一类新型催化剂载体材料的制备研究

用共沉淀法制备了NZP族磷酸盐类催化剂载体材料，着重研究了煅烧温度度不同的栽体化学组成对其物相、比表面积和孔结构的影响。所制备的载体通过BET氮吸附法（BET）、X射线衍射（XRD）以度透射电镜（TEM）对其进行了表征。结果表明：用共沉淀法制备NZP族栽体的合适的煅烧温度为700℃至900％，此娄栽体的比表面积在10m^2／g至40m^2／g之间，煅烧温度对载体的物相结构和比表面积有很大影响。     

NZP族磷酸盐材料研究进展

NZP族精细磷酸盐材料是一类具有相同晶体结构特征但化学组成各异的结晶化合物粉体及其陶瓷烧结体。综述了NZP族磷酸盐化合物的晶体结构特征、合成方法、NZP族陶瓷的快离子导电性、离子取代性、低热膨胀特性及其应用领域。介绍了NZP族磷酸盐材料作为抗热震催化剂载体和新型介孔分子筛催化剂的研究进展。     

共沉淀法制备CoFe_2O_4纳米颗粒及其磁电性能表征

通过热力学计算确定Me-NaOH-NH_3·H_2O体系中钴离子和铁离子的最佳共沉淀pH值,然后采用化学共沉淀法制备了CoFe_2O_4的前驱体粉体,再经过热处理制得纯相CoFe_2O_4粉体,并用X射线衍射仪、扫描电镜、振动样品磁强计和精密阻抗分析仪对其进行表征。结果表明,在pH值=11.4的的共沉淀条件下制备得到前驱体粉体,经400℃煅烧就已经开始形成CoFe_2O_4粉体,温度继续升高生成纯相粉体;并且样品的饱和磁化强度Ms、剩磁Mr及矫顽力Hc随温度升高先增大后减小,在500℃(接近居里温度点)附近达到最大值分别为Ms=14.40A·m~2/kg,Mr=3.15A·m~2/kg,Hc=3.22kA/m,与以往研究报道不同。     

Ca0.6Mg0.4Zr4P6O24粉体的合成

Ca0.6Mg0.4Zr4P6O24属于NZP结构族化合物,NZP陶瓷材料是一类新发现的低膨胀材料,其典型组成是NaZr2P2O12.本研究采用化学计量的ZrO(OH)2沉淀与Ca2+、Mg2+离子的酸式磷酸盐溶液混合,在80℃烘干.经900℃/16小时煅烧,合成出Ca0.6Mg0.4zr4P相粉体.利用DTA、TG和XRD研究了沉淀一溶液混合法合成Ca0.6Mg0.4Zr4P6O24相的温度和机理.     

并流共沉淀法合成Dy_(2)O_(3)-ZrO_(2)纳米粉体EI北大核心CSCD

采用并流化学共沉淀法合成了Dy_(2)O_(3)掺杂ZrO_(2)(DySZ)纳米粉体材料,系统研究稳定剂掺杂量、阳离子浓度、反应系统pH值和煅烧温度对粉体材料物相组成、晶体结构和微观形貌的影响。结果表明:不同合成工艺条件下,DySZ粉体材料均具有纳米尺度特征,球形颗粒尺寸为10~30 nm,Dy_(2)O_(3)的掺杂可以起到稳定晶型的作用;稳定剂掺杂量对DySZ粉体的物相组成具有明显影响,掺杂量为10%(质量分数)时可合成单一四方相结构的DySZ粉体;DySZ粉体材料的四方度和微观形貌对稳定剂掺杂量、阳离子浓度、反应体系pH值和煅烧温度均不敏感,但其平均晶粒尺寸随稳定剂掺杂量、阳离子浓度和反应体系pH值的升高略有降低,随煅烧温度的提高而显著增加。     

制备工艺对纳米级铟锡氧化物(ITO)形貌和电性能的影响

以SnCl4·5H2O、In和浓盐酸为原料,采用化学共沉淀法制备出了纳米级锡掺杂氧化铟(ITO)导电微粉,系统地研究了掺杂量,共沉淀温度,pH值,热处理时间、温度对粉体粒度、形貌和电性能的影响规律。研究表明,合成的ITO粉体分散性较好、导电性能优异,粒径在40nm左右具有立方铁锰矿结构。在ITO纳米导电粉的制备过程中,共沉淀温度和滴定终点pH值对其形貌和性能有很大影响,当共沉淀温度在60℃左右,pH=6时制得的粉体性能最佳。煅烧条件对粉体的形貌、粒度和导电性也有较大的影响,在700℃,4h条件下可以制得导电性能良好,结晶完好,粒度分布均匀的ITO粉体。掺入Sn(Ⅳ)的量对载流子的迁移率有很大的影响,在掺杂浓度为10%左右可制得导电性极佳的纳米ITO粉体。     

阴极材料Ba0.5Sr0.5Co0.8Fe0.2O3-σ合成工艺优化

为了在较低温度下合成具有高纯度的阴极材料Ba0.5Sr0.5Co0.8Fe0.2O3-σ(BSCF),采用X射线、扫描电镜以及能谱分析等方法,研究了共沉淀合成法中溶液pH值和煅烧温度等工艺条件对产物的相结构、组成成分和颗粒形貌的影响.结果表明,pH值的升高使前驱体由草酸盐沉淀向氢氧化物沉淀转化,在pH=10条件下,前驱体1100℃煅烧2 h后形成了单一的立方型钙钛矿型结构,比在pH=6条件下的前驱体煅烧温度降低了约100℃,而且成分配比更为准确.研究认为前躯体溶液的pH值对煅烧产物的组成和形貌影响至关重要,这主要是由于pH值的不同改变了前驱体的组成和颗粒形貌造成的.     

共沉淀法制备复合钙钛矿结构PLZST的研究

用改进的化学共沉淀法制备PLZST前驱体,讨论了共沉淀的最佳pH值范围.通过DTA-TG和XRD详细研究相组成随煅烧温度的变化,并通过和固相合成PLZST多晶料的条件比较可知,共沉淀法合成PLZST多晶料具有纯度高、组份均匀、合成温度低等特点.研究表明在700℃低温下即能合成纯钙钛矿相PLZST多晶料.利用化学分析法测定不同温度下合成的PLZST的铅含量表明低温下合成的PLZST,铅挥发量极少,不会由于铅的挥发造成计量比的改变和形成杂相.     

纳米ITO粉体制备中试剂及影响因素的研究

铟锡氧化物(Indium tin oxide)是一种优良的透明导电氧化物材料.叙述并对比了目前制备ITO粉体的几种方法的优缺点.对其中的化学共沉淀法和化学滴定法,讨论了从铟锡化合物的物理化学性质来选择原料和沉淀剂,分析了制备过程中各种离子的浓度、沉淀时的温度、终点pH值、煅烧温度的范围及时间、分散剂等影响因素.     

Sb掺杂SnO2（ATO）的制备及表面电荷对粉体导电性影响

以Na2SnO3.5H2O和Sb2O3为锡锑源,HNO3为沉淀剂,采用共沉淀法制备了结晶性良好,颗粒尺寸为7～10nm的Sb掺杂SnO2(ATO)纳米颗粒。借助XRD、TEM、EDS、粉体电阻率测试仪、zeta电位测试仪等研究了合成体系pH值、洗涤方式、表面活性剂、煅烧温度等因素对ATO性能的影响。结果表明,体系pH值对粉体颗粒尺寸和电导率影响显著。优选条件下,控制合成体系pH值为3,并经800℃煅烧所得ATO的晶粒尺寸约为8nm,电阻率为0.444Ω·cm。     

硅灰石制备多孔高比表面积二氧化硅机理探讨

通过对用硅灰石与盐酸反应制备多孔高比表面积SiO2最佳实验工艺条件的研究,确定了最佳试验工艺条件,即反应速度、反应时间、中和速度、反应最终pH值与SiO2比表面积的关系,探讨了其合成的机理。研究结果表明,当pH≤1.0时,硅灰石与盐酸反应生成大量稳定的硅酸溶胶;反应最终(pH＝4.0)使硅酸水解和缩聚以及Si—O与OH基团氢键的形成以适宜的速度进行,形成弱交联、网状、低密度的硅酸凝胶,最终产物SiO2的比表面积增大。     

液相沉淀法工艺条件对羟基磷灰石粉体的影响

采用液相沉淀法成功制备纳米羟基磷灰石陶瓷粉体,使用X-射线衍射、扫描电子显微镜等检测手段分析了粉体的组织结构,研究了反应温度、pH值、陈化时间对粉末粒径和物相组成等的影响。结果表明,反应温度为90℃、溶液pH值为10、陈化12 h,在700℃煅烧2 h可制备出高纯度、晶体完整的球形羟基磷灰石粉体,平均尺寸为60 nm。     

超细镍粉的制备及还原生长机理研究

以联氨为还原剂,在硫酸镍水溶液中控制液相还原反应条件制备了超细镍粉,并讨论了超细镍粉的还原生长机理.通过实验分析了工艺参数对还原反应的影响,采用X射线衍射(XRD),扫描电镜(SEM),比表面积测定等分析手段对超细镍粉进行表征,结果表明:超细镍粉的形核和生长独立进行;温度、Ni2+浓度和pH值调控着溶液中镍离子的释放并...     

Glass reactive sintering as an alternative route for the synthesis of NZP glass–ceramics

The NZP-type crystal structure allows a large number of ionic substitutions which leads to ceramics with adjustable thermal expansion properties or interesting ionic conductivity. However, NZP is difficult to fabricate into monoliths because it requires both high temperatures and long sintering times. An alternative low temperature route to obtain a tungsten (IV) and tin (IV) containing NZP crystalline phase uses a process of glass reactive sintering of a phosphate glass. Using a microwave oven, a glass with the appropriate composition in the NaPO3–Sn(II)O–W(VI)O3 ternary diagram is prepared by a conventional melting and casting technique. After crushing, the glass powder is pressed at room temperature. The green pellet is cured during various times at temperatures where glass reactive sintering takes place. From XRD and DTA experiments, we have shown that different parameters influence the achievement of NZP phase. Consequently, specific conditions, such as (i) initial glass composition, (ii) equimolar quantities of SnO and WO3, (iii) glass particle size lower than 100 μm, and (iv) curing conducted under air, are required to obtain a glass–ceramic with a single crystalline phase with the NZP-type crystal structure.     

高纯ZnAl_2O_4纳米颗粒的制备及其微结构分析

将机械力化学与超声波化学相结合制备出高纯度、结晶性良好的尖晶石型ZnAl_2O_4纳米颗粒。分析了样品的表面形貌、晶体结构及微观结构。研究结果表明:当焙烧温度为600~900℃时,ZnO与γ-Al_2O_3固相反应制备出高纯度、结晶性良好的尖晶石型ZnAl_2O_4纳米颗粒。随着焙烧温度的升高,材料的致密度增大,结晶度提高,平均孔径依次增大,比表面积明显下降,孔隙率降低。     

Preparation of copper powder by glycerol process

A simple, least energy intensive, efficient, low temperature chemical process for the production of copper powder of narrow size distribution is described. It involves reduction of copper salts by glycerol under atmospheric conditions at a temperature below 240°C. The powders produced by this process have been characterized by X-ray diffraction, chemical composition, BET surface area analysis and scanning electron microscopy. The powder is well crystalline and contains oxygen, carbon, and hydrogen as impurity elements. The purity of the powder produced by the process depends on the starting compound of copper. The glycerol process using copper acetate as starting compound yields copper powder having a purity of 99.7%.     

天然热释电材料电气石的微结构及对水的pH值影响机理的研究

以新疆产天然电气石为原料制备了电气石微粉,利用X射线衍射仪、扫描电镜、高分辨电镜、pH酸度计研究了电气石的物相、微结构特点和电气石对水酸度及其随温度变化的影响.结果表明,电气石单个微粒为单畴的铁电体,可视为电偶极子;利用电气石微粉可以使水的酸度呈弱碱性;电气石对水酸度的影响随温度的变化进一步佐证了电气石的热释电性,并探讨了电气石对水作用的可能机理.     

Formation characteristics of an aluminum hydroxide fiber by a hydrolysis of aluminum nano powder

Formation of aluminum hydroxide by a hydrolytic reaction of nano aluminum powder synthesized by a pulsed wire evaporation (PWE) method has been studied. The type and morphology of the hydroxides were investigated with various initial pH and temperatures. The nano fibrous boehmite (AlOOH) was formed predominantly over 40°C of the hydrolytic temperature, while the bayerite (Al(OH)₃) was formed predominantly below 30°C with a faceted crystalline structure. As a result, the boehmite showed a much larger specific surface area (SSA) than that of bayerite. The highest SSA of the boehmite was found about 409 m²/g.     

Thermal expansion studies on the Sodium Zirconium Phosphate family of compounds A1/2M2 (PO4)3: effect of interstitial and framework cations

Thermal expansion of the sodium zirconium phosphate (NZP) family of compounds A_1/2M₂(PO₄)₃ (A = Ca or Sr; M = Ti, Zr, Hf or Sn) has been measured in the temperature range 298–1273 K by high-temperature X-ray powder diffractometry. Some of the compounds in the series (calcium zirconium phosphate and calcium hafnium phosphate) display the typical thermal expansion behaviour of NZP compounds, namely expansion along the hexagonal c axis and contraction along the a axis. The other compounds, depending on their interstitial and framework composition, behave differently. The observed axial thermal expansion and contraction behaviour is explained on the basis of the crystal chemistry of the compounds. Low-expansion compounds in this series are identified and their expansion anisotropy examined. Infared spectra of the compounds are reported. Differential scanning calorimetry measurements on the tin compounds indicate the occurrence of a diffuse phase transformation at high temperatures.