Research progress in methods and applications of experimental mechanics using micro-Raman spectroscopy
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摘要:显微拉曼光谱是近十余年来实验力学领域迅速发展的一种实验应力分析新方法. 相比于大多数的光测力学方法, 显微拉曼能够实现对应力/应变相对直接的表征, 具有高空间分辨、高测试效率、无损非接触等特点, 适合于原位、在线、活体测量. 其对本征和非本征应力均敏感, 并能够开展多物理参量的协同表征, 是当前实验力学领域新方法研究的国际前沿之一, 也是微纳米力学实验分析的重要手段. 本文首先介绍了显微拉曼力学表征的实验原理, 随后论述了拉曼光谱用于力学研究的若干关键技术, 然后综述了基于显微拉曼实验的力学前沿研究进展, 最后讨论了显微拉曼光谱在实验固体力学领域的发展前景与方向. 本文通过对显微拉曼光谱力学实验方法最新理论、技术与应用进展的综述, 为从事微尺度、多尺度力学实验领域的科研工作者提供较为系统的信息参考, 同时为那些对微尺度光谱力学感兴趣的青年科研人员提供本领域系统全面的知识.Abstract:Micro-Raman spectroscopy (MRS) is a recently developed experimental method for stress analysis. It has the characteristics including high spatial resolution, high testing efficiency and collaborative measurement of multiple physical parameters. It is non-destructive and non-contact, and sensitive to both intrinsic and extrinsic stress, which makes MRS suitable for on-line, in-vito and even living experiments. Moreover, compared with most methods of photomechanics, MRS analyzes stress or strain by a relatively direct way. We illustrate the experimental theories of Raman-stress/strain analyses, and discourse upon several kernel techniques of MRS used in mechanical studies. Then, we summarize the research progress, and finally discuss its development prospects and directions, of MRS in solid mechanics and relative fields. We hope that this review provides a systematic reference for the experimental investigation of micro/nano/multi-scale mechanics using MRS, as well as a rapid and comprehensive understanding for young researchers interested in spectral mechanics.
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图 1拉曼光谱力学分析的基本理论框架 (Qiu et al. 2018)
图 2单向应力下背散射拉曼频移−应力关系标定实验. (a)(1 0 0)单晶硅 (de Wolf et al. 1996), (b) 单晶锗 (Gassenq et al. 2016)
图 3(a) 晶体坐标系和样品坐标系示意图, (b) 随机晶面旋转过程示意图 (Qiu et al. 2018)
图 4(a) Kevlar -29纤维施加应力前后拉曼G峰峰位, (b) Kevlar -29纤维的G峰拉曼频移随应力的变化 (Lei et al. 2010)
图 5纤维增强材料四点弯矩形楔口局部应变场 (Qiu et al. 2013). (a) 试件与加载方式, (b) 拉曼扫描区域, (c) 实测εX应变场, (d) 实测εY应变场, (e) 实测γXY应变场
图 6(a) 双层石墨烯2D拉曼峰的分峰分析 (Dou et al. 2018), (b) 全谱形分析用于研究石墨烯电极电化学诱导力学行为 (Song et al. 2022).
图 7(a) 基于角度分辨拉曼的应力信息提取 (1 1 0) 单晶硅面内应力各分量, (b) 拉曼频移的实验结果与拟合曲线 (Ma et al. 2019), (c) 拟合迭代法流程图 (Ma et al. 2021b)
图 8(a) 不同拉伸比下纤维素纳米晶体垂直偏振的角度分辨拉曼峰强度 (Chang et al. 2017), (b) 利用垂直偏振构型下Ag1和Ag2模的角度分辨拉曼峰强度识别黑磷晶向 (Li et al. 2021), (c) 利用无检偏构型下B2g模的角度分辨拉曼峰强度识别黑磷晶向 (Li et al. 2020)
图 9(a) CeO2-δ薄膜拉曼光谱应力分析, 其中左为样品结构示意图, 中为样品的拉曼光谱 (其插图是2110 cm−1左右范围的放大光谱), 右为CeO2-δ晶格因氧空位产生的“化学应变”和外部应力产生的“物理应变”而改变的示意图 (Li et al. 2016); (b) Si衬底Bi2Te3薄膜的拉曼光谱应力分析, 其中左为样品与加载示意图, 右为样品在不同温度下的拉曼光谱 (Huang et al. 2021); (c)蓝宝石衬底分子束外延生长In2Se3薄膜应变的拉曼测量 (Li et al. 2020)
图 10(a) TSV结构1到8横截面的拉曼频移扫描图像, (b) 由(a)中所示扫描图像合并为3D图像 (Kosemura & de Wolf 2015)
图 11(a) 拉曼分析微机电系统中凹槽结构的残余应力场 (Wang et al. 2019), (b) 拉曼测量分析压阻式MEMS力传感器的残余应力场 (Meszmer et al. 2017)
图 12(a) 电极微结构应变测量的原位拉曼实验系统, (b) 多层石墨烯电极在第三次嵌锂和脱锂过程中不同电位下的原位拉曼光谱, (c) 石墨烯电极脱嵌锂过程微结构演化示意图, (d) 不同充放电倍率下石墨烯电极微结构应力演化曲线 (Xie et al. 2019,Song et al. 2019,Song et al. 2022)
图 13(a) 裂纹纤维桥接实验示意图 (Bennett & Young 1998), (b) 平纹织物单元内的纤维应变拉曼Mapping测试示意图 (Lei & Young 2001), (c) 内嵌短纤维拉伸碎断实验示意图 (Young et al. 2001)
图 14拉伸载荷下碳纳米管纤维多尺度结构的承载与变形特性 (Li et al. 2012)
图 15(a) 七个不同长度的石墨烯/PET试件示意图 (不按比例); (b) 实验装置示意图 (显微拉曼系统和石墨烯/PET试件, 不按比例); (c) PET基体的应力−应变曲线; (d) 加载过程中石墨烯中心点处的应变与PET应变的关系曲线, 其中曲线以下阴影区域分别表示黏附 (红色)、滑动 (白色) 和剥离 (蓝色) 阶段 (Xu et al. 2016)
图 16(a) 使用显微拉曼分析三种循环载荷训练后与未循环的石墨烯/PET试件在界面脱粘后界面剪应力沿拉伸轴方向的分布, (b) 循环载荷训练改善界面贴合度的原子尺度和细观尺度示意图 (Du et al. 2018)
图 17使用显微拉曼手段分析双层石墨烯层间切应力. (a) 气泡加载 (Wang G et al. 2017), (b) 基底加载 (Liu et al. 2022)
图 18石墨烯/MoS2/PET异质结构拉伸载荷下的原位拉曼和荧光光谱分析 (Du et al. 2022). (a) 当衬底被拉伸至 2.5% 时异质结构中每一层的应变云图, (b) 633 nm 激光激发拉曼光谱定量表征上层石墨烯的应变, (c) 532 nm 激光荧光光谱定量表征下层MoS2的应变
表 1单晶硅常用晶面在简单应力状态下的应力-频移因子 (Qiu et al. 2018)
晶面 σ(非零) κ(cm−1/GPa) (0 0 1) σ′1 ‒2.298 σ′2 ‒2.298 σ′1=σ′2 ‒4.596 (1 1 0) σ′1 ‒2.587 σ′2 ‒1.712 σ′1=σ′2 ‒4.298 (1 1 1) σ′1 ‒2.531 σ′2 ‒1.597 σ′1=σ′2 ‒4.127 (1 1 −2) σ′1 ‒2.444 σ′2 ‒1.713 σ′1=σ′2 ‒4.154 
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