Skip to main content Accessibility help

We use cookies to distinguish you from other users and to provide you with a better experience on our websites. Close this message to accept cookies or find out how to manage your cookie settings.

Close cookie message
×
Hostname: page-component-78c5997874-94fs2 Total loading time: 0 Render date: 2024-11-15T19:21:08.178Z Has data issue: false hasContentIssue false

9 - Nanoindentation and Micropillar Compression

Published online by Cambridge University Press:  24 May 2021

T. W. Clyne  and
J. E. Campbell
T. W. Clyne
Affiliation:
University of Cambridge
J. E. Campbell
Affiliation:
Plastometrex, Science Park, Milton Road, Cambridge
Get access

Summary

Mechanical testing on a very fine scale, particularly indentation, has become extremely popular. Sophisticated equipment has been developed, often with accompanying software that facilitates the extraction of properties such as stiffness, hardness and other plasticity parameters. The region being tested can be very small – down to sub-micron dimensions. However, strong caveats should be noted concerning such measurements, particularly relating to plasticity. Some of these concern various potential sources of error, such as the effects of surface roughness, oxide films, uncertainty about the precise geometry of the indenter tip etc. Moreover, even if these can be largely eliminated, extraneous effects tend to arise when (plastically) deforming a small region that is constrained by surrounding (elastic) material. They are often grouped together under the heading of “size effects,” with a clear tendency observed for material to appear harder as the scale of the testing is reduced. Various explanations for this have been put forward, some based on dislocation characteristics, but understanding is incomplete and compensating for them in a systematic way does not appear to be viable. A similar level of uncertainty surrounds the outcome of fine scale uniaxial compression testing, although the conditions, and the sources of error, are rather different from those during nanoindentation. Despite the attractions of these techniques, and the extensive work done with them, they are thus of limited use for the extraction of meaningful mechanical properties (related to plasticity).

Keywords

Nanoindentationsize effectsconstraintmicro-pillar compression.
Type
Chapter
Information
Testing of the Plastic Deformation of Metals , pp. 192 - 218
Publisher: Cambridge University Press
Print publication year: 2021

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Oliver, WC and Pharr, GM, An improved technique for determining hardness and elastic-modulus using load and displacement sensing indentation experiments. Journal of Materials Research, 1992. 7(6): 1564–1583.Google Scholar
Wei, YG, Wang, XZ and Zhao, MH, Size effect measurement and characterization in nanoindentation test. Journal of Materials Research, 2004. 19(1): 208–217.Google Scholar
Fischer-Cripps, AC, Critical review of analysis and interpretation of nanoindentation test data. Surface and Coatings Technology, 2006. 200: 4153–4165.Google Scholar
Golovin, Y, Nanoindentation and mechanical properties of solids in submicrovolumes, thin near-surface layers, and films: a review. Physics of the Solid State, 2008. 50(12): 2205–2236.Google Scholar
Oliver, WC and Pharr, GM, Nanoindentation in materials research: past, present, and future. MRS Bulletin, 2010. 35(11): 897–907.Google Scholar
Morris, JR, Bei, H, Pharr, GM and George, EP, Size effects and stochastic behavior of nanoindentation pop in. Physical Review Letters, 2011. 106(16).CrossRefGoogle ScholarPubMed
Voyiadjis, GZ and Yaghoobi, M, Review of nanoindentation size effect: experiments and atomistic simulation. Crystals, 2017. 7(10).CrossRefGoogle Scholar
Shahbeyk, S, Voyiadjis, GZ, Habibi, V, Astaneh, SH and Yaghoobi, M, Review of size effects during micropillar compression test: experiments and atomistic simulations. Crystals, 2019. 9(11).Google Scholar
Fischer-Cripps, AC, Nanoindentation. Mechanical Engineering Series, Ling, FF, ed. New York: Springer-Verlag, 2004.Google Scholar
Chen, L, ed. Micro-Nanoindentation in Materials Science. ML Books International, 2015.Google Scholar
Tiwari, A and Natarajan, S, eds. Applied Nanoindentation in Advanced Materials. Hoboken, NJ: Wiley, 2017.CrossRefGoogle Scholar
Tsui, T and Volinsky, AA, eds. Small Scale Deformation Using Advanced Nanoindentation Techniques. MDPI, 2019.Google Scholar
Soler, R, Wheeler, JM, Chang, HJ, Segurado, J, Michler, J, Llorca, J and Molina-Aldareguia, JM, Understanding size effects on the strength of single crystals through high-temperature micropillar compression. Acta Materialia, 2014. 81: 50–57.Google Scholar
Bittencourt, E, Interpretation of the size effects in micropillar compression by a strain gradient crystal plasticity theory. International Journal of Plasticity, 2019. 116: 280–296.Google Scholar
Takata, N, Takeyasu, S, Li, HM, Suzuki, A and Kobashi, M, Anomalous size-dependent strength in micropillar compression deformation of commercial-purity aluminum single-crystals. Materials Science and Engineering: A Structural Materials: Properties, Microstructure and Processing, 2020. 772.Google Scholar
Li, WD, Bei, HB, Qu, J and Gao, YF, Effects of machine stiffness on the loading–displacement curve during spherical nano-indentation. Journal of Materials Research, 2013. 28(14): 1903–1911.Google Scholar
Dargenton, JC and Woirgard, J, Description of an electrostatic force nanoindenter. Journal de Physique III, 1996. 6(9): 1247–1260.Google Scholar
Woirgard, J and Dargenton, JC, A new proposal for design of high accuracy nanoindenters. Measurement Science and Technology, 1995. 6(1): 16–21.CrossRefGoogle Scholar
Yu, N, Bonin, WA and Polycarpou, AA, High-resolution capacitive load-displacement transducer and its application in nanoindentation and adhesion force measurements. Review of Scientific Instruments, 2005. 76(4).Google Scholar
Bobji, MS, Ramanujan, CS, Pethica, JB and Inkson, BJ, A miniaturized TEM nanoindenter for studying material deformation in situ. Measurement Science and Technology, 2006. 17(6): 1324–1329.CrossRefGoogle Scholar
Elhebeary, M and Saif, MTA, A micromechanical bending stage for studying mechanical properties of materials using nanoindenter. Journal of Applied Mechanics: Transactions of the ASME, 2015. 82(12).CrossRefGoogle Scholar
Wheeler, JM and Michler, J, Invited article: indenter materials for high temperature nanoindentation. Review of Scientific Instruments, 2013. 84(10): 101301.Google Scholar
Monclus, MA, Lotfian, S and Molina-Aldareguia, JM, Tip shape effect on hot nanoindentation hardness and modulus measurements. International Journal of Precision Engineering and Manufacturing, 2014. 15(8): 1513–1519.Google Scholar
Nohava, J, Randall, NX and Conte, N, Novel ultra nanoindentation method with extremely low thermal drift: principle and experimental results. Journal of Materials Research, 2009. 24(3): 873–882.Google Scholar
Wheeler, JM, Armstrong, DEJ, Heinz, W and Schwaiger, R, High temperature nanoindentation: the state of the art and future challenges. Current Opinion in Solid State & Materials Science, 2015. 19(6): 354–366.CrossRefGoogle Scholar
Chen, J, Bell, GA, Dong, HS, Smith, JF and Beake, BD, A study of low temperature mechanical properties and creep behaviour of polypropylene using a new sub-ambient temperature nanoindentation test platform. Journal of Physics D: Applied Physics, 2010. 43(42).CrossRefGoogle Scholar
Lee, SW, Cheng, YT, Ryu, I and Greer, JR, Cold-temperature deformation of nano-sized tungsten and niobium as revealed by in-situ nano-mechanical experiments. Science China Technological Sciences, 2014. 57(4): 652–662.CrossRefGoogle Scholar
Wheeler, JM, Oliver, RA and Clyne, TW, AFM observation of diamond indenters after oxidation at elevated temperatures. Diamond & Related Materials, 2010. 19: 1348–1353.CrossRefGoogle Scholar
Harris, A, Beake, BD, Armstrong, DEJ and Davies, MI, Development of high temperature nanoindentation methodology and its application in the nanoindentation of polycrystalline tungsten in vacuum to 950˚C. Experimental Mechanics, 2017. 57(7): 1115–1126.Google Scholar
Rzepiejewska-Malyska, KA, Buerki, G, Michler, J, Major, RC, Cyrankowski, E, Asif, SAS and Warren, OL, In situ mechanical observations during nanoindentation inside a high-resolution scanning electron microscope. Journal of Materials Research, 2008. 23(7): 1973–1979.CrossRefGoogle Scholar
Nowak, JD, Rzepiejewska-Malyska, KA, Major, RC, Warren, OL and Michler, J, In-situ nanoindentation in the SEM. Materials Today, 2010. 12: 44–45.CrossRefGoogle Scholar
Warren, OL, Shan, ZW, Asif, SAS, Stach, EA, Morris, JW and Minor, AM, In situ nanoindentation in the TEM. Materials Today, 2007. 10(4): 59–60.Google Scholar
Li, XD and Bhushan, B, A review of nanoindentation continuous stiffness measurement technique and its applications. Materials Characterization, 2002. 48(1): 11–36.Google Scholar
Wang, LG and Rokhlin, SI, Universal scaling functions for continuous stiffness nanoindentation with sharp indenters. International Journal of Solids and Structures, 2005. 42(13): 3807–3832.Google Scholar
Pharr, GM, Strader, JH and Oliver, WC, Critical issues in making small-depth mechanical property measurements by nanoindentation with continuous stiffness measurement. Journal of Materials Research, 2009. 24(3): 653–666.Google Scholar
Bolshakov, A and Pharr, GM, Influences of pileup on the measurement of mechanical properties by load and depth sensing indentation. Journal of Material Research, 1998. 13(4): 1049–1058.Google Scholar
Hay, JC, Bolshakov, A and Pharr, GM, A critical examination of the fundamental relations used in the analysis of nanoindentation data. Journal of Materials Research, 1999. 14(6): 2296–2305.Google Scholar
Nye, JF, Physical Properties of Crystals – Their Representation by Tensors and Matrices. Oxford: Clarendon, 1985.Google Scholar
Kim, SH, Kim, YC, Lee, S and Kim, JY, Evaluation of tensile stress–strain curve of electroplated copper film by characterizing indentation size effect with a single nanoindentation. Metals and Materials International, 2017. 23(1): 76–81.Google Scholar
Chen, X, Ashcroft, IA, Wildman, RD and Tuck, CJ, A combined inverse finite element – elastoplastic modelling method to simulate the size-effect in nanoindentation and characterise materials from the nano to micro-scale. International Journal of Solids and Structures, 2017. 104: 25–34.Google Scholar
Liu, H, Chen, Y, Tang, Y, Wei, S and Nuiu, G, Tensile and indentation creep behaviour of Mg-5%Sn and Mg-5%Sn-2%Di alloys. Materials Science and Engineering A, 2007. 464: 124–128.CrossRefGoogle Scholar
Takagi, H, Dao, M and Fujiwara, M, Analysis on pseudo-steady indentation creep. Acta Mechanica Solida Sinica, 2008. 21: 283–288.Google Scholar
Marques, VMF, Wunderle, B, Johnston, C and Grant, PS, Nanomechanical characterisation of Sn-Ag-Cu/Cu joints – part 2: nanoindentation creep and its relationship with uniaxial creep as a function of temperature. Acta Materialia, 2013. 61(7): 2471–2480.Google Scholar
Geranmayeh, AR and Mahmudi, R, Indentation creep of a cast Mg-6Al-1Zn-0.7Si alloy. Materials Science and Engineering: A Structural Materials: Properties, Microstructure and Processing, 2014. 614: 311–318.CrossRefGoogle Scholar
Chatterjee, A, Srivastava, M, Sharma, G and Chakravartty, JK, Investigations on plastic flow and creep behaviour in nano and ultrafine grain Ni by nanoindentation. Materials Letters, 2014. 130: 29–31.Google Scholar
Wang, Y and Zeng, J, Effects of Mn addition on the microstructure and indentation creep behaviour of the hot dip Zn coating. Materials & Design, 2015. 69: 64–69.CrossRefGoogle Scholar
Mahmudi, R, Shalbafi, M, Karami, M and Geranmayeh, AR, Effect of Li content on the indentation creep characteristics of cast Mg-Li-Zn alloys. Materials & Design, 2015. 75: 184–190.Google Scholar
Ma, Y, GJ Peng, DH Wen, and TH Zhang, Nanoindentation creep behavior in a CoCrFeCuNi high-entropy alloy film with two different structure states. Materials Science and Engineering: A Structural Materials: Properties, Microstructure and Processing, 2015. 621: 111–117.CrossRefGoogle Scholar
Ginder, RS, Nix, WD and Pharr, GM, A simple model for indentation creep. Journal of the Mechanics and Physics of Solids, 2018. 112: 552–562.Google Scholar
Goodall, R and Clyne, TW, A critical appraisal of the extraction of creep parameters from nanoindentation data obtained at room temperature. Acta Materialia, 2006. 54(20): 5489–5499.Google Scholar
Chen, J and Bull, SJ, The investigation of creep of electroplated Sn and Ni-Sn coating on copper at room temperature by nanoindentation. Surface and Coatings Technology, 2009. 203(12): 1609–1617.Google Scholar
Dean, J, Campbell, J, Aldrich-Smith, G and Clyne, TW, A critical assessment of the “stable indenter velocity” method for obtaining the creep stress exponent from indentation data. Acta Materialia, 2014. 80: 56–66.CrossRefGoogle Scholar
Campbell, J, Dean, J and Clyne, TW, Limit case analysis of the “stable indenter velocity” method for obtaining creep stress exponents from constant load indentation tests. Mechanics of Time-dependent Materials, 2016. 1: 31–43.Google Scholar
Nix, WD and Gao, H, Indentation size effects in crystalline materials: a law for strain gradient plasticity. Journal of the Mechanics and Physics of Solids, 1998. 46: 411–425.Google Scholar
Elmustafa, AA and Stone, DS, Nanoindentation and the indentation size effect: kinetics of deformation and strain gradient plasticity. Journal of the Mechanics and Physics of Solids, 2003. 51: 357–381.CrossRefGoogle Scholar
Zhao, MH, Slaughter, WS, Li, M and Mao, SX, Material-length-scale-controlled nanoindentation size effects due to strain-gradient plasticity. Acta Materialia, 2003. 51(15): 4461–4469.Google Scholar
Lee, H, Ko, S, Han, J, Park, H and Hwang, W, Novel analysis for nanoindentation size effect using strain gradient plasticity. Scripta Materialia, 2005. 53(10): 1135–1139.CrossRefGoogle Scholar
Gao, H, Huang, H, Nix, WD and Hutchinson, JW, Mechanism-based strain gradient plasticity – I: theory. Journal of Mechanics and Physics of Solids, 1999. 47: 1239–1263.Google Scholar
Fleck, NA and Hutchinson, JW, A reformulation of strain gradient plasticity. Journal of the Mechanics and Physics of Solids, 2001. 49(10): 2245–2271.Google Scholar
Lorenz, D, Zeckzer, A, Hilpert, U, Grau, P, Johansen, H, and Leipner, HS, Pop-in effect as homogeneous nucleation of dislocations during nanoindentation. Physical Review B, 2003. 67(17).Google Scholar
Shim, S, Bei, H, George, EP and Pharr, GM, A different type of indentation size effect. Scripta Materialia, 2008. 59(10): 1095–1098.CrossRefGoogle Scholar
Barnoush, A, Welsch, MT and Vehoff, H, Correlation between dislocation density and pop-in phenomena in aluminum studied by nanoindentation and electron channeling contrast imaging. Scripta Materialia, 2010. 63(5): 465–468.Google Scholar
Ahn, TH, Oh, CS, Lee, K, George, EP and Han, HN, Relationship between yield point phenomena and the nanoindentation pop-in behavior of steel. Journal of Materials Research, 2012. 27(1): 39–44.CrossRefGoogle Scholar
Chrobak, D, Nordlund, K and Nowak, R, Nondislocation origin of GaAs nanoindentation pop-in event. Physical Review Letters, 2007. 98(4).Google Scholar
Wang, ZG, Bei, H, George, EP and Pharr, GM, Influences of surface preparation on nanoindentation pop-in in single-crystal Mo. Scripta Materialia, 2011. 65(6): 469–472.Google Scholar
Watson, MC and Clyne, TW, The tensioned push-out test for measurement of fibre/matrix interfacial toughness under mixed mode loading. Materials Science and Engineering, 1993. A160: 1–5.Google Scholar
Eldridge, JI and Ebihara, BT, Fiber push-out testing apparatus for elevated temperatures. Journal of Materials Research, 1994. 9(4): 1035–1042.Google Scholar
Kalton, AF, Howard, SJ, Janczak-Rusch, J and Clyne, TW, Measurement of interfacial fracture energy by single fibre push-out testing and its application to the titanium–silicon carbide system. Acta Materiala, 1998. 46: 3175–3189.Google Scholar
Rebillat, F, Lamon, J, Naslain, R, Lara-Curzio, E, Ferber, MK and Besmann, TM, Interfacial bond strength in SiC/C/SiC composite materials, as studied by single-fiber push-out tests. Journal of the American Ceramic Society, 1998. 81(4): 965–978.Google Scholar
Uchic, MD and Dimiduk, DA, A methodology to investigate size scale effects in crystalline plasticity using uniaxial compression testing. Materials Science and Engineering: A Structural Materials: Properties, Microstructure and Processing, 2005. 400: 268–278.Google Scholar
Burek, MJ and Greer, JR, Fabrication and microstructure control of nanoscale mechanical testing specimens via electron beam lithography and electroplating. Nano Letters, 2010. 10(1): 69–76.Google Scholar
Chen, M, Wehrs, J, Michler, J and Wheeler, JM, High-temperature in situ deformation of GaAs micro-pillars: lithography versus FIB machining. JOM, 2016. 68(11): 2761–2767.Google Scholar
Hutsch, J and Lilleodden, ET, The influence of focused-ion beam preparation technique on microcompression investigations: lathe vs. annular milling. Scripta Materialia, 2014. 77: 49–51.Google Scholar
Kiener, D, Motz, C, Rester, M, Jenko, M and Dehm, G, FIB damage of Cu and possible consequences for miniaturized mechanical tests. Materials Science and Engineering: A Structural Materials: Properties, Microstructure and Processing, 2007. 459(1–2): 262–272.Google Scholar
Soler, R, Molina-Aldareguia, JM, Segurado, J, Llorca, J, Merino, RI and Orera, VM, Micropillar compression of LiF 111 Single crystals: effect of size, ion irradiation and misorientation. International Journal of Plasticity, 2012. 36: 50–63.Google Scholar
Uchic, MD, Dimiduk, DM, Florando, JN and Nix, WD, Sample dimensions influence strength and crystal plasticity. Science, 2004. 305(5686): 986–989.Google Scholar

Save book to Kindle

To save this book to your Kindle, first ensure [email protected] is added to your Approved Personal Document E-mail List under your Personal Document Settings on the Manage Your Content and Devices page of your Amazon account. Then enter the ‘name’ part of your Kindle email address below. Find out more about saving to your Kindle.

Note you can select to save to either the @free.kindle.com or @kindle.com variations. ‘@free.kindle.com’ emails are free but can only be saved to your device when it is connected to wi-fi. ‘@kindle.com’ emails can be delivered even when you are not connected to wi-fi, but note that service fees apply.

Find out more about the Kindle Personal Document Service.

Available formats
×

Save book to Dropbox

To save content items to your account, please confirm that you agree to abide by our usage policies. If this is the first time you use this feature, you will be asked to authorise Cambridge Core to connect with your account. Find out more about saving content to Dropbox.

Available formats
×

Save book to Google Drive

To save content items to your account, please confirm that you agree to abide by our usage policies. If this is the first time you use this feature, you will be asked to authorise Cambridge Core to connect with your account. Find out more about saving content to Google Drive.

Available formats
×