Bicrystal growth and characterization of copper twist grain boundaries

Schwarz, Stephen; Houge, E. C.; Giannuzzi, Lucille A.; King, Alexander H.

doi:10.1016/s0022-0248(00)00918-0

Cited by 13 publications

(10 citation statements)

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“…A grain boundary misorientation of 43.9 o /[1 30 0] was obtained using reconstructed diffraction patterns. This compares well with a value of 44.7 o /[100] that was obtained previously using the EBSD technique [2]. The acquisition of automatically obtained crystallographic information in the TEM will greatly aid in the microstructural evaluation of TEM specimens [6].…”

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confidence: 86%

“…The following results were obtained using a Philips/TEM Tecnai F30 TEM operating at 200 keV equipped with an EDAX/TSL ACT system. Two different samples were used for the study, the surface of abalone (Nacre) and a Cu bicrystal consisting of a 45 o /[100] twist boundary [2]. TEM specimens were prepared using an FEI 200TEM focused ion beam workstation equipped with an Omniprobe in-situ W probe.…”

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Automated Crystallography and Grain Mapping in the TEM

et al. 2002

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Obtaining crystallographic information automatically has become routine using computer acquisition of electron backscatter diffraction (EBSD) patterns in the scanning electron microscope (SEM) [1]. The crystallographic information that is acquired may be used to generate data from polycrystalline samples that include crystallographic texture information, grain boundary misorientation analysis, phase identification, grain size distribution, and grain mapping. A natural extension of the SEM analysis is to automate the acquisition of crystallographic information obtained from the transmission electron microscope (TEM). This has recently become a reality via a commercially available system. The system automatically acquires dark field images using conical scan methods. The dark field images are then used to reconstruct diffraction patterns for computer indexing. Once an orientation is assigned for each pixel, statistical manipulation of the data may be performed as with the EBSD data. In addition, grain maps may be obtained without any a priori knowledge of the orientation of each pixel. That is, just the position of the brightest reflectors from the reconstructed diffraction pattern may be used to differentiate between grains. Automatic grain mapping via crystallographic methods is a major breakthrough for TEM analysis since accurate grain size determination via the TEM often requires tedious analyses of multiple images obtained at different tilt conditions due to diffraction contrast effects. The following results were obtained using a Philips/TEM Tecnai F30 TEM operating at 200 keV equipped with an EDAX/TSL ACT system. Two different samples were used for the study, the surface of abalone (Nacre) and a Cu bicrystal consisting of a 45 o /[100] twist boundary [2]. TEM specimens were prepared using an FEI 200TEM focused ion beam workstation equipped with an Omniprobe in-situ W probe. The abalone was prepared using the ex-situ lift-out technique [3]. The Cu bicrystal was prepared using the in-situ liftout technique [4].FIG. 1 shows a cross-section TEM bright field (BF) image from the abalone. The abalone consists of layers of CaCO 3 (aragonite) separated by organic material [5]. An inset of a [010] selected area diffraction pattern from the dark grain in the Laue condition (and overlapping grains) is shown in FIG. 1. FIG. 2 is a grain map of the abalone using the ACT system. The grain boundaries within the CaCO 3 are readily observed as shown by the arrows and the apparent texture of the abalone is evident by the similar colors of contrast that is produced by the grain map. FIG. 3 is a processed lattice image and a simulation of a nominal Cu 45 o /[100] twist boundary. A grain map of the twist boundary at a lower magnification is shown in FIG. 4. A grain boundary misorientation of 43.9 o /[1 30 0] was obtained using reconstructed diffraction patterns. This compares well with a value of 44.7 o /[100] that was obtained previously using the EBSD technique [2]. The acquisition of automatically obtained crystallographic inf...

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Automated Crystallography and Grain Mapping in the TEM

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“…These facts make them preferential sites for precipitation of new phases and regions for atomic transition. Therefore the new aluminum grains tend to nucleate at the boundary of the field where aluminum atoms gather . It is found that initial deposition of aluminum grains proceeds gradually through two‐dimensional spreading.…”

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Study on the initial electrodeposition behavior of aluminum on TiB₂/A356 composite

Huang

Liu

Wang

et al. 2012

Materials & Corrosion

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The electrodeposition behavior of aluminum on TiB 2 /A356 composite from AlCl 3 -NaCl-KCl molten salt was studied in this paper. The surface morphology, microstructure, and phase composition of aluminum coating were characterized by scanning electron microscopy (SEM) and energy dispersive spectrometer (EDS). The phase composition of the composite was examined by X-ray diffraction technique. The polarization curves were measured and the corrosion current densities were obtained. The results indicated that the aluminum coating was preferentially electrodeposited on the surface of TiB 2 and Si phases. This phenomenon could be largely attributed to the different surface energies of TiB 2 , Si, and Al phases. With the increasing of deposition time, a continuous, dense, and faceted aluminum coating was finally obtained. It was inferred that the growth of aluminum coating on the surface of the composite was mainly through two-dimensional spreading. However, three-dimensional growth could also be seen. The corrosion current density of the aluminumcoated TiB 2 /A356 composite (1 min) decreased by an order of magnitude as compared with that of TiB 2 /A356 composite, and was close to that of A356 alloy, and also in the same order of magnitude with that of pure aluminum. It is evident that, the coverage of TiB 2 and Si phases by aluminum coating (1 min) can effectively improve the corrosion resistance of TiB 2 /A356 composite. In combination with SEM and EDS results, the behavior can be characterized as preferential electrodeposition.

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“…Such a systematic study of the influence of GB character on material properties requires a template-based approach to obtain desired GBs. For many metals, bicrystalline samples with predefined GB parameters have been grown using the vertical Bridgman technique for specific GB property studies [28]. However, in Ti, the hcp-bcc allotropic transition makes it impossible to fabricate bicrystals to form specific desired GBs.…”

Section: Introductionmentioning

confidence: 99%

Microstructure, grain boundary evolution and anisotropic Fe segregation in (0001) textured Ti thin films

Devulapalli¹,

Hans²,

Prithiv³

et al. 2021

Preprint

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The structure and chemistry of grain boundaries (GBs) are crucial in determining polycrystalline materials' properties. Faceting and solute segregation to minimize the GB energy is a commonly observed phenomenon. In this paper, a deposition process to obtain pure tilt GBs in titanium (Ti) thin films is presented. By increasing the power density, a transition from polycrystalline film growth to a maze bicrystalline Ti film on SrTiO 3 (001) substrate is triggered. All the GBs in the bicrystalline thin film are characterized to be Σ13 [0001] coincident site lattice (CSL) boundaries. The GB planes are seen to distinctly facet into symmetric { 7520} and asymmetric {10 10} // {11 20} segments of 20-50 nm length. Additionally, EDS reveals preferential segregation of iron (Fe) in every alternate symmetric { 7520} segment. Both the faceting and the segregation are explained by a difference in the CSL density between the facet planes. Furthermore, in the GB plane containing Fe segregation, atom probe tomography is used to experimentally determine the GB excess solute to be 1.25 atoms/nm 2 . In summary, the study reveals for the first time a methodology to obtain bicrystalline Ti thin films with strong faceting and an anisotropy in iron (Fe) segregation behaviour within the same family of planes.

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Bicrystal growth and characterization of copper twist grain boundaries

Cited by 13 publications

References 6 publications

Automated Crystallography and Grain Mapping in the TEM

Automated Crystallography and Grain Mapping in the TEM

Study on the initial electrodeposition behavior of aluminum on TiB₂/A356 composite

Microstructure, grain boundary evolution and anisotropic Fe segregation in (0001) textured Ti thin films

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Bicrystal growth and characterization of copper twist grain boundaries

Cited by 13 publications

References 6 publications

Automated Crystallography and Grain Mapping in the TEM

Automated Crystallography and Grain Mapping in the TEM

Study on the initial electrodeposition behavior of aluminum on TiB2/A356 composite

Microstructure, grain boundary evolution and anisotropic Fe segregation in (0001) textured Ti thin films

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Study on the initial electrodeposition behavior of aluminum on TiB₂/A356 composite