Bicrystal growth and characterization of copper twist grain boundaries

doi:10.1016/S0022-0248(00)00918-0

Journal of Crystal Growth

Volume 222, Issues 1–2, January 2001, Pages 392-398

https://doi.org/10.1016/S0022-0248(00)00918-0 Get rights and content

Abstract

Copper bicrystals with twist character were grown using the vertical Bridgman technique. Cu bicrystals were grown such that the grain boundary in each sample had a nominal twist misorientation consisting of either a low angle (10°), a special angle (Σ5=36.87°), or a high angle (45°). The grain boundary plane in all cases was (1 0 0). The grain boundaries were grown using single-crystal seeds that were oriented to within ±0.5° using the Laue back-reflection X-ray diffraction method. The misorientation of each twist boundary was characterized using electron backscattering diffraction patterns in a scanning electron microscope. All grain boundary misorientations were determined to be within the limits defined by the Brandon criterion.

Introduction

Grain boundary properties may govern the overall properties of polycrystalline materials. For example, it is well known that grain boundary diffusion governs solid-state reactions such as Coble creep, sintering, diffusion induced grain boundary migration, electromigration, discontinuous phase transformations, recrystallization, and grain growth [1]. Thus, an understanding of grain boundary diffusion and related phenomena may result in the use of grain boundary engineering to either enhance or reduce a particular solid-state reaction.

It is well known that grain boundary properties vary with misorientation angle [2]. In addition, special, low Σ boundaries tend to exhibit special properties [2]. Grain boundary features (i.e., those characteristics associated with the structure and crystallography of the grain boundary), and the mechanical, physical, and chemical properties of materials attributed to these grain boundary features have been studied extensively (see, e.g., Ref. [2]).

Many investigators have grown bicrystals of a particular misorientation to study specific grain boundary properties. Much of the literature on the production of bicrystals has focused on the production of thin film samples (see, e.g., Ref. [3], [4], [5]). However, King et al. [6], [7] were able to grow symmetric and asymmetric tilt grain boundaries in bicrystals based on the vertical Bridgman technique [8]. In an effort to understand grain boundary properties in twist boundaries, it is desired to produce bicrystal samples of significant size for subsequent diffusion analyses. Thus, the following is a detailed description of the production of copper bicrystals grown with pure twist character using the vertical Bridgman technique.

Section snippets

Experimental procedures

Single-copper crystals and subsequent bicrystals were grown using the vertical Bridgman technique. Bulk copper of 99.999% purity was either chemically polished or electropolished to remove any surface oxidation or impurities. Chemical polishing was performed with a solution consisting of a 1:1:1 mixture of acetic, nitric and phosphoric acids by volume. Each piece of bulk copper was placed in fresh solution for one to two minutes. Electropolishing was performed on the bulk copper using a

Results and discussion

The results of the bicrystal growth yielded samples greater than 10 cm in length with cross sections approximately 1 cm². The bicrystals were cut into approximately 5 mm thick slices to characterize their misorientation. The surfaces were ground and mechanically polished as outlined in the experimental section above. The bicrystal samples were then mounted on a sample stud and placed in a Hitachi 4100 scanning electron microscope (SEM) with a TSL Orientation Imaging Microscopy (OIM) electron

Conclusions

Copper twist bicrystals with nominal misorientations of 10°, $Σ$ 5, and 45° about [1 0 0] were grown using the vertical Bridgman technique. The bicrystals were characterized using electron backscattering diffraction in a SEM. The grown bicrystals were consistent with the Brandon criterion.

Acknowledgements

This work was made possible by NSF DMR #9703281.

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Bicrystal growth and characterization of copper twist grain boundaries

Abstract

Introduction

Section snippets

Experimental procedures

Results and discussion

Conclusions

Acknowledgements

Scripta Metall.

Scripta Metall.

Scripta Metall.

Fundamentals of Grain and Interphase Boundary Diffusion

The Role of the Coincidence Site Lattice in Grain Boundary Engineering