Abstract
Depending on the application of nanoparticles, certain characteristics of the product quality such as size, morphology, abrasion resistance, specific surface, and tendency to agglomeration are important. These characteristics are a function of the physicochemical properties of the nanostructured material and, thus, of the process parameters of the particle synthesis. Because of econimical reasons in large-scale production such as pyrolysis or precipitation processes, nanosized particles are produced not as single primary particles but rather as aggregates or agglomerates. The application properties of these aggregates are strongly affected by the micromechanical properties, which can be measured via nanoindentation. In this study, a flat punch method was used. For the measurements, model aggregates out of sol–gel produced silica with varying primary particle size and strength of solid bonds were used. Generally, the micromechanical properties can be characterized by measuring the micromechanical properties via nanoindentation and be described by different theoretical models.
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REFERENCES
J. Winkler: Nanopigmente dispergieren. Farbe und Lack 2, 35 (2006).
C. Schilde, S. Breitung-Faes, and A. Kwade: Dispersing and grinding of alumina nano particles by different stress mechanisms. Ceram. Forum Int. 84, 12 (2007).
K. Kendall and T.P. Weihs: Adhesion of nanoparticles within spray dried agglomerates. Appl. Phys. (Berl.) 25, 3 (1992).
Y. Raichman, M. Kazakevich, E. Rabkin, and Y. Tsur: Inter-nanoparticle bonds in agglomerates studied by nanoindentation. Adv. Mater. 18, 2028 (2006).
M.J. Adams, A. Akram, B.J. Briscoe, C. Lawrence, and D. Parsonage: Nanoindentation of particulate coatings. J. Mater. Res. 14, 2344 (1999).
C.R. Perrey, W.M. Mook, C.B. Carter, and W.W. Gerberich: Characterization of mechanical deformation of nanoscale volumes, in Nanomaterials for Structural Applications, edited by C.C. Berndt, T.E. Fischer, I. Ovid’ko, G. Skandan, and T. Tsakalakos (Mater. Res. Soc. Symp. Proc. 740, Warrendale, PA, 2003), I3.13, p. 87.
W.W. Gerberich, W.M. Mook, M. Cordill, J. Jungk, B. Boyce, T. Friedmann, N. Moody, and D. Yang: Nanoprobing fracture length scales. Adv. Fract. Res. 138, 75 (2006).
W.M. Mook, J.D. Nowak, C.R. Perrey, C.B. Carter, R. Mukherjee, S.L. Girshick, P.H. Mcmurry, and W.W. Gerberich: Compressive stress effects on nanoparticle modulus and fracture. Phys. Rev. B 75, 214112 (2007).
M. Roth, C. Schilde, P. Lellig, A. Kwade, and G.K. Auerhammer: Colloidal aggregates tested via nanoindentation and simultaneous 3D imaging. Stat. Mech. (2011, in press).
W. Stöber, A. Fink, and E. Bohn: Controlled growth of monodisperse silica spheres in the micron size range. J. Colloid Interface Sci. 26, 62 (1968).
C. Gellermann, T. Ballweg, and H. Wolter: Herstellung von funktionalisierten oxidischen Nano- und Mikropartikeln und deren Verwendung. Chemie Ingenieur Technik 79, 233 (2007).
J. Arfsten, C. Bradtmöller, I. Kampen, and A. Kwade: Compressive testing of single yeast cells in liquid environment using a nanoindentation system. J. Mater. Res. 23, 3153 (2008).
S. Antonyuk, J. Tomas, S. Heinrich, and L. Mörl: Breakage behavior of spherical granulates by compression. Chem. Eng. Sci. 60, 4031 (2005).
A. Balakrishnan, P. Pizette, C.L. Martin, S.V. Joshi, and B.P. Saha: Effect of particle size in aggregated and agglomerated ceramic powders. Acta Mater. 58, 802 (2010).
R. Bartali, V. Micheli, A. Gottardi, and N. Laidani: Nanoindentation: Unload-to-load work ratio analysis in amorphous carbon films for mechanical properties. Surf. Coat. Tech. 204, 2073 (2010).
J. Malzbender and G. De Witt: Indentation load-displacement curve, plastic deformation, and energy. J. Mater. Res. 17, 502 (2002).
J. Malzbender and G. De Witt: Energy dissipation, fracture toughness and the indentation load–displacement curve of coated materials. Surf. Coat. Tech. 135, 60 (2000).
S. Antonyuk, S. Palis, and S. Heinrich: Breakage behavior of agglomerates and crystals by static loading and impact. Powder Technol. 206, 88 (2010).
J. Arfsten, I. Kampen, and A. Kwade: Mechanical testing of single yeast cells in liquid environment: Effect of the extracellular osmotic conditions on the failure behavior. Int. J. Mater. Res. 100, 978 (2009).
C. Schilde, T. Gothsch, K. Quarch, M. Kind, and A. Kwade: Effect of important process parameters on the redispersion process and the micromechanical properties of precipitated silica. Chem. Eng. Technol. 32, 1078 (2009).
J. Arfsten: Mikromechanische Charakterisierung von Saccharomyces cerevisiae (TU Braunschweig, Braunschweig, 2009).
W.C. Oliver and G.M. Pharr: An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments. Int. J. Mater. Res. 7, 1564 (1992).
M.F. Doerner and W.D. Nix: A method for interpreting the data from depth-sensing indentation instruments. J. Mater. Res. 1, 601 (1986).
I.N. Sneddon: The relation between load and penetration in the axisymmetric Boussinesq problem for a punch of arbitrary profile. Int. J. Eng. Sci. 3, 47 (1965).
W. Goldsmith: Impact (Edward Arnold, London, 1960).
H. Hertz: Über die Berührung fester elastischer Körper. Journal für die reine und angewandte Mathematik 92, 156 (1881).
Y-T. Cheng and C-M. Cheng: Scaling, dimensional analysis, and indentation measurements. Mater. Sci. Eng., R 44, 91 (2004).
H. Rumpf: Zur Theorie der Zugfestigkeit von Agglomeraten bei Kraftübertragung an Kontaktpunkten. Chemie Ingenieur Technik 42, 538 (1970).
H. Rumpf: Particle adhesion, 2nd Int. Symp. Agglomeration, Atlanta, Conf. Proc., 97, (1977).
D. Bika, G.I. Tardos, S. Panmai, L. Farber, and J. Michaels: Strength and morphology of solid bridges in dry granules of pharmaceutical powders. Powder Technol. 150, 104 (2005).
R.K. Iler: The Chemistry of Silica, New York, 1979).
F.C. Bond: Crushing tests by pressure and impact. Mining technology. Technical Preprint No. 1895, 169, 58 (1946).
W.P.L. Vogel: From single particle impact behavior to modelling of impact mills. Chem. Eng. Sci. 60, 5164 (2005).
C. Schilde, S. Beinert, and A. Kwade: Comparison of the micromechanical aggregate properties of nanostructured aggregates with the stress conditions during stirred media milling. Chem. Eng. Sci. 66, 4943 (2011).
Y-T. Cheng and C.M. Cheng: Relationships between hardness, elastic modulus, and the work of indentation. Appl. Phys. Lett. 73, 614 (1998).
B.R. Lawn and V.R. Howes: Elastic recovery at hardness indentations. J. Mater. Sci. 16, 2745 (1981).
J. Mencik and M.V. Swain: Micro-indentation tests with pointed indenters. Mater. Forum 18, 277 (1994).
ACKNOWLEDGMENTS
The authors gratefully acknowledge the financial support of the German Research Foundation (DFG) within the priority programme (SPP) “colloid technology.” The SEM pictures were kindly taken by the Physikalisch-Technische Bundesanstalt (PTB), Braunschweig. The FIB pictures were kindly taken by Michael Kappl, Max Planck Institute for Polymer Research, Mainz. The Fraunhofer Institut für Silicatforschung, Würzburg, are acknowledged for the supply of the model silica aggregates produced by sol–gel synthesis.
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Schilde, C., Kwade, A. Measurement of the micromechanical properties of nanostructured aggregates via nanoindentation. Journal of Materials Research 27, 672–684 (2012). https://doi.org/10.1557/jmr.2011.440
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DOI: https://doi.org/10.1557/jmr.2011.440