Critical aspects of nano-indentation technique in application to hardened cement paste

• Published in: Cement and concrete research Vol. 41; no. 1; pp. 20 - 29
• Main Authors: Davydov, D., Jirásek, M., Kopecký, L.
• Format: Journal Article
• Language: English
• Published: Kidlington Elsevier Ltd 01-01-2011; Elsevier
• Subjects: ALKALINE EARTH METAL COMPOUNDS; Applied sciences; ATOMIC FORCE MICROSCOPY; BSE; BUILDING MATERIALS; Buildings. Public works; CALCIUM COMPOUNDS; CALCIUM SILICATES; Calcium-silicate-hydrate (C–S–H) (B); Cement concrete constituents; CEMENTS; COHERENT SCATTERING; DIFFRACTION; Elastic moduli (C); ELECTRON MICROSCOPY; Exact sciences and technology; HYDRATES; IMAGE PROCESSING; MATERIALS; MATERIALS SCIENCE; MECHANICAL PROPERTIES; Mechanical properties (C); Micromechanics (C); MICROSCOPY; Nanomaterials; Nanostructure; OXYGEN COMPOUNDS; Pastes; PENETRATION DEPTH; PROCESSING; Properties and test methods; Properties of anhydrous and hydrated cement, test methods; SCATTERING; SILICATES; SILICON COMPOUNDS; Statistical nanoindentation (B); TRANSMISSION ELECTRON MICROSCOPY; X-RAY DIFFRACTION; Elastic moduli (C); Statistical nanoindentation (B); Mechanical properties (C); Micromechanics (C); Calcium-silicate-hydrate (C–S–H) (B); Elastic modulus; Mechanical properties; Experimental study; Electron microscopy; Indentation; Statistics; Repeatability; Calcium-silicate-hydrate (C-S-H) (B); CSH phase; Hardened cement paste; Penetration; Application
• ISSN: 0008-8846; 1873-3948
• DOI: 10.1016/j.cemconres.2010.09.001

Several open questions related to the experimental protocol and processing of data acquired by the nano-indentation (NI) technique are investigated. The volume fractions of mechanically different phases obtained from statistical NI (SNI) analysis are shown to be different from those obtained by back-scattered electron (BSE) image analysis and X-ray diffraction (XRD) method on the same paste. Judging from transmission electron microscope (TEM) images, the representative volume element of low-density calcium-silicate hydrates (C–S–H) can be considered to be around 500
nm, whereas for high-density C–S–H it is about 100
nm. This raises the question how the appropriate penetration depth for NI experiments should be selected. Changing the maximum load from 1
mN to 5
mN, the effect of penetration depth on the experimental results is studied. As an alternative to the SNI method, a “manual” indentation method is proposed, which combines information from BSE and atomic-force microscopy (AFM), coupled to the NI machine. The AFM allows to precisely indent a high-density C–S–H rim around unhydrated clinkers in cement paste. Yet the results from that technique still show a big scatter.