Preparation of CaB_6 powder via calciothermic reduction of boron carbide

The method of calciothermic reduction of B_4C was proposed for preparing CaB_6. The phase transition and morphology evolution during the reaction were investigated in detail. The experimental results reveal that Ca first reacts with B_4C to generate CaB_2C_2 and CaB_6 at a low temperature and that the CaB_2C_2 subsequently reacts with Ca to produce CaB_6 and CaC_2 at a high temperature. After the products were leached to remove the byproduct CaC_2, pure CaB_6 was obtained. The grain size of the prepared CaB_6 was 2–3 μm, whereas its particle size was 4–13 μm; it inherited the particle size of B_4C. The residual C content of the product was decreased to 1.03 wt% after the first reaction at 1173 K for 4 h and the second reaction at 1623 K for 4 h.     

Pseudo-<Emphasis Type="Italic">in-situ</Emphasis> stir casting: a new method for production of aluminum matrix composites with bimodal-sized B<Subscript>4</Subscript>C reinforcement

A new method was applied to produce an Al-0.5wt%Ti-0.3wt%Zr/5vol%B₄C composite via stir casting with the aim of characterizing the microstructure of the resulting composite. For the production of the composite, large B₄C particles (larger than 75 μm) with no pre-heating were added to the stirred melt. Reflected-light microscopy, X-ray diffraction, scanning electron microscopy, field-emission scanning electron microscopy, laser particle size analysis, and image analysis using the Clemex software were performed on the cast samples for microstructural analysis and phase detection. The results revealed that as a consequence of thermal shock, B₄C particle breakage occurred in the melt. The mechanism proposed for this phenomenon is that the exerted thermal shock in combination with the low thermal shock resistance of B₄C and large size of the added B₄C particles were the three key parameters responsible for B₄C particle breakage. This breakage introduced small particles with sizes less than 10 μm and with no contamination on their surfaces into the melt. The mean particle distance measured via image analysis was approximately 60 μm. The coefficient of variation index, which was used as a measure of particle distribution homogeneity, showed some variations, indicating a relatively homogeneous distribution.     

Characterization and <Emphasis Type="Italic">in-situ</Emphasis> formation mechanism of tungsten carbide reinforced Fe-based alloy coating by plasma cladding

The precursor carbonization method was first applied to prepare W-C compound powder to perform the in-situ synthesis of the WC phase in a Fe-based alloy coating. The in-situ formation mechanism during the cladding process is discussed in detail. The results reveal that fine and obtuse WC particles were successfully generated and distributed in Fe-based alloy coating via Fe/W-C compound powders. The WC particles were either surrounded by or were semi-enclosed in blocky M₇C₃ carbides. Moreover, net-like structures were confirmed as mixtures of M₂₃C₆ and α-Fe; these structures were transformed from M₇C₃. The coarse herringbone M₃C carbides did not only derive from the decomposition of M₇C₃ but also partly originated from the chemical reaction at the α-Fe/M₂₃C₆ interface. During the cladding process, the phase evolution of the precipitated carbides was WC → M₇C₃ → M₂₃C₆+M₃C.     

Study on stable and meta-stable carbides in a high speed steel for rollers during tempering processes

A high speed steel (HSS) was studied for rollers in this work. The steel was quenched at 1150℃ and tempered at 520℃. The phase structures of the steel were determined by X-ray diffraction (XRD), and the hardness of specimens was measured. The volume fraction of carbides was counted by Image-Pro Plus software. The typical microstructures were observed by field emission scanning electron microscope (FESEM). Stable and meta-stable carbides were deduced by removing the existing phases one by one in the Fe-C equilibrium calculation. It is found that the precipitated carbides are bulk-like MC, long stripe-like M₂C, fishbone-like M₆C, and daisy-like M₇C₃ during the tempering process. The stable carbides are MC and M₆C, but the meta-stable ones are M₂C, M₇C₃, and M₃C.     

Evolution of ferronickel particles during the reduction of low-grade saprolitic laterite nickel ore by coal in the temperature range of 900–1250℃with the addition of CaO–CaF2–H3BO3

The method of producing ferronickel at low temperature(1250–1400℃)has been applied since the 1950s at Nippon Yakin Kogyo,Oheyama Works,Japan.Limestone was used as an additive to adjust the slag composition for lowering the slag melting point.The ferronickel product was recovered by means of a magnetic separator from semi-molten slag and metal after water quenching.To increase the efficiency of magnetic separation,a large particle size of ferronickel is desired.Therefore,in this study,the influences of CaO,CaF₂,and H₃BO₃ additives on the evolution of ferronickel particle at≤1250℃were investigated.The experiments were conducted at 900–1250℃with the addition of CaO,CaF₂,and H₃BO₃.The reduction processes were carried out in a horizontal tube furnace for 2 h under argon atmosphere.At 1250℃,with the CaO addition of 10 wt%of the ore weight,ferronickel particles with size of 20μm were obtained.The ferronickel particle size increased to 165μm by adding 10 wt%CaO and 10 wt%CaF₂.The addition of boric acid further increased the ferronickel particle size to 376μm,as shown by the experiments with the addition of 10 wt%CaO,10 wt%CaF₂,and 10 wt%H₃BO₃.     

Microstructural evolution of a heat-treated H23 tool steel

The microstructure and the stability of carbides after heat treatments in an H23 tool steel were investigated. The heat treatments consisted of austenization at two different austenizing temperatures (1100℃ and 1250℃), followed by water quenching and double-aging at 650℃, 750℃, and 800℃ with air cooling between the first and second aging treatments. Martensite did not form in the as-quenched microstructures, which consisted of a ferrite matrix, M₆C, M₇C₃, and MC carbides. The double-aged microstructures consisted of a ferrite matrix and MC, M₆C, M₇C₃, and M₂₃C₆ carbides. Secondary hardening as a consequence of secondary precipitation of fine M₂C carbides did not occur. There was disagreement between the experimental microstructure and the results of thermodynamic calculations. The highest double-aged hardness of the H23 tool steel was 448 HV after austenization at 1250℃ and double-aging at 650℃, which suggested that this tool steel should be used at temperatures below 650℃.     

Kinetics and mechanism of titanium hydride powder and aluminum melt reaction

Based on the measurement of the released hydrogen gas pressure (P_H2), the reaction kinetics between TiH₂ powder and pure aluminum melt was studied at various temperatures. After cooling the samples, the interface of TiH₂ powder and aluminum melt was studied. The results show that the 2 H P_H2-time curves have three regions; in the first and second regions, the rate of reaction conforms zero and one order, respectively; in the third region, the hydrogen gas pressure remains constant and the rate of reaction reaches zero. The main factors that control the rate of reaction in the first and second regions are the penetration of hydrogen atoms in the titanium lattice and the chemical reaction between molten aluminum and titanium, respectively. According to the main factors that control the rate of reaction, three temperature ranges are considered for the reaction mechanism:(a) 700-750℃, (b) 750-800℃, and (c) 800-1000℃. In the first temperature range, the reaction is mostly under the control of chemical reaction; at the temperature range of 750 to 800℃, the reaction is controlled by the diffusion and chemical reaction; at the third temperature range (800-1000℃), the dominant controlling mechanism is diffusion.     

Hydrometallurgical application for treating a Nigerian chalcopyrite ore in chloride medium: Part I. Dissolution kinetics assessment

The dissolution kinetics of a Nigerian chalcopyrite ore in hydrochloric acid was studied in this article. Acid concentration, reaction temperature, and ore particle size were chosen as experimental parameters. The chemical and morphological studies of the ore before and after leaching at optimal conditions were carried out by X-ray diffraction (XRD) and scanning electron microscopy (SEM). It is revealed that increasing the acid concentration and system temperature and decreasing the ore particle size greatly enhances the dissolution rate. The dissolution kinetics was found to follow the shrinking core model for the diffusion control mechanism where the activation energy (E_a) of 32.92 kJ·mol?1 was obtained for the process and supported by morphological changes at a higher dissolution of 91.33%.     

反应键合B4C–SiC复合材料的组织和力学性能

Reaction-bonded B₄C–SiC composites are highly promising materials for numerous advanced technological applications. However, their microstructure evolution mechanism remains unclear. Herein, B₄C–SiC composites were fabricated through the Si-melt infiltration process. The influences of the sintering time and the B₄C content on the mechanical properties, microstructure, and phase evolution were investigated. X-ray diffraction results showed the presence of SiC, boron silicon, boron silicon carbide, and boron carbide. Scanning electron microscopy results showed that with the increase in the boron carbide content, the Si content decreased and the unreacted B₄C amount increased when the sintering temperature reached 1650°C and the sintering time reached 1 h. The unreacted B₄C diminished with increasing sintering time and temperature when B₄C content was lower than 35wt%. Further microstructure analysis showed a transition area between B₄C and Si, with the C content marginally higher than in the Si area. This indicates that after the silicon infiltration, the diffusion mechanism was the primary sintering mechanism of the composites. As the diffusion process progressed, the hardness increased. The maximum values of the Vickers hardness, flexural strength, and fracture toughness of the reaction-bonded B₄C–SiC ceramic composite with 12wt% B₄C content sintered at 1600°C for 0.5 h were about HV 2400, 330 MPa, and 5.2 MPa·m0.5, respectively.     

A designed core-shell structural composite of lithium terephthalate coating on Li4Ti5O12 as anode for lithium ion batteries

A core-shell structural composite was synthesized with lithium terephthalate（Li₂C₈H₄O₄） coated on spinel Li₄Ti₅O₁₂（LTO）. The composite displays a capacity of about 200 mA h g^-1 and a good rate capability with two charge/discharge platforms at 1.55 and 0.8 V. The excellent cycling performance of the composite is attributed to the successful combination of high cycling stability of LTO and high specific capacity of Li₂C₈H₄O₄. In addition, an interesting phenomena is observed for the first time for this composite which is that lithium ions transfer between LTO and Li₂C₈H₄O₄ at a fast speed. This is investigated in details via the asymmetric charge/discharge measurement and cyclic voltammogram（CV）.The LTO/Li₂C₈H₄O₄ composite may have potential applications to be used as an anode material for the electric vehicle batteries, which is shallowly charged/discharged at ordinary times using the charge/discharge platform of LTO and fully charged/discharged at emergency to release the extra high capacity from Li₂C₈H₄O₄.     

超细磷酸锌钙粉体的制备与性能

采用正交实验设计,以Ca(OH)2,ZnO和H3PO4为原料,通过水热法合成出超细磷酸锌钙粉体.借助于动态光散射粒度分析仪、扫描电镜对产物的粒度和形貌进行分析表征,通过XRD图谱对反应机理进行研究,同时通过TG图谱对产物失水过程进行分析.实验结果表明:最佳反应条件是:Ca与Zn摩尔比n(Ca)∶n(Zn)=1∶2,反应温度为80℃,反应时间为12h,OP-10为表面活性剂:得到的产物颗粒大小均匀,粒度为1～2μm;最终产物CaZn2(PO4)2·2H2O是通过中间产物Ca[Zn(OH)3]2·2H2O与磷酸反应而生成的.CaZn2(PO4)2·2H2O分子的失水过程分为2个阶段,第1阶段失水温度为95～393℃,第2阶段失水温度为403～553℃.     

焙烧对自蔓延法制备的CaB_6粉末中氯含量的影响

考察了焙烧温度及焙烧时间对自蔓延法制备的CaB6中氯含量的影响,利用DSC,XRD及SEM等技术对产物进行了表征.结果表明:自蔓延反应产物是由CaB6,MgO及少量的Ca3(BO3)2和Mg3(BO3)2相组成;浸出产物为纯净的CaB6,其质量分数为96.82%,氯残留量为0.36%.随着焙烧温度升高及焙烧时间的增加,CaB6中氯去除率增加;720℃焙烧6 h,CaB6中氯去除率可达80.12%;焙烧温度过高,氯去除率下降,同时CaB6会氧化变质.     

Synthesis of Ultrafine AlN Powders in an Al-O-C-N System

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High thermal conductivity and high strength magnesium alloy for high pressure die casting ultrathin-walled components

With the rapid development of 3C industries,the demand for high-thermal-conductivity magnesium alloys with high mechanical performance is increasing quickly.However,the thermal conductivities of most common Mg foundry alloys(such as Mg-9wt%-1wt%Zn)are still relatively low.In this study,we developed a high-thermal-conductivity Mg-4Al-4Zn-4RE-1Ca(wt%,AZEX4441)alloy with good mechanical properties for ultrathin-walled cellphone components via high-pressure die casting(HPDC).The HPDC AZEX4441 alloy exhibited a fine homogeneous microstructure(average grain size of 2.8μm)with granular Al₁₁RE₃,fibrous Al₂REZn₂,and networked Ca₆Mg₂Zn₃ phases distributed at the grain boundaries.The room-temperature thermal conductivity of the HPDC AZEX4441 alloy was 94.4 W·m^-1·K^-1,which was much higher than 53.7 W·m^-1·K^-1 of the HPDC AZ91D alloy.Al and Zn in the AZEX4441 alloy were largely consumed by the formation of Al₁₁RE₃,Al₂REZn₂,and Ca₂Mg₆Zn₃ phases because of the addition of RE and Ca.Therefore,the lattice distortion induced by solute atoms of the AZEX4441 alloy(0.171%)was much lower than that of the AZ91D alloy(0.441%),which was responsible for the high thermal conductivity of the AZEX4441 alloy.The AZEX4441 alloy exhibited a high yield strength of~185 MPa,an ultimate tensile strength of~233 MPa,and an elongation of~4.2%.This result indicated that the tensile properties were comparable with those of the AZ91D alloy.Therefore,this study contributed to the development of high-performance Mg alloys with a combination of high thermal conductivity,high strength,and good castability.     

Preparation and densification of BaTiO3 nanopowder by sol-gel autoigniting synthesis

Autoigniting synthesis of gel from Ba(NO3)2, TiO(NO3)2 and C6H8O7H2O aqueous solution was investigated at an initial temperature of 600℃ and tetragonal BaTiO3 nanopowder with particle size of 80nm was prepared. It is indicated that the specific surface area of the combustion product before and after calcination is 14.74 m2/g and 12.49 m2/g, respectively. The combustion wave is composed of solid phase reaction zone and gaseous phase flame reaction zone. The combustion flametemperature is 1 123 K derived from thermocouple measurement. The characteristics and densification behavior of the sol-gel autoigniting synthesized BaTiO3 nanopowder were investigated.     

酸浸对钙化焙烧提钒工艺钒浸出率的影响

采用稀硫酸浸出法提取钙化焙烧后钒渣中的钒,考察了浸出参数:物料粒度、体系pH值、浸出温度和时间、液固比(L/S)、搅拌速度对钒及杂质元素浸出率的影响.结果表明:物料粒度小于75μm时对提高钒浸出率影响较小;液固比从2∶1增加到7∶1,搅拌速度由100增加到500r/min时,钒浸出率增长幅度均低于3%;钒浸出率在浸出前15min内迅速升高,之后增长变缓;浸出体系pH值对钒及杂质浸出率影响显著,pH值为2~3时钒浸出率达90%,杂质元素Ca,Mn,Mg,Al,Si,P浸出率为10%~30%;在较佳浸出条件下:粒度96～75μm,pH值为25,温度55℃,时间30min,L/S为3,搅拌速度500r/min,钒浸出率超过91%.     

片状纳米银的制备及表征

采用水热法将前驱体Ag2C2O4进行热分解制备出超大面积片状纳米银,实验探讨了反应温度及反应时间对纳米银形貌的影响,利用TG分析前驱体Ag2C2O4的热力学性能;利用SEM和XRD表征片状纳米银的特性.结果表明：在表面活性剂PVA的水溶液中,前驱体Ag2C2O4在温度120℃,反应时间为15 h的条件下,生成大量的厚度约45 nm、单边长约5μm的类三角形片状纳米银.     

TiO2空心微球的制备及其在模拟太阳光下光催化降解罗丹明B活性

以钛酸丁酯为反应原料、油胺为模板剂,采用溶剂热法制备了TiO2空心微球.通过XRD、SEM、TEM、HR-TEM、N2吸附-脱附实验及FT-IR对其晶体结构、形貌、表面性质及比表面积进行了表征.在模拟太阳光下研究了TiO2对罗丹明B的光催化降解活性,并与商品TiO2(P25)的活性相比较.结果表明,空心微球为纯相锐钛矿型TiO2,球的直径处于2-5 μm之间,构成微球的初级粒子的平均粒径为10.7 nm,BET比表面积为42.95 m2/g.所制备的TiO2空心微球在2h内对罗丹明B溶液的光降解率达72％.因粒径较大而使其不易团聚,且极易回收,有利于实际应用.