scholarly journals Effects of Annealing Temperature on Recrystallization Texture and Microstructure Uniformity of High Purity Tantalum

Metals ◽  
2019 ◽  
Vol 9 (1) ◽  
pp. 75 ◽  
Author(s):  
Jialin Zhu ◽  
Chao Deng ◽  
Yahui Liu ◽  
Nan Lin ◽  
Shifeng Liu

One hundred and thirty-five degree clock rolling significantly improves the texture homogeneity of tantalum sheets along the thickness, but a distinctly fragmented substructure is formed within {111} (<111>//normal direction (ND)) and {100} (<100>//ND) deformation grains, which is not suitable to obtain a uniform recrystallization microstructure. Thus, effects of different annealing temperatures on the microstructure and texture heterogeneity of tantalum sheets along the thickness were investigated by X-ray diffraction (XRD), electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). Results show that the texture distribution along θ-fiber and γ-fiber is irregular and many large grains with {111} orientation develop during annealing at high temperature. However, low-temperature annealing can not only weaken the texture intensity in the surface and the center layer but also introduce a more uniform grain size distribution. This result can be attributed to the subgrain-nucleation-dominated recrystallization mechanism induced by recovery at low temperature, and moreover, a considerable decline of recrystallization driving force resulting from the release of stored energy in the deformation matrix.

2014 ◽  
Vol 67 (5) ◽  
pp. 790
Author(s):  
Jiang Wang ◽  
Jian Li ◽  
Youwen Wang

One-dimensional PbTiO3 nanowires 40–500 nm in diameter and ~400 μm in length were synthesized via a hydrothermal strategy and characterized by X-ray diffraction, electron backscatter diffraction, scanning electron microscopy, and transmission electron microscopy. The results show that the PbTiO3 nanowires exhibit a new acicular crystal structure, which is a tetragonal superstructure composed of a large unit cell of 40 atoms (Pb : Ti : O = 1 : 1 : 3) with a = 12.35 Å, c = 3.83 Å. The PbTiO3 has a feature of unidirectional bending when observed through transmission electron microscopy several times. The bending can be controlled by the electron beam intensity in transmission electron microscopy and the bending process is reversible. Moreover, a possible mechanism for the bending behaviour was also studied, which indicates that macroscopic polarization is in the {110} plane and the direction is not consistent with the electric field, giving the possible driving force for the bending.


Metals ◽  
2019 ◽  
Vol 9 (3) ◽  
pp. 358
Author(s):  
Jialin Zhu ◽  
Shifeng Liu ◽  
Shuai Yang ◽  
Yu Zhang ◽  
Jing Zhang ◽  
...  

The texture and the bulk stored energy along the thickness direction were extremely inhomogeneous in the clock-rolled tantalum sheets with 70% reduction. Therefore, the effects of different annealing temperatures on the microstructure and texture distribution of tantalum plates through the thickness were investigated by X-ray diffraction (XRD) and electron backscatter diffraction (EBSD). The results showed that the occurrence of strong {111} recrystallization texture in the center layer can be attributed to the subgrains nucleation mechanism when annealed at the low temperature. Many subgrains with {111} orientation appeared in the center layer, due to its high stored energy and preferential nucleation sites of the {111} deformed matrix, and rapidly grew into the effective nucleus, resulting in the large {111} grain size and strong {111} texture after complete recrystallization. Contrarily, at the high temperature, high-angle grain boundaries had sufficient driving force to generate migration, due to the lack of recovery, and the growth time of recrystallized nucleus was much shorter, contributing to relatively uniform recrystallization microstructure and texture distribution along the thickness.


Metals ◽  
2021 ◽  
Vol 11 (9) ◽  
pp. 1405
Author(s):  
Tomonori Kitashima ◽  
Lingjian Meng ◽  
Makoto Watanabe

The effect of grain-interior α precipitation on the β texture evolution of the near-β Ti-6246 alloy during through-transus forging was investigated in two-step sequential forgings. The microstructure and texture were analyzed using scanning electron microscopy, electron-backscatter diffraction, and X-ray diffraction. The previous β forging was performed at 1253 K at 0.01/s, while the subsequent forging in the (α + β) region was conducted at 1073 K at 0.01/s. The forging in the β region facilitated the penetration of the interior α phase into β grains and reduced the formation of grain boundary α. The {001} texture intensity increased during the forging in the single β region. By contrast, the increase in the {001} texture intensity was moderate at a lower temperature (1073 K) because the Schmid factor (SF) value of the {110}<111> slip system drastically decreased, but those of the {112}<111> and {123}<111> slip systems increased before α precipitation. During α precipitation for all β forging ratios, the {110}<111> slip system was activated, resulting in a lowering of the {001} texture intensity. The lower the forging temperature before interior α precipitation under a constant total forging ratio, the more the {001} texture intensity was suppressed in the final β texture, accompanied by interior α precipitation.


Author(s):  
A. Leineweber ◽  
M. Löffler ◽  
S. Martin

Abstract Cu6Sn5 intermetallic occurs in the form of differently ordered phases η, η′ and η′′. In solder joints, this intermetallic can undergo changes in composition and the state of order without or while interacting with excess Cu and excess Sn in the system, potentially giving rise to detrimental changes in the mechanical properties of the solder. In order to study such processes in fundamental detail and to get more detailed information about the metastable and stable phase equilibria, model alloys consisting of Cu3Sn + Cu6Sn5 as well as Cu6Sn5 + Sn-rich melt were heat treated. Powder x-ray diffraction and scanning electron microscopy supplemented by electron backscatter diffraction were used to investigate the structural and microstructural changes. It was shown that Sn-poor η can increase its Sn content by Cu3Sn precipitation at grain boundaries or by uptake of Sn from the Sn-rich melt. From the kinetics of the former process at 513 K and the grain size of the η phase, we obtained an interdiffusion coefficient in η of (3 ± 1) × 10−16 m2 s−1. Comparison of this value with literature data implies that this value reflects pure volume (inter)diffusion, while Cu6Sn5 growth at low temperature is typically strongly influenced by grain-boundary diffusion. These investigations also confirm that η′′ forming below a composition-dependent transus temperature gradually enriches in Sn content, confirming that Sn-poor η′′ is metastable against decomposition into Cu3Sn and more Sn-rich η or (at lower temperatures) η′. Graphic Abstract


2018 ◽  
Vol 83 (4) ◽  
pp. 523-530 ◽  
Author(s):  
Victor V. Subbotin ◽  
Anna Vymazalová ◽  
František Laufek ◽  
Yevgeny E. Savchenko ◽  
Chris J. Stanley ◽  
...  

AbstractMitrofanovite, Pt3Te4, is a new telluride discovered in low-sulfide disseminated ore in the East Chuarvy deposit, Fedorovo–Pana intrusion, Kola Peninsula, Russia. It forms anhedral grains (up to ~20 μm × 50 μm) commonly in intergrowths with moncheite in aggregates with lukkulaisvaaraite, kotulskite, vysotskite, braggite, keithconnite, rustenburgite and Pt–Fe alloys hosted by a chalcopyrite–pentlandite–pyrrhotite matrix. Associated silicates are: orthopyroxene, augite, olivine, amphiboles and plagioclase. Mitrofanovite is brittle; it has a metallic lustre and a grey streak. Mitrofanovite has a good cleavage, along {001}. In plane-polarised light, mitrofanovite is bright white with medium to strong bireflectance, slight pleochroism, and strong anisotropy on non-basal sections with greyish brown rotation tints; it exhibits no internal reflections. Reflectance values for the synthetic analogue of mitrofanovite in air (Ro, Re’ in %) are: 58.4, 54.6 at 470 nm; 62.7, 58.0 at 546 nm; 63.4, 59.1 at 589 nm; and 63.6, 59.5 at 650 nm. Fifteen electron-microprobe analyses of mitrofanovite gave an average composition: Pt 52.08, Pd 0.19, Te 47.08 and Bi 0.91, total 100.27 wt.%, corresponding to the formula (Pt2.91Pd0.02)Σ2.93(Te4.02Bi0.05)Σ4.07 based on 7 atoms; the average of eleven analyses on synthetic analogue is: Pt 52.57 and Te 47.45, total 100.02 wt.%, corresponding to Pt2.94Te4.06. The density, calculated on the basis of the formula, is 11.18 g/cm3. The mineral is trigonal, space group R$\overline 3 $m, with a = 3.9874(1), c = 35.361(1) Å, V = 486.91(2) Å3 and Z = 3. The crystal structure was solved and refined from the powder X-ray-diffraction data of synthetic Pt3Te4. Mitrofanovite is structurally and chemically related to moncheite (PtTe2). The strongest lines in the powder X-ray diffraction pattern of synthetic mitrofanovite [d in Å (I) (hkl)] are: 11.790(23)(003), 5.891(100)(006), 2.851(26)(107), 2.137(16)(1013), 2.039(18)(0114), 1.574(24)(0120), 1.3098(21)(0027). The structural identity of natural mitrofanovite with synthetic Pt3Te4 was confirmed by electron backscatter diffraction measurements on the natural sample. The mineral name is chosen to honour Felix P. Mitrofanov, a Russian geologist who was among the first to discover platinum-group element mineralisation in the Fedorova–Pana complex.


2020 ◽  
Vol 14 (2) ◽  
pp. 113-118
Author(s):  
Daniel Ursu ◽  
Anamaria Dabici ◽  
Marinela Miclau ◽  
Nicolae Miclau

We report for the first time the fabrication of hierarchical ordered superstructure CuB2O4 with flower-like morphology via a one-step, low temperature hydrothermal method. The tetragonal structure of CuB2O4 was determined by X-ray diffraction and high-resolution transmission electron microscopy. Optical measurements attested of the quality of the fabricated CuB2O4 and high temperature X-ray diffraction confirmed its thermal stability up to 600 ?C. The oriented attachment growth and the hierarchical self-assembly of micrometer-sized platelets producing hierarchical superstructures with flower-like morphology are designed by pH of the hydrothermal solution. The excellent band gap, high thermal stability and hierarchical structure of the CuB2O4 are promising for the photovoltaic and photocatalytic applications.


Catalysts ◽  
2020 ◽  
Vol 10 (2) ◽  
pp. 202
Author(s):  
Long Lu ◽  
Xueman Wang ◽  
Chunhua Hu ◽  
Ying Liu ◽  
Xiongbo Chen ◽  
...  

Nanosized V-Ce oxides supported on TiO2 (VCT) were prepared and utilized in the low-temperature selective catalytic reduction (SCR) of NO with NH3. Compared with the other V-Ce oxides-based catalysts supported on Al2O3, ZrO2, and ZSM-5, VCT showed the best SCR activity in a low-temperature range. The NOx conversion of 90% could be achieved at 220 °C. Characterizations including X-ray diffraction (XRD), scanning election micrograph (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), temperature-programmed desorption with NH3 (NH3-TPD), and temperature-programmed reduction with H2 (H2-TPR) showed that V1.05Ce1/TiO2 exhibited a good dispersion of V2O5, enrichment of surface Ce3+ and chemical-absorbed oxygen, and excellent redox capacity and acidity, which resulted in the best SCR performance at low temperature.


Metals ◽  
2020 ◽  
Vol 10 (3) ◽  
pp. 406
Author(s):  
Samiha Saad ◽  
Zakaria Boumerzoug ◽  
Anne Laure Helbert ◽  
François Brisset ◽  
Thierry Baudin

The objective of this work is to study, on a copper wire, the effect of TiO2-nanoparticles on electrodeposited nickel. Both the microstructure and surface morphology (texture) of the coating were investigated. This deposit is obtained from baths of sulfated electroplating Watts. The Ni-TO2 composite coating is deposited at a temperature of 45 °C. The composite deposit is prepared by adding nanoparticles of TiO2 to the electrolyte. The characterization has been carried out by X-ray diffraction, scanning electron microscopy, microhardness measurements, and electron backscatter diffraction (EBSD). Vickers microhardness was used to characterize the mechanical properties of the electrodeposited nickel. The results showed the effects of the TiO2 on the composition, the surface morphology, and the hardness of the deposited layer. However, there was not an effect of TiO2 nanoparticles on texture.


2008 ◽  
Vol 41 (2) ◽  
pp. 310-318 ◽  
Author(s):  
Greg Johnson ◽  
Andrew King ◽  
Marcelo Goncalves Honnicke ◽  
J. Marrow ◽  
Wolfgang Ludwig

By simultaneous acquisition of the transmitted and the diffracted beams, the applicability of the previously introduced diffraction contrast tomography technique [Ludwig, Schmidt, Lauridsen & Poulsen (2008).J. Appl. Cryst.41, 302–309] can be extended to the case of undeformed polycrystalline samples containing more than 100 grains per cross section. The grains are still imaged using the occasionally occurring diffraction contribution to the X-ray attenuation coefficient, which can be observed as a reduction in the intensity of the transmitted beam when a grain fulfils the diffraction condition. Automating the segmentation of the extinction spot images is possible with the additional diffracted beam information, even in the presence of significant spot overlap. By pairing the corresponding direct (`extinction') and diffracted beam spots a robust sorting and indexing approach has been implemented. The analysis procedure is illustrated on a real data set and the result is validated by comparison with a two-dimensional grain map obtained by electron backscatter diffraction.


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