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úËõ Sept. 2012 Vol.25 No.5  285(C) 2012 The Japanese Society for Synchrotron Radiation ResearchFig. 3Fig. 1(Color online) Ferroelectric phase transition in BaTiO3. Six
kinds of domain are possible in the ferroelectric phase as­sociated with the phase transition from the cubic totetragonal symmetry.

(Color online) Schematic view of P_E hysteresis loop of
BaTiO3­type ferroelectric materials with domain structure
and crystal structure. Total polarization contains contribu­
tions of both the domain orientation (extrinsic) and crystal
structure (intrinsic).

ejdij Ei,

i1, 2, 3,

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(1
)_Q 4mm ÌêCÎÌ«Ì§ñ©ç³êép[^Í d31 d32, d33, d15 Ì 3 ÂÅ
Fig. 2(Color online) Schematic view of possible electric­eld­in­
duced strain in ferroelectric materials. (a) Piezoelectric andelectrostrictive strain. (b) Strain by orientation change of
spontaneous polarization. (c) Strain by electric­eld phasetransition.

é10) B ± ± Å BaTiO3 Ì cÊÉdÉðÆèÂ¯dêðóÁ·éêðl¦éBº·ÅÍ BaTiO3 ÌiqèÍ a3.9920 ÅCc4.0361 Å ÅC
³û»cÝÌÚÀÅ

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286  úËõ Sept. 2012 Vol.25 No.5

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gsbNX ¡ ­UdÌ BaTiO3 ÌdêUNiqcÝÌ_Ci~NXFª X üñÜÉæé¤Ï»ªN±èÇÌæ¤ÉÔÏ»·é©ð~NÈx
Å²×éKvªÉ¸xÇ­Ïª·éB»êçðÅ¬ñæ@ÉæÁÄðÍ

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GlM[úËõ X üP»ñÜÀ±Í SPring­8 ÌP»ñÜÀ±Æª\¢vªðgÝí¹½À±ðvP  » \ ¢ ð Í r [   C  BL02B1 É Ä s í ê ½ B
BL02B1 Í P  » Ì X ü ñ Ü À ± ð s ¤ X e [ V  æµ½BÅCå^pÈ IP JCCCD JCyÑ½²ñÜvªõ¦çêÄ¢éBgpÂ\È X üÌGlM[Í 8`115

3. ­UdÌ BaTiO3 ÌdêºÅÌª\¢vªkeV ÅM[ X üðp¢é±ÆÉæèCd´qðÜñ¾¨¿Å

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Ìå«¢ñÜwðp¢Äs[NÊuð¸xÇ­²×éÌ
ªà Á Æ àm À ÅéB±Ìr[CÌÁ¥ÌêÂÍCGlé11) B ³ çÉ C X ü Ìg · ð ·­ÁÄàzûÌøÊðÙÚ³µÄ\¢èÂ\È_ÅéBÁÉCGlM[ X üðå^pÈ IP JÆgÝí¹éÆC÷¬»ÅÁÄàv¸xÌ¢f[^ðiGlM[ð¬³­j·é±ÆÉæètóÔðgåµÄL¢tóÔÍÍÅûW·é±ÆªÅ«Cdq§xxÌÏªµC¢óÔªð\Åiqèðè·é±ÆàLø¸§\¢ðÍðs¤±ÆàÂ\Åé13,14)B{¤ÅÍCé12) B{À±ÅÍC¸§»\¢ðÍÌdêºÅÌ«IÉdq§xªzxÅÌªªèðÚwµCåÀ»ðÚwµC±êçÆÍtÌ­zÅGlM[ X ü^pÈ IP JðoíÆµÄIðµ½BdêóÁÌ½

ðp¢½ñÜÀ±ð¢µ½B

ßÌ¿ÉÍ BaTiO3 P»ðTCY 5~2.5~0.1 mm3 ÉÅáGlM[ X üÌ¿§ß\Í¬³­¿\ÊÌî½ÂÉÁHµ½àÌðp¢½B»É_f¹âÁHÉé½ßCoN©çÌñÜ­æécÝÈÇªÜÜêéêCOdêðóÁµ½Æ«Ìxð¾éÉÍGlM[ X üªæè]Üµ¢Æl¦ç

ªÉ½]ªN±èÃç­Èé±ÆªmçêÄ¢é15,16)B±

êéBÀ±ºõ¹ÆµÄæ­p¢çêé CuKa üCMoKa

CÌóCµêðñðµªÉ½]ðeÕÉ·é½ßC1200

üC»µÄ35 keV Ì X üðáÉÆèCBaTiO3 ÌüzûÍCÅ24Ô½Â¿ðAj[µ½B»ÌãC½Âñªæè­²³êéêªW  Æ  ¿ Ì ú ³ ª 0.1 mm Ì ê  Ì X ü Ì § ß ¦ ð¼ Ê É ú Ý 20 nm ö x Ì à d É ð h z µ ½ B SPring­8

Table 1 ÉÜÆß½B35 keV ÌúËõðp¢éÆ§ß¦Í

BL02B1 ÉÄ35 keV ÌúËõðp¢ÄU®Ê^@Éæè

0.8ÉàÈé½ß§ß@ÉæéªèªÂ\ÅC±Ìðºªèµ½ñÜp^[Ìêáð Fig. 4 É¦·B±±É¦·ÅÏª³êéñÜ X üÉÍoNÌîñª\ªÉÜÜêñÜX|bgÍ½Â¿ð§ßµ½ñÜüªL^³ê½àÄ¢éÅë¤B½­ÌñÜwÌ­xðKvÆ·é¸§ÌÅéBñÜpÌ¬³­­xÌå«¢X|bgÍà¿ë\¢ðÍÉÍGlM[ X üª{ü¢Ä¢é½ßC

ñC¼Ôu d0.25 Å Æ¢¤ñÜpÌå«¢X|bgà\±Ì_ÅàLÅªÈvÅªè³êÄ¢é±Æªí©éBéBÜ½C]Ì½­ÌªñÜÀ±ÅÍCÁèÌÂÌñÜs[NÉÚµÄ»ÌÊuâ­xÌÔÏ»ðªèµÄ¢éàÌª½¢ªC{À±ÅÍGlM[ÌúËõ X üðå^ñ³oíÆÆàÉp
¢é±ÆÉæé·ðpµ½BÂÜèCGlM[
X üÉæèñÜ

ðå«­µCæè½­ÌñÜs[NÌÊuð¯Éªè·éBñÜÌgåÉæÁÄpxªð\ª]µÆÈéªC»êðPxÉwü«ÌúËõðgp
·é±ÆÉæÁÄâ¢C½­ÌñÜs[NÊuÆ­xð¯

Table 1

Energy of X­rays, X­ray linear absorption coecient m of
BaTiO3, and transmission ratio I/I0 of X­rays when BaTiO3
plate with thickness l0.1 mm is interposed normally intoa parallel beam of X­rays. I0 and I are the intensities of ini­tial and transmitted X­ray beams, respectively.

Energy of X­rays (keV)

m(BaTiO3) (cm|1)

I/I0

8 (CuKa)

1400

8~10|717 (MoKa)

170

0.18

35

24

0.78

Fig. 4(Color online) Diraction image of BaTiO3 single crystal
recorded on two­dimensional detector Imaging Plate (IP) at
SPring­8 BL02B1 using high­energy SR X­ray of 35 keV (l0.35 Å). The diraction spots in the range of d0.25 Åare clearly observed.

úËõ Sept. 2012 Vol.25 No.5  287

Fig. 5

(Color online) Diraction spots of BaTiO3 recorded on IP
under static external electric eld. At E0, the peak of(440)c from the c­domain and the peak of (044)a from the a­domain are observed in this area. With increasing E, the in­tensity of (044)a decreases. The sample is monodomain at E
4 kV/cm.
Fig. 6ªªèÉæ§¿C\õªèÆµÄÃdêóÁÀ±ðsÁ½Bªè·xÍ BaTiO3 ª³û»nÆÈé300 K ÅéBFig. 5 É(440)X|bgð²«oµ½àÌð¦·Bd
êðóÁµÈ¢óÔÅÍÚßµ½ 2 ÂÌX|bgªÏª³êéB1 ÂÍ©­ªÉûüÅ¿Ì@üûüjÆ½sÅ

é c ²ªdêûüi½Â

é c ªæ©çÌ(440)c X|bgCà¤ 1 ÂÍ c ²ªdêûüÆ¼Å(044)a X|bgÅ

(Color online) Experimental setup for time­resolved single
crystal diraction measurement installed in SPing­8
BL02B1. The SR X­ray is monochromatized to be 35 keV,and the 1667 ms X­ray pulse is generated by an X­ray chop­per. The external electric potential Vext(t) is a bipolar squarewave whose period is 1667 ms. The diraction spots from the
BaTiO3 single crystal plate at each Dt are detected by a large
cylindrical IP camera.

é a ªæ©çÌ

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µÉÎµ¿ÉUN³êé»ÛàJèÔ·±ÆÅéÌ¶Ý·é±Æªí©éBdêðóÁµÄ¢­ÆCdêûü

ÅC»Ìæ¤È V(t) ª¾çêéæ¤É Vext Ìðð²ß

ÉªÉðàÂªæÌªå·é±ÆÉº¢±êçÌ­µÄ¾½àÌª Fig. 7(a)Ì V(t) ÅéBVext Ìüúª t0

éÌÉÎµÄ V(t) à t0 ÌüúðÁÄ

xäªÏ»µCÅIIÉ»SÌªdêûüÉªÉðàÂ1667 mm Å

c ªæÖÆPªæ»·éB¡ñp¢½¿ÅÍC­È­Æ¢éBV(t) Í V(Dt{nt0 )V(Dt) Æ\»Å«CÜ½Càdêð 4 kV/cm ÈãÆ·é±ÆÉæèPªæ»³êé

Vext ªðÏ¦éÆ V(Dt) Ìà½]µ V(Dt{t0 /±Æªí©Á½B±Ìæ¤ÈdêÍRdêÆÄÎêéB

2)|V(Dt) ÌÖWð½µÄ¢éÌÅCV(Dt) Ì«¿

ÉC|v_v[u@Éæé®IP» X üñÜð 0[Dt833 ms ÌÍÍÅ²×êÎÇ¢B±êðgåµ½ûWVXeð\zµ½BTO}ð Fig. 6 É¦·B{ªèàÌª Fig. 7(b)Å

ÅÍCªªèÌ½ßÌ|vÆµÄÌOd³ Vext

IÈdêiFig. 3 Ì¡² E jÉÎ·éBFig. 7(b)Ì I

Ìg`Í600 Hziüú t0 1667 msjÅðÔ·éé`gÆÌÌ æÅÍ ¿SÌªº ü«Ì©­ª ÉðàÁÄ ¢éµ½B±ÌðºÅÍ ms I[_[ÅÏ»·éßn»ÛÌ

iFig. 3 Ì¶ºÉÎjBDt0 Å}É Vext 0 Æ·é±¤¿`103 ms ¢ÅÏ»ª®¹·é»Ûð²×é±ÆªÅÆÉæè¿ÅªÉ½]ªXÉø«N±³êCII Ì

éBV(Dt) Í¿SÌÉ©©éÀø«CãÅq×éªC{¤Åp¢½ BaTiO3 ¿Ì³dU

ÌæÅÍÁÉ}É½]ªN±ÁÄ¢éiFig. 3 Ì P ª P®ÌoÉKµÄ¢éB±Ì Vext ÌUðÃdêóÁ0 ©ç P0 É§¿ãªéªiE0jÉÎjB{ÀÌRdêÌðæèå«­·é±ÆÉæèCBaTiO3 »±Åp¢½¿Æ Vext ÌðºÅÍñ50 ms ÌÔÉªÉ½

ÅÍ|Ps ©ç{Ps C{Ps ©ç|Ps ÖÌªÉ½]ª833]ªN±é±Æªí©éBIII ÌÌæÍªÉ½]ª®¹µms ÉJèÔµUN³êéBÂÜè Fig. 3 Ì¶ºÆEãÉÄSÌªãü«Ì©­ªÉðàÁ½uÔÅCV Í½tl¦·óÔÔÌÚèÏíèªJèÔ³êéBVext Æ¯úµ½ðs«ß¬Äêxå«­ÈèiFig. 3 ÌEãÌ³çÉEÉ

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VI ÌÌæÌèíóÔÆÈéBÌæ III È~ÌU®¬ªÍ±ÅÌÔªð\Í 4 ms Å0 ÉÏíÁ½uÔ©çÌÔ Dt ÅÌÝ X üª¿ÉÆ}ÉOdêðÏ»µ½±ÆÉæÁÄ¶¶½³dU®ÉË³êéæ¤x@\ðp¢Ä`bp[ð§ä·é±ÆæéàÌÅÉæèCCÓÌ Dt ÅÌñÜp^[ð IP ÉL^·éB1ÁÄ¢é½ß½ªæóÔÅéBII ÌÌæÅÍ»ÅªÉ½]ªN±
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ñÌ X üÆËÉæéñÜ­xÍÉßÄ¬³¢ªCé`g

ÉCFig. 7(a)ÅÝ½ I`VI ÌÌæÌ»ê¼êÅÇÌæ

Vext ÌeüúÌe Dt ÉÄ¯lÉ X üð¿ÉÆËµC»¤ÈiqÏ`ªN±é©ð²×é½ßC¢­Â©Ì Dt ÅêçÌ­xðJèÔµ IP ÉL^·é±ÆÉæèðÍÉ\BaTiO3 Ì U ® Ê ^ ð B e µ ½ B e Dt Å ¾ ç ê ½ ñ ÜªÈ­xð¾éBs[NÌ¤¿ d0.4 Å ÌÍÍÌñ600ÂÌs[NÊuðFig. 7(a)É¿Éé`g Vext ðóÁµ½êÌ¿¼[p¢ÄÅ¬ñæ@ÉæéðÍðs¤±ÆÉæè²ä c/a ÌÌdÊ·ÌÔÏ» V(t) ð¦·B|v|v[u^Ì

Dt ÉÎ·éÏ»ð²×½BÊð Fig. 7(c)É¦·BÜ¸C

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gsbNX ¡ ­UdÌ BaTiO3 ÌdêUNiqcÝÌ_Ci~NXFª X üñÜÉæé¤

Fig. 8(Color online) Relationship between c/a and E of BaTiO3 intime­resolved measurement. The tendency is well tted byc/a(c/a)0(1{aE), where (c/a)01.01092}0.00001 anda100}30 pm/V for Dt0`49 ms, at which the sample isin the transient multidomain state, and (c/a)01.01093}
0.00003 and a210}30 pm/V for Dt58`830 ms, at which
the sample is in the monodomain state. Here, a is identical tod33|d13.

¤È½ªæóÔÌ»Éãü«Ì Vext ðóÁ·éÆCåªÌªæÅÍ©­ªÉÆtü«Ì Vext ªóÁ³êÄ¢Fig. 7(Color online) (a) Time dependence of electric voltage V(t)between electrodes of BaTiO3 single crystal plate when a cy­
clic driving electric voltage of bipolar square wave type is ap­
plied. When the direction of Vext changes, V(t) changes
gradually in that direction and shows the behavior of adamped oscillation. The shape of V has a periodicity of 1667
ms, which is the same as that of Vext. Dt is dened as the timein each period. (b) Enlarged V(t) within half period. Thereare characteristic time regions named I to VI. (c)Tetragonality c/a versus Dt plot. (c/a)01.0110 in thesteady state.

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¾ÄÈØÍ¾çêÈ©Á½Bµ½ªÁÄÌæ II Åè³ê½ c/a Í¿SÌÌ½ÏlÆÝÈ·×«ÅéB¼ª

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éÌæ I Æ VI ÅÌlð©ÄÝéBc/aµÄ¢éæ¤Å

éB±êÍ BaTiO3 oNÌ³dU®ðÍ Dt|3 ms ÌÆ« c/a1.01100(3)CDt827 ms ÌÆ

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« c/a1.01098(4)ÅC¼ÒÍë·`10|5 ÌÍÍàÅÌæ¤ÉCBaTiO3 ÉªÉ½]Æ³dU®ªN±éðÅµ¢BÌæ I ÅÍªÉÍºü«CÌæ VI ÅÍªÉÍãü«ÅéÉàWíç¸±êçÌÌæÌiqcÝ eij ªµ¢Æ¢¤±ÌÊÍCeij ª 2 Ke\ÅÌRÌAdêðóÁµ½Æ«CiqcÝªÇÌæ¤ÉÔÏ»·é©ð}CNbI[_[Åo·é±ÆÉ¬÷µ½B

é±Æ©çÅãÉCFig. 8 ÌÊðp¢Ä®i1
jÌ³dè dji

ÅCtÉ¾¦Î eij ªm©É¸xÇ­è³ð©ÏàÁÄÝéBFig. 8 Í c/a ð EE3 ÉÎµÄvbêÄ¢é±ÆÌØ¾Åà
éÅÅ

éB±

éBÉªÉ½]ªN±ÁÄ¢éÌæ II ÌÊðl@·éB±ÌÌæÅÍC

Fig. 5 É¦µ½æ¤È90
ªæóÔð¦´·éX|bgÌªgµ½àÌÅCæÍ½ªæóÔÌÆ«CåÍPªæóÔÌÆ«ÌÊÅ

éBÇ¿çÌêàü`ÉÏ»µÄ¢é

ªCX«ªÙÈéBc/a Íü`ÌÍÍàÅÍ

ôÍÏª³êÈ©Á½Bµ½ªÁÄC{À±ÌðºÅÍªÉ½]Í180ªæð`¬µÈªçN±ÁÄ¢éÆl¦c/a(c/a)0(1{(d33|d31)E )(c/a)0(1{aE)(2)

çêéB±ÌÌæÌ c/a Íí¸©Èªç¸­µ½ãåµÄ¢éBªÉ½]ÌúiKÅÍC»ÌåªÍºüÆ\³êéBic/a)0 Í E0 ÌÆ«Ì c/a Å«Ì©­ªÉðàÁ½ªæÅèßçêCê¾¯ªãü«ÌÆ«Íic/a)01.01092}0.00001Ca100}10 pm/VC

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PªæÌÆ«Íic/a)0 1.01093}0.00003Ca210}10

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úËõ Sept. 2012 Vol.25 No.5  289

pm/V ÅÁ½B½ªæóÔÌ a ÍPªæóÔÌ a ÆärµÄñ 1/2 Å{Mv¤õCØºæ¶C»w¤Ìc¹÷æ

éB±êÍCãü«ÌªÉÆºü«Ì¶CåwÌkC÷mCìûSñæ¶C{Ræ¶ªÉª»É¬ÝµÄ¢é±ÆÉNö·éBµ½ªÁçÆÌ¤¯¤Å·B±Ì¤ÌêÍCSPring­8 pÄCPªæóÔÌÆ«Ì a ª BaTiO3 Ì intrinsic È³dÒwèd_¤i¤ã\ÒFV2009_2011jÌêÂÆ

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gsbNX ¡ ­UdÌ BaTiO3 ÌdêUNiqcÝÌ_Ci~NXFª X üñÜÉæé¤

ÒÐî
XgçÀq

Låwåw@w¤È y³ö
E­mail: moriyosisci.hiroshima­u.ac.jpêåFUdÌ»Ì\¢¨«
mªðn
1997NLåwåw@w¤ÈmÛöãúC¹Bú{wpU»ïÁÊ¤õC
Låw³ðoÄC2009N 1 æè»
EB

âFO

Låwåw@w¤È ³ö
E­mail: kuroiwasci.hiroshima­u.ac.jp
êåF_»¨iåÆµÄ­UdÌâ¼±ÌjðÎÛÆµ½úËõ¸§\¢¨«mªðn
1990 N } g å w H w ¤  È  m Û ö C¹BçtåwèCªRåw³öðoÄC
2005N10æè»EB

Observation of Intrinsic Lattice Strain of
Ferroelectric BaTiO3 during Domain Reversal andPiezoelectric Vibration under Electric Field:Time­Resolved Synchrotron Radiation Single
Crystal Diraction Study
Chikako MORIYOSHI

Department of Physical Science, Graduate School of Science,
Hiroshima University, Higashi­Hiroshima, Hiroshima 739_8526, Japan

Yoshihiro KUROIWA

Department of Physical Science, Graduate School of Science,
Hiroshima University, Higashi­Hiroshima, Hiroshima 739_8526, Japan

Abstract

The dynamic response of an intrinsic lattice strain in a ferroelectric tetragonal BaTiO3 single crys­
tal to an electric eld is successfully observed by using the time­resolved single crystal diraction
measurement. High­energy synchrotron radiation enables us to detect the time dependence of thesmall change in the tetragonality of BaTiO3 during polarization reversal and piezoelectric vibration
after a step like electric eld antiparallel to the spontaneous polarization is applied to the BaTiO3
sample.

úËõ Sept. 2012 Vol.25 No.5  291