SELF- PROPAGATING HIGH TEMPERATURE SYNTHESIS OF (W,Ti)C POWDERS

The effects of preheating temperature and W powder size on the Self propagating High temperature Synthesis(SHS) of Ti W C system were studied. Preheated mixtures and the decrease of W powder size can accelerate the formation of (W,Ti)C powders. The uniphase (W,Ti)C (WC∶TiC=5∶5) powders with 0.32% free carbon were synthesized from Ti, W, C powders by SHS. The powder size of the product was 3～5 μm.

Self-propagating High-temperature Synthesis, Microstructure and Mechanical Properties of TiC-TiB_2-Cu Composites

TiC-TiB2-Cu composites were produced by self-propagating high-temperature synthesis combined with pseudo hot isostatic pressing using Ti, B4C and Cu powders. The microstructure and mechanical properties of the composites were investigated. The X-ray diffraction （XRD） and scanning electron microscopy （SEM） results showed that the final products were only TiC, TiB2 and Cu phases. The clubbed TiB2 grains and spheroidal or irregular TiC grains were found in the microstructure of synthesized products. The reaction temperature and grain size of TiB2 and TiC particles decreased with increasing Cu content. The introduction of Cu into the composites resulted in a drastic increase in the relative density and flexual strength, and the maximum values were obtained with the addition of 20 wt pct, while the fracture toughness was the best when Cu content was 40 wt pct.

Preparation of Nano-sized Zirconium Carbide Powders through a Novel Active Dilution Self-propagating High Temperature Synthesis Method

High quality nano-sized zirconium carbide （ZrC） powders were successfully fabricated via a developed chemical active dilution self-propagating high-temperature synthesis （SHS） method assisted by ball milling pretreatment process using traditional cheap zirconium dioxide powder （ZrO2）, magnesium powder （Mg） and sucrose （C12H22Oll） as raw materials. FSEM, TEM, HRTEM, SAED, XRD, FTIR and Raman, ICP- AES, laser particle size analyzer, oxygen and nitrogen analyzer, carbon/sulfur determinator and TG-DSC were employed for the characterization of the morphology, structure, chemical composition and thermal stability of the as-synthesized ZrC samples. The as-synthesized samples demonstrated high purity, low oxygen content and evenly distributed ZrC nano-powders with an average particle size of 50nm. In addition, the effects of endothermic rate and the possible chemical reaction mechanism were also discussed.

Influence of Fe Addition on Products of Self-Propagating High-Temperature Synthesis Reaction in 3Ti-Si-2C System

Influence of Fe addition on products of self-propagating high-temperature synthesis (SHS) reaction in 3Ti-Si-2C system was investigated in the present study. Without Fe addition, Ti5Si3 and TiC are the dominant phases along with a small amount of Ti3SiC2 phase and unreacted C left in the final products. As Fe content ranges from 10% to 30%, the products consist of TiC, Ti5Si3, Fe2Ti and unreacted C, but no trace of Ti3SiC2 phase is detected. Furthermore, the amounts of both Fe2Ti and C phases increase with Fe content increasing. Addition of Fe has a great effect on the reaction route and significantly restrains the formation of Ti3SiC2 during the combustion synthesis process, and therefore, the SHS is not an effective fabrication technique to synthesize the ternary Ti3SiC2 ceramic in either 3Ti-Si-2C or Fe-3Ti-Si-2C system. Besides, without Fe addition, Ti5Si3 presents as the coarse irregular appearance with an obviously sintered morphology. In contrast, the shape of Ti5Si3 exhibits more and more spherical (cobblestone-like) and the surface becomes increasingly smooth, because the amount of liquids formed during the SHS reaction increases with the increase of Fe content. On the other hand, with Fe content increasing from 0 to 30 wt.%, the particulate size of TiC decreases from more than 5 μm to 1 μm or less, mainly due to the fact that the combustion temperature decreases with the increase of Fe content in the preforms.

Effect of inner oxidant on self-propagating high-temperature synthesis of MnZn-ferrite powder

Using KClO3 as an inner oxidant, MnZn-ferrite powder was synthesized by a self-propagating high-temperature synthesis (SHS) process in normal air atmosphere. The effects of the inner oxidant on combustion temperature, combustion velocity, microstructure and the phase of the product were investigated by XRD and SEM,respectively. The results show that a highly ferritized powder can be obtained as well as the highest combustion temperature and the highest combustion velocity when the inner oxidant content m equals 54(k-16).

Self-propagating high temperature synthesis of MoSi_2 matrix composites

MoSi2 is presently regarded as the most important material for electrical heating and as one with huge potential for high temperature structural uses. MoSi2 and MoSi2 matrix composites were prepared by self-propagating high temperature synthesis （SHS）. Pure MoSi2 was obtained and a compound of MoSi2 and WSi2was synthesized in the form of predominant solid solution （Mo,W）Si2. By adding aluminum of 5.5 at.% to Mo-Si, the crystal structure of MoSi2 changed into a mixture of tetragonal Cllb MoSi2and hexagonal C40 Mo（Si,Al）2. The （Mo,W）Si2-Mo（Si,Al）2-W（Si,Al）2 composite materials were synthesized by adding aluminum of 5.5 at.% to Mo-W-Si. However, if the amount of the added aluminum was not larger than 2.5 at.%, it did not have any significant effect. SHS is an effective technology for synthesis of MoSi2 and MoSi2 matrix composites.

Dissolution-precipitation mechanism of self-propagating high-temperature synthesis of TiC-Cu cermets

The mechanism of self-propagating high-temperature synthesis （SHS） of TiC-Cu cermets was studied using a combustion front quenching method. Microstructural evolution in the quenched sample was observed using scanning electron microscope （SEM） with energy dispersive X-ray （EDX） spectrometry, and the combustion temperature was measured. The results showed that the combustion reaction started with local formation of Ti-Cu melt and could be described with the dissolution-precipitation mechanism, namely, Ti, Cu, and C particles dissolved into the Ti-Cu solution and TiC particles precipitated in the saturated Ti-Cu-C liquid solution. The local formation of Ti-Cu melt resulted from the solid diffusion between Ti and Cu particles.

A Self-propagating high-temperature synthesis process for the fabrication of Fe（Cr）–Al2O3 nanocomposite

Self-propagating high-temperature synthesis(SHS)was used to fabricate a Fe(Cr)–Al2O3 nanocomposite.The composite was fabricated by the reactions between the powders of Fe,Fe2O3,Cr2O3,and Al.The effect of blending ratio and mechanical activation of the initial powders and the precursor compressing pressure on the microstructure of the final product was studied by optical microscopy,scanning electron microscopy,transmission electron microscopy,and X-ray diffraction.The significance of the effect of each of the aforementioned parameters on the quality of the composite(assessed by measuring the compressive strength and wear resistance)was determined using a full-factorial design of experiments method.The results showed that the best molar powder ratio that produced the most homogeneous product through a sustainable SHS reaction was Fe:Fe2O3:Cr2O3:Al=10:1:1:4.A lower Fe content caused the Fe(Cr)phase to melt and separate from the rest of the materials.

Preparation of ZrB_2 Ceramics by Self-propagating High-temperature Synthesis and Hot Pressing Sintering

ZrB2 ceramics were prepared by self-propagating high-temperature synthesis（SHS） and were sintered by hot pressing（HP）.The effects of the granularities and doses of raw materials in Zr-B2O3-Mgon SHS process and product were investigated.XRD and combustion temperature curves prove that the ideal SHS reactants of Zr-B2O3-Mg are 50μm Zr powder,75μm B2O3 powder and 400μm Mg powder with 45% excessive.The particle sizes of SHS product,acid-leached product,sintered product are 2-5μm,0.5-2μm,2-10μm respectively.Chemical analysis indicates that the acid-leached product consists of ZrB2（94.59%）,ZrO2（3.87%）,and H3BO3（1.54%）,The sintered product has a relative density of 95.4%.

ZrB_2/Al_2O_3 composite powders prepared by self-propagating high-temperature synthesis

Self-propagating high-temperature synthesis（SHS） method was used to synthesize ZrB2/Al2O3 composite powders from B2O3-ZrO2-Al system. X-ray diffractometry（XRD） and scanning electron microscopy（SEM） analyses show the presence of ZrB2 and Al2O3 as the primary phases in the composite powders, while the presence of a very small amount of ZrO2 is thought to be unreacted zirconium oxide. Transmission electron microscopy（TEM） and high resolution electron microscopy（HREM） observations of microstructure of the composite powders indicate that the interfaces of ZrB2/Al2O3 bond well without any interfacial reaction products. It is proposed that the good interfacial bonding of composite powders results from the ZrB2 particles crystallizing and growing on the Al2O3 particles surface with surface defects acting as nucleation centers.

Microstructural Evolution During Self-propagating High-temperature Synthesis of Ti-Al System

In order to investigate the microstructural evolution during self-propagating high-temperature synthesis （SHS） of Ti-Al powder mixture with an atomic ratio of Ti： Al=1：1, a combustion front quenching method （CFQM） was used for extinguishing the propagating combustion wave, and the microstructures on the quenched sample were observed with scanning electron microscope （SEM） and analyzed with energy dispersive spectrometry （EDS）. In addition, the combustion temperature of the reaction was measured, and the phase constituent of the synthesized product was inspected by X-ray diffraction （XRD）. The results showed that the combustion reaction started from melting of the Al particles, and the melting resulted in dissolving of the Ti particles and forming of Al3Ti grains. As the Al liquid was depleted, the combustion reaction proceeded through solid-state diffusion between the solid Al3Ti and the solid Ti. This led to the forming of TiAl and Ti3Al diffusing layers. In addition, the combustion reaction is incomplete besides TiAl, there are a large amount of Ti3Al and TiAl3 and a small amount of Ti in the final product. This incompleteness chiefly results from the using of coarser Ti powder.

Fabrication of Titanium Diboride-Cu Composite by Self-High Temperature Synthesis plus Quick Press

Titanium diboride based composites, good candidates for contact materials, have high hardness, Young＇s modulus, high temperature stability, and excellent electrical, thermal conductivity. However a good interface of TiB2/Cu is very difficult to achieve for oxidation of TiB2. To avoid this oxidation behavior, the in situ combusting synthesis technology, SHS, was used to prepare TiB2/Cu composite. The characters of Ti-B-xCu SHS were studied in detail, such as combustion temperature, products phases and grain size. Based on the experimental results a proper technology way of self-high temperature synthesis plus quick press （SHS/QP） was determined and compact TiB2/Cu composites with relative density over than 97 pct of the theoretical were fabricated by this method. The properties and microstructures of these TiB2 based composites were also investigated.

SHS制备高熵合金块体及表征凝固组织

利用自蔓延高温合成技术(SHS)制备高熵合金,即以三氧化二铬、三氧化二铁、三氧化二钴、氧化镍、二氧化钛粉末及铝粉为试验原料。确定了反应物质量配比后均匀混合,并用镁条将其点燃,此时铝热反应立即开始,反应凭借自身持续放热迅速合成所需材料。表征铸态高熵合金与经热轧后合金的组织差异性,同时也为消除铸态块体中的空隙而对合金进行热轧处理。结果表明:高熵合金在经过热变形后获得了部分板织构,因此热轧态合金比铸态合金的晶粒尺寸大。其次讨论了SHS技术在实际应用中的特点、合金的微观组织与元素成分占比。

Synthesis of SrTiO_3 for immobilization of simulated HLW by SHS

Strontium titanate synroc samples were synthesized by self-propagating high-temperature synthesis （SHS）. Sr directly took part in the synthesis process. As a result, the loading content issue is basically resolved. The products were characterized by density, microhardness X-ray diffraction, and scanning electron microscopy （SEM/EDS）. The leaching rate was measured by the method of PCT （product consistency test）. The results indicate that the Sr^2＋-SrTiO3 compound is of high density, low leach rate and high stability and the synthesis process is feasible in technology and economy. It can be concluded that the strontium titanate synroc is a perfect material to immobilize HLW.

CALCULATION OF ADIABATIC TEMPERATURE THROUGH COMPUTER PROGRAM IN PROCESS OF COMBUSTION SYNTHESIS

The adiabatic temperature in the process of self-propagating high temperature synthesis iscalculated through FOXBASE language program on the base of establishing thermodynamic datapool concerned.The adiabatic temperature of some common self-propagating high temperaturesynthesis has been calculated,and the computed results are compared with the adiabatic tempera-ture reported.At the same time,the curve about the influence of preheating temperature andadding diluent on Tadis drawn as an example.

Influences of Ignition Temperature, Urea-to-Metal Nitrates Molar Ratio, and Further Calcination on Synthesis of C_4AF via the SPCR Method

The self-propagating combustion reaction（SPCR）method was employed to synthesize C4AF using metal nitrates as cation precursors and urea as fuel.Thermal decomposition behavior of dried gels,phase identification and crystallinity of synthesized C4AF,and impact of urea to metal nitrates（UR/MN）molar ratio on synthesis effect were investigated with the aid of differential thermogravimetric analysis,X-ray diffraction and Fourier transform inferred spectrometry.It is found that pure C4AF can be prepared by the SPCR method in 2 h at 500℃.The UR/MN molar ratio plays a significant role in the thermal decomposition behavior of dried gel,purity,crystallinity and crystallite size of synthesized C4AF.Ignition temperature should be not lower than 500℃but higher temperatures were unnecessary.No trace of free lime in synthesized C4AF is detected and calcium carbonate is the transition phase.Further calcining the synthesized C4AF at high temperatures is beneficial for increasing crystallinity,purity and crystallite size.Reaction activation energy of the further calcination process is 119.6 kJ/mol.It is more efficient to improve the synthesis effect by increasing UR/MN molar ratio than further calcination at high temperatures.

Kinetics and numerical simulation of self-propagating high-temperature synthesis in Ti–Cr–Al–C systems

In this paper, Ti–Cr–Al–C materials were investigated by self-propagating high-temperature synthesis（SHS） according to the experimental study and numerical simulation results. The highest adiabatic combustion temperature Tadof 2,467.45 K indicates that the2Ti–0Cr–Al–C is the highest exothermic reaction system in the Ti–Cr–Al–C system. The adiabatic combustion temperature decreases with the increase of the Cr content. And a higher exothermal reaction would result in higher porosity which is induced by the high temperature and pressure of C reducing atmosphere and Al vapor. Combustion characterization of the products shows that the geometrical alternating layers result in the high exothermal reaction and flame-front propagating velocity. The higher the Tadis, the thinner the layer is. To demonstrate the process of the microscopic characterization and show the detailed combustion process closed to the experimental observations, the flame-front propagating velocity and temperature distribution were simulated numerically.

Self-propagating high-temperature synthesis of ZrO_2 incorporated Gd_2Ti_2O_7 pyrochlore

In this research, Zr-doped Gd_2Ti_2O_7 pyrochlores, with the composition of Gd_2(Ti_(1-x)Zr_x)_2O_7, were firstly synthesized by self-propagating high-temperature synthesis plus quick pressing(SHS/QP) using CuO as the oxidant and Ti as the reductant. To improve the radiation resistance of titanate–pyrochlore, up to 35 at% Zr was incorporated to substitute the Ti site of Gd_2Ti_2O_7 pyrochlore(Gd_2(Ti_(0.75)Zr_(0.35))_2O_7). XRD and SEM microstructural characterizations showed the formation of a composite ceramic with the major pyrochlore phase and the minor Cu phase. The generated temperature of samples decreased from 1702to 1011 ℃ with increasing Zr content. The effects of sintering temperature and pressure time on phase composition and microstructure were systematically studied. Besides, the influence of thermal transmission on the whole combustion process was also explored. The pyrochlore-based waste form possessed high bulk density of 6.25 g/cm^3 and Vickers hardness of 10.81 GPa. The MCC-1 leaching test showed the normalized elemental leaching rates(42d) of Cu, Gd, and Zr are 1.27×10^(-2), 1.33×10^(-3), and 8.44×10^(-7)g·m^(-2)·d^(-1), respectively.

High-efficiency Joining of C_f/Al Composites and TiAl Alloys under the Heat Effect of Laser-ignited Self-propagating High-temperature Synthesis

The aim of this study was to develop a high-efficiency joining method of Cf/Al composites and TiA l alloys under the heat effect of laser-ignited self-propagating high-temperature synthesis（SHS）. The SHS reaction of Ni–Al–Zr interlayer was induced by laser beam and acted as local high-temperature heat source during the joining. Sound joint was obtained and verified the feasibility of this joining method. Effect of filler metals on the joint microstructure and shear strength was evaluated. When the joining pressure was 2 MPa with additive filler metals, joint shear strength reached the maximum of 41.01 MPa.

Sintering behavior of aluminum nitride powder prepared by self-propagating high-temperature synthesis method

Fully dense aluminum nitride(AIN) ceramics were synthesized by self-propagating high-temperature synthesis(SHS) method using AIN powder as raw material with Y2O3additive. The sintering behavior was studied at different sintering temperatures and additive contents. The change of phase compositions, secondary phase distributions and grain morphologies during sintering process were investigated. It is shown that fully dense ceramics using AIN powder prepared by SHS method can be obtained when the sintering temperature is above 1830 ℃. Both Y2O3content and sintering temperature have an important influence on the formation of Y-Al-O phase and grain shape. When Y2O3content is identified, the grain morphology converts from polyhedron into sphere-like shape with the rise of sintering temperature. At a certain sintering temperature,the grain size decreases with the increase in Y2O3content. The influencing mechanisms of different YAl-O secondary phases and sintering temperatures on the grain size and morphology were also discussed based on the experimental results.