高岭土在碳热还原氮化过程中的相变

系统研究了苏州高岭土碳热还原氮化合成SiAlON过程在不同温度下的相变。对试样的XRD、SEM以及EDXA分析结果表明 ,1 30 0℃之前 ,试样中没有氮化物生成 ,物相为莫来石、石英和方石英 ;1 30 0℃时 ,高岭土开始发生氮化反应 ,生成过渡型SiAlON和β SiAlON。此时 ,石英和方石英相基本消失 ;1 4 0 0℃时 ,过渡型SiAlON、β SiAlON和X SiAlON三相共存 ,β SiAlON有所增多并有少量刚玉相生成 ;从 1 4 50℃到 1 550℃ ,Z值为 3的β SiAlON成为惟一的氮化产物 ,与少量SiC和刚玉相并存。莫来石在 1 50 0℃时完全消失     

Carbothermal nitridation process of mechanically milled silica sand using Taguchi's method

This paper reported on the work performed to study the formation of silicon nitride and silicon carbide whiskers using the carbothermal nitridation process. A distinctive aspect of the present study lies in the use of the mechanical milling method to alter the regularity of the crystalline network of the silica sand. In order to optimise the processing parameters for the synthesis of silicon carbide, the concept of Taguchi's Design of Experiments was considered, the analysis being based on Taguchi's signal to noise ratio and variance techniques to obtain optimum combination of process parameters. Important factors influencing the formation of silicon carbide were the duration of the mechanical milling, followed by temperature, time and heating rate.     

Synthesis of ultra-fine hafnium carbide powders combining the methods of liquid precursor conversion and plasma activated sintering

Ultra-fine hafnium carbide (HfC) powders were synthesized using a novel method combining liquid precursor conversion and plasma activated sintering (PAS). Solution-based processing was used to achieve a fine-scale mixing of the reactants, and further treatment by PAS allowed fast formation of HfC. We investigated the effect of the type of acid used during the liquid precursor conversion on the synthesized powders, where mixtures were prepared using salicylic acid, citric acid, or a combination of these. The results show that pure HfC powders (with an average particle sizes of 350 nm) were obtained at a relatively low temperature (1550 °C) using a HfOCl₂·8H₂O precursor with the mixed acids. The oxygen content of the synthesized powders was only 0.97 wt%. The type of acid had a significant effect on the synthesis product. When using only citric acid, the temperature required to produce pure hafnium carbide increased to 1700 °C. In the case of a salicylic acid precursor, pure HfC was not obtained, even at a synthesis temperature of 1700 °C.     

Highly transparent AlON ceramics sintered from powder synthesized by carbothermal reduction nitridation

Aluminum oxynitride (AlON) powders were synthesized by the carbothermal reduction and nitridation process using commercial γ-Al₂O₃ and carbon black powders as starting materials. And AlON transparent ceramics were fabricated by pressureless sintering under nitrogen atmosphere. The effects of ball milling time on morphology and particle size distribution of the AlON powders, as well as the microstructure and optical property of AlON transparent ceramics were investigated. It is found that single-phase AlON powder was obtained by calcining the γ-Al₂O₃/C mixture at 1550 °C for 1 h and a following heat treatment at 1750 °C for 2 h. The AlON powder ball milled for 24 h showed smaller particles and narrower particle size distribution compared with the 12 h one, which was benefit for the improvement of optical property of AlON transparent ceramics. With the sintering aids of 0.25 wt% MgO and 0.04 wt% Y₂O₃, highly transparent AlON ceramics with in-line transmittance above 80% from visible to infrared range were obtained through pressureless sintering at 1850 °C for 6 h.     

Fabrication and microstructure of 3D Cf /ZrC-SiC composites: through RMI method with ZrO2 powders as pore-making agent

3D C_f/ZrC–SiC composites were prepared by a combination process of slurry infiltration and reactive melt infiltration. ZrO₂ powders and ZrSi₂ alloy, both of which reacted with amorphous carbon, were used as pore-making agent and infiltrator, respectively. After carbothermal reduction at 1650 °C, X-ray diffraction analysis revealed that ZrO₂ powders were completely converted into ZrC by reacting with amorphous carbon, and an in-situ formed submicron porous configuration was observed at the areas containing ZrO₂. Results showed that the matrix in composites mainly consisted of SiC, ZrC and a small quantity of residual metal. SEM and TEM images revealed the formation of ZrC or SiC intergranular particles in the matrix and the characteristic around the residual resin carbon. The composites had a bending strength of 94.89±16.7 MPa, fracture toughness of 11.0±0.98 MPa m^1/2, bulk density of 3.36±0.01 g/cm³, and open porosity of 4.64±0.40%. The formation mechanisms of ZrC–SiC dual matrix and intrabundles׳ structure were discussed in the article.     

Carbothermal reduction synthesis of TiB2 ultrafine powders

Submicrometric TiB₂ powders were synthesized by carbothermal reduction process using titanium dioxide, boron carbide and carbon black as the starting materials. The influence of different amount of boron carbide (22.0–26.8 wt%), calcination temperature (1400–1900 °C) and holding time (15–90 min) on the composition and microstructure of the product was investigated. The resultant powders were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). Results showed that hexagonal impurity-free TiB₂ crystalline powders with the grain size below 1.0 μm could be successfully prepared at 1600 °C for 30 min in Ar atmosphere when the amount of boron carbide was 25.3 wt%. The increase in temperature contributed to reaction completion and grain growth, but the abnormal grain growth and oversintering took place above 1800 °C.     

Synthesis of SiC whiskers by VLS and VS process

This study investigates the mechanisms of SiC whisker formation in the carbothermal reduction of quartz to SiC in different gas atmospheres. Reduction of quartz by graphite was studied in Ar, H₂, and CH₄–H₂–Ar gas mixture in a laboratory fixed bed reactor. The reduction products were characterised by XRD, SEM and TEM. Whiskers were not formed in the carbothermal reduction of quartz in argon. Two types of SiC whiskers were observed in the carbothermal reduction of quartz in H₂ and CH₄–H₂–Ar gas mixture. In the process of reduction at 1400–1600 °C in H₂ and at 1200–1600 °C in CH₄–H₂–Ar gas mixture, whiskers with hexagonal shape with diameter 100–800 nm and length up to tens of microns were formed by the VLS mechanism under catalytic effect of iron. The whiskers with the characteristics of cylindrical shape and high aspect ratio were synthesized in CH₄–H₂–Ar gas mixture at 1400–1600 °C by VS mechanism.     

Carbothermal treatment for the improved discharge performance of primary Li/CFx battery

Carbothermal treatment was used to improve the discharge rate performance of primary lithium/carbon monofluoride (Li/CF_x with x = 1) batteries. The treatment was carried out by heating a mixture of CF_x and carbon black (CB) just below the decomposition temperature of CF_x under nitrogen for 2 h. In the treatment, poly(vinylidene fluoride-co-hexafluoropropylene) (Kynar) was used as a fluorinated polymer binder to press the CF_x/CB mixture into pellets. It was shown that the content of Kynar significantly affected the discharge performance of the resulting treated-CF_x (T-CF_x). This can be attributed to the catalytic effect of HF formed by the pyrolysis of Kynar on the decomposition of CF_x and on the reaction of CB with the volatile fluorocarbons formed by the decomposition of CF_x. The discharge performance of T-CF_x cathode was also affected by the temperature of carbothermal treatment and by the ratio of CF_x to CB. In this work the best result was obtained from a treatment conducted at 470 °C on a 87CF_x/10CB/3Kynar (by weight) mixture. In the discharge condition of C/5 and 20 °C, the Li/CF_x cell with such-obtained T-CF_x cathode showed about 95 mV higher voltage than the control cell while retaining nearly the same specific capacity. Impedance analyses indicate that the improved discharge performance is mainly attributed to a reduction in the cell reaction resistance (R_cr) that includes an ohmic resistance related to the ionic conductivity of the discharge product shell and a Faradic resistance related to the processes of charge-transfer and Li⁺ ion diffusion in the CF_x reaction zone.     

SiCnw@SiC foam prepared based on vapor-solid mechanism for efficient microwave absorption

A SiC_nw@SiC foam with highly efficient microwave absorption (MA) performance was successfully synthesized based on Vapor-Solid (V–S) growth mechanism. SiC nanowire (SiC_nw) and SiC foam skeleton efficiently form a double network coupling structure, which gives additional interface polarization and dielectric loss for the SiC foam, significantly enhancing the MA capacity of the foam. In this study, the SiC_nw@SiC foam has a minimum reflection loss (RL_min) of ?86.31 dB and an effective absorption bandwidth (EAB) of 12.55 GHz in room-temperature environment. However, the MA performance of SiC_nw@SiC foam decreases with increasing temperature, which may be due to the thickening of the SiO₂ layer in the SiC_nw at high temperature. At 600 °C, it has no effective absorption bandwidth, while at 1000 °C, the EAB and RL_min were 0.6 GHz and ?13.04 dB, respectively. As the temperature reaches 1000 °C, the defects in the material further increase, leading to a recovery in the MA performance.     

Effects of Technological Parameters on Carbothermal Reduction and Nitridation of Zircon

Carbothermal reduction and nitridation(CRN)of zircon(ZrSiO4)permits obtaining different composites of oxides and nitrides such as ZrO2-Si2N2O and ZrN-Si3N4.The effects of technological parameters(carbon source,reaction temperature,and carbon content)on the reaction rate and product phase composition of CRN of zircon were investigated by TGA and XRD.The results show that:(1)carbon source is an important factor for a rapid reaction,and activated carbon is chosen as the carbon source considering the expect pro...