scholarly journals Optimization of the SiC Powder Source Material for Improved Process Conditions During PVT Growth of SiC Boules

Materials ◽  
2019 ◽  
Vol 12 (19) ◽  
pp. 3272
Author(s):  
Ellefsen ◽  
Arzig ◽  
Steiner ◽  
Wellmann ◽  
Runde
Keyword(s):  
Crystal Growth ◽  
Size Distribution ◽  
Growth Conditions ◽  
Source Material ◽  
Process Time ◽  
Process Conditions ◽  
Powder Size ◽  
Growth Interface ◽  
X Ray

We have studied the influence of different SiC powder size distributions and the sublimation behavior during physical vapor transport growth of SiC in a 75 mm and 100 mm crystal processing configuration. The evolution of the source material as well as of the crystal growth interface was carried out using in situ 3D X-ray computed tomography (75 mm crystals) and in situ 2D X-ray visualization (100 mm crystals). Beside the SiC powder size distribution, the source materials differed in the maximum packaging density and thermal properties. In this latter case of the highest packaging density, the in situ X-ray studies revealed an improved growth interface stability that enabled a much longer crystal growth process. During process time, the sublimation-recrystallization behavior showed a much smoother morphology change and slower materials consumption, as well as a much more stable shape of the growth interface than in the cases of the less dense SiC source. By adapting the size distribution of the SiC source material we achieved to significantly enhance stable growth conditions.

Optimization of the SiC Powder Source Size Distribution for the Sublimation Growth of Long Crystals Boules

2019 ◽  
Vol 963 ◽  
pp. 42-45
Author(s):  
Johannes Steiner ◽  
Matthias Arzig ◽  
Ta Ching Hsiao ◽  
Peter J. Wellmann
Keyword(s):  
Size Distribution ◽  
Shape Change ◽  
Growth Conditions ◽  
Powder Size ◽  
Growth Interface ◽  
Morphology Change ◽  
Powder Density ◽  
Stable Growth ◽  
Sublimation Growth

The influence of four different SiC source powder size distributions on the sublimation behavior during physical vapor transport growth of SiC was studied. The growth processes were carried out in a 3 inch crystal growth setup and observed in situ using advanced 3D computed tomography X-ray visualization. The single modal D90 size distribution of two source powders was 50 μm and 200 μm, respectively, with a corresponding average powder density of 1.17 g/cm3. The third source powder consisted of a blend of the previously named powders and exhibited an average powder density of 1.66 g/cm3 with a bimodal particle size distribution. The last source was composed of a solid polycrystalline SiC cylinder. The bimodal powder source exhibited a smoother morphology change and material consumption during the growth run and led to a much more stable shape change of the growth interface compared to the single modal source powders. The solid source featured the least morphology change. Therefore, with a careful adaption of the source material stable growth conditions can be achieved.

Application of In Situ 3D Computed Tomography during PVT Growth of 4H-SiC for the Study of Source Material Consumption under Varying Growth Conditions

2016 ◽  
Vol 858 ◽  
pp. 49-52 ◽  
Author(s):  
P.J. Wellmann ◽  
Lars Fahlbusch ◽  
Michael Salamon ◽  
Norman Uhlmann
Keyword(s):  
Growth Parameters ◽  
Growth Conditions ◽  
Source Material ◽  
Gas Pressure ◽  
Inert Gas ◽  
Material Surface ◽  
Growth Interface ◽  
Axial Temperature ◽  
The Stability

2D and 3D in-situ X-ray visualization was applied to study the behavior of the SiC source material during PVT growth under various growth conditions. Experiments were carried out in two growth chambers for the growth of 3 inch and 4 inch crystals. Growth parameters were varied in the gas room in terms of axial temperature and inert gas pressure. The study addresses the stability of the SiC source material surface. It is shown that a higher inert gas pressure (e.g. 25 mbar) inhibits an unintentional upward evolution of the SiC feedstock that interferes with the crystal growth interface. The latter is related to a suppression of a pronounced recrystallization inside the SiC source. For a low inert gas pressure (e.g. 10 mbar) it is concluded that the axial temperature gradient inside the source material needs to be decreased to less than ca. 10 K/cm.

Application of 3-D X-Ray Computed Tomography for the In Situ Visualization of the SiC Crystal Growth Interface during PVT Bulk Growth

2013 ◽  
Vol 740-742 ◽  
pp. 27-30 ◽  
Author(s):  
Georg Neubauer ◽  
Michael Salamon ◽  
Florian Roider ◽  
Norman Uhlmann ◽  
Peter J. Wellmann
Keyword(s):  
Computed Tomography ◽  
Crystal Growth ◽  
Vapor Transport ◽  
Growth Interface ◽  
X Ray ◽  
Bulk Growth ◽  
Growth System ◽  
X Ray Computed ◽  
First Time

In this paper, we present for the first time an in-situ 3-D reconstruction of the SiC crystal growth interface using X-ray computed tomography (CT). We show that the shape of the growth interface can be determined with high precision at growth temperatures above 2100 °C in a conventional 3” PVT (physical vapor transport) growth system.

Growth Conditions and In Situ Computed Tomography Analysis of Facetted Bulk Growth of SiC Boules

2018 ◽  
Vol 924 ◽  
pp. 245-248
Author(s):  
Matthias Arzig ◽  
Michael Salamon ◽  
Norman Uhlmann ◽  
Bertil A. Johansen ◽  
Peter J. Wellmann
Keyword(s):  
Computed Tomography ◽  
Packing Density ◽  
Thermal Gradient ◽  
Growth Conditions ◽  
Source Material ◽  
Lateral Growth ◽  
Growth Interface ◽  
Bulk Growth ◽  
Tomography Analysis

Two 3inch SiC boules were grown in a PVT setup using source material of different packing density. During the growth, in-situ computed tomography of the growing boules showed differences in the development of the growth interface. A slightly bent growth interface was found for the smaller packing density. For the higher packing density the resulting crystal exhibits the onset of 6 pyramidal facets on its flanks. Besides that, strong anisotropic lateral growth was found on its (000-1) facet. Numerical simulations show an impact of the powder on the thermal gradient in the growth cell and therefore on the supersaturation. It is discussed that a higher supersaturation can account for the anisotropy in the growth rate of the [1-100] and the [11-20] direction.

Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Growth Technique ◽  
Salt Hydrate ◽  
X Ray

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.

scholarly journals In situ X-ray Diffraction Investigation of the Crystallisation of Perfluorinated Ce(IV)-based Metal-Organic Frameworks with UiO-66 and MIL-140 architectures

2020 ◽  
Author(s):  
Stephen Shearan ◽  
Jannick Jacobsen ◽  
Ferdinando Costantino ◽  
Roberto D’Amato ◽  
Dmitri Novikov ◽  
...  
Keyword(s):  
Crystal Growth ◽  
Metal Organic Frameworks ◽  
Building Blocks ◽  
Nucleation And Growth ◽  
X Ray Diffraction ◽  
X Ray ◽  
Rate Determining Step ◽  
Wide Range ◽  
Metal Organic

We report on the results of a thorough <i>in situ</i> synchrotron powder X-ray diffraction study of the crystallisation in aqueous medium of two recently discovered perfluorinated Ce(IV)-based metal-organic frameworks (MOFs), analogues of the already well investigated Zr(IV)-based UiO-66 and MIL-140A, namely, F4_UiO-66(Ce) and F4_MIL-140A(Ce). The two MOFs were originally obtained in pure form in similar conditions, using ammonium cerium nitrate and tetrafluoroterephthalic acid as building blocks, and small variations of the reaction parameters were found to yield mixed phases. Here, we investigate the crystallisation of these compounds <i>in situ</i> in a wide range of conditions, varying parameters such as temperature, amount of the protonation modulator nitric acid (HNO<sub>3</sub>) and amount of the coordination modulator acetic acid (AcOH). When only HNO<sub>3</sub> is present in the reaction environment, F4_MIL-140A(Ce) is obtained as a pure phase. Heating preferentially accelerates nucleation, which becomes rate determining below 57 °C, whereas the modulator influences nucleation and crystal growth to a similar extent. Upon addition of AcOH to the system, alongside HNO<sub>3</sub>, mixed-phased products, consisting of F4_MIL-140A(Ce) and F4_UiO-66(Ce), are obtained. In these conditions, F4_UiO-66(Ce) is always formed faster and no interconversion between the two phases occurs. In the case of F4_UiO-66(Ce), crystal growth is always the rate determining step. An increase in the amount of HNO<sub>3</sub> slows down both nucleation and growth rates for F4_MIL-140A(Ce), whereas nucleation is mainly affected for F4_UiO-66(Ce). In addition, a higher amount HNO<sub>3</sub> favours the formation of F4_MIL-140A(Ce). Similarly, increasing the amount of AcOH leads to slowing down of the nucleation and growth rate, but favours the formation of F4_UiO-66(Ce). The pure F4_UiO-66(Ce) phase could also be obtained when using larger amounts of AcOH in the presence of minimal HNO<sub>3</sub>. Based on these <i>in situ</i> results, a new optimised route to achieving a pure, high quality F4_MIL-140A(Ce) phase in mild conditions (60 °C, 1 h) is also identified.

scholarly journals X-Ray Tomography Study on Porosity and Particle Size Distribution in In Situ Al-4.5Cu-5TiB2 Semisolid Rolled Composites

JOM ◽  
2019 ◽  
Vol 71 (11) ◽  
pp. 4050-4058 ◽  
Author(s):  
Swapnil Morankar ◽  
Monalisa Mandal ◽  
Nadia Kourra ◽  
Mark A. Williams ◽  
Rahul Mitra ◽  
...  
Keyword(s):  
Particle Size ◽  
Particle Size Distribution ◽  
Size Distribution ◽  
X Ray

In situ Small-Angle and Wide-Angle X-ray Scattering Investigation on Nucleation and Crystal Growth of Nanosized Zeolite A

2007 ◽  
Vol 19 (8) ◽  
pp. 1906-1917 ◽  
Author(s):  
Wei Fan ◽  
Masaru Ogura ◽  
Gopinathan Sankar ◽  
Tatsuya Okubo
Keyword(s):  
Crystal Growth ◽  
Small Angle ◽  
Wide Angle ◽  
Zeolite A ◽  
X Ray ◽  
X Ray Scattering ◽  
Nanosized Zeolite ◽  
Ray Scattering
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