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固相反应法制备稀土掺杂YAG透明陶瓷及其性能研究

发布时间:2018-12-14 08:00
【摘要】:钇铝石榴石(Y3Al5O12, YAG),由于其优越的化学稳定性、光学和机械性能而作为一种重要的陶瓷材料。它可以被用作电子器件的耐热涂层和掺杂稀土离子的基体用作固体激光器工作物质。近年来,作为YAG单晶的替代品YAG多晶透明陶瓷受到了广泛的关注。目前,YAG粉体的合成方法主要有固相反应法,共沉淀法,溶胶-凝胶法,其中固相反应法因为具有产量高,工艺简单的特点被广泛应用。本文采用商业Al2O3、Y2O3和稀上氧化物粉体通过固相反应法制备了透明的稀土掺杂YAG透明陶瓷。 用商业Al2O3、Y2O3、Gd2O3粉体和Ce(NO3)3·xH2O晶体制备了化学式为CexY1.5-xGd1.5Al5O12和CexY3-xAl5O12的透明陶瓷,当Ce3+掺入量增加时,晶粒尺寸明显变小,透过率降低,当x=0.02时CexY1.5-xGd1.5Al5O12口CexY3-XAl5O12在λ=800nm的直线透过率分别为65.24%和76.59%;CexY3-xAl5O12的发光强度随着Ce3+掺入量的增加先增强后减弱,当x=0.05时达到最大,而对于CexY1.5-xGd1.5Al5O12,其发光强度随着Ce3+掺入量的增加而减弱,x=0.02其发光最强。对比CexY1.5-xGd1.5Al5O12和CexY3-xAl5O12,当掺入Gd3+后发光强度会减弱;对于这两组样品,退火只会影响样品的发光强度,而对激发与发射波长不会产生影响。 以聚丙烯酸铵为分散剂,水为分散介质的Yb:YAG悬浮体系,最佳分散剂含量为0.5wt%;不需要调整pH值,最佳球磨时间为16h;生坯密度随固相含量的提高而升高;对比不同温度煅烧的粉体得出1200℃煅烧后的粉体烧结性能较好,但是在成型过程中容易分层,1300℃煅烧后的粉体烧结性能差,但成型过程中不容易分层;对比不同方法对粉体进行表面处理的结果,发现用磷酸在50℃处理的粉体分散效果好,可以制的固含量高达40vo1%的浆料。 通过模压成型,制备了层状复合结构的Yb:YAG/YAG坯体,在不同温度真空烧结,1700℃烧结后的样品略有透明;样品中的晶粒和气孔大小随着烧结温度的升高长大,气孔是影响样品透明的主要原因。
[Abstract]:Yttrium aluminum garnet (Y3Al5O12, YAG),) is an important ceramic material due to its excellent chemical stability, optical and mechanical properties. It can be used as the heat resistant coating of electronic devices and the substrate doped with rare earth ions as the working material of solid state lasers. In recent years, YAG polycrystalline transparent ceramics, as a substitute for YAG single crystal, have received wide attention. At present, the synthesis methods of YAG powder mainly include solid state reaction, coprecipitation and sol-gel method. Among them, solid state reaction is widely used because of its high yield and simple process. Transparent rare-earth doped YAG transparent ceramics were prepared by solid state reaction with commercial Al2O3,Y2O3 and thin oxide powders. Transparent ceramics with the chemical expressions CexY1.5-xGd1.5Al5O12 and CexY3-xAl5O12 were prepared from commercial Al2O3,Y2O3,Gd2O3 powder and Ce (NO3) 3 xH2O crystal. When the amount of Ce3 was increased, the grain size became smaller and the transmittance decreased. The straight line transmittance of CexY1.5-xGd1.5Al5O12 mouth CexY3-XAl5O12 at 位 = 800nm is 65.24% and 76.59%, respectively. The luminescence intensity of CexY3-xAl5O12 increases first and then decreases with the increase of Ce3 incorporation, and reaches its maximum when x0. 05. For CexY1.5-xGd1.5Al5O12, the luminescence intensity decreases with the increase of Ce3 incorporation, and x0. 02 is the strongest. Compared with CexY1.5-xGd1.5Al5O12 and CexY3-xAl5O12, the luminescence intensity decreases when Gd3 is added, but annealing only affects the luminescence intensity of the samples, but has no effect on the excitation and emission wavelengths. The optimum dispersant content of Yb:YAG suspension system with ammonium polyacrylate as dispersant and water as dispersing medium is 0.5 wt. the optimum milling time is 16h without adjusting pH value, and the density of green increases with the increase of solid content. Compared with the calcined powders at different temperatures, the sintering properties of the powders calcined at 1200 鈩,

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