单分散钛酸钡纳米晶的制备

采用溶剂热法制备出表面包裹油酸的单分散立方相钛酸钡纳米晶, 晶粒平均尺寸为6.0 nm, 采用TEM和XRD对其微结构进行了表征; 研究了醇的链长度、油酸用量和热处理温度等对钛酸钡的相组成和形貌的影响规律. 研究结果表明, 产物粒径较小, 粒度分布较窄, 单分散性较好, 其表面为非极性, 可溶于非极性试剂; 由于纳米晶表面由亲油性的长链烷基所覆盖, 与周围的水性环境不相容, 产生一定的斥力; 在重力和该斥力的共同作用下, 纳米晶可以有效地从液相环境中分离出来.     

纳米晶钛酸钡的介电性能

采用硬脂酸凝胶法制备了纳米晶BaTiO3,用差热热重分析、红外光谱分析、X射线衍射分析等手段对产物的形成过程、晶型、粒径进行了分析.通过对材料介电性能的研究发现,纳米材料的静态介电常数远大于常规材料的介电常数,随着粒径的减小,纳米材料的介电常数先增大而后有所降低.随着环境湿度的升高,纳米晶材料的介电常数逐渐增大,在高湿度条件下,其介电常数与湿度成线性关系.     

微波液相沉淀法制备CeO2纳米晶

以硝酸铈为原料,碳酸氢铵为沉淀剂,用微波加热的方法制备了纳米CeO2超细粉体,用X射线衍射法和透射电子显微镜等检测手段进行表征,结果表明,微波法制备样品的平均晶粒度为8nm,而传统加热法则为16nm,反应时间由60分钟缩短为5分钟,并提高了颗粒的分散性.     

BaTiO3纳米晶的制备和结构

ＢａＴｉＯ_３纳米晶的制备和结构方佑龄，赵文宽，邹化民，王仁卉（武汉大学化学系，武汉大学物理系，武汉，４３００７２）关键词钛酸钡纳米晶，过氧化物，制备，结构ＢａＴｉＯ３具有高介电常数及优异的铁电、压电性能，是一种重要的电子陶瓷材料，因此，对其纳米晶的?..     

简捷水热前驱物技术制备钛酸钡纳米棒与纳米球

A facile synthesis route has been developed to prepare barium titanate nanoparitcles via a low temperature (120 ℃) hydrothermal decomposition of single-source metal-organic precursor. A mixture of tetramethylammonium hydroxide (TMAH) and distilled water was used as reaction media, and Barium titanium ethyl-hexano- isoproxide [BaTi(O₂CC₇H₁₅)(OC₃H₇)₅] was used as precursor. The architecture of products can be selectively controlled from nanorods to nanospheres by adjusting the precursor′s concentration in the reaction system. Powder X-ray diffraction (XRD) analysis indicated that the products were in cubic phase. Transmission electronic microscopy (TEM) observation showed that the nanospheres were 30～50 nm in diameter, and the nanorods were 5～10 nm in diameter and 100～600 nm in length, respectively. Phase transformation behavior of the as-prepared products was also investigated.     

微波法制备金属钴纳米晶棒及其表征

微波法制备金属钴纳米晶棒及其表征;微波法;钴;纳米晶棒;表面活性剂;表面修饰     

掺镁钛酸钡纳米棒的水热合成和光催化性能

用水热法制备掺镁钛酸钡(Ba1-xMgxTiO3(x=0,0.10,0.20,0.30,0.40),BMT)纳米粉体。运用X射线衍射仪(XRD)、场发射扫描电子显微镜(FESEM)、透射电子显微镜(TEM)、紫外可见漫反射光谱技术(DRS)等手段对样品进行了表征,并在可见光照射下于溶液中考察了其光催化降解甲基橙反应活性。结果表明,通过控制氢氧根浓度可以得到不同形貌的纳米粉体。基于不同条件下制备的样品的微结构分析,提出了这些不同形貌的形成机制。制备出的BMT材料的带隙能约为2.61 eV。光催化反应结果表明BMT的光催化活性比掺氮TiO2高得多。OH-浓度为8 mol·L-1时制备的BMT纳米棒光催化效率最高,经可见光照射360 min,浓度为0.01 mmol·L-1甲基橙溶液的降解率可达到93.0%,且循环使用4次后,其光催化活性并没有明显降低,表明BMT是一种稳定有效的可见光催化剂.     

不同形态SnO2纳米晶的制备

In this paper, we report our research on morphologically selective synthesis of nanocrystalline SnO2 by the combination of hydrothermal preparation and calcinated process. We firstly prepared SnO2 nanocrystals by the hydrothermal method at 140 ℃ for 3 h, using SnCI4 as the reactant. With the initial pH of 1.8 or 1.34, we prepared uniform and well-dispersed SnO2(tetragonal) nanocrystals, with similar size of about 3 nm, as determined by TEM. However, after being calcinated at 500 ℃ for 2 h, specimen 1 prepared at pH＝1.8 showed the rod-like shape with an average size of 5 nm×20 nm, while the other one(specimen 2)prepaed at pH＝1.34 showed a granular shape with an average size of 10 nm. XRD experiments showed that specimen 1 had a new diffraction peak after calcination, which was contributed by the (023) face of orthorhombic SnO2. The experiment results indicated that the morpholgy of SnO2 nanocrystals after calcination was closely related to the initial acidity of the reaction solution, possibly due to the difference in surface properties, e.g. the difference in crystalline faces exposed to the surface of particals, under different hydrothermal conditions.     

四方相钛酸钡纳米枝晶阵列的水热合成

采用水热法,在表面活性剂十六烷基三甲基溴化铵(CTAB)和合适的矿化剂NaOH的作用下,得到具有新颖结构的钛酸钡纳米枝晶阵列。X射线衍射(XRD)和拉曼光谱(Raman)结果分析显示该枝晶为四方相,随着时间的延长其结晶性增强、四方相更加明显。利用扫描电子显微镜(SEM)、高分辨透射电子显微镜(HRTEM)和电子衍射(ED)研究了该枝晶的生长特点和生长机理,结果表明该枝晶其各枝均沿着[111]方向生长,并且同级枝相互平行形成阵列;在枝晶阵列的外侧部分会有2级子枝长出,中间部位由于空间阻碍没有子枝形成。同时探讨了CTAB和NaOH在枝晶形成过程中的作用机理,以及枝晶产品的介电性能。     

纳米钛酸钡及其烧结物的制备

溶胶 凝胶技术已为制备各种金属氧化物纳米材料的较普遍方法[1],其优点是产物具有超细颗粒尺寸 ,高纯度和化学均匀性 .溶胶 凝胶法制备纳米钛酸钡时一般将钛的有机醇盐与钡盐反应生成溶胶 ,然后形成凝胶 ,再进行热处理制得纳米钛酸钡[2 ,3].本文以钛酸丁酯和氢氧化钡为原料 ,采用溶胶 凝胶工艺制备出纳米钛酸钡晶体粉末 .用ＴＧ ＤＴＡ和ＦＴＩＲ技术考查了纳米晶钛酸钡凝胶先体热分解反应过程 ,用ＳＥＭ和ＸＲＤ对粉体形貌和晶型进行分析 ;并用上述粉体制成了微观组织结构仍保持纳米尺寸的陶瓷材料 .粉体制备 :称 15 7ｇ氢氧化钡 (Ｂａ(…     

超细钛酸钡粉体的水热合成

以偏钛酸和氢氧化钡为原料,用水热反应制备了超细钛酸钡粉体,其结构经XRD和-IEM表征。粒径60nm-100nm。较佳的反应条件为：偏钛酸20mmol,n(Ba)：n(Ti)=1．2,于240℃反应8h,加入少量异丙醇可明显改善粉体的分散性能。     

溶胶-凝胶法制备掺锰钛酸钡纳米粉体及其陶瓷

The Mn-doped barium titanate nanosized powders and ceramics were prepared via the sol-gel process. The powders and ceramics were characterized by XRD， SEM and TEM. The dielectric properties of the ceramics were also measured. The influences of calcination temperature and Mn concentration on the microstructure， dielectric properties and phase composition of BaTiO₃ nano-powders and ceramics were discussed. The results indicated that the BaTiO₃-based powders doped with 1.0mol% Mn were mainly in cubic BaTiO₃ phase， but the tetragonal phase became more evident when the calcination temperature increased. After sintering， Mn-doped ceramics were mainly composed of cubic BaTiO₃. Specially， a new phase of hexagonal crystal BaTiO₃ and BaMnO₃ existed in the ceramics doped with 5.0mol% Mn and the ceramic grains were in ‘clintheriform’. The structure of ‘clintheriform’ led to the poor densification of ceramics， reducing the dielectric constant obviously. The dielectric constants of BaTiO₃ ceramics first increased and then decreased as the Mn concentration increased. The room temperature dielectric constant was 2 290 and the lowest dielectric loss was 0.004 when the Mn concentration was 0.5mol%.     

Size Effect on Crystal Structures of Barium Titanate Nanoparticles Prepared by a Sol-Gel Method

Barium titanate nanoparticles were synthesized by the hydrolysis of complex alkoxide precursor that was prepared in a reflux of metallic barium and tetraethylorthotitanate in solvent. The hydrolysis was performed by the addition of water/ethanol solution to the precursor solution. As reflux time increased, particle sizes, which were measured with transmittance electromicroscopy, became smaller followed by sharpening of size distribution. As water concentration and benzene content in the hydrolysis increased, the particle size increased with crystallite size that was determined with X-ray diffractometry. No significant difference was observed between the particle and crystallite sizes up to 30 nm. Over the size of 30 nm, the particle size was larger than the crystallite size because of generation of polycrystallites. Annealing treatments in air at 400 and 1000°C also increased both the particle and crystallite sizes. The crystallite sizes estimated from the (111) peaks were smaller than those from (110) peaks in a range of sizes larger than 40 nm, which indicated that the critical crystallite size of transformation from cubic to tetragonal structures was approximately 40 nm.     

溶胶-凝胶模板法制备钛酸钡纳米管

采用氢氧化钡和钛酸四丁酯为前驱体, 溶胶-凝胶结合模板法制备了钛酸钡纳米管, 通过SEM, TEM, XPS和XRD等表征分析, 钛酸钡纳米管直径100 nm, 钛酸钡为立方相结构, 晶胞参数a＝3.995 Å.     

Structural Study of Inclusion Complex of Andrographolide with β-Cyclodextrin Prepared under Microwave Irradiation

Andrographolide (Andro) (Figure 1) is a diterpene lactone isolated from Andrographis paniculate Nees1. It has showed several biological activities including analgesic, antipyretic and anti-inflammatory effects2. However, its poor water solubility and unstability towards oxygen restrained its application. In pharmaceutics, b-CD is used to increase solubility and stability3. We have prepared the inclusion compound of Andro/b-CD (Figure 2) under microwave irradiation4. It has been found…     

微波法制备3.5 G PAMAM树状大分子保护的金纳米粒子

以3.5 G PAMAM(3.5代聚酰胺-胺型)树状大分子为保护剂,利用微波法还原HAuCl₄溶液制备金纳米粒子.考察了当3.5 G PAMAM与HAuCl₄物质的量的比一定时,微波照射不同时间对金纳米粒子大小及形状的影响;以及同一照射条件下,3.5 G PAMAM与HAuCl₄不同的物质的量比值对金纳米粒子大小及形状的影响.利用紫外可见分光光度计、透射电子显微镜对其进行了表征.结果表明,当3.5 G PAMAM与HAuCl₄物质的量的比值一定时,金纳米粒子的形状和大小受微波照射时间长短的影响不大;适当延长照射时间,制得的金纳米粒子的分散性较好.在相同照射条件下,随着3.5 G PAMAM与HAu-Cl₄物质的量比值的减小,得到的金纳米粒子粒径逐渐变大,且分散性变差.     

微波辐射下2-芳基取代苯并噁唑的合成

邻氨基酚和芳香羧酸在微波辐射条件下缩合,合成了4种2-芳基取代苯并噁唑化合物。优化反应条件为：多聚磷酸为催化剂,辐射功率500W,辐射时间4min。     

嘧啶酮衍生物的微波合成

在微波辅助下,Baylis-Hillman加成物与4-氨基-6-氯嘧啶或2-氨基-噻唑反应,快速合成了两类嘧啶酮衍生物——3-取代-7-氯-4H-嘧啶[1,2-b]哒嗪-4-酮和6-取代-5H-噻唑[3,2-a]嘧啶-5-酮,收率81%～98%,其结构经1H NMR,13C NMR,IR和MS确证。