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Thermally induced microstrain broadening in polycrystalline materials: Powder-diffraction studies on hexagonal zinc metal and hexagonal ε-iron nitride

Andreas Leineweber 1Thomas Gressmann 1Eric J. Mittemeijer 1Angus C. Lawson 2James A. Valdez 2Joice A. Roberts 2Wolfgang S. Kreher 3

1. Max Planck Institute for Metals Research, Heisenbergstrasse 3, Stuttgart 70569, Germany
2. Los Alamos National Laboratory (LANL), Los Alamos, NM 87545, United States
3. Institute for Materials Science, Dresden University of Technology, Dresden 01069, Germany

Abstract
Spatial variations of the thermal-expansion tensors in multiphase materials or in non-cubic, single-phase polycrystalline materials induce upon temperature change locally varying microstresses [1]. Thus local plastic deformation or even grain-boundary cracking can occur. Understanding and experimental analysis of such thermally-induced microstresses, during production and during service, can be decisive for accurately estimating the strength properties of materials. These microstresses can be studied by analysing the associated microstrains by powder diffraction, because (within the Stokes-Wilson approximation [2]) the line broadening of a reflection hkl is determined by the projection of the microstrain distribution on the diffraction vector.

In the present contribution monophase hexagonal polycrystals showing anisotropic thermal expansion are considered. If the polycrystal is stress-free at T0, temperature change to T1 will lead to thermal misfit between differently oriented grains causing the above-mentioned thermal microstresses and microstrains. The corresponding multivariate Gaussian microstrain distribution can be calculated (neglecting plastic deformation and surface effects; assuming randomly oriented grains) on the basis of statistical and internal-energy considerations [1,3]:

(i) The average strain leads to average lattice parameters somewhat different from the equilibrium lattice parameters at T1. The average strain can be used to define a strain scale with <Δεij> = 0.

(ii) The joint second central moments <ΔεijΔεmn> of the microstrain distribution around the average <Δεij> = 0 are proportional (constant K) to the corresponding components of the elastic compliance tensor in the crystal’s frame of reference, <ΔεijΔεmn> = Ksijmn. On the basis of these second moments the expected hkl-dependent microstrain broadening can be calculated [4].

The following experimental model cases were considered:

(a) Neutron-diffraction experiments on polycrystalline hexagonal zinc at ambient temperature (T0, microstrain-free state) and after cooling to T1 = 10 K.

(b) Synchrotron X-ray diffraction applied to polycrystalline hexagonal ε-iron nitride after cooling from 673 K (production temperature, T0) to ambient temperature, T1.

Both materials exhibit hkl-dependent microstrain broadening at T1. For zinc this broadening is especially pronounced for 00l reflections, which is compatible with zinc’s high elastic compliance along [001] directions. In both cases, comparison of the experimental data with theory [1,3] indicates that local plastic deformation had occurred. This conclusion is also supported by the observed characteristic reflection asymmetries, where the skewnesses of the hk0 and 00l reflections have inverse signs.

[1] W. Kreher, W. Pompe, Internal Stresses in Heterogeneous Solids, Akademie-Verlag Berlin (1989).

[2] A. J. C. Wilson, Nuovo Cimento 1 (1955) 277.

[3] W. S. Kreher, Comp. Mater. Sci. 7 (1996) 147.

[4] A. Leineweber, J. Appl. Cryst. 39 (2006) 509.

 

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Related papers

Presentation: Oral at 11th European Powder Diffraction Conference, Microsymposium 4, by Andreas Leineweber
See On-line Journal of 11th European Powder Diffraction Conference

Submitted: 2008-04-29 15:06
Revised:   2009-06-07 00:48