Pressureless Sintering of MoSi2 Materials

1994 ◽  
Vol 364 ◽  
Author(s):  
Roland Scholl ◽  
Thomas JÜngling ◽  
Bernd Kieback

AbstractVarious powder mixtures were prepared by a modified mechanical alloying technique. Starting from elemental Mo-, Si- and C-powders the influence of milling conditions on phase formation during the milling process and the subsequent heat treatment was investigated. Phase formation during sintering and sintering kinetics of activated starting mixtures were studied by differential scanning calorimetry (DSC), thermal graphimetry (TG), X-ray diffraction (XRD) and dilatometry. The results show that phase formation during milling or sintering strongly depends on milling conditions. Optimized powder mixtures of single phase and reinforced molybdenum silicides show high densities up to 98,5 % TD by pressureless sintering in various atmospheres. Full density is possible by post-HIP because the samples show only closed porosity. The microstructure was studied in dependence of sintering parameters. The level of impurities, i.e. C, O2 was determined. Hardness, fracture toughness and bending strength were measured for single phase and particle reinforced materials.

2012 ◽  
Vol 512-515 ◽  
pp. 676-680 ◽  
Author(s):  
Liang Li ◽  
Ai Guo Zhou ◽  
Li Bo Wang ◽  
Fei Xiang Hu

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.


2015 ◽  
Vol 817 ◽  
pp. 96-103
Author(s):  
Wei Ping Fang ◽  
Yao Yong Yi ◽  
Feng Mei Liu ◽  
Zheng Lin Liu ◽  
Zhen Hua Deng

A silver free amorphous Cu-35Ti-12Ni active brazing alloy was successfully prepared in this work. The crystallinity, microstructure, and chemical composition were characterized with X-ray diffraction (XRD), scanning electron microscope (SEM), and energy-dispersive spectrometry (EDS), respectively. A typical characteristic peak of amorphous material was observed in the XRD pattern. The microstructures and chemical compositions of the silver free amorphous alloy were uniform. Differential scanning calorimetry (DSC) result shows that the amorphous silver free brazing alloy has higher melting temperature than commercial silver brazing alloy (Ag-26.5Cu-1.5Ti). Wetting contact angle and spreading area on Si3N4 ceramic substrate were used to evaluate the wetting ability of brazing alloy. The wetting angle was smaller than 5o, and the spreading area was 141.6 mm2 at 1100°C. The bending strength of silver free brazing alloy/Si3N4 was also carried out. The mechanical test shows that the amorphous Cu-35Ti-12Ni/Si3N4 has higher joint strength (304.7MPa) than the crystal Cu-35Ti-12Ni/Si3N4 (294.7MPa) at room temperature.


2020 ◽  
Vol 856 ◽  
pp. 190-197
Author(s):  
Pornsit Chaiya ◽  
Thawatchai Phaechamud

Compatibility investigation was performed between magnesium stearate and acidic drug compounds (ibuprofen, indomethacin and valproic acid) and acidic pharmaceutical excipients (lactic acid and citric acid) using differential scanning calorimetry (DSC). DSC study indicated the possible incompatibility for the mixture between magnesium stearate and any compounds. Alteration in DSC thermogram was found in all mixtures. The eutectic phenomenon was found in the powder mixture of magnesium stearate and ibuprofen. In addition, the presence of melting endothermic peak of stearic acid in other powder mixtures except the mixture of magnesium stearate and indomethacin indicating breakage of salt form of magnesium stearate. This alteration could relate to the influence on physicochemical properties of drug compounds and pharmaceutical excipients which powder x-ray diffraction (PXRD) and Fourier Transform Infrared Spectroscopy (FT-IR) should be further analyzed to confirm the interactions between compounds.


2011 ◽  
Vol 412 ◽  
pp. 263-266
Author(s):  
Hong Wei Zhang ◽  
Li Li Zhang ◽  
Feng Rui Zhai ◽  
Jia Jin Tian ◽  
Can Bang Zhang

The higher mechanical strength of Al87Ce3Ni8.5Mn1.5 nanophase amorphous composites has been obtained with two methods. The first nanophase amorphous composites are directly produced by the single roller spin quenching technology. The method taken for the second nanophase amorphous composites is at first to obtain amorphous single-phase alloy, followed by annealed at different temperatures .The formative condition, the microstructure, the particle size, the volume fraction of α-Al phase and microhardness of nanophase amorphous composites etc have been investigated and compared by X-ray diffraction (XRD) and transmission electron microscopy (TEM) and differential scanning calorimetry (DSC). The microstructure of composites produced by the second method is higher than the former, the fabricated material structure of the system is more uniform and the process is easier to control.


Proceedings ◽  
2018 ◽  
Vol 2 (23) ◽  
pp. 1407
Author(s):  
Serkan Abalı ◽  
Cem Uğur Karaçam

In the scope of this study, a powder mixture was prepared that contained 3 Al2O3-Y2O3 consisting of 99.99% pure Al2O3 and aluminum oxide of 65–67% and 70% by weight of 99.999% pure Y2O3 powders. After the powders were weighed on a precision scale, the milling process was carried out in a vibratory disc mill. For the granulation, 3 powder mixtures that were subject to sintering were sieved to a size of less than 106 µm in a powder sieve shaker. The powders were shaped with a cold isostatic press after this step and the 3 acquired samples were sintered for 12 h under a temperature of 1923 K. Selected physical and mechanical behaviors were taken by evaluating microhardness measurements, bending strength XRD analysis and electron microscope images of the 3 sintered samples. The changes in the Y2O3 additive and phase composition, microstructure, and mechanic properties were examined.


2011 ◽  
Vol 172-174 ◽  
pp. 646-651 ◽  
Author(s):  
Gamra Tellouche ◽  
Khalid Hoummada ◽  
Dominique Mangelinck ◽  
Ivan Blum

The phase formation sequence of Ni silicide for different thicknesses is studied by in situ X ray diffraction and differential scanning calorimetry measurements. The formation of a transient phase is observed during the formation of δ-Ni2Si; transient phases grow and disappear during the growth of another phase. A possible mechanism is proposed for the transient phase formation and consumption. It is applied to the growth and consumption of θ-Ni2Si. A good accordance is found between the proposed model and in situ measurement of the kinetics of phase formation obtained by x-ray diffraction and differential scanning calorimetry for higher thickness.


1997 ◽  
Vol 12 (1) ◽  
pp. 133-146 ◽  
Author(s):  
K. Barmak ◽  
C. Michaelsen ◽  
G. Lucadamo

We have investigated reactive phase formation in magnetron sputter-deposited NiyAl multilayer films with a 1 : 3 molar ratio and various periodicities, L, ranging from 320 nm down to a codeposited film with zero effective periodicity. The films were studied by x-ray diffraction, differential scanning calorimetry, electrical resistance measurements, and transmission electron microscopy. We find that Ni and Al have reacted during deposition to form the B2 NiAl phase and an amorphous phase. The formation of these phases substantially reduces the driving force for subsequent reactions and explains why nucleation kinetics become important for these reactions. Depending on the periodicity, these reactions result in the formation of NiAl3 or Ni2Al9 followed by NiAl3. Detailed calorimetric analysis reveals differences in the nucleation and growth behavior of NiAl3 compared with other studies.


2011 ◽  
Vol 412 ◽  
pp. 271-274
Author(s):  
Ying Li ◽  
Qiang Xu ◽  
Ling Dai

In order to prepare ultrafine La3NbO7 powder, a potential material for thermal barrier coatings, the calcination process of La3NbO7 was studied in this paper.The precursor of La3NbO7 was synthesized by using a citric acid complex method. A calcination process had been systematically investigated. The reaction temperature was determined by differential scanning calorimetry (DSC). The phase composition of powders was characterized by X-ray diffraction (XRD), and the morphology was obtained by scanning electron microscope (SEM). The results revealed that the single-phase La3NbO7 powder could be successfully prepared while the calcination temperature exceeded 800°C and a better morphology could be maintained at 800°C for 4 hours. Considering all above, an optimum calcination scheme was adopted at 800°C for 4 hours. The as-prepared La3NbO7 powders had a grain size of about 50nm and an average particle size of about 300nm.


2008 ◽  
Vol 23 (11) ◽  
pp. 2880-2885 ◽  
Author(s):  
Herbert Willmann ◽  
Paul H. Mayrhofer ◽  
Lars Hultman ◽  
Christian Mitterer

Microstructure and hardness evolution of arc-evaporated single-phase cubic Al0.56Cr0.44N and Al0.68Cr0.32N coatings have been investigated after thermal treatment in Ar atmosphere. Based on a combination of differential scanning calorimetry and x-ray diffraction studies, we can conclude that Al0.56Cr0.44N undergoes only small structural changes without any decomposition for annealing temperatures Ta ⩽ 900 °C. Consequently, the hardness decreases only marginally from the as-deposited value of 30.0 ± 1.1 GPa to 29.4 ± 0.9 GPa with Ta increasing to 900 °C, respectively. The film with higher Al content (Al0.68Cr0.32N) exhibits formation of hexagonal (h) AlN at Ta ⩾ 700 °C, which occurs preferably at grain boundaries as identified by analytical transmission electron microscopy. Hence, the hardness increases from the as-deposited value of 30.1 ± 1.3 GPa to 31.6 ± 1.4 GPa with Ta = 725 °C. At higher temperatures, where the size and volume fraction of the h-AlN phase increases, the hardness decreases to 27.5 ± 1.0 GPa with Ta = 900 °C.


2008 ◽  
Vol 368-372 ◽  
pp. 995-997
Author(s):  
Cui Wei Li ◽  
Hong Xiang Zhai ◽  
Yang Zhou ◽  
Shi Bo Li ◽  
Zhi Li Zhang

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.


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