様式：論文博士用平成 26 年 6 月 30 日

機能材料工学
申請者

工学専攻

清水一行

氏名

論 文 要 旨
論文題目
(要旨紹介教員小林 正和(博士)

先進材料開発のための放射光 X 線トモグラフィの高度化に関する研究

1,200 字程度)

放射光 X 線トモグラフィは西暦 2000 年頃から急速に発展し，今日ではトモグラフィ画像の空間分解能は物理限界に迫り，金属ミクロ組織の評価が可能な水準となっている．X 線トモグラフィによる材料評価の最大の利点は，三次元（3D）観察を四次元（4D）観察（時間発展挙動の 3D 連続観察）へ拡張可能なことにある．すなわち，熱処理，引張・圧縮および疲労などによって生じる組織変化および変形・損傷挙動を 3D/4D でその場観察できる．本研究では，一連の調査により放射光 X 線トモグラフィがロバストな 3D/4D 定量評価ツールであることを実証した．二次元観察からでは理解が不可能ないしは不十分であった現象を 3D/4D で明瞭に捉え，先進材料開発のために制御すべき因子を提案する．
はじめに，放射光 X 線トモグラフィを組織・構造だけでなく，元素濃度も解析可能なツールとして拡張した．K 吸収端差分イメージングによる 3D/4D 元素濃度マッピングを実現し，材料のミクロ組織評価に活用できる精度および再現性を担持した．熱処理前後でのイメージングにより，Cu 濃度分布の変化を 4D 解析した．教科書的には均質とされる熱処理状態であっても，局所的には Cu 濃度ゆらぎが生じることが明らかとなった．
つぎに，材料の高温変形挙動の解析に放射光 X 線トモグラフィを適用した．これまでは室温に限られていたその場試験を 800K までの高温変形においても適用できるよう拡張し，Al-Mg 合金の高温変形過程をトモグラフィ 4D 観察し，損傷挙動を定量評価した．高温変形において，粒界すべりおよび粒内変形に起因するキャビティより，内在水素ポアを起源とするキャビティの方が材料の損傷に強く影響した．故に内在水素ポアの制御は，室温だけでなく高温においても力学特性の向上が望めることが明らかになった．
つづいて，き裂が導入された Al-Mg-Zn 系実用合金の破壊挙動について破壊力学パラメータを用いて 3D/4D 評価した．き裂先端のひずみ分布は破壊力学で規定されるそれとは大きく異なり，き裂先端前方に形成されるせん断帯内で局在化した．この局在化は，時効状態など従来から知られている要因だけでなく，多結晶組織や結晶方位に大きく影響されることが明らかとなった．
さらに，鉄鋼材料における力学特性の 3D/4D 評価を行った．X 線の線吸収係数の高い鉄鋼材料においても高空間分解能で 3D/4D イメージング可能であることを示し，鋳鉄の疲労き裂進展挙動へ適用した．き裂進展挙動はき裂近傍の黒鉛や介在物と複雑に相互作用し，結果としていびつなき裂前縁形状や加減速の多い不規則なき裂進展を呈した．
また，膨張黒鉛の圧縮・復元挙動の解析にも放射光 X 線トモグラフィを適用した．これにより，従来では切断した断面にてマクロに考察されていた膨張黒鉛の変形挙動をミクロ構造単位で 3D/4D評価した．ワームの屈曲，厚さの変化，および空間分布といったミクロ構造因子とマクロな圧縮・復元挙動を対応付けた．最後に，研究結果を総括し，本論文を結んだ．

year month2014 6
Department Functional Materials Engineering
Supervisor
Name

day30

Masakazu
Kobayashi

Kazuyuki Shimizu
AbstractTitle

Study on sophistication of synchrotron X-ray tomography for advanced materials development（800 words）
Synchrotron X-ray tomography has been rapidly developed in the science and engineering fields since2000. At present, the spatial resolution of tomographic images approaches the physical limit, and themicrostructure of metals can be analyzed. The greatest benefit of material characterization via X-ray
tomography is that 4D imaging (i.e., the continuous 3D imaging of time evolutionary behavior) can beexpanded from 3D imaging, i.e., the structural changes and the deformation/damage behavior caused bythermal processes, tensile and compression stresses, and fatigue can be analyzed in 3D/4D. In this study,
through a series of investigations it has demonstrated that synchrotron X-ray tomography is a robust 3D/4D
characterization technique. Phenomena that are difficult or impossible to understand by conventional 2D
observations are revealed by 3D/4D quantitative analyses. The results of present 3D/4D investigationsuggest that factors should be controlled to enable the development of advanced materials.
First, synchrotron X-ray tomography was expanded to a chemical qualitative elemental analysis
technique, not just a structural analysis technique. 3D/4D elemental concentration mapping was realized byK-edge subtraction imaging, and the accuracy and the repeatability of K-edge subtraction imaging wereevaluated. The changes in the concentration distribution of copper in aluminum alloy before and afterthermal annealing were analyzed in 4D. It is found that the local chemical fluctuation of copper occurred
even though it was in a homogeneous annealed state.
Second, synchrotron X-ray tomography was used to analyze the high-temperature deformation behavior
of aluminum alloys. The high-temperature deformation process of Al-Mg alloys was observed in 4D and
was quantitatively analyzed. High-density hydrogen micropores were observed in the alloys Althoughcontinuous nucleation occurred together with the growth of pre-existing hydrogen micropores, the effects ofthe pre-existing hydrogen micropores, especially those located on grain boundaries, were predominant in
the overall damage evolution. It seemed likely that supersaturated hydrogen in the aluminum alloys mightalso make an appreciable contribution to cavitation during high-temperature loading.
Next, the fracture behavior of pre-cracked Al-Mg-Zn practical alloy was evaluated in 3D/4D on the basisof fracture mechanics parameters. The strain distribution near the crack tip was substantially different fromthe definition of fracture mechanics and was localized in shear bands that formed ahead of the crack tip. Ithas clarified that this strain localization is influenced a great deal by not only generally known aging
conditions but also the polycrystalline structure and crystallographic orientation.
Moreover, 3D/4D mechanical-property evaluations of steel materials were performed. High-resolution
3D/4D imaging was realized for the steel material, which had a high X-ray absorption coefficient and wasapplied to the analysis of the fatigue-crack growth behavior of cast iron. The crack growth behavior of castiron was observed on the graphite near the crack and the inclusion. As a result, a complicated crack frontline and irregular crack growth were observed.
In addition, synchrotron X-ray tomography was used to analyze the compression and recovery behaviorof flexible graphite. Deformation behavior of flexible graphite was assessed in the microscopic 3D/4D
imaging instead of the conventional macroscopic 2D observation of sliced cross-sections. Macroscopic
compression and recovery behavior was characterized on the basis of microstructural factors, such as thebending of worms, changes in thickness, and the spatial distribution of graphite.
Finally, the findings of the present study were summarized and conclusions were reported.