Identification of Logarithmic-Type Creep of Calcium-Silicate-Hydrates by Means of Nanoindentation Ch. Pichler* and R. Lackner† *Institute for Mechanics of Materials and Structures, Vienna University of Technology, Vienna, Austria † Material-Technology Unit, University of Innsbruck, Technikerstraße 13, 6020 Innsbruck, Austria In order to relate the complex macroscopic behaviour of concrete with finer-scale properties of cement paste, aggregates, porous space, etc. multiscale models are developed. Here, in addition to homogenisation schemes establishing the relation between the properties of the constituents, e.g. matrix and inclusions, and the properties of the composite material, experimental methods for identification of finer-scale properties are required. Recently, the elastic properties of the main clinker phases in ordinary Portland cement (OPC) and calcium-silicate-hydrates (CSH) were identified by nanoindentation (NI). In this paper, the NI technique is extended towards identification of the viscous, time-dependent behaviour of CSH, i.e. the main finer-scale binding phase in OPC-based material systems. Hereby, a logarithmic-type creep behaviour is identified, corresponding perfectly to the creep behaviour encountered for mortars and concrete. ABSTRACT: KEY WORDS: logarithmic creep, nanoindentation, Sneddon solution, Tresca criterion, viscoelastic– cohesive indentation Introduction Objectives of this study Experimental methods for determination of mechanical properties (elasticity, time-dependent behaviour, strength) may be classified according to load history (static or cyclic tests) and the stress distribution induced by loading of the specimen (uniform or non-uniform). Among the experiments for the identification of mechanical properties of concrete characterised by a uniform stress distribution (apart from the domain of load application) are uniaxial, biaxial and triaxial tests. Experiments with non-uniform stress distribution include the Brazilian test, pull-out tests and four-point bending experiments. Indentation tests rank among identification experiments inducing a non-uniform stress distribution. They have been employed in material science for determination of material ‘hardness’ for over a century (Johan A. Brinell presented his ‘Spherical Indentation Test’ at the World Fair in Paris in 1900). As the only prerequisite for indentation tests is a sufficiently plane sample surface, they may be conducted at small length scales of observation. This has led to the development of the so-called nanoinden- tation (NI) technique in the 1980s. Hereby, the applied load ranges in the micro-Newton range and the penetration depth in the nanometre level. An NI test is characterised by driving a tough (usually a diamond-) tip into the ground and polished sample surface, with load history P(t) (N) prescribed and penetration history h(t) (m) being monitored. Loadcontrolled NI tests usually include a loading, a dwelling and an unloading phase (see Figure 1). Based on the so-obtained penetration history data, mechanical properties of the indented material can be computed. In this paper, the NI technique is extended from extraction of elastic and strength (hardness) properties of calcium silicate hydrates (CSH) to the identification of the viscous, timedependent behaviour of CSH. With this information at hand, recently developed multiscale models can be used to predict and optimise the creep and relaxation behaviour of concrete and concrete structures [1–4]. Classical Indentation Analysis – Literature Review Assuming purely elastic unloading, the indentation (plane stress) modulus M ¼ E/(1)m2), with m as Poisson’s ratio and E as Young’s modulus, is determined 2008 The Authors. Journal compilation 2008 Blackwell Publishing Ltd j Strain (2009) 45, 17–25 17 Identification of Logarithmic-Type Creep of CSH : Ch. Pichler and R. Lackner (A) (C) (B) Figure 1: Typical NI-test (single indent) result for OPC paste: (A) load history, (B) penetration history, and (C) load-penetration curve from the initial slope of the load-penetration curve during the unloading phase S ¼ dP/dh|h¼hmax (see Figure 1C) according to the so-called BASh equation (Bulychev–Alekhin–Shoroshorov equation) [5, 6]: pffiffiffiffiffiffi 2 S ¼ pffiffiffi M Ac ; p (1) where Ac is the projected area of contact of the indenter. The projected area of contact for conical tips is given as Ac ¼ ph2c tan2 h; (2) where h is the indenter half angle and hc denotes the contact depth, i.e. the height of the (conical) indenter tip in contact with the sample. Pyramidshaped indenter tips might be represented by a cone such that the cross-sectional area of the pyramidshaped tip and the cone are equal [6]. Accordingly, the three-sided Berkovich tip may be represented by a cone with a half angle of h ¼ 70.32. In order to avoid measuring the projected area of contact, a procedure to determine the contact depth based on the solution of the elastic contact problem was proposed in Ref. [5] as 2 Pmax hc ¼ hmax 2 1 ; S p (3) with Pmax denoting the maximum load acting at the beginning of the unloading phase. As pointed out in Ref. [7], Equation (3) is widely used to estimate the contact depth for elastic–plastic solids. However, Equation (3) may only be applied for (2 · cohesion)/ 18 stiffness ratios of 2c/E > 0.05 in case of a Tresca-type material, when no ‘piling-up’ occurs. Equation (1) was derived using the analytical solution (Sneddon solution) for the contact problem of a rigid indenter penetrating an elastic halfspace, given as [8–10]: P 2 tan h ¼ Eh2 p 1 m2 (4) and hc 2 ¼ : p h (5) Hereby, the radial displacement of points along the surface of contact under the indenter was constrained for the derivation of Equations (4) and (5). Multiplication of the right-hand side of Equation (4) with the correction term b [6] gives access to the so-called ‘modified Sneddon solution’: P 2 tan h ¼b : Eh2 p 1 m2 (6) According to Ref. [6], b depends on Poisson’s ratio m and the indenter half angle h. Results of a parameter study focusing on b as a function of indenter half angle and Poisson’s ratio [4, 11, 12] (see Figure 2) are in good agreement with the numerical results given in Ref. [6]. For a Berkovich indenter characterised by a half angle of h ¼ 70.32 and m ¼ 0.24, b was found to be 1.081. (In Ref. [19], a value of m ¼ 0.24 was suggested for CSH.) Differentiation of Equation (6) with respect to h, specialised for h ¼ hmax, and considering S ¼ dP/dh|h¼hmax and Equations (5) and (2) 2008 The Authors. Journal compilation 2008 Blackwell Publishing Ltd j Strain (2009) 45, 17–25 Ch. Pichler and R. Lackner : Identification of Logarithmic-Type Creep of CSH Figure 2: Correction term b as a function of indenter half angle h and Poisson’s ratio m [4, 11, 12] gives access to the corrected form of the BASh equation as 2 E pffiffiffiffiffiffi Ac S ¼ b pffiffiffi p 1 m2 (7) which is used for determination of the elastic properties of the constituents of cement paste throughout this paper. Utilisation of the NI Technique Towards Identification of Creep and Strength Properties of CSH Experimental programme The test series presented in this paper focus on the extraction of viscoelastic and strength properties of CSH, i.e. the main finer-scale binding phase in hydrated ordinary Portland cement (OPC) paste. The NI tests were performed in grids, with the so-called ‘grid-indentation technique’ [13], giving access to: (i) the spatial distribution and (ii) material properties of the different material phases at the micrometre scale of observation of cement paste. Table 1 summarises all relevant information on the experimental programme presented in this paper. Whereas the first test series (see Table 1) focused on the extraction of Table 1: Experimental parameters for NI-testing of ordinary elastic properties of CSH, the remaining test series were characterised by a vast dwelling phase, hence, aimed at the extraction of viscous material behaviour. Hereby, the influence of the Blaine (grinding) fineness was investigated. All tests presented in this paper were characterised by • the use of well-hydrated samples with an age of approximately 1 year; • a distance between neighbouring grid points of 5 lm for grid indentation; and • the use of a Hysitron TriboIndenter and a Berkovich diamond tip (Hysitron Inc., Minneapolis, MN, USA). Figure 3 shows: (i) the spatial and (ii) the frequency distribution of Young’s modulus E determined using Equation (7) for OPC paste characterised by a Blaine fineness of 4000 cm2 g)1 and a water/cement ratio w/c of 0.5 (see Table 1). Hereby, m in Equation (7) was set to 0.24 [14]. Extraction of strength properties While elastic material properties are determined from the unloading branch of NI tests, strength properties may be deduced from the loading branch, characterised by plastic deformations in the vicinity of the indenter tip. The hardness H (Pa) of the material is determined at the end of the loading phase with the maximum load Pmax and its corresponding projected area of contact as Portland cement paste H¼ No. indents ()) Blaine fineness w/c Load history* (cm2 g)1) ratio ()) (s–s–s/lN) Results given in: 25 · 25 ¼ 525 4000 0.5 5–5–5/500 Figure 3 20 · 20 ¼ 400 3890 0.4 1–100–1/1000 Figures 6B and 7 20 · 20 ¼ 400 3000 0.4 1–100–1/1000 [4] 20 · 20 ¼ 400 4850 0.4 1–100–1/1000 [4] 1 (single indent) 4000 0.5 10–350–10/1000 Figures 1 and 5 *Duration of loading–dwelling–unloading/maximum load. Employed indenter: Hysitron TriboIndenter with a Berkovich tip; age of specimens: 1 year; distance between neighbouring grid points: 5 lm. Pmax : Ac (8) The hardness represents the material response corresponding to the stress state under the indenter tip, characterised by predominant hydrostatic loading. As the tip shape influences the latter, the hardness depends on the indenter tip employed (Berkovich hardness, Vickers hardness, etc.). Hence, H is not a fundamental material property. In order to determine material parameters describing plastic material behaviour, experimental data have to be analysed in combination with analytical/numerical methods. 2008 The Authors. Journal compilation 2008 Blackwell Publishing Ltd j Strain (2009) 45, 17–25 19 Identification of Logarithmic-Type Creep of CSH : Ch. Pichler and R. Lackner Figure 3: Young’s modulus E for material phases encountered in cement paste determined by the corrected form of the BASh equation (Equation 7) (grid-indentation with 25 · 25 indents and distance between adjacent grid points of 5 lm on OPC paste characterised by w/c ¼ 0.5 and a Blaine fineness of 4000 cm2 g)1) 1 In case the material strength is a linear function of the applied hydrostatic pressure, i.e. the material behaviour can be described by, e.g. the Mohr– Coulomb failure criterion, the so-called ‘dualindentation technique’ for identification of cohesion and angle of internal friction was developed in Ref. [15]. This technique is based on the use of two different, but geometrically similar indenter tips, e.g. two conical tips with different half angles. A Berkovich tip and a ‘cube-corner’ tip, characterised by h ¼ 70.32 and h ¼ 42.28, respectively, were used in Ref. [15]. Numerically obtained (employing a limit analysis-based approach) relations for the hardness/cohesion ratio as a function of the angle of internal friction yield two constraints for the determination of the unknown values for the cohesion and the angle of internal friction. 2 For elastoplastic materials obeying the von Mises yield criterion, Tabor [16] postulated a relation between the yield strength fy and the (Brinell) hardness H as: H 2.6/3fy. Recently, this relation was expanded towards conical indentation of strain-hardening materials [7]. In Ref. [7], numerical results are given in the form (H/fy) as a function of (fy/E) for different values of the strainhardening exponent n. 3 In Refs [4, 11, 12], scaling relations for conical viscoelastic–cohesive indentation are derived employing the finite element method. For an elastic–ideally plastic Tresca-type material, given by Young’s modulus E and cohesion c, the scaling function G0(c/E) [4, 11, 12] is given by n h ioc0 ; G0 ðc=EÞ ¼ 1 exp a0 ðc=EÞb0 (9) with a0 ¼ 20.62, b0 ¼ 0.6852 and c0 ¼ 1.360. G0 accounts for the effect of plastic material response on the respective (constant) value of the dimensionless quantity Pp, with Pp ¼ P(t)/[Eh(t)2]. 20 Figure 4: Scaling function G0(c/E) obtained from numerical simulation of conical indentation [4, 11, 12], with Pp ¼ P(t)/[Eh(t)2] and Pep ¼ 2b=p tan h=ð1 m2 Þ (see Equation 6) Thus, G0 ¼ 1 refers to the purely elastic loading situation (see Figure 4). With Young’s modulus at hand [determined according to Equation (7)], the experimental data of the loading phase of the NI test can be plotted in terms of the dimensionless quantity Pp ¼ P(t)/[Eh(t)2] (see Figure 5). These data indicate a progressive switch from spherical to conical indentation. The initial contact of the indenter tip is characterised by spherical indentation because of the small (but ever present) bluntness of the indenter tip. The initially large values for Pp reflect this type of loading situation. With increasing penetration depth, however, the experiment is characterised by conical indentation, with Pp reaching a constant value. The observed horizontal asymptote indicates that, for the employed loading rate of 100 lm s)1 (see Figure 5), the loading phase of the NI test is characterised by mainly elastoplastic material response. Viscoelastic–plastic material response, on the other hand, would have resulted in a monotonically decreasing value for Pp during the loading phase of the NI test [4, 11, 12]. When the value for Pp representing the horizontal asymptote is scaled by the respective value corresponding to the elastic solution, Pp =Pep , with Pep ¼ 2b=p tan h=ð1 m2 Þ [see Equation (6)], the elastoplastic scaling relation G0(c/E) [see Equation 2008 The Authors. Journal compilation 2008 Blackwell Publishing Ltd j Strain (2009) 45, 17–25 Ch. Pichler and R. Lackner : Identification of Logarithmic-Type Creep of CSH Figure 5: Extraction of plastic material properties from loading phase of NI-test data for OPC (9)] gives access to the cohesion/stiffness-ratio c/E of the tested material (see Figure 5) and, thus, to the cohesion c. Based on NI tests on OPC presented in the next section, c/E at the investigated observation scale is in the range 1/100 to 1/200. Remark 1 The cohesion of the Tresca criterion extracted from NI-test data characterises plastic material failure because of predominant hydrostatic loading under the indenter tip. Hence, the so-obtained failure surface may not be used to determine material properties describing material failure under mainly deviatoric loading, such as, e.g. the uniaxial tensile or compressive strength. Identification of logarithmic-type creep properties Whereas the loading branch is characterised by mainly elastoplastic material response and unloading is predominated by elastic behaviour, hence, are used for determination of strength and elastic properties, the viscous material response during the dwelling phase of NI tests may be employed to quantify the creep behaviour of cement-based materials at the micrometre scale. The NI data are characterised by a pronounced increase of the penetration depth during the dwelling phase (see Figure 1C), particularly during the first minute after load application. Recently, analytical solutions for conical indentation of the viscoelastic halfspace characterised by the Maxwell model, the Kelvin–Voigt model and the threeparameter model were derived in Ref. [14]. In Refs [4, 11, 12], this approach is extended towards: 1 a logarithmic-type creep model [17, 18]: according to Ref. [18], the two mechanisms leading to logarithmic creep in crystalline solids are either (i) 2 work hardening: dislocations move forward under the applied stress by overcoming potential barriers, while successively raising the height of the potential barriers or (ii) exhaustion: while neglecting work hardening the barriers to dislocation motion do not have equal activation energies; those with relatively small activation energies are overcome faster than those with relatively large activation energies; if each barrier which is overcome contributes an equal increment of strain, the total strain increases linearly with the increasing activation energy, where the latter is a logarithmic function of time; and the incorporation of plastic deformations modelled by the Tresca criterion, using, similar to the previous section, scaling relations for the viscoelastic–plastic material response. The mentioned logarithmic-type model is characterised by a creep compliance proportional to ln (1 + t/sv), where sv denotes the characteristic time of the creep process. In fact, this model shows the best agreement with the obtained experimental data. Whereas elastic material behaviour is considered for hydrostatic loading, the viscoelastic deviatoric creep compliance function J dev ðtÞ ¼ 1 t þ J v;dev ln 1 þ v;dev l s (10) is employed [4, 12]. Hereby, l ¼ E/2/(1 + m) (Pa) denotes the shear modulus given by the unloading branch of the NI data, and Jv,dev(Pa)1) and sv,dev (s) are the creep compliance parameters to be identified. In case of a step load P(t) ¼ H(t)Pmax applied during the loading phase onto a conical indenter, where H(t) denotes the Heaviside step function, the deviatoric creep law (Equation 10) gives the penetration history for the dwelling phase as [4, 12] 2008 The Authors. Journal compilation 2008 Blackwell Publishing Ltd j Strain (2009) 45, 17–25 21 Identification of Logarithmic-Type Creep of CSH : Ch. Pichler and R. Lackner HðtÞPmax p 1 m2 h2 ðtÞ ¼ 2 tan h E b 1 t þ sv;dev v;dev : 1þb ln v;dev lJ 2ð1 mÞ s An experimental study was conducted in order to identify the influence of the Blaine fineness / on the finer-scale creep properties (see Table 1). Hereby, the three test series were characterised by / ¼ 3000, 3890 and 4850 cm2 g)1, respectively, w/c ¼ 0.4, and a relative humidity in the test chamber of hexp ¼ 50%. The result for / ¼ 3890 cm2 g)1 is shown in Figure 7. The grid indentation, with 20 · 20 ¼ 400 indents for each grid, gives access to the spatial distribution of mechanical properties. Hereby, the specimen with / ¼ 3000 cm2 g)1 is characterised by a coarser microstructure with some anhydrous clinker grains, the specimens with / ¼ 3890 and 4850 cm2 g)1 by a finer and more homogeneous microstructure. Whereas the frequency distributions for Young’s modulus E show two (or three) maxima in the range 15–35 GPa, corresponding to different types of CSH [19] [low-density (LD) and high-density (HD) CSH] and portlandite, the frequency distributions of v;dev 1=JCSH are characterised by one pronounced peak. Hereby, this peak value amounts to 22.5 GPa for / ¼ 3000 cm2 g)1, 27.5 GPa for / ¼ 3890 cm2 g)1, and 32.5 GPa for / ¼ 4850 cm2 g)1 [4]. The corresv;dev are 0.044, 0.036 and ponding values for JCSH )1 0.031 GPa [4]. (11) In order to account for the plastic deformations during the loading phase, the analytical solution (Equation 11) is scaled by [G0 + glog(1)G0)])1, i.e. HðtÞPmax p 1 m2 h2 ðtÞ ¼ 2 tan h E b 1 t þ sv;dev 1þb lJ v;dev ln v;dev 2ð1 mÞ s 1 G0 þ glog ð1 G0 Þ ; (12) where G0(c/E) denotes the elastoplastic scaling relation already used in the previous section (see Figure 5) and glog(m,c/E, Jv,dev, sv,dev) is an interpolation function, which accomplishes the transition between elastoplastic (short-term) response and viscoelastic (long-term) response (see Figure 6A; [4, 12]). The unknown deviatoric creep parameters Jv,dev and sv,dev are determined employing a least-square fitting method. Hereby, the error between the measured penetration history in the dwelling phase, h2exp ðtÞ, and h2(t,Jv,dev,sv,dev) for a step load according to Equation (12) is minimised: X 2 ½hexp ðtn Þ h2 ðtn ; J v;dev ; sv;dev Þ2 ; R J v;dev ; sv;dev ¼ Remark 2 The reasonable duration of the dwelling phase of an NI test is limited by the so-called machine drift of the NI-testing rig, h_ rig . This drift is mainly caused by creep of the three-axis piezo-scanner [20], which is part of the measuring head holding the indenter tip [whereas a capacitive transducer is employed for load application, a three-axis piezo-scanner is adopted for 3D imaging of the sample surface, as well as for the (final) approach of the indenter tip to the sample surface before NI testing]. It is determined prior to the actual NI test by putting the indenter tip on the sample surface, applying a small force, e.g. 2 lN and recording the deformation rate – ideally until a steady state is reached. n (13) where n denotes the number of data points of the dwelling phase considered in the minimisation scheme. Figure 6B shows the distribution of R obtained for one indent on OPC as a function of the unknown model parameters Jv,dev and sv,dev, indicating a clear (global) minimum. Thus, the proposed parameter-identification scheme leads to a unique solution for Jv,dev and sv,dev for the respective indent. The steps necessary for the identification of the creepcompliance parameters are summarised in Box 1. (A) (B) Figure 6: (A) Interpolation function glog(m,c/E,Jv,dev,sv,dev) for different values of Pl ¼ lJv,dev, v ¼ 0.24, and Pc ¼ c/E ¼ 1/100 [4, 12]; (B) distribution of R as a function of Jv,dev and sv,dev (see Equation 13) showing uniqueness of the solution obtained by the proposed parameter-identification scheme 22 2008 The Authors. Journal compilation 2008 Blackwell Publishing Ltd j Strain (2009) 45, 17–25 Ch. Pichler and R. Lackner : Identification of Logarithmic-Type Creep of CSH Box 1: Identification of creep-compliance parameters by nanoindentation 1. Determination of Young’s modulus E from the initial slope of the load-penetration curve during the unloading phase according to Equation (7) 2. Calculation of cohesion c based on the scaling function G0(c/E) (see Equation 9) and the measured dimensionless quantity Pp ¼ P(t)/Eh(t)2] at the end of the loading phase 3. Identification of creep parameters by backcalculation of the penetration history during the dwelling phase of the indentation test (see Equation 12) (A) (B) (C) Figure 7: (A) Young’s modulus E according to Equation (7); creep parameters (B) Jv,dev and (C) sv,dev obtained from backcalculation of the dwelling phase (grid indentation with 20 · 20 indents and distance between adjacent grid points of 5 lm on OPC paste characterised by w/c ¼ 0.4 and a Blaine fineness of 3890 cm2 g)1) However, for materials with low viscosity (i.e. high compliance), the compliance of the indented specimen may spuriously be interpreted as machine drift when employing the mentioned procedure. During the NI tests presented in this paper, jh_ rig j ranged from 0.01 to 0.1 nm s)1. Once jh_ rig j is in the range of the penetration rate, the test data lose their relevance. For the tested OPC pastes and the employed NI-testing equipment, a reasonable duration of the dwelling phase was found to be around 2–3 min. On the other hand, the average value of the penetration rate at the beginning of the dwelling phase was approximately 30 nm s)1 for the NI tests conducted, which is significantly larger than the jh_ rig j encountered. Another source of measuring errors is the so-called thermal drift. It is associated with thermal dilation of test rig and specimen. The thermal-drift error can be minimised by: (i) setting up the NI test rig in a temperature-controlled environment and (ii) storing 2008 The Authors. Journal compilation 2008 Blackwell Publishing Ltd j Strain (2009) 45, 17–25 23 Identification of Logarithmic-Type Creep of CSH : Ch. Pichler and R. Lackner the specimen in the test rig (which is hooded) prior to testing. Remark 3 Viscous material response influences the unloading slope and, thus the determination of elastic properties [7]. This effect can even cause ‘outbulging’ in the load-penetration diagram, characterised by increasing penetration depth for decreasing loading of the indenter tip. Two measures minimise the described deviation from purely elastic unloading: (i) a sufficiently long dwelling phase: when the creep response subsides, i.e. the creep potential is consumed to a great part, unloading is not influenced either (ii) fast unloading: for the theoretical situation of infinitely fast unloading, only elastic material response occurs. The two measures are also visible when deriving a criterion for a suitable duration of the unloading time, su, in order to exclude viscoelastic behaviour during the unloading branch [14]. For a finite unloading period following a step load, this criterion reads for the logarithmic-type model [4] su 2ð1 mÞ ðtu þ sv;dev Þ; blJ v;dev (14) with tu denoting the time instant at the beginning of the unloading phase. Hence, for the load history considered in the NI tests performed, characterised by a duration of the dwelling phase of 100 s, and l ¼ E/[2(1 + m)] ¼ 20/[2(1 + 0.24)] ¼ 8 GPa, su ¼ 1 s>2 (1)0.24)(101 + 0.1)/(1.081Æ8Æ0.037) ¼ 480 s, thus satisfying condition (14). Concluding Remarks In this paper, elastic, strength, and, finally, viscous properties of cement paste at the micrometre scale were determined by means of NI. The material parameters obtained serve as input for the recently developed multiscale model for upscaling of viscoelastic properties [3, 4], autogenous shrinkage deformations [2, 4], and strength properties [21, 22] of early-age cement-based materials. Whereas the elastic properties of the constituents of OPC paste at finer scales of observation were similar to recently published values in the open literature [13, 19, 23, 24], a logarithmic-type creep behaviour was identified during NI creep tests. Interestingly, this type of creep behaviour is also observed at the macroscale, i.e. is immanent to the scale of observation. Recently, the origin of these viscous deformations was explained by the rearrangement (dislocation) of CSH globules 24 under shear stresses [25]. [In Ref. [25] CSH is described as an aggregation of precipitated, colloidsized particles with the ‘basic building blocks’ (radius of 1.1 nm) aggregating into ‘spherical globules’ (radius of 2.8 nm). The latter aggregate further into: (i) LD CSH or (ii) HD CSH, depending on w/c ratio, age and environmental conditions]. According to Ref. [18], dislocation-based mechanisms lead to logarithmic-type creep behaviour. In order to analyse the obtained NI data, analytical solutions for conical indentation with viscoelastic–plastic material response, constructed in dimensionless form by means of the finite element (FE) method, were employed [4, 11, 12]. The scaling relations derived in Ref. [4, 12] provide the mean to identify logarithmictype creep behaviour and to backcalculate the respective model parameters. ACKNOWLEDGEMENTS The authors thank Franz-Josef Ulm, Georgios Constantinides and Matthieu Vandamme for fruitful discussions and helpful comments during and after their stay at the CEE department at MIT. The authors further thank Erwin Schön, Rupert Friedle and Gernot Tritthart (LAFARGE CTEC, Mannersdorf) for providing the cements employed in the experimental study, and Andreas Jäger for conducting the nanoindentation tests included in this paper. Financial support granted by the Austrian Science Fund (FWF) via project P15912-N07 is appreciated. REFERENCES 1. Bernard, O., Ulm, F.-J. and Lemarchand, E. (2003) A multiscale micromechanics–hydration model for the early-age elastic properties of cement-based materials. Cement Concrete Res. 33, 1293–1309. 2. Pichler, Ch., Lackner, R. and Mang, H. A. 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