改进的溶胶-凝胶法制备YAG纳米粉体

采用低成本的无机有机复合体系的溶胶凝胶法成功制备出了Y3Al5O12 (YAG)纳米粉体。实验中通过将Y(NO3)3 和Al(NO3)3 按摩尔比3:5 溶解于异丙醇中,再加入适量柠檬酸后生成溶胶,经过脱醇、干燥形成纳米胶球前驱体,将其在适当温度下焙烧后生成YAG纳米粉体。在此过程中,采用了独特的循环水真空泵负压脱醇技术,大大缩减了脱醇和干燥时间,由40h降为4h。分别采用XRD,TEM和TG/DTA分析了不同温度下焙烧所得粉体的物相、形貌以及前驱体热分解特性。结果表明,与其它有机和无机体系制备方法相比,得到的YAG粉体颗粒近似球形,细小均匀,平均尺寸为20~40nm,并具有很好的分散性。     

溶剂对溶胶-凝胶燃烧法合成YAG粉体的影响

以Y(NO3)3.6H2O、Al(NO3)3.9H2O和柠檬酸为原料,分别以去离子水和无水乙醇为溶剂,采用溶胶-凝胶燃烧法合成YAG粉体。借助FT-IR、XRD、SEM等分析仪器研究了溶胶-凝胶燃烧法合成YAG粉体的过程,重点讨论了前躯体溶液不同溶剂对溶胶-凝胶燃烧法合成过程及合成产物的影响。结果表明:去离子水和无水乙醇对合成的YAG粉体的形貌和分散性有重要的影响。     

溶胶-凝胶法制备YAG荧光粉及其性能研究

以金属硝酸盐为原料,柠檬酸为络合剂,采用溶胶一凝胶法制备出了Y_3Al_5O_(12):Ce~(3+)黄色荧光粉.用X射线粉晶衍射(XRD)对其进行了物相鉴定,表明900℃时已经得到纯的钇铝石榴石相(YAG).用红外吸收光谱对所得粉体进行分析表明,当煅烧温度升高到900℃时,在低频区出现了位于724cm~(-1)、792cm~(-1)的峰,这是YAG晶相金属与氧原子间的特征振动峰,说明YAG相已经形成.用扫描电镜(SEM)对其形貌分析,结果表明得到的产物粒径大致在3～10μm之间,平均粒径为6μm.用荧光光谱仪对其荧光光谱进行了研究,结果显示,在煅烧温度为1200℃时,其发光光谱强度最大.     

溶胶-凝胶法制备钛酸钡陶瓷纤维

首次采用乙酰丙酮作为钛醇盐的稳定剂，醋酸钡和钛酸丁酯为原料，无水乙醇-冰醋酸作为溶剂，用sol-gel法制备了长达50cm的BaTiO3凝胶纤维。用FT-IR、XRD、TGA．DTA、SEM等手段对凝胶纤维或陶瓷纤维进行一系列表征，最终得到单一钙钛矿相钛酸钡陶瓷纤维，纤维直径4～10μm，具有椭圆形截面。     

溶胶-凝胶法制备MgO薄膜的研究

本文采用非金属醇盐以醋酸镁为起始原料,胶棉液为添加剂,在Ｓｉ（１００） 衬底上成功地制备了ＭｇＯ 薄膜。结果表明,薄膜的晶体结构与胶棉液的含量及退火温度有关。同时,用Ｘ射线衍射（ ＸＲＤ） 、原子力显微电镜（ＡＦＭ） 和透射电镜（ ＴＥＭ） 对薄膜的微观结构进行了分析。这种制备ＭｇＯ 薄膜的新方法还未见有报道。     

溶胶-凝胶法制备纳米复合材料的研究进展

溶胶-凝胶法用于制备纳米粒子复合材料，因组分、制备途径和结构等可优化设计，故产物性能优异。本文介绍了溶胶-凝胶法制备的纳米粒子复合材料在光学、电子、磁学、生物、催化等领域的应用和最新研究进展。     

柠檬酸溶胶-凝胶法制备纳米铜

以硝酸铜、柠檬酸和氨水为原料,利用柠檬酸溶胶-凝胶法制备含铜凝胶,在氮气气氛下将干凝胶煅烧得到纳米铜粉,探讨成胶反应温度、原料配比、pH等因素对制备过程的影响,确定最低煅烧温度;采用热重-差热分析和红外光谱分析对柠檬酸溶胶-凝胶法制备纳米铜粉的过程进行分析,利用X射线衍射和扫描电镜对实验产物进行结构、形貌表征。结果表明,将柠檬酸与硝酸铜的物质的量比控制为1∶2时溶解混合,调节pH为7,在80℃下制成凝胶,在100℃下干燥后,250℃下煅烧0.5 h,可制得粒径为70⁹0 nm的球型铜粉;推断干凝胶的结构主要为柠檬酸根与铜离子以双齿配位,以及部分为桥式配位。     

溶胶-凝胶法制备纳米二氧化钛探究

采用溶胶-凝胶法，以醇钛盐Ti（OR）4为前驱体、无水醇为有机溶剂，再把醇、水、酸混合液逐滴滴入溶液中，经凝胶化后的湿凝胶置于真空炉中干燥，得到松散干凝胶粉末，对干凝胶粉末进行热处理，得粒径为．20—100nm TiO2粒子。     

溶胶-凝胶法制备纳米薄膜的研究进展

溶胶-凝胶法是制备纳米薄膜的常用方法.综述了溶胶-凝胶法制备纳米薄膜的原理与特点及其最新研究进展,最后指出了溶胶-凝胶法制备纳米薄膜今后急需解决的问题.     

溶胶-凝胶法制备多晶莫来石纤维

以廉价的铝粉、工业盐酸和酸性硅溶胶为主要原料, 通过溶胶凝胶法制备了多晶莫来石纤维. 采用²⁷Al NMR测试了聚合氯化铝溶胶中Al³⁺的聚集状态, 采用XRD、FT-IR、SEM和TG-DTA等手段表征了不同热处理温度下莫来石纤维的物相组成、纤维形貌以及纤维的热分解特性. ²⁷Al NMR结果表明, Al³⁺主要以Keggin结构的Al₁₃形态存在于聚合氯化铝溶胶中. 具有24个活性Al-OH键的Al₁₃聚阳离子易与硅溶胶中的Si-OH发生失水缩聚反应, 生成具有长链结构的纺丝溶液. XRD、FT-IR和TG-DTA结果表明, 纤维热处理到950℃时开始结晶, 到1000℃可获得单一的莫来石晶相, 整个过程的纤维失重在48.24％. 经1250℃热处理, 获得的莫来石纤维的直径为3～5μm, 晶粒尺寸约为240 nm, 拉伸强度为1.1GPa.     

共沉淀法制备纯相钇铝石榴石(YAG)纳米粉体中的若干影响因素

探讨了影响生成纯相YAG纳米粉体的各种因素,并通过优化工艺参数,得到了纯相并具有单分散、无团聚、颗粒尺寸分布窄且近似球形特点的YAG纳米粉体.实验中,配制不同浓度的NH4HCO3水溶液作为沉淀剂,配制不同浓度的Y(NO3)3和NH4Al(SO4)2混合水溶液作为母液,在不同的的温度下,采用不同的滴定速度,得到不同的前驱体,前驱体在900℃以上的温度焙烧2h即可获得不同的粉体.主要采用X射线衍射(XRD)对这些粉体进行了物相分析,同时结合红外光谱法(F-IR)对部分前驱体进行了定性分析,用透射电子显微镜(TEM)对纯相粉体进行了形貌观察.结果表明,在共沉淀过程中,混合溶液和沉淀剂的浓度直接决定了是否生成YAG为主相的粉体,环境温度和滴定速度则对是否生成纯相粉体有较大的影响.     

Synthesis of YAG powder by alcohol-water co-precipitation method

Yttrium Aluminum Garnet (YAG) precursors were co-precipitated by using alcohol-water as the precipitant solvent. The effects of different volume ratios of alcohol to water (R) and ambient temperature (T) on the preparation of pure-phase YAG powders have been mainly studied. The results show that alcohol-water solvent with proper R (0.2-1.2) is effective for the uniform distribution of Al and Y elements in the precursor under low ambient temperature (5-20 °C). Pure-phase YAG powder can be obtained by calcining at 900 °C for 2 h under optimal conditions (R = 0.8; T = 15 °C). Moreover, the elliptical YAG powder calcined at 1000 °C for 2 h is well-crystallized with an average size of 30 nm, and a little agglomeration exists.     

共沉淀法制备YAG超细粉及透明陶瓷

研究了共沉淀法制备YAG透明陶瓷的工艺。采用Al(NO3)3和Y(NO3)3的混合溶液为母盐,以碳酸氢铵为沉淀剂,采用共沉淀法制备了化学组成为Y2(CO3)3·nH2O+NH4AlO(OH)HCO3的碳酸盐先驱沉淀物。使用透射电镜和X射线衍射对先驱沉淀物的形貌及煅烧过程的相转变进行了研究。结果表明先驱沉淀物在900℃煅烧2h后完全转变为YAG相。1100℃煅烧后得到的YAG粉体具有良好的烧结性能。使用0.5%(质量分数)的TEOS(正硅酸乙酯)作为烧结添加剂,1700℃真空烧结5h后,得到了透明YAG烧结体。     

溶胶-凝胶法制备适用于还原性气氛下烧结的钛酸钡基超细粉体

以醋酸钡、钛酸四丁酯和冰醋酸为主要原料,采用溶胶-凝胶方法制备出适用于还原气氛下烧结的超细钛酸钡基陶瓷粉体.利用差热分析研究了前驱体的热转变过程.利用XRD分析了在不同烧结温度下,粉体的相结构.利用透射电镜研究了温度对粉体粒度和形貌的影响.实验结果表明,所得干凝胶在600℃度煅烧后就可以得到均匀且均相的掺杂改性钛酸钡粉体.在700℃度煅烧1h后,就可以得到形貌规则,粒度为100nm左右的高纯掺杂改性钛酸钡粉体.     

放电等离子烧结(SPS)YAG陶瓷的初步研究

研究了采用放电等离子烧结(Spark Plasma Sintering SPS),利用高纯的氧化钇和氧化铝,在1500～1700℃,真空度优于10Pa,反应快速合成YAG陶瓷,但试样的致密度不高,而低气孔率是制备透明陶瓷的关键,实验表明,TEOS的掺加和粉料粒度的减小对烧结试样致密度的提高有一定的作用.     

Evaluation and characterization of nanostructure hydroxyapatite powder prepared by simple sol-gel method

Many attempts have been focused on preparing of synthetic hydroxyapatite (HA), which closely resembles bone apatite and exhibits excellent osteoconductivity. Low temperature formation and fusion of the apatite crystals have been the main contributions of the sol-gel process in comparison with conventional methods for HA powder synthesis. This paper describes the synthesis of nano-HA particles via a sol-gel method. Nanocrystalline powder of hydroxyapatite (HA) was prepared using Ca(NO₃)₂·4H₂O and P₂O₅ by a simple sol-gel approach. X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used for characterization and evaluation of the phase composition, morphology and particle size of products. The presence of amorphous and crystalline phases in the as-dried gel precursor was confirmed by the evaluating technique. Single phase of HA was also identified in the heat treated powder by XRD patterns. SEM and TEM evaluations showed that the obtained powder after heat treatment at 600 °C was agglomerated and composed of nanocrystalline (25-28 nm) HA particles. Increasing the sintering temperature and time could cause decomposition of HA into β-tricalcium phosphate and calcium oxide. The prepared nanocrystalline HA is able to improve the contact reaction and the stability at the artificial/natural bone interface for medical applications.     

Effect of cerium addition on phase transformation and microstructure of cordierite ceramics prepared by sol-gel method

Low-temperature sintering of cordierite ceramic depends on the phase transformation into cordierite and the properties depend on its microstructure. In the present work, the effect of cerium on the phase transformation and microstructure of cordierite ceramics prepared by sol-gel method is studied by X-ray diffraction (XRD), differential thermal analysis (DTA) and scanning electron microscopy (SEM) in order to lower the sintering temperature and improve the properties of cordierite ceramic with the addition of cerium. It is observed that the cerium addition obviously lowers the crystallization temperature of -cordierite while slightly raises that of -cordierite. The lowest temperature for cordierite transformation, which approaches the crystallization temperature of -cordierite, is achieved in the sample containing 4 wt% of cerium, implying a possibility to lower the sintering temperature of cordierite ceramics. The Ce-contained ceramics show a biphasic microstructure that is dependent on sintering temperature. Sintered below 1300°C, a cordierite-CeO₂ microstructure is present; while sintered at the temperature above 1300°C, appears a cordierite-glass microstructure, of which the amount of glass phase is limited to a small extent. Since the addition of 4 wt% cerium to this MgO-Al₂O₃-SiO₂ system substantially enhances the densification of cordierite ceramics and lowers the sintering temperature to the level of around 1000°C, it makes the ceramics suitable for such applications, where the low-temperature sintering is required, as the substrates for electronic circuit and the catalytic supports (with oxygen storage capacity) for cleaning of automotive exhaust emissions.     

光学基质粉体YAG及荧光粉体Ce:YAG的制备与表征

采用共沉淀法制备出尺寸分布均匀、分散性良好的立方相钇铝石榴石(YAG)与Ce:YAG纳米粉体.考察了煅烧温度和时间对粉体物相和颗粒大小的影响及Ce~(3+)的掺杂量对Ce:YAG粉体的荧光光谱的影响.借助IR、XRD、BET、SEM和荧光分析仪等测试手段对前驱体、YAG及Ce:YAG纳米粉体进行了表征与分析.结果表明:共沉淀前驱体经900℃煅烧2h后可得到纯立方相的YAG(Ce:YAG)纳米粉体;所得Ce:YAG粉体具有较好的荧光特性且Ce~(3+)的掺杂量增加会造成其荧光光谱红移.