Low-force AFM nanomechanics with higher-eigenmode contact resonance spectroscopy

Atomic force microscopy (AFM) methods for quantitative measurements of elastic modulus on stiff (>10 GPa) materials typically require tip-sample contact forces in the range from hundreds of nanonewtons to a few micronewtons. Such large forces can cause sample damage and preclude direct measurement of ultrathin films or nanofeatures. Here, we present a contact resonance spectroscopy AFM technique that utilizes a cantilever's higher flexural eigenmodes to enable modulus measurements with contact forces as low as 10 nN, even on stiff materials. Analysis with a simple analytical beam model of spectra for a compliant cantilever's fourth and fifth flexural eigenmodes in contact yielded good agreement with bulk measurements of modulus on glass samples in the 50-75 GPa range. In contrast, corresponding analysis of the conventionally used first and second eigenmode spectra gave poor agreement under the experimental conditions. We used finite element analysis to understand the dynamic contact response of a cantilever with a physically realistic geometry. Compared to lower eigenmodes, the results from higher modes are less affected by model parameters such as lateral stiffness that are either unknown or not considered in the analytical model. Overall, the technique enables local mechanical characterization of materials previously inaccessible to AFM-based nanomechanics methods.

[1]  U. Dürig,et al.  Relations between interaction force and frequency shift in large-amplitude dynamic force microscopy , 1999 .

[2]  Ricardo Garcia,et al.  Calibration of higher eigenmode spring constants of atomic force microscope cantilevers , 2010, Nanotechnology.

[3]  Amelio,et al.  Quantitative determination of contact stiffness using atomic force acoustic microscopy , 2000, Ultrasonics.

[4]  P. Hansma,et al.  Using force modulation to image surface elasticities with the atomic force microscope , 1991 .

[5]  Joseph A. Turner,et al.  Sensitivity of flexural and torsional vibration modes of atomic force microscope cantilevers to surface stiffness variations , 2001 .

[6]  Mechanical Characterization of Thin Films by Use of Atomic Force Acoustic Microscopy , 2011 .

[7]  Bharat Bhushan,et al.  Applied Scanning Probe Methods Xi , 2006 .

[8]  J. Gómez‐Herrero,et al.  Noninvasive protein structural flexibility mapping by bimodal dynamic force microscopy. , 2011, Physical review letters.

[9]  H. Hölscher,et al.  Determination of Tip-Sample Interaction Potentials by Dynamic Force Spectroscopy , 1999 .

[10]  K. Johnson Contact Mechanics: Frontmatter , 1985 .

[11]  H. Butt,et al.  Force measurements with the atomic force microscope: Technique, interpretation and applications , 2005 .

[12]  R. Cook,et al.  Mapping the elastic properties of granular Au films by contact resonance atomic force microscopy , 2008, Nanotechnology.

[13]  Ute Rabe,et al.  Simulation of vibrational resonances of stiff AFM cantilevers by finite element methods , 2009 .

[14]  J. Bechhoefer,et al.  Calibration of atomic‐force microscope tips , 1993 .

[15]  J. Pethica,et al.  Tip Surface Interactions in STM and AFM , 1987 .

[16]  D. Torres-Torres,et al.  Atomic force microscopy cantilever simulation by finite element methods for quantitative atomic force acoustic microscopy measurements , 2006 .

[17]  Ute Rabe,et al.  Vibrations of free and surface‐coupled atomic force microscope cantilevers: Theory and experiment , 1996 .

[18]  Mathias Göken,et al.  Imaging and measurement of local mechanical material properties by atomic force acoustic microscopy , 2002 .

[19]  R. Geiss,et al.  Contact mechanics and tip shape in AFM-based nanomechanical measurements. , 2006, Ultramicroscopy.

[20]  R. Colton,et al.  Measuring the nanomechanical properties and surface forces of materials using an atomic force microscope , 1989 .

[21]  G. Lévêque,et al.  Vibration of the cantilever in Force Modulation Microscopy analysis by a finite element model , 2003 .

[22]  Arvind Raman,et al.  Equivalent point-mass models of continuous atomic force microscope probes , 2007 .

[23]  Jennifer Y. Kelly,et al.  Quantitative subsurface contact resonance force microscopy of model polymer nanocomposites , 2011, Nanotechnology.

[24]  Donna C. Hurley,et al.  Contact Resonance Force Microscopy Techniques for Nanomechanical Measurements , 2008 .

[25]  M. Seah,et al.  Modelling of nanomechanical nanoindentation measurements using an AFM or nanoindenter for compliant layers on stiffer substrates , 2006 .

[26]  Oliver B. Wright,et al.  Vibrational dynamics of force microscopy: Effect of tip dimensions , 1997 .

[27]  Joseph A. Turner,et al.  Analysis of the high-frequency response of atomic force microscope cantilevers , 1997 .

[28]  Siqun Wang,et al.  Nanoscale characterization of natural fibers and their composites using contact-resonance force microscopy , 2010 .

[29]  Robert W. Stark,et al.  Higher harmonics imaging in tapping-mode atomic-force microscopy , 2003 .

[30]  R. Geiss,et al.  Continuous measurement of atomic force microscope tip wear by contact resonance force microscopy. , 2011, Small.