An international round-robin calibration protocol for nanoindentation measurements

M. Cabibbo*, P. Ricci, R. Cecchini, Z. Rymuza, J. Sullivan, S. Dub, S. Cohen

*Corresponding author for this work

Research output: Contribution to journalArticle

Abstract

Nanoindentation has become a common technique for measuring the hardness and elastic-plastic properties of materials, including coatings and thin films. In recent years, different nanoindenter instruments have been commercialised and used for this purpose. Each instrument is equipped with its own analysis software for the derivation of the hardness and reduced Young's modulus from the raw data. These data are mostly analysed through the Oliver and Pharr method. In all cases, the calibration of compliance and area function is mandatory. The present work illustrates and describes a calibration procedure and an approach to raw data analysis carried out for six different nanoindentation instruments through several round-robin experiments. Three different indenters were used, Berkovich, cube corner, spherical, and three standardised reference samples were chosen, hard fused quartz, soft polycarbonate, and sapphire. It was clearly shown that the use of these common procedures consistently limited the hardness and reduced the Young's modulus data spread compared to the same measurements performed using instrument-specific procedures. The following recommendations for nanoindentation calibration must be followed: (a) use only sharp indenters, (b) set an upper cut-off value for the penetration depth below which measurements must be considered unreliable, (c) perform nanoindentation measurements with limited thermal drift, (d) ensure that the load-displacement curves are as smooth as possible, (e) perform stiffness measurements specific to each instrument/indenter couple, (f) use Fq and Sa as calibration reference samples for stiffness and area function determination, (g) use a function, rather than a single value, for the stiffness and (h) adopt a unique protocol and software for raw data analysis in order to limit the data spread related to the instruments (i.e. the level of drift or noise, defects of a given probe) and to make the H and E r data intercomparable.

Original languageEnglish
Pages (from-to)215-222
Number of pages8
JournalMicron
Volume43
Issue number2-3
Early online date12 Aug 2011
DOIs
Publication statusPublished - Feb 2012

Fingerprint

Songbirds
Nanoindentation
nanoindentation
Calibration
Hardness
polycarbonate
Elastic Modulus
stiffness
Software
hardness
Stiffness
Quartz
Aluminum Oxide
modulus of elasticity
Elastic moduli
Plastics
Compliance
computer programs
Noise
Hot Temperature

Bibliographical note

© 2012, Elsevier. Licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/

Keywords

  • calibration
  • hardness
  • nanoindentation
  • round-robin
  • Young's modulus

Cite this

Cabibbo, M., Ricci, P., Cecchini, R., Rymuza, Z., Sullivan, J., Dub, S., & Cohen, S. (2012). An international round-robin calibration protocol for nanoindentation measurements. Micron, 43(2-3), 215-222. https://doi.org/10.1016/j.micron.2011.07.016
Cabibbo, M. ; Ricci, P. ; Cecchini, R. ; Rymuza, Z. ; Sullivan, J. ; Dub, S. ; Cohen, S. / An international round-robin calibration protocol for nanoindentation measurements. In: Micron. 2012 ; Vol. 43, No. 2-3. pp. 215-222.
@article{4500f4f7776541d885e98a10b4ad33f5,
title = "An international round-robin calibration protocol for nanoindentation measurements",
abstract = "Nanoindentation has become a common technique for measuring the hardness and elastic-plastic properties of materials, including coatings and thin films. In recent years, different nanoindenter instruments have been commercialised and used for this purpose. Each instrument is equipped with its own analysis software for the derivation of the hardness and reduced Young's modulus from the raw data. These data are mostly analysed through the Oliver and Pharr method. In all cases, the calibration of compliance and area function is mandatory. The present work illustrates and describes a calibration procedure and an approach to raw data analysis carried out for six different nanoindentation instruments through several round-robin experiments. Three different indenters were used, Berkovich, cube corner, spherical, and three standardised reference samples were chosen, hard fused quartz, soft polycarbonate, and sapphire. It was clearly shown that the use of these common procedures consistently limited the hardness and reduced the Young's modulus data spread compared to the same measurements performed using instrument-specific procedures. The following recommendations for nanoindentation calibration must be followed: (a) use only sharp indenters, (b) set an upper cut-off value for the penetration depth below which measurements must be considered unreliable, (c) perform nanoindentation measurements with limited thermal drift, (d) ensure that the load-displacement curves are as smooth as possible, (e) perform stiffness measurements specific to each instrument/indenter couple, (f) use Fq and Sa as calibration reference samples for stiffness and area function determination, (g) use a function, rather than a single value, for the stiffness and (h) adopt a unique protocol and software for raw data analysis in order to limit the data spread related to the instruments (i.e. the level of drift or noise, defects of a given probe) and to make the H and E r data intercomparable.",
keywords = "calibration, hardness, nanoindentation, round-robin, Young's modulus",
author = "M. Cabibbo and P. Ricci and R. Cecchini and Z. Rymuza and J. Sullivan and S. Dub and S. Cohen",
note = "{\circledC} 2012, Elsevier. Licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/",
year = "2012",
month = "2",
doi = "10.1016/j.micron.2011.07.016",
language = "English",
volume = "43",
pages = "215--222",
journal = "Micron",
issn = "0968-4328",
publisher = "Elsevier",
number = "2-3",

}

Cabibbo, M, Ricci, P, Cecchini, R, Rymuza, Z, Sullivan, J, Dub, S & Cohen, S 2012, 'An international round-robin calibration protocol for nanoindentation measurements', Micron, vol. 43, no. 2-3, pp. 215-222. https://doi.org/10.1016/j.micron.2011.07.016

An international round-robin calibration protocol for nanoindentation measurements. / Cabibbo, M.; Ricci, P.; Cecchini, R.; Rymuza, Z.; Sullivan, J.; Dub, S.; Cohen, S.

In: Micron, Vol. 43, No. 2-3, 02.2012, p. 215-222.

Research output: Contribution to journalArticle

TY - JOUR

T1 - An international round-robin calibration protocol for nanoindentation measurements

AU - Cabibbo, M.

AU - Ricci, P.

AU - Cecchini, R.

AU - Rymuza, Z.

AU - Sullivan, J.

AU - Dub, S.

AU - Cohen, S.

N1 - © 2012, Elsevier. Licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/

PY - 2012/2

Y1 - 2012/2

N2 - Nanoindentation has become a common technique for measuring the hardness and elastic-plastic properties of materials, including coatings and thin films. In recent years, different nanoindenter instruments have been commercialised and used for this purpose. Each instrument is equipped with its own analysis software for the derivation of the hardness and reduced Young's modulus from the raw data. These data are mostly analysed through the Oliver and Pharr method. In all cases, the calibration of compliance and area function is mandatory. The present work illustrates and describes a calibration procedure and an approach to raw data analysis carried out for six different nanoindentation instruments through several round-robin experiments. Three different indenters were used, Berkovich, cube corner, spherical, and three standardised reference samples were chosen, hard fused quartz, soft polycarbonate, and sapphire. It was clearly shown that the use of these common procedures consistently limited the hardness and reduced the Young's modulus data spread compared to the same measurements performed using instrument-specific procedures. The following recommendations for nanoindentation calibration must be followed: (a) use only sharp indenters, (b) set an upper cut-off value for the penetration depth below which measurements must be considered unreliable, (c) perform nanoindentation measurements with limited thermal drift, (d) ensure that the load-displacement curves are as smooth as possible, (e) perform stiffness measurements specific to each instrument/indenter couple, (f) use Fq and Sa as calibration reference samples for stiffness and area function determination, (g) use a function, rather than a single value, for the stiffness and (h) adopt a unique protocol and software for raw data analysis in order to limit the data spread related to the instruments (i.e. the level of drift or noise, defects of a given probe) and to make the H and E r data intercomparable.

AB - Nanoindentation has become a common technique for measuring the hardness and elastic-plastic properties of materials, including coatings and thin films. In recent years, different nanoindenter instruments have been commercialised and used for this purpose. Each instrument is equipped with its own analysis software for the derivation of the hardness and reduced Young's modulus from the raw data. These data are mostly analysed through the Oliver and Pharr method. In all cases, the calibration of compliance and area function is mandatory. The present work illustrates and describes a calibration procedure and an approach to raw data analysis carried out for six different nanoindentation instruments through several round-robin experiments. Three different indenters were used, Berkovich, cube corner, spherical, and three standardised reference samples were chosen, hard fused quartz, soft polycarbonate, and sapphire. It was clearly shown that the use of these common procedures consistently limited the hardness and reduced the Young's modulus data spread compared to the same measurements performed using instrument-specific procedures. The following recommendations for nanoindentation calibration must be followed: (a) use only sharp indenters, (b) set an upper cut-off value for the penetration depth below which measurements must be considered unreliable, (c) perform nanoindentation measurements with limited thermal drift, (d) ensure that the load-displacement curves are as smooth as possible, (e) perform stiffness measurements specific to each instrument/indenter couple, (f) use Fq and Sa as calibration reference samples for stiffness and area function determination, (g) use a function, rather than a single value, for the stiffness and (h) adopt a unique protocol and software for raw data analysis in order to limit the data spread related to the instruments (i.e. the level of drift or noise, defects of a given probe) and to make the H and E r data intercomparable.

KW - calibration

KW - hardness

KW - nanoindentation

KW - round-robin

KW - Young's modulus

UR - http://www.scopus.com/inward/record.url?scp=84855230142&partnerID=8YFLogxK

U2 - 10.1016/j.micron.2011.07.016

DO - 10.1016/j.micron.2011.07.016

M3 - Article

AN - SCOPUS:84855230142

VL - 43

SP - 215

EP - 222

JO - Micron

JF - Micron

SN - 0968-4328

IS - 2-3

ER -

Cabibbo M, Ricci P, Cecchini R, Rymuza Z, Sullivan J, Dub S et al. An international round-robin calibration protocol for nanoindentation measurements. Micron. 2012 Feb;43(2-3):215-222. https://doi.org/10.1016/j.micron.2011.07.016