ZrO2-Si3N4陶瓷复合材料中的化学不相容性

ＺｒＯ２与Ｓｉ３Ｎ４之间存在化学反应生成ＺｒＮ或氧氮化锆,ＺｒＯ２也可能被氮稳定形成氮稳定的ＺｒＯ２。本文对ＺｒＯ２－Ｓｉ３Ｎ４陶瓷复合材料中的化学不相容性及抑制措施进行了综述。     

溶胶-凝胶法制备纳米Si_3N_4(Y_2O_3)粉末的研究

本文以硅溶胶、尿素和炭黑为原料，采用溶胶-凝胶碳热氮化法在1500℃、2h条件下制得粒径为50～80nm的Si3N4纳米粉末．比较了由硅溶胶与尿素经氨解合成的前驱体和硅溶胶二种不同起始物料的反应活性，研究了氮化条件对合成反应的影响．结果表明：氨解前驱体使硅溶胶中的结构水排除，有助于加快反应速率，提高产物氮含量．本文同时以Y（NO3）3为添加剂，在溶液状态与硅源混合，合成了Si3N4－Y2O3纳米复合粉末.     

SHS-β-Si3N4的气氛加压烧结

本文用硅粉和氮通过高温自蔓延方法合成β－Ｓｉ３Ｎ４粉末，以此为原料，采用气氛加压烧结工艺，研究了烧结助剂ＹＡＧ的添加剂量及烧结保温时间对其性能的影响，研究结果表明在１９４０℃、１．２ＭＰａＡｒ，保温１ｈ的条件下，β－Ｓｉ３Ｎ４粉烧结后可达９９％的理论密度并且具有较高的断裂韧性及硬度。     

氧氮玻璃连接Si3N4陶瓷的可行性研究

本文采用Ｙ－Ｓｉ－Ａｌ－Ｏ－Ｎ系氧氮玻璃对Ｓｉ３Ｎ４陶瓷进行了１４５０，１６００℃保温３０ｍｉｎ的润湿实验和连接实验，结果表明，氧氮玻璃对Ｓｉ３Ｎ４的润湿性较好，１４５０℃时两者的热膨胀系数差异明显，而１６００℃时热膨胀系数差异减小，接头附近存在扩散区，氧氮玻璃可以连接Ｓｉ３Ｎ４陶瓷。     

SiO2-Si3N4复合材料的力学性能及其增韧机理

采用热压工艺制备了ＳｉＯ２－Ｓｉ３Ｎ４复合材料，其抗弯强度和断裂韧性达到１４３ＭＰａ和１．７ＭＰａ．ｍ＾１／２，比基体ＳｉＯ２材料分别提高１０７％和７０％，复合材料改善是由于高弹性模量的Ｓｉ３Ｎ４引入以及ＳｉＯ２和Ｓｉ３Ｎ４热膨胀系数不匹配导致的残余应力。     

纳米SiC—Si3N4复合粉体的制备及研究

本文以炭黑和气凝氧化硅为原料，采用碳热还原氮化的方法制备纳米ＳｉＣ－Ｓｉ３Ｎ４复合粉体；复合粉中ＳｉＣ的含量由起始粉中Ｃ：ＳｉＯ２的摩尔比控制。在复合粉体的表征中用ＸＲＤ线宽法测量ＳｉＣ粒径大小。ＴＥＭ照片显示Ｓｉ３Ｎ４粒径在１００￣２００ｎｍ；ＳｉＣ为纳米级。文中还对生成复合粉体的反应机理进行了探讨。同时利用这一工艺制备出单相的Ｓｉ３Ｎ４粉和ＳｉＣ粉。     

晶内型Al2O3—SiC纳米复合陶瓷的制备

研究了沉淀法制备Ａｌ２Ｏ３－ＳｉＣ纳米复合陶瓷的工艺过程，利用Ａｌ２Ｏ３从γ相到α相的蠕虫状生长过程，使大部分纳米ＳｉＣ颗粒位于Ａｌ２Ｏ３晶粒内，用沉淀法制得的、含有５ｖｏｌ％ＳｉＣ的Ａｌ２Ｏ３－ＳｉＣ纳米复合陶瓷，其强度为４６７ＭＰａ，韧性为４．７ＭＰａ．ｍ＾１／２，与一般的Ａｌ２Ｏ３陶瓷相比有较大的提高，显示了沉淀法制备Ａｌ２Ｏ３－ＳｉＣ纳米复合陶瓷的优点。     

SiO2—C—N2系统中气相对相稳定的影响

研究了ＳｉＯ２－Ｃ－Ｎ２系统中一定Ｎ２分压下，温度与Ｏ２、ＳｉＯ、ＣＯ气体分压对相稳定性的影响，绘制了平衡状态下的相稳定性关系图，并以此指导碳热还原氮化法合成高纯Ｓｉ３Ｎ４粉的工艺制备条件。     

化学气相淀积制备Si3N4超细粉末

本文研究了ＳｉＣｌ４－ＮＨ３－Ｎ２－Ｈ２系统平衡热力学，确定了Ｓｉ３Ｎ４合成的最佳热力学条件。采用电阻炉化学气相淀积法制备了Ｓｉ３Ｎ４超细粉末，并考察了工艺条件对颗粒形貌的影响。     

熔盐热析出反应金属化Si3N4与Si3N4的连接

在采用熔盐热析出反应在Ｓｉ３Ｎ４陶瓷表面沉积钛金属膜的基础上,对ＣｕＡｇ合金在金属化表面的润湿性进行了研究,结果表明,ＣｕＡｇ合金能对采用该方法金属化的Ｓｉ３Ｎ４陶瓷实现良好润湿,在此基础上,成功实现了钛金属化Ｓｉ３Ｎ４陶瓷与Ｓｉ３Ｎ４陶瓷的连接并对连接工艺进行了系统研究。连接界面的ＴＥＭ研究发现,界面上广泛存在Ｔｉ－Ｃｕ－Ｓｉ－Ｎ相并对这种相对连接强度的影响进行了讨论。     

多孔氮化硅表面封孔增强涂层研究

以CaO-SiO2-B2O3体系作为α-Si3N4的结合剂和助烧剂,采用溶胶-凝胶法在多孔氮化硅表面制备了防潮增强涂层.采用X射线衍射(XRD)方法对涂层进行了相结构分析;用扫描电子显微镜(SEM)观察了涂层的微观形貌;用阿基米德法测量了封孔前后基体的密度、吸水率和显气孔率;分别在SANS电子式材料实验机和1MHz LCR测试仪上测量了封孔前后材料的抗弯强度、介电常数和介电损耗.结果表明:封孔防潮处理使基体吸水率下降了90.99%～96.97%,强度提高了9%～22%,而对多孔体的密度、介电常数和介电损耗影响很小.     

Si3N4/BN(f)复合材料的相界面

本文借助高分辩电子普微镜研究了Ｓｉ３Ｎ４／ＢＦ（ｆ）复合材料的相界面。研究发现，ＢＮ纤维的两端与基体结合牢固，界面不易解离，材料民裂过程中纤维很难拔出。材料的韩性主要通过ＢＮ纤维自身（００１）面上的滑移、撕裂和弯曲以及ＢＮ纤维的侧表与Ｓｉ３Ｎ４颗粒的颗上的解离等途径得以提高．     

原位生成TiC/Ti5Si3纳米复合材料的显微结构研究

研究了原位生成ＴｉＣ／ＴＩ５Ｓｉ３纳米复合材料的显微结构,实验结果表明,以ＳｉＣ和Ｔｉ原料,通过反应热压工艺可以原位合成ＴｉＣ／Ｔｉ５Ｓｉ２复合材料,其中的大部分ＴｉＣ粒子为纳米粒子,ＴｉＣ晶粒与Ｔｉ５Ｓｉ３晶粒的晶界上存在原子台阶,复合材料还含有少量Ｔｉ３ＳｉＣ２相,这些Ｔｉ３ＳｉＣ２相主要呈棒状分布在Ｔｉ５Ｓｉ３基体中,另有少量ＴｉｅＳｉＣ２相位震大的ＴｉＣ晶粒内。     

纳米SiC及Si3N4/SiC的高温等静压研究

采用高温等静压工艺，制备了纳米结构的单相ＳｉＣ及Ｓｉ３Ｎ４／ＳｉＣ复相陶瓷，并通过Ｘ射线衍射分析透射有高分辨电镜对其相组成及结构进行了表征。实验表明，在温度１８５０℃，压力２００ＭＰａ条件下保温１ｈ，要获得晶粒尺寸〈１００ｎｍ，结构均匀，致密的单相ＳｉＣ纳米结构陶瓷。     

Large-scale synthesis of ear-like Si3N4 dendrites from SiO2/Fe composites and Si powders

Large-scale ear-like Si₃N₄ dendrites were prepared by the reaction of SiO₂/Fe composites and Si powders in N₂ atmosphere. The product was characterized by field emission scanning electron microscopy, X-ray diffraction, and transmission electron microscopy. The results reveal that the product mainly consists of ear-like Si₃N₄ dendrites with crystal structures, which have a length of several microns and a diameter of 100-200 nm. Nanosized ladder-like Si₃N₄ was also obtained when changing the Fe content in the SiO₂/Fe composites. The Si₃N₄ nanoladders have a length of hundreds nanometers to several microns and a width of 100-300 nm. The ear-like Si₃N₄ dendrites are formed from a two-step growth process, the formation of inner stem structures followed by the epitaxial growth of secondary branches.     

过渡金属元素(Fe与Cr)掺杂Bi4Si3O12晶体闪烁性能的研究

本文采用坩埚下降法生长出20mm×20mm×100mm优质Bi₄Si₃O₁₂及Fe、Cr掺杂Bi₄Si₃O₁₂晶体．测试了晶体的透射光谱、能谱及光产额、FWHM能量分辨率和激发一发射光谱．总结并解释了掺杂影响Bi₄Si₃O₁₂晶体闪烁性能的规律．     

Synthesis,characterization and fabrication of Na1+xZr2SixP3−xO12

A wet chemical technique was used to prepare Na_1+xZr₂Si_xP_3?xO₁₂. The precursor was prepared using a finely divided silica sol and a fine zirconia slurry mixed with a solution of sodium carbonate and ammonium dihydrogen phosphate. The mixture was dried by flash evaporation and then calcined at 750°C. The effect of sintering conditions and atmosphere on density and phase formation in the system was examined. Single phase material was obtained by controlling the soda loss during processing.     

Characterization of porous silicon nitride/silicon oxynitride composite ceramics produced by sol infiltration

Porous silicon nitride/silicon oxynitride composite ceramics were fabricated by silica sol infiltration of aqueous gelcasting prefabricated Si₃N₄ green compact. Silica was introduced by infiltration to increase the green density of specimens, so suitable properties with low shrinkage of ceramics were achieved during sintering at low temperature. Si₂N₂O was formed through reaction between Si₃N₄ and silica sol at a temperature above 1550 °C. Si₃N₄/Si₂N₂O composite ceramics with a low linear shrinkage of 1.3–5.7%, a superior strength of 95–180 MPa and a moderate dielectric constant of 4.0–5.0 (at 21–39 GHz) were obtained by varying infiltration cycle and sintering temperature.     

Interfacial microstructure of Si3N4/Si3N4 brazing joint with Cu–Zn–Ti filler alloy

In this study, Si₃N₄ ceramic was jointed by a brazing technique with a Cu–Zn–Ti filler alloy. The interfacial microstructure between Si₃N₄ ceramic and filler alloy in the Si₃N₄/Si₃N₄ joint was observed and analyzed by using electron-probe microanalysis, X-ray diffraction and transmission electron microscopy. The results indicate that there are two reaction layers at the ceramic/filler interface in the joint, which was obtained by brazing at a temperature and holding time of 1223 K and 15 min, respectively. The layer nearby the Si₃N₄ ceramic is a TiN layer with an average grain size of 100 nm, and the layer nearby the filler alloy is a Ti₅Si₃N_x layer with an average grain size of 1–2 μm. Thickness of the TiN and Ti₅Si₃N_x layers is about 1 μm and 10 μm, respectively. The formation mechanism of the reaction layers was discussed. A model showing the microstructure from Si₃N₄ ceramic to filler alloy in the Si₃N₄/Si₃N₄ joint was provided as: Si₃N₄ ceramic/TiN reaction layer/Ti₅Si₃N_x reaction layer/Cu–Zn solution.