A review on the application of neutron and high-energy X-ray diffraction characterization methods in engineering materials
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摘要: 以先進鋼鐵、高溫合金、鈦合金、鋁合金為代表的工程材料研究，亟待發展先進的原位微結構與應力表征技術，以揭示材料與工程部件在制備與服役過程中晶體結構與多尺度微觀組織／應力場的演化規律，闡明溫度、應力、電、磁等復雜多外場作用下包括形變損傷、相變微觀機制在內的工程材料微觀力學行為。在評述了中子與同步輻射先進原位表征技術的方法原理、裝置發展與各自優勢特點的基礎之上，總結了其在金屬材料形變與相變基礎與應用研究中的新進展及展望。Abstract: As powerful techniques for multidisciplinary research, the neutron and synchrotron radiation sources have the advantages of deep penetration and high brilliance, providing advanced and powerful tools for characterizing microstructures and revealing deformation/damage micromechanisms of materials. For research on engineering materials, such as advanced steel, superalloy, titanium alloy, and aluminum alloy, it is necessary to develop advanced in-situ microstructure and stress characterization methods to reveal the evolution of the multiscale microstructures and stress fields during preparation and service and investigate the micromechanical behaviors, including deformation damage and phase transformation, under complex external factors, such as temperature, stress, electric, and magnetic fields. The basic principles of quantitative characterization of texture and multiscale stress using neutron and X-ray diffraction (XRD) techniques were introduced in this paper. The global development and status of advanced characterization techniques based on neutron and synchrotron radiation sources were expounded. The advantages of neutron and synchrotron radiation techniques were also analyzed. The application of neutron and synchrotron-based XRD techniques in the research of structural engineering materials and components, thermoelastic martensitic transformation, and new structural materials were reviewed. The use of neutron diffraction and HE-XRD techniques on structural engineering materials mainly focuses on multiphase microstructure evolution, intergranular and interphase stress distribution in elastic/plastic zone during deformation, and temperature/stress-induced phase transformation behaviors. The microscopic stress measurement is crucial for verifying the micromechanical model of engineering structural material, which is closely related to the texture evolution during the deformation and phase transformation. The simultaneous acquisition of microscopic stress and macroscopic stress can provide essential data for the service reliability and failure evaluation standards of engineering structural materials/components. Using the μXRD characterization method with submicron resolution, through the combination of monochromatic and polychromatic diffraction analysis, the precise characterization of large stress gradient and slight orientation gradient, caused by the dislocation structures inside the grain, can be realized to achieve submicron damage evaluation. The research on thermoelastic martensitic transformation by neutron scattering (diffraction) and HE-XRD technology includes external field-assisted thermoelastic martensitic transformation, narrow hysteresis thermoelastic martensitic transformation, and colossal elastocaloric effect. Neutron diffraction and HE-XRD techniques have advantages in studying emerging structural materials, such as high-entropy alloys and heterogeneous materials, which often have complex microstructures and exhibit unique mechanical behaviors and are important for revealing their deformation and damage mechanisms. The neutron and synchrotron-based technology, combined with in-situ environmental devices, can be used to measure and analyze the multiscale microstructures/stress and service damage behaviors of key engineering components in a near-service environment. Finally, the development and application of characterization techniques based on neutron and synchrotron radiation sources have prospects.
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Key words:
- neutron diffraction /
- high energy X-ray diffraction /
- deformation /
- phase transformation /
- stress
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圖 2 基于同步輻射源基的先進表征技術. (a) 高能同步輻射衍射; (b) 微束衍射
Figure 2. Advanced characterization techniques based on synchrotron radiation source: (a) high-energy X-ray diffraction; (b) X-ray microdiffraction
圖 3 三維微束衍射技術表征不銹鋼疲勞組織[38]. (a) 實驗示意圖; (b) 以羅德里格斯向量在LD、TD、ND方向分量表示的取向分布圖；(c) 應力分布圖
Figure 3. Characterization of fatigued stainless steel microstructure by 3D μXRD technique[38]: (a) experimental schematic diagram; (b) orientation map in terms of components of the Rodrigues vector along LD, TD, and ND; (c) stress map
Note：qFWHM means the full width at half maximum of diffraction peak；LD?TD?ND is the sample coordinate system and LD is along the tensile loading direction
圖 4 Ti3010合金拉伸力學行為的HE-XRD研究[40]. (a) 應力/硬化率?應變曲線；(b) 不同外加應力下的二維衍射圖
Figure 4. Mechanical behavior and HE-XRD studies of the microstructure for Ti3010 alloy under tension[40]: (a) uniaxial tensile true stress–strain curve with the strain hardening rate of the Ti3010 alloy; (b) 2D HE-XRD patterns at different stresses
圖 5 中子衍射和高能X射線衍射原位實驗研究馬氏體變體去孿晶過程. (a)中子衍射實驗; (b) 高能X射線衍射實驗; (c) 取向相關畸變能
Figure 5. In-situ neutron diffraction and HE-XRD studies on detwinning behavior of martensites: (a) neutron diffraction experiments; (b) HE-XRD experiments; (c) orientation-dependent distortion energy
圖 6 HE-XRD原位實驗研究NiTiNb復合材料[62]. (a) 應力?應變曲線; (b) 高能X射線二維衍射花樣; (c) 不同應力狀態下的一維衍射花樣; (d) 晶格應變?宏觀應變曲線
Figure 6. In-situ HE-XRD study on NiTiNb composite materials : (a) stress–strain curves; (b) 2D HE-XRD patterns; (c) 1D HE-XRD patterns at different stresses; (d) lattice-strain vs macro-strain curves
圖 7 高能X射線衍射原位實驗研究NiCoFeGa單晶纖維[63]. (a) Co10和Co20合金纖維的加卸載力學曲線; (b) Co10和Co20合金纖維拉伸過程中(004)A衍射峰演化; (c) Co20合金纖維不同溫度下的加卸載力學曲線; (d) Co20合金纖維循環加卸載8000周力學曲線; (e) HAADF反傅里葉變換圖像顯示L21相（品紅色）和類ω相（紅色）
Figure 7. In-situ HE-XRD study on NiCoFeGa single crystal fiber: (a) loading-unloading stress-strain curves of Co10 and Co20 fibres; (b) variation in the d-spacing corresponding to the (004)A crystal plane during loading-unloading cycles for Co10 and Co15 fibres; (c) loading–unloading stress–strain curves of Co20 fibres at different temperatures; (d) cyclic loading–unloading stress–strain curves for 8000 cycles; (e) IFFT of the HAADF image showing more distinguishable L21 (magenta ellipses) and ω-like (red ellipses) structures
圖 8 共晶魚骨高熵合金及其HE-XRD原位表征. (a) 定向凝固組織SEM圖; (b) L12和B2相分布（左）及反極圖分布（右）；(c) ~48%拉伸變形后的二維衍射圖；(d) 拉伸過程中的應力配分[66]
Figure 8. Hierarchically arranged herringbone EHEA microstructure and in-situ HE-XRD characterization: (a) SEM backscatter electron image showing that the microstructure is composed of columnar grains; (b) electron backscattering diffraction phase map (left) and inverse pole figure map (right); (c) selected 2D X-ray diffraction images along the full azimuthal angle (0° to 360°) at the tensile strain of ~48%; (d) real-time stress partitioning of B2 and L12 phases during tensile loading
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