氮化制度对Si-Al-Al2O3体系合成Sialon的影响

以SiC、α-Al2O3微粉、Si粉、Al粉为原料,在1450℃流动氮气中制备Sialon/SiC材料。研究了不同温度保温氮化对Sialon合成的影响。研究结果表明:有部分硅粉残余没有氮化;在1100℃保温氮化的氮化率高于在1150℃、1200℃保温氮化;1100℃保温氮化,残余Si量少、分布均匀,残余硅熔聚现象较轻,利于Sialon的合成。     

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     

Numerical modeling of high-temperature corrosion processes

Numerical modeling of the diffusional transport associated with high-temperature corrosion processes is reviewed. These corrosion processes include external scale formation and internal subscale formation during oxidation, coating degradation by oxidation and substrate interdiffusion, carburization, sulfidation and nitridation. The studies that are reviewed cover such complexities as concentration-dependent diffusivities, cross-term effects in ternary alloys, and internal precipitation where several compounds of the same element may form (e.g., carbides of Cr) or several compounds exist simultaneously (e.g., carbides containing varying amounts of Ni, Cr, Fe or Mo). In addition, the studies involve a variety of boundary conditions that vary with time and temperature. Finite-difference (F-D) techniques have been applied almost exclusively to model either the solute or corrodant transport in each of these studies. Hence, the paper first reviews the use of F-D techniques to develop solutions to the diffusion equations with various boundary conditions appropriate to high-temperature corrosion processes. The bulk of the paper then reviews various F-D modeling studies of diffusional transport associated with high-temperature corrosion.     

碳热还原氮化一步法制备钒氮合金工艺研究

对V2O5自还原氮化过程进行热力学分析,并以工业级V2O5和炭黑为原料,经过混料、研磨、压制成块后进行烧结和还原氮化,制得含氮量较高的钒氮合金。结果表明,为了避免V2O5在还原过程中挥发,预还原温度应控制在V2O5熔点（678℃）以下;经过650℃预还原4h,试样中的V2O5才能全部转化为低价态的钒氧化物;V2O5在N2气氛下自还原时,还原终温低于1 271℃时,还原产物优先生成VN,还原终温高于1 271℃时,还原产物中才会出现大量VC;为保证还原产物的高氮和低碳含量,应将还原氮化最终温度控制在1 200～1 300℃。     

直接氮化法制备纳米晶TiN薄膜

首先采用溶胶-凝胶法在Al2O3基体上制备了TiO2纳米晶薄膜，然后在管式气氛炉中，用氨气作为还原剂，直接氮化制备TiO2纳米晶薄膜；从而成功地的α-Al2O3陶瓷基片上制备了纳米晶TiN薄膜。利用XRD、XPS、FE-SEM等分析技术，研究了制备的纳米晶TiN薄膜的相组成及形貌。结果表明最佳工艺条件为：氮化温度为700℃，氮化时间为1h。     

反应烧结法制备高强度多孔氮化硅陶瓷

以硅粉(Si)为起始原料, 氧化钇(Y₂O₃)为烧结助剂, 利用干压成型工艺制备出不同气孔率的多孔硅坯体, 通过反应烧结得到高强度多孔氮化硅(Si₃N₄)陶瓷. 研究了Y₂O₃添加量在不同升温制度下对于氮化率的影响, 以及1500~1750℃后烧结对多孔材料强度的影响. 结果表明: 添加9%Y₂O₃的样品具有较高的氮化率, 主要是Y₂O₃与Si粉表面的SiO₂在较低的温度下反应生成了Y₅Si₃O₁₂N. 在不同的反应条件下可得到气孔率为30%~50%, 强度为160~50MPa的样品. 在1750、 0.5MPaN₂气压下对样品进行后处理, α-Si₃N₄完全转变成柱状β-Si₃N₄, 晶型转变有利于强度提高,气孔率为46%的多孔Si₃N₄其强度可达140MPa.     

烧结气氛对合成MgAl2O4-Ti(C,N)复合陶瓷的影响

以金属铝粉、钛白粉和轻烧MgO细粉为原料,通过设计100%焦炭粒(简称C气氛),10%钛白粉 90%焦炭粒(简称TC气氛),以及10%硅微粉 90%焦炭粒(简称SC气氛)3种埋粉条件下的高温烧结还原性气氛,采用X射线衍射仪(XRD)、扫描电镜(SEM)和微区电子探针分析(EPMA)等手段,研究了铝热还原氮化法(1600℃3h)制备MgAl2O4-Ti(C,N)复合陶瓷在不同烧结气氛下的相组成和显微结构的变化。结果表明在不同气氛下,烧后试样的主要物相均为MgAl2O4和Ti(C,N),Ti(C,N)可能会固溶氧,气氛对Ti(C,N)的影响较大。和单纯埋炭气氛下相比,在TC气氛下有助于Ti(C,N)的生成,但晶粒细小;在SC气氛下不利于Ti(C,N)的生成,且有玻璃相存在。     

Study on rapid nitridation process of molten silicon by thermogravimetry and in situ Raman spectroscopy

The melt of silicon, hindering nitridation for its agglomeration, should be avoided in the direct nitridation of silicon to synthesize silicon nitride powders, although liquid phase facilitates nitridation. Therefore, we proposed a method to nitride molten silicon without agglomeration. Thermogravimetric and in situ Raman studies on the nitridation process of molten silicon were performed. The as-prepared silicon nitride samples were found to be micron clusters composed of submicron grains with high α-Si₃N₄ content. The nitridation of molten silicon at 1500°C was completed after 500 s and 109 times faster than the nitridation of solid silicon at 1350°C. β-Si₃N₄ is produced dominantly by α–β-phase transition. Less nitridation time and low temperature can decrease the β-Si₃N₄ content. The rapid nitridation was owning to core–shell structure Si@Si₃N₄, which was formed after the initial nitridation of silicon particles and hindered the agglomeration of molten silicon.