journal article·2021-06-14Open access

Direct determination of the area function for nanoindentation experiments

Christian Saringer, Michael Tkadletz, Markus Kratzer, Megan J. Cordill

Journal of Materials Research· Volume 36· Issue 11

Abstract

Abstract The determination of a suitable correction for tip blunting is crucial in order to obtain useful mechanical properties from nanoindentation experiments. While typically the required area function is acquired from the indentation of a reference material, the direct imaging by suitable methods is an interesting alternative. In this paper, we investigate the applicability of confocal laser scanning microscopy (CLSM), atomic force microscopy (AFM), and self-imaging by scanning a sharp silicon tip using the scanning probe microscopy extension of the nanoindentation system and compare the results to the area function obtained by the indentation of fused silica. The important tip characteristics were determined by various methods based on the analysis of the obtained 3D data sets. It was found that the suitability of CLSM and AFM depend on the resolution and the operation mode, respectively. While for these methods only limited consistency of the determined tip characteristics was found, self-imaging resulted in an excellent overall agreement. Graphic abstract
Source: crossref · Quality: baseline

Research context

OpenAlex topics: Force Microscopy Techniques and Applications · Metal and Thin Film Mechanics · Integrated Circuits and Semiconductor Failure Analysis

SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.

References (33)

Show source-provided references
1. A.C. Fischer-Cripps, Nanoindentation, 2nd edn. (Springer, New York, 2004).10.1007/978-1-4757-5943-3 ↗
2. W.C. Oliver, G.M. Pharr, An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments. J. Mater. Res. 7(6), 1564 (1992)10.1557/JMR.1992.1564 ↗
3. W.C. Oliver, G.M. Pharr, Measurement of hardness and elastic modulus by instrumented indentation: advances in understanding and refinements to methodology. J. Mater. Res. 19(1), 3 (2004)10.1557/jmr.2004.19.1.3 ↗
4. G.M. Pharr, A. Bolshakov, Understanding nanoindentation unloading curves. J. Mater. Res. 17(10), 2660 (2002)10.1557/JMR.2002.0386 ↗
5. J.-S. Park, Y.-H. Lee, Y. Kim, J.-H. Hahn, Prediction of bluntness for pyramidal indenters from nanoindentation curves. Surf. Coat. Technol. 211, 148 (2012)10.1016/j.surfcoat.2011.06.059 ↗
6. J. Čech, P. Haušild, O. Kovářík, A. Materna, Examination of Berkovich indenter tip bluntness. Mater. Des. 109, 347 (2016)10.1016/j.matdes.2016.07.033 ↗
7. M.R. VanLandingham, T.F. Juliano, M.J. Hagon, Measuring tip shape for instrumented indentation using atomic force microscopy. Meas. Sci. Technol. 16(11), 2173 (2005)10.1088/0957-0233/16/11/007 ↗
8. K. Herrmann, N.M. Jennett, W. Wegener, J. Meneve, K. Hasche, R. Seemann, Progress in determination of the area function of indenters used for nanoindentation. Thin Solid Films 377–378, 394 (2000)10.1016/S0040-6090(00)01367-5 ↗
9. J. McMinis, R. Crombez, E. Montalvo, W. Shen, Determination of the cross-sectional area of the indenter in nano-indentation tests. Phys. B 391(1), 118 (2007)10.1016/j.physb.2006.09.006 ↗
10. A.C. Barone, M. Salerno, N. Patra, D. Gastaldi, E. Bertarelli, D. Carnelli, P. Vena, Calibration issues for nanoindentation experiments: direct atomic force microscopy measurements and indirect methods. Microsc. Res. Techniq. 73(10), 996 (2010)10.1002/jemt.20850 ↗
11. G. Aldrach-Smith, N.M. Bennett, U. Hangen, Direct measurement of nanoindentation area function by metrological AFM. Z. Metallkd. 96(11), 1267 (2005)10.3139/146.101173 ↗
12. J.H. Choi, C.S. Korach, Tip bluntness transition measured with atomic force microscopy and the effect on hardness variation with depth in silicon dioxide nanoindentation. Int. J. Precis. Eng. Man. 12(2), 345 (2011)10.1007/s12541-011-0045-4 ↗
13. T. Chudoba, N.M. Jennett, Higher accuracy analysis of instrumented indentation data obtained with pointed indenters. J. Phys. D Appl. Phys. 41(21), 215407 (2008)10.1088/0022-3727/41/21/215407 ↗
14. ISO: Metallic materials—Instrumented Indentation Test for Hardness and Materials Parameters. Geneva, Switzerland, 2015.
15. J.C. Hay, A. Bolshakov, G.M. Pharr, A critical examination of the fundamental relations used in the analysis of nanoindentation data. J. Mater. Res. 14(6), 2296 (1999)10.1557/JMR.1999.0306 ↗
16. W.J. Zong, D. Wu, C.L. He, Radius and angle determination of diamond Berkovich indenter. Measurement 104, 243 (2017)10.1016/j.measurement.2017.03.035 ↗
17. A.S. Useinov, K.S. Kravchuk, A.A. Rusakov, I.V. Krasnogorov, A.P. Kuznetsov, T.V. Kazieva, Indenter shape characterization for the nanoindentation measurement of nanostructured and other types of materials. Phys. Proc. 72, 194 (2015)10.1016/j.phpro.2015.09.060 ↗
18. D.J. Munoz-Paniagua, M.T. McDermott, P.R. Norton, S.M. Tadayyon, Direct tip shape determination of a Berkovich indenter: effect on nanomechanical property measurement and description of a worn indenter. IEEE Trans. Nanotechnol. 9(4), 487 (2010)10.1109/TNANO.2009.2030888 ↗
19. K. Ikezawa, T. Maruyama, Sharp tip geometry and its effect on hardness in nanoindentation experiments. J. Appl. Phys. 91(12), 9689 (2002)10.1063/1.1478794 ↗
20. J. Woirgard, C. Tromas, J.C. Girard, V. Audurier, Study of the mechanical properties of ceramic materials by the nanoindentation technique. J. Eur. Ceram. Soc. 18(15), 2297 (1998)10.1016/S0955-2219(98)00083-1 ↗
21. C.-J. Lu, D.B. Bogy, The effect of tip radius on nano-indentation hardness tests. Int. J. Solids Struct. 32(12), 1759 (1995)10.1016/0020-7683(94)00194-2 ↗
22. A.C. Fischer-Cripps, The sharpness of a Berkovich indenter. J. Mater. Res. 25(5), 927 (2010)10.1557/JMR.2010.0111 ↗
23. F. Zhang, Y. Huang, K.-C. Hwang, The indenter tip radius effect in micro- and nanoindentation hardness experiments. Acta Mech. Sinica 22(1), 1 (2006)10.1007/s10409-005-0084-0 ↗
24. Y. Wang, Effects of indenter angle and friction on the mechanical properties of film materials. Results Phys. 6, 509 (2016)10.1016/j.rinp.2016.08.008 ↗
25. J.S. Villarrubia, Algorithms for scanned probe microscope image simulation, surface reconstruction, and tip estimation. J. Res. Natl. Inst. Standard Technol. 102(4), 425 (1997)10.6028/jres.102.030 ↗
26. S. van der Walt, S.C. Colbert, G. Varoquaux, The NumPy array: a structure for efficient numerical computation. Comput. Sci. Eng. 13(2), 22 (2011)10.1109/MCSE.2011.37 ↗
27. P. Virtanen, R. Gommers, T.E. Oliphant, M. Haberland, T. Reddy, D. Cournapeau, E. Burovski, P. Peterson, W. Weckesser, J. Bright, S.J. van der Walt, M. Brett, J. Wilson, K.J. Millman, N. Mayorov, A.R.J. Nelson, E. Jones, R. Kern, E. Larson, C.J. Carey, İ Polat, Y. Feng, E.W. Moore, J. VanderPlas, D. Laxalde, J. Perktold, R. Cimrman, I. Henriksen, E.A. Quintero, C.R. Harris, A.M. Archibald, A.H. Ribeiro, F. Pedregosa, P. van Mulbregt, SciPy 10: fundamental algorithms for scientific computing in Python. Nat. Methods 17(3), 261 (2020)10.1038/s41592-019-0686-2 ↗
28. W.E. Lorensen, H.E. Cline, Marching cubes: a high resolution 3D surface construction algorithm. Comput. Graphics 21(4), 163 (1987)10.1145/37402.37422 ↗
29. S. van der Walt, J.L. Schönberger, J. Nunez-Iglesias, F. Boulogne, J.D. Warner, N. Yager, E. Gouillart, T. Yu, scikit-image: image processing in Python. PeerJ 2, 453 (2014)10.7717/peerj.453 ↗
30. J.D. Hunter, Matplotlib: A 2D graphics environment. Comput. Sci. Eng. 9(3), 90 (2007)10.1109/MCSE.2007.55 ↗
31. shapely. https://github.com/Toblerity/Shapely. Accessed 27 Aug 2020
32. PyQt5. https://riverbankcomputing.com/software/pyqt. Accessed 27 Aug 2020
33. pyqtgraph. http://www.pyqtgraph.org. Accessed 27 Aug 2020