢϚΠΫϩϏʔϜΛ‫ܗ‬੒ͨ͠ɽSi νϟϯωϧ
Χοτ݁থͱ̭ઢϛϥʔΛ૊Έ߹Θͤͯɼ΄΅ճં‫ݶ‬քʹୡͨ͠ϚΠΫϩϏʔϜΛ‫ܗ‬੒͢Δ͜ͱʹ੒ޭͨ͠ɽ
͜ͷϏʔϜΛ༻͍ɼϑΥτχΫε༻ͷγϦίϯ্ Ge ϝαʢ୆‫ߏܗ‬଄ʣ͓Αͼྊߏ଄γϦίϯͷ࿪ΈධՁΛߦͳͬͨɽγϦίϯ্ Ge ϝαͷଌఆͰ͸ɼGe ϝα͕γϦίϯ‫ج‬൘͔ΒͷҾͬுΓԠྗΛड͚ɼ໿ 0.17 %֨ࢠ
ऩॖ͍ͯ͠Δ͜ͱΛ໌Β͔ʹͨ͠ɽ͜Ε͸༗‫ݶ‬ཁૉ๏ʹΑΔγϛϡϨʔγϣϯ݁ՌͱΑ͘Ұக͍ͯ͠Δɽྊ
ߏ଄γϦίϯͷ࿪ଌఆͰ͸ɼྊ্Ͱ֨ࢠఆ਺͕΄΅ҰఆͰ͋Δ͜ͱΛ໌Β͔ʹͨ͠ɽ·ͨɼྊͷ෇͚͔ࠜΒ 8µm ্Ͱ͸֨ࢠ໘ִ͕ؒ 0.03 %ఔ౓ॖখ͍ͯ͠Δ͜ͱ͕൑໌ͨ͠ɽ͜ͷͱ͖ɼSi ͷόϯυΪϟοϓ΁ͷ‫د‬༩͸
–1.7×10−4 eV ఔ౓Ͱ͋ΔɽΩʔϫʔυɿɹ̭ઢϚΠΫϩϏʔϜɼ൒ಋମ݁থɼ࿪Έ‫ܭ‬ଌഎ‫ڀݚͱܠ‬໨తࢼྉͷಛੑʹैͬͯબ୒Ͱ͖ΔΑ͏४උͨ͠ɽ·ͨɼۙ೥ͷ൒ಋମσόΠεͷߏ଄͸ɼߴ‫ػ‬ೳԽɼߴूੵ
Խͷཁ‫ͱʹٻ‬΋ͳͬͯɼ‫ۃ‬Ίͯඍࡉ͔ͭෳࡶʹͳΓͭͭ͋Δɽ൒ಋମσόΠεͱͯ͠ྫ͑͹ɼγϦίϯ LSI
ʹ͓͚ΔઈԑບΤοδ΍ SOIʢSilicon-on-insulatorʣ΢ΣʔϋɼԽ߹෺൒ಋମΛ࢖ͬͨ LED ΍ LD ͳͲͷ൒ಋମσόΠεධՁ΁ͷԠ༻ͱͯ͠ Si ϑΥτχΫε
༻୯݁থͷ࿪ΈධՁΛߦͬͨɽ࣮‫ݧ‬̍ʣߴฏߦ౓̭ઢϚΠΫϩϏʔϜͷ‫ܗ‬੒ൃޫૉࢠɼ࿪Έ௒֨ࢠ΍ྔࢠҪ‫ށ‬ʢMQWʣΤϐλΩߴฏߦ౓̭ઢϚΠΫϩϏʔϜ͸ SPring-8 BL24XUγϟϧ૚Λ‫ؚ‬Ήޫूੵճ࿏ͳͲɼҙਤత͋Δ͍͸ඇҙ࣮‫ݧ‬ϋον B1 ʹ‫ܗ‬੒ͨ͠ɽߴฏߦ౓̭ઢϚΠΫϩϏʔਤతΛผʹͯ͠ɼ࿪Έͷ‫͕ࡏہ‬ૉࢠಛੑ΍݁থ੒௕ʹϜޫֶ‫ܥ‬Λ Fig. 1 ʹࣔ͢ [1]ɽӨ‫ڹ‬Λ༩͍͑ͯΔ΋ͷ͕গͳ͘ͳ͍ɽ͜ΕΒͷ‫ॴہ‬తೋ݁থ෼ޫ‫ʹث‬ΑΓ 15 keV ʹ୯৭Խ͞ΕͨΞϯδϡͳ࿪ΈΛߴਫ਼౓ʹଌఆ͢Δʹ͸ඍখྖҬߴਫ਼౓̭ઢճ

ϨʔλޫΛɼਫฏ 30 µm × Ԗ௚ 100 µm ͷεϦοτʹ

ં͕༗༻Ͱ͋ΓɼͦΕΛ࣮‫͢ݱ‬Δʹ͸ɼฏߦ౓ͷߴ͍Αͬͯ੔‫͢ܗ‬Δɽͦͷ‫ޙ‬ɼ(111) ද໘Λ࣋ͭ 2 ͭͷ Si

̭ઢϚΠΫϩϏʔϜ͕ඞཁͰ͋Δɽ

νϟϯωϧΧοτ݁থΛ༻͍ͯɼ4 ճͷ 333 ൓ࣹΛߦຊ՝୊Ͱ͸ɼϏʔϜαΠζ΍ൃࢄ֯ͷҟͳΔ 3 छͷ͍ɼ̭ઢϏʔϜͷΤωϧΪʔ෯Λ੍‫͢ݶ‬Δɽ͜ͷϏʔ̭ઢϚΠΫϩϏʔϜΛ੔උ͠ɼϢʔβʔ͸ɼͦΕͧΕϜΛਫฏํ޲ʹϕϯτͨ͠‫཰ۂ‬൒‫ ܘ‬4 mm ͷγϦϯ– 57 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)
Table 1. Characteristics of microbeams.
Concave curveture
Beam size (Hor.)

Beam 1

Beam 2

Beam 34 mm
0.9 µm8 mm
1.7 µm

35 µm

Beam size (Ver.)0.4 µm

0.7 µm

35 µm

Beam divergence (Hor.)
Emittance (Hor.ʣ

45 µrad0.41 Å

25 µrad0.43 Å

3.5 µrad1.23 Å

͍ͯΔɽޫϑΝΠό௨৴ʹ༻͍ΒΕΔޫͷΤωϧΪʔྖҬ͸ 0.95 eV ͓Αͼ 0.83 eV Ͱɼલऀ͕ 1.3 µm ଳɺ‫ ͕ऀޙ‬1.55 µm ଳͰ͋Δ͕ɼνοϓ಺ड৴‫ͯ͠ͱث‬Ge Λར༻͢Δ৔߹ɼͦͷ‫౓ײ‬ͷ೾௕ґଘੑ͕ॏཁͰ
͋ΔɽFig. 2 ʹ Ge ͷ࿪Έྔʹର͢Δ೾௕‫౓ײ‬ґଘੑΛࣔ͢ [2]ɽFig. 2 ͔Β෼͔ΔΑ͏ʹɼ1.55 µm ͷ೾௕ҬͰ͸ɼແ࿪Έͷ Ge ΑΓ 0.1 %Ҏ্ͷҾͬுΓ࿪

Fig. 1. Highly parallel X-ray microbeam optics.

͕ҹՃ͞Εͨ Ge ͷํ͕ߴ͍‫౓ײ‬Λ࣋ͭ͜ͱ͕෼͔Δɽ
ͦ͜Ͱɼ্ड़ͷϏʔϜ 2 Λ༻͍ͯɼγϦίϯ্ʹબ୒υϦΧϧϛϥʔͰαϯϓϧ্ʹूޫ͢Δɽϛϥʔ΁ͷࣼೖࣹ֯͸ 0.24◦ Ͱ͋ΓɼલஔεϦοτʹΑΓ੍‫͠ݶ‬੒௕͞Εͨ Ge ϝαͷ֨ࢠఆ਺ଌఆΛߦͬͨɽ̭ͨઢϏʔϜͷϛϥʔද໘্ͷরࣹྖҬ͸ 7 mm ×

0.1 mm ఔ౓ͷ‫͍ڱ‬ൣғͰ͋Δɽ͜ͷͨΊɼճసପԁ໘ϛϥʔͱͷ‫ܗ‬ঢ়ࠩ͸΄ͱΜͲͳ͍ɽಘΒΕͨϏʔϜͷαΠζ͸ 0.9 µm(ਫฏ) × 0.4 µm(Ԗ௚)ɼਫฏํ޲
ͷൃࢄ֯͸ 45 µrad Ͱ͋Δɽ·ͨϏʔϜͷ‫౓ڧ‬͸໿

106 cps Ͱ͋ΔʢϏʔϜ 1ʣɽ্‫ܥֶޫه‬ͷϛϥʔΛɼ‫཰ۂ‬൒‫ ܘ‬8 mm ͷϕϯτγϦϯυϦΧϧϛϥʔʹަ‫͢׵‬Δ͜ͱͰϏʔϜαΠ
ζ 1.7 µm(ਫฏ) × 0.7 µm(Ԗ௚)ɼਫฏํ޲ͷൃࢄ֯͸໿ 25 µrad ͷϏʔϜʢϏʔϜ 2ʣ͕ಘΒΕΔɽ͞ΒʹɼΑΓ݁থੑͷߴ͍ࢼྉଌఆ༻ʹɼूޫϛϥʔΛୀආ͠ɼαΠζ 35 µm(ਫฏ) × 35 µm(Ԗ௚)ɼਫฏํ޲

Fig. 2. Responsivity of strained Ge.

ͷൃࢄ֯ 3.5 µrad ͷϏʔϜʢϏʔϜ 3ʣ΋ར༻ՄೳͰ

͋Δɽ͜ΕΒɼ3 ͭͷϚΠΫϩϏʔϜͷಛੑΛ Table

1 ʹ·ͱΊΔɽϏʔϜ 1 ͱϏʔϜ 2 ͷਫฏํ޲ͷϏʔϜαΠζͱൃࢄ֯ͷੵ͸ 0.4 Å ఔ౓Ͱ͋Γɼ༻͍͍ͯΔ̭ઢͷ೾௕༻͍ͨࢼྉͷ໛ࣜਤΛ Fig. 3 ʹࣔ͢ɽγϦίϯ‫ج‬൘্ʹ SiO2 ϚεΫΛ‫ܗ‬੒͠ɼͦͷ‫ ޙ‬Ge ૚͕બ୒੒
௕͞Ε͍ͯΔɽ੒௕Թ౓͸ 600 ◦ C Ͱ͋Δɽ

ʢ0.827 ÅʣҎԼʹͳ͍ͬͯΔɽ͜Ε͸ɼ‫ޫʹط‬ͷճં‫ݶ‬քʹୡ͍ͯ͠Δ͜ͱΛҙຯ͠ɼ͜ΕҎ্ͷϏʔϜαΠζͱൃࢄ֯ͷॖখΛಉ࣌ʹୡ੒͢Δ͜ͱ͸‫ݪ‬ཧతʹෆՄೳͰ͋Δɽ̎ʣϑΥτχΫε༻γϦίϯ্ϝαͷ֨ࢠ࿪ΈධՁSi ϑΥτχΫε͸ɼνοϓ಺഑ઢΛޫ௨৴΁Ҡߦ͠ɼLSI ͷߴੑೳԽΛਤΔͨΊͷٕज़ͱͯ͠‫ظ‬଴͞Ε

– 58 –

Fig. 3. Area selective Ge layer on Si.

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

Fig. 4. Lattice parameter changes along (a) the long side and (b) short side of a rectangle.

Ge ૚ͷ֨ࢠఆ਺͸ɼ‫ࢠ֨ٯ‬ϚοϓଌఆΑΓ‫ٻ‬Ίͨɽ
Fig. 3 ͷ Ge ૚ʹରͯ͠ɼ୹खํ޲ɼ௕खํ޲ʹ̭

SOI ΢ΣʔϋͰɼ͘Γ͵͔Εͨ෦෼͸ Fig. 5 ʹࣔ͢Α͏ͳதۭͷྊঢ় Si ͷߏ଄Λ࣋ͭɽઢͷরࣹҐஔΛม͑ͳ͕Β‫ࢠ֨ٯ‬ϚοϓଌఆΛߦ͍ɼGe ૚ͷ֨ࢠఆ਺෼෍΋͋Θͤͯଌఆͨ͠ɽͦͷ݁Ռ
Λ Fig. 4 ʹࣔ͢ɽFig. 4 ͷ (a) ͸୹खํ޲ɼ(b) ͸௕खํ޲ʹԊͬͨ֨ࢠఆ਺ͷมԽͰ͋Δɽ·ͨɼࠇͷσʔλ఺͕ଌఆ͔Β‫ٻ‬Ίͨ֨ࢠఆ਺Ͱ͋Δɽ

Fig. 4 ͔Β Ge ͷ֨ࢠఆ਺͸ɼόϧΫ݁থͷͦΕͱൺ΂ͯখ͘͞ɼ͞Βʹɼ୺෦ʹൺ΂ͯத৺෦Ͱ͸ΑΓେ͖ͳ֨ࢠऩॖ͕‫͍ͯͬ͜ى‬Δ͜ͱ͕෼͔ͬͨɽ֨ࢠ

Fig. 5. Beam structure of Si.

ऩॖͷ࠷େ஋͸ Ge ͷόϧΫ݁থʹൺ΂ 0.171 %খ͍͞ɽ͜ͷ֨ࢠऩॖ͸ɼSi ͱ Ge ͷ೤๲ு܎਺ͷҧ͍͕ྊͷ௕͓͞Αͼ෯͸ɼ20 µmɼ5 µm Ͱ͋Γɼྊʹ‫ݪ‬ҼͰ͋ΔɽSi ‫ج‬൘্ʹ Ge ΛΤϐλΩγϟϧ੒௕͞ྗΛՃ͑Δ͜ͱͰ Si ʹ࿪ΈΛՃ͑Δ͜ͱ͕ՄೳͰ͋

ͤɼ݁থ੒௕࣌ͷߴԹ͔ΒࣨԹʹྫྷ٫͢ΔաఔͰɼGe

Δ͕ɼࠓճ͸ҙਤతͳ࿪Έ͸Ճ͍͑ͯͳ͍ɽ͜ͷྊߏʹ͸ҾͬுΓԠྗ͕ੜ͡ɼ<001> ํ޲ͷ݁থऩॖ͕

଄ Si ʹ̭ઢΛরࣹ͠ɼϩοΩϯάΧʔϒଌఆͱ‫ࢠ֨ٯ‬‫͜ى‬ΔɽFig. 4 ͷ੺ͷσʔλ఺͸ɼ༗‫ݶ‬ཁૉ๏Λ༻͍ϚοϐϯάʹΑΓ݁থੑ͓Αͼ֨ࢠఆ਺Λଌఆͨ͠ɽ

ͨγϛϡϨʔγϣϯ݁ՌͰ͋Γɼଌఆ஋ͱΑ͘Ұக̭͠ઢͷরࣹҐஔΛม͑ͳ͕ΒɼϩοΩϯάΧʔϒଌఆΛߦͬͨͱ͜Ζɼྊͷ෇͚ࠜۙ๣਺ µm Ͱ SOI ૚͕͍ͯΔ [3]ɽ

Ԝತߏ଄Λͱ͍ͬͯΔ͜ͱ͕൑໌ͨ͠ɽSOI ΢Σʔϋ̏ʣϑΥτχΫε༻ྊߏ଄γϦίϯͷ࿪ΈධՁϑΥτχΫε༻ड৴‫ث‬ͷผͷީิͱͯ͠ɼྊߏ଄
γϦίϯͷ֨ࢠఆ਺ධՁ΋ߦͬͨɽSi ‫ݻ‬༗ͷόϯυΪϟοϓ͸ 1.11 eV Ͱɼ௨৴ʹ༻͍ΒΕΔ೾௕ଳͷޫʹ͸‫౓ײ‬Λ΋ͨͳ͍ɽ͜ͷ໰୊͸ɼSi ݁থʹ࿪ΈΛ෇Ճ͢Δ͜ͱͰରԠͰ͖ΔՄೳੑ͕͋ΔɽͦΕʹ͸ɼडޫૉࢠ༻࿪Έ Si ͷ࿪Έ੍‫͕ޚ‬ॏཁͰ͋Δɽ
ͦ͜Ͱɼ্ड़ͷϏʔϜ 1 Λ༻͍ͯɼϑΥτχΫε༻ྊߏ଄γϦίϯͷ࿪ΈධՁΛߦͬͨɽ༻͍ͨࢼྉ͸ɼ

SOI ૚ͱ SiO2 ૚͕ίͷࣈͷύλʔϯͰ͘Γ͵͔Εͨ࡞੡ͷ޻ఔͰ Si ͱ SiO2 ͱͷ೤๲ு܎਺ͷҧ͍͔Βɼ

SOI ૚Ͱ͸֨ࢠऩॖ͕ੜ͡Δ͜ͱ͕஌ΒΕ͍ͯΔɽͦ͜΁ύλʔϯΛඳ͘͜ͱʹΑΓɼྊͷ෇্͚ࠜ෦Ͱ‫ہ‬ॴతͳ֨ࢠ໘܏͕ࣼੜͨ͡ͱߟ͑ΒΕΔɽ
·ͨɼরࣹҐஔΛม͑ͳ͕Β‫ࢠ֨ٯ‬ϚοϐϯάΛߦ͍ɼ<004> ํ޲ͷ֨ࢠఆ਺ͷมԽΛଌఆͨ͠ɽTable 2ʹ‫ࢠ֨ٯ‬Ϛοϓଌఆ͔Β‫ٻ‬Ίͨ֨ࢠఆ਺ͷ݁ՌΛࣔ͢ɽྊ্Ͱͷ֨ࢠ໘ִؒ͸΄΅ҰఆͰ͋Δ͕ɼྊͷ෇͚͔ࠜΒ 8 µm ্Ͱ͸֨ࢠ໘ִ͕ؒ 0.03 % ఔ౓ॖখ͠

– 59 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)͕ɼ̭ઢϛϥʔΛ༻͍ͳ͍৔߹͸ɼճં‫ݶ‬քʹୡͯ͠

Table 2. Results of lattice parameter measurements.
Distance from the baseof Si beam

Lattice parameter+37 µm

1.35785 [Å]

+8 µm
+1 µm

1.35725 [Å]
1.35773 [Å]

01.35774 [Å]

-2 µm

1.35791 [Å]

-3 µm

1.35789 [Å]

-8 µm
-13 µm

1.35786 [Å]
1.35790 [Å]͓Βͣɼ͞ΒͳΔ޻෉ͷ༨஍͕͋ΔͱࢥΘΕΔɽ
‫ܗ‬੒ͨ͠ϚΠΫϩϏʔϜΛ༻͍ͯɼϑΥτχΫε༻ͷγϦίϯ্ Ge ϝα͓Αͼྊߏ଄γϦίϯͷ࿪ΈධՁΛߦͬͨɽࠓճͷଌఆͰɼे෼ͳҐஔ෼ղೳͰ Ge
͓Αͼ Si ͷ֨ࢠఆ਺͕ଌఆͰ͖Δ͜ͱ͕෼͔ͬͨɽࠓ
‫ޙ‬ɼҙਤతͳ࿪ΈΛҹՃͨ͠ྊߏ଄γϦίϯ΍ͦͷଞͷϑΥτχΫεࢼྉͷ֨ࢠఆ਺ଌఆ͓Αͼ࿪ΈଌఆΛߦ͏༧ఆͰ͋Δɽࢀߟจ‫ݙ‬

͍ͯΔ͜ͱ͕൑໌ͨ͠ɽ͜ͷͱ͖ɼόϯυΪϟοϓ΁
ͷ‫د‬༩͸ −1.7×10−4 eV ఔ౓Ͱ͋Δɽࠓ‫ޙ‬ͷ՝୊

SPring-8 BL24XU ࣮‫ݧ‬ϋον B1 ʹ 3 छͷߴฏߦ౓̭ઢϚΠΫϩϏʔϜΛ‫ܗ‬੒ͨ͠ɽ͜ͷ͏ͪɼ̭ઢϛ[1] S. Takeda, K. Yokoyama, Y. Tsusaka, and Y.
Kagoshima, J. Matsui, and A. Ogura: J. Synchrotron Rad. 13, 373 (2006).
[2] Y. Ishikawa, K. Wada, J. Liu, D. Cannon, H.
Luan, J. Michel, and L. Kimerling: J. Appl.
Phys. 98, 013501 (2005).
[3] Y. Tsusaka, H. Takano, K. Kagoshima, J.
Matsui, S. Park, Y. Ishikawa, and K. Wada:
Diamond Light Source Proceedings 1/SRMS-7,
e117 (2010).

ϥʔΛ༻͍ͨϚΠΫϩϏʔϜ͸΄΅ճં‫ݶ‬քʹୡͨ͠– 60 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

2009A3203, 2009B3203, 2010A3203, 2010B3203,
2011A3203, 2011B3203

BL24XU

BL24XU ʹ͓͚ΔϚΠΫϩϏʔϜɼϚΠΫϩΠϝʔδϯάͷߴ౓ԽDevelopment of X-ray Microfocusing and Microimaging Station
at BL24XUߴ໺ ल࿨
Hidekazu Takanoฌ‫ཱݝݿ‬େֶେֶӃ෺࣭ཧֶ‫ڀݚ‬ՊGraduate School of Material Science, University of Hyogo֓ཁɿɹ BL24XU ͷ B2 ϋονʹ͓͍ͯల։͞Ε͍ͯΔϚΠΫϩϏʔϜٕज़ɼϚΠΫϩΠϝʔδϯάٕज़ͷߴ౓Խ‫͍ͯͭʹڀݚ‬ใࠂ͢Δɽ࣮‫ݧ‬՝୊͸ฌ‫ཱݝݿ‬େֶ̭ઢޫֶߨ࠲ʹΑΔֶज़‫ͳߦͯ͠ͱڀݚ‬ΘΕ͓ͯΓɼؔ࿈͢Δ͞·͟·ͳ࣮‫ݧ‬Λߦ͍ͬͯΔɽ͜ΕΒʹΑΔٕज़։ൃ͸Ϣʔβʔར༻ޫֶ‫ܥ‬ͷߴ౓Խʹ΋ີ઀ʹ͔͔Θ͍ͬͯΔɽຊߘͰ͸͍͔ͭ͘ͷτϐοΫεʹ͍ͭͯɼಘΒΕͨ੒Ռͷ঺հΛߦ͏ɽΩʔϫʔυɿɹ X-ray focusing, X-ray microscopy, X-ray tomography, Phase contrast imaging

എ‫ڀݚͱܠ‬໨త̍ʣ৽‫̭ن‬ઢޫֶૉࢠͷ։ൃBL24XU ͷ B ϒϥϯνͰ͸ɼϚΠΫϩϏʔϜར༻ʹಛԽͨ͠εςʔγϣϯͷߏங͓Αͼӡ༻Λߦ͍̭ͬͯઢΛूޫ·ͨ͸ޫֶ݁૾͢Δ‫ػ‬ೳΛ࣋ͭޫֶૉ
ࢠ͸ɼߴۭؒ෼ղೳΠϝʔδϯάʹ͓͍ͯඇৗʹॏ
ཁͰ͋Δɽ‫ࡏݱ‬ɼߗ̭ઢྖҬʹ͓͚ΔूޫαΠζͷ࠷ΔɽதͰ΋্ྲྀଆͷϋονͰ͋Δޫֶϋον B2ʢҎԼখ஋͸ 7 nm ʹୡ͓ͯ͠Γ [1]ɼ͞ΒͳΔඍখԽʹ޲

ϋον B2ʣ͸ɼࢼྉͷߴۭؒ෼ղೳ‫࡯؍‬Λ໨తͱͯ͠

͚༷ͯʑͳޫֶૉࢠ͕ఏҊɼ։ൃ͞Ε͍ͯΔɽΘΕΘ͓ΓɼϚΠΫϩϏʔϜ͚ͩͰͳ͘ϚΠΫϩΠϝʔδϯΕ͸ɼ‫ط‬ଘͷޫֶૉࢠʹൺ΂ͯ࡞੡͕༰қ͔ͭɼφϊάʹ͍ͭͯͷ૷ஔల։Λߦ͍ͬͯΔɽ͜ΕΒͷ૷ஔ։ϝʔλʔΦʔμʔͷूޫ͕‫ݪ‬ཧతʹՄೳͳ৽͍̭͠

ൃʹ͓͚Δཁૉٕज़ͱͯ͠ɼ̭ઢޫֶૉࢠ։ൃɼ̭ઢ
ཱ֬͞Ε͍ͯΔٕज़Ͱ͸ͳ͍ͨΊʹ‫ۃ‬Ίͯઐ໳ੑ͕ߴ

ઢूޫૉࢠ։ൃͰ͋Δɼશ൓ࣹκʔϯϓϨʔτ (Total
reflection zone plate: TRZP) ͷ։ൃΛߦ͍ͬͯΔ [2]ɽTRZP ͸ Fig. 1(a) ͷΑ͏ʹɼฏ໘‫ج‬൘ʹ൓ࣹ‫ܕ‬ෆ౳͍ɽΘΕΘΕฌ‫ཱݝݿ‬େֶ̭ઢޫֶߨ࠲͸ɼ͜ΕΒͷִؒճં֨ࢠΛඳըͨ͠΋ͷͰ͋Γɼ̭ઢΛࣼೖࣹ͢ཁૉٕज़։ൃΛֶज़‫͓ͯͬߦͯ͠ͱڀݚ‬Γੈքతʹ΋

Δ͜ͱͰ‫্͚͔ݟ‬ͷ֨ࢠִ͕ؒখ͘͞ͳΔޮՌΛར༻ߴ͍ਫ४ͷٕज़Λ༗͍ͯ͠Δɽ·ͨຊߨ࠲Ͱ͸ɼϋο͢Δ͜ͱͰɼඳըαΠζʹൺ΂ͯඇৗʹখ͍͞ूޫαूޫධՁɼޫֶ‫ܥ‬ධՁ͕ඇৗʹॏཁͰ͋Δ͕ɼे෼ʹν B2 ʹ͓͚Δεςʔγϣϯ؅ཧɼӡӦʹ͍ͭͯओମ

ΠζΛՄೳʹ͢Δɽ௨ৗͷϦιάϥϑΟٕज़Λ༻͍ͯతʹ‫ܞ‬Θ͓ͬͯΓɼϢʔβʔར༻ޫֶ‫ܥ‬ͷ४උɼ࣮‫ݧ‬αϙʔτΛߦ͍ͬͯΔɽٕज़૬ஊ౳ʹΑΓϢʔβʔͷཁ๬ʹରͯ͠ཁૉٕज़ΛԠ༻ͨ͠ιϦϡʔγϣϯͷఏҊ͕Ͱ͖ΔͨΊɼϢʔβʔར༻ޫֶ‫ܥ‬΍ଌఆํ๏΁ͷཁૉٕज़ͷ௚઀తͳϑΟʔυόοΫΛՄೳͱ͍ͯ͠ΔɽຊߘͰ͸ɼ2011B ‫ֶ͖ͨͯͬߦʹͰ·ظ‬ज़‫͓ڀݚ‬ΑͼϢʔβʔར༻ޫֶ‫ܥ‬։ൃͷ͏ͪɼҎԼͷτϐοΫεʹ
͍ͭͯ঺հ͢Δɽ

Fig. 1. Schematic drawing of the TRZPs. (a) linear
focusing type, (b) point focusing type.

– 61 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)࡞੡ՄೳͰ͋Δʹ΋͔͔ΘΒͣɼଟ૚ບඇ‫ٿ‬໘‫ڸ‬ɼϥར༻͢ΔͨΊɼߴ଎౓ΧϝϥΛ૊Έ߹Θͤͨ X ઢը΢ΤϨϯζͷΑ͏ͳ࣍ੈ୅‫̭ܕ‬ઢޫֶૉࢠͱಉ౳ͷ૾‫ݕ‬ग़‫ث‬Λ։ൃ͠ɼߴ଎Ͱ CT ଌఆ͕Մೳͳޫֶ‫ܥ‬ͷߴ͍ཧ࿦ूޫੑೳΛ༗͢Δɽ·ͨɼFig. 1(b) ͷΑ͏ߏஙΛߦ͍ͬͯΔ [3]ɽ࣌‫ྻܥ‬ͷ࿈ଓଌఆ͕ՄೳͰ͋

ͳԁਲ਼‫ج‬൘Λ༻͍Δ͜ͱʹΑΓɼ̎࣍‫͕ޫूݩ‬ՄೳͱΓɼैདྷͷ̏࣍‫ۭؒݩ‬৘ใʹ࣌ؒͷ࣍‫ݩ‬Λ෇༩ͨ͠ɼͳΔɽ̐࣍‫ ݩ‬CT ͷଌఆ͕ՄೳͱͳΔɽࢼྉͷಈతมԽΛଊ
͑Δ͜ͱ͕Ͱ͖ɼՃ೤΍ྫྷ٫ɼԠྗҹՃ౳ͷ in-situ̎) ϚΠΫϩϏʔϜԠ༻ޫֶ‫ܥ‬ͷ։ൃ̭ઢूޫϏʔϜΛࢼྉʹরࣹ͠ɼࢼྉΛ૸ࠪ͢Δ͜ଌఆ΁ͷԠ༻͕ՄೳͰ͋ΔɽͱͰߴҐஔ෼ղೳͰͷϚοϐϯάଌఆ͕Ͱ͖Δɽࢼྉ͔Β͸༷ʑͳ৴߸͕ಘΒΕΔͨΊɼͦΕΒΛར༻͢Δ࣮‫ݧ‬͜ͱͰଟ‫ݩ‬తͳଌఆ͕ՄೳͱͳΔɽ

ϒϥϯν B Ͱ͸ɼγϦίϯਫฏΦϑηοτͷೋ݁থ‫ࡏݱ‬ɼϢʔβʔར༻ޫֶ‫ͯ͠ͱܥ‬ɼ޿֯ճં (Wide෼ޫ‫ث‬Λ༗͓ͯ͠Γɼ୯৭̭ઢΛ࢖༻Ͱ͖Δɽͨͩ͠ɼ

angle x-ray diffraction: WAXD) ͓Αͼ‫ޫܬ‬෼ੳ (X-ޫ‫ݯ‬Λϒϥϯν A ͱ‫͍ͯ͠༻ڞ‬ΔͨΊΞϯδϡϨʔray fluorescence analysis: XRF) ଌఆ͕ՄೳͰ͋Δɽλʔͷఆ֨Ϊϟοϓ஋Λ 11.3 mm ʹ‫ݻ‬ఆ͍ͯ͠Δɽ͜

WAXD ଌఆͰ͸ɼ಺෦Ԡྗɼ݁থԽ౓౳ʹ͍ͭͯ‫ॴہ‬ͷͱ͖ɼ‫ج‬ຊ೾ͷΤωϧΪʔ͸ 10 keV Ͱ͋Δ͕ɼ̔ͷతʹධՁ͢Δ͜ͱ͕Ͱ͖ɼXRF Ͱ͸ࢼྉͷ‫ݩ‬ૉ૊੒ͷࣈΞϯδϡϨʔλʔ༝དྷͷ൒੔਺࣍ͷߴ࣍ߴௐ೾Λ࢖Πϝʔδϯάଌఆ͕Ͱ͖ΔɽWAXD ଌఆʹϑϥοτ

༻Ͱ͖ΔͨΊɼ5ʙ35 keV ͷΤωϧΪʔൣғͰ 5 keVύωϧ‫ݕ‬ग़‫( ث‬FPD) Λ༻͍Δ͜ͱͰɼWAXDɼXRF

ຖͷ X ઢΤωϧΪʔΛ೚ҙʹར༻Ͱ͖Δɽ·ͨɼϋοΛಉ࣌ʹଌఆ͢Δ͜ͱ΋Մೳͱͳ͍ͬͯΔɽν B2 Ͱ͸෼ޫ‫ث‬Λୀආͤ͞Δ͜ͱʹΑΓɼ‫ͳྗڧ‬Ξ·ͨɼ৽͍͠Πϝʔδϯάޫֶ‫ܕࠪ૸ͯ͠ͱܥ‬ඍ෼ϯδϡϨʔλʔ์ࣹΛ௚઀࢖༻Ͱ͖ΔϞʔυ͕͋ΔɽҐ૬‫ݦ‬ඍ‫( ܥֶޫڸ‬Differential phase contrast: DPC)ϋον಺ͷεςʔγϣϯߏ੒͸ɼ্ྲྀΑΓ̭ઢ‫ٵ‬ऩ୺ͷ੔උΛߦͬͨɽඇৗʹ؆୯ͳηοτΞοϓͷޫֶ‫ܥ‬ඍࡉߏ଄෼ੳ (X-ray absorption edge fine structureΛߟҊ͠ɼैདྷͷޫֶ‫ʹܥ‬૊ΈࠐΜͰ࢖༻Ͱ͖ΔͨΊɼanalysis: XAFS) εςʔγϣϯɼଟ໨తεςʔγϣϯɼ

XRF ͱͷಉ࣌ଌఆ΍ɼΦϑηοτʢճં֯ʹରͯ͠ʣϚΠΫϩϏʔϜԠ༻εςʔγϣϯͱͳ͍ͬͯΔɽޫֶ

৚݅Ͱ͋Ε͹ WAXD ͱ΋ಉ࣌ଌఆ͕ՄೳͰ͋Δɽ

ૉࢠධՁɼ৽‫ܥֶޫن‬ͷςετ։ൃ౳ͷઌਐੑͷߴ͍̭ઢͷҐ૬มԽΛར༻͢Δ͜ͱͰɼ‫ٵ‬ऩࠩͷগͳֶ͍ज़‫͓ڀݚ‬Αͼɼߴۭؒ෼ղೳ CTɼ̐࣍‫ ݩ‬CT ͳͲࢼྉΛߴίϯτϥετͰ‫͢࡯؍‬Δ͜ͱ͕Ͱ͖ΔͨΊɼͷΠϝʔδϯά๏։ൃɼϢʔβʔར༻ͷޫֶ‫͍ͭʹܥ‬ܰ‫ݩ‬ૉࢼྉ΍ബ൘ࢼྉͷΠϝʔδϯά΍ҐஔϞχλʔͯ͸ଟ໨తεςʔγϣϯʹεΫϥοϓ&ϏϧυͰߏஙͱͯ͠ར༻Ͱ͖Δɽ͞ΒʹɼࢼྉΛճసͯ͠૸ࠪΛߦ͞ΕɼूޫϏʔϜΛ༻͍ͨ WAXDɼXRF ౳ͷԠ༻ޫ͏͜ͱͰɼࢼྉஅ໘ͷ۶ં཰෼෍͕ಘΒΕΔҐ૬τϞֶ‫ܥ‬͸ɼ൚༻ϚΠΫϩϏʔϜεςʔγϣϯʹৗઃ͞ΕάϥϑΟଌఆ΁ͷԠ༻͕ՄೳͰ͋Γɼ௨ৗͷ‫ٵ‬ऩ๏Ͱ

͍ͯΔɽͨͩ͠ɼϢʔβʔʹΑͬͯΤωϧΪʔɼϏʔ͸‫ࠔ͕࡯؍‬೉ͳࢼྉͷ಺෦ߏ଄ΛඇഁյͰಘΔ͜ͱ͕

ϜαΠζɼൃࢄ֯౳ͷϏʔϜύϥϝʔλʔ΍ɼଌఆࢼͰ͖Δɽ

ྉ͕ҟͳΔͨΊɼϢʔβʔ͝ͱʹޫֶ‫ܥ‬ͷௐ੔Λߦ͏ɽ̏ʣߴۭؒ෼ղϚΠΫϩτϞάϥϑΟ͓Αͼ̐࣍‫ݩ‬τ̍ʣTRZP ͷूޫαΠζධՁϞάϥϑΟ๏ͷ։ൃฏ໘‫ج‬൘Λ༻͍ͨ̍࣍‫ ܕޫूݩ‬TRZP ʹ͍ͭͯू̭ઢ‫ػࢉܭ‬τϞάϥϑΟ(CT) ๏͸ɼ෺ମ಺෦ߏ଄

ޫαΠζධՁ࣮‫ݧ‬ΛߦͬͨɽTRZP ͸ɼγϦίϯ‫ج‬൘ΛඇഁյͰ‫͢࡯؍‬Δख๏Ͱ͋Γɼҩྍ਍அͷΈͳΒ্ͣʹ‫ܗ‬੒͞Εͨް͞ 10 nm ͷനۚͷෆ౳ִؒ֨ࢠͰ

͞·͟·ͳ෼໺Ͱར༻͞Ε͍ͯΔɽ์ࣹޫΛར༻ͨ͋͠ΓɼిࢠઢϦιάϥϑΟʹΑΓ࡞੡ͨ͠ɽ֨ࢠͷ࠷CT ͸ɼߴ͍ۭؒ෼ղೳ͕ಘΒΕΔ͚ͩͰͳ͘ɼ۶ં

খઢ෯͸ 700 nmɼκʔϯ਺͸ 1000 Ͱ͋Γɼ10 keVίϯτϥετͷར༻ʹΑΓߴ͍ີ౓෼ղೳ͕ಘΒΕͷ X ઢΛࣼೖࣹ֯ 6 mrad Ͱೖࣹͨ͠ͱ͖ʹɼ࠷খઢΔɽΘΕΘΕ͸ߴ෼ղೳγϯνϨʔλʔΛ༻͍ͨՄࢹ

෯ͷκʔϯҐஔΑΓ 1.72 mm Լྲྀʹ͓͍ͯɼനۚύޫม‫ ܕ׵‬X ઢը૾‫ݕ‬ग़‫ث‬Λ։ൃ͠ɼߴ෼ղೳ CT ޫֶλʔϯ͔Βͷ൓ࣹճંޫ͕ूޫ͢ΔΑ͏ʹઃ‫ͨ͠ܭ‬ɽ‫ܥ‬Λߏஙɼӡ༻͍ͯ͠Δɽ͞Βʹɼ์ࣹޫͷେ‫౓ڧ‬Λ͜ͷͱ͖ͷޫֶ‫ܥ‬ͷ։‫਺ޱ‬ΑΓܾ·ΔϨʔϦʔ‫ݶ‬ք– 62 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू
͸ 13 nm Ͱ͋ΔɽूޫαΠζ͸҉ࢹ໺φΠϑΤοδં‫ܭ‬ʢਫฏํ޲ʣʹઃஔ͞Ε͓ͯΓɼΧ΢ϯλʔΛ༻εΩϟϯ๏ʹΑͬͯଌఆ͞ΕͨɽφΠϑΤοδ͔Βͷ͍ͨଌఆ΋ՄೳͰ͋ΔɽDPC ଌఆͰ͸‫ݕ౓ڧ‬ग़‫ث‬ΛΤοδճંޫͷΈΛ‫ݕ‬ग़͢Δ͜ͱʹΑΓɼߴ͍ۭؒ‫ײ‬̎ͭ༻͍ɼҰͭΛࢼྉಁաޫʢΠΦϯνΣϯόʔͳͲ౓Ͱઢ૾෼෍ؔ਺͕ಘΒΕΔ [4]ɽφΠϑΤοδʹ͸ͷಁա‫ݕܕ‬ग़‫ث‬ʣɼ΋͏Ұͭ͸ࢼྉಁաޫΛ൒෼ःณ௚‫ ܘ‬300 µm ͷനۚϫΠϠʔΛ࢖༻͠ɼ੩ి༰ྔมҐͯ͠‫ݕ‬ग़͢Δɽ͜ΕΒΛར༻͢ΔͱɼࢼྉʹΑΔ۶ં‫ܭ‬Λ಺ଂͨ͠Ϋϩʔζ੍‫ޚ‬ͷώΤκεςʔδʹΑΓ‫ۦ‬ͷมԽΛ‫౓ڧ‬มԽʹม‫͖Ͱ׵‬ΔͨΊɼࢼྉͰͷҐ૬มಈͨ͠ɽεςʔδͷ‫ۦ‬ಈਫ਼౓͸ 1.7 nm Ͱ͋ͬͨɽ

ԽͷҐஔඍ෼৘ใ͕நग़Ͱ͖Δɽඍ෼Ґ૬Λੵࢉ͢Δ
͜ͱͰҐ૬ίϯτϥετ૾͕ಘΒΕΔɽ

̎ʣϚΠΫϩϏʔϜԠ༻ޫֶ‫ܥ‬൚༻ͷϚΠΫϩϏʔϜޫֶ‫Ͱܥ‬͸ɼ̭ઢͷूޫʹϑ̏ʣߴۭؒ෼ղೳ CT ͓Αͼ 4 ࣍‫ ݩ‬CT ޫֶ‫ܥ‬ϨωϧκʔϯϓϨʔτʢFZPʣΛ༻͍͍ͯΔɽ‫ج‬ຊతߴۭؒ෼ղ CT ͸ɼYAG ୯݁থγϯνϨʔλʔͱ

ʹ 3 छྨɼ࠷େ 8 छྨͷ FZP Λޫֶ‫ܥ‬΍ࢼྉʹԠ͡ྫྷ٫ CCD ΧϝϥΛར༻ͨ͠ը૾‫ݕ‬ग़‫ث‬Λ༻͍ΔɽϦͯબ୒ՄೳͰ͋ΔɽूޫαΠζ͸࠷খ 100 nmɼϏʔϨʔޫֶ‫ʹܥ‬͸ޫֶ‫ݦ‬ඍ‫༻ڸ‬ର෺ϨϯζΛ࢖༻͠ɼ20Ϝൃࢄ֯͸ 0.05ʙ2.5 mrad Ͱ೚ҙʹઃఆՄೳͰ͋Δɽഒʹ͓͍࣮ͯޮըૉαΠζ͸ 0.68 µm ͱͳΔɽ௨ৗϏʔϜ‫౓ڧ‬͸ɼαΠζɼൃࢄ֯ͱτϨʔυΦϑͱͳΓɼͷଌఆʢ1200 ౤Өʣʹཁ͢Δଌఆ࣌ؒ͸ 40 ෼ఔ౓Ͱ࠷େͰ 1011 ޫࢠຖඵఔ౓͕ՄೳͰ͋Δʢ͜ͷͱ͖ͷ͋ΔɽϏʔϜαΠζ͸ 3 µm × 10 µmʣɽFZP Ͱ͸ूޫϏʔ

4 ࣍‫ ݩ‬CT ޫֶ‫Ͱܥ‬͸ɼൃޫ‫ݮ‬ਰͷૣ͍ P46 ค຤ϜҎ֎ͷޫΛ཈੍͢ΔͨΊʹϐϯϗʔϧ͕ඞཁͰ͋

‫ޫܬ‬ମͱ CMOS ϕʔεͷߴ଎౓ΧϝϥΛ૊Έ߹ΘͤΓɼ͜ͷͨΊʹࢼྉपΓͷ࡞ಈ௕͕਺ mm ʹ੍‫͞ݶ‬ΔɽϦϨʔޫֶ‫ܥ‬͸ɼऔΓࠐΈޮ཰ͷߴ͍ΧϝϥϨϯ

ΕΔɽͳ͓ɼΞϯδϡϨʔλʔͷߴ࣍ߴௐ೾ʹΑΔߴζ‫ܥ‬Λ࢖༻͠ɼ࣮ޮըૉαΠζΛ 3ʙ5 µm ʹઃఆ͢ΤωϧΪʔ੒෼͸ FZP ্ྲྀͷશ൓ࣹϛϥʔʹΑͬͯ

Δɽ͜ͷͱ͖ɼߴ଎౓Χϝϥʹ͓͍ͯ 1500ʙ6000 ϑΧοτ͞ΕΔɽଌఆޫֶ‫ܥ‬ͷ֓ཁΛ Fig. 2 ʹࣔ͢ɽϨʵϜຖඵͰͷࡱӨ͕ՄೳͱͳΔɽࢼྉΛߴ଎ʹճస
ʢ࠷଎ 17.3 ճసຖඵʣͤ͞ɼ࿈ଓը૾औಘΛߦ͏͜ͱͰ࣌‫ྻܥ‬ͷ CT ଌఆ͕ߦΘΕΔɽCT ޫֶ‫͚͓ʹܥ‬Δ࠷େࢹ໺ͷαΠζ͸ೖࣹϏʔϜʹΑܾͬͯ·͓ͬͯΓɼ
ॎ 1.2 mmɼԣ 1.7 mm Ͱ͋Δɽ݁Ռ͓Αͼߟ࡯
্ड़ͷ࣮‫Ͱݧ‬ಘΒΕͨ݁Ռʹ͍ͭͯ঺հΛߦ͏ɽҎԼ͸͢΂ͯ 10 keV ͷ̭ઢʢ݁থ෼ޫ‫ʹث‬ΑΔ୯৭ޫʣΛ࢖༻ͨ͠ɽ
̍ʣTRZP ͷूޫαΠζධՁFig. 2. Schematic diagram of a measurement systemusing an X-ray focusing beam.

Fig. 3(a) ʹ̍࣍‫ ܕޫूݩ‬TRZP ͷूޫαΠζධՁ݁ՌΛࣔ͢ [5]ɽϝΠϯϐʔΫͷ൒஋શ෯͸ 14.4 nmͰ͋Γɼ͢΂ͯͷκʔϯʹ͍ͭͯϑϨωϧɾΩϧώϗࢼྉ͔Βͷ‫̭ޫܬ‬ઢɼࢄཚ̭ઢ͸γϦίϯυϦϑ
τ‫ݕ‬ग़‫ʹث‬Αͬͯ‫ݕ‬ग़͞ΕɼϚϧννϟϯωϧ෼ੳ‫ث‬
ʢMCAʣͰหผ͞ΕΔɽ૸ࠪ఺͝ͱʹ MCA ͰಘΒΕΔεϖΫτϧΛऔಘ͢ΔଌఆϞʔυΛ༻͍Ε͹ɼྭ‫ى‬Մೳͳશ‫ݩ‬ૉϚοϐϯάଌఆ͕ՄೳͰ͋Δɽࢼྉ͔Βϑճંੵ෼ͨ͠‫݁ࢉܭ‬Ռʢ੺ઢʣͱ΄΅Ұகͨ͠ɽϝΠϯϐʔΫ͸΄΅ճં‫ݶ‬քͷूޫαΠζΛ͍ࣔͯ͠Δ
͕ɼ͍͔ͭ͘ͷαΠυϐʔΫʹύϫʔ͕෼ࢄ͞Ε͍ͯ
Δɽඳը͞ΕͨκʔϯͷҐஔ‫ࠩޡ‬͸‫ڐ‬༰಺Ͱ͋ΔͨΊɼ‫ج‬൘ͷฏୱ౓ʹ‫ى‬Ҽ͍ͯ͠Δ΋ͷͱߟ͍͑ͯΔɽͷճંઢ͸ FPD Ͱ‫ݕ‬ग़͞Εɼ2θ Ͱ࠷େ 30 ౓ఔ౓ͷશपଌఆ͕ՄೳͰ͋Δɽߴ֯౓෼ղೳଌఆʹ͸ΠϝʔδϯάϓϨʔτ΋ར༻Ͱ͖Δɽ·ͨɼࢼྉ͸ θ–2θ ճ

1 ࣍‫ ܕݩ‬TRZP ͱಉ͡ύϥϝʔλʔΛ΋ͭκʔϯΛԁਲ਼‫ج‬൘ʹඳըͨ̎࣍͠‫ ܕޫूݩ‬TRZP ʹ͍ͭͯɼूޫ఺ͷ‫ࢉܭ‬Λͨ͠΋ͷΛ Fig. 3(b) ʹࣔ͢ [6]ɽ͜

– 63 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

Fig. 3. (a) An experimental focusing result of a linear focusing type TRZP. (b) A focusing calculation resultof a point focusing type TRZP.

ͷͱ͖ɼԁਲ਼ͷ‫཰ۂ‬൒‫ܘ‬͸κʔϯͷ্ྲྀଆͰ 50 µmɼ

4(a) Ͱ͸ΩϡʔςΟΫϧߏ଄༝དྷͷࢄཚ͕খ֯ྖҬʹԼྲྀଆͰ 35 µm Ͱ͋ΔͨΊɼ࡞੡Λߟྀͯ͠։์‫ܕ‬‫ݟ‬ΒΕɼFig. 4(c) Ͱ͸ɼໟ൅த৺෦ͷϝσϡϥྖҬͷԁਲ਼‫ج‬൘Λ૝ఆ͠ɼಈ‫ ֯ܘ‬90 ౓෼Λ։‫ྖޱ‬Ҭͱ͠ʹ͓͚Δඍྔ‫ؚ‬༗ۚଐ༝དྷͷճં఺‫͞࡯؍͕܈‬Ε͍ͯͨʢ෦෼ྠଳ։‫ޱ‬ʣɽ‫݁ࢉܭ‬ՌͰ͸൒஋શ෯Ͱ 4.5 nmΔɽఆʹΑΔଟ‫ݩ‬ૉಉ࣌Ϛοϐϯά૾Ͱ͋Δɽ‫ݩ‬ૉʹ

ʷ 12.2 nm ͷूޫαΠζ͕ಘΒΕɼ‫ۃ‬Ίͯඍখͳ 2 ࣍

ΑΔ෼෍ͷҧ͍Λߴ͍෼ղೳͰ‫͍͖ͯͰ࡯؍‬Δɽ

Fig. 5 ͸ɼथࢷแຒͯ͠ബยԽͨ͠ࢼྉͷ XRF ଌ‫͕ޫूݩ‬ՄೳͰ͋Δ͜ͱ͕ࣔࠦ͞ΕͨɽఆʹΑΔଟ‫ݩ‬ૉಉ࣌Ϛοϐϯά૾Ͱ͋Δɽ‫ݩ‬ૉʹΑΔ̎ʣϚΠΫϩϏʔϜԠ༻ޫֶ‫ܥ‬ϚΠΫϩϏʔϜޫֶ‫Ͱܥ‬ಘΒΕΔσʔλͷྫʹ͍ͭ෼෍ͷҧ͍Λߴ͍෼ղೳͰ‫͍͖ͯͰ࡯؍‬Δɽ

Fig. 6 ͸ DPC ଌఆΛҐ૬ CT ʹԠ༻ͯ͠ಘΒΕͨͯख๏ผʹࣔ͢ɽࢼྉ͸͢΂ͯະॲཧͷໟ൅Ͱ͋Δɽ

Fig. 4 ͸ɼԼଆͷਤʹରԠ͢Δ෦ҐʹϏʔϜ͕ೖࣹͨ͠ͱ͖ʹಘΒΕͨͦΕͧΕͷ WAXD ૾Ͱ͋ΔɽFig.

Fig. 4. Local WAXD images of a human hair using
an X-ray focusing beam. Each image shown in (a),(b), (c) was obtained at different positions of sample
shown in the lower figure, respectively.

Fig. 5. Multi-elemental images of a cross-sectionalslice of a human hair obtained by a scanning XRF
measurement.

– 64 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू
࠶ߏ੒૾Ͱ͋ΔɽࢼྉΛซਐʢਫฏํ޲ʣͱճసʢਨ
௚࣠पΓʣͰ 2 ࣍‫ࠪ͢૸ݩ‬Δ͜ͱͰଌఆ͠ɼͦͷ૸ࠪஅ໘ͷ۶ં཰෼෍ʢ࣮਺෦ʣ͕ಘΒΕ͍ͯΔɽ௨ৗͷ‫ٵ‬ऩίϯτϥετͰ͸‫͕࡯؍‬೉͍͠ίϧςοΫεࡉ๔ؒͷۭܺͳͲ͕‫͍͖ͯͰ࡯؍‬Δɽ

Fig. 7. A reconstructed slice image of a wooden tissue obtained by a high-resolution CT system.

Fig. 6. A reconstructed cross-sectional image of ahuman hair obtained by phase contrast X-ray scanning tomography.
̏ʣߴۭؒ෼ղ CT ͓Αͼ 4 ࣍‫ ݩ‬CT ޫֶ‫ܥ‬ߴۭؒ෼ղ CT ޫֶ‫Ͱܥ‬ಘΒΕͨ২෺૊৫ʢ௺༶
ࢬʣͷஅ૚࠶ߏ੒૾Λ Fig. 7 ʹࣔ͢ɽ਺ϛΫϩϯͷ
ඍখ؅Λղ૾Ͱ͖͓ͯΓɼߴ͍ۭؒ෼ղೳ͕ಘΒΕͯ
͍Δɽ

Fig. 8 ͸ɼൃ๐ͷ༷ࢠΛ 4 ࣍‫ ݩ‬CT Ͱ‫݁ͨ͠࡯؍‬ՌΛ͍ࣔͯ͠Δɽ௚‫ ܘ‬1 mm ͷΨϥεΩϟϐϥϦʔ಺ʹอ࣋ͨ͠ϗοτέʔΩϛοΫεਫ༹ӷΛϏʔϜরࣹʹΑͬͯൃ๐ͤͨ͞ɽ࣮ޮըૉαΠζ 3.4 µm ʹ͓͍ͯࡱӨ଎౓͸ 3000 ϑϨʔϜ/ඵɼࢼྉΛ 10 ճసຖඵͷ଎౓Ͱճసͤͨͨ͞Ίɼ౤Ө਺ 150 ͷ CT ૾Λඵؒ

20 औಘͰ͖ͨɽFig. 8 ͸ಉ͡ߴ͞ͷஅ૚࠶ߏ੒૾Λநग़ͯ࣌͠‫ʹྻܥ‬දࣔͨ͠΋ͷͰ͋Γɼ֤ը૾ͷࠨ্

Fig. 8. A experimental result of four-dimensionalʹࡱӨ։͔࢝Βͷ‫ܦ‬ա࣌ؒΛ͍ࣔͯ͠Δɽ

CT measurement. The sample is water solution of
baking powder in a glass capillary with outer diam-ࠓ‫ޙ‬ͷ՝୊

eter of 1 mm. Reconstructed cross sectional images
in time series were shown in the figure.

TRZP ͷࠓ‫ޙ‬ͷ։ൃʹ͍ͭͯɼ·ͣ 1 ࣍‫͍͓ʹܕݩ‬ͯ͸ɼ ް͍ฏ໘‫ج‬൘Λ࢖༻͢Δ͜ͱͰύλʔχϯάϛφʔ‫ࢠ֨ܕ‬Λ࠾༻͠ɼճંޮ཰ͷ޲্Λૂ͏ɽ͞ΒʹΑΔฏୱ౓ͷཚΕΛճආ͢Δɽκʔϯύλʔϯʹϥʹɼ࠷খઢ෯Λ 70 nm ఔ౓ʹઃఆ͢Δ͜ͱͰɼ5 nmҎԼͷूޫαΠζ࣮‫ݱ‬Λ໨ඪͱ͢Δɽ·ͨɼয఺͕Ұ– 65 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)
க͢ΔΑ͏ʹͨ͠ 1 ࣍‫ ܕݩ‬TRZP ΛλϯσϜʹ௚ަྖҬʹ͓͚Δूޫٕज़ɼΠϝʔδϯάٕज़ʹ͍ͭͯͷ

഑ஔ͠ɼ2 ࣍‫ޫूݩ‬ΛࢼΈΔɽ2 ࣍‫͍͓ͯʹܕݩ‬͸ɼ։ൃߴ౓ԽΛߦ͍ͬͯ͘ɽ

‫཰ۂ‬൒‫ܘ‬ͷେ͖͍ԁ౵‫ج‬൫Λར༻ͨ͠ϓϩτλΠϓʹ
͍ͭͯࢼ࡞Λߦ͍ɼूޫධՁΛߦ͏ɽ‫ۂ‬໘‫ج‬൘΁ͷύࢀߟจ‫ݙ‬λʔϯඳըʹ͍ͭͯ͸ɼ௕য఺ਂ౓ͷ X ઢूޫϏʔ

[1] H. Mimura, S. Handa, T. Kimura, H. Yumoto,D. Yamakawa, H. Yokoyama, S. Matsuyama, K.
Inagaki, K. Yamamura, Y. Sano, K. Tamasaku,
Y. Nishino, M. Yabashi, T. Ishikawa, and K.
Yamauchi: Nat. Phys. 6, 122-125 (2010).
[2] T. Tsuji, H. Takano, T. Koyama, Y. Tsusaka,
and Y. Kagoshima: Jpn. J. Appl. Phys. 49,
030207 (2010).
[3] H. Takano, K. Yoshida, T. Tsuji, T. Koyama, Y.
Tsusaka, and Y. Kagoshima: J. Phys. Conf. Ser.
186, 012049 (2009).
[4] H. Mimura, H. Yumoto, S. Matsuyama, S.
Handa, T. Kimura, Y. Sano, M. Yabashi, Y.
Nishino, K. Tamasaku, T. Ishikawa, and K.
Yamauchi: Phys. Rev. A 77, 015812 (2008).
[5] H. Takano, T. Tsuji, T. Hashimoto, T. Koyama,
Y. Tsusaka, and Y. Kagoshima: Appl. Phys.
Express 3(7), 076702 (2010).
[6] H. Takano, T. Tsuji, and Y. Kagoshima: Proc.
SPIE Vol. 8139, 81390D (2011).
[7] H. Takano, T. Hashimoto, T. Tsuji, T. Koyama,
Y. Tsusaka, and Y. Kagoshima: Rev. Sci.
Instrum. 81(7), 073702 (2010).

Ϝར༻Λ‫ݕ‬౼͢Δɽ
ϚΠΫϩϏʔϜԠ༻ޫֶ‫͍ͯͭʹܥ‬͸ɼࢼྉ͔ΒͷίϯϓτϯࢄཚΛར༻ͨ͠ɼॏ‫ݩ‬ૉதͷܰ‫ݩ‬ૉหผΠϝʔδϯά๏ʹ͍ͭͯ։ൃΛߦ͏ɽ·ͨɼࢼྉ૸ࠪ
ͰಘΒΕͨ WAXD ૾͔Β݁থཻɼཻքɼԠྗ෼෍౳
ͷ৘ใΛநग़ͯ͠Ϛοϐϯά͢ΔγεςϜͷߏஙΛߦ͍ɼΑΓଟ‫ݩ‬తͳ෼ੳ͕Մೳͳεςʔγϣϯ΁ͷ֦ுΛߦ͏ɽߴ෼ղೳ CT ޫֶ‫Ͱܥ‬͸ɼ‫ݕ‬ग़‫ث‬ͷߴ౓ԽΛߦ͍ɼΑΓߴ͍ೱ౓෼ղೳͰ୹࣌ؒ‫ܭ‬ଌ͕ՄೳͳγεςϜ΁
ͷվྑΛߦ͏ɽ4 ࣍‫ ݩ‬CT γεςϜͰ͸ɼ࣌ؒ෼ղೳɼ
ۭؒ෼ղೳͷߴ౓ԽΛߦ͍ͬͯ͘ɽࢼྉʹ͍ͭͯ΋ɼՃ೤ɼྫྷ٫ɼԠྗҹՃ౳ͷଌఆ‫ڥ؀‬੔උΛߦ͍ͬͯ͘ɽ
·ͨ CT ࠶ߏ੒ʹ͍ͭͯɼGPU ʹΑΔฒྻ‫ࢉܭ‬Λར༻ͨ͠γεςϜΛಋೖ͠ɼ‫ࢉܭ‬଎౓ͷ޲্Λߦ͏ɽͦͷଞɼ͜͜Ͱ͸঺հ͍ͯ͠ͳ͍ࣄྫͱͯ͠ɼ̭ઢ
݁૾‫ݦ‬ඍ‫ڸ‬ɼΤοδճંΠϝʔδϯά [7] ౳ͷ։ൃ΋ຊ՝୊Ͱߦͳ͓ͬͯΓɼҾ͖ଓ͖͜ΕΒΛ‫ؚ‬Ί̭ͨઢ– 66 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

BL24XU

2011B3255

ඍখ֯ೖࣹ̭ઢճં๏ʹΑΔϙϦ-α-ΦϨϑΟϯ/઀ணࡎք໘ͷඍࡉߏ଄

Microstructures of Poly-α-olefin/Adhesives Interface ɹUsing Grazing Incidence X-ray Diffractionখࣉ ‫ ݡ‬1 ɼۨా Ί͙Έ 1 ɼԣࢁ ࿨࢘ 2 ɼ஛ా ৾‫ ޗ‬3 ɼদҪ ७࣐ 2 ɼ੢໺ ޹ 1
Masaru Kotera1 , Megumi Komada1 , Kazushi Yokoyama2 , Shingo Takeda3 ,Junji Matsui2 , Takashi Nishino11ਆ‫ށ‬େֶେֶӃ޻ֶ‫ڀݚ‬Պɼ2 ʢެࡒʣͻΐ͏͝Պֶٕज़‫ڠ‬ձ์ࣹޫφϊςΫ‫ॴڀݚ‬ɼ
3εϓϦϯάΤΠταʔϏε‫ࣜג‬ձࣾ

1

2

Department of Chemical Science and Engineering, Kobe University,
Synchrotron Radiation Nanotechnology Laboratory, Hyogo Science and Technology Association,
3

SPring-8 Service Co. Ltd.

֓ཁɿɹΞΠιλΫνοΫϙϦϓϩϐϨϯʢit.PPʣʹର͢ΔϓϥΠϚʔॲཧͷޮՌΛɼඍখ֯ೖࣹ̭ઢճંଌ
ఆʹΑΓඍࡉߏ଄ʢಛʹ it.PP ݁থͷ഑޲มԽʣͷ‫఺؍‬ΑΓ‫ݕ‬౼ͨ͠ɽͦͷ݁ՌɼϓϥΠϚʔॲཧʹΑΓ it.PP݁থͷ 111 ൓ࣹͷ૬ର‫౓ڧ‬ൺ͕ in-plane ํ޲ͷΈͰ૿Ճͨ͠ɽ͜ΕΑΓɼit.PP ݁থ͸ϓϥΠϚʔॲཧʹΑΓ഑޲มԽ͠ɼ͜ͷมԽ͕઀ண‫্౓ڧ‬ঢʹ݁ͼ͍ͭͨ΋ͷͱߟ͑ΒΕͨɽΩʔϫʔυɿɹϙϦ-α-ΦϨϑΟϯ, ϓϥΠϚʔɼ഑޲มԽɼ઀ணද໘ʗք໘

૚Λ‫ؚ‬Ίͨඃணମͷք໘ྖҬ͸શମੵ͔Βൺֱ͢Δͱഎ‫ڀݚͱܠ‬໨త޻‫ۀ‬తʹ࠷΋൚༻͞ΕΔߴ෼ࢠࡐྉ͸ɼϙϦΤνϨϯ΍ϙϦϓϩϐϨϯͳͲʹ୅ද͞ΕΔϙϦ-α-ΦϨϑΟϯྨͰ͋Δ͕ɼ͜ΕΒ͸‫ۃ‬ੑ‫׭‬ೳ‫ج‬Λ࣋ͨͳ͍͜
ͱ͔Βɼͨͱ͑͹ɼॠؒ઀ணࡎͱͯ͠୅දతͳγΞϊΞΫϦϨʔτ (CA) ‫઀ܥ‬ணࡎͰ͸Ұൠʹ઀ண͕ࠔ೉Ͱ
͋ΔɽͦͷͨΊɼ༧Ίඃண໘ʹରͯ͠ϓϥΠϚʔͱ‫ݺ‬͹ΕΔΞϛϯྨͳͲͷ௿෼ࢠ༹ӷΛృ෍ɾ‫ס‬૩ॲཧΛࢪͨ͠‫ޙ‬ɼ઀ணࡎΛృ෍͢Δɻ͜ͷख๏ʹΑΓɼ઀ண‫౓ڧ‬͸ 1.8 N/cm(೪ணςʔϓఔ౓) ͔Β 30 N/cm Ҏ্ (‫ࡐج‬ͷ‫ूڽ‬ഁյ) ͱ໿ 15 ഒ΋૿Ճ͢Δ [1]ɽ·ͨɼϓϥΠϚʔ༹ӷృ෍͔Β઀ணࡎృ෍·Ͱͷ‫ס‬૩࣌ؒΛʮΦʔϓϯλΠϜʯͱ‫ͼݺ‬ɼ͜ͷ઀ண‫౓ڧ‬͸Φʔϓϯͦͷମੵ෼཰͕Θ͔ͣͱͳΔͷΈͳΒͣɼຒ΋Εͨք໘૚Ͱ͋ΔͨΊɼߴ S/N ൺͰߏ଄৘ใΛଊ͑Δ͜ͱ͸‫ۃ‬Ίͯࠔ೉Ͱ͋Δɽຊ࣮‫Ͱݧ‬͸ɼ̭ઢΛࢼྉද໘ʹରͯ͢͠Ε͢Εͷ֯౓Ͱೖࣹ͢Δඍখ֯ೖࣹ̭ઢճં๏Λ༻͍ɼ‫ج‬൘ͱͯ͠ϙϦ-α-ΦϨϑΟϯྨͷͳ͔Ͱ΋଱೤ੑ΍଱ༀ඼ੑʹ༏ΕΔΞΠιλΫνοΫϙϦϓϩϐϨϯʢit.PPʣΛऔΓ্͛ɼϓϥΠϚʔॲཧ͕༩͑Δ઀ணྗ૿ՃͷϝΧχζϜղ໌Λ໨తͱ͠ɼit.PP ݁থͷඍࡉߏ଄Λ‫ݕ‬౼ͨ͠ɽ࣮‫ݧ‬ΞλΫνοΫ੒෼ͷআ‫ڈ‬Λ໨తʹιοΫεϨʔநग़λΠϜʹґଘ͢Δ͜ͱ΋஌ΒΕ͍ͯΔ.
Ұൠతʹ઀ணͱ͍͏‫ݱ‬৅ͷ‫ݪ‬Ҽͱͯ͠͸ɼΞϯΧʔͨ͠ it.PP(ॅ༑Խֶ (‫)ג‬ɼNOBLEN HD 100G2) ΛޮՌ΍Խֶ݁߹ɼ੩ిత૬‫༻࡞ޓ‬ɼ෼ࢠؒྗɼ෼ࢠ֦

170 ◦ C ʹͯςτϥϦϯʹ༹ղ (0.3 wt%) ͤ͞ɼ170 ◦ CࢄͳͲ͕ߟ͑ΒΕ͍ͯΔ͕ɼ࣮‫ݧ‬తͳূ໌͸ͳ͞ΕͯʹอԹͨ͠ Si ΢Σϋ্΁εϐϯίʔτ๏ʢ1500 rpm,͓Βͣɼͦͷৄࡉ͸ະͩෆ໌Ͱ͋Δɽ͜Ε͸ɼϓϥΠ

1 2sec + 2500 rpm, 60 secʣʹΑΓ੒ບͨ͠ɽͳ͓ɼ

Ϛʔ༹ӷͷృ෍ʹΑΓӨ‫ڹ‬Λड͚ΔྖҬ͕‫ج‬൘ͷ‫ۃ‬ද̭ઢ൓ࣹ཰ଌఆΑΓධՁͨ͠ບް͸ 40 nm Ͱ͋ͬͨɽ

໘ۙ๣ͷΈͱߟ͑ΒΕɼϓϥΠϚʔॲཧ૚‫઀ͼٴ‬ணࡎ

N,N-δϝνϧ-n-ΦΫλσγϧΞϛϯͷΤλϊʔϧ༹

– 67 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)ӷ (0.1 wt%) ΛϓϥΠϚʔ༹ӷͱͯ͠༻͍ɼit.PP ബ

݁Ռ͓Αͼߟ࡯

ບ্ʹεϐϯίʔτ๏ (800 rpm, 12 sec + 1500 rpm,

60 sec) ʹΑΓృ෍ͨ͠ɽ
ඍখ֯ೖࣹ̭ઢճંଌఆ͸ɼBL24XUA2 ϋονʹઃஔͨ͠ճં‫ܭ‬Λ༻͍ɼࣗ࡞νϟϯόʔʹΑΓࢼྉงғ‫ؾ‬Λ He ஔ‫ͨ͠׵‬ɽೖࣹଆεϦοτʹΑΓ੔‫ͨ͠ܗ‬̭ઢʢ̭ઢΤωϧΪʔ:10 keVɼ0.15 mm(Horizontal)

× 0.15 mm(Vertical)ʣΛɼit.PP ͷ̭ઢྟք֯ʢαc =0.12 deg.) Ҏ্Ͱ͋Δ α = 0.16 deg. ʹͯೖࣹ͠ɼड

ޫଆιʔϥʔεϦοτʢ0.4 deg.ʣΛ౥ࡌͨ͠ NaI γ
ϯνϨʔγϣϯ‫ݕ‬ग़‫ࢼͰث‬ྉ໘಺͓Αͼ໘֎ํ޲ʹεΩϟϯʢεΩϟϯ৚݅ɿ0.1 deg./step, 2 sec/stepʣͨ͠ɽ઀ணࢼ‫͍ͯͭʹݧ‬͸ɼϓϥΠϚʔ༹ӷΛృ෍ͨ͠

it.PP ϑΟϧϜʢ20 mm × 50 mmʣ2 ຕʹରͯ͠ɼΦʔϓϯλΠϜΛมԽͤͯ͞γΞϊΞΫϦϨʔτ‫઀ܥ‬ணࡎΛృ෍ɾ઀ணͤ͞Δ͜ͱͰࢼྉΛ࡞੡͠ɼ180◦ ണ཭ࢼ‫ʹݧ‬ΑΓɼͦͷണ཭‫౓ڧ‬ͷฏ‫ۉ‬஋Λ઀ணྗͱͨ͠.

Fig. 1 ʹ͸ɼϓϥΠϚʔ༹ӷృ෍લ‫ޙ‬ʢృ෍‫ ޙ‬3࣌ؒ‫ޙ‬ʣʹ͓͚Δ it.PP ബບͷʢaʣ໘಺͓Αͼʢbʣ໘֎̭ઢճંϓϩϑΝΠϧΛࣔͨ͠ɽNatta ΒʹΑΔ
ͱ it.PP ͷ݁থߏ଄͸୯ࣼথ‫ʹܥ‬ଐ͠ɼͦͷ֨ࢠఆ਺͸ a= 6.65 Åɼb= 20.96 Åɼc(ણҡ࣠)= 6.50 Åɼ

β = 99.3 deg. ͱใࠂ͞Εɼ෼ࢠ࠯͕ 3 ϞϊϚʔͰ 1
ճస͢Δ α ‫ ܕ‬3/1 ΒͤΜߏ଄Λ༗͢Δ [2]ɽճંϓϩϑΝΠϧΑΓɼit.PP ബບ͸ α ‫݁ͯ͠ͱܕ‬থԽ͍ͯ͠
Δ͜ͱ͕෼͔ͬͨɽ͔͠͠ɼ໘಺͓Αͼ໘֎ͷճંϓϩϑΝΠϧʹ͓͍֤ͯ൓ࣹͷ૬ର‫౓ڧ‬ൺ͕ҟͳΔ͜ͱ
͔Βɼࠓճ࡞੡ͨ͠ it.PP ബບ͸ a ͕࣠‫ج‬൘ʹରͯ͠΄΅ਨ௚ͱͳΔΑ͏ʹ݁থ഑޲͍ͯ͠Δ͜ͱ͕໌Β͔ͱͳͬͨɽ͜ͷബບʹϓϥΠϚʔ༹ӷΛృ෍͢Δͱɼ
໘಺ճંʹ͓͚Δ 111 ൓ࣹ‫౓ڧ‬ͷΈ͕େ͖͘૿Ճ͠
ͨɽͨͩ͠ɼ֤൓ࣹͷճંϐʔΫҐஔ͓Αͼ൒஋෯ͷେ͖ͳมԽ͸‫ݟ‬ΒΕͳ͍͜ͱ͔Βɼit.PP ݁থͷ໘ִ͓ؒΑͼඍ݁থαΠζʹมԽ͸ͳ͔ͬͨɽ

Fig. 1. Grazing incidence X-ray diffraction profiles of it.PP+Primer thin films.

– 68 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

Fig. 2. it.PP molecular models in surface before and after applying primer.

Fig. 2 ʹ͸ɼϓϥΠϚʔ༹ӷృ෍લ‫͚͓ʹޙ‬ΔബບϜ͓Αͦ 4 ࣌ؒΛ࠷େ஋ͱ͢ΔΑ͏ະॲཧʹൺֱ͠தͰͷ it.PP ݁থͷ഑޲มԽ໛ࣜਤΛࣔͨ͠ɽϓϥΠ໿ 15 ഒ૿Ճ͕ͨ͠ɼͦͷ‫ޙ‬͸઀ண‫౓ڧ‬ͷ௿Լ͕ΈΒϚʔ༹ӷͷృ෍ʹΑΓ໘಺ճં 111 ൓ࣹ‫౓ڧ‬ͷΈ͕େΕɼΦʔϓϯλΠϜ 10 ࣌ؒͰ͸࠷େ஋ͷ൒෼ఔ౓ͷ͖͘૿Ճͨ͜͠ͱ͔Βɼ111 ൓ࣹͷࢄཚϕΫτϧ͕ࢼ઀ண‫͔ͨͬͳ͔ࣔ͞͠౓ڧ‬ɽ͜ͷ઀ண‫౓ڧ‬ͷ‫ڍ‬ಈ͸໘ྉද໘ͱ΄΅ฏߦͱͳΔΑ͏ʹ഑޲มԽͨ͠΋ͷͱߟ

಺ 111 ൓ࣹ‫౓ڧ‬ͷ‫ڍ‬ಈͱ΄΅ରԠ͍ͯ͠Δ͜ͱ͔Βɼ͑ΒΕͨɽͭ·Γɼit.PP ݁থͷ a,c ͕࣠ b ࣠पΓʹϓϥΠϚʔ༹ӷృ෍ʹΑΔ it.PP ݁থͷ഑޲มԽ͕઀

ճసͨ͠ɽணྗ૿ՃͷҰҼʹͳ͍ͬͯΔͱߟ͑ΒΕͨɽ͜ͷϝΧ

Fig. 3 ʹ͸ɼΦʔϓϯλΠϜͷ‫࣌ܦ‬มԽʹ൐͏ɼʢaʣ໘಺ճંϓϩϑΝΠϧ͓Αͼʢbʣ໘಺ճંϓϩϑΝΠϧʹ͓͚Δશͯͷ݁থճંϐʔΫ໘ੵʹର͢Δ 111
൓ࣹͷճંϐʔΫ໘ੵൺͱ઀ண‫౓ڧ‬ͷؔ܎Λࣔͨ͠ɽϓϥΠϚʔ༹ӷͷృ෍ʹΑΓɼΘ͔ͣ 0.3 ࣌ؒͱ͍͏
୹࣌ؒͷΦʔϓϯλΠϜͰ໘಺ 111 ൓ࣹ‫౓ڧ‬͸‫ܹٸ‬ʹ૿Ճ͠ɼͦͷ‫ޙ‬Θ͔ͣͳ૿Ճ͕‫ݟ‬ΒΕͨɽ͔͠͠ɼ
͓Αͦ 5 ࣌ؒ‫ޙ‬Ҏ߱Ͱ͸؇΍͔ʹ‫ݮ‬গ͠ɼΦʔϓϯλ
ΠϜ 10 ࣌ؒʹ͓͍ͯ΋ॳ‫ظ‬ͷճં‫Ͱ·౓ڧ‬໭Δ͜ͱ

χζϜͷৄࡉʹ͍ͭͯ͸‫ݕ‬౼தͰ͋Δ͕ɼ௿෼ࢠͰ͋
ΔϓϥΠϚʔ༹ӷ͸ృ෍‫ ʹͪͩͨޙ‬it.PP ബບද໘͔
Β಺෦΁ਁಁ͢Δͱߟ͑ΒΕΔɽ͔͠͠ɼit.PP ݁থͷ໘ִ͓ؒΑͼඍ݁থαΠζ͸มԽ͠ͳ͔ͬͨ͜ͱ͔
ΒɼϓϥΠϚʔ෼ࢠͰ͋Δ N,N-δϝνϧ-n-ΦΫλσγϧΞϛϯ͸༏ઌతʹ it.PP ͷඇথྖҬʹ֦ࢄ͢Δ͜
ͱͰɼ͜ͷΑ͏ͳϞϧϑΥϩδʔมԽ͕ it.PP ݁থͷ഑޲มԽΛ΋ͨΒͨ͠ͱਪଌ͍ͯ͠Δɽ

͸ͳ͔ͬͨɽ·ͨɼ઀ண‫͍ͯͭʹ౓ڧ‬΋ΦʔϓϯλΠ– 69 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

Fig. 3. (a) Grazing incidence X-ray diffraction profiles of it.PP+Primer at several open time. (b) Relationships between open time and area ratio/peel
stregth.
·ͱΊͱࠓ‫ޙ‬ͷ՝୊δʔʹ‫ى‬Ҽ͢Δද໘ϥϑωε͕େ͖͘ɼશ൓ࣹ৚݅Ͱ

೉઀ணੑߴ෼ࢠͰ͋ΔϙϦ-α-ΦϨϑΟϯྨͷͳ͔Ͱ΋ɼࠓճ͸ಛʹ it.PP ΛऔΓ্͛ɼϓϥΠϚʔॲཧʹΑΔ઀ணྗ૿ՃͷϝΧχζϜղ໌Λ໨తʹඍখ֯ೖࣹ̭ઢճં๏ʹΑΓ it.PP ബບͷඍࡉߏ଄Λ‫ݕ‬౼ͨ͠ɽͦͷ݁ՌɼϓϥΠϚʔॲཧʹΑΓ it.PP ݁থʹ഑޲มԽ͕ੜ͡ɼ͜Ε͕઀ண‫౓ڧ‬ͷ૿ՃΛ΋ͨΒͨ͠ͱߟ͑
ΒΕͨɽࠓ‫ޙ‬͸ɼ͜ͷ഑޲มԽͷ‫࣌ܦ‬มԽΛೋ࣍‫ݕݩ‬ग़‫ث‬ʢϓϥΠϚʔ༹ӷృ෍௚‫ޙ‬͸‫ʹܹٸ‬มԽ͢Δͱ༧૝͞ΕΔͨΊɼߴ‫ݕ‬ग़ޮ཰͔ͭ࣌෼ׂଌఆՄೳͳ‫ݕ‬ग़‫ͯ͠ͱث‬ɼͨͱ͑͹ PILATUS ‫ݕ‬ग़‫Ͳͳث‬ʣͷར༻ʹΑΓɼϝΧχζϜͷৄࡉΛ‫ݕ‬౼͢Δɽ·ͨɼit.PP ͸݁থԽ଎౓͕ൺֱతେ͖͘ɼ੒ບ௚‫Ͱޙ‬΋ߴ͍݁থԽ
౓Λ༗͢ΔɽͦͷͨΊɼബບද໘͸݁থԽϞϧϑΥϩ

ͷଌఆ͕ࠔ೉Ͱ͋Δɽࠓճͷ࣮‫Ͱݧ‬͸ɼບް 40 nm ͷບશମΛଌఆ͠ɼ͜ΕΛʮࡐྉද໘ۙ๣ʯͱԾఆͯ͠
͍ΔͨΊɼ͞Βʹ௒ബບࢼྉͰͷଌఆ΋ඞཁͰ͋Δɽ
·ͨɼit.PP ಺෦΁ͷϓϥΠϚʔ෼ࢠͷਁಁɾ֦ࢄঢ়
ଶΛ‫ݕ‬౼͢ΔͨΊɼͨͱ͑͹̭ઢ൓ࣹ཰ଌఆΛ༻͍ͨີ౓෼෍ධՁ΍ɼ̭ઢޫిࢠ෼ޫ๏ͳͲͷ෼ޫख๏ʹΑΓϓϥΠϚʔ෼ࢠͷ݁߹ঢ়ଶͳͲʹ͍ͭͯ‫ݕ‬౼Λߦ͏༧ఆͰ͋Δɽࢀߟจ‫ݙ‬[1] Y. Okamoto and T. Philip: J. Adhesion 40, 8191 (1993).
[2] G. Natta and P. Corradini: Nuovo Cimento
Suppl. 15, 40 (1960).

– 70 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

2009B3225, 2010A3225, 2010B3225, 2011A3225

BL24XU޿֯ࢄཚޫֶ‫ܥ‬ͷߏஙͱ೪ணࡎͷണ཭աఔʹ͓͚Δߏ଄มԽͷͦͷ৔‫࡯؍‬

Establishment of WAXS System and In-situ Observation of
Structural Change in Pressure-Sensitive Adhesive
during the Peeling Process஛ా ৾‫ ޗ‬1,3 , தલ উ඙ 2 , ࢁԼ ‫ ีܙ‬3 , ੴా ੒ 1 , ໺੉ ૜ࢢ 1 , ೔ࢁ ͓͞Γ 2 , ཥ ཕ 2 ,‫܂‬ຊ ࣎ੜ 2 , ࣫‫ྑ ݪ‬ণ 2 , ԣࢁ ࿨࢘ 2 , দҪ ७࣐ 2,3
1,3
Shingo Takeda , Katsuhiko Nakamae2 , Keisuke Yamashita3 , Shigeru Ishida1 , Souici Nose1 ,Saori Hiyama1 , Lei Li2 , Shigeo Kuwamoto2 , Yoshimasa Urushibara2 , Kazushi Yokoyama2 ,Junji Matsui2,31εϓϦϯάΤΠταʔϏε‫ࣜג‬ձࣾ, 2 (ެࡒ) ͻΐ͏͝Պֶٕज़‫ڠ‬ձ์ࣹޫφϊςΫ‫ॴڀݚ‬ɼ
3ฌ‫ཱݝݿ‬େֶେֶӃ෺࣭ཧֶ‫ڀݚ‬Պ
1

2

SPring-8 Service Co. Ltd.,
Synchrotron Radiation Nanotechnology Laboratory, Hyogo Science and Technology Association,
3

Graduate School of Material Science, University of Hyogo֓ཁɿɹ SPring-8 BL24XU ͷ࣮‫ݧ‬ϋον A ʹ͓͍ͯɼκʔϯϓϨʔτ (ZP) Λूޫૉࢠͱͨ͠ϚΠΫϩ޿̭֯ઢࢄཚ૷ஔͷ੔උΛߦͬͨɽຊ૷ஔͰ͸ɼूޫαΠζɼԣํ޲ 43 µmɼॎํ޲ 12 µm Λୡ੒͓ͯ͠ΓɼඍখྖҬͷ̭ઢࢄཚଌఆΛ͓͜ͳ͏͜ͱ͕Ͱ͖Δɽຊ૷ஔΛ༻͍ͯɼ೪ணࡎͷണ཭աఔʹ͓͚Δඍࡉߏ଄มԽͷͦͷ৔‫࡯؍‬Λߦͬͨͱ͜Ζɼ೪ணࡎதͷఱવΰϜ݁থԽ‫ݱ‬৅ͷ‫ʹ࡯؍‬͸͡Ίͯ੒ޭͨ͠ɽ
ΩʔϫʔυɿɹϚΠΫϩ޿̭֯ઢࢄཚɼ೪ணࡎɼin-situ ‫࡯؍‬͜͜Ͱ͸ಛʹɼϚΠΫϩ޿֯ࢄཚ૷ஔͷੑೳͱɼ૷

എ‫ڀݚͱܠ‬໨తฌ‫ݝݿ‬ϏʔϜϥΠϯʢBL24XU ͓Αͼ BL08B2ʣͰ͸ɼϚΠΫϩϏʔϜɾ̭ઢ‫ݦ‬ඍ‫ڸ‬౳ͷֵ৽తͳ‫ڀݚ‬։ൃɼ࢈‫ۀ‬քͷ޿ൣғͷ෼໺Ͱͷ‫ڀݚ‬՝୊Λத৺ʹ์ࣹޫͷ࢈‫ۀ‬ར༻Λࢧԉ͖ͯͨ͠ɽφϊίϯϙδοτࡐྉ‫Ͳͳڀݚ‬ͷϓϩδΣΫτ΁ͷऔΓ૊Έ΋ͦͷҰ‫͋Ͱ؀‬ஔͷσϞϯετϨʔγϣϯͱͯ͠ߦͬͨɼ೪ணࡎͷണ཭աఔʹ͓͚Δඍࡉߏ଄มԽͷͦͷ৔ʢin-situʣ‫࡯؍‬ͷ‫ڀݚ‬੒Ռʹ͍ͭͯใࠂ͢Δɽ
ϚΠΫϩ޿̭֯ઢࢄཚޫֶ‫ܥ‬Δɽಛʹ BL24XU Ͱ͸ɼϚΠΫϩϏʔϜ‫ܗ‬੒ͷ‫ૅج‬ϚΠΫϩ޿̭֯ઢࢄཚޫֶ‫ܥ‬͸େ͖͘෼͚ͯ 4 ͭͷ‫ͱͱڀݚ‬΋ʹɼWAXSɼSAXSɼ‫ޫܬ‬෼ੳɼΠϝʔδίϯϙʔωϯτͰߏ੒͞Εɼ্ྲྀ͔Βɼޫ‫ݯ‬ɼूޫޫϯά౳Λ૯߹తʹ‫ۀ࢈ͨ͠༻׆‬ར༻ΛਐΊ͍ͯΔɽֶ‫ܥ‬ɼࢼྉ୆ (ΰχΦϝʔλ)ɼ‫ݕ‬ग़‫ͳͱث‬Δɽޫ‫͔ݯ‬ैདྷͷ‫ڀݚ‬Λ௨ͯ͡ɼ஝ੵͨ͠‫ݧܦ‬΍஌‫ݟ‬Λ‫͢༻׆‬Βͷ์ࣹޫΛμΠϠϞϯυೋ݁থ෼ޫ‫ Ͱث‬10 keV ͷ

Δ͜ͱͰɼ࢈‫ۀ‬քʹ͓͚Δ͞·͟·ͳχʔζʹԠ͑Δ

̭ઢʹ෼ޫ͠ɼ࣮‫ݧ‬ϋονʹೖࣹ͢Δɽ࣮‫ݧ‬ϋονͰ

΂͘ɼBL24XU ͷ࣮‫ݧ‬ϋονΛվ଄͠ɼখ֯ɾ޿֯ࢄ

͸ 4 ৅‫ݶ‬εϦοτΛ࢖༻̭ͯ͠ઢΛ੔‫͠ܗ‬ɼZP ʹೖཚϞʔυΛ࣮‫ݱ‬Մೳͱͨ͠ɽ۩ମతʹ͸ BL24XU ʹ

ࣹ͢ΔɽZP ʹΑͬͯूޫ͞Ε̭ͨઢͷয఺Ґஔʹࢼ͓͚Δ৽ͨͳଌఆϞʔυͱͯ͠ɼϚΠΫϩখ̭֯ઢࢄ

ྉΛ഑ஔ͠ɼଌఆΛߦ͏ɽ֤ίϯϙʔωϯτʹؔ͢Δ

ཚʢϚΠΫϩ SAXSʣɼϚΠΫϩ޿̭֯ઢࢄཚʢϚΠৄࡉΛԼ‫ࣔ͢ʹه‬ɽ·ͨɺຊϚΠΫϩ޿̭֯ઢࢄཚͷΫϩ WAXSʣɼBonse-Hart ‫ߴܕ‬෼ղೳ SAXS ౳ͷ੔ུ֓Λ Fig. 1 ʹࣔ͢ɽඋΛਐΊɼϢʔβ΁ͷ‫༻ڙ‬Λ։͍࢝ͯ͠Δɽ

– 71 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

Fig. 1. Schematic of the micro-WAXS system.
• ޫ‫ݯ‬

ϚΠΫϩϏʔϜΛ༻͍ͨ‫ྖॴہ‬Ҭͷ̭ઢࢄཚଌఆʹ͸ɼߴً౓͔ͭࢦ޲ੑͷྑ͍̭ઢ͕ཁ‫͞ٻ‬ΕΔͨΊɼޫ‫ ͯ͠ͱݯ‬SPring-8 ͷΞϯδϡϨʔλΛ༻͍ͨɽΞϯδϡϨʔλΛޫ‫͍༻ͯ͠ͱݯ‬Δ͜ͱʹΑΓɼ̭ઢͷूޫޮ཰ͷ޲্΍ूޫαΠζͷॖখ͕Մೳͱͳͬͨɽ

• ूޫޫֶ‫ܥ‬̭ઢࢄཚଌఆͰ͸ɼ̭ઢʹΑͬͯরࣹ͞ΕͨࢼྉྖҬͷฏ‫ۉ‬৘ใ͕ಘΒΕΔɽࢼྉʹೖࣹ͢Δ̭ઢͷαΠζΛॖখ͠ϚΠΫϩϏʔϜԽ͢Δ͜ͱʹΑΓɼߴҐஔ෼ղೳͰඍখͳྖҬͷධՁΛߦ͏͜ͱ͕ՄೳʹͳΔɽ
·ͨɼ୯Ґ໘ੵ͋ͨΓͷޫࢠີ౓͕ߴ͘ͳΔͨΊʹɼඍখͳࢼྉ͔Βͷ৴߸Λޮ཰Α͘औಘ͢Δ͜ͱ͕Ͱ͖
ΔɽຊϚΠΫϩ޿֯ࢄཚ૷ஔͰ͸ɼ̭ઢϚΠΫϩϏʔϜͷޫֶૉࢠͱͯ͠ ZP Λ༻͍ͨɽ‫ܗ‬੒͞Ε̭ͨઢϚΠΫϩϏʔϜͷαΠζ͸ɼԣํ޲ 43 µmɼॎํ޲ 12µm Λୡ੒ͨ͠ɽφΠϑΤοδεΩϟϯ๏ͰͷϏʔϜαΠζͷධՁ݁ՌΛ Fig. 2 ʹࣔ͢ɽ·ͨɼࢼྉʹೖࣹ
͢Δ̭ઢͷ‫౓ڧ‬͸ 1 × 1010 photons/sec Ͱ͋Γɼू

Fig. 2. Profiles of the focused X-ray beam. (a) Horizontal direction and (b) vertical direction.
ͰՄมͰ͋Δɽ͜ΕʹΑΓɼ਺ nm ͔Β਺ 10 nm ·ͰͷαΠζ‫ͼٴ‬प‫ߏظ‬଄ʹؔ͢Δ৘ใΛಘΔ͜ͱ͕Ͱ͖Δɽ࣮‫ݧ‬ͷഎ‫ܠ‬ຊϚΠΫϩ޿֯ࢄཚޫֶ‫ܥ‬ͷσϞϯετϨʔγϣϯޫޫֶ‫͕ܥ‬ແ͍৔߹ͱൺֱͯ͠ɼ̭ઢޫࢠີ౓ΛҰܻͱͯ͠ɼ೪ணࡎͷണ཭աఔʹ͓͚Δඍࡉߏ଄มԽͷͦҎ্޲্ͤ͞Δ͜ͱ͕Ͱ͖ͨɽ

ͷ৔‫࡯؍‬Λߦͬͨɽ‫ײ‬ѹ೪ணࡎ͸ɼ೔ৗੜ‫͍͓ͯʹ׆‬• ࢼྉ୆ʢΰχΦϝʔλʣ࢈‫ۀ‬΍ༀࡎ෼໺Ͱ޿͘༻͍ΒΕ͍ͯΔɽఱવΰϜΛ‫ݪ‬ूޫ̭ઢͷয఺Ґஔʹࢼྉ͕Ϛ΢ϯτ͞ΕΔΑ͏ྉͱͨ͠‫ײ‬ѹ೪ணࡎ͸ɼߴ͍ണ཭‫౓ڧ‬Λ༗͢Δɽ͜Εʹઃ‫͞ܭ‬Ε͍ͯΔɽࢼྉ୆ͷ‫ۦ‬ಈ‫ߏػ‬͸ϚΠΫϩϏʔ͸ണ཭աఔʹ͓͍ͯ೪ணࡎதͷఱવΰϜͷߏ଄͕มԽ

ϜʹରԠͰ͖ΔΑ͏ 1 µm ҎԼͷਫ਼౓Λ༗ͨ͠ΰχΦ͢Δ͔ΒͰ͋Δͱਪଌ͞ΕΔɽఱવΰϜͷΞϞϧϑΝ

ϝʔλΛ࢖༻͓ͯ͠Γɼࢼྉͷฒਐ΍ճస૸ࠪΛ࠶‫ݱ‬ε࠯͸Ұํ޲ʹ໿ 400 %Ԇ৳͞ΕΔ͜ͱʹΑΓ݁থੑྑ͘ߦ͏͜ͱ͕Ͱ͖Δɽ·ͨɼߴഒ཰ͷՄࢹޫ CCD

Խ͕࢝·Δ͜ͱ͸ɼྑ͘஌ΒΕ͍ͯΔ‫ݱ‬৅Ͱ͋Δ [1]ɽΧϝϥΛ̭ઢͱಉ࣠ʹ഑ஔ͓ͯ͠ΓɼࢼྉͷଌఆҐஔ͜ͷ‫ݱ‬৅͸ҾͬுΓԠྗ͕‫ݪ‬ҼͰ͋Δͱਪଌ͞Ε͍ͯΛਫ਼౓ྑܾ͘ఆ͢Δ͜ͱ͕ՄೳͰ͋Δɽ

Δ͕ɼ͜Ε·Ͱ‫ײ‬ѹ೪ணςʔϓͷണ཭աఔʹ͓͚Δ೪• ‫ݕ‬ग़‫ث‬ணࡎதͷఱવΰϜ݁থԽͷͦͷ৔‫ʹ࡯؍‬͸੒ޭ͍ͯ͠

ΠϝʔδϯάϓϨʔτΛ࠾༻ͨ͠ɽ·ͨɼࢼྉ͔Β‫ݕ‬ͷͦͷ৔‫࡯؍‬ΛࢼΈͨɽຊޫֶ‫Ͱܥ‬͸‫ݕ‬ग़‫ͯ͠ͱث‬ൺֱత‫ݕ‬ग़໘ੵ͕େ͖͍

ͳ͔ͬͨɽͦ͜Ͱɼຊޫֶ‫ܥ‬Λ༻͍ͯɼ͜ͷߏ଄มԽग़໘·ͰͷΧϝϥ௕͸ɼ໿ 300 mm ͔Β 950 mm ·

– 72 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

࣮‫ݧ‬ࢼྉʹ͸ϕʔεް͞ 40 µmɼ೪ணࡎް͞ 10 µm ͷࢢൢ͞Ε͍ͯΔఱવΰϜ‫ܥ‬೪ணςʔϓΛ༻͍ͨɽςʔϓͷ೪ணࡎ໘ΛுΓ߹ΘͤɼͦΕͧΕͷςʔϓ୺Λ 90౓ํ޲ʹԆ৳ɾണ཭͠ɼͦͷաఔʹ͓͚Δ೪ணࡎͷ̭ઢ޿֯ࢄཚଌఆΛߦͬͨɽ·ͨɼԆ৳͸খ‫ܕ‬ϕΞϦϯάΛ༻͍ͨ೪ணςʔϓҾͬுΓࢼ‫ثݧ‬Λ༻͍ͯߦ͍ɼ
೪ணࡐʹ͔͔ΔԠྗ͕ҰఆʹอͨΕΔΑ͏ௐ੔ͨ͠ɽ

Fig. 3 ʹണ཭աఔʹ͓͚Δ‫ײ‬ѹ೪ணࡎͷޫֶ‫ݦ‬ඍ‫ࣸڸ‬ਅΛࣔ͢ɽന࢛֯Ͱࣔͨ͠ྖҬ͕̭ઢͷরࣹྖҬͰ͋ΓɼͦͷαΠζ͸ 50 µm × 20 µm Ͱ͋ΔɽZ Ͱ

Fig. 3. Optical microscope image of the adhesive.

աఔʹ͓͍ͯ೪ணࡎ͕࠷΋Ԇ৳͞ΕͨҐஔͰ͋ΔɽҰ݁Ռ͓Αͼߟ࡯

ࣔͨ͠஋͕̭ઢͷরࣹҐஔͰ͋ΓɼZ = 0 µm ͸ണ཭ํɼZ = 240 µm ͸ണ཭લͷঢ়ଶͰ೪ணࡎ͕Ԇ৳͞೪ணࡎ͕ണ཭ɾԆ৳͞Ε͍ͯͳ͍ Z = 240 µm ͷΕ͍ͯͳ͍ҐஔΛ͍ࣔͯ͠ΔɽZ = 0 µm ͷҐஔ͔ΒҐஔͰ͸ɼΞϞϧϑΝεύλʔϯͷΈ͔͠‫͞࡯؍‬Εͳ

Z = 240 µm ʹ޲͚ͯ 30 µm εςοϓͰɼ̭ઢͷճ͔ͬͨɽ͜Ε͸ɼఱવΰϜ͸Ԇ৳͞Ε͍ͯͳ͍ঢ়ଶͰ

ંύλʔϯΛଌఆ͢Δ͜ͱʹΑΓɼണ཭աఔʹ͓͚Δ͸ΞϞϧϑΝεͰ͋Γɼ೪ண෇༩ࡎ͸೪ணঢ়ଶͷఱવ೪ணࡎͷԆ৳཰ͱߏ଄มԽͷ૬ؔΛ‫ͨ͠࡯؍‬ɽΰϜதʹ༹ղ͍ͯ͠Δ͔ΒͰ͋ΔɽԆ৳཰ͷҧ͏֤Ґஔʹ͓͚Δ̭ઢͷճંύλʔϯΛ Fig. 4 ʹࣔ͢ɽ

Fig. 4. Diffraction patterns of the adhesive during peeling process.

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Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)ਤ͔Β෼ΔΑ͏ʹɼԆ৳཰͕େ͖͍ҐஔͰ͸ɼ200ɼ

102ɼ201 ͷճં͕‫͞࡯؍‬Εͨɽ͜ΕΒͷճં‫౓ڧ‬͸೪ͷ݁থ૬͕ണ཭‫౓ڧ‬ͷ޲্ʹ‫د‬༩͍ͯ͠Δͱߟ͑ΒΕΔɽணࡎ͕ണ཭͞Ε͍ͯͳ͍Ԇ৳཰ 100 % (Z = 240 µm)
ͷҐஔͰ͸‫͞࡯؍‬Εͣɼണ཭͕ਐߦ͠೪ணࡎͷԆ৳཰

·ͱΊͱࠓ‫ޙ‬ͷ՝୊͕େ͖͘ͳΔʹͭΕঃʑʹ૿େ͠ɼԆ৳཰໿ 800 %(Z = 60 µm) ͷҐஔͰ࠷େͱͳͬͨɽ‫ʹٯ‬ɼFig. 4 ͰϦϯάঢ়ʹ‫͞࡯؍‬ΕΔΞϞϧϑΝεࢄཚ͸೪ணࡎͷԆ৳ͱ‫ʹڞ‬ঃʑʹ‫ݮ‬গ͍ͯ͠Δɽ͜Ε͸ɼ೪ணࡎ͕Ԇ৳͞ΕΔʹͭΕͯ೪ணࡎதͷΞϞϧϑΝε੒෼͕݁থԽ
݁͠থԽ౓͕૿͍ͯ͠Δ͜ͱΛҙຯ͍ͯ͠ΔɽԆ৳཰͕࠷େͱͳΔ Z = 0 µm ͷҐஔͰ݁থ͔Βͷճં‫౓ڧ‬͕খ͘͞ͳ͕ͬͨɼ͜Ε͸೪ணࡎ͕গͣͭ͠ք໘͔Β
ണ཭͢Δ͜ͱʹΑΓɼ̭ઢͷඃরࣹମੵ͕‫ݮ‬গͨ͜͠ͱͷ݁ՌͰ͋Δͱߟ͑ΒΕΔɽҰํɼԆ৳཰ͷҟͳΔ֤Ґஔʹ͓͍ͯɼ݁থ͔ΒͷճંϐʔΫͷ൒Ձ෯ʹ΄΅มԽ͕‫ݟ‬ΒΕͳ͍ɽ͜Ε͸ɼ೪ணࡎͷԆ৳ͱ‫݁ʹڞ‬থԽ౓͸૿Ճ͢Δ͕ɼ݁থ૬ͷ഑޲౓͸݁থ૬͕ग़‫ݱ‬ͨ͠ͱ͖͔Β΄΅มԽ͕ແ͍͜ͱΛ͍ࣔͯ͠Δɽͭ·Γɼ݁থ૬͸ग़‫ͱݱ‬ಉ࣌ʹ഑޲͓ͯ͠Γɼ഑޲౓͸Ұൠతͳ݁থੑߴ෼ࢠͷԆ৳഑޲ੑʹൺ΂ͯɼҾͬுΓ

SPring-8 BL24XU ʹϚΠΫϩ޿֯ࢄཚ૷ஔΛߏஙͨ͠ɽຊ૷ஔͷҐஔ෼ղೳ͸ԣํ޲ 43 µmɼॎํ޲

12 µm Λୡ੒͍ͯ͠ΔɽࢼྉҐஔʹরࣹ͞ΕΔ̭ઢͷ‫౓ڧ‬͸ 1 × 1010 photons/sec Ͱ͋Δɽ·ͨɼຊޫֶ‫ܥ‬Λ༻͍ͯɼണ཭աఔ͓͚Δ೪ணࡎͷߏ଄มԽͷͦͷ৔‫࡯؍‬Λߦͬͨͱ͜Ζɼ‫ײ‬ѹ೪ணςʔϓதͷఱવΰϜ݁থԽաఔΛॳΊͯ‫͢࡯؍‬Δ͜ͱ͕Ͱ͖ͨɽ͜ΕΒͷ݁থԽ૬͸ɼ‫ײ‬ѹ೪ணςʔϓͷണ཭‫ڧ‬౓ͷิ‫ͯ͠ͱࡎڧ‬ಇ͍͍ͯΔͱߟ͑ΒΕΔɽࠓ‫ޙ‬͸ɼఆྔతʹ΋ߋͳΔଌఆΛߦ͏༧ఆͰ͋ΓɼఱવΰϜ‫ܥ‬Ҏ֎ͷ೪ணࡎͷ‫ڍ‬ಈʹ͍ͭͯ΋‫ݕ‬౼͍ͨ͠ɽ
ࢀߟจ‫ݙ‬[1] S. Toki, I. Sics, S. Ran, L. Liu, Hsiao S.
Benjamin, S. Murakami, K. Senoo, and S.
Kohjiya: Macromolecules 35, 6578-6584 (2002).

ํ޲ʹߴ౓ʹ഑޲͍ͯ͠Δ͜ͱ͕໌Β͔ʹͳͬͨɽ͜

– 74 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

BL24XU

2011B3253, 2012A3253, 2012B3253

ϚΠΫϩ XAFS ޫֶ‫૷ݧ࣮ͱܥ‬ஔͷελσΟ

Study of X-ray Optics and Experimental Setup
for Micro-XAFS Measurementഷ ࿨ً 1 ɼඌ্ ‫و‬༸ 1 ɼԣࢁ ࿨࢘ 2,3 ɼ஛ా ৾‫ ޗ‬4 ɼ௡ࡔ Ղ޾ 1 ɼদҪ ७࣐ 2,3
Kazuki Hazama1 , Takahiro Onoue1 , Kazushi Yokoyama2,3 , Shingo Takeda3 ,Yoshiyuki Tsusaka1 , Junji Matsui2,31ฌ‫ཱݝݿ‬େֶେֶӃ෺࣭ཧֶ‫ڀݚ‬Պɼ2 ʢެࡒʣͻΐ͏͝Պֶٕज़‫ڠ‬ձ์ࣹޫφϊςΫ‫ॴڀݚ‬ɼ
3ʢࠃେ๏ʣਆ‫ށ‬େֶ࿈‫ܞ‬૑଄ຊ෦ɼ4 εϓϦϯάΤΠταʔϏε‫ࣜג‬ձࣾ1

2

Graduate School of Material Science, University of Hyogo,
Synchrotron Radiation Nanotechnology Laboratory, Hyogo Science and Technology Association,
3

Center for Collaborative Research and Technology Department, Kobe University,
4
SPring-8 Service Co. Ltd.

֓ཁɿɹຊ՝୊Ͱ͸ɼΫϦʔϯΤωϧΪʔ෼໺ʹ͓͍ͯɼಛʹϦν΢ϜΠΦϯೋ࣍ి஑ͷਖ਼‫ۃ‬΍ɼ‫ݻ‬ମ೩ྉి஑ͷΠΦϯ఻ಋମͷࡐྉ։ൃʹ޲͚ͨධՁखஈͱͯ͠ɼϚΠΫϩ XAFS ͷ‫ػ‬ೳ࣮‫ݱ‬Λ໨తͱͯ͠औΓ૊ΜͰ͍ΔɽBL24XU ͷߴً౓ޫ‫ݯ‬Λ‫͠༻׆‬ɼ࠷ॳͷࢼΈͱͯ͠ϛΫϩϯαΠζͷҐஔ෼ղೳੑೳΛ༗͢Δઐ༻ޫֶ‫ܥ‬Λࢼ࡞͠ɼੑೳධՁΛߦͬͨɽධՁʹ͸Ϧν΢ϜΠΦϯೋ࣍ి஑ͷ࣮ࡐྉΛ༻͍࣮ͯࢪͨ͠ɽ՝୊΍ߴ‫ػ‬ೳԽͷରԠʹ͍ͭͯ΋੔උΛਐΊͭͭɼ࢈‫ۀ‬քϢʔβʔʹରͯ͠ຊ‫ػ‬ೳΛఏ‫͢ڙ‬Δ༧ఆͰ͋ΔɽΩʔϫʔυɿɹϚΠΫϩ XAFSɼ஝ి஑ɼϦν΢ϜΠΦϯೋ࣍ి஑ɼ೩ྉి஑ɼߏ଄ධՁ

ͷ੔උΛߦ͍ɼ࢈‫ۀ‬քϢʔβʔͷ‫ྗڠ‬Λಘͳ͕Β࣮ࡐഎ‫ڀݚͱܠ‬໨త̭ઢ‫ٵ‬ऩ෼ޫ๏Ͱ͸ɼ̭ઢճંʹΑΔ݁থߏ଄ධՁ

ྉ΁ͷԠ༻Λऔ૊Ή͜ͱΛ໨తͱ͍ͯ͠ΔɽͰ͸ಘΒΕͳ͍‫ߏॴہ‬଄ʹؔ͢Δ৘ใ͕ղੳͰ͖Δͱͱ΋ʹɼిࢠ‫ܥ‬ͷঢ়ଶΛߟ࡯͢ΔͨΊͷ৘ใ΋Ҿ͖ग़͢͜ͱ͕ՄೳͰ͋Δɽฌ‫ݝݿ‬ϏʔϜϥΠϯʹ͓͍ͯɼ࢈‫ۀ‬ք޲͚ͱͯ͠ఏ‫͍ͯ͠ڙ‬Δ XAFS ʹؔͯ͠͸ɼΫϦʔϯΤωϧΪʔʹؔ܎͢Δ֤छ஝ి஑΁ͷར༻͕૿
͍͑ͯΔʢFig. 1ʣɽ஝ి஑ࡐྉͷ։ൃͰ͸ɼి஑ͷߴ༰ྔԽ΍௕ण໋ԽΛ࣮‫͢ݱ‬ΔͨΊͷࡐྉ։ൃΛޮ཰Α͘ਐΊΔ໨తͰɼXAFS Λར༻ͨ͠ߏ଄ղੳ͕ར
༻͞Ε͍ͯΔɽ‫ࢠݪ‬Ϩϕϧͷ‫ߏॴہ‬଄৘ใɼ͋Δ͍͸

Fig. 1. Schematic image for X-ray microbeam appli-ిࢠ‫ܥ‬ͷঢ়ଶʹؔ͢Δ৘ใΛ୳Δ͜ͱͰɼ൓ԠͷϝΧ

cation.

χζϜΛղ໌͢Δૂ͍͕͋Δɽ͜ͷΑ͏ͳঢ়‫͍͓ʹگ‬ͯɼߴҐஔ෼ղೳͷੑೳΛ༗͢Δ̭ઢճં๏΍̭ઢ‫ٵ‬࣮‫ݧ‬ऩ෼ޫ๏͕༗ޮͳπʔϧͱͳΓ͏Δɽ

஝ి஑ࡐྉΛ͸͡Ίͱ͢ΔࡐྉͷඍখྖҬ෼ੳͰҎ্ͷഎ‫ܠ‬ͷ΋ͱͰɼຊར༻՝୊͸ BL24XU [1] ͕͸ɼ໨తʹԠͯ͡ϛΫϩϯαΠζ͔ΒφϊαΠζʹࢸ༗͢Δ̭ઢूޫٕज़ΛԠ༻ͨ͠ϚΠΫϩ XAFS ‫ػ‬ೳΔ͞·͟·ͳεέʔϧͰͷҐஔ෼ղೳ͕‫ٻ‬ΊΒΕ͍ͯ– 75 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)໘ʹϩδ΢Ϝ૚Λίʔτͨ͠΋ͷΛ࠾༻͠ɼ഑ஔۭؒ
Λߟྀͯ͠ 100 mm ௕ͱͨ͠ɽ̎ຕΛਫฏ෼ࢄ഑ஔ
ͱ͢Δߏ੒ͱ͍ͯ͠Δɽ͜ΕʹΑΓɼޮՌతʹߴ࣍ޫ੒෼Λ཈੍͢Δ͜ͱ͕ՄೳͰ͋Δͱͱ΋ʹɼϛϥʔޫֶ‫ܥ‬ͷલ‫͚͓ʹޙ‬Δޫ࣠ͷฏߦੑΛ֬อ͍ͯ͠Δɽ̎ຕͷ̭ઢશ൓ࣹϛϥʔ͸ɼ্ྲྀଆ͕ฏ൘λΠϓɼԼྲྀଆ͕γϦϯυϦΧϧ‫ܗ‬ঢ়ͷ΋ͷͰ͋Δɽ͍ͣΕ΋ਆ௡ਫ਼‫ػ‬੡Ϟϯϒϥϯεςʔδ্ʹ౥ࡌ͠ɼਫ਼ີͳҐ

Fig. 2. Schematic view of X-ray optics for micro-ஔ੍‫ޚ‬ΛՄೳͱ͍ͯ͠ΔɽಛʹԼྲྀଆϛϥʔʹ͍ͭͯ

XAFS measurements. Using a double mirror system,
the content of higher order harmonic can be reduced͸ɼτϠϚ੡ͷϛϥʔ࿷‫૷ۂ‬ஔΛ࢖༻ͯ͠ࢼྉҐஔʹ

sufficiently low. A monochromatic X-ray beam is
focused on a sample using a bent-cylindrical mirror.

ঢ়ͷ‫཰ۂ‬൒‫ܘ‬͸ 4 mm ͱখ͍͞ઃ‫ܭ‬஋Λ࠾༻ͨ͠ɽ

͓͚Δ̎࣍‫ޫूݩ‬Λ࣮‫͍ͯ͠ݱ‬ΔɽγϦϯυϦΧϧ‫ܗ‬࣮‫ݧ‬ϋον B2 ಺ͷޫֶ‫ܥ‬෦෼͸ɼѴ޻‫ॴۀ‬੡ΞΫϦϧνϟϯόʹऩೲ͠ɼϔϦ΢Ϝงғ‫͢ͱؾ‬Δ͜ͱ͕

ΔɽBL24XU Ͱ͸ɼ࢈‫ۀ‬քϢʔβʔͷχʔζΛ࢕͍ͭՄೳͰ͋Δɽଌఆ‫ܥ‬෦෼ͱ෼཭࣮ͨ͠‫ݧ‬Ս୆্ʹޫֶͭɼૢ࡞ͷ؆ศੑɼࢼ࡞తͳࢼΈɼ੔උίετͱ͍ͬ‫ܥ‬Λ഑ஔͨ͠ɽ

ͨ఺Λߟྀ͠ɼϛΫϩϯαΠζͷҐஔ෼ղೳੑೳΛ༗ޫֶ‫ʹܥ‬͸ɼνϟωϧΧοτ݁থ΋ซઃ͍ͯ͠Δɽ

͢ΔϚΠΫϩ XANES Λ੔උ͢Δ͜ͱΛ໨ඪͱͨ͠ɽ

෼ޫ‫ͱث‬ͷؒͰ (ʴʵʵʴ) ഑ஔͷߏ੒Ͱ͋Γɼ‫ޙ‬ड़ର৅ͱ͢Δ࢈‫ۀ‬෼໺͸ɼϦν΢ϜΠΦϯೋ࣍ి஑ͷͷΑ͏ʹΤωϧΪʔͷ֦͕Γ͕খ͍̭͞ઢϏʔϜ‫ܗ‬੒ਖ਼‫ࡐۃ‬΍ɼ೩ྉి஑ͷΠΦϯ఻ಋମͰ͋Γɼࡐྉʹ‫ؚ‬΋Մೳͱ͍ͯ͠Δɽ

·ΕΔୈҰભҠۚଐ‫ݩ‬ૉʢओʹϚϯΨϯ͔Βχοέϧ
ͷൣғʣͷ K ‫ٵ‬ऩ୺ۙ๣Ͱͷ XANES ධՁͰ͋Δɽ
̍ʣϚΠΫϩ XAFS ͷ̭ઢޫֶ‫ܥ‬ͷ੔උ̎ʣࢼྉଌఆ෦෼ͷ੔උࢼྉଌఆ෦ʹ͍ͭͯͷશମུ֓ਤΛ Fig. 3 ʹࣔ͢ɽ͜͜Ͱ͸ɼޫֶ‫ͱܥ‬෼཭͢Δ‫Ͱܗ‬ઐ༻Ս୆Λ४උ͠ɼϚΠΫϩ XAFS ଌఆʹཁ͢Δޫֶ‫͍ͯͭʹثػܥ‬͜ͷ্ʹ‫ݕ‬ग़‫ث‬ɼࢼྉεςʔδΛ഑ஔ͍ͯ͠Δɽ

͸ɼຊ೥ใʮฌ‫ݝݿ‬ϏʔϜϥΠϯ BL24XUʯਤ 1ʢ13

ूޫϛϥʔ͕ࣔ͢ूޫ‫཭ڑ‬͸ 250 mm લ‫͋Ͱޙ‬Γɼϖʔδʣʹࣔ͢ʮߴ෼ղೳ XAFS εςʔγϣϯʯɼ͢͜ͷ‫ݶ‬ΒΕͨϫʔΩϯάεϖʔεʹೖࣹ‫౓ڧ‬Ϟχλ༻ͳΘͪɼγϦίϯೋ݁থ෼ޫ‫ث‬ͷԼྲྀʹ͋Δ࣮‫ݧ‬ϋοͷΠΦϯνΣϯόɼΨʔυεϦοτɼࢼྉεςʔδΛν B2 ಺ʹ഑ஔ͍ͯ͠ΔɽFig. 2 ʹࣔ͢Α͏ʹɼूޫ

഑ஔ͢Δඞཁ͕͋Δɽೖࣹ‫౓ڧ‬Ϟχλ༻ͱ͢ΔΠΦϯޫֶ‫ܥ‬ͷओͳߏ੒ཁૉ͸ɼInsync Inc. ੡Ͱ͋Δ̭ઢ

νΣϯόʹ͸ɼ࣮ޮి‫ۃ‬௕͕ 33 mm Ͱ͋Δখ‫ܕ‬λΠશ൓ࣹϛϥʔΛ࠾༻͍ͯ͠Δʢ‫ࣜג‬ձࣾΞόϯηʣɽϓΛ࠾༻ͨ͠ʢԠ༻ޫ‫ݚ‬੡ S-1329AʣɽΨʔυεϦο̭ઢશ൓ࣹϛϥʔͷ࢓༷͸ɼੴӳΛ‫ج‬൘ͱͯͦ͠ͷද

Fig. 3. Overview diagram of the experimental apparatus for micro-XAFS measurement.

– 76 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू
τͷ‫ػ‬ೳ΋ίϯύΫτʹऩΊΔͨΊɼΠΦϯνΣϯόXAFS ଌఆͷ࣮ߦʹ͸ɼJASRI ͷ XAFS άϧʔϓͷ૭෦ʹεϦοτ౥ࡌ෦Λઃ͚ͯɼ‫ݕ‬ग़‫ث‬શମΛҐஔ͕։ൃͨ͠ GUI ࢓༷ͷϓϩάϥϜΛ࠾༻͍ͯ͠Δɽ੍͜‫͖Ͱޚ‬Δࣗಈεςʔδ্ʹ౥ࡌ͍ͯ͠Δɽ͜ΕʹΑͷ΄͔ૢ࡞ੑΛߟྀͨ͠ϓϩάϥϜΛஞ࣍੔උ͠ɼ࢈

Γɼޫֶ‫ܥ‬ௐ੔ͱଌఆΛޮ཰Α࣮͘ߦՄೳͱ͍ͯ͠Δɽ‫ۀ‬քϢʔβʔ͕‫ྗۃ‬ར༻͠қ͍‫ڥ؀‬Λఏ‫͍ͯ͠ڙ‬Δɽ

ϚΠΫϩϏʔϜͷ෼ੳҐஔΛܾఆ͢ΔͨΊʹɼࢼྉ্ͷଌఆྖҬ෇ۙͰ‫̭ޫܬ‬ઢϚοϐϯάΛར༻͍ͯ͠

݁ՌΔɽ͜ͷͨΊɼϞʔλʔͷൃ೤ରࡦΛࢪͨ͠ਫ਼ີ‫ۦ‬ಈ̍ʣϚΠΫϩϏʔϜͷੑೳධՁεςʔδΛ࠾༻͍ͯ͠ΔɽධՁର৅‫ݩ‬ૉ͕ୈҰભҠۚଐ‫ݩ‬ૉͰ͋ΔͨΊɼ‫ ޫܬ‬XAFS ଌఆ࣌Λߟྀͯ͠ɼࢼ
ྉपล෦ʹ͸ςϑϩϯࡐ౳ͷथࢷࡐྉΛ࠾༻ͨ͠ɽ࣮
ࡍʹ࢖༻͞Εͨࢼྉεςʔδपลͷ༷ࢠΛ Fig. 4 ʹࣔ͢ɽమ‫ݩ‬ૉͷ K ‫ٵ‬ऩ୺ΤωϧΪʔ෇ۙʹ͓͍ͯूޫௐ
੔ΛߦͬͨɽޫࢠΤωϧΪʔ 7100 eV Ͱूޫௐ੔Λߦ͍ɼϏʔϜϓϩϑΝΠϧͷධՁΛ࣮ߦͨ͠ɽ௚‫ ܘ‬100µm Ͱ͋Δϓϥνφ੡ࡉઢΛར༻ͨ͠φΠϑΤοδ૸ࠪ๏Ͱ͋ΔɽूޫεϙοτΛԣஅ͢ΔΑ͏ࡉઢΛࢼྉεςʔδͰ૸ࠪ͠ɼࡉઢ‫΁ํޙ‬ͷಁա̭ઢ‫౓ڧ‬Λଌఆ͠ɼղੳॲཧΛߦ͏͜ͱͰϏʔϜϓϩϑΝΠϧΛ֬ೝͨ͠ɽ

Fig. 4. Photograph showing the sample stage. SamR
plate to avoidples were mounted on the Teflon
background signals for fluorescence-XAFS experiments.
XAFS ৴߸ͷ‫ݕ‬ग़͸ɼಁա XAFS ༻ͱͯ͠ΠΦϯνΣϯόΛ࢖༻͢Δɽ‫ ޫܬ‬XAFS ༻ʹ͸̎ͭͷ‫ݕ‬ग़‫ث‬Λඋ͓͑ͯΓɼRONTEC ੡ XFlash ‫ݕ‬ग़‫ث‬ʢηΠίʔɾΠʔδʔΞϯυδʔ‫ࣜג‬ձࣾʣɼΩϟϯϕϥ੡ 19ૉࢠ൒ಋମ‫ݕ‬ग़‫ث‬ʢGe ૉࢠʣΛར༻Մೳͱͨ͠ɽ19ૉࢠ൒ಋମ‫ݕ‬ग़‫͍ͯͭʹث‬͸ϢʔβʔʹΑΔૢ࡞ͷ؆ศੑΛߟྀ͠ɼXIA ੡ͷσδλϧ৴߸ॲཧγεςϜΛ
࠾༻͍ͯ͠Δʢਔ໦޻ܳ‫ࣜג‬ձࣾʣɽ‫ ޫܬ‬XAFS ଌఆ࣌Ͱ͸஄ੑࢄཚͷ৴߸੒෼Λ཈੍͢Δ໨తͰɼLytle‫ݕ‬ग़‫ث‬λΠϓͷ‫ܗ‬ঢ়Λ༗͢ΔΞϧϛ੡ιʔϥʔεϦοτΛઃ‫ܭ‬ɼ੡࡞ͨ͠ɽ‫ݕ‬ग़‫͍ͯͭʹث‬͸ɼࣼग़ࣹ഑ஔ
͢ΔεϥΠυεςʔδ্ʹ౥ࡌ͠ɼ‫ݕ‬ग़‫ث‬ͷ‫ݻ‬ఆҐஔ

Fig. 5. Profiles of X-ray microbeam evaluated. To
evaluate the beam profiles, knife-edge scans are per-Λઃఆ͠΍͍ͯ͘͢͠Δɽ‫ ޫܬ‬X ઢ‫ݕ‬ग़‫͍ͯͭʹث‬

formed using a 100-µm-diameter platinum wire in΋ࢼྉεςʔδ෦ͷՍ୆ͱ෼཭഑ஔ͍ͯ͠Δɽ(a) vertical and (b) horizontal directions.

Λ༰қʹઃఆՄೳͱ͢ΔͨΊɼϩϯάετϩʔΫΛ༗

– 77 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)̭ઢશ൓ࣹϛϥʔͷࢹࣼ֯৚݅͸ 0.4 ౓Ͱ͋Δɽಁ

Πϝϯτ࡞‫ۀ‬લʹޫ࣠ධՁΛߦͬͨ݁ՌͰ͋Δɽχοա‫౓ڧ‬ͷඍ෼ॲཧʹΑͬͯಘͨϏʔϜϓϩϑΝΠϧΛ

έϧͷ XANES ྖҬ෇ۙʹରͯ͠ɼࢼྉҐஔʹ͓͚Δ

Fig. 5 ʹࣔ͢ɽԖ௚ํ޲͓Αͼਫฏํ޲ͦΕͧΕͼͷޫ࣠ҐஔΛԖ௚͓Αͼਫฏͷ྆ํ޲Ͱଌఆͨ͠ɽ͍ͣ

ϏʔϜ෯͸ɼ൒஋શ෯Ͱ 1.0 µm ͓Αͼ 1.8 µm Ͱ͋ͬΕ΋‫׈‬Β͔ͳυϦϑτ‫ڍ‬ಈΛ͍ࣔͯ͠ΔɽԖ௚ํ޲ͷͨɽ͜ͷ৔߹ͷɼԼྲྀଆϛϥʔͷத৺͔ΒूޫҐஔ·υϦϑτ‫ڍ‬ಈʹؔͯ͠͸ɼγϦίϯೋ݁থ෼ޫ‫ث‬ͷୈ9Ͱͷ‫཭ڑ‬͸໿ 280 mm Ͱ͋ΔɽϏʔϜ‫౓ڧ‬͸ 2.9×10

Ұ݁থͷૢ࡞ʹ࢖༻͢Δฒਐ͕࣠༗͢ΔϤʔΠϯάɼ

photons/sec Ͱ͋ΔɽϐονϯάʹґΔ΋ͷͱߟ͑ͨɽਫฏํ޲ʹ͍ͭͯ͸ϚΠΫϩ XAFS ଌఆͷؒ͸ɼৗʹࢼྉ্ͷಉҰҐఆҐஔग़ࣹͷϛεɾΞϥΠϝϯτͱࢥΘΕΔɽ

ஔΛ̭ઢ͕রࣹ͢Δඞཁ͕͋Δɽ͜ΕΛཚ͢ཁҼͱ͜͠ͷޫֶ‫ܥ‬ͷॳ‫ظ‬ঢ়ଶʹରͯ͠ɼ‫ز‬Կޫֶతͳ‫ݕ‬౼ͯ͸ޫֶૉࢠͷΞϥΠϝϯτෆ଍ɼεςʔδϞʔλ͔Λߦ͍ͳ͕Βޫֶ‫ܥ‬ͷΞϥΠϝϯτ࡞‫ۀ‬Λ࣮ߦͨ͠ɽ

Βͷൃ೤ʹΑΔεςʔδͷυϦϑτɼϋον಺ͷࣨԹௐ੔‫ޙ‬ͷ݁ՌΛ Fig. 7 ʹࣔ͢ɽޫࢠΤωϧΪʔͷૢ΍ۭ‫ؾ‬ͷରྲྀͷӨ‫͑ߟ͕Ͳͳڹ‬ΒΕΔɽ࡞ൣғʹ͓͍ͯɼυϦϑτྔΛϏʔϜαΠζΑΓ΋̍ޫֶૉࢠͷΞϥΠϝϯτ࡞‫͍ͯͭʹۀ‬ɼχοέϧͷܻখ͍͞αΠζʹ཈͑͑Δ͜ͱ͕Ͱ͖ͨɽυϦϑτྔK ‫ٵ‬ऩ୺ۙ๣Ͱ࣮ߦͨ݁͠ՌΛࣔ͢ɽFig. 6 ͸ɼΞϥΛ͞Βʹ཈੍͢ΔͨΊɼޫࢠΤωϧΪʔΛεςοϓ૸

Fig. 6. Microbeam stability measurement showing

Fig. 7. Microbeam stability measurement showing

position drift features of optical axes in (a) verticaland (b) horizontal directions against photon energy

position drift features of optical axes in (a) vertical and (b) horizontal directions against photon en-

before precise optical alignment. Knife-edge scans
are performed at several points in the 8150-8500 eV

ergy after precise optical alignment. The stability isfound to be improved.

energy range.

– 78 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

Fig. 8. Sample for the first feasibility study of X-ray microbeam. Cathode materials of LiNiO2 -based lithiumion battery is used.

Fig. 9. Nickel X-ray fluorescence intensity distribution map of the sample when the X-ray microbeam isscanned over the sample cross-section.

ࠪ͢Δ౎౓ɼ֤ޫֶૉࢠͷҐஔͷิਖ਼ྔΛௐ੔ͨ͠ɽ

ޫ࣠ͷ҆ఆੑධՁͰ͸ɼLiNiO2 ‫׆‬෺࣭͕थࢷதʹूޫੑೳʹ͍ͭͯ͸ɼޫࢠΤωϧΪʔ૸ࠪൣғͰ 0.3

ຒΊࠐ·Εͨ΋ͷΛ࢖༻ͨ͠ɽॆ์ిαΠΫϧ͸ະ࣮µm ͷมಈ෯಺ʹ͋Δ͜ͱΛ֬ೝͨ͠ɽ

ࢪͰ͋Δɽ͜ΕͷϚοϐϯάଌఆΛ࣮ࢪ͠ɼ‫ྖ࡯؍‬ҬϚΠΫϩϏʔϜʹΑΔ‫ޫܬ‬ϚοϐϯάଌఆͰ͸ɼ௕ͷද໘૚ͷཻࢠ෼෍ͷ‫࡯؍‬Λɼ‫̭ޫܬ‬ઢϚοϐϯάଌ࣌ؒɼࢼྉεςʔδΛ࿈ଓૢ࡞ͤ͞Δɽ͜ͷͨΊϞʔఆͰࢼΈͨɽଌఆ༻ࢼྉ͸ɼFig. 8 ͷࣸਅ͓Αͼஅλʔ͔Βͷൃ೤ͷӨ‫͕ڹ‬༧૝͞Ε͕ͨɼ͜ͷ఺ʹ͍ͭ໘໛ࣜਤʹࣔ͢Α͏ʹਖ਼‫ۃ‬அ໘Ͱ͋Δɽೖࣹ̭ઢͷޫͯ͸Ϟʔλʔຊମͱεςʔδ෦ͱͷؒʹஅ೤ࡐΛૠೖࢠΤωϧΪʔ͸χοέϧͷ K ‫ٵ‬ऩ୺ۙ๣Ͱબ୒ͨ͠ɽ

͢ΔରࡦΛ࠾༻ͨ͠ɽ

SDD ‫ݕ‬ग़‫ث‬Λ࢖༻͠ɼχοέϧ‫ݩ‬ૉ͔Βͷ Kα ઢΛϋον಺ͷ‫ڥ؀‬ରࡦʹ͍ͭͯ͸ɼҰ࿈ͷଌఆͷؒ͸‫ͨ͠࡯؍‬ɽͦͷ݁ՌΛ Fig. 9 ʹࣔ͢ɽ‫̭ޫܬ‬ઢ‫౓ڧ‬‫ྗۃ‬ɼ࣮‫ݧ‬ϋονͷ։ดૢ࡞Λආ͚ΔΑ͏ʹ஫ҙΛͷ̎࣍‫ݩ‬ίϯτϥετύλʔϯ্Ͱɼཻࢠͷ෼෍ͷ༷෷͍ͬͯΔɽ

ࢠΛ֬ೝ͢Δ͜ͱ͕Ͱ͖ͨɽ

LiCoO2 ਖ਼‫ʹࡐۃ‬ରͯ͠ϚΠΫϩ XAFS ΛԠ༻ͨ̎͠ʣϦν΢ϜΠΦϯೋ࣍ి஑ࡐྉ΁ͷԠ༻BL24XU ʹ͓͍ͯߏஙͨ͠ϚΠΫϩ XAFS ͷੑೳ݁ՌΛ࣍ʹࣔ͢ɽଌఆ஋Λܾఆ͢ΔͨΊɼίόϧτ‫ݩ‬ΛධՁ͢Δ໨తͰɼϦν΢ϜΠΦϯೋ࣍ి஑ͷਖ਼‫ࡐۃ‬ૉ͔Βͷ Kα ઢΛར༻ͨ͠‫̭ޫܬ‬ઢϚοϐϯάΛߦͬͷଌఆΛࢼΈͨɽͨɽྭ‫̭ͨ͠༻࢖ʹى‬ઢͷޫࢠΤωϧΪʔ͸ 7800 eV– 79 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)
Ͱ͋Δʢίόϧτͷ K ‫ٵ‬ऩ୺ΤωϧΪʔ͸ 7709 eVʣɽ

Fig. 10 ʹͦͷ݁ՌΛࣔ͢ɽίϯτϥετΠϝʔδ্Ͱ‫׆‬෺ཻ࣭ࢠͷ෼෍ͷ༷ࢠΛଊ͑ɼ͜ͷσʔλ্ͰϚΠΫϩ XAFS ͷଌఆҐஔΛܾఆͨ͠ɽ

Fig. 10. Cobalt X-ray fluorescence intensity distribution map of the sample when the X-ray microbeam isscanned over the sample cross-section. Cathode materials of LiCoO2 -based lithium-ion battery is usedin this case.
‫ ޫܬ‬XANES ͷଌఆ݁ՌΛ Fig. 11 ʹࣔ͢ɽK ‫ٵ‬ऩ୺͕‫ݱ‬ΕΔޫࢠΤωϧΪʔҐஔʹ஫໨͢ΔͱɼຆͲͷ

Fig. 11. (a) Cobalt K-edge XANES spectra after৔ॴͰॆ์ిʹ൐͏ίόϧτͷՁ਺มԽͱҰக͢Δ‫ڍ‬charge and discharge reactions and (b) their detailaround the absorption edge.

ಈͰ͋ͬͨɽͨͩ͠ॆి‫ʹޙ‬ධՁΛߦͬͨࢼྉʹ͍ͭͯ͸ɼද໘ۙ๣ʹ͓͍ͯબ୒ͨ͠෼ੳҐஔʹ͓͍ͯ์BL24XU ͷϚΠΫϩ XAFS ʹ͍ͭͯɼ࢈‫ۀ‬քϢʔిঢ়ଶʹ૬౰͢ΔϓϩϑΝΠϧΛ֬ೝͨ͠ɽ
Ҏ্ͷ݁Ռ͸ɼϚΠΫϩ XAFS ͕ॆ์ిϓϩηεβʔ΁ͷར༻֦େΛਤΔͨΊҎԼͷऔΓ૊ΈΛਐΊΔɽʹ͓͚Δߏ଄มԽΛɼҐஔΛ۠ผͯ͠ධՁՄೳͰ͋Δ

̍ʣXAFS εϖΫτϧଌఆͷΤωϧΪʔߴ෼ղೳԽ

͜ͱΛࣔ͢΋ͷͱߟ͑ΒΕΔɽྼԽաఔ΍ߴ༰ྔԽͱ

ࡐྉதͰͷΠΦϯ఻ಋʹ͍ͭͯ͸ɼ‫׆‬෺ཻ࣭ࢠશମ

ߏ଄ͱͷ૬ؔੑΛɼి‫্ۃ‬ͷҐஔΛ۠ผͯ͠ৄ͘͠ௐ

͋Δ͍͸ද໘૚ͷߏ଄࿪Έ͕Ө‫͠ڹ‬ɼσόΠεੑೳΛ΂Δ͜ͱ͕Ͱ͖Δ΋ͷͱ‫ظ‬଴͞ΕΔɽ

ࢧ഑͢ΔՄೳੑ͕ߟ͑ΒΕΔɽ͜ͷ࿪Έͷ༷ࢠΛৄ͘͠ௐ΂Δ໨తͰɼΤωϧΪʔ෼ղೳੑೳΛߴΊΔޫֶ·ͱΊͱࠓ‫ޙ‬ͷ՝୊‫ܥ‬ͷ࠾༻Λ‫ݕ‬౼͢Δɽྫ͑͹஫໨‫ݩ‬ૉͷपΓʹ͋Δࢎ

஝ి஑෼໺ͷϢʔβʔχʔζΛҙࣝ͠ɼඍখྖҬͷධՁΛՄೳͱ͢ΔϚΠΫϩ XAFS ͷଌఆ‫ܥ‬Λ੔උ͠ૉʹ͍ͭͯɼཱମతͳ഑ҐରশੑΛ൓өͨ͠৴߸ΛऔಘՄೳͱ͢ΔɽΤωϧΪʔ෼ղೳΛߴΊͨޫֶ‫Ͱܥ‬ɼͨɽϛΫϩϯαΠζͷҐஔ෼ղೳΛ࠷ॳͷ໨ඪͱ͠ɼ

pre-edge ྖҬʹ‫ݱ‬ΕΔ‫ٵ‬ऩϐʔΫͷਫ਼ີ‫͍ͯͭʹ࡯؍‬γϦϯυϦΧϧϛϥʔΛར༻ͨ͠ूޫޫֶ‫ܥ‬Λ࠾༻͠͸ɼBL24XU ʹ͓͍ͯ‫ʹط‬औΓ૊ΜͰ͍Δɽ

Fig. 12 ͸ඪ४తͳޫֶ‫ܥ‬഑ஔͰͷ XAFS ଌఆͷͨɽޫֶ‫ܥ‬ௐ੔Λߦ͍ɼޫ࣠ͷ҆ఆԽΛਤͬͨɽ࠷ॳͷࢼΈͱͯ͠ɼϦν΢ϜΠΦϯೋ࣍ి஑ͷਖ਼‫ۃ‬໛ࣜਤͰ͋Δɽ͜ͷ৔߹ɼσϡϞϯυਤ (Du-MondࡐධՁʹԠ༻͠ɼ‫̭ޫܬ‬ઢϚοϐϯάɼϚΠΫϩ XAFS

diagram) ʹࣔ͢Α͏ʹɼ෼ޫ‫ͱث‬εϦοτ഑ஔͱͰଌఆͷ༗ޮੑΛ֬ೝ͢Δ͜ͱ͕Ͱ͖ͨɽ

ܾ·Δಛੑ૭͕ࣔ͢೾௕֦͕ΓΛ༗͢ΔϏʔϜͰͷ෼ੳධՁͱͳΔɽ– 80 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

Fig. 12. (a) Schematic view of X-ray optics in astandard XAFS measurement case and (b) a DuMond diagram of the reflected X-rays.
೾௕ͷ֦͕ΓΛ཈੍͢Δखஈͱͯ͠ɼFig. 13 ʹࣔ͢Α͏ʹɼSi 111 ൓ࣹͷ෼ޫ݁থͱɼSi 400 ൓ࣹ͋Δ
͍͸ Si 220 ൓ࣹͷ௥Ճ݁থΛʢʴ, ʴʣ഑ஔͱͯ͠࠾
༻͢Ε͹ɼଌఆ‫͕ࣔ͢ܥ‬෼ղೳΛߴΊΔ͜ͱ͕Մೳͱ
ͳΔ [2, 3] ʢFig. 13(b) ͓Αͼ (c) ࢀরʣɽ௥Ճ͢Δ

Fig. 13. (a) Schematic view of X-ray optics in ahigh-energy-resolution XAFS measurement case and෼ޫૉࢠͷ൓ࣹࢦ਺ʹΑΓɼ෼ղೳ͕ܾఆ͞ΕΔɽࢎ

Du-Mond diagrams of the reflected X-rays for (b)Si 111 + Si 400 reflections and (c) Si 111 + Si 220ૉ഑ҐʹΑͬͯ pre-edge ྖҬʹ‫ݱ‬ΕΔ‫ٵ‬ऩϐʔΫΛreflections.

ର৅ͱ͢Δ৔߹ɼϐʔΫ͕༗͢ΔΤωϧΪʔ෯ΛߟྀࢼྉΛ༻͍ͯɼద༻͢ΔΞϧΰϦζϜ͝ͱʹ‫ࢉܭ‬ਫ਼౓ͨ͠બ୒͕ՄೳͰ͋Δɽ
ूޫޫֶ‫ʹܥ‬ରͯ͠ߴ෼ղೳԽͷੑೳΛ෇Ճͨ͠৔
߹ɼ࣮༻తͳϨϕϧͷ̭ઢ‫͕౓ڧ‬ಘΒΕΔ͔൱͔͕໰

ͷ֬ೝΛߦ͏͜ͱ͕ඞཁͱߟ͑ΒΕΔɽ
̏ʣूޫϏʔϜͷαϒϛΫϩϯԽ

୊ͱͳΔɽҐஔ෼ղೳͱΤωϧΪʔ෼ղೳΛซཻͤ࣋ͭքྖҬͷධՁͳͲɼαϒϛΫϩϯͷҐஔ෼ղೳΛޫֶ‫͍ͯͭʹܥ‬ɼεϧʔϓοτੑೳ౳ͷධՁΛࠓ‫ߦޙ‬‫ٻ‬ΊΒΕΔ৔߹ʹରԠ͢ΔͨΊɼूޫޫֶ‫ܥ‬ͷվ଄Λ͏༧ఆͰ͋Δɽ‫ݕ‬౼͢ΔɽγεςϜ੔උʹ޲͚ͨϓϩδΣΫτఏҊ΋

̎ʣXANES σʔλղੳମ੍ͷ੔උϢʔβʔͱ૬ஊ࣮ͭͭ͠ࢪ͍ͨ͠ɽ

ଌఆ‫ߏ͍͓ͯʹޙ‬଄Λٞ࿦͢ΔࡍɼൺֱՄೳͳσʔ̐ʣԽֶঢ়ଶϚοϐϯά‫ػ‬ೳ

λϕʔε͕΄͍͠ɽ͜Ε͸ϚΠΫϩ XAFS ʹ‫ݶ‬Βͣྫ͑͹ɼి஑ͷॆ์ిաఔʹର͢Δߏ଄มԽ΍ߏ଄ࠓ‫ޙ‬ͷ՝୊ͱߟ͍͑ͯΔɽඪ४ࢼྉͷ࡞੒͕ϙΠϯτ࿪Έͷ෼෍ͷ༷ࢠΛɼΠϝʔδϯάख๏Λར༻ͯ͠ࢹʹͳΔɽ

֮తσʔλͱͯ͠දࣔ͢Ε͹ɼి஑ಛੑͱͷ૬ؔੑΛ·ͨɼ‫ࢉܭ‬Պֶతͳख๏ʹΑΔγϛϡϨʔγϣϯ [4]ΑΓৄ͘͠ཧղͰ͖Δͱߟ͑ΒΕΔɽ͜ΕΛ࣮‫͢ݱ‬Δ

΋‫༻׆‬Λߟ͍͑ͨɽ͜Εʹ͍ͭͯ΋ɼߏ଄‫ط‬஌Ͱ͋Δ– 81 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)̑ʣࡐྉ΁ͷԠ༻‫ڀݚ‬ϚΠΫϩ XAFS ͷ༗ޮੑΛੜ͔ͯ͠ɼࠓ‫ޙ‬͸‫ݻ‬ମ೩ྉి஑ࡐྉɼϦν΢ϜΠΦϯೋ࣍ి஑ࡐྉͳͲ΁ͷԠ༻‫ʹڀݚ‬औΓ૊Ή͜ͱͱ͍ͨ͠ɽ
ँ࣮ࣙ‫ݧ‬ΛਐΊΔʹ͋ͨΓɼ‫ࣜג‬ձࣾॅԽ෼ੳηϯλʔߴ‫͔༷ڮ‬Β͸‫و‬ॏͳධՁ༻ࢼྉͷ࡞੒ͱ͝ࢦಋΛ௖͍
ͨ. ·ͨɼຊར༻՝୊ʹؔ܎͢Δ‫͍͓ͯʹڀݚ‬ɼଟ͘ͷํʑʹ͝‫ྗڠ‬௖͍ͨɽ์ࣹޫʹؔ͢Δٕज़ɼ̭ઢޫ
ֶ͓Αͼଌఆٕज़ʹؔͯ͠ɼฌ‫ཱݝݿ‬େֶେֶӃ෺࣭ཧֶ‫ڀݚ‬Պ ࿜ౡ‫ڭ‬तɼ௡ࡔ।‫ڭ‬तɼߴ໺ॿ‫͔ڭ‬Β͝ࢦಋ௖͍ͨɽϏʔϜϥΠϯͷར༻ʹؔͯ͠ɼฌ‫ݝݿ‬ிͷؔ܎ऀͷօ༷ɼެӹࡒஂ๏ਓͻΐ͏͝Պֶٕज़‫ڠ‬ձ໺੉‫ڀݚ‬һɼ‫܂‬ຊ‫ڀݚ‬һɼཥ‫ڀݚ‬һɼ࣫‫ڀݚݪ‬һɼट౻༷ɼখྛ༷ɼ೔ࢁ༷ͷ͝‫ྗڠ‬ɼ͝ࢧԉΛ௖͍ͨɽֶ෦ࡏ੶͔࣌Β͜Ε·Ͱͷ̎೥ؒʹ͓͚Δ‫׆ڀݚ‬ಈʹ͓͍ͯɼ͝ࢦಋɼ͝‫ྗڠ‬௖͖·ͨ͠օ༷ʹ৺ΑΓ‫ײ‬ँக͠·͢ɽ

Fig. 14. Schematic image of 2-dimensional XAFS.
ࢀߟจ‫ݙ‬
खஈͱͯ͠ɼޫࢠΤωϧΪʔ૸ࠪͱϏʔϜরࣹҐஔͷ̎࣍‫ݩ‬ϚοϐϯάͱΛ૊Έ߹Θͤͨଌఆํ๏΋‫ݕ‬౼͍ͨ͠ɽՁ਺ͷҧ͍౳ɼҟͳΔঢ়ଶ͕෼෍͍ͯ͠Δ৔߹ɼ‫ٵ‬ऩ୺લ‫ޙ‬ͷޫࢠΤωϧΪʔʹ͓͍ͯऔಘ͢ΔϚοϐϯάσʔλؒͰࠩ෼ॲཧΛߦ͑͹ɼ̎࣍‫ݩ‬ͷίϯτϥ
ετύλʔϯͱͯ͠ঢ়ଶ෼෍Λද‫͖Ͱݱ‬Δ΋ͷͱߟ͑ΒΕΔ [5]ɽ
Πϝʔδϯάతͳଌఆखஈͱͯ̎࣍͠‫ݕݩ‬ग़‫ث‬Λ࠾༻͢Ε͹ɼ޿ൣғͷ XAFS ৘ใΛਝ଎ʹऔಘՄೳͰ
͋ΔʢFig. 14ʣɽͦͷ݁ՌΛ‫ʹج‬ɼಛఆҐஔʹ͍ͭͯϚΠΫϩ XAFS Λద༻͢Δํ๏΋༗ޮͰ͋Δͱߟ͑ΒΕΔɽ

[1] Y. Tsusaka, K. Yokoyama, K. Takai, S. Takeda,
Y. Kagoshima, and J. Matsui: Nucl. Instrum.
Methods A467-468, 670 (2001).
[2] L. Galoisy, G. Calas and M. A. Arrio: Chemical
Geology 174, 307 (2001).
[3] F. Farges, S. Rossano, Y. Lefr‘ere, M.Wilke, andG. E. Brown Jr.: Physica Scripta. T115, 957(2005).
[4] T. Tamura, T. Ohwaki, A. Ito, Y. Ohsawa,
R. Kobayashi, and S. Ogata: Modelling Simul.
Mater. Sci. Eng. 20, 045006 (2012).
[5] S. Iida, T. Noma, S. Hayakawa, M. Takahashi,
and Y. Gohshi: Japan. J. Appl. Phys. 32, Suppl.
32-2 160 (1993).

– 82 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

BL24XU

2010B3237, 2011A3237

̭ઢ 3D τϙάϥϑΟʔʹΑΔ 4H-SiC ‫ج‬ఈ໘సҐ͓Αͼ؏௨ਕঢ়సҐͷΠϝʔδϯά

X-ray Three-Dimensional Topography Imaging of Basal-Plane andThreading Edge Dislocations in 4H-SiC
ాপ ྑฏ 1 ɼ৿ େี 2 ɼ‫ ึޭ ాח‬1 ɼ౔ా लҰ 1
Ryohei Tanuma1 , Daisuke Mori2 , Isaho Kamata1 , Hidekazu Tsuchida11(Ұࡒ) ిྗதԝ‫ॴڀݚ‬ɼ2 ෋࢜ి‫)ג( ػ‬1
CRIEPI, 2 Fuji Electric Co., Ltd.

֓ཁɿɹ̭ઢ 3D τϙάϥϑΟʔʹΑΓ 4H-SiC ͷ‫ج‬ఈ໘సҐ (BPD) ͓Αͼ؏௨ਕঢ়సҐ (TED) ͷղੳΛߦͬͨɽసҐͷཱମը૾͔Β BPD ͷ 1 ͭ͸Τϐ/‫ج‬൘ք໘Ͱ TED ʹมԽ͠ɼଞͷ BPD ͸‫ج‬൘͔ΒΤϐ૚·Ͱ࿈ଓ͍ͯ͠Δ͜ͱ͕໌ྎʹ‫͖ͨͰ࡯؍‬ɽ̭ઢ 3D τϙάϥϑΟʔ͕ 4H-SiC ͷ BPD ͓Αͼ TED ʹे෼ద
༻Ͱ͖Δ͜ͱ͕Θ͔ͬͨɽΩʔϫʔυɿɹ X ઢτϙάϥϑΟʔɼࡾ࣍‫ݩ‬ɼ3Dɼ4H-SiCɼਕঢ়సҐɼ‫ج‬ఈ໘సҐഎ‫ڀݚͱܠ‬໨త࣍ੈ୅ిྗม‫׵‬ɾ੍‫ޚ‬ૉࢠͱ࣮ͯ͠༻Խ͕‫ظ‬଴͞Ε͍ͯΔ SiC όΠϙʔϥσόΠε (IGBTɼp-n μΠΦʔυͳͲ) ʹ͓͍ͯɼΦϯ఍߅૿େͷ‫ݪ‬ҼͱͳΔ‫ج‬ఈ໘సҐ (BPD) [1] Λ؏௨ਕঢ়సҐ (TED) ʹม‫͢׵‬Δ͜ͱʹΑͬͯɼͦͷີ౓Λ௿‫͢ݮ‬Δํ๏͕஫໨͞Ε͍ͯ
Δ [2]ɽ͔࣮͠͠༻্͸ม‫཰ޮ׵‬ͷ͞ΒͳΔ޲্͕ඞཁͰɼͦͷͨΊʹ͸ BPD-TED ม‫׵‬ͷϝΧχζϜղ໌͕ෆՄܽͰ͋Δɽ
̭ઢ 3D τϙάϥϑΟʔ͸؏௨ΒͤΜసҐ (TSD) ͷղੳʹେ͖ͳޮՌΛൃ‫͢ش‬Δ͜ͱ͕෼͔͍ͬͯΔ [3,4]ɽ
ࠓճͷ‫[ ڀݚ‬5] ͸͜ͷख๏Λ BPD ͓Αͼ TED ʹద༻ͯ͠ BPD-TED ม‫׵‬ͷϝΧχζϜղ໌ʹͭͳ͛Δ
͜ͱΛ໨తͱ͍ͯ͠Δɽ

Fig. 1. Setup of microbeam X-ray diffraction forthe 3D topography.

࣮‫ݧ‬ଌఆʹ༻͍ͨࢼྉ͸ɼްΈ 20 µm ͷΤϐ૚Λ༗̭͢ઢ 3D τϙάϥϑΟʔͷଌఆ͸ BL24XU Ͱ࣮ࢪ

Δ 4H-SiC ΢Τϋ (Φϑ֯ 8◦ ɼSi ໘) Ͱ͋Δɽ࣮‫ݧ‬͸

ͨ͠ʢFig. 1ʣɽଌఆʹ͸̭ઢϚΠΫϩϏʔϜ [ूޫSPring-8 ฌ‫ݝݿ‬ϏʔϜϥΠϯͰ࣮ࢪͨ͠ɻ̭ઢ 3D τ‫ ܘ‬1.9 µm(H) × 0.6 µm(V)ɼE = 15 keVɼൃࢄ֯ 25ϙάϥϑΟʔͷଌఆʹઌཱͪɼBL08B2 ʹ͓͍ͯ௨ৗ

µrad] Λ༻͍Δ [6]ɽൃੜ͢Δճં̭ઢ (g = [11212]ʣ

൓ࣹ̭ઢτϙάϥϑΟʔΛଌఆͨ͠ʢg = [1128]ɼEΛඍࡉεϦοτ (V-slit) [4, 5] ʹ௨͠ɼV-slit Λಁա͢= 8.046 keVʣɽΔϏʔϜΛγϯνϨʔγϣϯΧ΢ϯλ (SC) ʹಋ͍ͯ– 83 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)ͦͷ‫౓ڧ‬Λଌఆ͢Δɽࠓճ༻͍ͨ V-slit ͸։͖֯ 20◦ͷ΋ͷͰ͋Δɽ͜ͷํ๏Ͱࢼྉ಺෦ͷ఺ Q ʹ͓͚Δ
ճં‫౓ڧ‬ΛϐϯϙΠϯτଌఆ͠ɼࢼྉΛ 3D εΩϟϯ͢Δ͜ͱʹΑͬͯ 3D τϙάϥϑΟʔΛಘΔ [5]ɽ݁Ռ͓Αͼߟ࡯

Fig. 2 ͸௨ৗͷ൓ࣹ̭ઢτϙάϥϑΟʔΛΤϐ੒௕ͷલ‫Ͱޙ‬ଌఆͨ͠΋ͷͰ͋Δɽ͜ΕΒͷൺֱʹΑΓɼ‫ج‬൘தͷ 2 ͭͷ BPD(B1ɼB2) ͷ͏ͪ B1 ͸Τϐ/‫ج‬൘ք໘Ͱ TED(E1) ʹมԽ͠ɼB2 ͸ͦͷ··ΤϐதΛ఻೻ͯ͠ද໘·Ͱୡ͍ͯ͠Δ͜ͱ͕Θ͔Δɽ
ಉ͡ྖҬͰ 3D τϙ૾Λଌఆͨ݁͠ՌΛ Fig. 3 ʹࣔ͢ɽଌఆྖҬͷਂ͞͸ 30 µm Ͱ͋Δɽฏ໘ਤʢFig.

Fig. 2. Back reflection X-ray topographs obtained
before and after 4H-SiC epitaxial growth for the3(a)ʣʹ‫ݟ‬ΒΕΔ 2 ͭͷϐοτ͸ E1 ͱ B2 ʹରԠ͠same position.

͍ͯΔɽFig. 3(b)ɼ3(c) ͸ B1 ͕ਂ͞ 20 µm ͷΤϐ/Fig. 3. Stereographic views of BPDs (B1, B2) and a TED (E1). (a) The two pits visible in the top viewcorrespond to E1 and B2, (b) B2 propagates from the deep substrate to the epilayer, and B1 converts to E1
near the epilayer/substrate interface (20 µm deep). The high-intensity region (arrow in (b)) will be causedby surface strain. (c) B1 and B2 lie on the basal plane at an angle of 8◦ with the surface, and E1 is almost
parallel to the surface normal. (d)-(f) Based on the complicated morphologies between E1 and B2 (circles),we anticipate the interaction of dislocations with other defects, or with the epilayer/substrate interface.

– 84 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू
‫ج‬൘ք໘෇ۙͰ E1 ʹมԽ͠ɼB2 ͸‫ج‬ఈ໘ (Basalຊ‫ڀݚ‬ͷҰ෦͸ɼ૯߹Պֶٕज़ձٞʹΑΓ੍౓ઃ‫͞ܭ‬plane) ʹԊͬͯද໘·Ͱ఻೻͍ͯ͠Δ͜ͱΛࣔͯ͠Εͨ࠷ઌ୺‫ڀݚ‬։ൃࢧԉϓϩάϥϜʹΑΓɼ೔ຊֶज़

͍Δɽৼ‫ڵ‬ձΛ௨ͯ͠ॿ੒͞Εͨ΋ͷͰ͢ɽද໘෇ۙͷߴ൓ࣹ‫౓ڧ‬෦෼ʢFig. 3(b) ͷ໼ҹʣ͸ද໘࿪ΈʹΑΔফਰίϯτϥετʹ‫ى‬Ҽ͢Δͱߟ͑Βࢀߟจ‫ݙ‬

ΕΔɽ͞Βʹ Fig. 3(d), 3(e), 3(f) ͷପԁͰࣔͨ͠෦

[1] M. Skowronski and S. Ha: J. Appl. Phys. 99,
011101 (2006).
[2] H. Tsuchida, M. Ito, I. Kamata, and M. Nagano:Phys. Status Solidi B 246, 1553 (2009).
[3] R. Tanuma, T. Kubo, F. Togoh, T. Tawara, A.
Saito, K. Fukuda, K. Hayashi, and Y. Tsusaka:
Phys. Status Solidi A 204, 2706 (2007).
[4] R. Tanuma, T. Tamori, Y. Yoneawa, H.
Yamaguchi, H. Matsuhata, K. Fukuda, and K.
Arai: Material Sci. Forum 615-617, 251 (2009).
[5] R. Tanuma, D. Mori, I. Kamata, and H.
Tsuchida: Material Sci. Forum 717-720, 323(2012).
[6] S. Takeda, K. Yokoyama, Y. Tsusaka, Y.
Kagoshima, J. Matsui, and A. Ogura: J. Synchrotron Radiat. 13, 373 (2006).

෼͸ɼసҐͱଞͷܽؕɼ͋Δ͍͸సҐͱΤϐ/‫ج‬൘ք໘ͱͷ૬‫༻࡞ޓ‬ΛٙΘͤΔ΋ͷͰ͋Δɽࠓ‫ޙ‬ͷ՝୊
Ҏ্ͷ݁Ռɼ̭ઢ 3D τϙάϥϑΟʔ͕ 4H-SiC ͷ

BPD ͓Αͼ TED ͷղੳʹे෼ద༻Ͱ͖Δ͜ͱ͕Θ͔ͬͨɽࠓ‫ޙ‬͸͜ͷख๏Λ BPD-TED ม‫׵‬ͷϝΧχζϜղ໌ʹ‫͢༻׆‬Δ༧ఆͰ͋Δɽँ̭ࣙઢϚΠΫϩϏʔϜͷߴ౓ͳௐ੔Λ਱ߦͯ͠௖͍ͯ
͍Δฌ‫ཱݝݿ‬େֶͷ௡ࡔՂ޾।‫ڭ‬तʹ‫ँײ‬க͠·͢ɽ– 85 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

BL24XU

2009B3230, 2010A3230, 2010B3230‫ࢠݪ‬೩ྉඃ෴؅ࡐͷࢎԽບɾۚଐք໘෦ͷαϒϚΠΫϩϏʔϜʹΑΔඍࡉߏ଄ղੳ

Micro Structre Analysis of Oxide Films and Interface Formed on
Zirconium Alloys by X-ray Micro-Beamᖒ෦ ޹࢙, Ԃా ݈, ‫ݹ‬୩ ਖ਼༟, ๺ౡ ঙҰ
Takashi Sawabe, Takeshi Sonoda, Masahiro Furuya, Shoichi KitajimaҰൠࡒஂ๏ਓɹిྗதԝ‫ॴڀݚ‬Central Research Institute of Electric Power Industry֓ཁɿɹ೩ྉඃ෴؅ͷ଱৯ੑͱ଱ਫૉ‫ٵ‬ऩಛੑΛ޲্ͤ͞ΔͨΊɼ౰ॴͰ͸δϧίχ΢Ϝ߹ۚͷද໘ΛࢎԽͱ୸ԽΛಉ࣌ʹਐߦͤ͞୸ૉυʔϓࢎԽδϧίχ΢Ϝͱ͢Δද໘վ࣭ٕज़ϑϨογϡάϦʔϯʢFGʣΛ։ൃ͠
ͨɽFG ॲཧΛࢪͨ͠ඃ෴؅ࡐ͸ΦʔτΫϨʔϒʹΑΔ࿍֎෗৯ࢼ‫͍͓ͯʹݧ‬෗৯ྔͱਫૉ‫ٵ‬ऩྔͷ௿‫͕֬ݮ‬ೝ͞Εͨɽ͜ͷ FG ࢎԽບʢບް 1∼2 µmʣͷྑ޷ͳ଱৯ੑɾ଱ਫૉ‫ٵ‬ऩಛੑͷཁҼΛ໌Β͔ͱ͢ΔͨΊɼFGࢎԽບͱେ‫ؾ‬த͓ΑͼߴԹਫதͰ‫ܗ‬੒ͨ͠ࢎԽບͷ݁থߏ଄ΛαϒϚΠΫϩྖҬͷ‫ ॴہ‬X ઢճંଌఆʹΑΓൺ
ֱͨ͠ɽFG ॲཧʹΑΔࢎԽບͷ‫ܗ‬੒͸؇΍͔Ͱ͋ΓɼଞͷࢎԽບͱൺֱͯ͠៛ີੑ͕ߴ͍ͱਪఆ͞ΕͨɽΩʔϫʔυɿɹ೩ྉඃ෴؅ɼࢎԽບɼδϧίχ΢Ϝ߹ۚɼ์ࣹޫɼX ઢճં݅ʹͯ FG ॲཧͨ͠ࢎԽບͷஅ໘Λ݁থߏ଄ղੳɼ͓

എ‫ڀݚͱܠ‬໨త‫ࢠݪ‬೩ྉΛܰਫ࿍Ͱ௕‫ؒظ‬ར༻͢Δ͜ͱΛ໨తʹɼ଱෗৯ͱ଱ਫૉ‫ٵ‬ऩੑʹ༏Εͨඃ෴؅ࡐͷ։ൃ͕ਐΊΒΕ͍ͯΔɽ౰ॴ͸଱෗৯ɾ଱ਫૉ‫ٵ‬ऩੑͷ޲্ࡦͱͯ͠ද໘վ࣭ٕज़ΛఏҊ͓ͯ͠Γɼδϧίχ΢Ϝ߹ۚΑͼେ‫ࢎؾ‬Խບ͓ΑͼߴԹਫࢎԽບͷղੳ݁ՌͱͷൺֱΛ࣮ࢪ͖ͯͨ͠ [2, 3]ɽຊ੒ՌใࠂॻͰ͸ɼ͜Ε·Ͱʹ µ-XRD ଌఆ͔Β໌Β͔ͱͨ͠ FG ࢎԽບͷಛ௃͓Αͼࠓ‫ޙ‬ͷ‫ݕ‬౼՝୊Λ·ͱΊͨɽͷද໘ʹΧʔϘϯυʔϓࢎԽδϧίχ΢ϜൽບΛ‫ܗ‬੒ͤ͞ΔϑϨογϡάϦʔϯ (FG) ॲཧΛ։ൃͨ͠ [1]ɽ࣮‫ݧ‬͜Ε·Ͱͷ࿍֎෗৯ࢼ‫͔ݧ‬ΒɼFG ॲཧΛࢪͨ͠ඃ෴

ࢼ‫ݧ‬ยͱ͢Δδϧίχ΢Ϝ߹ۚ͸ް͞ 0.6 mm ͷδ؅ࡐͷଟ͘͸ɼະॲཧࡐ΍େ‫ࢎؾ‬Խॲཧࡐͱൺֱͯ͠ɼ

ϧΧϩΠ-2 ൘ࡐΛ༻͍ɼTable 1 ʹࣔ͢৚݅Ͱද໘Λࢎ༏Εͨ଱৯ੑͱ଱ਫૉ‫ٵ‬ऩੑΛࣔͨ͠ɽҰํͰߴԹͰ

Խॲཧͨ͠ɽࢎԽॲཧํ๏ͷ‫ه‬ड़͸ɼFG ͕ϑϨογϡ

FG ॲཧͨ͠ඃ෴؅ࡐ͸ɼ଱৯ੑɾ଱ਫૉ‫ٵ‬ऩಛੑͱάϦʔϯॲཧɼOD ͕େ‫ࢎؾ‬ԽॲཧɼAC ͕ߴԹਫࢎ

΋ʹ௿Լͨͨ͠ΊɼFG ॲཧ৚݅ʹ͸࠷ద஋͕͋ΔͱԽॲཧΛࣔ͢ɽࢎԽບͷް͞͸ɼࢼྉͷॏྔ૿Ճͱ୯

ਪଌ͞Εͨɽࠓ‫ޙ‬ɼFG ॲཧΛ࠷దԽ͢Δʹ͋ͨͬͯࣼথࢎԽδϧίχ΢Ϝ (m-ZrO2 ) ͷີ౓ (1.47 g/cm3 )͸ɼFG ࢎԽບ૊৫ͱ଱৯ੑɾ଱ਫૉ‫ٵ‬ऩಛੑͱͷ૬͔Βࢉग़ͨ͠ɽ·ͨɼް͞͸ຊଌఆ͔Β΋ ZrO2 ͷճؔΛཧղ͢Δඞཁ͕͋Δɽં͕‫ݕ‬ग़͞ΕΔൣғ͔ΒධՁͰ͖ɼଞʹಁա‫ݦࢠిܕ‬FG ࢎԽບ͸ް͞ 1∼2 µm ʹ͓͍ͯಛʹߴ͍଱৯ੑඍ‫( ڸ‬TEM) ʹΑΔஅ໘‫͔࡯؍‬Β΋ଌఆ͕ՄೳͰ͋

Λࣔ͢͜ͱ͔ΒɼࢎԽບ૊৫ͷଌఆʹ͸αϒϚΠΫϩ

ΔɽTable 1 ʹࣔ͢Α͏ʹɼ͜ΕΒͷ݁Ռ͸Α͘ҰகΦʔμʔͷߴ͍ۭؒ෼ղೳ͕‫ٻ‬ΊΒΕΔɽͦ͜Ͱຊ‫ݚ‬

͍ͯ͠ΔɽຊଌఆͰ͸ࢼྉ୆Λ্ԼʹҠಈͯ͠ް͞ํ

‫Ͱڀ‬͸ɼFG ࢎԽບͷಛ௃Λ໌Β͔ͱ͢ΔͨΊɼ์ࣹ޲Ͱͷ݁থ૬ͷมԽΛଌఆ͢Δ͕ɼTable 1 ͷ݁Ռ͔ޫʹΑΓ࣮‫͖Ͱݱ‬Δඍখ‫ ܘ‬X ઢϏʔϜΛ༻͍̭ͨઢ

ΒɼࢼྉͷҠಈ͸े෼ͳਫ਼౓Ͱ͋Δͱ൑அ͞ΕΔ [3]ɽճંଌఆʢҎԼɼµ-XRD ଌఆʣʹண໨͠ɼෳ਺ͷ৚– 86 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

Table 1. Surface treatment conditions of Zircaloy-2 and thickness of their oxide filmes
Treatment

Temperature (◦ C)

Time

FG

500

2h

0.92

0.8

FG
FG

500
630

10 h
20 min

1.89
2.05

1.7
2.8

FG

815

2h

19.27

15.3

-

OD
OD

500
630

2h
20 min

0.89
2.27

1.3
3.3

1.0 ∼ 1.2
-

AC

360

14 days-

1.9

2.2 ∼ 2.4

Thickness (µm)
weight gain µ-XRD
TEM
0.8 ∼ 1.0
1.7 ∼ 2.0-

SampleX-ray: 10 keV

Flat panel
detector

Image

Fig. 1. Layout of µ-XRD measurement and 2D image of the Debye-Scherre ring.

µ-XRD ଌఆ͸ɼฌ‫ݝݿ‬ϏʔϜϥΠϯͷ BL24XU ʹʹ͜ΕΒͷࢎԽບද໘͔Β‫Ͱ·ࡐج‬ͷ̭ઢϓϩϑΝΠ

࣮ͯࢪͨ͠ɽ̭ઢͷϏʔϜ‫ܘ‬͸ 0.3 µm Ͱ͋Γɼ̭ઢϧΛࣔ͢ɽ500◦ C, 2h Ͱ FG ॲཧͨ͠ࢎԽບ͔Β͸ɼͷΤωϧΪʔ͸ 10 keV (λ = 0.1240 nm) Ͱ͋Δɽࢼ

m-ZrO2 ͱͱ΋ʹൺֱతେ͖ͳਖ਼ํথࢎԽδϧίχ΢

‫ݧ‬ย͸थࢷʹแຒͯ͠ߴ଎ΧολʔͰ੾அ‫ޙ‬ɼஅ໘ΛϜ (t-ZrO2 ) ͷϐʔΫΛ‫ݕ‬ग़ͨ͠ɽҰํɼ815◦ C, 2h Ͱ‫ڸ‬໘‫ݚ‬ຏͯ͠ଌఆ໘ͱͨ͠ɽࢼ‫ݧ‬ย͔Βͷճં೾͸ೋ

FG ॲཧͨ͠ࢎԽບͰ͸ɼt-ZrO2 ͷճંϐʔΫ͸খ࣍͞‫ݕݩ‬ग़‫ث‬Λ༻͍ͯɼσόΠϦϯάͷҰ෦Λ‫ݕ‬ग़ͨ͠ɽ͘ຆͲ‫ݕ‬ग़͞Εͳ͔ͬͨɽt-ZrO2 ͸ѹॖԠྗԼʹ͓͍ଌఆ͸൓ࣹ๏ʹΑ࣮ͬͯࢪ͠ɼࢼ‫ݧ‬ยΛ্Լํ޲ʹҠಈͤͯ͞ࢎԽບද໘ଆ͔Β‫Ͱ·ࡐج‬Λɼ0.125 µm ·ͨ͸ 0.250 µm ͷεςοϓͰଌఆͨ͠ɽଌఆ࣌ؒʢ࿐
ޫ࣌ؒʣ͸ 1 εςοϓ͋ͨΓ 10 ඵͱͨ͠ɽFig. 1 ʹµ-XRD ଌఆ‫ܥ‬ͷϨΠΞ΢τΛࣔ͢ɽଌఆ໘͔Βೋ࣍‫ݕݩ‬ग़‫Ͱ·ث‬ͷ‫཭ڑ‬ʢΧϝϥ௕ʣ͸ 5∼6 cm Ͱ͋Γɼͯ҆ఆʹଘࡏ͠ɼ௿ԹॲཧͰ‫ܗ‬੒ͨ͠ FG ࢎԽບͷѹॖԠྗ͸ߴԹॲཧͷ৔߹ΑΓ΋େ͖͍ͱਪఆ͞ΕΔɽ
ѹॖԠྗͷେ͖͍ࢎԽບ͸៛ີͰ͋Δ͜ͱ͔Βɼࢎૉ֦ࢄΛ཈੍͢Δͱߟ͑ΒΕ͓ͯΓ [4, 5]ɼ௿Թ FG ࢎԽບͰͷ଱৯ੑΛ޲্ͤͨ͞ͱߟ͑ΒΕΔɽ
ࢎԽບͱ‫ࡐج‬ͷք໘Ͱ͸ɼδϧίχ΢ϜͷѥࢎԽ෺ճં೾͕ࢼ‫ݧ‬ยʹःΒΕͳ͍Α͏ௐ੔ͨ݁͠Ռɼೖࣹ

Ͱ͋Δ Zr3 O (PDF #22-1025) ͕֬ೝ͞ΕͨɽZr3 O

X ઢͱଌఆ໘ͷͳ֯͢͸ 11◦ ͱͨ͠ɽX ઢϏʔϜத৺͓ΑͼΧϝϥ௕͸ Zr ͷճંϦϯά͸ Zr ͷߏ଄ۭ޸ʹ O ͕ਁೖͨ͠ࢎૉ‫༹ݻ‬ମͰɼ݁থ

Λ‫ج‬४ͱܾͯ͠ఆͨ͠ɽZrO2 ͷճંϦϯά͸पํ޲֨ࢠαΠζ͸ Zr ΑΓΘ͔ͣʹେ͖͘ͳΔɽ͜ͷͨΊɼʹੵࢉͯ͠ճંϓϩϑΝΠϧΛ‫ٻ‬Ίͨɽ

Zr3 O ͷճંઢ͸ Zr ͷճંઢΑΓΘ͔ͣʹ௿֯ଆʹ‫ݱ‬ΕΔɽµ-XRD ଌఆͰ͸ɼ୯৭ʹ͍̭ۙઢΛ༻͍Δ

݁Ռ͓Αͼߟ࡯

͜ͱͰ Zr ͱ Zr3 O ͷճંઢΛ෼཭ͯ͠‫ݕ‬ग़͢Δ͜ͱFG ॲཧ৚͕݅ 500◦ C, 10h ͓Αͼ 815◦ C, 2h ͷδϧΧϩΠ-2 ࢎԽບͷஅ໘Λ µ-XRD ଌఆͨ͠ɽFig. 2͕Ͱ͖ͨɽZr3 O ͸ FG ࢎԽບɼେ‫ࢎؾ‬Խບ͓ΑͼߴԹਫࢎԽບͰ‫ݕ‬ग़͞Εͨɽ– 87 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)ͯ‫ܗ‬੒͞ΕΔͨΊɼେ‫ࢎؾ‬ԽບͰ͸ Zr3 O ૬ͷ‫ܗ‬੒͕

Zr3 O ૬ͷࢎԽΑΓ΋଎͍͜ͱΛ͍ࣔͯ͠Δɽ௿Թ FGॲཧͰ͸ࢎԽບ͕Ώͬ͘Γͱ੒௕͢ΔͨΊɼେ‫ࢎؾ‬Խॲཧͱൺ΂ͯ៛ີͳࢎԽບΛ‫ܗ‬੒͢Δͱߟ͑ΒΕΔɽ
ߴԹਫࢎԽບͷ݁থ૬ͷભҠͰ͸ɼFG ࢎԽບ΍େ‫ࢎؾ‬Խບͷ݁Ռͱൺֱͯ͠ɼt-ZrO2 ճં‫͕౓ڧ‬ද໘෇ۙͰେ͖͘௿Լͨ͠ɽࢎԽບதͷ t-ZrO2 ͷମੵׂ߹ fT ͸ɼҎԼͷ Garvie-Nicholson ͷࣜ [6] ʹΑΓද
͞ΕΔɽ

fT =

It101
Im111 + It101 + Im111

͜͜ͰɼIm111 , Im111 , It101 ͸ɼͦΕͧΕ m-ZrO2 (111)ɼ

(a) FG 500◦ C, 10h

m-ZrO2 (111)ɼt-ZrO2 (101) ͷճં‫͋Ͱ౓ڧ‬Δɽͨ
ͩ͠ɼGarvie-Nicholson ͷࣜ͸ࢎԽδϧίχ΢Ϝͷ݁থํҐ͕ϥϯμϜͳঢ়ଶͰఆྔతʹద༻͞ΕΔɽҰൠʹδϧίχ΢Ϝ߹ۚද໘ʹ‫ܗ‬੒͢ΔࢎԽບ͸഑޲ੑ͕͋Γɼࢉग़஋͸࣮ࡍΑΓ΋େ͖͍܏޲Λࣔ͢ [7]ɽFig. 4 ʹ֤ࢎԽບͷް͞ํ޲ʢք໘͔Βͷ‫ͯ͠ͱ཭ڑ‬͍ࣔͯ͠Δʣʹର͢Δ t-ZrO2 ͷମੵׂ߹ͷมԽΛࣔ
͢ɽFG ࢎԽບͱେ‫ࢎؾ‬ԽບͰ͸ɼt-ZrO2 ͸ք໘Ͱଟ͘ଘࡏ͠ɼք໘ΑΓ 0.5 µm ෇ۙ·Ͱ‫ݮ‬গͯ͠ɼҎ߱͸ද໘·ͰҰఆͰ͋ΔɽҰํɼߴԹਫதࢎԽບͰ͸ɼ◦ք໘͔Βද໘·Ͱ t-ZrO2 ͷମੵׂ߹͸୯ௐʹ‫ݮ‬গ͠(b) FG 815 C, 2hFig. 2. XRD profiles of FG samples from surface tomatrix. (a) FG 500◦ C, 10h and (b) FG 815◦ C, 2h.

ͨɽ͜ͷཧ༝͸໌Β͔Ͱ͸ͳ͍͕ɼFG ࢎԽບͱେ‫ؾ‬ࢎԽບʹ͓͍ͯͷมԽ͕ࣅͯΔ͜ͱ͔Βɼ‫ؾ‬தͱਫதͷࢎԽ‫ʹڥ؀‬ΑΔࢎԽ‫ߏػ‬ͷҧ͍͕ཁҼͱͯ͠ߟ͑Β
ΕΔ [8]ɽ

‫ݕ‬ग़ͨ͠ m-ZrO2 , t-ZrO2 , Zr3 O, Zr ʹ͍ͭͯɼࢎԽ

µ-XRD ଌఆΑΓɼ௿Թͷ FG ॲཧ͸δϧΧϩΠ-2ບް͞ํ޲΁ͷճં‫౓ڧ‬ͷมԽΛ Fig. 3 ʹࣔ͢ɽճં

ද໘ʹ t-ZrO2 ͕ଟ͍៛ີͳࢎԽບΛ‫ܗ‬੒ͤ͞Δ͜ͱϐʔΫʹ͸ɼm-ZrO2 (111), t-ZrO2 (101), Zr3 O (022͕෼͔ͬͨɽFG ॲཧΛߦΘͳ͍৔߹ʹ‫ܗ‬੒͢ΔࢎԽ10), Zr (1012) Λ༻͍ɼ֤݁থ૬͝ͱʹ૬ର‫౓ڧ‬มԽບ͸ߴԹਫதࢎԽບͰ͋Γɼͦͷද໘Ͱ͸ t-ZrO2 ͷͱ͍ͯࣔͯ͠͠ΔɽFig. 3 ΑΓɼࢎԽບද໘͔Β‫ࡐج‬‫ݮ‬গʹΑΓ៛ີੑ͕௿Լ͍ͯ͠Δͱߟ͑ΒΕΔɽFG

ʹ͔͚ͯͷ݁থߏ଄͸ɼm-ZrO2 > t-ZrO2 > Zr3 O >ॲཧ͸ද໘ͷ t-ZrO2 Λҡ࣋͠ɼ៛ີੑΛߴΊΔ͜ͱ

Zr ͷॱʹભҠ͢Δ͜ͱ͕෼͔Δɽm-ZrO2 ͱ t-ZrO2

Ͱ଱৯ੑΛ޲্͍ͤͯ͞Δͱߟ͑ΒΕΔɽͷճંϐʔΫ͕‫ݕ‬ग़͞ΕΔൣғ͕ࢎԽບް͞ʹ૬౰͠ɼಉॲཧ৚݅ʢԹ౓ɾ࣌ؒʣͷ FG ࢎԽບͱେ‫ࢎؾ‬ࠓ‫ޙ‬ͷ՝୊

ԽບͰ͸ FG ࢎԽບͷํ͕ബ͘ɼ·ͨ Zr3 O ૬΋ FGδϧίχ΢Ϝ߹ۚʹ‫ܗ‬੒ͨ͠ FG ࢎԽບͷ݁থߏࢎԽບͷํ͕ബ͍͜ͱ͕֬ೝ͞Εͨɽ௿ԹͰॲཧͨ͠

FG ࢎԽບ (500◦ C, 2h, 10h) Ͱ͸ɼZr3 O ૬͕ࢎԽບ
ͷҰ෦ͱॏͳͬͯ‫؍‬ଌ͞Εɼେ‫ࢎؾ‬ԽບͰ͸ Zr3 O ૬͕ࢎԽບͱ‫ࡐج‬ͷؒʹ‫؍‬ଌ͞Εͨɽ௿Թ FG ࢎԽບͰ
͸ Zr3 O ૬ͷ‫ܗ‬੒ʢࢎૉͷ‫΁ࡐج‬ͷਁೖʣ͕ Zr3 O ૬ͷࢎԽΑΓ΋஗͘ɼZr3 O ૬ͱࢎԽບ͕ॏͳΔΑ͏ʹ଄ͱ଱৯ੑͱͷؔ܎Λௐ΂ΔͨΊɼ์ࣹޫΛར༻ͨ͠µ-XRD ଌఆΛ࣮ࢪͨ͠ɽ଱৯ੑʹ༏ΕΔ௿Թॲཧ͠
ͨ FG ࢎԽບͰ͸ t-ZrO2 ͕ଟ͘ଘࡏ͠ɼ៛ີͳࢎԽ
ບΛ‫ܗ‬੒͢Δ͜ͱ͕෼͔ͬͨɽҰํɼ଱৯ੑͷ޲্͕‫ݟ‬ΒΕͳ͍ߴԹॲཧͨ͠ FG ࢎԽບͰ͸ t-ZrO2 ͕΄‫ݕ‬ग़͞Εͨͱߟ͑ΒΕΔɽҰํɼࢎԽບ͸ Zr3 O Λ‫ܦ‬– 88 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

(a) FG-500◦ C-2h(b) OD-500◦ C-2h(c) FG-630◦ C-20min(d) OD-630◦ C-20min(e) FG-500◦ C-10h(f) AC-360◦ C-14days

Fig. 3. Changes in nomalized intensities of (111)m, (101)t, (022 10) Zr3 O and (1012) Zr peak from the surface
to the matrix [3].

– 89 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)ີͳࢎԽບΛ‫ܗ‬੒ͯ͠଱৯ੑΛ޲্ͤ͞Δͱߟ͑ΒΕΔɽࠓճͷ࣮‫ݧ‬ΑΓɼFG ॲཧ͸δϧίχ΢Ϝ߹ۚͷද໘ʹ៛ີͳࢎԽບΛ‫ܗ‬੒͠ɼࢎૉͷ֦ࢄΛ཈੍͢Δͱߟ͑ΒΕͨɽ͜ͷ៛ີ͞ͷධՁํ๏ͱͯ͠ɼບԠྗͷଌఆ͕‫͛ڍ‬ΒΕΔɽࠓ‫ޙ‬͸ FG ࢎԽບͷԠྗঢ়ଶʢಛ
ʹද໘΍ք໘ʣΛ೺Ѳ͠ɼࢎૉ֦ࢄΛ཈੍͢ΔϝΧχζϜΛղ໌͍ͯ͘͠ɽ
ࢀߟจ‫ݙ‬

Fig. 4. Tetragonal fraction of the oxide layers, as afunction of distance from interface [3].

ͱΜͲ‫ݕ‬ग़͞Εͳ͔ͬͨ͜ͱΑΓɼࢎԽບ͸៛ີͰͳ͘଱৯ੑͷ޲্ΛಘΒΕͳ͔ͬͨͱ݁࿦͚ͮͨɽ

µ-XRD ଌఆ͔Β͸ࢎԽບͷ݁থߏ଄ͷભҠ͕໌֬ʹ‫؍‬ଌ͞Εɼද໘͔Β‫ Ͱ·ࡐج‬m-ZrO2 > t-ZrO2 >Zr3 O > Zr ͷॱʹมԽͨ͠ɽFG ࢎԽບͷք໘Ͱ͸
Zr3 O ૬͕ࢎԽບͱॏͳΔΑ͏ʹ‫ݕ‬ग़͞Εͨ͜ͱ͔Βɼ
FG ࢎԽບͰ͸ࢎԽບ͔Β‫΁ࡐج‬ͷࢎૉ֦ࢄ͕େ‫ࢎؾ‬Խບͱൺֱͯ͠஗͍ͱਪఆ͞Εͨɽ·ͨɼFG ࢎԽບද໘Ͱͷ t-ZrO2 ͷମੵׂ߹͸ɼߴԹਫࢎԽບͱൺֱ
ͯ͠େ͖͘ɼ FG ॲཧ͕δϧίχ΢Ϝ߹ۚͷද໘ʹ៛

[1] ‫ݹ‬୩ਖ਼༟ɼৗ൬Ҫकହଞ: ೔ຊ‫ֶྗࢠݪ‬ձ 2009 ळͷେձ ༧ߘू N19 (2009).
[2] ᖒ෦޹࢙ɼԂా݈ଞɼ೔ຊ‫ֶྗࢠݪ‬ձ 2010 ळͷେձ ༧ߘू G14 (2009).
[3] T. Sawabe, T. Sonoda, M. Furuya, S. Kitajima,
M. Kinoshita, and M. Tokiwai: J. Nucl. Mater.
419, 310-319 (2011).
[4] W. Qin, C. Nam, H.L. Li, and J.A. Szpunar:
Acta Mater. 55 1695-1701 (2007).
[5] B. Wadman94, Z. Lai, H.-O. Andren, A.-L.
Nysrom, P. Pudling, and H. Pettersson: ASTM
STP 1245 579-598 (1994).
[6] R.C. Garvie and P.S. Nicholson: J. Am. Ceram.
Soc. 55 303-305 (1972).
[7] A. Yilmazbayhan, A.T. Motta, R.J. Comstock,
G.P. Sabol, B. Lai, and Z. Cai: J. Nucl. Mater.
324 6-22 (2004).
[8] D.G. Franklin and P.M. Lang: ASTM STP 1132
3-32 (1991).

– 90 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

2009B3102, 2010B3102, 2011A3102, 2011B3102

BL24XU

Real-time Synchrotoron Radiation X-Ray Diffraction from
Erbium Silicate Formations on SiO2 /Si Substrates
Hiroo Omi1,2
1

NTT Basic Research Laboratories, NTT Corporation,
2
NTT Nanophotonics Center, NTT Corporation

Abstractɿ The erbium silicate formation processes during annealing in Ar gas were monitored bysynchrotron radiation grazing incidence X-ray diffraction (GIXD) in real time. The GIXD measurements
show that erbium silicates and erbium oxide are formed by interface reactions between silicon oxideand erbium oxides deposited on silicon oxide by reactive sputtering in Ar gas and O2 /Ar mixture gas
ambiences. The erbium silicates are formed above 1060 ◦ C in Ar gas ambience and above 1010 ◦ C in
O2 /Ar gas ambience, and erbium silicides are dominantly formed above 1250 ◦ C.
Keywordsɿ Real-time grazing incidence X-ray diffraction, Erbium silicate, thin film, silicon

Introduction

the duration of the thermal annealing. The rela-Erbium silicates and erbium oxide, such as Er2 SiO5
and Er2 Si2 O7 , are promising materials as light emitters at the telecommunications wavelength and as
optical amplifiers in the field of silicon photonics[1–8]. In the erbium compounds, the density of erbium ions is 1022 atoms/cm3 , which is orders of magnitude greater than that typically obtained by Er ion
implantation in silicon substrate, allowing access toa huge number of emitting centers.
A variety of growth methods are used to fabricate
erbium silicates and erbium oxides on the surfacesof SiO2 and Si substrate, including sole gel methods, reactive sputtering, pulse laser deposition, andthermal annealing in Ar, N2 , and oxygen gas ambiences. Previous work revealed that the processes in
the growth methods significantly affect the photoluminescence (PL) intensities of Er+3 ions in the materials [1–8]. According to Ref. 7, for example, thePL intensity of Er2 O3 grown on Si and SiO2 by magnetron sputtering becomes large with an increase ofannealing temperature up to 1200 ◦ C, depending on

tionship between the structural features and the increase of PL intensity is, however, not clear. Furthermore, it has been reported that the crystal structureof erbium silicates strongly depends on the growthmethod and thermal annealing procedures, but it
has been reported that there exist several phases ofmono-silicates and di-silicates [5].
For more precise control of the silicate formation
and a better understanding of the behavior of the PL
intensities, it is therefore necessary to investigate theformation processes in order to tune the growth conditions appropriately and obtain intense Er3+ photoluminescence from the resultant crystal of erbium
silicates. We have previously developed a grazing
incidence synchrotron X-ray diffraction (GIXD) apparatus that can monitor the annealing behavior inreal time in O2 /Ar mixture gases [9]. The real-time
GIXD is promising for characterizing the structuresand silicate formation processes.
In this work [10], we performed real-time GIXD
experiments to reveal formation processes of erbium
silicates on silicon substrate. We determined the
crystallographic structures and the temperature of– 91 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)
crystallization, and assessed the possible reactions

system (SPring-8). Anneal temperatures were cal-for the silicate formation on silicon.

ibrated by measuring the thermal expansion coefficient of Er2 O3 in the real-time GIXD measurements.

Experimental
The 100-nm-thick erbium oxides were deposited

Results and Discussion

on 100-nm-thick silicon oxide film grown on Si(001)Fig. 1 shows the powder diffraction pattern ob-

substrates by reactive sputtering at room tempera-

tained by the synchrotron radiation GIXD at room

ture. The samples are then annealed at up to 1300

temperature from a sample annealed at 1060 ◦ C in◦

C in Ar and O2 /Ar mixture gases. The deposition

Ar gas ambience. The peaks can be assigned torate of erbium oxide was ∼ 0.1 nm/s.

Er2 O3 , Er2 SiO5 , and Er2 Si2 O7 phases, indicating

Grazing incidence X-ray diffraction experiments

the formation of mixtures of these phases as a re-were performed during the annealing in real timesult of the annealing. The peaks at 26.78◦ , 33.1◦ ,at beam line BL24XU in SPring-8 using the X-ray

34.73◦ , 38.65◦ , 42.84◦ , 43.83◦ , and 45.65◦ are fromwavelength of 1.24 Å [9]. The incidence angle of the(400), (422), (431)/(134), (440), (611), (026), and◦

X-ray was 0.2∼1.0 . The gas flow rates of Ar and(622) planes of cubic Er2O3 (JCPDS card no. 40-

oxygen gases were 2 L/min and 50 – 500 cc/min,384), space group Ia3 . The peaks at 11.82◦ , 16.12◦ ,respectively. The duration of the X-ray diffraction

17.31◦ , 18.21◦ , 19.3◦ , 20.13◦ , 21.39◦ , 22.61◦ , 24.44◦ ,was about 30 minutes. The temperature rise time

25.82◦ , and 28.06◦ are from (200), (202)/(211), (112)

was about 10 ◦ C/min. The annealing experiments, (211), (112), (202), (020), (121), (402), (622), andabove 1200 ◦ C were done in a high-temperature SiC(411) planes of monoclinic Er2 SiO5 (JCPDS card

furnace like the one in the synchrotron radiation

no. 43-1007), space group I2/a , and the peaks at

Fig. 1. X-ray powder pattern obtained from samples annealed at 1060 ◦ C in Ar gas ambience.

– 92 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू
◦

◦

◦

◦

12.94 , 15.02 , and 29.16 are from (002), (100), andpeaks at 12.84 and 14.84◦ , which can be signed not(113)/(112) planes of Er2 Si2 O7 (JCPDS card no. 24-

to mono-silicate but to di-silicate E2 Si2 O7 (See Fig.

62), space group P21/b , respectively. The main peak1).

◦

A comparison between Fig. 1 and 2(a) shows thatplane of Er2 SiO5 .

the peaks at 18.56◦ from the (012) planes of theat 23.64 is from (222) plane of Er2 O3 and (013)
Fig. 2(a) and (b) show real-time diffraction pat-di-silicate appear after the thermal annealing. Pos-

terns obtained during thermal annealing in Ar gas

sible reactions at this temperature are as follows:

and O2 /Ar gas ambiences.

Er2 O3 + 2SiO2 → Er2 Si2 O7 or Er2 SiO5 + SiO2

In the Ar gas ambi◦

ence (Fig. 2(a)), the broad peaks at 23.45 obtainedat room temperature are from the as-grown amor-→ Er2 Si2 O7 . Noted that the mono- and di-silicate

structures are not stable during thermal annealing

phous erbium oxide. The thermal annealing at 415

above 1250 ◦ C in the Ar gas ambience, because we◦

C sharpened the broad peak, indicating the crystal-observed ErSi2 at the 1250 ◦ C as a dominant phase.

lization of erbium oxide on the 100-nm-thick silicon

In the 2.4 % O2 /Ar ambience, on the other hand,oxide layers. The feature of the diffraction patternpattern evolution is similar to that in the Ar ambi-

remains up to 815 ◦ C. The thermal annealing at 1011

ence. It should be noted, however, that the onset◦

C suddenly produces new small peaks at 21.26◦ andtemperature of the formation of mono-silicate and25.74◦ , which can be assigned to (020) and (022) re-di-silicate becomes lower than that in the Ar am-

flections of the mono-silicate phase of Er2 SiO5 (Fig.

bience. The erbium silicate formation temperatures1). This clearly shows that the interface reaction

are compared in Table 1.

occurs between crystal Er2 O3 and amorphous SiO2

The results support desorption of Si from the sur-as Er2 O3 (s) + SiO2 (a) → Er2 SiO5 . Further ther-face via SiO gas during the thermal annealing. The

mal annealing up to 1060 ◦ C produces additional

additional oxygen insertion prevents desorption ofFig. 2. X-ray powder patterns obtained during thermal annealing (a) in pure Ar gas ambience and (b) 2.4% O2 /Ar mixture gas ambience. White and black stars represent the reflection from mono- and di-silicate,respectively.

– 93 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)
Table 1. Nucleation temperatures of crystalline Er2 O3 , Er2 SiO5 , and Er2 Si2 O7
in pure Ar and Ar/O2 mixture gas ambiences.
Crystalization in Ar ambience

Temperature in O2 /Ar ambience

225 ∼ 620 ◦ C
1010 ∼ 1060 ◦ C
1060 ◦ C∼ 620 ◦ C
∼ 1010 ◦ C∼ 1010 ◦ C

Er2 O3 :Er2 SiO5 :Er2 Si2 O7 :SiO, meaning oxygen plays an important role in the
mono- and di-silicate formation.

The distances between Er ions in the silicates are
one of significant parameters which govern efficiency

To see the effect of annealing at higher tempera-of light emission from Er ions through energy mi-ture on the silicate formation, we obtained the pow-

grations between Er ions. We are estimating the

der diffraction pattern from the sample annealed at

distance using extended X-ray absorption measure-1250 ◦ C in the Ar gas ambience for 1 h. The peaks

ments at present. We hope that the precise determi-

at 17.23◦ , 21.63◦ , 27.93◦ , and 35.17◦ are assigned tonation of the Er ions will help us to improve quantum(001), (100), (101), and (002) planes of hexagonal

efficiency of Er emissions from the Er silicates.

ErSi2 phase (JCPDS card no. 12-37), space group
P6/mmm . This indicates that erbium oxides and sil◦

icates at 1060 C (Fig. 1) disappear but ErSi2 appears on the film, which means that oxygen atoms
are preferentially desolated from the erbium oxideand silicates.
The X-ray diffraction results indicate that the thermal stability of erbium oxide and silicates on silicon
depends on the annealing temperature, which supports the finding that the oxygen desorption is critical during thermal annealing as seen in Fig. 2(a)and (b).
Conclusion
We grew Er2 SiO5 , Er2 Si2 O7 , and Er2 O3 on silicon substrates using the interface reaction between
Er2 O3 and SiO2 film grown on Si(001) substrates in
Ar and 2.4 % O2 /Ar gas ambiences. The Er2 SiO5
and Er2 Si2 O7 phases are assigned to JCPDS card
no. 43-1007 and no. 24-62, respectively. The formation of erbium mono- and di-silicate prefers theO2 /Ar mixture gas ambience. Annealing above 1250◦

C produces erbium silicides, which are optically in-

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E. F. Pecora, A. Irrera, and F. Priolo: Optical
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active.

– 94 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

BL24XU

2010B3241

์ࣹޫ̭ઢࢄཚ๏Λ༻͍ͨໟ൅ͷઢҡ഑޲ղੳ

Synchrotron Radiation X-Ray Scattering Analysis ofFilament Orientation in Hair‫ٱ‬ถ ୎ࢤɼಙ‫ึࢤ ݪ‬ඒ ∗ ɼ୮࣏ ൣจ
Takuji Kume, Shihomi Takuhara∗ , Noriyuki TanjiՖԦ‫ࣜג‬ձࣾղੳՊֶ‫ॴڀݚ‬R&D - Analytical Science Research, Kao Corporation֓ཁɿɹໟ൅ߏ଄͸ໟ൅ͷ‫౓ڧ‬΍‫ܗ‬ঢ়ʹ‫د‬༩͢Δͱߟ͑ΒΕɼͦͷղੳ͸ໟ൅μϝʔδ౳ͷໟ൅ʹؔΘΔ͞·
͟·ͳ‫ݱ‬৅ͷ೺ѲͷͨΊʹॏཁͰ͋Δɽຊ՝୊Ͱ͸ɼϛΫϩϑΟϒϦϧதͷέϥνϯઢҡʹண໨͠ɺϚΠΫϩϏʔϜ̭ઢ޿֯ࢄཚ๏Λ༻͍ͯԽֶॲཧ΍෺ཧॲཧʹ൐͏έϥνϯઢҡͷߏ଄มԽΛղੳͨ͠ɽͦͷ݁Ռɼະॲཧໟ൅ͱൺֱͯ͠ɼύʔϚॲཧΛߦͬͨໟ൅Ͱ͸ α-ϔϦοΫεߏ଄ʹಛҟͳߏ଄มԽ͸‫͕͍ͳ͍͖ͯى‬ɼԆ৳ॲཧΛߦͬͨໟ൅Ͱ͸ɼα-ϔϦοΫεߏ଄͔Β β-γʔτߏ଄΁ͷมԽ͕ੜ͍ͯ͡Δ͜ͱ͕൑໌ͨ͠ɽ
Ωʔϫʔυɿɹໟ൅ɼέϥνϯઢҡɼϚΠΫϩϏʔϜ̭ઢɼ޿֯ࢄཚ

എ‫ڀݚͱܠ‬໨త͜ͷΑ͏ͳໟ൅ߏ଄͸ໟ൅ͷ‫౓ڧ‬΍‫ܗ‬ঢ়ʹ‫د‬༩͢Δ

ໟ൅͸ɼ಄෦Λ֎తܹࢗ΍ຎࡲ͔Βͷอ‫͢ޢ‬ΔͨΊͷ‫͋Ͱ׭ث‬Δͱಉ࣌ʹɼਓͷ֓‫؍‬Λࠨӈ͢Δॏཁͳ໾ׂ΋୲͍ͬͯΔɽ·ͨɼγϟϯϓʔɾϦϯε౳ͷϔΞέΞ੡඼͸ɼࠃ಺Ͱͷച্͕೥ؒ໿ 2,000 ԯԁ‫ن‬໛ͱ͍͏େ͖ͳࢢ৔Ͱ͋Γɼໟ൅ͷ‫ૅج‬త‫ڀݚ‬Λ঎඼։ൃ΁ͷԠ༻ʹ‫͛ܨ‬Δ͜ͱ͸‫ࡁܦ‬తͳଆ໘͔Β΋ඇৗʹॏཁͰ͋Δɽͱߟ͑ΒΕΔɽͦͷͨΊɼໟ൅಺෦ͷߏ଄ղੳ͸ໟ൅μϝʔδ౳ͷໟ൅ʹؔΘΔ͞·͟·ͳ‫ݱ‬৅ͷ೺ѲͷͨΊʹॏཁͰ͋Δɽຊ՝୊Ͱ͸ɼϚΫϩϑΟϒϦϧதͷέϥνϯઢҡʹண໨͠ɼϚΠΫϩϏʔϜ̭ઢ޿֯ࢄཚ
๏Λ༻͍ͯɼԽֶॲཧ΍෺ཧॲཧʹ൐͏έϥνϯઢҡͷߏ଄มԽɼͱ͘ʹɼέϥνϯઢҡͷ α-ϔϦοΫε
ߏ଄͔Β β-γʔτߏ଄΁ͷมԽͷ೺ѲΛ໨తͱͨ͠ɽ

ໟ൅ͷߏ଄ղੳ͸ɼ͜Ε·Ͱʹ΋ओʹిࢠ‫ݦ‬ඍ‫ڸ‬΍

AFMɼ̭ઢࢄཚ౳ͷख๏Λ༻͍ͯߦΘΕɼଟ͘ͷ੒Ռ͕ಘΒΕ͍ͯΔɽͦΕΒͷ֤छ‫ܗ‬ଶ‫ʹ࡯؍‬ΑΓಘΒΕͨ৘ใ͔Βɼໟ൅͸ Fig. 1(a) ʹࣔͨ͠Α͏ʹɼੜମ಺ͷଞͷ૊৫ͱಉ༷ɼඇৗʹෳࡶͳ֊૚ߏ଄Λऔͬ
͍ͯΔ͜ͱ͕൑໌͍ͯ͠Δɽ͢ͳΘͪɼΩϡʔςΟΫϧʹ෴ΘΕͨໟ൅಺෦͸ਊ෦Ͱ͋ΔϝσϡϥͷपΓΛίϧςοΫεࡉ๔͕઎Ί͓ͯΓɼ֤ʑͷίϧςοΫε
ࡉ๔͸ϚΫϩϑΟϒϦϧͱϚτϦοΫεʢඇথ࣭‫ٿ‬ঢ়λϯύΫʣ͔Β‫ܗ‬੒͞ΕΔɽ͞ΒʹɼϚΫϩϑΟϒϦ
ϧ͸έϥνϯઢҡʢதؒ‫ܘ‬ϑΟϥϝϯτ = IFʣ͔Βߏ੒͞ΕΔɽ

Fig. 1. (a) Structure of hair, (b) TEM section
image of hair.

∗ ‫ࡏݱ‬ͷॴଐ: ՖԦ‫ࣜג‬ձࣾεΩϯϏϡʔςΟ‫ॴڀݚ‬

Present Address: R&D - Skin Beauty Research, Kao Corporation– 95 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)࣮‫ݧ‬จ‫ʹݙ‬ΑΔͱɼ໼ҹ 1 ͷεϙοτ͸έϥνϯઢҡͷຊ՝୊ͷ࣮‫Ͱݧ‬͸ɼ
1 Խֶॲཧྺͷແ͍ໟ൅ʢະॲཧໟʣɼ
2 ύʔϚॲཧΛࢪͨ͠ໟ൅ʢύʔϚॲཧໟʣɼ
3 Ԇ৳ॲཧΛߦͬͨໟ൅ʢԆ৳ໟʣΛࢼྉͱͯ͠༻
͍ͨɽύʔϚॲཧໟ͸ɼԽֶॲཧྺͷແ͍ໟ൅ΛνΦάϦ
ίʔϧࢎਫ༹ӷதʹҰఆ࣌ؒਁ௮‫ޙ‬ɼաࢎԽਫૉਫ༹
ӷʹҰఆ࣌ؒਁ௮͠ɼΠΦϯަ‫׵‬ਫͰ୕͙͜ͱʹΑΓ࡞੡ͨ͠ɽԆ৳ໟ͸ɼԽֶॲཧྺͷແ͍ໟ൅ΛνΦάϦίʔϧࢎਫ༹ӷʹҰఆ࣌ؒਁ௮‫ޙ‬ɼ໿ 1.4 ഒͷԆ৳ॲཧΛߦ͍ɼΠΦϯަ‫׵‬ਫͰ୕͙͜ͱʹΑΓ࡞੡ͨ͠ɽ

α-ϔϦοΫεؒͷ‫཭ڑ‬ʢ0.96 nmʣɼ໼ҹ 2 ͷεϙοτ
͸έϥνϯઢҡͷ β-γʔτؒͷ‫཭ڑ‬ʢ0.47 nmʣʹ૬౰͢Δ [1]ɽ্‫ه‬ͷ݁ՌΑΓɼະॲཧໟͱύʔϚॲཧໟ͸ α-ϔϦοΫεߏ଄͕ओͰ͋ΓɼԆ৳ໟͰ͸ α-ϔϦοΫεߏ଄ʹՃ͑ͯ β-γʔτߏ଄͕ଘࡏ͢Δͱߟ͑ΒΕͨɽҎ্ͷ͜ͱΑΓɼԽֶॲཧྺͷແ͍ໟ൅ͱ
ൺֱͯ͠ύʔϚॲཧΛߦͬͨໟ൅Ͱ͸ α-ϔϦοΫε
ͷಛҟͳߏ଄มԽ͸‫͕͍ͳ͍͖ͯى‬ɼԆ৳ॲཧΛߦͬͨໟ൅Ͱ͸ɼα-ϔϦοΫε͔Β β-γʔτߏ଄΁ͷมԽ͕ੜ͍ͯ͡Δ͜ͱ͕໌Β͔ͱͳͬͨɽ

͜ΕΒͷໟ൅ʹର͠ɼໟ൅ଠ͞ͷ 1/3 ͱͳΔ෦Ґ΁ɼໟ൅࣠ʹਨ௚ͳํ޲͔ΒϚΠΫϩϏʔϜ̭ઢʢϏʔϜαΠζ 1.4 µm × 8 µmʣΛೖࣹ͠ɼ2 ࣍‫ࢄ֯޿ݩ‬ཚ૾Λଌఆͨ͠ɽϚΠΫϩϏʔϜ̭ઢΛໟ൅ଠ͞ͷ 1/3
ͱͳΔ෦Ґ΁রࣹͨ͠ҙਤ͸ҎԼͷͱ͓ΓͰ͋Δɽ

Fig. 1(a) ʹࣔͨ͠ͱ͓Γɼໟ൅಺෦͸ਊ෦ͷϝσϡϥͱͦͷपΓͷίϧςοΫεࡉ๔ͱͰ‫ܗ‬੒͞Ε͍ͯΔɽ
ͦͷ͏ͪɼຊ՝୊Ͱߏ଄มԽΛଌఆɾղੳ͍ͨ͠ϚΫϩϑΟϒϦϧதͷέϥνϯઢҡ͸ɼίϧςοΫεࡉ๔ͷதʹଘࡏ͢Δɽͦ͜ͰɼFig. 1(b) ͷໟ൅அ໘ͷిࢠ‫ݦ‬ඍ‫ͨࣔ͠ʹ্૾ڸ‬Α͏ʹɼଌఆͷࡍʹத৺෦ͷϝσϡϥΛ֎ͯ͠ϚΠΫϩϏʔϜ̭ઢΛໟ൅ʹরࣹ͢Ε͹ɼϝσϡϥͷӨ‫ڹ‬Λഉ͠ɼ΄΅ίϧςοΫε͢ͳΘͪϚΫϩϑΟϒϦϧதͷέϥνϯઢҡ͕ओମͷ৘ใΛಘΔ͜ͱ͕Ͱ͖Δͱߟ͑ͨɽ
ͳ͓ɼϚΠΫϩϏʔϜ̭ઢ޿֯ࢄཚଌఆʹ͸ɼSPring-

8 ͷϏʔϜϥΠϯ BL24XU Λ༻͍ͨɽ̭ઢͷ೾௕͸
0.124 nm (10 keV)ɼ‫ݕ‬ग़‫ʹث‬͸ϑϥοτύωϧσΟ
ςΫλʔʢ1032 × 1032 pixelsɼ1 pixel = 50 µmʣΛFig. 2. 2D-images of microbeam wide angle Xray scattering. (a) untreated hair, (b) hair withpermanent wave treatment, (c) elongated hair.

࢖༻ɼϚΠΫϩϏʔϜ̭ઢͷूޫʹ͸ϑϨωϧκʔϯϓϨʔτ (FZP) ํࣜΛ࢖༻ͨ͠ɽࢼྉ-‫ݕ‬ग़‫཭ڑؒث‬·ͱΊͱࠓ‫ޙ‬ͷ՝୊

͸ 58.1 mmɼ1 ఺ͷরࣹ࣌ؒ͸Ͱ 2 ඵͰɼଌఆԹ౓͸ຊ՝୊ͷ‫ݕ‬౼ͰɼύʔϚॲཧΛߦͬͨໟ൅Ͱ͸ α-ࣨԹͱͨ͠ɽ

ϔϦοΫεߏ଄ʹಛҟͳߏ଄มԽ͸‫͕͍ͳ͍͖ͯى‬ɼԆ৳ॲཧΛߦͬͨໟ൅Ͱ͸ α-ϔϦοΫεߏ଄͔Β β-݁Ռ͓Αͼߟ࡯

γʔτߏ଄΁ͷมԽ͕ੜ͍ͯ͡Δ͜ͱ͕൑໌ͨ͠ɽ
ϚΠΫϩϏʔϜ̭ઢ޿֯ࢄཚଌఆʹΑΓಘΒΕͨ 2ࠓ‫ޙ‬ͷ՝୊ͱͯ͠͸ɼύʔϚॲཧ΍Ԇ৳ॲཧͱ͍ͬ

࣍‫ࢄ֯޿ݩ‬ཚ૾Λ Fig. 2 ʹࣔ͢ɽFig. 2(a) ͕ະॲཧͨμϝʔδͷఔ౓ʹΑΔϔϦοΫεߏ଄ͷมԽͷ೺Ѳ

ໟɼ(b) ͕ύʔϚॲཧໟɼ(c) ͕Ԇ৳ໟͷ݁ՌͰ͋Δɽ

΍ɼ෼ޫֶతଌఆ๏ʢϥϚϯଌఆ౳ʣͳͲଞͷख๏Ͱະॲཧໟ͓ΑͼύʔϚॲཧໟ͸ɼ੺ಓํ޲ͷ໼ҹ 1ͷέϥνϯઢҡߏ଄ͷมԽͷղੳͱͷൺֱͱ͍ͬͨ͜

ͷҐஔʹεϙοτ͕‫؍‬ଌ͞Εͨͷʹର͠ɼԆ৳ໟ͸໼ͱ͕‫͛ڍ‬ΒΕΔɽ

ҹ 1 ʹՃ͑໼ҹ 2 ͷҐஔʹεϙοτ͕‫؍‬ଌ͞Εͨɽ– 96 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू
͜ͷΑ͏ͳ‫ݕ‬౼͔Βɼໟ൅‫Ͱॴہ‬ͷߏ଄ͷมԽΛଊ͑Δ͜ͱͰɼໟ൅ͷμϝʔδͷ࣮ଶ͕೺ѲͰ͖ɼμϝʔδ͕ਐߦ͍ͯ͘͠աఔΛΑΓৄࡉʹཧղͰ͖Δ΋ͷͱ‫ظ‬଴͞ΕΔɽ

ࢀߟจ‫ݙ‬[1] L. Kreplak, J. Doucet, P. Dumas, and F. Briki:“New aspects of the α-helix to β-sheet transitionin stretched hard α-keratin fibers.” BiophysicalJournal 87, 640 (2004).

– 97 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

BL24XU

2011B3204, 2012A3204

Ϧν΢ϜΠΦϯೋ࣍ి஑ͷෛ‫͚͓ʹۃ‬Δ

Mn ෼෍ͷϚΠΫϩϏʔϜ XRF ๏ʹΑΔධՁ
Distribution of Mn Ions in the Anodes of Lithium-Ion
Rechargeable Batteries by Micro-Beam X-ray Fluorescent
Spectroscopy‫ ాށ‬ত෉
Akio Toda
NEC εϚʔτΤωϧΪʔ‫ॴڀݚ‬
Smart-Energy Research Laboratories, NEC Corporation֓ཁɿɹϚΠΫϩ XRF Λ༻͍ͯϦν΢ϜΠΦϯೋ࣍ి஑ͷෛ‫ۃ‬ද໘ͱஅ໘ͷ Mn ෼෍ΛධՁͨ͠ɽฏ໘ଌఆ
͔Β͸ Mn ͕‫׆‬෺࣭ͷද໘ʹ෇ண͍ͯ͠Δ͜ͱ΍ɼ෇ணྔͱి஑ͷྼԽ౓ʹରԠ͕͋Δ͜ͱ͕Θ͔ͬͨɽ·ͨɼࢼߦతʹߦͬͨஅ໘ଌఆ͔ΒɼMn ෼෍͸ి‫ۃ‬ද໘͔Βूిମʹ޲͔ͬͯ‫ݮ‬ਰ͢Δ෼෍Ͱ͋Δ͜ͱ͕ࣔ͞ΕͨɽΩʔϫʔυɿɹϦν΢ϜΠΦϯೋ࣍ి஑, ϚΠΫϩ XRF, Mn ༹ग़എ‫ڀݚͱܠ‬໨తԠ༗ແΛ‫ݕ‬౼ͨ͠ɽՃ͑ͯɼஅ໘ࢼྉΛ࡞੡ͯ͠ Mn

Ϧν΢ϜΠΦϯೋ࣍ి஑ (Lithium-ion rechargeable

Batteries: LiB) ͸ΤωϧΪʔີ౓ɼग़ྗີ౓΍ಈ࡞ిѹ͕ߴ͍͜ͱͳͲ༏ΕͨಛੑΛ࣋ͭɽ͜ͷͨΊɼ‫ܞ‬ͷஅ໘෼෍ͷධՁՄೳੑ΋‫ݕ‬౼ͨ͠ɽ࣮‫ݧ‬ଳి࿩΍ϊʔτ‫ܕ‬ύιίϯΛ͸͡Ίͱ͢Δ‫ܞ‬ଳ‫ܕ‬৘ใ

LiB ͷෛ‫෇ʹۃ‬ணͨ͠ Mn ͷ෼෍ΛධՁ͢ΔͨΊɼ୺຤΍࢈‫͍༻͘޿ʹثػ༻ۀ‬ΒΕ͍ͯΔɽۙ೥ɼి‫ؾ‬య‫ܕ‬తͳϚϯΨϯ/ΧʔϘϯ‫ ܥ‬LiB Λ࡞੡͠ɼॆ์ి

ࣗಈं΍ిྗஷଂͳͲ΁ͷԠ༻ʹ޲͚ͯେ‫ܕ‬Խ͕‫ظ‬଴ࢼ‫ݧ‬Λߦͬͨɽͦͷ‫ޙ‬ɼి஑ੑೳͷྼԽ౓͕ҟͳΔ 2

͞Ε͓ͯΓɼ‫ڀݚ‬։ൃ͕ਐΊΒΕ͍ͯΔɽ্‫ه‬ͷԠ༻ͭͷి஑͔Βෛ‫ۃ‬ΛऔΓग़͠ଌఆʹ࢖༻ͨ͠ (ྼԽ౓ʹ͓͍ͯ͸ɼߴ༰ྔԽɼ҆શੑͷ֬อ΍௕ण໋Խ͕՝

খɿ sample BɼྼԽ౓େɿ sample C)ɽ·ͨࢀরࢼ୊Ͱ͋Δɽ͜ΕΒͷ՝୊ͷղܾʹ͸ి஑ྼԽ‫ߏػ‬Λ໌ྉͱͯ͠ࢼ‫ి͍ͳ͍ͯ͠ݧ‬஑͔ΒऔΓग़ͨ͠ෛ‫ۃ‬΋४Β͔ʹ͢Δ͜ͱ͕͔ܽͤͳ͍ɽ

උͨ͠ (sample A)ɽஅ໘ࢼྉ࡞੡ʹ͸ɼΫϩηΫγϣ

ϚϯΨϯࢎϦν΢ϜΛਖ਼‫ ͍ͨ༻ʹۃ‬LiB Ͱ͸ɼॆφϧϙϦογϟΛ༻͍ͨඪ४తͳํ๏Λ༻͍ͨɽ์ిಈ࡞த΍อଘ࣌ʹɼҰ෦ͷ Mn ΠΦϯ͕ిղӷ΁ϚΠΫϩ XRF ଌఆ͸ SPring-8 ฌ‫ݝݿ‬ϏʔϜϥΠ

༹ग़͢Δͱ͍͏‫ݱ‬৅͕஌ΒΕ͓ͯΓɼ༹ग़ Mn ྔͱ༰ϯ BL24XU ʹͯߦͬͨɽκʔϯϓϨʔτͱεϦοτྔ௿Լʹ૬͕ؔ͋Δͱ͞Ε͍ͯΔ [1]ɽ͔͠͠ɼ༹ग़

ʹΑΓ‫ܗ‬੒ͨ͠ϚΠΫϩϏʔϜͷϏʔϜαΠζ͸ɼԣͨ͠ Mn ΠΦϯ͕ؔ༩͢Δి஑༰ྔͷ௿ԼϝΧχζϜ

ํ޲໿ 0.4 µmɼॎํ޲ ໿ 0.1 µm Ͱ͋ͬͨɽࢼྉε͸ඞͣ͠΋໌Β͔Ͱ͸ͳ͍ɽςʔδΛॎԣํ޲ʹ 0.5 µm ͳ͍͠ 1.0 µm εςοϓຊ‫Ͱڀݚ‬͸͜ͷΑ͏ͳి஑ྼԽ‫ߏػ‬Λ໌Β͔ʹ͢ΔͰεΩϟϯ͠ͳ͕Β֤఺Ͱ‫̭ޫܬ‬ઢεϖΫτϧΛଌఆखஈͱͯ͠ɼϚΠΫϩ XRF Λ༻͍ͯి‫಺ۃ‬ͷભҠۚͨ͠ɽଌఆͷ‫ ޙ‬Mn-K ಛੑ̭ઢ‫౓ڧ‬Λϓϩοτ͠ Mn

ଐ‫ࢠݪ‬෼෍ΛධՁ͢Δ͜ͱΛ‫ݕ‬౼͍ͯ͠ΔɽຊใࠂͰ

෼෍Λಘͨɽ

͸ɼਖ਼‫͔ۃ‬Β༹ग़͠ෛ‫΁ۃ‬౸ୡͨ͠ Mn ΠΦϯʹ͍ͭͯɼෛ‫ۃ‬ද໘্Ͱͷ෼෍ΛධՁͯ͠ి஑ྼԽ౓ͱͷର– 98 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

Fig. 1. Elemental mappings on LiB anode surface by SEM-EDX, (a) intensity distribution of C-K characteristic X-ray and (b) intensity distribution of Mn-K characteristic X-ray.

Fig. 2. Intensity distribution of Mn-K characteristic X-ray on LiB anode surface by micro-beam XRF, (a)sample A (before charge-discharge cycling test), (b) sample B (after charge-discharge cycling test, small
capacity decrease case), and (c) sample C (after charge-discharge cycling test, large capacity decrease case).

– 99 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

Fig. 3. Intensity distribution of Mn-K characteristic X-ray in LiB anode cross-section by micro-beam XRF,(a) SEM image of measured region and (b) intensity distribution of Mn-K characteristic X-ray.

ϯτϥετͷมԽ͕‫ݟ‬ΒΕͳ͍ɽ͜Εʹର͠ɼࢼ‫ޙݧ‬݁Ռ͓Αͼߟ࡯
‫ݩ‬ૉ෼෍Λ µm ͔Βαϒ µm εέʔϧͰଌఆํ๏ͱ
ͯ͠͸ɼϚΠΫϩϏʔϜ XRF ͷ΄͔ʹిࢠϓϩʔϒΛ༻͍ͨ EPMA ΍ SEM-EDX ͕͋ΔɽFig. 1 ʹ༧උతʹߦͬͨ SEM-EDX ʹΑΔΧʔϘϯෛ‫ۃ‬ද໘ͷ‫ݩ‬ૉϚοϐϯάͷ݁ՌΛࣔ͢ɽࢼྉʹ͸࠷΋ྼԽͨ͠ి

ͷࢼྉ (sample Bɼsample C) Ͱ͸ෛ‫׆ۃ‬෺࣭ͷେ͖͞Λ൓өཻͨ͠ঢ়ͷ෼෍͕‫͞࡯؍‬Εͨɽ͜ͷ݁Ռ͸ɼ

sample Bɼsample C Ͱ͸ɼෛ‫׆ۃ‬෺࣭ͷද໘ʹ Mn‫෇͕ࢠݪ‬ண͍ͯ͠Δ͜ͱΛ͍ࣔͯ͠Δɽ·ͨɼ૾ͷ໌Δ͔͞Βɼsample B ΑΓ΋ sample C ͷ΄͏͕ Mn ‫ݪ‬ࢠͷ෇ணྔ͕ଟ͍͜ͱ΋Θ͔Δɽ͢ͳΘͪɼి஑ಛੑ

஑͔ΒऔΓग़ͨ͠ෛ‫ۃ‬Λ༻͍ͨ (sample C)ɽ

Fig. 1(a) ͸ C-K ಛੑ̭ઢͷ‫౓ڧ‬෼෍Ͱ͋Δɽ‫׆‬෺࣭ (ΧʔϘϯཻࢠͷ) ‫ܗ‬ঢ়Λ൓өͨ͠෼෍͕ಘΒΕͯͷྼԽ౓ͱෛ‫෇ʹ্ۃ‬ணͨ͠ Mn ΠΦϯͷྔͱͷؒʹରԠ͕‫ݟ‬ΒΕͨɽ͍Δɽ͜Εʹର͠ Mn-K ಛੑ̭ઢͷϚοϐϯά͸΄࣍ʹɼsample C ͷஅ໘ࢼྉΛ࡞੡͠ɼి‫ۃ‬அ໘ʹ͓΅Ұ༷Ͱ͋Δɽ͜Ε͸ಘΒΕͨಛੑ̭ઢͷ‫͕౓ڧ‬খ͍ͯ͞ Mn-K ಛੑ̭ઢͷ‫౓ڧ‬ϚοϐϯάΛࢼΈͨɽFig.

͍ͨΊͰ͋Δͱߟ͑ΒΕΔɽSEM-EDX Ͱ͸ɼMn ͕

3(a) ͸ଌఆྖҬͷ SEM ૾Ͱ͋Δɽ޲͔ͬͯࠨଆ͕ి

ଘࡏ͢Δ͜ͱ͸໌Β͔ʹͳΔ͕ɼ෼෍ʹؔ͢Δ৘ใΛ‫ۃ‬ද໘Ͱ͋Γɼӈଆͷଳঢ়ͷന৭ͷྖҬ͕ूిମͰ͋

ಘΔ͜ͱ͸ࠔ೉Ͱ͋Δɽ์ࣹޫΛ༻͍ͨ XRF ଌఆͰΔɽ(b) ͸ Mn-K ಛੑ̭ઢͷ‫౓ڧ‬෼෍Ͱ͋Δɽి‫ۃ‬ද͸ߴً౓ͷ̭ઢΛ༻͍Δ͜ͱ͕Ͱ͖ΔɽΑͬͯɼ‫ݩ‬ૉ໘ʹ͍ۙྖҬͰ‫͕౓ڧ‬େ͖͘ɼूిମ΁޲͔͏ʹͨ͠Ϛοϐϯάʹे෼ͳ‫౓ڧ‬ͷಛੑ̭ઢΛಘΔ͜ͱ͕Ͱ͖

͕ͬͯ‫ݮ͕౓ڧ‬ਰ͍ͯ͠Δ͜ͱ͕Θ͔Δɽਖ਼‫͔ۃ‬Β౸

Δͱ‫ظ‬଴͞ΕΔɽ

ୡͨ͠ Mn ΠΦϯ͕‫׆‬෺࣭ͷද໘ʹ෇ண͍ͯ͠Δͱ

Fig. 2 ʹෛ‫ۃ‬ද໘ͷ Mn-K ಛੑ̭ઢͷ‫౓ڧ‬෼෍Λߟ͑Δͱɼ‫׆‬෺࣭ͷ୺෦Ͱ‫͕౓ڧ‬େ͖͍Ϛοϐϯά݁ࣔ͢ʢࢼྉεςʔδ͸ 1.0 ɹ µm εςοϓͰεΩϟϯՌ͕ಘΒΕΔ͸ͣͰ͋Δɽ͔͠͠ɼಛੑ̭ઢ‫͕౓ڧ‬େ

ͨ͠ʣɽFig. 2(a) ͔Β (c) ͸ͦΕͧΕ sample A(ࢀ͖͍Ґஔ͕‫׆‬෺࣭୺෦ʹҰக͍ͯ͠ͳ͍ྖҬ΋ଘࡏ͢রࢼྉ)ɼsample B(ྼԽখ)ɼsample C(ྼԽେ) ͷ݁Δɽͨͱ͑͹‫ؙ‬ҹͰғΜͩྖҬͷ‫͕౓ڧ‬େ͖͍෦෼͸

ՌͰ͋Δɽ໌Δ͍΄Ͳ Mn-K ಛੑ̭ઢͷ৴߸‫͕౓ڧ‬

ରԠ͢Δ SEM ૾Ͱ‫׆‬෺࣭ͷ֎‫ͱܗ‬Ұக͍ͯ͠ͳ͍ɽ

େ͖͍ɽsample A ͸৴߸‫͕౓ڧ‬খ͘͞ɼ΄ͱΜͲίࠓճͷଌఆʹ͓͍ͯ͸ೖࣹ̭ઢͷਐߦํ޲ʹ਺े µm– 100 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू
ͷਂ͔͞Βͷಛੑ̭ઢΛ‫ݕ‬ग़͍ͯ͠ΔɽΑͬͯɼஅ໘

ࠓ‫ޙ‬͸ɼਖ਼‫͚͓ʹۃ‬ΔભҠۚଐ෼෍ͷධՁ΍ྼԽ౓

SEM Ͱ͸‫͞࡯؍‬Εͳ͍಺෦ͷ‫׆‬෺࣭‫ܗ‬ঢ়΋ಛੑ̭ઢͷҟͳΔి‫ۃ‬ͷભҠۚଐ෼෍ධՁͳͲʹຊख๏Λద༻ͷ‫౓ڧ‬෼෍ʹ൓ө͞Ε͍ͯΔՄೳੑ͕͋Δɽ

͠ɼϦν΢ϜΠΦϯೋ࣍ి஑ͷྼԽ‫ߏػ‬Λ໌Β͔ʹ͢Δ༧ఆͰ͋Δɽࠓ‫ޙ‬ͷ՝୊
Ϧν΢ϜΠΦϯೋ࣍ి஑ͷྼԽ‫ߏػ‬Λղ໌͢Δखஈँࣙͱͯ͠ɼϚΠΫϩ XRF Λ༻͍ͨભҠۚଐϚοϐϯά

ຊ‫ڀݚ‬͸ SPring-8 ฌ‫ݝݿ‬ϏʔϜϥΠϯ BL24XU ʹΛ‫ݕ‬౼ͨ͠ɽෛ‫ۃ‬ද໘্ͱஅ໘ͷ Mn ෼෍ΛධՁͯ͠ߦΘΕ·ͨ͠ɽ࣮‫ݧ‬શൠʹ͓͍ͯฌ‫ݝݿ‬φϊςΫ‫ݚ‬ͨ݁ՌɼҎԼͷ͜ͱΛ໌Β͔ʹͨ͠ɽฏ໘ଌఆ͔Β͸‫֤ॴڀ‬Ґɼฌ‫ཱݝݿ‬େֶେֶӃ෺࣭ཧֶ‫ڀݚ‬Պ ࿜ౡ‫ݚ‬Mn ͕‫׆‬෺࣭ͷද໘ʹ෇ண͍ͯ͠Δ͜ͱɼ෇ணྔͱి

‫֤ࣨڀ‬Ґʹ͝‫ͨ͠·͖͍ͩͨྗڠ‬ɽਂँ͍ͨ͠·͢ɽ஑ͷྼԽ౓ʹରԠ͕͋Δ͜ͱ͕໌Β͔ʹͳͬͨɽࢼߦ
తʹߦͬͨஅ໘ଌఆ͔Β͸ɼMn ͷ෼෍͕ి‫ۃ‬ද໘͔ࢀߟจ‫( ݙ‬References)Βूిମʹ޲͔ͬͯ‫ݮ‬ਰ͢Δ෼෍Ͱ͋Δ͜ͱ໌Β͔ʹ

[1] H. Tsunekawa, S. Tanimoto, R. Marubayashi, M.
Fujita, K. Kifune, and M. Sano: J. Electrochem.
Soc. 149, A1326 (2002).

ͳͬͨɽ– 101 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

BL08B2

2012A3306

߹੒ΰϜͷߏ଄ͱಛੑͱͷ૬ؔੑ– ̭ઢࢄཚղੳʹΑΔҰ࣠৳௕݁থԽ‫ڍ‬ಈͷ‫– ࡯؍‬Relationship Between Structure and Properties
on Synthetic Rubber– Observation of Uniaxial Strain-Induced Crystallization
by Wide Angle X-ray Scattering (WAXS) Measurement –‫ ੉ؠ‬উ߂ 1 ɺࠓઘ ެ෉ 2 ɺদԼ ࢙஧ 2 ɺࡔຊ ௚‫ ل‬2
Katsuhiro Iwase1 , Kimio Imaizumi2 , Tadashi Matsushita2 , Naoki Sakamoto2
1
1

ѴԽ੒έϛΧϧζ‫ࣜג‬ձࣾɼ2 ѴԽ੒‫ࣜג‬ձࣾ

Asashi Kasei Chemicals Corporation, 2 Asashi Kasei Corporation֓ཁɿɹ߹੒ΰϜͷߏ଄ͱ෺ੑͱͷ૬ؔੑΛௐ΂Δ໨తͰɼछʑͷϙϦϒλδΤϯ‫ࡐܥ‬ྉΛ༻͍ͯɼҰ࣠৳௕ม‫࣌ܗ‬ͷߏ଄มԽΛ̭ઢࢄཚख๏ʹΑͬͯղੳͨ͠ɽͦͷ݁ՌɼϙϦϒλδΤϯ‫ࡐܥ‬ྉʹ͓͍ͯҰఆͷԆ৳ഒ཰ʹ·Ͱ৳௕͞Εͨࢼྉʹ͍ͭͯ݁থԽ͢Δ͜ͱ͕֬ೝ͞Εͨɽ͜ͷ͜ͱ͸ɼैདྷ͔Β஌ΒΕ͍ͯΔఱવΰϜͷ৳௕݁থԽʹ૬౰͢Δ‫ݱ‬৅Ͱ͋Δ͜ͱ͕ࣔࠦ͞ΕΔɽΩʔϫʔυɿɹϙϦϒλδΤϯɼҰ࣠৳௕ɼ৳௕݁থԽɼ̭ઢࢄཚ

എ‫ڀݚͱܠ‬໨తҰํɼ্ड़ͷఱવΰϜͷ‫ج‬ຊߏ଄Λ߹੒ΰϜͷਫ਼ີఱવΰϜ͸ɼैདྷ͔Β༷ʑͳ෼໺ʹ༻͍ΒΕ͖ͯͨ୅දతͳ൚༻ߴ෼ࢠࡐྉͰ͋Δɽۙ೥ɼ‫ʹڥ؀‬΍͍͞͠ɼলࢿ‫ݯ‬ɾΤωϧΪʔʹ༏Εͨૉࡐͱͯ͠ɼఱવΰϜฒͼʹ߹੒ΰϜͱछʑͷॆరࡐͱΛෳ߹Խͨ͠ࡐྉ
͕஫໨͞Ε͍ͯΔɽΑ͘஌ΒΕ͍ͯΔΑ͏ʹɼఱવΰϜ͸‫ۃ‬Ίͯ༏Εͨ‫ػ‬ցతͳಛੑͱ଱‫ٱ‬ੑͱΛ͋Θͤ΋ͪɼྫ͑͹ɼҾுԠྗΛ֎৔ͱͯ͠ҹՃ͢Δ͜ͱʹΑͬͯɼ৳௕ํ޲ʹ
݁থԽ͢Δ‫ݱ‬৅ʢ৳௕݁থԽʣ͕ใࠂ͞Ε͍ͯΔ [1]ɽ͜͏ͨ͠ಛҟతͳ෺ੑΛൃ‫͢ݱ‬Δཧ༝ͱͯ͠ɼఱ
વΰϜͷ‫ج‬ຊߏ଄Λͳ͢ϙϦʢγε 1,4-ΠιϓϨϯʣʹඇΰϜ੒෼Ͱ͋ΔλϯύΫ࣭΍ࢷ࣭͕ଘࡏ͢Δ͜ͱɼϙϦʢγε 1,4-ΠιϓϨϯʣͷ΋ͭߴཱ͍ମ‫ن‬ଇߏ଄͕ߟ͑ΒΕ͍ͯΔ [2]ɽ͜ΕΒͷϛΫϩߏ଄ʹͭͳ෼ࢠઃ‫ʹܭ‬Αͬͯୡ੒͠Α͏ͱ͢ΔࢼΈʹ͍ͭͯ΋‫਺͕ྫڀݚ‬ଟ͘ใࠂ͞Ε͍ͯΔɽྫ͑͹ɼ߹੒ΰϜͷ୅දతͳྫͱͯ͠ɼϙϦϒλδΤϯ΍ϙϦΠιϓϨϯ
౳ͷ‫ج‬ຊࠎ֨ߏ଄Λਫ਼ີॏ߹๏ʹΑ੍ͬͯ‫͠ޚ‬ɼ͞ΒʹɼͦΕΒͷՍ‫ڮ‬ମʹΧʔϘϯϒϥοΫ΍γϦΧͳͲͷແ‫ॆػ‬రࡐྉΛ഑߹ͤ͞Δࡍͷ෼ࢄੑΛ੍‫͢ޚ‬ΔͳͲͷ‫ݕ‬౼΋ߦΘΕ͓ͯΓɼࡐྉͱͯ͠ͷಛੑΛ͞Βʹ޲্ͤ͞Δ͜ͱ͕Մೳͱͳ͍ͬͯΔɽ
ΘΕΘΕ͸ɼ͜ΕΒͷߴ‫ػ‬ೳੑࡐྉΛ։ൃ͢Δʹࡍͯ͠ɼߴ౓ʹ෼ࢠઃ‫͞ܭ‬ΕͨϙϦϚʔͷߏ଄ͱ෺ੑͱ
ͷؔ܎Λղ໌͢ΔͨΊʹɼେ‫ࢪޫࣹ์ܕ‬ઃʢSPring-8ʣΛ΋͍ͪͨߏ଄ղੳΛߦ͍ͬͯΔɽ
ϙϦϒλδΤϯ‫ࡐܥ‬ྉͷҰ࣠Ԇ৳ʹΑΔ݁থԽ‫ڍ‬ಈ͍ͯɼ̭ઢࢄཚʢWAXS ˍ SAXSʣ΍தੑࢠઢࢄཚ

ࢢൢͷ߹੒ΰϜʢTable 1ʣ͓ΑͼఱવΰϜΛೖख

ʢSANSʣʹΑΔղੳ͕ߦΘΕ͓ͯΓɼ্‫ه‬ͷΑ͏ͳಛͯ͠ɼͦΕͧΕҎԼͷํ๏ʹͯҰ࣠ํ޲΁ͷ৳௕աఔҟతͳ෺ੑൃ‫ͱݱ‬ͷؔ܎ʹ͍ͭͯ΋ৄࡉͳ‫͞ͳ͕ڀݚ‬Λ޿̭֯ઢࢄཚ๏ʢWAXSʣʹͯ௥੻ͨ͠ɽTable 1Ε͍ͯΔ [3]ɽ

ʹ͓͍ͯɼ“Micro-Structure” ͸֤ࢼྉͷγεߏ଄୯ҐϞϧ෼཰ [%] Λࣔ͠ɼML1+4 ɼMw ɼMn ɼMw /Mn– 102 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

Table 1. Samples (commercial products).
SampleMicro-Structure

ML1+4

Mw [10−4 ]Mn [10−4 ]Mw /MnSample A

97

60

68

28

2.4

Sample B
Sample C

97
96

25
45

42
52

18
22

2.3
2.4

Sample D
Sample E
Sample F

97
98
97

42
45
45

47
45
51

19
16
14

2.5
2.8
3.7

͸ͦΕͧΕɼϜʔχʔ೪౓ʢ100◦ Cʣɼॏྔฏ‫ۉ‬෼ࢠ3) Ұ࣠Ԇ৳഑޲ྔɼ਺ฏ‫ۉ‬෼ࢠྔɼ෼ࢠྔ෼෍Λද͢ɽࢼྉΛઐ༻ͷҰ࣠Ԇ৳૷ஔʹͯɼԆ৳଎౓ɿ0.1ɼ1.0ɼ࣮‫ݧ‬͸ SPring-8 ϏʔϜϥΠϯɿBL08B2 ʹ͓͍ͯଌఆ࣮ࢪͨ͠ɽ

͓Αͼ 5.0 mm/sec Ͱ৳௕ͤͨ͞ʢ࠷େԆ৳ഒ཰ɿ1400

%ʣ.

1) ࢼྉ
ϙϦϒλδΤϯʢະՍ‫ڮ‬ʣࢼྉΛ༻͍ͨɽΫϩϩ݁Ռ͓Αͼߟ࡯

ϑΥϧϜ·ͨ͸ THF ʹ༹ղʢ1 wt%) ͤͨ͞‫ޙ‬ɼৗԹࠓճͷଌఆʹ༻͍ͨະՍ‫ڮ‬ϙϦϒλδΤϯࢼྉͰԼʹ੩ஔ༹ͯ͠ഔΛআ‫ͯ͠ڈ‬ബບΛௐ੡ͨ͠ʢບްɿ

0.2ʙ2.0 mmtʣɽ͸ɼԆ৳ഒ཰ґଘੑ͕͋ΓɼԆ৳ഒ཰͕໿ 1,150 %Ͱ

2) ̭ઢࢄཚଌఆʢFig. 1 ࢀরʣ͸݁থԽ͕‫ݟ‬ΒΕͣɼඇথͷϋϩʔ͕‫͞࡯؍‬ΕΔͷΈҰ࣠৳௕աఔʹ͓͚Δࢄཚଌఆʢin-situ WAXSʣΛͰ͋ͬͨɽͦΕʹରͯ͠Ԇ৳ഒ཰͕໿ 1,200 %Ҏ্Ͱ࣮ࢪͨ͠ɿ݁থԽ͢Δ͜ͱ͕෼͔ͬͨʢFig. 2 ࢀরʣɽ͜͜Ͱड़

ʀ‫ݕ‬ग़
೾௕ɿ0.1 nmʀΧϝϥ௕ɿ104.3 mmʢWAXSʣ΂ͨԆ৳ഒ཰͸νϟοΫؒ‫͔཭ڑ‬Βࢉग़͞Εͨ΋ͷͰʀଌఆ࣌ؒɿ0.2ɼ
‫ث‬ɿೋ࣍‫ݩ‬൒ಋମ‫ݕ‬ग़‫ث‬ʢPILATUSʣ͋Γɼଌఆ෦ҐͷԆ৳ഒ཰ͱ͸ҟͳΔɽ࣮ࡍɼࢼྉԆ

1.0ɼ5.0 sec/ճɽ৳աఔΛϞχλʔ͢Δ͜ͱʹΑΓɼ݁থԽ௚લʹࢼྉ

Fig. 1. Uniaxial extensometer for in situ WAXS measurement.

– 103 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

Fig. 2. Uniaxial strain-WAXS in situ measurement with Sample A.

͕ωοΩϯά͍ͯ͠Δ͜ͱΛ֬ೝ͍ͯ͠ΔɽFig. 2 ʹΤϯ‫ࡐܥ‬ྉͷઃ‫ܭ‬৚݅ͱ෺ੑͱͷؔ܎Λ໌Β͔ʹ͢Δࣔͨ͠Α͏ʹɼ݁থԽલ‫ࢼͰޙ‬ྉͷ̭ઢಁա཰͕େ͖

ͱͱ΋ʹɼԆ৳݁থԽ‫ڍ‬ಈʹ͓͚ΔఱવΰϜͱͷ‫ڍ‬ಈ͘૿Ճ͍ͯ͠Δ͜ͱ͕෼͔ΔɽҼΈʹɼఱવΰϜʹͭͷҧ͍Λൺֱ‫ݕ‬౼͢Δ༧ఆͰ͋Δɽ͍ͯ͸ൺֱత௿Ԇ৳ഒ཰ʢ300∼400 %ʣʹ͓͍ͯԆ৳ँࣙ݁থԽ͢Δ͜ͱ͕ใࠂ͞Ε͍ͯΔɽ
ͳ͓ɼࠓճͷଌఆ݁Ռ͔ΒɼະՍ‫ڮ‬ϙϦϒλδΤϯ
ࢼྉͷԆ৳Ͱ͸ɼԆ৳଎౓ґଘੑ͕‫ݦ‬ஶͰ͋Γɼ‫ۃ‬ΊͯΏͬ͘ΓͱԆ৳ͨ͠৔߹ʢԆ৳଎౓ɿ0.1 mm/secʣͰ͸݁থԽ͕ೝΊΒΕͳ͔ͬͨɽҰํɼൺֱతߴ͍Ԇ৳଎౓Լʢ1.0ɼ5.0 mm/secʣͰ͸ɼ໌Β͔ʹ݁থԽ͕ೝΊΒΕͨʢFig. 2 ࢀরʣɽ͜Ε͸ߴ෼ࢠ࠯ͷ؇࿨‫ݱ‬৅͕Ө‫͍ͯ͠ڹ‬Δ΋ͷͱߟ͑ΒΕɼࠓ‫ޙ‬ɼࢼྉͷ೪஄ੑಛੑͱͷ૬ؔɼಛʹ؇࿨࣌ؒͱԆ৳଎౓͓Αͼ݁থԽͷؔ܎Λௐ΂͍ͯ͘ඞཁ͕͋Δͱߟ͑Δɽެӹࡒஂ๏ਓͻΐ͏͝Պֶٕज़‫ڠ‬ձʢ์ࣹޫφϊςΫ‫ॴڀݚ‬ʣ‫܂‬ຊ ࣎ੜࢯଞͷؔ܎ऀͷօ༷ʹ‫ँײ‬ਃ্͛͠·͢ɽࢀߟจ‫ݙ‬[1] Y. Ikeda and S. Kohjiya: J. Soc. Rheol. Jpn. 36,
9-17 (2008).
[2] Y. Tanaka: Rubber Chem. Technol. 74, 355-375(2001).
[3] T. Karino et al: Biomacromol. 8, 693-699 (2007).

ࠓ‫ޙ‬ͷ՝୊
ࠓ‫ޙ‬ɼΘΕΘΕ͸ߴ౓ʹ෼ࢠઃ‫͞ܭ‬ΕͨϙϦϒλδ

– 104 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

BL24XU

2011B3205

Ϧν΢ϜΠΦϯి஑ਖ਼‫ࡐۃ‬ͷ์ిաఔʹ͓͚Δ‫ߏॴہ‬଄มԽThe Structure of LiCoO2 -Type Cathodes with the Discharge
Process at the Local Areas in Li Ion Batteriesத઒ ෢ࢤɼ੨໦ ༃ਔɼԬా Ұ޾
Takeshi Nakagawa, Yasuhito Aoki, Kazuyuki Okada(‫ )ג‬౦ϨϦαʔνηϯλʔ
Toray Research Center Inc.

֓ཁɿຊ‫Ͱڀݚ‬͸ɼϦν΢ϜΠΦϯి஑ਖ਼‫͍ͯͭʹۃ‬ɼ์ిաఔʹ͓͚Δి‫ࡎ߹ۃ‬ͷްΈํ޲ͷ Li ઎༗ঢ়ଶ
Λ஌ΔͨΊʹɼ์ࣹޫϚΠΫϩϏʔϜʹΑΔϥΠϯଌఆΛߦͬͨɽͦͷ݁Ռɼ‫׬‬શʹ์ిͨ͠ࢼྉʹؔͯ͠͸ɼ૚ঢ়‫ؠ‬Ԙߏ଄ͷ c ࣠ʹ૬౰͢Δ 003 ϐʔΫҐஔ͸ްΈํ޲Ͱ໌֬ͳมԽ͸ͳ͍͕ɼ‫׬‬શ์ిʹͳΔલʹ์ిΛऴྃͨ͠ࢼྉʹؔͯ͠͸ɼి‫ࡎ߹ۃ‬ͷද໘ଆͰଞͷՕॴΑΓ΋௿֯ଆʹ‫͞࡯؍‬Εͨɽ003 ϐʔΫͷ௿֯΁ͷγϑτ͸ Li ͷ୤཭ʹΑͬͯ‫͞࡯؍‬ΕΔͨΊɼ‫׬‬શ์ిʹͳΔલʹ์ిΛऴྃͨ͠ࢼྉʹ͓͍ͯ͸ Li ͕୤཭ͨ͠
··ͷՕॴ͕ి‫ࡎ߹ۃ‬ͷද໘ଆʹଘࡏ͢ΔͱࢥΘΕΔɽͭ·ΓɼAl ूిഩଆ͔Βॱʹ Li ͷ‫ٵ‬ଂ͕ߦΘΕɼి‫ࡎ߹ۃ‬ද໘ଆ͸‫͔ޙ‬Β‫ٵ‬ଂ͞ΕΔͱࢥΘΕΔɽΩʔϫʔυɿɹ์ࣹޫϚΠΫϩϏʔϜɼ̭ઢճંɼϦν΢ϜΠΦϯి஑ɼਖ਼‫ۃ‬എ‫ڀݚͱܠ‬໨త

situ ΍ in situ XRD ʹΑΔ݁থߏ଄ͷมԽ͕‫͞ڀݚ‬ΕϦν΢ϜΠΦϯి஑͸ 2 ࣍ి஑ͱ༷ͯ͠ʑͳ༻్Ͱ࢖༻͞ΕΔɽߴ༰ྔɼ௿ྼԽͳͲɼଞͷ 2 ࣍ి஑ͱൺ
ֱͯ͠༗རͳϦν΢ϜΠΦϯి஑Ͱ͋Δ͕ɼॆ์ిͷ‫܁‬Γฦ͠ɼྼѱͳ࢖༻‫ڥ؀‬ɼॆిঢ়ଶͷ์ஔ౳ͰྼԽ
͢Δ͜ͱ͕஌ΒΕ͍ͯΔɽ·ͨɼCo ͸‫ك‬গۚଐͱͯ͠
ߴՁͳࡐྉͰ͋Γɼͦͷ࢖༻ྔΛ࡟‫ͤ͞ݮ‬Δඞཁ΋͋Δɽ‫Ͱࡏݱ‬͸ɼ૊੒ΛมԽ༷ͤͨ͞ʑͳ૊੒ͷਖ਼‫ࡐۃ‬͕։ൃ͞Ε͓ͯΓɼ૚ঢ়‫ؠ‬Ԙߏ଄Λ΋ͭχοέϧ‫ܥ‬΍ 3‫( ܥݩ‬Ni,Co,Mn)ɼ·ͨεϐωϧ‫ܥ‬ʢLi(Fe,Mn)PO4 ʣͳͲଟ༷ͳਖ਼‫͕ࡐۃ‬ੜΈग़͞Ε͍ͯΔɽ·ͨɼͦΕͧΕͷࡐྉͷಛ௃Λੜ͔͠ɼͦΕΒΛࠞ߹ͯ͠࢖༻͢Δ
ͳͲ༷ʑͳࢼΈ͕ͳ͞Ε͍ͯΔɽ
Ϧν΢ϜΠΦϯి஑ͷॆ์ి͸ɼLi ͷ୤཭ɼ‫ٵ‬ଂɼ͓ΑͼిࢠͷतडʹΑͬͯͳ͞ΕΔɽਖ਼‫׆ۃ‬෺࣭ͷ Liใࠂ͞Ε͍ͯΔ [1, 2]ɽ͔͠͠ͳ͕Βɼి‫ࡎ߹ۃ‬ͷৄࡉͳߏ଄มԽ΍ߏ଄෼෍ʹؔͯ͠ͷ‫ྫڀݚ‬͸গͳ͍ɽ์ࣹޫϚΠΫϩϏʔϜ̭ઢճંͰ͸ɼ1 µmφ ͋Δ͍͸ͦΕҎԼͷϏʔϜαΠζ͕ར༻Մೳͱͳ͖ͬͯͯ
͓ΓɼϑΟϧϜ΍ણҡࢼྉͳͲͷߴ෼ࢠࡐྉ͔ΒɼηϥϛοΫε΍ۚଐࡐྉͳͲແ‫ࡐػ‬ྉͱ༷ʑͳ෼໺Ͱɼ
ද૚ɼ಺෦ͷ݁থੑ΍݁থ഑޲ੑͳͲɼࢼྉͷ৔ॴʹΑΔҧ͍͕ΑΓৄࡉʹղੳ͞Ε͍ͯΔɽͦ͜Ͱɼຊ‫ݚ‬‫Ͱڀ‬͸ɼ์ి‫ܦ‬աͷ్தʹ͓͚Δి‫͍ͯͭʹࡎ߹ۃ‬ϚΠΫϩϏʔϜΛ༻͍ͨϥΠϯ෼ੳΛߦ͏͜ͱʹΑΓɼి‫ࡎ߹ۃ‬ͷްΈํ޲ͷߏ଄ࠩҟΛ‫ݟ‬ग़͢͜ͱΛ໨తͱ
ͨ͠ɽ
࣮‫ݧ‬

ͷ୤཭͸ͦͷߏ଄ʹมԽΛ༩͑ΔͨΊɼLi ͷ୤཭ͷఔଌఆʹ͸ɼ૚ঢ়‫ؠ‬Ԙߏ଄Λ΋ͭਖ਼‫׆ۃ‬෺࣭Ͱߏ੒͞

౓ʹΑΓɼͦͷߏ଄มԽͷ౓߹͍͕ҟͳΔɽͦͷͨΊɼΕΔࢢൢͷి‫ࡎ߹ۃ‬Λࢼྉͱͯ͠༻͍ͨɽॆ์ి༻

Li ΍ిࢠͷतडʹΑΔਖ਼‫׆ۃ‬෺࣭ͷߏ଄มԽ͕ɼి‫ۃ‬ϋʔϑηϧΛ༻͍ɼ4.2 V ·Ͱॆిͨ͠ɽ࣍ʹ 3.5 V߹ࡎશମʹ͓͍ͯͲͷΑ͏ʹ෼෍͍ͯ͠Δ͔ΛධՁ͢·Ͱ์ి͠ɼͦͷిѹʹୡͨ͠‫ޙ‬ɼిྲྀͷ‫ؒ࣌څڙ‬ΛΔ͜ͱ͸ɼి஑ͷੑೳɼྼԽΛ‫ݕ‬౼͢Δ্ͰॏཁͰ͋

ม͑ͨ΋ͷ 2 ࢼྉʢ(1)30 ෼ (ҎԼ sample1)ɼ(2) ‫׬‬શΔͱࢥΘΕΔɽਖ਼‫׆ۃ‬෺࣭ͷߏ଄มԽʹؔͯ͠͸ɼex– 105 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)์ి (ҎԼ sample2) ΛͦΕͧΕ࡞੡͠ɼथࢷแຒ͠ɼ

݁Ռ͓Αͼߟ࡯

அ໘࡞੡Λߦͬͨɽ
࣮‫ݧ‬͸ BL24XU B2 ϋονʹͯߦ͍ɼ‫ݕ‬ग़‫ʹث‬͸

FlatPanel Λ༻͍ͨɽೖࣹϏʔϜ͸κʔϯϓϨʔτΛ༻͍ͨूޫޫֶ‫͍ߦͰܥ‬ɼೖࣹϏʔϜαΠζ͸໿ 0.3µm × 0.6 µmɼ೾௕͸໿ 0.827 Åʢ15 keVʣɼΧϝϥ௕͸໿ 55 mm Ͱ͋ΔɽଌఆՕॴ͸ɼAl ഩి‫ۃ‬ଆ͔Β‫׆‬෺࣭ද໘ଆʹ޲͔ͬ
ͯ 10 µm εςοϓͰϥΠϯଌఆͨ͠ɽ࿐ޫ࣌ؒ͸֤Ґஔʹ͓͍ͯ 60 ඵͰ͋ΔɽಘΒΕͨ 2 ࣍‫ݩ‬ճં૾ (Fig.

1) ͸ɼ‫౓ڧ‬ͷิਖ਼౳Λߦ͍ɼԁ‫ੵ؀‬෼Λͯ͠Ұ࣍‫ݩ‬Խ
(Fig. 2) ͯ͠ղੳʹ༻͍ͨɽ

sample1 ͷ֤Օॴͷ޿̭֯ઢճંύλʔϯΛ Fig. 2ʹࣔ͢ɽ֤ϐʔΫ͸ɼ૚ঢ়‫ؠ‬Ԙ‫ߏܕ‬଄Ͱࢦ਺෇͚͞ΕΔϐʔΫ͕‫͞࡯؍‬Εͨɽ͜ͷߏ଄ͷ c ࣠ํ޲ʹਨ௚ͳ໘ִؒʹରԠ͢Δ 003 ϐʔΫʹ஫໨͢Δͱɼsample1
ͱ sample2 Ͱ͸ɼLi ͷೖΓ۩߹͕ूిഩʹ͍ۙՕॴͱ཭ΕͨՕॴͰ͸ɼҟͳΔ͜ͱ͕Θ͔ͬͨɽFig. 3 ͓Αͼ Fig. 4 ʹɼ֤ࢼྉͷ֤ଌఆՕॴʹ͓͚Δ޿̭֯
ઢճંύλʔϯ (003 ϐʔΫ෇ۙ) Λࣔ͢ɽsample2 ʹؔͯ͠͸ɼ૚ঢ়‫ؠ‬Ԙߏ଄ͷ c ࣠ʹ૬౰͢Δ 003 ϐʔΫҐஔ͸ి‫ࡎ߹ۃ‬ͷްΈํ޲Ͱ໌֬ͳมԽ͸ͳ͍ɽ

Fig. 3. The diffraction profile of the sample1 at 003
reflection.
Fig. 1. The X-ray diffraction photograph of the sample1 at 60 µm from the Al electrodes.

Fig. 4. The diffraction profile of the sample2 at 003
reflection.
Fig. 2. The X-ray diffraction patterns, which diffraction peaks are integrated circularly in Fig. 1.

Ұํɼsample1 ʹؔͯ͠͸ɼి‫ࡎ߹ۃ‬ͷද໘ଆͰ 003
ϐʔΫ͕ଞͷՕॴΑΓ΋௿֯ଆʹ‫͞࡯؍‬Εͨɽ003 ϐʔΫͷ௿֯΁ͷγϑτ͸ Li ͷ୤཭ʹΑͬͯ‫͞࡯؍‬ΕΔ
܏޲Ͱ͋Γ [1]ɼ‫׬‬શ์ిʹͳΔલʹిྲྀΛ్தͰࢭΊͨ΋ͷʹ͓͍ͯ͸ɼLi ͕୤཭ͨ͠··ͷՕॴ͕ి‫ۃ‬– 106 –

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू
߹ࡎͷද໘ଆʹଘࡏ͢ΔͱࢥΘΕΔɽͭ·ΓɼAl ूࠓճ͸ɼ૚ঢ়‫ؠ‬Ԙ‫ߏܕ‬଄Λ༗͢Δ‫׆‬෺࣭ʹ͍ͭͯిഩଆ͔Βॱʹ Li ͷ‫ٵ‬ଂ͕ߦΘΕɼి‫ࡎ߹ۃ‬ද໘ଆߦ͕ͬͨɼࠓ‫ޙ‬ɼεϐωϧߏ଄Λ΋ͭ Li(Fe,Mn)PO4͸‫͔ޙ‬Β‫ٵ‬ଂ͞ΕΔͱࢥΘΕΔɽ

΍ҟͳΔ૊੒ͷ‫׆‬෺࣭ʹؔͯ͠΋ߦ͏ඞཁ͕͋Δͱߟ͑Δɽࠓ‫ޙ‬ͷ՝୊
ࢀߟจ‫ݙ‬
ຊ‫͍͓ͯʹڀݚ‬ɼਖ਼‫׆ۃ‬෺࣭಺ͷ෦ࡐશମͱͯ͠ͷߏ଄มԽΛ์ࣹޫϚΠΫϩ XRD ͔ΒͱΒ͑Δ͜ͱ͕
Ͱ͖ɼ์ి‫ܦ‬աͷ్தʹ͓͚Δਖ਼‫׆ۃ‬෺࣭ͷ Li ͷ઎༗ঢ়ଶͷްΈํ޲ͷҧ͍Λ‫ݟ‬ग़͢͜ͱ͕Ͱ͖ͨɽ

[1] J. N. Reimers and J. R. Dahn: J. Electrochem.
Soc. 139, No.8, 2091 (1992).
[2] T. Ohzuku and A. Ueda: J. Electrochem. Soc.
141, No.11, 2972 (1994).

– 107 –

ɹ

兵庫県ビームライン成果発表一覧（２００６年度以降）

発表形式
原著論文

：原著論文／博士論文／査読付きプロシーディングス

総説

：総説

査読無

：査読なしプロシーディングス

招待講演

：招待講演

口頭／ポ

：口頭発表／ポスター発表

JASRI No. ：JASRI 研究成果番号– 109 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)兵庫県ビームライン BL08B2 関連外部発表リスト
JASRI
No.

タイトル

主著者氏名

発表先（日付）所属

実験課題番号

発表形式

Structure Analysis of Nano Particle Suspension by
11425

2007A3300

Ultra-SAXS using Synchrotron Radiation

藤村 栄作
口頭/ポ
兵庫県立大学秋季 応用物理学会学術講演会 （2007.09）

Analysis of PVA-iodine Film with I K-edge Polarization
12833

2007A3303

Dependence XANES Spectra
XAFS 討論会（2008.08）

15111

三木 達郎
口頭/ポ
千葉大学

中津 和弘

2009A3324

高輝度放射光を用いた各種機能性材料の評価

2009A3325

実用表面分析セミナー2009（2009.11）㈱ 住化分析

口頭/ポセンター
SCFT Simulation and SANS Study on Spatial
Distribution of Solvents in Microphase Separation
Induced by a Differentiating Non-Solvent in a

18019

2008A3306

Semi-Dilute Solution of an Ultra-High-Molecular-Weight
Block Copolymer

Koji Ando

原著論文

名古屋工業大学

Journal of Physics: Conference Series
vol. 247, 012040（2010）
Small-Angle X-ray and Neutron Scattering Study on
Microphase Separation Induced by Non-Solvent in a
18024

2008A3306

Semi-Dilute Solution of an Ultra-High-Molecular-Weight Shigeru Okamoto
Block Copolymer

口頭/ポ名古屋工業大学

International Conference on Neutron and X-ray
Scattering 2009 (ICNX2009) （2009.06）
New Analytical Methods for the Surface/Interface andthe Micro-Structure in Advanced Nanocomposite
18794

2008B3300

Materials by Synchrotron Radiation
Atom Indonesia

中前 勝彦
ひょうご科学技術協会

vol. 36, 125-128（2010）– 110 –

招待講演ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

19529

21466

22055

2007A3300

Size of Elementary Clusters and Process Period in Silver

2007B3300

Nanoparticle Formation

2008A3300

Journal of the American Chemical Society

2008B3300

vol. 133, 14164-14167（2011）

2010B3237

X-ray Microbeam Three-Dimensional Topography

2011A3237

Imaging and Strain Analysis of Basal-Plane Dislocations

2011B3237

and Threading Edge Dislocations in 4H-SiC

2011A3321

Applied Physics Express

2011B3321

vol. 5, 061301（2012）

2009B3322

武居 正史
原著論文
バンドー化学㈱田沼 良平(一財）電力中央

原著論文

研究所

Transmission Electron Microscopy Analysis of Threading

Yoshihiro

Dislocation with c + a Burgers Vector in 4H-SiC

Sugawara

Applied Physics Express㈶ファインセラ

vol. 5, 081301（2012）

ミックセンター

原著論文

Drastically Improved Performances of

22076

2011A3346
2011B3346

Graphite/Li1.26Mn0.52Fe0.22O2 Cell with Stepwise

Kentaro

Pre-Cycling Treatment that Causes Peroxide Forming

Nakahara

Journal of the Electrochemical Society

日本電気 ㈱原著論文

vol. 159, A1398-A1404（2012）

22424

2009B3322

LACBED Analysis of Threading Dislocation with c+a

Yoshihiro

Burgers Vector in 4H-SiC

Sugawara

2012 International Conference on Solid State Devices㈶ファインセラand Materials（2012.09）

ミックセンター– 111 –

口頭/ポ

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)兵庫県ビームライン BL24XU 関連外部発表リスト
JASRI
No.

タイトル

主著者氏名

発表先（日付）所属

実験課題番号

発表形式

大視野高分解能 X 線顕微鏡 CT 光学系の構築
16189

2009A3203

橋本 琢人

日本放射光学会年会・放射光科学合同シンポジウム

口頭/ポ兵庫県立大学（2010.01）

フレネルゾーン型 X 線導波路の開発
16192

2009A3202

奥村 健一

日本放射光学会年会・放射光科学合同シンポジウム

口頭/ポ兵庫県立大学（2010.01）

高平行度 X 線マイクロビームによるシリコンエピタキシャ
16343

2006A3202

高畑

小百合

ル層の格子定数評価

口頭/ポ
兵庫県立大学秋季 応用物理学会学術講演会（2006.08）

硬 X 線 Young 干渉計を用いた放射光の空間コヒーレンス評
16344

2007A3203

価秋季 応用物理学会学術講演会 (2007.09)

Ｘ線多層膜ラウエレンズの開発(2) 作製と構造評価
16369

2007B3200

2005B3203

2008B3203

SPring-8/JASRI

市丸(2008.01)

テクノロジ㈱日本放射光学会年会・放射光科学合同シンポジウム

硬 X 線用全反射ゾーンプレートの開発
秋季 応用物理学会学術講演会（2009.09）

辻

口頭/ポ

卓也

SPring-8/JASRI

辻

口頭/ポ

智

NTT アドバンス(2009.01)

16415

卓也

日本放射光学会年会・放射光科学合同シンポジウム

硬 X 線用全反射型集光素子の開発
16414

辻

口頭/ポ

卓也

SPring-8/JASRI

口頭/ポ

斜入射 X 線回折によるシリコンナノ薄膜の歪解析
16519

2006A3102

表面科学

尾身 博雄

Journal of the Surface Science Society of Japan
vol. 28, 678-681（2007）– 112 –

日本電信電話 ㈱総説ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

ナノシリコン層の歪み解析
16520

2007A3102

真空(Journal of the Vacuum Society of Japan)
vol. 51, 298-300（2008）

尾身 博雄
日本電信電話 ㈱総説

斜入射Ｘ線回折による歪み SOI および SOI 基板の評価：ブ16527

2006A3102

ラッグ反射強度の出射角依存性

尾身 博雄

春季 応用物理学関係連合講演会

日本電信電話 ㈱口頭/ポ(2007.03)
斜入射Ｘ線回折による歪 SOI 基板の薄層化プロセスのリア
16530

2008B3102

ルタイム観察
秋季 応用物理学会学術講演会 (209.09)

尾身 博雄
日本電信電話 ㈱口頭/ポDevelopment of Multilayer Laue Lenses; (2) Circular
17387

2009B3200

Type

小山 貴久

International Conference on X-ray Microscopy (XRM)

SPring-8/JASRI

口頭/ポ(2010.08)
フレッシュグリーン表面改質技術によるジルカロイ被覆管
澤部 孝史
17478

2010A3230の耐食性・耐水素吸収特性向上（２）皮膜部の結晶構造解（一財）電力中央

口頭/ポ析
日本原子力学会 2010 年秋の大会(2010.09)

研究所

Development of a Reflection Zone Plate for Hard X-ray
17491

2009A3203

Nanofocusing

辻International Conference on X-ray Microscopy (XRM)

卓也

SPring-8/JASRI

口頭/ポ(2010.08)
X-Ray Micro-Imaging Activities at BL24XU-C1 of
17497

2006A3203

SPring-8

高野 秀和

International Conference on Synchrotron Radiation

兵庫県立大学

口頭/ポInstrumentation (SRI) (2006.05)
Synchrotron Radiation Based Hard X-ray Microscopy at
17498

2005B3203

BL24XU-C1 of SPring-8

高野 秀和

International Microscopy Congress (IMC16)

兵庫県立大学(2006.09)– 113 –

口頭/ポ

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)
SPring-8 兵庫県 ID ビームラインにおけるマイクロイメ
17500

2006B3203

ージング

2007A3203

第９回 X 線結像光学シンポジウム

高野 秀和
口頭/ポ

(2007.11)

兵庫県立大学X 線多層膜ラウエレンズの開発（3） 放射光による性能評
17501

2007A3200

価法の開発

高野 秀和

2007B3200

日本放射光学会年会・放射光科学合同シンポジウム

兵庫県立大学口頭/ポ(2008.01)

17502

2007A3203
2007B3203

2005B3203
17504

2008B3203
2009A3203

Fast X-ray Micro-CT for Real-timee 4D Observation
International Conference on X-ray Microscopy (XRM)(2008.07)

高野 秀和
口頭/ポ
兵庫県立大学全反射型不等間隔回折格子を利用した硬Ｘ線ナノ集光

高野 秀和

第 10 回 X 線結像光学シンポジウム

兵庫県立大学(2009.11)

口頭/ポ

New Nano-scale Imaging with a Simple Hard X-ray
17505

2009A3203“Nano-Slit”

高野 秀和

2009B3203

International Conference on X-ray Microscopy (XRM)

兵庫県立大学口頭/ポ（2010.08）
A Simple Hard X-ray “Nanoslit” for Measuring
17507

2009A3203

Wavefront Intensity

高野 秀和

Review of Scientific Instruments

兵庫県立大学

原著論文

vol. 81, 073702（2010）
Crystallinity Estimation of Area Selective Ge Epitaxial
Layer Grown on Si Substrate by Means of
17550

2008B3202

High-Resolution X-ray Micro Diffraction
International Conference on Synchrotron Radiation in

津坂 佳幸
口頭/ポ
兵庫県立大学

Materials Science (SRMS) (2010.07)
17575

2010A3203

高速Ｘ線マイクロＣＴ光学系の高度化

森川 美穂

秋季 応用物理学会学術講演会 （2010.09)

兵庫県立大学

口頭/ポ
小西 繁輝

17594

2010A3200

Ｘ線円形多層膜ラウエレンズの集光特性評価
秋季 応用物理学会学術講演会 (2010.09)– 114 –

スプリングエイト
サービス(株)口頭/ポฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

Development of Linear and Circular Multilayer Laue
17743

2010A3200

Lenses小山 貴久

The 6th International Workshop on Nano-scale

SPring-8/JASRI

口頭/ポSpectroscopy and Nanotechnology (2010.10)
Separately Contacted Monocrystalline Silicon
Double-Layer Structure with an Amorphous Silicon
17847

2008B3102

Dioxide Barrier Made by Wafer Bonding
Semiconductor Science and Technology

Kei Takashina
日本電信電話 ㈱原著論文

vol. 25, 125001（2010）
2005B3010
2006A3010
18203

2006B3010
2009A3010
2009B3010

Application of SPring-8 to Measure Changes of Internal
Structure of Hair Fiber
光学 (Japanese Journal of Optics)
vol. 39, 550-552（2010）

佐野 則道
P&G イノベーショ

総説

ン合同会社

多層膜ラウエレンズの現状と円形型ラウエレンズへの発展
18310

2009B3200

小山 貴久
日本放射光学会年会・放射光科学合同シンポジウム(2011.01)

SPring-8/JASRI

口頭/ポ

A Structure-based Mechanism for Benzalactone
Synthase from Rheum palmatum
18318

2008A3005

Proceedings of the National Academy of Sciences of theUnited States of America

森田 洋行
原著論文
富山大学

vol. 107, 669-673（2010）
硬 X 線用全反射ゾーンプレートの開発および集光特性評価
18340

2009A3203

日本放射光学会年会・放射光科学合同シンポジウム(2011.01)

辻卓也

SPring-8/JASRI

口頭/ポ

3ｄ遷移金属化合物のプレエッジピーク観察のための高エ18348

2010A3233

ネルギー分解能ＸＡＮＥＳ手法の開発

山下 恵輔

日本放射光学会年会・放射光科学合同シンポジウム

兵庫県立大学口頭/ポ(2011.01)– 115 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

Reply to "Comment on 'Sub-15nm Hard X-Ray Focusing
18491

2009A3203

with a New Total-Reflection Zone Plate' "Applied Physics Express vol. 4, 019102（2011）
金属ワイヤーのみで可能な新しい X 線ナノイメージング法

18492

2009B3203

18652

2009A3203

SPring-8 兵庫県ビームラインにおけるマイクロ CT 及びナ

2009B3203

ノ集光の現状2010A3203

X 線分析討論会 (2010.10)

2009A3203

X 線ナノ集光の現状と展望

2009A3200

Ｘ線分析の進歩 (Advances in X-ray Chemical Analysis,

2009B3200

Japan)

2009B3200

高野 秀和
口頭/ポ
兵庫県立大学高野 秀和
招待講演
兵庫県立大学

vol. 42, 83-94（2011）

Development of Multilayer Laue Lenses; (1) Linear Type
19948

口頭/ポ

日本放射光学会年会・放射光科学合同シンポジウム(2011.01)

18495

高野 秀和
兵庫県立大学4 次元 X 線マイクロ CT の現状
2010A3203

原著論文
兵庫県立大学

日本放射光学会年会・放射光科学合同シンポジウム(2011.01)

18493

高野 秀和

AIP Conference Proceedings
vol. 1365, 24-27（2011）

高野 秀和
総説
兵庫県立大学

小山 貴久
SPring-8/JASRI

原著論文

Development of Multilayer Laue Lenses; (2) Circular
19949

2009B3200

Type

小山 貴久

AIP Conference Proceedings

SPring-8/JASRI

原著論文

vol. 1365, 100-103（2011）
Total-Reflection Zone Plates as New Devices for X-Ray
20339

2009A3203

Nanofocusing

招待講演

SPIE Optics + Photonics 2011(2011.08)
New X-ray Nanofocusing Devices Based on
20340

2009A3203

高野 秀和

Total-Reflection Zone Plates
Proceedings of SPIE vol. 8139,81390D（2011）– 116 –

兵庫県立大学高野 秀和
査読無
兵庫県立大学ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

2008B3203
20341

2009A3203
2009B3203

New Nanoscale Imaging with a Simple Hard X-Ray
Nanoslit

高野 秀和

AIP Conference Proceedings

兵庫県立大学

原著論文

vol. 1365, 297-300（2011）

2008B3203
2009A3203
20342

2009B3203
2010A3203

エッジ回折効果を利用した X 線ナノイメージング法の開発

高野 秀和

第 11 回 X 線結像光学シンポジウム

兵庫県立大学(2011.11)

招待講演

2011A3203

20572

2010B3200

傾斜式微小プリズムアレイＸ線粗集光素子の開発
第 11 回 X 線結像光学シンポジウム(2011.11)

篭島 靖
口頭/ポ
兵庫県立大学

Microstructure of Oxide Layers Formed on Zirconium
Alloy by Air Oxidation,
20595

2009B3230

Uniform Corrosion and Fresh-Green Surface

2010A3230

Modification

澤部 孝史（一財）電力中央

原著論文

研究所

Journal of Nuclear Materials
vol. 419, 310-319（2011）

20686

20799

2010A3203

高速 X 線マイクロ CT 光学系の開発およびダイナミクス測2010B3203

定への応用

2011A3203

第 11 回 Ｘ線結像光学シンポジウム

2010B3203

SPring-8 BL24XU における走査型 X 線顕微鏡の開発

2011A3203

X 線結像光学シンポジウム (2011.11)

2010A3203
20889

2010B3203
2011A3203

口頭/ポ(2011.11)

2010B3200

兵庫県立大学下村 翔
口頭/ポ
兵庫県立大学高速 X 線マイクロ CT 光学系の開発およびダイナミクス測
定への応用

森川 美穂

日本放射光学会年会・放射光科学合同シンポジウム

兵庫県立大学口頭/ポ(2012.01)
放射光 X 線ビームライン用粗集光素子の開発

20912

森川 美穂

篭島

靖

日本放射光学会年会・放射光科学合同シンポジウム

口頭/ポ兵庫県立大学(2012.01)– 117 –

Status Report of Hyogo-Beamlines with Research Results, Vol. 1 (2012)

20934

2011A3203

結像型硬Ｘ線暗視野顕微鏡光学系の開発

東 宏昭

X 線結像光学シンポジウム (2011.11)

兵庫県立大学口頭/ポReal-time Synchrotoron Radiation X-ray Diffraction andAbnormal Temperature Dependence of
20967

2010B3102

Photoluminescence from Erbium Silicates on SiO2/Si
Substrates

尾身 博雄
日本電信電話 ㈱原著論文

AIP Advances vol. 2, 012141（2012）
Energy Transfers between Er3+ Ions Located at the Two
Crystalographic Sites
21032

2011A3102

of Er2O3 Grown on Si(111)Japanese Journal of Applied Physics

尾身 博雄
日本電信電話 ㈱原著論文

vol. 51, 02BG07（2012）
CT 再構成法による X 線円形多層膜ラウエレンズの集光特
21220

2011A3200

性評価
第 11 回

スプリングエイト
X 線結像光学シンポジウム (2011.11)

CT 再構成法による X 線円形多層膜ラウエレンズの集光特
21221

2011A3200

性評価

2011B3200

日本放射光学会年会・放射光科学合同シンポジウム

口頭/ポサービス(株)小西 繁輝
スプリングエイト

口頭/ポサービス(株)(2012.01)

21466

小西 繁輝

2010B3237

X-ray Microbeam Three-Dimensional Topography

2011A3237

Imaging and Strain Analysis of Basal-Plane Dislocations

2011B3237

and Threading Edge Dislocations in 4H-SiC

2011A3321

Applied Physics Express

2011B3321

vol. 5, 061301（2012）

田沼 良平（一財）電力中央

原著論文

研究所

Circular Multilayer Zone Plate for High-Energy X-ray
21784

2010A3200

Nano-Imaging

2010B3200

Review of Scientific Instruments

小山 貴久
SPring-8/JASRI

原著論文

vol. 83, 013705（2012）
Excellent Crystallinity of Truly Bulk Ammonothermal
21813

2007A3222

GaN

R. Dwilięski
Ammono Sp.

Journal of Crystal Growthvol. 310, 3911-3916（2008）– 118 –

z o.o.

原著論文

ฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू

21814

2008A3222

Bulk Ammonothermal GaN

R. Dwilięski

Journal of Crystal Growth

Ammono Sp.

vol. 311, 3015-3018（2009）z o.o.

X-Ray Three-Dimensional Topography Imaging of
21821

2010B3237

Basal-Plane and Threading-Edge Dislocations in 4H-SiC

2011A3237

Materials Science Forumvol. 717-720, 323-326（2012）

原著論文

田沼 良平
（一財）電力中央

原著論文

研究所

Imaging and Strain Analysis of Threading-Edge and21822

2010B3237
2011A3237

Basal-Plane Dislocations in 4H-SiC Using X-ray
Three-Dimensional Topography
Materials Science Forum

田沼 良平（一財）電力中央

原著論文

研究所

vol. 725, 3-6（2012）
X-Ray Three-Dimensional Topography Imaging of
21823

2010B3237

Basal-Plane and Threading-Edge Dislocations in 4H-SiC
International Conference on Silicon Carbide and RelatedMaterials (2011.09)

田沼良平（一財）電力中央

口頭/ポ

研究所

Imaging and Strain Analysis of Threading-Edge andBasal-Plane Dislocations in 4H-SiC Using X-Ray
21824

2011A3237

Three-Dimensional Topography
14th International Conference on Defects-Recognition,

田沼 良平（一財）電力中央

口頭/ポ

研究所

Imaging and Physics in Semiconductors (2011.09)
Ｘ線 3D トポグラフィーによる 4H-SiC 基底面転位および貫21825

2011B3237

田沼 良平

通刃状転位のイメージング
第 20 回 シリコンカーバイド(SiC)及び関連ワイドギャップ
半導体研究会 (2011.12)（一財）電力中央

口頭/ポ

研究所

Inclined-Incidence Quasi-Fresnel Lens for Prefocusing of
22312

2009B3200

Synchrotron Radiation X-ray Beams

2010B3200

Applied Physics Letters

篭島 靖
原著論文
兵庫県立大学

vol. 101, 163102（2012）– 119 –

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ʢদҪɹ‫ه‬ʣฌ‫ݝݿ‬ϏʔϜϥΠϯ೥ใɾ੒Ռू
Vol. 1 20122012 ೥ 12 ݄ ൃ ߦฤूɾҹ࡮ɹฌ‫ޫࣹ์ݝݿ‬φϊςΫ‫ॴڀݚ‬˟ 679-5165 ฌ‫ͭͨݝݿ‬ͷࢢ৽‫ٶ‬ொޫ౎̍ஸ໨ 490-2

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