Synthesis and Characterization of Barium Amidoborane

Barium amidoborane was synthesized for the first time by the reaction of metal barium with ammonia borane. The compound was characterized by the methods of the solid-phase ¹¹B NMR and IR spectroscopy and elemental analysis. It was shown by simultaneous thermal analysis that hydrogen is the only volatile product of barium amidoborane decomposition in the temperature range 50–240°C.     

Nanocrystalline Calcium Carbonate Hydroxyapatites Containing Multiwall Carbon Nanotubes: Synthesis and Physicochemical Characterization

Nanocomposites (NCs) based on carbonated calcium hydroxyapatite (CHA) (bioapatite, an analogue of the inorganic component of mammalian bone tissue), carbonate apatite (Ca₁₀(PO₄)₆CO₃, CA), and multiwall carbon nanotubes (CNTs) are prepared in the system CaCl₂–(NH₄)₂HPO₄–NH₄HCO₃–NH₃–CNT–H₂O (25°C) by coprecipitation of calcium and phosphorus salts with CNTs from aqueous solutions. The physicochemical properties of nanocomposites are studied as dependent on their formation conditions and composition using the solubility (residual concentrations) method and pH measurements. The composition, crystal structure, morphology, spectroscopic and thermal characteristics of the synthesized CHA/CNT and CA/CNT NCs are determined using chemical analysis, X-ray powder diffraction, thermal analysis, and IR spectroscopy. Either CHA/CNT NCs of composition Ca₁₀(PO₄)₆(CO₃)_x(OH)_2–2х · yCNT · zH₂O, where х = 0.2; 0.5; 0.8; y = 1, 2, 3; z = 6.8–10.8, or (when х = 1) CA/CNT NCs of composition Ca₁₀(PO₄)₆CO₃ · yCNT · zH₂O, where y = 1–3; z = 6.9–10.8, are formed as the carbonate and CNT contents of the NC increase. Our results favor the understanding of the effect of carbonization and CNTs on the metabolic formation of native bone tissue apatite and can be used for the design of efficient ceramics for bone implants.     

X型六角晶系钡铁氧体纳米晶的制备和表征

用硬脂酸凝胶法制备了Co₂-X型六角晶系钡铁氧体纳米晶,在750℃热处理得到的纳米晶形貌为球形,粒径范围为15～25nm.随着热处理温度的升高,粒子逐渐长大并呈块状.振荡样品磁强计测试结果表明,Co₂-X型六角晶系钡铁氧体纳米晶具有与常规体材料不同的磁性能,其比饱和磁化强度σ_s低于后者.产物的矫顽力、比饱和磁化强度随粒子的长大呈规律性的变化.     

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.     

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.     

铈酸钡和钇掺杂的铈酸钡复合氧化物的制备及其在钌基氨合成催化剂中的应用

 采用柠檬酸法合成了 BaCeO3 和掺杂 Y3+的 BaCe0.9Y0.1O3-δ 复合氧化物, 以 Ru3(CO)12 为前体, 利用浸渍法制备了 Ru/BaCeO3 和 Ru/BaCe0.9Y0.1O3-δ 催化剂. 通过 X 射线衍射、扫描电镜和透射电镜技术对样品进行了表征, 并在固定床反应器中考察了催化剂的氨合成反应活性. 结果表明, 载体 BaCeO3 的稳定性优于 BaCe0.9Y0.1O3-δ, 但 Ru/BaCe0.9Y0.1O3-δ 催化剂的氨合成活性明显高于 Ru/BaCeO3, 在 3.0 MPa, 15 000 h1, 425 oC 反应时, Ru/BaCe0.9Y0.1O3-δ 催化剂上氨合成反应速率达到 432.5 ml/(g•h), 是 Ru/BaCeO3 催化剂的 1.6 倍. 这种活性和稳定性的显著差异来自载体中 Ce4+ 与 Ru 纳米粒子间的电子作用.     

聚苯胺/钛酸钡纳米复合粒子的制备与表征

采用原位复合法制备出聚苯胺/钛酸钡复合粒子,借助TEM、XRD、FT-IR、 XPS、TG等分析手段研究了复合粒子的形貌、结构及其热性能.结果表明,复合粒子的粒径为1 μm左右,BaTiO3以40 nm左右的晶粒分散于聚苯胺基体之中,聚苯胺与钛酸钡之间存在化学键合作用,同时在一定程度上减少了纳米粒子的团聚.     

水合烟酸钡的合成、±结构表征和热化学性质

选择烟酸和氢氧化钡作为反应物, 利用室温固相合成方法, 借助于球磨技术, 合成了一种新的化合物——水合烟酸钡. 利用化学分析、元素分析、FTIR和X射线粉末衍射等方法确定了它的组成和结构为Ba(Nic)2·3H2O(s). 利用精密自动绝热热量计直接测定了此化合物在78-400 K温区的摩尔热容. 在热容曲线上出现了一个明显的吸热峰, 通过对热容曲线的解析, 得到了相变过程的峰温、相变焓和相变熵分别为(327.097±1.082) K、(16.793±0.084) kJ·mol-1和(51.340±0.164) J·K-1·mol-1. 将该温区的摩尔热容实验值用最小二乘法拟合得到摩尔热容(Cp,m)对温度(T)的多项式方程, 并且在此基础上计算出了它的舒平热容值和各种热力学函数值. 另外, 依据Hess定律, 通过设计合理的热化学循环, 选择体积为100 mL、浓度为0.5 mol·L-1的盐酸作为量热溶剂, 利用等温环境溶解-反应热量计分别测量固相反应的反应物和产物在所选溶剂中的溶解焓, 利用溶解焓确定固相反应的反应焓为⊿rH0m=-(84.12±0.38) kJ·mol-1. 最后, 利用固相反应的反应焓和其它反应物和产物已知的热力学数据计算出水合烟酸钡的标准摩尔生成焓为⊿fH0m[Ba(Nic)2·3H2O(s)]=-(2115.13±1.90) kJ·mol-1.     

水合烟酸钡的合成、结构表征和热化学性质

选择烟酸和氢氧化钡作为反应物,利用室温固相合成方法,借助于球磨技术,合成了一种新的化合物-水合烟酸钡.利用化学分析、元素分析、FTIR和X射线粉末衍射等方法确定了它的组成和结构为Ba(Nic)2·3H2O(s).利用精密自动绝热热量计直接测定了此化合物在78-400 K温区的摩尔热容.在热容曲线上出现了一个明显的吸热峰,通过对热容曲线的解析,得到了相变过程的峰温、相变焓和相变熵分别为(327.097±1.082)K、(16.793±0.084)kJ·mol-1和(51.340±0.164)J·K-1·mol-1将该温区的摩尔热容实验值用最小二乘法拟合得到摩尔热容(Cp,m)对温度(T)的多项式方程,并且在此基础上计算出了它的舒平热容值和各种热力学函数值.另外,依据Hess定律,通过设计合理的热化学循环,选择体积为100mL、浓度为0.5mol·L-1的盐酸作为量热溶剂,利用等温环境溶解-反应热量计分别测量固相反应的反应物和产物在所选溶剂中的溶解焓,利用溶解焓确定固相反应的反应焓为△rH0m=-(84.12±0.38)kJ·mol-1.最后,利用固相反应的反应焓和其它反应物和产物已知的热力学数据计算出水合烟酸钡的标准摩尔生成焓为△rH0m[Ba(Nic)2·3H2O(s)]=-(2115.13±1.90)kJ·mol-1.     

钡铁氧体微管的制备及镧掺杂对其性能的影响

以Ba(NO₃)₂和Fe(NO₃)₃为原料与不同比例的柠檬酸在水溶液中形成溶胶,把溶胶滴于脱脂棉模板上,水分挥发后在脱脂棉表面形成凝胶,于马弗炉中850 ℃煅烧2 h后制得了BaFe₁₂O₁₉微管,并在最佳柠檬酸用量时对BaFe₁₂O₁₉微管进行掺杂制得了BaLa_xFe_12-xO₁₉(x=0～0.3)微管。利用X射线衍射(XRD)﹑扫描电子显微镜(SEM)﹑透射电子显微镜(TEM)对样品的物相﹑形貌和粒径进行表征,并利用振荡样品磁强计(VSM)对样品进行磁性能研究。结果表明：借助脱脂棉模板,采用溶胶凝胶法制备了外径在8～13 μm之间,壁厚在0.5～2 μm之间的BaFe₁₂O₁₉微管,柠檬酸的加入使得微管出现破裂,随着柠檬酸用量的增加,BaFe₁₂O₁₉微管的矫顽力和饱和磁化强度先提高后下降,随着La掺入量的增加BaFe₁₂O₁₉微管的矫顽力、饱和磁化强度以及剩余磁化强度都先增加后减小,但饱和磁化强度和剩余磁化强度的最大值滞后于矫顽力的最大值,当柠檬酸与金属离子的物质的量之比为1∶1,x为0.05时850 ℃煅烧后制得了矫顽力、饱和磁化强度和剩余磁化强度分别为6 153.6 Oe,61.1和36.1 emu·g^-1的BaLa_xFe_12-xO₁₉微管。并就柠檬酸和La掺杂对微管的形成和磁性能的影响原理做了系统的研究。     

Fabrication and Characterization of Sol-Gel Derived Potassium Sodium Strontium Barium Niobate

Potassium sodium strontium barium niobate (K_0.2Na_0.2Sr_0.48Ba_0.32Nb₂O₆, KNSBN) powder and thin films dip coated onto Si(100) substrates have been prepared by sol-gel route. The thermal evolution of these sol-gel derived KNSBN was studied by differential thermal analysis (DTA) and thermogravimetry (TG). Their structural changes at different annealing temperatures were examined by X-ray diffraction (XRD) and Raman spectroscopy. Our results suggest that the KNSBN tetragonal tungsten bronze (TTB) phase is formed via an intermediate orthorhombic phase. Pure TTB phase KNSBN was obtained at annealing temperatures of 1200°C and 600°C for powder and films respectively.     

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.     

氧化铜转化法制备氢氧化钡

以硫化钡为原料,在水溶液中与氧化铜反应,生成氢氧化钡。副产物硫化铜经氧化焙烧生成氧化铜,循环使用于下一次合成中。放出的二氧化硫经石灰乳吸收用来制备亚硫酸氢钙。     

枝晶簇四方相钛酸钡的制备及其电场响应性能的研究

为了提高BaTiO3粒子在含水复合弹性体中的电场响应能力,本文采用简单的水热合成法,在不引入任何表面活性剂的情况下,仅通过对反应温度和溶液pH值的调控获得了新颖形貌的钛酸钡粒子。通过借助X射线衍射(XRD)、拉曼光谱(Raman)、扫描电子显微镜(SEM)及接触角(Contact Angle)测量等手段对粒子的微观结构和表面特性进行表征发现:该粒子为高纯四方相枝晶簇结构,具有良好的亲水性,而且在含水复合弹性体中对电场具有优良的响应能力。     

Preparation of Barium Titanate and Related Materials by the Alkoxide-Hydroxide Route

Formation of perovskites MTiO₃ (M = Ba, Sr) at low temperature (< 100°C) by heterogeneous reactions of M(OH)₂ aqueous solutions with hydrolysis products of Ti(OBu)₄ is discussed. Reaction products are characterized by means of chemical and X-ray analysis, and electron microscopy. Reaction rate is enhanced by hydroxide concentration and reaction temperature, and increases drastically when Sr(OH)₂ is used instead of Ba(OH)₂. Particles shape and size of the perovskites formed is independent of morphology of Ti(OBu)₄ hydrolysis product. The main factor of perovskites morphology regulation lies in the rate of M(OH)₂ absorption. Lowering the absorption rate allows us to prepare uniform perovskite powders which can be readily sintered to ceramic bodies with high dielectric permittivity.     

Takiyama法制备均分散碳酸钡粒子

Ｔａｋｉｙａｍａ法制备均分散碳酸钡粒子王世权，王泽新，伍世英，陈宗淇（青岛化工学院应用化学系，青岛，２６６０４２）关键词均分散料子，碳酸钡，Ｔａｋｉｙａｍａ法均分散体系的制备是近年来胶体化学领域中深受重视的研究课题，由于均分散体系的粒子形状相同、尺寸...     

Bimetallic Alkoxides of Barium and Zirconium: Preparation of BaZrO3 Powder

Complex formation in solutions of barium and zirconium alkoxides in ROH (R=i-Pr, Et) was studied. A number of bimetallic complexes were isolated, and their structure and properties were studied. The sol-gel method yields a single-phase BaZrO₃ powder only wheni-PrOH solutions of the alkoxides are used. In this case, the oxocomplex, BaZrO(OPr-i)₄.(1–2)i-PrOH, is the precursor of the mixed oxide.     

络合法制备纳米硫酸钡及其影响因素的分析

以Na2SO4和BaCl2为原料,EDTA为络合剂,水为反应介质,采用络合法制备纳米BaSO4。并研究了反应物浓度、体系pH、反应温度、滴加速度和干燥方式等因素对产物粒径大小和粒径分布的影响。通过考察和分析,初步得出纳米BaSO4最佳制备条件为:反应温度为35℃,pH为6,3种反应物EDTA、BaCl2、Na2SO4的反应浓度均为0.5 mol/L。