A novel methodology to determine the mechanical properties of amorphous materials through! instrumented nanoindentation!! M. Rodríguez, J. M.

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1 A novel methodology to determine the mechanical properties of amorphous materials through instrumented nanoindentation M. Rodríguez, J. M. Molina-Aldareguía, C. González, J. LLorca Polytechnic University of Madrid & IMDEA Materials Institute Madrid, Spain 2012 MRS Fall Meeting Boston, November 25th-30th, 2012

2 SUMMARY 1. INTRODUCTION - Motivation - Objectives 2. METHODOLOGY - Background of indentation test - Main assumptions 3. NUMERICAL SIMULATIONS - Finite element model - Validation of assumptions 4. INSTRUMENTED INDENTATION AS A CHARACTERIZATION TECHNIQUE 5. APPLICATION 6. CONCLUSIONS

3 MECHANICAL BEHAVIOR of AMORPHOUS SOLIDS Introduction Mechanical behavior of amorphous solids (ceramic glasses, metallic glasses and thermoset/thermoplastic polymers) presents a number of similar features: Brittle in tension Ductile in compression/shear by the propagation of shear bands Yield strength is pressure-sensitive Limited strain hardening yc t Determination of the mechanical properties by standard tests is sometimes difficult (brittle behavior in tension). Instrumented nanoindentation emerges as an alternative with the additional advantage of in situ testing.

4 MECHANICAL BEHAVIOR of AMORPHOUS SOLIDS Introduction Mechanical behavior of amorphous solids is well represented by the Drucker-Prager model (rate effects are neglected): Drucker-Prager yield surface = p 3J 2 d + I 1 tan =0 3 I 1 = 0 ii ij = ij I 1 /3 J 2 = ij 0 ji yc t = 1 + tan Mechanical properties of amorphous solids are determined by: (rate effects are neglected): Cohesion: Friction angle: Elastic constants: d E, Can they be obtained from instrumented indentation tests?

5 INSTRUMENTED INDENTATION TEST methodology Four parameters: P max,h max,s,w p /(W e + W p ) but only two are independent... c p Uncertainty in the contact area H ap = P q max c A p = A/A ap ap is given by analytical expressions (Oliver & Pharr, 1992) This information is used to compute the hardness and the elastic modulus H = P max A E = Sp 2 p A 1 E = 1 2 E i E i

6 INVERSE PROBLEM methodology The inverse problem (determination of yield stress from hardness) is not trivial in general because different combinations of material properties (yield stress, pressure sensitivity, strain hardening) may lead to the same hardness. Known results: Von Mises solid H yc yc = f E f 3 in the fully-plastic regime Drucker-Prager solid: H yc yc = f E, Main assumption: yc and are replaced by a characteristic indentation stress r H r r = d h tan = d ah tan = f r E yc = r + ah tan 1 tan /2 The validity of this assumption and the value of the constant a can be obtained from the finite element simulation of the indentation test in a Drucker-Prager solid

7 FINITE ELEMENT MODEL numerical simulations Axisymmetric model, large deformations. Elasto-plastic Drucker-Prager material. Rigid conical indenter equivalent to a Berkovich tip (θ = 70.30º). Frictionless indenter/material contact. Discretization with first order elements with full integration (CAX4). Mesh refined at the contact area with the tip (40 nodes in contact). Simulations carried out with Abaqus/ Standard. In cases of excessive distortion, simulations were carried out with Abaqus/explicit and arbitrary Lagrangian Eulerian mesh adaptivity.

8 NUMERICAL RESULTS numerical simulations Elasto-plastic regime yc/e =0.02 H yc yc = f E,? H r = f r E

9 NUMERICAL RESULTS numerical simulations H r = f r E r = d 0.29H tan

10 NUMERICAL RESULTS numerical simulations W e /W t is closely related to r/e

11 INVERSE PROBLEM Determination of E, ycand from instrumented indentation: characterization by indentation H ap,s,w e /W t W t = W e + W p H ap = P max A ap

12 MASTER CURVES characterization by indentation Master curves are built as a function of parameters readily measurable and incorporate the effect of the pile-up The master curves allow to determine σyc from the indentation data when β is known and viceversa In addition, it is possible to determine β from the independent measurement of the real contact area Ac if We/Wt < 0.5

13 MATERIALS experimental validation Bulk metallic glasses: Zr65Cu15Al10Ni10, Mg58.5Cu30.5Y11 and Mg61 Cu28Gd11 Ceramic glasses: Soda-lime glass (Starphire ) and borosilicate glass (Borofloat ) Glassy polymers: epoxy, PMMA and PVD Wide range of σyc/e and β EXPERIMENTAL TECHNIQUES Experiments conducted using a Nanoindenter XP At least 10 indentations in each material with Berkovich tip at a strain rate s -1 Residual imprints measured by AFM using a Park XE150

14 Analysis Strategy W e /W t 0.31 No prior knowledge of σ yc or β available Bulk Metallic Glasses Measurement of Residual Imprint by AFM experimental validation A ap A c c p W e /W t β W e /W t, H ap σ yc Analysis Strategy Ceramic Glasses W e /W t in the range Oliver & Pharr provides A c but β cannot be determined from A c σ yc determined by mechanical testing W e /W t, H ap /σ yc β

15 Analysis Strategy Glassy polymers experimental validation W e /W t in the range Residual imprint cannot be measured because of viscoelastic effects σ yc determined by mechanical testing W e /W t, H ap /σ yc β

16 Experimental Range experimental validation

17 Literature Comparison experimental validation Bulk Metallic Glasses Ceramic Glasses Glassy Polymers B

18 CONCLUSIONS A novel methodology based on instrumented indentation was developed to characterize the mechanical properties (E, σ yc or β) of amorphous materials. The approach is based on the concept of a universal postulate that assumes the existence of a characteristic indentation pressure proportional to the hardness. This hypothesis was numerically validated. This method overcomes the limitation of the conventional indentation models (pile-up effects and pressure sensitivity materials) M. Rodríguez, J. M. Molina-Aldareguía, C. González, J. LLorca, Acta Materialia, 60, , Research Projects Ministry of Science and Innovation, National Program on Materials (MAT ) Comunidad de Madrid, Program ESTRUMAT-CM EU project MAAXIMUS