Å-Indentation for non-destructive elastic moduli measurements of supported ultra-hard ultra-thin films and nanostructures
Abstract
During conventional nanoindentation measurements, the indentation depths are usually larger than 1–10 nm, which hinders the ability to study ultra-thin films (<10 nm) and supported atomically thin two-dimensional (2D) materials. Here, we discuss the development of modulated Å-indentation to achieve sub-Å indentations depths during force-indentation measurements while also imaging materials with nanoscale resolution. Modulated nanoindentation (MoNI) was originally invented to measure the radial elasticity of multi-walled nanotubes. Now, by using extremely small amplitude oscillations (<<1 Å) at high frequency, and stiff cantilevers, we show how modulated nano/Å-indentation (MoNI/ÅI) enables non-destructive measurements of the contact stiffness and indentation modulus of ultra-thin ultra-stiff films, including CVD diamond films (~1000 GPa stiffness), as well as the transverse modulus of 2D materials. Our analysis demonstrates that in presence of a standard laboratory noise floor, the signal to noise ratio of MoNI/ÅI implemented with a commercial atomic force microscope (AFM) is such that a dynamic range of 80 dB –– achievable with commercial Lock-in amplifiers –– is sufficient to observe superior indentation curves, having indentation depths as small as 0.3 Å, resolution in indentation <0.05 Å, and in normal load <0.5 nN. Being implemented on a standard AFM, this method has the potential for amore »
- Authors:
- Publication Date:
- Research Org.:
- New York Univ. (NYU), NY (United States)
- Sponsoring Org.:
- USDOE Office of Science (SC)
- OSTI Identifier:
- 1619543
- Alternate Identifier(s):
- OSTI ID: 1613027
- Grant/Contract Number:
- SC0018924
- Resource Type:
- Published Article
- Journal Name:
- Scientific Reports
- Additional Journal Information:
- Journal Name: Scientific Reports Journal Volume: 9 Journal Issue: 1; Journal ID: ISSN 2045-2322
- Publisher:
- Nature Publishing Group
- Country of Publication:
- United Kingdom
- Language:
- English
- Subject:
- 36 MATERIALS SCIENCE; Science & Technology - Other Topics
Citation Formats
Cellini, Filippo, Gao, Yang, and Riedo, Elisa. Å-Indentation for non-destructive elastic moduli measurements of supported ultra-hard ultra-thin films and nanostructures. United Kingdom: N. p., 2019.
Web. doi:10.1038/s41598-019-40636-0.
Cellini, Filippo, Gao, Yang, & Riedo, Elisa. Å-Indentation for non-destructive elastic moduli measurements of supported ultra-hard ultra-thin films and nanostructures. United Kingdom. https://doi.org/10.1038/s41598-019-40636-0
Cellini, Filippo, Gao, Yang, and Riedo, Elisa. Mon .
"Å-Indentation for non-destructive elastic moduli measurements of supported ultra-hard ultra-thin films and nanostructures". United Kingdom. https://doi.org/10.1038/s41598-019-40636-0.
@article{osti_1619543,
title = {Å-Indentation for non-destructive elastic moduli measurements of supported ultra-hard ultra-thin films and nanostructures},
author = {Cellini, Filippo and Gao, Yang and Riedo, Elisa},
abstractNote = {During conventional nanoindentation measurements, the indentation depths are usually larger than 1–10 nm, which hinders the ability to study ultra-thin films (<10 nm) and supported atomically thin two-dimensional (2D) materials. Here, we discuss the development of modulated Å-indentation to achieve sub-Å indentations depths during force-indentation measurements while also imaging materials with nanoscale resolution. Modulated nanoindentation (MoNI) was originally invented to measure the radial elasticity of multi-walled nanotubes. Now, by using extremely small amplitude oscillations (<<1 Å) at high frequency, and stiff cantilevers, we show how modulated nano/Å-indentation (MoNI/ÅI) enables non-destructive measurements of the contact stiffness and indentation modulus of ultra-thin ultra-stiff films, including CVD diamond films (~1000 GPa stiffness), as well as the transverse modulus of 2D materials. Our analysis demonstrates that in presence of a standard laboratory noise floor, the signal to noise ratio of MoNI/ÅI implemented with a commercial atomic force microscope (AFM) is such that a dynamic range of 80 dB –– achievable with commercial Lock-in amplifiers –– is sufficient to observe superior indentation curves, having indentation depths as small as 0.3 Å, resolution in indentation <0.05 Å, and in normal load <0.5 nN. Being implemented on a standard AFM, this method has the potential for a broad applicability.},
doi = {10.1038/s41598-019-40636-0},
journal = {Scientific Reports},
number = 1,
volume = 9,
place = {United Kingdom},
year = {Mon Mar 11 00:00:00 EDT 2019},
month = {Mon Mar 11 00:00:00 EDT 2019}
}
https://doi.org/10.1038/s41598-019-40636-0
Web of Science
Works referenced in this record:
Nanoscale Tunable Reduction of Graphene Oxide for Graphene Electronics
journal, June 2010
- Wei, Z.; Wang, D.; Kim, S.
- Science, Vol. 328, Issue 5984
Elastic coupling between layers in two-dimensional materials
journal, June 2015
- Gao, Yang; Kim, Suenne; Zhou, Si
- Nature Materials, Vol. 14, Issue 7
Nanoindentation Studies Reveal Material Properties of Viruses
journal, March 2009
- Roos, Wouter H.; Wuite, Gijs J. L.
- Advanced Materials, Vol. 21, Issue 10-11
Fast, High Resolution, and Wide Modulus Range Nanomechanical Mapping with Bimodal Tapping Mode
journal, October 2017
- Kocun, Marta; Labuda, Aleksander; Meinhold, Waiman
- ACS Nano, Vol. 11, Issue 10
Water-Dependent Micromechanical and Rheological Properties of Silica Colloidal Crystals Studied by Nanoindentation
journal, January 2012
- Gallego-Gómez, Francisco; Morales-Flórez, Víctor; Blanco, Álvaro
- Nano Letters, Vol. 12, Issue 9
Using force modulation to image surface elasticities with the atomic force microscope
journal, April 1991
- Maivald, P.; Butt, H. J.; Gould, S. A. C.
- Nanotechnology, Vol. 2, Issue 2
Adhesive elastic contacts: JKR and more
journal, July 2008
- Barthel, E.
- Journal of Physics D: Applied Physics, Vol. 41, Issue 16
Method for the calibration of atomic force microscope cantilevers
journal, July 1995
- Sader, John E.; Larson, Ian; Mulvaney, Paul
- Review of Scientific Instruments, Vol. 66, Issue 7
A practical guide for analysis of nanoindentation data
journal, August 2009
- Oyen, Michelle L.; Cook, Robert F.
- Journal of the Mechanical Behavior of Biomedical Materials, Vol. 2, Issue 4
Thermal Transport into Graphene through Nanoscopic Contacts
journal, November 2013
- Menges, Fabian; Riel, Heike; Stemmer, Andreas
- Physical Review Letters, Vol. 111, Issue 20
Nanoscale effects in the characterization of viscoelastic materials with atomic force microscopy: coupling of a quasi-three-dimensional standard linear solid model with in-plane surface interactions
journal, January 2016
- Solares, Santiago D.
- Beilstein Journal of Nanotechnology, Vol. 7
Elastic and plastic properties of thin films on substrates: nanoindentation techniques
journal, August 1997
- D. Nix, William
- Materials Science and Engineering: A, Vol. 234-236
Ultrahard carbon film from epitaxial two-layer graphene
journal, December 2017
- Gao, Yang; Cao, Tengfei; Cellini, Filippo
- Nature Nanotechnology, Vol. 13, Issue 2
Voltage-controlled quantum light from an atomically thin semiconductor
journal, May 2015
- Chakraborty, Chitraleema; Kinnischtzke, Laura; Goodfellow, Kenneth M.
- Nature Nanotechnology, Vol. 10, Issue 6
Calibration of rectangular atomic force microscope cantilevers
journal, October 1999
- Sader, John E.; Chon, James W. M.; Mulvaney, Paul
- Review of Scientific Instruments, Vol. 70, Issue 10
Novel ultra nanoindentation method with extremely low thermal drift: Principle and experimental results
journal, March 2009
- Nohava, J.; Randall, N. X.; Conté, N.
- Journal of Materials Research, Vol. 24, Issue 3
Fast nanomechanical spectroscopy of soft matter
journal, January 2014
- Herruzo, Elena T.; Perrino, Alma P.; Garcia, Ricardo
- Nature Communications, Vol. 5, Issue 1
Uncertainty quantification in nanomechanical measurements using the atomic force microscope
journal, October 2011
- Wagner, Ryan; Moon, Robert; Pratt, Jon
- Nanotechnology, Vol. 22, Issue 45
Hertzian contact of anisotropic bodies
journal, May 1966
- Willis, J. R.
- Journal of the Mechanics and Physics of Solids, Vol. 14, Issue 3
An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments
journal, June 1992
- Oliver, W. C.; Pharr, G. M.
- Journal of Materials Research, Vol. 7, Issue 06, p. 1564-1583
Elastic properties of human cortical and trabecular lamellar bone measured by nanoindentation
journal, October 1997
- Rho, Jae-Young; Tsui, Ting Y.; Pharr, George M.
- Biomaterials, Vol. 18, Issue 20
Atomically thin two-dimensional organic-inorganic hybrid perovskites
journal, September 2015
- Dou, L.; Wong, A. B.; Yu, Y.
- Science, Vol. 349, Issue 6255
A comparison of JKR-based methods to analyze quasi-static and dynamic indentation force curves
journal, June 2006
- Ebenstein, Donna M.; Wahl, Kathryn J.
- Journal of Colloid and Interface Science, Vol. 298, Issue 2
Continuous Stiffness Measurement During Instrumented Indentation Testing
journal, January 2010
- Hay, J.; Agee, P.; Herbert, E.
- Experimental Techniques, Vol. 34, Issue 3
Stochastic noise in atomic force microscopy
journal, September 2012
- Labuda, Aleksander; Lysy, Martin; Paul, William
- Physical Review E, Vol. 86, Issue 3
Development of a precision nanoindentation platform
journal, July 2013
- Nowakowski, B. K.; Smith, D. T.; Smith, S. T.
- Review of Scientific Instruments, Vol. 84, Issue 7
Dynamic nanoindentation by instrumented nanoindentation and force microscopy: a comparative review
journal, January 2013
- Cohen, Sidney R.; Kalfon-Cohen, Estelle
- Beilstein Journal of Nanotechnology, Vol. 4
Viscoelastic Property Mapping with Contact Resonance Force Microscopy
journal, December 2011
- Killgore, J. P.; Yablon, D. G.; Tsou, A. H.
- Langmuir, Vol. 27, Issue 23
A review of nanoindentation continuous stiffness measurement technique and its applications
journal, February 2002
- Li, Xiaodong; Bhushan, Bharat
- Materials Characterization, Vol. 48, Issue 1
Determination of mechanical properties by nanoindentation independently of indentation depth measurement
journal, August 2012
- Guillonneau, Gaylord; Kermouche, Guillaume; Bec, Sandrine
- Journal of Materials Research, Vol. 27, Issue 19
Force measurements with the atomic force microscope: Technique, interpretation and applications
journal, October 2005
- Butt, Hans-Jürgen; Cappella, Brunero; Kappl, Michael
- Surface Science Reports, Vol. 59, Issue 1-6
Epitaxial two-layer graphene under pressure: Diamene stiffer than Diamond
journal, July 2018
- Cellini, Filippo; Lavini, Francesco; Cao, Tengfei
- FlatChem, Vol. 10
A simple predictive model for spherical indentation
journal, February 1993
- Field, J. S.; Swain, M. V.
- Journal of Materials Research, Vol. 8, Issue 2
Elastic Property of Vertically Aligned Nanowires
journal, October 2005
- Song, Jinhui; Wang, Xudong; Riedo, Elisa
- Nano Letters, Vol. 5, Issue 10
Nanoindentation of polymers: an overview
journal, March 2001
- VanLandingham, Mark R.; Villarrubia, John S.; Guthrie, William F.
- Macromolecular Symposia, Vol. 167, Issue 1
Mechanical properties of atomically thin boron nitride and the role of interlayer interactions
journal, June 2017
- Falin, Aleksey; Cai, Qiran; Santos, Elton J. G.
- Nature Communications, Vol. 8, Issue 1
Extraction of Mechanical Properties with Second Harmonic Detection for Dynamic Nanoindentation Testing
journal, October 2011
- Guillonneau, G.; Kermouche, G.; Bec, S.
- Experimental Mechanics, Vol. 52, Issue 7
Plate geometries for contact resonance atomic force microscopy: Modeling, optimization, and verification
journal, July 2018
- Aureli, Matteo; Ahsan, Syed N.; Shihab, Rafiul H.
- Journal of Applied Physics, Vol. 124, Issue 1
Atomic force acoustic microscopy methods to determine thin-film elastic properties
journal, August 2003
- Hurley, D. C.; Shen, K.; Jennett, N. M.
- Journal of Applied Physics, Vol. 94, Issue 4
Comparative study of lithium fluoride and graphite by atomic force microscopy (AFM)
journal, October 1988
- Meyer, E.; Heinzelmann, H.; Grütter, P.
- Journal of Microscopy, Vol. 152, Issue 1
Mechanical behavior of nanocrystalline metals and alloys11The Golden Jubilee Issue—Selected topics in Materials Science and Engineering: Past, Present and Future, edited by S. Suresh
journal, November 2003
- Kumar, K. S.; Van Swygenhoven, H.; Suresh, S.
- Acta Materialia, Vol. 51, Issue 19
Atomically thin p–n junctions with van der Waals heterointerfaces
journal, August 2014
- Lee, Chul-Ho; Lee, Gwan-Hyoung; van der Zande, Arend M.
- Nature Nanotechnology, Vol. 9, Issue 9
A General Equation for Fitting Contact Area and Friction vs Load Measurements
journal, March 1999
- Carpick, Robert W.; Ogletree, D. Frank; Salmeron, Miquel
- Journal of Colloid and Interface Science, Vol. 211, Issue 2
Q-carbon harder than diamond
journal, March 2018
- Narayan, Jagdish; Gupta, Siddharth; Bhaumik, Anagh
- MRS Communications, Vol. 8, Issue 02
Quantitative subsurface contact resonance force microscopy of model polymer nanocomposites
journal, March 2011
- Killgore, Jason P.; Kelly, Jennifer Y.; Stafford, Christopher M.
- Nanotechnology, Vol. 22, Issue 17