Synthesize Ti3SiC2 from TiH2 by Pressureless Sintering

2012 ◽  
Vol 512-515 ◽  
pp. 676-680 ◽  
Author(s):  
Liang Li ◽  
Ai Guo Zhou ◽  
Li Bo Wang ◽  
Fei Xiang Hu
Keyword(s):  
Electron Microscopy ◽  
Single Phase ◽  
Argon Atmosphere ◽  
Pressureless Sintering ◽  
X Ray Diffraction ◽  
Powder Mixtures ◽  
Titanium Silicon Carbide ◽  
X Ray ◽  
Titanium Silicon ◽  
Scanning Electron

In this paper, titanium silicon carbide (Ti3SiC2) powders were synthesized from TiH2 as Ti source by pressureless sintering in flowing argon atmosphere without preliminary dehydrogenation. Starting materials are powder mixtures with the mole ratio of 3TiH2/Si/2C or 3TiH2/SiC/C. Both kinds of starting materials were sintered in a tube furnace at the temperature range from 1300°C to 1500°C for 10~180min in flowing argon atmosphere. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to characterize the phase compositions and morphology of the products after different treatments. It was showed that almost single phase Ti3SiC2 powder (94.7 wt.%) can be synthesized by pressureless sintering from 3TiH2/Si/2C powders at 1400~1425°C for about 180min or from 3TiH2/SiC/C powders at 1425~1500°C for about 180min. From SEM micrographs, as-synthesized samples were porous. Most plate-like grains were about 5~10 μm in diameter and 1~2 μm in thickness. The speed of temperature increasing is an important factor to affect the purity of as-synthesized Ti3SiC2.

Synthesis of Ti3Si0.4Al0.8C1.8 Solid Solution

2008 ◽  
Vol 368-372 ◽  
pp. 995-997
Author(s):  
Cui Wei Li ◽  
Hong Xiang Zhai ◽  
Yang Zhou ◽  
Shi Bo Li ◽  
Zhi Li Zhang
Keyword(s):  
Electron Microscopy ◽  
Solid Solution ◽  
Scanning Electron Microscopy ◽  
Single Phase ◽  
Lattice Parameters ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Powder Mixtures ◽  
X Ray ◽  
Scanning Electron

In this study, free Ti/Si/Al/C powder mixtures with molar ratio of 3:0.4:0.8:1.8 were heated in Argon with various schedules, in order to reveal the possibility for the synthesis of Ti3Si0.4Al0.8C1.8 solid solution powder. X-ray diffraction (XRD) was used for the evaluation of phase identities of the powder after different treatments. Scanning electron microscopy (SEM) was used to observe the morphology of the Ti3Si0.4Al0.8C1.8 solid solution. XRD results showed that predominantly single phase samples of Ti3Si0.4Al0.8C1.8 was prepared after heating at 1400oC for 5 min in Argon and the lattice parameters of Ti3Si0.4Al0.8C1.8 lay between those of Ti3SiC2 and Ti3AlC2.

Structural Evaluation of Ti-22.2Si-11.1B Powders Milled with PCA Addition

2008 ◽  
Vol 591-593 ◽  
pp. 147-153
Author(s):  
Gilbert Silva ◽  
Erika Coaglia Trindade Ramos ◽  
N.S. da Silva ◽  
Alfeu Saraiva Ramos
Keyword(s):  
Electron Microscopy ◽  
Ball Milling ◽  
Ball Mill ◽  
Milling Process ◽  
Argon Atmosphere ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structural Evaluation ◽  
Equilibrium Structures ◽  
Scanning Electron

A large amount of the Ti6Si2B compound can be formed by mechanical alloying and subsequent heat treatment from the elemental Ti-22.2at%Si-11.1at%B powder mixture, but the yield powder after ball milling is reduced due to an excessive agglomeration of ductile particles on the balls and vial surfaces. This work reports on the structural evaluation of Ti-22.2at%Si-11.1at%B powders milled with PCA addition, varying its amount between 1 and 2 wt-%. The milling process was carried out in a planetary ball mill under argon atmosphere, and the milled powders were then heated at 1200oC for 1h under Ar atmosphere in order to obtain equilibrium structures. Samples were characterized by X-ray diffraction, scanning electron microscopy, and thermal analysis. Results revealed that the PCA addition reduced the excessive agglomeration during the ball milling of Ti-22.2at-%Si-11.1at-%B powders. After heating at 1200oC for 1h, the Ti5Si3, Ti3O and/or Ti2C phases were preferentially formed in Ti-22.2at%Si-11.1at%B powders milled with PCA addition, and the Ti6Si2B formation was inhibited.

Crystal Chemistry and Phase Equilibrium Studies of the Bao(baco3)‐r2o3‐cuo Systems. V. Melting Relations in ba2(y,nd,eu)cu3o6+x

1989 ◽  
Vol 169 ◽  
Author(s):  
Winnie Wong‐Ng ◽  
Lawrence P. Cook ◽  
Michael D. Hill ◽  
Boris Paretzkin ◽  
E.R. Fuller
Keyword(s):  
Electron Microscopy ◽  
Single Phase ◽  
X Ray Diffraction ◽  
Equilibrium Studies ◽  
X Ray ◽  
Helium Gas ◽  
Ionic Size ◽  
Differential Thermogravimetric Analysis ◽  
Melting Relations ◽  
Scanning Electron

AbstractThe influence of the ionic size of the lanthanides R on melting relations of Ba2RCu3O6+x, where R=Y, Eu and Nd, was studied and compared with that of a high Tc superconductor mixed‐lanthanide phase Ba2(Y.75Eu.125Nd 125)Cu3O6+xThese materials have been characterized by a variety of methods including differential thermogravimetric analysis (DTA), scanning electron microscopy (SEM) with energy dispersive X‐ray spectroscopy (EDX) and X‐ray powder diffraction. Single phase samples of Ba2(Y.75Eu.125Nd.125)Cu3O6+x were annealed at 1004, 1040, 1052, 1060, 1078, 1107 and 1160°C and quenched into a helium gas container cooled by liquid nitrogen. The SEM micrographs of these samples showed the progressive chnages in features of the microstructures from sintering and grain growth through melting and then recrystallization from the melt. The addition of the SEM technique in conjunction with X‐ray diffraction has been helpful in the study of phase equilibria in this system.

Microstructure and Properties of Nanosemicrystalline Si3N4 Ceramics with Doped Sintering Additives: Part II. Phase Transformation and Microstructural Control

1998 ◽  
Vol 13 (9) ◽  
pp. 2588-2596 ◽  
Author(s):  
K. H. Ryu ◽  
J-M. Yang
Keyword(s):  
Electron Microscopy ◽  
Pressureless Sintering ◽  
Particle Sizes ◽  
X Ray Diffraction ◽  
X Ray ◽  
Sintering Additives ◽  
Different Temperatures ◽  
Si3n4 Ceramics ◽  
Scanning Electron ◽  
Microstructural Control

The low temperature pressureless sintering of a nanosized Si3N4 powder with doped sintering additives was investigated. The microstructural evolution during sintering at different temperatures was analyzed using x-ray diffraction and scanning electron microscopy. The effect of using nanosized Si3N4 powder as a catalyst to accelerate the α→β–Si3N4 transformation of a commercial Si3N4 powder with larger particle sizes was also investigated. Finally, two stage sintering was used to study the feasibility of controlling the microstructure and the mechanical properties of the nanosized silicon nitride.

Nanocrystalline Barium Zirconium Titanate Synthesized by the Sonochemical Process

2013 ◽  
Vol 802 ◽  
pp. 119-123
Author(s):  
Supamas Wirunchit ◽  
Rangson Muanghlua ◽  
Supamas Wirunchit ◽  
Wanwilai Vittayakorn ◽  
Naratip Vittayakorn
Keyword(s):  
Crystal Structure ◽  
Electron Microscopy ◽  
Reaction Time ◽  
Single Phase ◽  
Zirconium Titanate ◽  
X Ray Diffraction ◽  
X Ray ◽  
Large Particles ◽  
Barium Zirconium Titanate ◽  
Scanning Electron

Nanocrystalline barium zirconium titanate, BaZr0.4Ti0.6O3, was synthesized successfully via the sonochemical process. The effects of reaction time on the precipitation of Ba(Zr,Ti)O3 particles were investigated briefly. The crystal structure as well as molecular vibrations and morphology were investigated. X-ray diffraction indicated that the powders exhibited a single phase perovskite structure, without the presence of pyrochlore or unwanted phases at the reaction time of 60 min. Nanocrystals were formed before being oriented and aggregated into large particles in aqueous solution under ultrasonic irradiation. A scanning electron microscopy (SEM) photograph showed the BZT powder as spherical in shape with uniform nanosized features.

Reactivity in the chromium oxide-calcium fluoride system: An empirical approach

1999 ◽  
Vol 14 (6) ◽  
pp. 2518-2523
Author(s):  
Frans Vos ◽  
Luc Delaey ◽  
Marc De Bonte ◽  
Ludo Froyen
Keyword(s):  
Electron Microscopy ◽  
Thermal Analysis ◽  
Calcium Fluoride ◽  
Reaction Mechanisms ◽  
Sintering Temperature ◽  
X Ray Diffraction ◽  
Powder Mixtures ◽  
Reaction Behavior ◽  
X Ray ◽  
Scanning Electron

The reaction mechanisms observed when sintering loose Cr2O3–CaF2 powder mixtures were analyzed, and the influence of the sintering parameters on the reaction behavior is presented. Using x-ray diffraction (XRD), energy-dispersive spectroscopy (EDS), and differential thermal analysis (DTA) measurements, CaCrO4 was shown to be the reaction product when sintering in air. The reaction occurs in two steps: CaF2 transforms to CaO at the Cr2O3–CaF2 interface, followed by a CaO–Cr2O3 interaction, which creates the reaction product. Scanning electron microscopy (SEM) and x-ray fluorescence (XRF) analysis showed an increasing loss of CaF2 with increasing sintering temperature and heating rate, while an opposite evolution of the amount of reaction product was observed.

Influence of Annealing Time on Microstructure of Ni-W Alloys

2013 ◽  
Vol 747-748 ◽  
pp. 613-618
Author(s):  
Qiao Zhang ◽  
Shu Hua Liang ◽  
Chen Zhang ◽  
Jun Tao Zou
Keyword(s):  
Electron Microscopy ◽  
Solid Solution ◽  
Grain Size ◽  
Grain Boundaries ◽  
Annealing Time ◽  
Single Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Average Grain Size ◽  
Scanning Electron

The as-cast Ni-W alloys with 15wt%W, 25wt%W and 30wt%W were annealed in hydrogen at 1100. The effect of the annealing time on the microstructure of Ni-W alloys was studied, and the phase constituents and microstructure of annealed Ni-W alloys were characterized by the X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results showed that no any phase changed for Ni-15%W, Ni-25%W and Ni-30%W alloys annealed for 60 min, 90 min and 150 min, which were still consisted of single-phase Ni (W) solid solution. However, microstructure had a significant change after annealing. With increase of annealing time, the microstructure of Ni-15%W alloy became more uniform after annealing for 90 min, and the average grain size was 95μm, whereas the grain size of Ni-15%W alloy increased significantly after annealing for 150 min. For Ni-25%W and Ni-30%W, there was no obvious change on the grain size with increase of annealing time, and the amount of oxides at grain boundaries gradually reduced. After annealing for 150 min, the impurities at grain boundaries almost disappeared. Subsequently, the annealing at 1100 for 150 min was beneficial for the desired microstructure of Ni-25%W and Ni-30%W alloys.

Synthesis, Phase Formation and Characterization of Co4Nb2O9 Powders Synthesized by Solid-State Reaction

2008 ◽  
Vol 55-57 ◽  
pp. 873-876 ◽  
Author(s):  
N. Chaiyo ◽  
R. Muanghlua ◽  
A. Ruangphanit ◽  
Wanwilai C. Vittayakorn ◽  
Naratip Vittayakorn
Keyword(s):  
Electron Microscopy ◽  
Solid State ◽  
Solid State Reaction ◽  
Dwell Time ◽  
Single Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Xrd Techniques ◽  
Scanning Electron

A corundum-type structure of cobalt niobate (Co4Nb2O9) has been synthesized by a solid-state reaction. The formation of the Co4Nb2O9 phase in the calcined powders was investigated as a function of calcination conditions by differential thermal analysis (DTA) and X-ray diffraction (XRD) techniques. Morphology and particle size have been determined by scanning electron microscopy (SEM). It was found that the minor phases of unreacted Co3O4 tend to form together with the columbite CoNb2O6 phase at a low calcination temperature and short dwell time. It seems that the single-phase of Co4Nb2O9 in a corundum phase can be obtained successfully at the calcination conditions of 900°C for 60 min, with heating/cooling rates of 20°C /min.

Crystal Structure of BiFeO3 Synthesized Using the Hydrothermal Processing

2014 ◽  
Vol 602-603 ◽  
pp. 947-950
Author(s):  
Zhen Wang ◽  
Hai Yan Chen ◽  
Lin Qiang Gao ◽  
Xin Zou
Keyword(s):  
Crystal Structure ◽  
Electron Microscopy ◽  
Thermal Analysis ◽  
Scanning Electron Microscopy ◽  
Single Phase ◽  
Hydrothermal Processing ◽  
Optimal Conditions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Scanning Electron

BiFeO3 nanoparticles were successfully synthesized by a hydrothermal method by a mineralizer (KNO3). Structural characterization was performed by thermal analysis, powder X-ray diffraction (XRD) and scanning electron microscopy (TEM).The results showed that the products were perovskite structure BiFeO3 powders. Optimal conditions for the synthesis of single-phase BiFeO3 ceramics were obtained.

FABRICATION AND CHARACTERISTICS OF ALN NANOWIRES

2001 ◽  
Vol 15 (30) ◽  
pp. 1455-1458 ◽  
Author(s):  
H. CHEN ◽  
X. K. LU ◽  
S. Q. ZHOU ◽  
X. H. HAO ◽  
Z. X. WANG
Keyword(s):  
Crystal Structure ◽  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Single Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Selected Area Electron Diffraction ◽  
Transmission Electron ◽  
Sublimation Method ◽  
Scanning Electron

Single phase AlN nanowires are fabricated by a sublimation method. They were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), typical selected area electron diffraction (SAED) and high-resolution transmission electron microscopy (HRTEM). The SEM and TEM images show that most of the nanowires have diameters of about 10–60 nm. The crystal structure of AlN nanowires revealed by XRD, SAED and HRTEM shows the AlN nanowires have a wurtzite structure.

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