钇铝石榴石长纤维制备研究

本文以氯化铝、金属铝粉、氧化钇、冰醋酸为原料,采用溶胶-凝胶法制备了钇铝石榴石纤维。研究了纺丝助剂的不同种类对前驱体凝胶纤维长度的影响。结果表明,以聚乙烯吡咯烷酮为纺丝助剂,得到的凝胶纤维长度最长,达25cm。凝胶纤维在1000℃煅烧2小时,全部结晶为钇铝石榴石,纤维的直径为15～18μm,表面光滑。     

钇铝石榴石纤维的应用与制备

钇铝石榴石纤维具有抗氧化、耐高温、抗高温蠕变等特点,可作为高温耐火材料,也可作为高温复合材料的增强材料。本文对钇铝石榴石的晶体结构、应用和制备方法进行了介绍,并展望了钇铝石榴石纤维的发展趋势。     

溶胶-凝胶法制备多晶钇铝石榴石纤维

以廉价的铝粉、工业盐酸和醋酸钇为主要原料,通过溶胶-凝胶法制各了高性能的多晶钇铝石榴石纤维.采用X射线衍射、Fourier变换红外光谱、扫描电镜和热重-差示扫描热分析等表征了不同温度下焙烧所得纤维的物相组成、纤维形貌以及前驱体纤维的热分解特性.结果表明:纤维经热处理到900℃时可获得纯相的钇铝石榴石晶体.经1550℃热处理后,所得到的多晶钇铝石榴石纤维的平均晶粒尺寸在200 nm左右,拉伸强度在485MPa.     

溶胶–凝胶法制备多晶钇铝石榴石纤维

以廉价的铝粉、工业盐酸和醋酸钇为主要原料,通过溶胶–凝胶法制备了高性能的多晶钇铝石榴石纤维。采用X射线衍射、Fourier变换红外光谱、扫描电镜和热重–差示扫描热分析等表征了不同温度下焙烧所得纤维的物相组成、纤维形貌以及前驱体纤维的热分解特性。结果表明:纤维经热处理到900℃时可获得纯相的钇铝石榴石晶体。经1550℃热处理后,所得到的多晶钇铝石榴石纤维的平均晶粒尺寸在200nm左右,拉伸强度在485MPa。     

铒钇铝石榴石激光晶体的研究

研究了引上法生长铒钇铝石榴石的生长工艺。对于不同的铒离子渡度(15—100at.％),获得了直径23—25mm、有效长度100mm以上的优良单晶。测试了与晶体激光行为有关的性能:吸收光谱、荧光光谱和折射率。从铒离子浓度为50at.％的晶体中获得了2.938μm激光。最后讨论了提高激光效率的途径。     

钕镱共掺钇铝石榴石纳米粉体

采用溶胶-凝胶燃烧法,制备了钕镱共掺钇铝石榴石(Nd3+/Yb3+:YAG)透明陶瓷纳米粉体,并用热分析、X射线衍射、红外光谱、透射电镜、吸收及荧光光谱等测试方法对其结构、形貌及性能进行分析.结果表明:经900℃煅烧,Nd3+/YB3+:YAG透明陶瓷的质量损失为49.56%,所得到的Nd3+:Yb3+:YAG纳米粉体结晶好,烧结性好,纯度较高,形状规则,粒径均匀,均在60～100衄之间.在808 nm处具有较强的吸收带,对应于Nd离子4I9/2-4F7/2跃迁,有利于对808nm激光二级管泵浦光的吸收.在1064nm处,Nd3+/Yb3+:YAG的发射峰要强于Nd3+:YAG,说明在Nd3+/Yb3+:YAG中,通过[(4F3/2)Nd),(2F7/2)Yb]→[(4I9/2)nd,(2F5/2)Yb]离子问的交叉弛豫,产生了有效的Yb3+到Nd3+的能量转移,从而实现激光的高效输出.     

钇铝石榴石纤维的制备和应用研究进展

钇铝石榴石纤维具有耐高温、抗氧化、低导热率、优异的抗高温蠕变性和良好的光学性能,是一种理想的结构增强材料、绝热耐火材料和光学材料.本文重点评述了近年来钇铝石榴石纤维制备和应用的研究进展,并展望了钇铝石榴石纤维制备和应用的发展趋势.     

共沉淀法制备钇铝石榴石(YAG)纳米粉体

透明YAG陶瓷具有较好的化学稳定性、光学性能和高温性能，很可能成为有竞争力的用来替代单晶的激光材料。纳米YAG撤体的合成有利于制备性能优异的YAG透明陶瓷。通过在NH4HCO3溶液中滴加NH4Al(SO4)2和Y(NO3)3的混合溶液，共沉淀生成YAG的碳酸盐前驱体；并采用IR，TG／DTA，XRD和SEM等测试手段对YAG前驱体进行表征。对YAG前驱体在不同温度下进行灼烧，结果发现，在1000℃左右已完全转变成YAG相，最终获得单分散、无团聚、形状规则的YAG纳米粉体。     

Sintering and Crystallization of Glass at Constant Heating Rates

The densification and shear behavior of glass powder compacts were determined by measuring their axial strain and radial strain during uniaxial compression. The experiments were conducted nonisothermally at constant rates of heating. The densification and the shear strain were plotted as a function of temperature. Both showed sigmoidal behavior, reaching a plateau at high temperature. The density saturated because the powder compact had sintered to completion, but the shear strain saturated because of the onset of crystallization. The technique offers a method for studying the interaction between densification and crystallization of glass powders.     

Initial Sintering with Constant Rates of Heating

Initial sintering of several materials was studied by measuring powder compact densification at constant rates of heating (CRH). The CRH technique was extremely sensitive to the particle size distribution and other characteristics of the compacts. Although the CRH method circumvents several problems encountered in isothermal studies, it cannot be used to identify the mechanism of diffusion. Using the method on carefully prepared alumina powder compacts and assuming a grain-boundary diffusion mechanism, an activation energy of 115±10 kcal/mol was obtained. Zirconia (yttria-stabilized) and titania also exhibited a single densification mechanism with diffusion coefficients which correlate well with values obtained by isothermal measurements.     

Sintering of Glass Powders During Constant Rates of Heating

Analytical expressions for the initial sintering of glass powders were developed to describe shrinkage of powder compacts at a constant rate of heating. Data describing sintering of soda-lime glass spheres as measured by shrinkage of powder compacts at rates of heating from 0.46 to 2.91°C/min are consistent with the model analytical expressions. Compacts of glass spheres decreased in size exponentially with increasing temperature as predicted by the model.     

Sintering Kinetics at Constant Rates of Heating: Mechanism of Silica-Enhanced Sintering of Fine Zirconia Powder

The sintering behavior of 3 mol% Y₂O₃-doped ZrO₂ powders with and without a small amount of SiO₂ was investigated to clarify the effect of SiO₂ addition on the initial sintering stage. The shrinkage behavior of a powder compact was measured under constant rates of heating (CRH). The sintering rate increased remarkably with the addition of a small amount of SiO₂. The apparent activation energy ( nQ ) and apparent frequency factor     , where n is the order depending on the diffusion mechanism, were estimated at the initial sintering stage by applying the sintering-rate equation to the CRH data. The diffusion mechanism changed from grain-boundary diffusion (GBD) to volume diffusions (VD) on SiO₂ addition, and both nQ and     increased with the GBD→VD change. It is, therefore, concluded that the sintering rate increases by SiO₂ addition because the increase in     rather than nQ is predominant.     

Reaction Sintering of Zinc Ferrite during Constant Rates of Heating

The reaction sintering of equimolar quantities of zinc oxide and ferric oxide was investigated under conditions of constant rates of heating (1–10°C/min from room temperature to 1350°C) and the data were compared with those for a calcined, single-phase zinc ferrite powder. For the heating rate of 1°C/min, the densifications of the reaction-sintered sample and the calcined sample were approximately the same. However, as the heating rate increased, the density at any temperature increased slightly for the reaction-sintered sample but decreased slightly for the calcined powder. The factors responsible for this slight difference in sintering between the reaction-sintered sample and the calcined sample are discussed. For the constant heating rates used, the reaction was completed prior to any significant densification. Relative densities of >95% were obtained for both the reaction-sintered sample and the calcined sample under identical sintering conditions (1–10°C/min to 1350°C). Reaction sintering in a steep temperature gradient produced a nearly fully dense body prior to complete reaction; a composite microstructure consisting of fine zinc oxide grains in a matrix of zinc ferrite was obtained.     

Compaction and Pressureless Sintering of Zirconia Nanoparticles

Four nanometer-sized zirconia powders stabilized by 3 mol% Y₂O₃ were used for the preparation of dense bulk ceramics. Ceramic green bodies were prepared by cold isostatic pressing at pressures of 300–1000 MPa. The size of the pores in ceramic green bodies and their evolution during sintering were correlated with the characteristics of individual nanopowders and with the sintering behavior of powder compacts. Only homogeneous green bodies with pores of <10 nm could be sintered into dense bodies (>99% t.d.) at a sufficiently low temperature to keep the grain sizes in the range <100 nm. Powders with uniform particles 10 nm in size yielded green bodies of required microstructure. These nanoparticle compacts were sintered without pressure to give bodies (diameter 20 mm, thickness 4 mm) with a relative density higher than 99% and a grain size of about 85 nm (as determined by the linear intercept method).     

Sintering Kinetics at Constant Rates of Heating: Effect of Al2O3 on the Initial Sintering Stage of Fine Zirconia Powder

The sinterabilities of fine zirconia powders including 5 mass% Y₂O₃ were investigated, with emphasis on the effect of Al₂O₃ at the initial sintering stage. The shrinkage of powder compact was measured under constant rates of heating (CRH). The powder compact including a small amount of Al₂O₃ increased the densification rate with elevating temperature. The activation energies at the initial stage of sintering were determined by analyzing the densification curves. The activation energy of powder compact including Al₂O₃ was lower than that of a powder compact without Al₂O₃. The diffusion mechanisms at the initial sintering stage were determined using the new analytical equation applied for CRH techniques. This analysis exhibited that Al₂O₃ included in a powder compact changed the diffusion mechanism from grain boundary to volume diffusions (VD). Therefore, it is concluded that the effect of Al₂O₃ enhanced the densification rate because of decrease in the activation energy of VD at the initial sintering stage.     

Effect of Heating Rate on Phase and Microstructural Evolution During Pressureless Sintering of a Nanostructured Transition Alumina

Deagglomeration of a nanocrystalline transition alumina performed using different techniques was first demonstrated to be active in the achievement of a better powder compaction ability under uniaxial pressing and consequently in the development of a highly dense and homogeneous microstructure during pressureless sintering. A major effect, however, was associated to the heating rate chosen during the densification cycle. In fact, the influence of different heating rates (10°C/min or 1°C/min) on phase and microstructural evolution during sintering was investigated in depth on the above best green bodies. A low-rate thermal cycle leads to a significant reduction of the α-Al₂O₃ crystallization temperature and promotes a more effective particle rearrangement during phase transformation. As a consequence, in the low-rate treated material, it was possible to avoid the development of a vermicular structure as usually expected during the densification of a transition alumina and to yield a more homogenously fired microstructure.