Synthesis of (Ca, Mg)-α′-Sialon-AlN-BN powders from boron-rich blast furnace slag by microwave carbothermal reduction-nitridation

(Ca, Mg)-α′-Sialon-AlN-BN powders were synthesized by the carbothermal reduction and nitridation (CRN) method using boron-rich slag, one of the intermediate products from pyrometallurgy separation of pageit, as the staring material. The influences of synthesis temperature and holding time on the phase composition and microstructure during the microwave CRN were studied by XRD, SEM and EDS. The comparison between two heating techniques, conventional and microwave heating, on the synthesized powder was presented as well. The experimental results revealed that the phase compositions and microstructures of the synthesized products were greatly affected by the synthesis temperature and holding time. With an increase in the synthesis temperature or holding time, the relative amount of α′-Sialon increased and α′-Sialon became the main crystalline phase at 1400 °C for 6 h. The synthesized products also contained AlN, BN and a small amount of β-SiC. Elongated α′-Sialon grains, short rod AlN grains, aggregate nanoscale BN grains were observed in the synthesized powders. The reaction temperature of microwave heating method was reduced by 80 °C, the reaction time was shortened by 2 h, and more elongated α′-Sialon grains with large aspect ratio were observed.

Fabrication of β-Sialon/ZrN/ZrON composites using fly ash and zircon

β-Sialon/ZrN/ZrON composites were successfully fabricated by an in-situ carbothermal reduction？nitridation process with fly ash, zircon and active carbon as raw materials. The effects of raw materials composition and holding time on synthesis process were investigated, and the formation process of the composites was also discussed. The phase composition and microstructure of the composites were characterized by means of XRD and SEM. It was found that increasing carbon content in a sample and holding time could promote the formation of β-Sialon, ZrN and ZrON. The proper processing parameters to synthesize β-Sialon/ZrN/ZrON composites were mass ratio of zircon to fly ash to active carbon of 49：100：100, synthesis temperature of 1550 °C and holding time of 15 h. The average grain size ofβ-Sialon and ZrN（ZrON） synthesized at 1550 °C for 15 h reached about 2 and 1μm, respectively. The fabrication process ofβ-Sialon/ZrN/ZrON composites included the formation ofβ-Sialon and ZrO2 as well as the conversion of ZrO2 to ZrN and ZrON.

煤矸石在高温材料中的应用研究进展

围绕煤矸石在高温材料领域的应用和研究现状,概述了煤矸石的分类、化学组成及主要矿物成分高岭石的结构特征。分析了煤矸石经过氧化和非氧化气氛下的高温煅烧过程和反应机理,可以充分利用煤矸石中Al2O3、SiO2、有机碳三种主要成分合成耐火材料和陶瓷。阐述了煤矸石通过碳热还原氮化反应合成Saloon材料及其Sialon复相材料的研究成果和进展,为煤矸石的综合利用、提高产品附加值和品位提供了一个重要途径和研究方向。

由煤矸石制备塞隆材料的反应条件研究

以内蒙古煤矸石为主要原料,采用高温还原氮化方法合成塞隆材料,研究了碳含量、煅烧温度以及保温时间对煤矸石碳热还原氮化反应程度和反应产物的影响.通过试样烧失率的计算,以及采用XRD和SEM分析,研究煤矸石在碳热氮化反应过程中得到β′-SiAlON相、X相及O′-SiAlON相的反应条件.研究表明:反应过程中,随着还原剂碳的增加,试样的烧失率逐渐增大,而保温时间对烧失率和反应生成物的影响不大;在煤矸石碳热还原氮化反应中,反应生成物X相均较少,最高只有12.88%,反应条件应为反应温度高于1 420℃,含碳量大于10%;还原剂碳含量和温度对生成β′-SiAlON相、O′-SiAlON相有显著影响,还原剂碳的合适加入量为10%～16%;当反应温度高于1 420℃×6h时,有利于β′-SiAlON相、O′-SiAlON相的生成.在1 420℃、含碳量14%时,生成主晶相β′-SiAlON相占57.21%;在1 350℃,Z=0.4时,碳含量为16%时,生成O′-SiAlON相占23.80%.

高钛渣碳热还原氮化合成TiN/O′-Sialon导电陶瓷粉体

以高钛渣、硅灰和高铝矾土熟料为原料,采用碳热还原氮化法合成TiN/O′-Sialon导电陶瓷粉体。利用XRD、SEM和EDS检测手段研究合成温度及恒温时间对粉体相组成和显微形貌的影响,并探讨合成机理。结果表明：随合成温度的升高和恒温时间的延长,产物中O′-Sialon的含量逐渐增加,并在1 375~1 400℃、恒温7 h时成为产物主晶相,此时产物中还有较多TiN和少量β′-Sialon生成。继续提高温度和延长反应时间,体系气氛的改变导致O′-Sialon迅速向β′-Sialon转化。合成粉体中O′-Sialon晶粒多呈等轴状,粒度约2μm,TiN晶粒为细小粒状。此外,反应体系中还有大量白色β′-Sialon晶须状沉积物生成。

Influence of processing parameters on the phase composition of ZrN-Si_3N_4 synthesized from zircon

The optimum parameters were determined for synthesizing ZrN-Si3N4 composite powder from zircon by carbothermal reduction-nitridation （CTRN） process. The samples were prepared by mixing the carbon black of an average particle size less than 30 μm and the zircon of 40 μm with C/ZrSiO4 mass ratios of 0.2, 0.3, 0.4, and 0.5. The prepared samples were subjected to the CTRN process at temperatures of 1673, 1723, 1753, and 1773 K for 6, 9, and 12 h. The CTRN process was conducted in an atmosphere-controlled tubular furnace in a nitrogen gas flow of 1.0 L/rain. All the products were examined by X-ray powder diffraction to determine the transformation. The results showed that the proper transformation of ZrN-Si3N4 occurred at 1773 K for 12 h with a C/ZrSiO4 mass ratio of 0.4.

Effects of synthesis temperature and raw materials composition on preparation of β-Sialon based composites from fly ash

β-Sialon based composites were successfully prepared from fly ash and carbon black under nitrogen atmosphere by carbothermal reduction-nitridation process. Effects of heating temperature and raw materials composition on synthesis process were investigated, and the formation process of the composites was also discussed. The phase composition and microstructure of the composites were characterized by X-ray diffraction and scanning electronic microscopy. The results show that increasing heating temperature or mass ratio of carbon black to fly ash can promote the formation of β-Sialon. The β-Sialon based composites can be synthesized at 1723 K for 6 h while heating the sample with mass ratio of carbon black to fly ash of 0.56. The as-received β-Sialon in the composites exists as granular with an average particle size of 2-3 μm. The preparation process of β-Sialon based composites includes the formation of O′-Sialon, X-Sialon and β-Sialon as well as the conversion processes of O′-Sialon and X-Sialon to β-Sialon.

Zr-Si-C-N-O系复相材料的制备及热力学分析（英文）

为了得到锆英石碳热还原氮化反应时产物相的稳定存在区域,用ΔfG1=A+BT法对Zr-Si-C-N-O系进行了热力学计算和分析,绘制了Zr-Si-C-N-O系优势区相图。结果表明:通过控制配碳量、反应温度、炉内的CO分压和N2分压,可以获得组成分别为ZrO2-Si2N2O、ZrN-Si2N2O或ZrN-Si3N4等的复相材料。根据热力学分析结果,以锆英石、活性炭为原料,N2(99.999%)为氮源,研究了配碳量(10%,20%,22%,30%,质量分数)对锆英石碳热还原氮化反应失重率及产物相组成的影响。结果表明:配碳量不仅显著影响锆英石碳热还原氮化反应产物的物相组成,而且配碳量的增加还会降低锆英石碳热还原氮化反应的开始温度。

碳热还原氮化法合成MgAlON

利用重力计,比重仪,SEM,XRD,碳素分析仪,XFS和氧氮分析仪检测了不同加热条件下碳热还原氮化法合成镁阿隆(MgAlON)的密度、微观结构、相组成以及Mg,Al,O,N和C含量,讨论了碳热还原氮化法合成MgAlON的机理.结果表明,加热温度为1100℃时,原料中所有的MgO反应生成镁铝尖晶石(MgAl_2O_(4ss));当加热温度高于1300℃时,发生碳热还原氮化反应,N固溶于MgAl_2O_(4ss)生成MgAlON;由于碳热还原氮化反应不断消耗Al_2O_3,加热温度为1600℃时试样中Al_2O_3大颗粒的尺寸较加热温度为1500℃时的小;随着石墨和Al_2O_3在反应过程被完全消耗,在1650℃下加热获得了单相MgAlON.另外,碳热还原氮化反应中N原子向尖晶石结构MgAl_2O_(4ss)中固溶时导致晶格畸变而使原子间隙扩大,从而Al在MgAlON的固溶量高于其在MgAl_2O_(4ss)中的固溶量.由于碳热还原氮化反应过程产生气体及高温下Mg蒸汽分压较高,即使加热温度提高至1800℃,试样中仍然存在大量密闭气孔.

Anisotropic, biomorphic cellular Si_(3)N_(4) ceramics with directional well-aligned nanowhisker arrays based on wood-mimetic architectures

Inspired by the transport behavior of water and ions through the aligned channels in trees,we demonstrate a facile,scalable approach for constructing biomorphic cellular Si_(3)N_(4) ceramic frameworks with well-aligned nanowhisker arrays on the surface of directionally aligned microchannel alignments.Through a facile Y(NO_(3))_(3) solution infiltration into wood-derived carbon preforms and subsequent heat treatment,we can faultlessly duplicate the anisotropic wood architectures into free-standing bulk porous Si_(3)N_(4) ceramics.Firstly,α-Si3N4 microchannels were synthesized on the surface of CB-templates via carbothermal reduction nitridation(CRN).And then,homogeneous distributed Y–Si–O–N liquid phase on the walls of microchannel facilitated the anisotropicβ-Si3N4 grain growth to form nanowhisker arrays.The dense aligned microchannels with low-tortuosity enable excellent load carrying capacity and thermal conduction through the entire materials.As a result,the porous Si_(3)N_(4) ceramics exhibited an outstanding thermal conductivity(TC,k_(R)≈6.26 W·m^(−1)·K^(−1)),a superior flexural strength(σ_(L)≈29.4 MPa),and a relative high anisotropic ratio of TC(k_(R)/k_(L)=4.1).The orientation dependence of the microstructure–property relations may offer a promising perspective for the fabrication of multifunctional ceramics.

Incorporation of europium (Ⅱ) nanostructures into the channels of mesoporous silicon oxy-nitride for enhanced photoluminescence

Divalent europium（Ⅱ）-doped mesoporous silicon oxy-nitride materials, as a novel type of nanoscopic photoluminescent material, are studied in which the optically active luminescent centers are isolated within the pores. Colorless and transparent blue emitting luminous Eu2＋-doped mesoporous silicon oxy-nitride materials were prepared from mesoporous silica via impregnation, nanocasting and nitrogen-assisted carbothermal reduction and nitridation method. The morphology and porosity of the silica remain unchanged during the synthesis process as revealed by SEM images and by nitrogen sorption studies. Photoluminescence studies reveal a strong blue emission band for Eu2＋ centered at 425 nm with a quantum efficiency of 47%. The luminescent intensity is greatly influenced by the amount of co-dopant, AI3＋ ions.