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.

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.

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.

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).

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.

Self-propagating fabrication of 3D porous MXene-rGO film electrode for high-performance supercapacitors

2D MXene nanosheets with metallic conductivity and high pseudo-capacitance are promising electrode materials for supercapacitors.Especially,MXene films can be directly used as electrodes for flexible supercapacitors.However,they suffer from sluggish ion transport due to self-restacking,causing limited electrochemical performance.Herein,a flexible 3D porous MXene film is fabricated by incorporating graphene oxide(GO) into MXene film followed by self-propagating reduction.The self-propagating process is facile and effective,which can be accomplished in 1.25 s and result in 3D porous framework by releasing substantial gas instantaneously.As the 3D porous structure provides massive ion-accessible active sites and promotes fast ion transport,the MXene-rGO films exhibit superior capacitance and rate performance.With the rGO content of 20%,the MXene-rGO-20 film delivers a high capacitance of 329.9 F g^(-1) at 5 mV s^(-1) in 3 M H2 SO4 electrolyte and remains 260.1 F g^(-1) at 1,000 mV s^(-1) as well as good flexibility.Furthermore,the initial capacitance is retained above 90% after 40,000 cycles at 100 A g^(-1),revealing good cycle stability.This work not only provides a high-performance flexible electrode for supercapacitors,but also proposes an efficient and time-saving strategy for constructing 3D structure from 2D materials.

Thermodynamic Study on Self-propagating High Temperature Synthesis of TiB2/Fe Composites

Based on the experimental analysis and theoretical calculation, the self-propagating high temperature synthesis of TiB2/Fe composite was studied. The experimental results show that the interfacial between TiB2 and Fe was smooth and clear, and the composite bending strength increased with the addition of Fe, however, the hardness decreased accordingly. The thermodynamics of the composites preparation process was calculated. The calculation results show that the primary chemical reaction was the reaction between Ti and B. The extra B can react with Fe, producing the brittle phase Fe2 B. By increasing Ti, the production of Fe2B will decrease and a few of Ti-Fe intermetallic compound will be produced by the reaction between Ti and Fe in the composites. Finally, according to the Merzhanov condition of the adiabatic system, it is concluded that the Fe content must be selected between 16.3% and 54.3% by the thermodynamics temperature of reaction calculation.

Reaction mechanism of self-propagating magnesiothermic reduction of ZrB_2 powders

Fine zirconium diboride （ZrB2） powders with high purity were successfully prepared by combustion synthesis through magnesiothermic reduction process in Mg-B2O3-ZrO2 system. The reaction mechanism was investigated by differential thermal analysis and quenching experiment. The results show that the whole magnesio-thermic reduction process includes three stages： first, molten B2O3 and Mg formed above the temperature of 650 ℃, and glassy B2O3 and solid ZrO2 particles were coated on the surface of the molten Mg; thus, the hollow balls can be formed when the molten Mg was exuded under capillary function. Second, ZrO2 particles reacted with molten Mg to form Zr and MgO with dissolution-precip-itation mechanism, which released a large amount of heat to induce the diffusion reaction between B203 and Mg to form B and MgO. Last, Zr reacted with B to form ZrB2 grains. The preparation of ZrB2 by self-propagating syn-thesis in Mg-B2O3-ZrO2 system is a solid-liquid-liquid reaction.

Characterizations and Photocatalytic Activities of Nanocrystalline MTiO_3 (M=Sr, Pb, Co) Prepared via a General Self-propagating Combustion Method

Nanocrystalline MTiO3 （M = St, Pb, Co） were prepared by a general self-pro- pagating combustion method. The samples were characterized by X-ray diffraction （XRD） analysis, scanning electron microscopy （SEM）, transmission electron microscopy （TEM）, N2 adsorption and UV-vis diffuse reflectance spectra （DRS）. The photocatalytic activity of MTiO3 （M = Sr, Pb, Co） was evaluated by the photocatalytic degradation of methyl orange （MO）. MTiO3 （M = Sr, Pb, Co） having the same core element showed distinctly different photocatalytic activity due to the different coordinating atoms. Factors affecting the photocatalytic activity of MTiO3 （M = Sr, Pb, Co） were discussed. It was suggested that the structures of TiO6 octahedra and the electronic property were the predominant factors of the photocatalytic behavior for MTiO3 （M = Sr, Pb, Co）.

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%.

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.

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.

Synthesis Mechanism and Material Characterization of C4AF Obtained by the Self-propagating Combustion Reaction Method

To investigate the influence of preparation process on the properties of synthesized C4AF,the powder was prepared via the self-propagating combustion reaction（SPCR）method using urea as fuel and metal nitrates as cation precursors.Synthesis mechanism of the SPCR method,calculation and adjusting principles of urea dosage were detailedly introduced.Material characterization of synthesized C4AF was performed with the aid of X-ray diffractometry,Fourier transform infrared spectrometry,scanning electron microscopy,energydispersive X-ray spectroscopy,^27Al nuclear magnetic resonance and isothermal microcalorimetric technique.Remaining content of transition phase of calcium carbonate in synthesized C4AF was determined by quantitative analysis of X-ray diffractometry.It was found that there was no difference in the hydration behavior of C4AF synthesized by the SPCR method and the traditional solid-state reaction（SSR）method.C3AH6 and amorphous iron（III）hydroxide（Fe（OH）3）would be formed during the hydration of C4AF while CH not.Crystallite size of synthesized C4AF was 16.1 A and the apparent activation energy was 36.2 kJ/mol.Coordinated condition of Al in C4AF can be detected by ^27Al NMR technique,but the peaks were broadened and the intensities were relatively low,supporting the use of ^27Al NMR for the quantitative analysis of C3A in Portland cements.

Ultra-fast synthesis and thermodynamic analysis of MoAlB by self-propagating high-temperature combustion synthesis

MoAlB as a typical member of MAB phases has attracted much-growing attention due to its unique properties.However,the low production of MoAlB powders limits its further development and potential applications.In the present work,the ultra-fast preparation of high-purity MoAlB powders in a few seconds is achieved by self-propagating high-temperature synthesis(SHS)using a raw powder mixture at an atomic ratio of Mo:Al:B=1:1.3:1.SHS reaction mechanism is obtained by analyzing the corresponding composition changes of starting materials.Furthermore,the thermodynamic prediction for the SHS reaction is consistent with the present experiments,where the preparation of MoAlB also conforms to two common self-propagating conditions of the SHS.The enthalpy vs.temperature curve shows that the adiabatic temperature of the reaction decreases with the amount of excuse Al increasing but increases when pre-heating the reactants.Also,this thermodynamic calculation provides a new idea for the preparation of other MAB phases by the SHS.

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.

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.

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.

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.

Optimal design of self-propagating high temperature one-dimensional nano-SnO_2 synthesis

The success in synthesizing high purity SnO2 nanobelts via self-propagating high tem- perature synthesis was achieved. According to the experimental results, a relationship between the residual heat of the reaction system at 2848 K and SnO2 nanobelts yield was identified. The most appropriate formula for this self-propagating high tempera- ture synthesis method is turned out to be composed of Sn powder and thermite with weight ratio of 1：1.

Structural,magnetic and dielectric properties of nano-crystalline Ni-doped BiFeO_(3) ceramics formulated by self-propagating high-temperature synthesis

Ni-doped BiFeO_(3) powders with the composition BiFe_(1-x)Ni_(x)O_(3)(x=0.05,0.1 and 0.15)were prepared by a self-propagating high-temperature synthesis(SHS),using metal nitrates as oxidizers and glycine as fuel.The X-ray diffraction(XRD)patterns depict that Ni-doped BiFeO_(3) ceramics crystallize in a rhombhohedral phase.The scanning electron micrographs of Ni-doped BiFeO_(3) ceramics show a dense morphology with interconnected structure.It is found that,the room-temperature magnetization measurements in Ni-incorporated BiFeO_(3) ceramics give rise to nonzero magnetization.The magnetization of Ni-doped BiFeO_(3) ceramics is significantly enhanced when Ni doping concentration reaches to x=0.1 at 5 K.The variations of dielectric constant with temperature in BiFe_(0.95)Ni_(0.05)O_(3),BiFe_(0.9)Ni_(0.1)O_(3) and BiFe_(0.85)Ni_(0.15)O_(3) samples exhibit clear dielectric anomalies approximately around 450℃,425℃and 410℃respectively,which correspond to antiferromagnetic to paramagnetic phase transition of the parent compound BiFeO_(3).