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%.     

溶胶-凝胶法制备钛酸钡超细粉体的研究

钛酸钡是一种非常重要的铁电材料 ,其合成方法主要分为固相反应法和液相反应法。传统的固相反应法是以ＴｉＯ2 和ＢａＣＯ3 经高温反应制取钛酸钡粉体 ,该法产品杂质含量高 ,颗粒粗 ,均匀性差 ,粉体烧结温度高。与高温固相反应相比 ,液相法合成的钛酸钡粉体具有化学纯度高 ,颗粒细小 ,粒度分布均匀等优点。特别是以醇盐为原料 ,采用溶胶 凝胶法制备的钛酸钡粉体 ,其性能非常优异 ,已为许多研究者所关注[1,2 ] 。文献[3 ] 报道了以异丙醇钛和醋酸钡为原料 ,采用溶胶 凝胶法制备钛酸钡物体的研究 ,但未见有以钛酸丁酯及醋酸钡为原料制备钛酸钡…     

磁电CoFe2O4/BaTiO3纳米管的溶胶-凝胶模板法合成和表征

用溶胶-凝胶模板法合成了 CoFe2O4)/BaTiO3(CFO/BTO)复合纳米管,管的直径约为 100、200 和 300 nm,其长度约为100 μm.x射线衍射(xRD)和选区电子衍射(sAED)都显示复合纳米管中同时存在尖晶石相的CoFe2O4(CFO)和钙钛矿相的 BaTiO3(BTO),进一步的透射电子显微镜(TEM)研究证实合成的纳米复合物具有明显的管状结构.磁、电研究表明,该复合纳米管的磁性与纯 CFO 纳米管的磁性相当;而铁电性与纯BTO纳米管的铁电性相当.     

溶胶凝胶模板法制备羟基磷灰石纳米线

以氯化钙和五氧化二磷的醇溶液为前驱体溶液,多孔阳极氧化铝(AAO)膜为模板,通过溶胶凝胶-模板法成功制备出羟基磷灰石(Ca10(PO4)6(OH)2,HAP)纳米线;利用扫描电镜、能量色散谱仪、透射电镜、X射线衍射仪及傅立叶变换红外光谱仪等分析了产物的组成和微结构;并讨论了纳米线的生长机理.结果表明,所制备的羟基磷灰石纳米线直径约为50nm、长度达20μm,分别与模板的孔径和厚度一致.     

氧化铁纳米线阵列的溶胶-凝胶模板法制备与表征

0引言氧化铁在颜料、磁记录材料和催化剂等方面具有广泛的应用[1,2]。尤其是纳米氧化铁在纳米尺度具有良好的气敏特性[3]。纳米材料可以分为零维、一维、二维纳米材料,一维材料是纳米材料的重要组成部分,是纳米组装的基础。一维纳米材料的制备方法中氧化铝模板法占有极其重要的     

磁电CoFe2O4/BaTiO3纳米管的溶胶-凝胶模板法合成和表征

用溶胶-凝胶模板法合成了CoFe2O4/BaTiO3(CFO/BTO)复合纳米管, 管的直径约为100、200和300 nm, 其长度约为100 μm. X射线衍射(XRD)和选区电子衍射(SAED)都显示复合纳米管中同时存在尖晶石相的CoFe2O4 (CFO)和钙钛矿相的BaTiO3(BTO), 进一步的透射电子显微镜(TEM)研究证实合成的纳米复合物具有明显的管状结构. 磁、电研究表明, 该复合纳米管的磁性与纯CFO纳米管的磁性相当; 而铁电性与纯BTO纳米管的铁电性相当.     

WO3纳米管的模板法制备及表征

0引言 WO3纳米材料具有光致变色、电致变色、气致变色等特性,可用于光学信息和储存显示器、pH值探测器、气敏传感器、灵敏窗口等[1,2];并且在太阳能的储存与利用、光电转换、光催化降解大气和水中的污染物等方面有着广阔的应用前景[3,4],成为近几年重点研究的半导体材料之一.以前纳米WO3的制备主要集中在薄膜上,其薄膜的制备工艺已经相当成熟,主要包括蒸发法、溅射法、CVD法、喷涂法、阳极氧化法、溶胶-凝胶法等[3].     

溶胶-凝胶模板法合成SmFeO3纳米线

通过阳极氧化在质量分数为0.3 mol·L^-1草酸溶液中制得多孔氧化铝膜。经5%（质量分数）的磷酸扩孔处理得到具有孔径大小均一,排列有序,并具有一定厚度的阳极氧化铝模板（AAO）。用溶胶-凝胶法在氧化铝模板中制备了直径约为50 nm的有序SmFeO3纳米线阵列。用扫描电镜（SEM）、透射电镜（TEM）和X射线衍射仪（XRD）对SmFeO3纳米线的形貌、结构以及相组成进行了分析。结果发现：纳米线的长度受控于氧化铝模板的厚度,直径与氧化铝模板的孔径相等。同时分析了纳米线的形成机制。     

介孔氧化铝的溶胶-凝胶法制备

以硝酸铝为铝源,十六烷基三甲基溴化铵和尿素为复合模板剂,采用溶胶-凝胶法制备了介孔氧化铝（1）,其结构经TEM, XRD, TG-DTA和N₂-BET表征。结果表明：1比表面积较大（＞400 m²·g^-1）,孔径分布窄(3～5 nm),形成的蠕虫状孔道具有短程有序性。     

溶胶-凝胶法制备Bi-Pb-Sr-Ca-Cu-O微粉

以金属醋酸盐为原料,用溶胶-凝胶技术制备了Bi-Pb-Sr-Ca-Cu-O微粉,并用TG、DTA、IR、XRD和TEM等手段对Bi_1.85Pb_0.35Sr_1.9Ca₂Cu_3.1O_y粉末的热分解和晶化行为以及粉末粒度进行了分析测试,并用此微粉制备出以2223相为主要物相、零电阻为105K的高温陶瓷超导体。     

Synthesis and Electrorheological Characterization of Polyaniline/Barium Titanate Hybrid Suspension

As organic/inorganic composites having attracted much attention due to their heterogeneous physical properties, conducting polyaniline (PANI) and barium titanate (BaTiO₃) which possesses large electronic resistance and excellent dielectric strength, were utilized to synthesize PANI/BaTiO₃ hybrid which is applicable for an electrorheological (ER) material via ‘in-situ’ oxidative polymerization. Physical properties of the obtained PANI/BaTiO₃ composites were characterized via Fourier-transform infrared spectra (FT-IR), thermogravimetry analysis (TGA), and scanning electron microscopy (SEM). The ER behaviors were investigated via a rotational rheometer, and their shear stresses were fitted using our previously proposed rheological equation of state.     

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。     

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。     

Synthesis of Free-Standing Crystalline Barium Titanate Films at Vapor/Liquid or Liquid/Liquid Interface

Synthesis of free-standing crystalline barium titanate (BaTiO₃) films at vapor/liquid or liquid/liquid interface at room temperature has been investigated. High concentration Ba, Ti alkoxides precursor solution (1.2 mol/l) or pre-hydrolyzed precursor solutions by water vapor in a H₂O/Ba molar ratio of 0 to 6 were used as dropping solutions at the interfaces. Transparent gel films were formed when partially hydrolyzed precursors (H₂O/Ba = 2 to 3) were spread out on a N₂/liquid paraffin interface. The films shrank from syneresis and vaporization of the solvent during aging at room temperature. As a result, free-standing transparent films with a thickness of around 1 m and little stoichiometric deviation were obtained by separation from the liquid surface and rinse by hexane. The films consisted of crystalline BaTiO₃ particles of less than a few nanometers. Nanostructured dense BaTiO₃ free-standing films with a grain size less than 100 nm were obtained at 1030°C.     

钛酸钡掺杂磺化聚醚酮质子膜的制备与性能

将纳米钛酸钡(BT)在环己烷中超声分散制得均匀的悬浊液后,与磺化聚醚酮的二甲亚砜溶液均匀混合,然后采用流延法制备了掺杂质子交换膜。 通过环镜扫描电子显微镜表征发现BT在膜中分散均匀,通过吸水率、溶剂吸收率、尺寸变化、电导率、甲醇透过率、力学性能及稳定性等测试发现掺杂膜虽然电导率有所下降,但是其抗溶胀性、稳定性和力学性能显著提高。     

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.     

微波照射制备钛酸钡纳米晶

Cubic barium titanate nanocrystals were prepared by Ti(OC₄H₉)₄ and C₂H₅OH mixture with BaCl₂ aqueous solution under normal atmosphere microwave irradiation. Experiment results showed that when n_Ba / n_Ti=1.1, φ_EtOH=25%,highly dispersed barium titanate with particle size about 30 nm were completely formed by microwave irradiation only for 0.5 h. Microwave irradiation time had almost no effects on particle size and morphology of the product. Particle sizes were decreased with the increased EtOH amount, when φ_EtOH=50%, microwave irradiation 2 h, barium titanate nanocrystals with average size only about 22 nm were obtained.     

水/油型微乳液中球形及棒状钛酸锶钡纳米粒子的控制合成

Barium strontium titanate nanoparticles with spherical and rod-like morphologies were synthesized in water/Triton X-100/n-hexanol/cyclohexane quaternary reverse microemulsion solution. The influences of the molar ratio of water to surfactant (ω₀) and the concentration of reactants on the morphology and size of barium strontium titanate nanoparticles were studied. The structure, compositions and morphology of the prepared products were characterized by XRD, SAED, ICP, EDS and TEM. The results show that the obtained Ba_0.7Sr_0.3TiO₃ spherical nanoparticles with diameters of 20～100 nm and the Ba_0.7Sr_0.3TiO₃ nanorods with diameters of 70～120 nm and lengths up to 600～800 nm are a single crystal, with a cubic phase. The molar ratio for barium, strontium and titanate in products is about 0.7:0.3:1.