采用原子力显微镜直接扫描纳米压痕仪针尖法、球面拟合法和熔融石英标准样块的间接测量法对极浅压入下纳米压痕仪的针尖面积函数进行比较分析。实验表明,在极浅压入下,原子力显微镜直接法由于真实地反映了针尖尖端的几何形貌因而获得的面积函数更为准确可靠。建立了相应的数学模型,对于直接法测量中主要的误差,即由于原子力显微镜针尖曲率半径带来的误差进行了分析,结果表明在极小压入深度下压入深度越小,原子力显微镜针尖曲率半径带来的压痕仪针尖面积函数相对误差越大。
Abstract
Three methods were used to calibrate the tip area function of the nanoindenter at super low indentation depth, they are direct method based on atomic force microscope (AFM), spherical surface fitting method and indirect method based on the measurement results of the reference block of fused silica. It was revealed that tip area function calibrated by the direct method is mostly reliable and precise, of which the geometry morphology of the top end of the nanoindenter tip was truly fitted. Moreover, the corresponding mathematical model was established to analysis the main error of the AFM method, which was the error caused by the curvature radius of the AFM tip. The results show, under the super low indentation depth, the relative error of the tip area function of the nanoindentation is increasing with the decrease of indentation depth, which is mainly due to the curvature radius of the AFM tip. The result of the study is meaningful to the nanoindentation measurement of the thin films, of which super low indentation depth is usually required.
关键词
计量学 /
纳米压痕 /
原子力显微镜 /
针尖面积函数 /
校准 /
极浅压入深度
Key words
metrology /
nanoindentation /
atomic force microscope /
tip area function /
calibration /
super low depth
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参考文献
［1］朱瑛,姚英学,周亮. 纳米压痕技术及其试验研究［J］.工具技术,2004,38(8):13-16.
［2］Oliver W C, Pharr G M. An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments［J］. Journal of Materials Research,1992, 7(6):1564-1583.
［3］韩高荣, 王建勋, 杜丕一, 等. 纳米复合薄膜的制备及其应用研究［J］. 材料科学与工程, 1999, 17(4):1-6.
［4］Herrmann K, Jennett N M, Wegener W, et al. Progress in determination of the area function of indenters used for nanoindentation［J］. Thin Solid Films, 2000, 377-378: 394-400.
［5］邓墨林, 高思田, 卢明臻, 等. 纳米力学测量系统的载荷与位移溯源校准方法研究［J］. 计量学报, 2012,33(4): 289-293.
［6］Shimamoto A, Tanaka K, Akiyma Y, et al. Nanoindentation of glass with a tip-truncated Berkovich indenter［J］. Philosohical Magazine A,1996, 74(5):1097-1105.
［7］黎正伟, 陶兴付, 树学峰, 等. 纳米压痕仪的压头面积函数校准方法的比较研究［J］. 计量学报, 2015, 36(4):403-407.
［8］Jiao Y, Scheffer T E. Accurate height and volume measurements on soft samples with the atomic force microscope［J］. Langmuir, 2004, 20(23):10038-10045.
［9］Barone A C, Salerno M, Patra N, et al. Calibration issues for nanoindentation experiments: Direct atomic force microscopy measureents and indirect methods［J］. Microscopy Research and Technique, 2010, 73(10):996-1004.
［10］张泰华. 微/纳米力学测试技术及其应用［M］. 北京:机械工业出版社, 2005:21.
［11］ISO 14577-1:2002. Metallic materials-Instrumented indentation test for hardness and materials parameters-Part 1:Test method ［S］.
［12］龚江宏, 赵喆, 吴建军, 等. 陶瓷材料Vickers硬度的压痕尺寸效应［J］. 硅酸盐学报, 1999, 27(6):693-700.
［13］Rester M, Mota C, Pippan R. Microstructural investigation of the volume beneath nanoindentations in copper［J］. Acta Materialia,2007, 55(19):6427-6435.
［14］Jager I L.Surface free energy-a possible source of error in nanohardness［J］. Surface Science, 2004, 565(2-3):173-179.
［15］杨序纲, 杨潇. 原子力显微术及其应用［M］. 北京:化学工业出版社, 2012:44.
［16］Takagi S, Usuda T, Kongkavitool R. Nanoscale Verification of Hardness Indenters by Atomic Force Microscopy［J］. Journal of Material Testing Research Association of Japan, 2007, 52(3):169-175.
基金
国家科技支撑计划(2011BAK15B07)
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