In-situ nano-mechanical tests in the light of μlaue diffraction

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1 Engineering Conferences International ECI Digital Archives Nanomechanical Testing in Materials Research and Development V Proceedings Fall In-situ nano-mechanical tests in the light of μlaue diffraction Thomas Cornelius Aix-Marseille Université, thomas.cornelius@im2np.fr Cedric Leclere Aix-Marseille Université Zhe Ren Aix-Marseille Université Anton Davydok Aix-Marseille Université Olivier Thomas Aix-Marseille Université Follow this and additional works at: Part of the Materials Science and Engineering Commons Recommended Citation [1] B. Wu, A. Heidelberg, J.J. Boland, Nature Materials 4 (2005) 525 [2] G. Richter, K. Hillerich, D.S. Gianola, R. Mönig, O. Kraft, C.A. Volkert, Nano Lett. 9 (2009) 3048 [3] F. Östlund, et al., Adv. Funct. Mat. 19 (2009) 2439 [4] Z. Ren et al., J. Synchrotron Radiat. 21 (2014) 1128 [5] C. Leclere et al., J. Appl. Cryst. 48 (2015) 291 [6] C. Kirchlechner et al., Acta Materialia 60 (2012) 1252 [7] R. Maaß, S. van Petegem, C.N. Borca, H. van Swygenhoven, Mater. Sci. Eng. A 524 (2009) 40 This Abstract and Presentation is brought to you for free and open access by the Proceedings at ECI Digital Archives. It has been accepted for inclusion in Nanomechanical Testing in Materials Research and Development V by an authorized administrator of ECI Digital Archives. For more information, please contact franco@bepress.com.

2 ECI Nanomechanical Testing in Materials Research and Development V Albufeira, Portugal October 4-9, 2015 In situ three-points bending tests of Au nanowires in the light of µlaue diffraction T.W. Cornelius, Z. Ren, C. Leclere, A. Davydok, O. Thomas Aix-Marseille Université, CNRS, IM2NP UMR 7334, Marseille, France J.-S. Micha, O. Robach BM32 beamline, ESRF, Grenoble, France G. Richter MPI for Intelligent Systems, Stuttgart, Germany

3 SFINX Scanning Force microscope for In situ Nanofocused X-ray diffraction z-scanner sample long range xyz stages xy-scanner Z. Ren et al., J. Synchrotron Radiat. 21 (2014) 1128 indentation compression long range xy stages bending

4 in situ µlaue diffraction setup at ESRF MAR CCD MAR CCD diffracted X-rays KB mirrors incident white X-ray beam

5 Au nanowires Si(hkl) cleaned by rinsing in acetone, ethanole fabrication sequence cathodic etching + 30 nm C sputtering transfer to UHV annealing at 680 C, 5 min nanowire growth by physical vapor deposition 10 µm G. Richter, MPI Stuttgart

6 µlaue diffraction SEM 5 µm topography (222) (222) shadow from shadow from AFM head AFM head Au-LIII fluorescence (313) (313) red circles indicate Laue spots from Au nanowire C. Leclere, T.W. Cornelius et al., J. Appl. Cryst. 48 (2015)

7 nanowire bending Si cantilever 3 Au NW UB matrix computed from position and displacement of Laue spots calculation of crystal orientation bending + rotation bending angle (deg) 2 1 loading unloading piezo movement (nm) bending angle β increases up to 3.5 for [111] and [0-11] direction, while for [2-11] β < 1 force not perfectly vertical but finite lateral force exist due to cantilever deflection C. Leclere, T.W. Cornelius et al., J. Appl. Cryst. 48 (2015)

8 FEM simulation a) bending angle [deg] experiment classical beam theory simulation with geometric non-linearities piezo movement [nm] experiment well described by FEM simulations bulk elastic constants geometric non-linearities due to strain inhomogeneity σ max > 450 Mpa>> bulkyieldstrength max. theoreticalshearstress forau τ max = G/2π~ 4.8 GPa C. Leclere, T.W. Cornelius et al., J. Appl. Cryst. 48 (2015)

9 plasticity 1 µm 10 µm Au nanowires plastically deformed using AFM Ex situ scans with µlaue diffraction along nanowire

10 plasticity µm motor position (mm) deformation (µm) bending angle (deg) 20

11 identifying slip systems experiment inverse pole figure theory Stress distribution compression tensile Au 222 (01-1)[111] GNDs expected mainly activated slip system: (0-11),[111] slight deviation observed second slip system calulated geometry clamped boundary conditions expected slip system: (0-11),[111] dislocation stored for compatible deformation of crystal (GNDs) N. Fleck et al., Acta Metall. Mater. 42 (1994)

12 in situ KB scan incident white X-ray beam Si(004) Au(222) C. Leclere et al., in preparation

13 in situ KB scan incident white X-ray beam C. Leclere et al., in preparation

14 in situ KB scan

15 in situ plasticity loading-unloading cycle piezo movement KB KB KB KB KB KB KB + normal scan time peak splitting AFM-tip peak splitting

16 dislocations Calculations based on: F. Hofmann et al., Nature Comm. 4, 2774 (2013) beam profile rotation due to dislocations Geometrically necessary boundary (GNB) with 20 dislocations bending angles: (11-2)=0.13⁰, (1-10)=1.05⁰, (111)=0.93⁰ inverse pole figure indicates single slip oriented rotation ~ 1 facilitates «counting» number of dislocations

17 conclusions Scanning force microscope for in situ nanofocused XRD Combination with µlaue diffraction In-situ imaging Elastic bending of NWs Plastic deformation of NWs In situ studies Elastic properties of NWs Defining activated slip system «counting» number of dislocations

18 Registration deadline: October 11 th, 2015

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