共沸蒸馏法合成CeO2纳米颗粒研究

分别以乙醇、正丙醇、异丙醇、正丁醇、异丁醇、仲丁醇及叔丁醇等七种有机醇作为共沸剂,采用液相沉淀法结合共沸蒸馏处理前驱体成功合成了分散性良好、粒子尺寸分布为10-20nm的纳米CeO2颗粒,运用TG／DTA、FI—IR、XRD、TEM等方法对不同有机醇的共沸蒸馏作用以及产品性能进行了分析和表征,探讨了共沸蒸馏法制备纳米CeO2的机理。结果表明：共沸蒸馏能起到有效脱除前驱体凝胶中的水分,防止其干燥和焙烧过程中的硬团聚形成的作用,其中七种醇中以正丁醇的共沸蒸馏效果最佳,所得纳米CeO2颗粒的粒度、均匀及分散性能最好。     

共沸蒸馏法制备单分散氧化镍微粉

先采用均匀沉淀法制得单分散的氧化镍前驱体粉末 ,然后用正丁醇进行共沸蒸馏脱水处理。经干燥、煅烧后成功地制成了单分散性相当好的氧化镍微粉。实验证明 ,共沸蒸馏能有效地脱除湿粉末中的水分 ,丁氧基取代了颗粒表面的羟基 ,从而防止了颗粒间Ni—O—Ni的形成 ,消除了硬团聚形成的可能性。     

超声模板法制备纳米二氧化铈的研究

采用超声模板法结合共沸蒸馏和水热法处理前驱体成功制备出了纳米CeO2颗粒,通过TEM、XRD、FT-IR、UV-Vis等分析方法对产物形貌、结构和性能进行了表征;研究了模板剂的性质、模板剂的用量、共沸蒸馏和水热处理对纳米CeO2颗粒形态、尺寸的影响。实验结果表明,与OP-10和SDBS比较,CTAB最适合应用于制备纳米CeO2颗粒。当模板剂用量为n(CTAB)∶n(Ce(NO3)3.6H2O)=1∶2,制备出粒径约为6.1nm的球形纳米CeO2;共沸蒸馏能有效去除前驱体中的模板剂和吸附水,丁氧基的取代吸附及其空间位阻作用有利于制得分散性好、粒度分布均匀、粒径约为1.5～2.2nm的纳米CeO2颗粒;水热处理改善了纳米CeO2颗粒的晶化度,避免了高温焙烧过程时硬团聚体的生成,颗粒尺寸为2.5～3.8nm;纳米CeO2颗粒具有良好的可见光透过和优异的紫外光吸收性能。     

纳米氧化结粉体的共沸蒸馏法制备及研究

采用非均相共沸蒸馏工艺成功地制备得到了纳米级氧化锆超细粉体．这种工艺能够非常有效地对水合氧化锆胶体进行脱水，防止粉体硬团聚的形成．采用这种工艺制备的氧化锆粉体常规烧结时能够在１２５０℃达到９９．５％的致密化，晶粒尺寸约２００ｎｍ；快速烧结条件下达到９７５％的致密化，晶粒尺寸约１２０ｎｍ．本文同时对该工艺防止硬团聚形成的机理进行了初步讨论．     

纳米氧化锆粉体的表面改性研究

本文初步研究了己二酸，硬脂酸对纳米氧化锆陶瓷粉体的表面改性作用及其对粉体的极性和流动性的影响。实验结果表明，己二酸，硬脂酸中的羧基与纳米氧化锆粉体颗粒表面的羟基发生类似于酸和醇的酯化反应，并在其表面形成单分子膜。经过表面改性的纳米氧化锆粉体由极性转化为非极性，同时表现出良好的流动性能。     

制备低团聚掺锑氧化锡超细粉体的新方法

以SnCl4·5H2O和SbCl3为原料,用醇盐水解法制备了纳米掺锑氧化锡(ATO)导电粉体。用正丁醇—二甲苯的混合溶剂共沸蒸馏、有机脱水剂以及其它方法对前驱体胶态沉淀进行脱水处理,以消除粉体团聚。运用XRD、TEM、BET等手段对粉体进行表征,比较了各种脱水处理方法对ATO纳米导电粉体的粒度、团聚度、晶粒生长以及电阻率的影响。结果表明,混合溶剂共沸蒸馏处理以及有机脱水剂是比较有效的脱水方法,可以用来制备比表面积大(85.32m2·g—)、团聚小、电阻率低1的纳米ATO导电粉体。     

醇盐水解法制备二氧化钛纳米粉体

利用控制醇盐水解的方法，分析采用正丁醇共沸蒸馏和乙醇洗涤这两种工艺，详细研究了超细二氧化钛粉体的制备过程，采和ＸＲＤ、ＴＥＤ、ＢＥＴ、ＴＧ和ＤＴＡ等方面对用直接沉淀、正丁醇共沸和乙醇洗涤三种方法获得的粉体进行了表征。发现用直接沉淀和乙醇洗涤法均能获得团聚少、颗粒在１５ｎｍ左右的粉体，且乙醇洗涤能进一步减少粉体的团聚，但共沸蒸馏反而增加了粉体的团聚度。     

纳米氧化锆的制备新工艺研究

以ZroCl2·8H2O和H2O2为原料,采用中和沉淀法制备纳米氧化锆,在制备工艺过程中2次(前驱体制备过程和研磨过程)加入分散剂(表面活性剂)来抑制粉体的团聚.探讨了有关因素对制备氧化锆产品的影响,例如前驱体氢氧化锆的煅烧温度对氧化锆晶型的影响,表面活性剂对产品粒径的影响,煅烧时间对ZrO2平均粒径的影响,研磨助剂对ZrO2平均粒径的影响等,研究得到了最佳工艺条件,并在优化实验条件下制备出平均粒径为50nm、粒径分布均匀的球形纳米氧化锆粉末.     

纳米二氧化硅的制备及表征

以水玻璃为原料,采用微乳液法和正丁醇共沸蒸馏法制备纳米级二氧化硅粉体.并通过扫描电镜,红外光谱分析,X射线衍射等手段对制备的纳米二氧化硅进行了表征.     

纳米Ni(OH)2的控制结晶法制备

纳米Ni(OH)2可以有效地提升镍氢电池的性能.本文以NiSO4和NaOH为原料,聚乙二醇为分散剂,采用控制结晶法制备了纳米Ni(OH)2的胶体溶液,控制结晶的pH值和温度分别为11.0和45℃.然后用正丁醇进行共沸蒸馏处理.制备了分散性良好的纳米Ni(OH)2粉体,粉体颗粒粒径20nm左右,团聚体系数为1.07.并用TEM和XRD对粉体进行了表征.所制备的样品在1C倍率放电时电容量达到258mAh·g-1.     

堇青石-氧化锆红外辐射复合粉体的制备

为获得具有高红外辐射性能的粉体,以堇青石颗粒为基体,采用液相共沉淀法,用氧化锆前驱体包覆堇青石基体,煅烧后得到堇青石-氧化锆红外辐射复合粉体;对制备的复合粉体进行热分析、物相分析及形貌分析,并测试其红外辐射性能。结果表明,利用非均匀形核可将氧化锆前驱体包覆于堇青石颗粒表面,氧化锆结晶温度在800～900℃之间,900℃煅烧后得到的氧化锆晶粒尺寸约为8 nm;当在一定初始溶液浓度范围内改变反应物的用量时,可以控制氧化锆的包覆量并且避免其自发团聚;通过氧化锆纳米颗粒包覆的工艺可以提高堇青石粉体在3～5μm波段的红外辐射性能,当氧化锆包覆质量分数为21.11%时,复合粉体具有最佳的红外辐射性能。     

Nanocoating of Al<Subscript>2</Subscript>O<Subscript>3</Subscript> additive on ZrO<Subscript>2</Subscript> powder and its effect on the sintering behaviour in ZrO<Subscript>2</Subscript> ceramic

ZrO₂ powder was coated with Al₂O₃ precursor generated by a polymeric precursor method in aqueous solution. The system of nanocoated particles formed a core shell-like structure in which the particle is the core and the nanocoating (additive) is the shell. A new approach is reported in order to control the superficial mass transport and the exaggerated grain growth during the sintering of zirconia powder. Transmission electron microscopy (TEM) observations clearly showed the formation of an alumina layer on the surface of the zirconia particles. This layer modifies the sintering process and retards the maximum shrinkage temperature of the pure zirconia.     

液相等离子喷涂制备纳米ZrO2/Y2O3涂层的研究

传统的喷涂技术制备的ZrO2/Y2O3涂层存在原料需团聚烧结致密,纳米晶粒不定和物理性能不佳等缺点.采用一种新型的液相等离子喷涂法制备了纳米氧化锆热障涂层,初步分析了液相前驱体液滴在等离子焰流中和基体表面的沉积变化过程,研究了雾化液滴尺寸对纳米氧化锆涂层的显微结构,特别是其相结构的影响;同时分析了纳米氧化锆涂层的抗热震循环性能.结果表明,纳米氧化锆涂层可以承受1 000多次的热循环试验,具有优良的抗热震性能.     

Synthesis of polycrystalline zirconia fibre with organozirconium precursor

Polycrystalline zirconia fibre was successfully synthesized by pyrolysis of preceramic fibre formed from an organozirconium compound. Dibutoxybis(2, 4-pentadionato)zirconium (BPZ) was polymerized at 150° C and 10² Pa, yielding a viscous polymeric product. The infrared absorption bands of the Zr-O bond changed from separate to coalesced bands after polymerization. The signals of the¹³C NMR spectrum of BPZ changed from sharp singlets to multiplets after polymerization. The molecular weight of the polymer was between 400 and 1000. The viscosity of polymer was 580 Pa sec at 30° C and a shear rate of 1.0 sec^–1. The polymer viscosity decreased with increased temperature from 30 to 60° C. The precursor polymer pyrolysed at 400° C in air was amorphous to X-rays, and crystallized in a mixture of monoclinic and tetragonal phases at 450° C. Tetragonal zirconia was synthesized from the polymer including 4.3 mol % yttrium compound (2.2 mol % yttria) after heat treatment at 1200° C for 1 h. The precursor fibres were pyrolysed to yield fine-grained fibres of tetragonal zirconia at 1200° C for 1 h.     

纳米四方多晶氧化锆粉体的低温制备及反应机理研究

采用引入有机添加剂的低温超强碱法制备出纳米四方多晶氧化锆粉体.采用X射线荧光光谱、X射线衍射、透射电镜对粉体物相组成和微观结构进行了分析.结果表明,有机添加剂-低温超强碱法在反应初期氧化锆晶核就已经形成,这与普通的湿化学法显著不同;同时有机添加剂的引入,在反应开始就减少了粉体的团聚,利于获得分散性好的高质量粉体;所制备的粉体具有粒度小、粒度均匀和分散性好等特点;该方法具有低温高效节能的特点.     

由醋酸锆前驱体制备ZrO_2连续纤维的过程及研究

为了制得耐高温、高强度的氧化锆连续纤维,利用新制醋酸锆作为前驱体,通过溶胶－凝胶法合成含有Ｚｒ－Ｏ长链的溶胶,干法纺丝,制备ＺｒＯ２连续纤维．研究了醋酸锆的光谱和热学性质,并对烧结后的纤维做扫描电镜观察、ＸＲＤ分析和纤维抗拉强度的测试．测试结果表明醋酸锆前驱体溶胶中含有以Ｚｒ－Ｏ为骨架的长链,具有良好的可纺性和稳定性．直径在十几个微米以下的连续纤维具有一定的强度和韧性,添加 ５ｍｏｌ％的 Ｙ２Ｏ３可将 ＺｒＯ２的晶相稳定在四方相．     

Solution phase synthesis of t-ZrO2 nanoparticles in ZrO2–SiO2 mixed oxide

A solution phase synthesis is used to prepare tetragonal zirconia nanoparticles. Ammonia solution and zirconia precursor solution were prepared separately and then mixed together to get colloidal hydroxide precipitate. The colloidal hydroxide was treated with silica sol and then the precipitate was separated and dried. The dried powder was then calcined at different temperatures for 2 and 6?h. The mean particle size of the powder calcined at 1000°C was found to be around 8–10?nm. The thermal analysis of dried powder indicates the formation of bulk tetragonal zirconia phase at 780°C. X-ray diffraction (XRD) and infrared spectroscopic analyses confirm the presence of 100% tetragonal zirconia phase in the powder calcined at 1000°C. The addition of silica stabilised the tetragonal zirconia phase. It is advantageous to use this powder as catalyst or catalyst support that operates at high temperatures.     

溶胶-凝胶法制备钇掺杂氧化锆的工艺研究

论述了用溶胶-凝胶法制备钇掺杂的氧化锆前驱体的过程,系统地研究草酸溶液的浓度、pH值、加热温度以及添加方式对溶胶、凝胶的影响,得出制备氧化锆前驱体的最佳工艺条件:当氧氯化锆溶液与草酸溶液的浓度比为1.25～2,草酸溶液pH值为1～2,加热温度为40～80℃,制得的前驱体溶胶、凝胶均匀,透明.正加方式得到的溶胶淡蓝色透明,较反加方式下的溶胶的胶凝时间短.并对最佳工艺条件制备的粉体进行SEM分析,结果表明,很好地合成了钇掺杂的纳米氧化锆粉体.     

Preparation and characterization of an Al2O3–ZrO2 nanocomposite,Part I: Powder synthesis and transformation behavior during fracture

An alumina–zirconia composite containing 5 mol% zirconia was prepared by following a wet interaction process in aqueous medium via the sol–gel route. The formed hydrogel which was aged for proper growth and orientation at room temperature, was then dried at a low temperature to minimize agglomeration. The sol–gel derived precursor powder was properly characterized through determination of surface area, particle size and thermal analysis. The sintering behavior was studied by compacting the nano-powder through cold isostatic pressing where maximum densification of 98.4% was achieved at 1550 °C. During Vickers indentation using a 5 kg load, cracks were propagating around the grain boundaries and fractured the ZrO₂ particles, which was associated with t-ZrO₂ to m-ZrO₂ transformation. Sintering was studied in the absence of a mineraliser.     

Cellulose tris(3,5-dimethylphenylcarbamate)-coated zirconia as a chiral stationary phase for HPLC.

In this work we explore the use of microparticulate porous zirconia coated with cellulose tris(3,5-dimethylphenyl-carbamate) (CDMPC) as a support for separation of chiral compounds by HPLC. The surface of zirconia, previously sintered but not rehydroxylated, provides a stable surface for depositing the chiral polymer. Zirconia's surface prior to coating was investigated by diffuse reflectance FT-IR. The spectra indicate the presence of residual hydroxyl groups even after treatment at 750 degrees C for 5 h. The amount of chiral polymer deposited was systematically varied, and the pore structure of the resulting particles was assessed by nitrogen sorptometry. Dynamic studies of columns packed with these stationary phases were also conducted. We found that columns packed with about 3-4% (w/w) CDMPC coated on 2.5-micron zirconia particles provide an excellent compromise between loading need to impart good chiral recognition ability to the stationary phase and column's chromatographic efficiency. Preliminary results show resolutions higher than 1 for 9 out of 16 racemic mixtures in packed 5-cm columns. The use of shorter columns combined with reduced particle size to provide sufficient resolution has the advantage of decreasing the analysis times and reducing eluent volumes. CDMPC-coated zirconia columns exhibit high stability under normal-phase conditions at relatively high linear velocities.