草酸铵沉淀法制备纳米氧化钇研究

以氧化钇、浓硝酸为原料,草酸铵为沉淀剂,十六烷基三甲基溴化铵为分散剂,采用草酸铵沉淀法制备纳米氧化钇前驱体,将前驱体在空气中焙烧制备纳米氧化钇粉体。用差热-热重分析确定了前驱体分解温度,用 X射线衍射和扫描电镜对样品进行表征,用激光粒度仪测量不同反应物物质的量比所得产品的粒度分布,得到制备纳米氧化钇最佳条件。实验表明,在最佳条件下可以制得平均粒径为40 nm的氧化钇粉体,其形貌为椭球形。     

溶胶-胶水热合成法制备纳米CoAl2O4粉体

以仲丁醇铝和硝酸钴为原料,用溶胶-凝胶水热合成法制备了纳米CoAl2O4粉体,探讨了水热合成中前驱体的制备工艺条件,并用X射线衍射和扫描电镜等手段分析了水热系统中反应温度、反应时间对纳米CoAl2O4粉体的形成以及形貌的影响.结果表明:前驱体在250℃的水热系统中反应24 h,能制备出较纯净、结晶完整、粒度均匀、粒径小、尖晶石结构的纳米CoAl2O4粉体,其平均粒度约为50～60nm.     

纳米氧化钕的制备及其性能研究

以硝酸钕和碳酸铵为原料,用直接沉淀法制备纳米氧化钕.讨论了碳酸铵浓度、煅烧时间以及不同添加剂对氧化钕粒径的影响,通过添加活性炭成功地解决了干燥和煅烧前驱物的硬团聚问题,确定了制取纳米氧化钕的最佳工艺.用XRD,SEM和TG-DTA手段对产物进行表征,结果表明,在一定条件下可获得粒径为30 nm的氧化钕,合成的氧化钕为六方型.工艺简单、操作方便.用制得的氧化钕作催化剂合成乙酸正丁酯,反应时间短,并且可重复利用,产率为54%左右.     

超细氧化钇合成与表征

以硝酸钇为原料,氨水、碳酸铵、酒石酸铵为沉淀剂,聚乙二醇、十二烷基苯磺酸钠、十六烷基三甲基溴化铵为表面活性剂,在水溶液中制备氧化钇前驱体,在空气中焙烧制备氧化钇粉体;用X射线衍射(XRD)、扫描电镜(SEM)、红外光谱(IR)对样品进行表征,用激光粒度仪分析样品的晶粒团聚度.结果表明,使用氨水、碳酸铵、酒酸铵为沉淀剂所得前驱体在673 K焙烧2 h,均获得立方晶相氧化钇粉体,一级晶粒直径分别为13,40,63 nm;用小分子有机醇回流处理氧化钇前驱体(氢氧化钇),团聚体粒径为58.8 nm,焙烧后的氧化钇团聚体粒径为423 nm,说明有机醇回流处理阻止了粒子团聚.     

氨解法制备超细高纯氮化铬粉体的研究

以氨水直接沉淀法制备的CrO3为前驱体，采用氨解法制备了超细CrN粉体。对不同氨解温度、氨解时间和不同前驱体合成的CrN粉体用x射线衍射（XRD）、扫描电镜（SEM）和氮／氧分析仪等方法进行了表征。研究了反应温度、时间和前驱体粒度对CrN粉体性能的影响。结果表明。在800℃氮化12h可得到纯度为99％以上的高纯超细CrN粉体。     

室温固相反应制备超细前驱体及其分散性的研究

研究以结晶氯化铝和碳酸氢铵为原料，采用室温固相反应制备尺寸均一、颗粒细小分散的包含有少量纳米晶γ-AIOOH的碱式碳酸铝钱前驱体。用XRD、Zeta电位及粒度分析仪表征，研究了起声分散、聚乙二醇聚合度及其加入量和pH值等对制备起细前驱体的影响。结果表明：在起声分散及酸性条件下，PEG为不同分子量匹配得到的前驱体．在水中的分散和稳定性最好，并制备出比表面高达66.32m^2／g（1100℃煅烧）的纳米α-Al2O3粉体。     

柠檬酸凝胶法制备Mn-Ni-Fe基负温度系数热敏陶瓷

采用柠檬酸凝胶法制备锰-镍-铁基前驱体,在300℃煅烧干燥的前驱体得到纳米粒度粉末,压制成圆片坯体后在1100～1300℃烧结得到负温度系数(negative temperature coefficient,NTC)热敏陶瓷样品。研究了粉体和烧结样品的相结构、微观形貌、电性能和热敏特性。结果表明:合成粉体的纳米颗粒为单相Mn1/3Ni2/3Fe2O4尖晶石,粉体具有高化学均匀性。烧结的Mn1/3Ni2/3Fe2O4陶瓷样品具有均匀的微观结构,陶瓷样品的烧结密度和材料敏感指数β随着烧结温度的增加而增加。测量温度为50～150℃范围时,1300℃烧结的Mn1/3Ni2/3Fe2O4样品,其β可高达4300K。     

固相法制备高纯纳米碳化硼

以聚乙烯醇为碳源,硼酸为硼源,利用固相热反应法制备了高纯度纳米碳化硼(B_4C)粉体,用红外光谱分析、X射线衍射仪、场发射扫描电子显微镜对产物的物相、结构与形貌做了表征,并研究了制备条件对碳化硼粉体的影响。结果表明,将聚乙烯醇与硼酸在250℃以下反应可制备聚合物前驱体;将该聚合物前驱体于750℃低温裂解2 h可以得到裂解前驱体;该裂解前驱体在1 450℃下反应2 h,可得到高纯纳米碳化硼。     

轻烧菱镁矿制备高纯纳米氧化镁

以轻烧菱镁矿为原料,通过酸浸去除杂质得到纯净的含镁溶液,以草酸为沉淀剂,采用直接沉淀法制备纳米氧化镁粉体。考察了草酸和氧化镁的摩尔比、反应温度、前驱体草酸镁热分解温度及时间对纳米氧化镁粒径大小的影响。采用热重-差热分析仪、激光粒度仪、X射线衍射仪、扫描电子显微镜等对前驱体的热分解情况、产品的粒径及晶型结构进行检测。结果表明:合成的氧化镁粉体的粒径分布较窄,分散性良好,平均粒径在80nm左右,纯度达到99.1%。     

草酸沉淀法制备超细氧化镧粉体研究

以工业生产萃取、分离及提纯过的稀土氯化镧溶液为原料,一定条件下制备出D₅₀小于10 μm的超细氧化镧粉体,研究了制备过程中焙烧温度、分散剂种类、溶液pH对氧化镧粉体粒径分布的影响。用激光粒度仪测得样品的粒度分布,用X射线衍射和扫描电镜对样品进行表征。结果表明,焙烧温度为750 ℃、焙烧时间为2 h、加入质量分数为1%的分散剂PEG2000,在酸性反应条件下可制备出粒度均匀,分散性好的超细氧化镧粉体。     

Isothermal Crystallization Studies on Neodymium Oxide Filled Nylon 6

Melt mixing of nylon 8 with neodymium oxide particles was carried out with a single-screw extruder. The crystal behaviors of plain nylon 6 and the neodymium oxide filled nylon 6 mixture were studied by means of isothermal crystallization kinetic analysis. Isothermal crystallization thermograms obtained by differential scanning calorimetry (DSC) were analyzed based on the Avrami equation. The neodymium oxide particles acted as a nucleating agent in the mixture. The overall rate of di-isothermal crystallization of the neodymium oxide filled nylon 6 mixture is higher than that of plain nylon 6. The mechanism and modes of plain nylon 6 were the same as those of neodymium oxide filled PA6 mixture.     

钴钕软磁性复合氧化物的溶胶-凝胶法合成及表征

以Co(NO3)2.6H2O和Nd(NO3)3.6H2O、PVA等为原料,采用溶胶-凝胶法制备出前驱体,将其高温煅烧获得钴钕复合氧化物粉体。通过TG-DSC、FT IR、Raman、TEM、XRD、PPMS等检测对前驱体及产物的物性和结构进行表征。结果表明:钕元素已掺入到钴氧化物的晶格之中,形成了优良的软磁性钴钕复合氧化物。     

Synthesis and characterization of neodymium doped ceria nanocrystalline ceramic structures

In this study, a new method to synthesize neodymium doped ceria ceramic nanopowders by the electrospinning of the hybrid polymers solution of their composite precursor was put forward. Calcined and sintered nanopowders were characterized by FT-IR, XRD, BET, SEM, and AFM techniques. According to the XRD analysis, the obtained powders are single phase and independent of the dopant concentration in the range investigated. The crystallite sizes were calculated using Scherrer equation. Moreover, lattice parameters, dislocation densities and microstrain values were calculated. BET results show that the increase of the neodymium doped content decrease the surface area of the composite powders, confirming the highly ordered micro and mesostructure. SEM and AFM results show that the samples have spherical grains. According to the surface roughness measurements, the increase in the amount of neodymium and the decrease in the amount of cerium decreased the surface roughness.     

不同碳酸盐沉淀剂热分解法制备纳米氧化锌

以硝酸锌为锌源,分别以碳酸钠和碳酸氢铵为沉淀剂,采用热分解碱式碳酸锌工艺制备纳米氧化锌。通过热重分析、晶型测试、平均粒径测试、微观形貌观察等系列对比,分析了以两种碳酸盐为沉淀剂制备氧化锌的过程,建立了生长动力学方程,对比了微观形貌和分散状态。实验结果表明,以碳酸氢铵为沉淀剂制备的前驱体在煅烧温度为200 ℃后直接生成纳米氧化锌,而以碳酸钠为沉淀剂制备的前驱体在煅烧温度为200~250 ℃时先生成碳酸锌然后在300 ℃时完全转变为氧化锌;两种沉淀剂制备纳米氧化锌的生长过程符合不同指数方程生长关系,以碳酸钠为沉淀剂制备纳米氧化锌的生长满足方程y=2.775 04e^{0.004 76x},而以碳酸氢铵为沉淀剂制备纳米氧化锌的生长满足方程y=5.152 96e^{0.002 85x},对比来看以碳酸氢铵为沉淀剂制备纳米氧化锌在相同温度下得到的晶粒尺寸要小;从粒度分布和透射电镜观察分析,在相同温度下也是以碳酸氢铵为沉淀剂制备的纳米氧化锌的粒径较小。     

Oxidative coupling of methane over strontium-doped neodymium oxide: Parametric evaluations

Since its discovery in 1982, oxidative coupling of methane (OCM) has been considered one of the most promising approaches for the on-purpose synthesis of ethylene. The development of more selective catalysts is essential to improve process economics. In this work, undoped neodymium oxide as well as neodymium oxide doped with high (20%) and low (2.5%) levels of strontium were tested in a high-throughput fashion covering a wide range of operating conditions. The catalysts were shown to be able to achieve greater than 18% C₂+ yield. Space velocity was shown to play a significant role in C₂+ selectivity. For a methane to oxygen feed ratio of 3.5, selectivity increased with increasing space velocity, reaching a maximum of 62% at a methane conversion of 30% at an optimal space velocity of ~250,000 ml/h/g. The difference in activity between the three samples was linked to the contribution of different oxygen centers.     

工业级纳米氧化锌的合成及性能

以七水硫酸锌、碳酸氢铵为原料,通过液相沉淀法合成纳米氧化锌前体,并焙烧获得纳米氧化锌。本文采用XRD、TG-DSC、TEM、BET等测试手段对纳米氧化锌及其前体进行表征,研究了焙烧温度对所制备氧化锌形貌、晶型及脱硫活性的影响,结果表明:所获得的碱式碳酸锌为不规则纳米晶,晶粒尺寸约为2~10nm;在不同的焙烧温度下所获得的纳米氧化锌的综合性能存在较大差异,其中在焙烧温度300℃处理所得纳米氧化锌综合性能较高,其晶粒尺寸为5~10nm之间,结晶度较完整,比表面积为41.41m²/g,在220℃脱硫活性较高,穿透硫容>25%;随着焙烧温度的提高,纳米氧化锌的晶化程度加大,表面性质被破坏,比表面积急剧下降,颗粒团聚严重;焙烧温度太低,则纳米氧化锌前体分解不完全,影响其纯度。     

体相掺镁球形钴酸锂前驱体的制备及表征

文章通过沉淀法合成了体相掺杂镁元素的球形钴酸锂正极材料前驱体。通过SEM形貌、密度测量、粒度表征等手段研究了共沉淀工艺对合成体相掺杂镁元素钴酸锂前驱体的影响,并通过EDS及ICP测试表征了镁元素掺杂的均匀性。研究结果表明:共结晶的反应时间对颗粒密度、颗粒形貌、粒度大小及分布有较大的影响,随着时间延长密度逐渐增加,颗粒形貌变好,粒度变大且趋于集中;共结晶体相掺杂镁的钴酸锂前驱体,镁元素能达到原子级混合均匀的要求;掺杂镁后,钴酸锂前驱体四氧化三钴物相未发生变化。掺镁钴酸锂前驱体在高压实密度钴酸锂得到了广阔的应用。     

Total oxidation of methane over doped nanophase cerium oxides

The formation of solid solutions of cerium oxide with the oxides of calcium, manganese, or neodymium enhances the catalytic activity of cerium oxide for the total oxidation of methane, whereas solid solutions with lead oxide showed an opposite effect. Reasons for this are discussed in terms of oxygen vacancy concentrations and mobilities, local structure configurations, number of oxidation states of dopant, and electron transfer properties. The effects of increased oxygen ion mobility and a more beneficial local structure support the increased catalytic activity for the calcium- and neodymium-doped cerium oxide samples. In addition, a reduced energy for charge transfer from oxygen to cerium supports a higher activity for the calcium-doped sample. The activity data were fitted to an Arrhenius equation, and the apparent activation energies were found to be between 110 and 130 kJ/mol. The particle sizes and the BET areas of the samples were only little affected by the reactor runs, and none of the samples were subjected to phase changes. This revised version was published online in July 2006 with corrections to the Cover Date.     

Effect of process parameters on the production of nanocrystalline silicon carbide from water glass

Nanocrystalline silicon carbide was synthesized from the precursor prepared by spray drying slurry of water glass and carbon black. The effect of process parameters, such as reaction temperature, reaction time and carbon content, on phase evolution, crystallite size and specific surface of the resulting samples were characterized by XRD, SEM and BET. The results show the powder produced in this process has a very fine crystallite size and high specific area and the reaction can be completed at 1550 °C for 2 h when the C/Si ratio is 5 or larger. In addition, the powder is of high purity, because sodium oxide in the precursor can be eliminated by the escape of sodium at high temperature. It is a simple and cost-efficient method to synthesize nanocrystalline silicon carbide using cheap and abundant water glass as silicon source.     

稀土氧化钕填充尼龙6体系的流变行为研究

用锥板粘度仪测试仪测试了稀土氧化钕填充尼龙６体系的流变行为，填充体系的熔融粘度明显低于空白尼龙６，体系的粘度随稀土氧化物含量的增加而降低，填充后试样具有良好的流动性和加工稳定性。