固相剪切碾磨方法制备聚丙烯/钛酸钡高介电常数复合材料

采用固相剪切碾磨方法(S3M)制备高介电常数聚丙烯/钛酸钡复合材料。当钛酸钡体积分数φBaTiO3=0.50时,体系的介电常数由纯聚丙烯的2.3增加到108.7(1 kHz)。复合材料断面的SEM照片显示,粒径约100 nm的钛酸钡粒子均匀分散在聚丙烯基体中。复合粉体的SEM、TGA和FT-IR分析表明固相剪切碾磨产生的强大剪切、挤压、摩擦等作用在聚合物相引起多种复杂的物理及化学变化,聚合物粒径变小,粒子比表面积增大,表面能大幅增加,与具有较高表面活性的钛酸钡粒子形成较强的界面相互作用。     

聚丙烯/硫酸钡复合体系的界面相互作用与流变性质和结晶行为的关系

制备了一系列具有不同界面状态的聚丙烯 (PP) 硫酸钡 (BaSO4)复合体 .PP BaSO4的界面分别用硅烷、硬脂酸、马来酸酐接枝聚丙烯 (PP g MAH)改性 .研究表明 ,填充体系的熔体粘度和熔体弹性均高于基体 .以硅烷和PP g MAH进行界面改性后 ,PP BaSO4的界面相互作用加强 ,导致复合体系中的熔体粘度和熔体弹性进一步提高 ,同时BaSO4对PP的成核活性提高 .填料用硬脂酸处理后 ,硬脂酸能够在填料粒子表面上形成一个包覆层 ,使粒子与PP的亲和性改善 .同时该包覆层具有润滑作用 ,使得复合体系的熔体粘度和熔体弹性下降 ,并使得该体系中BaSO4的成核活性低于硅烷和处理的体系 .本文探讨了由复合体系的熔体粘度定量比较填充复合体系中聚合物 填料界面相互作用的方法 ,讨论了界面改性对复合体系流变性质和结晶行为影响的机理     

超细钛酸钡的表面改性

利用Sol-gel法成功地在超细钛酸钡粉体表面包覆了厚度约5nm的均匀SiO2膜。采用HRTEM,XPS和XRD等多种分析方法,证实了SiO2薄膜的存在。并首次提出钛酸钡水解后水玻璃在TiO2-x表面溶胶-凝胶化的包覆机理。改性后的钛酸钡与纯钛酸钡相比,SiO2包覆可促进烧结,包覆SiO2坯体在1190℃达到最大收缩速率,而纯钛酸钡坯体达到最大收缩速率的温度为1260℃。坯体的收缩率由未包覆前的-15%变化到-19.3%。包霖工艺改善了介电性能,使介温曲线平坦,对制造钛酸钡薄层电容器有重要的价值。     

核壳型聚苯胺/钛酸钡的结构及其电流变性能

用改进的溶胶-凝胶法制备了核壳型聚苯胺/钛酸钡复合微粉,通过TEM及FT-IR分析表征了其形貌及微观结构,用复合微粉与氯化石蜡油配制成无水电流变(ER)液,研究其不同膜厚核壳粒子的电流变性能.研究结果表明,聚苯胺/钛酸钡复合粒子配置成的电流变液的电流变性能较纯聚苯胺的为强;钛酸钡的涂层厚度对复合粒子电流变性能有重要影响;并在d=20 nm时获得最佳电流变性能.     

具有双交联网络结构的纳米复合材料的制备及介电性能

利用官能团反应活化能的差异, 通过控制反应温度和时间制备了一种具有双交联网络结构的钛酸钡/聚芳醚酮纳米复合膜(BT-BCB/c-DPAEK). 对比研究纯聚合物薄膜及未经交联处理和仅进行单交联处理的复合薄膜发现, BT-BCB/c-DPAEK具有更加优异的力学性能和热性能, 并且其介电性能表现出良好的频率稳定性和温度稳定性. 由于双交联网络对于复合材料两相间界面的改善及高温下对聚合物分子链运动的限制, BT-BCB/c-DPAEK表现出十分优异的储能性能, 特别是在150 ℃, 300 MV/m场强下依然保持1.75 J/cm³的储能密度和80%的放电效率.     

界面改性对玻纤增强聚丙烯弯曲强度的影响

为了提高玻纤增强聚丙烯（ＰＰ）的界面粘结，分别用Ｂ３０１或硅烷偶联剂对玻纤表面进行了处理，用过氧化物和顺丁烯二酸酐对ＰＰ进行了改性。经处理和改性后，ＰＰ／ＧＦ复合材料的弯曲强度有明显提高，对玻纤增强聚丙烯的界面结构也作了探讨。     

水润滑下稀土处理碳纤维填充聚四氟乙烯复合材料摩擦学性能

分别用氧化法、稀土处理法、氧化后稀土处理法对碳纤维进行表面处理，然后开展拉伸试验来对不同方法处理的碳纤维填充聚四氟乙烯复合材料进行界面粘着研究，并在UMT-2MT型摩擦磨损试验机上对水润滑条件下聚四氟乙烯复合材料摩擦学性能进行研究，使用扫描电镜对磨损表面进行观察，研究结果表明稀土处理方法在提高复合材料摩擦学性能上优于氧化方法，稀土处理碳纤维填充的聚四氟乙烯复合材料优良的摩擦学性能来自于碳纤雏增强体与聚四氟乙烯基体间强的界面粘着力。     

纳米SiO_2粒子表面官能团对尼龙6原位聚合的影响

研究了无机纳米粒子表面反应性官能团对尼龙 6 纳米SiO2 原位聚合的影响 .红外光谱和热重分析结果证实了无论对SiO2 进行表面处理与否 ,在原位聚合过程中其表面均能形成一定量的接枝聚合物 .随表面反应性官能团数目的增加 ,SiO2 的表面接枝率呈上升趋势 .与纯的尼龙 6相比 ,带有不同反应性官能团的纳米SiO2 的加入使复合产物的分子量呈下降的趋势 .对应于复合体系中可能发生的反应 ,提出了几种可能的表面接枝的键接方式 .力学性能测试结果显示经表面处理的SiO2 的加入能同时提高复合物的强度和韧性 ,而加入未处理的SiO2 时 ,材料强度可得到提高 ,但韧性明显降低 ,表明由偶联剂处理引入的柔性界面层的存在对于复合材料的力学性能有重要的影响     

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.     

纳米银修饰的超疏水界面用于农药的超灵敏检测

采用化学还原法,在具有不同微观结构的规整的不锈钢网和聚纤维素酯薄膜表面合成了银纳米颗粒.利用氟化试剂对复合界面进行处理,形成超疏水性能的界面,能有效地浓缩目标分子.以罗丹明6G(R 6G)为分析物,纳米银修饰聚纤维素酯薄膜为基底,采用表面增强拉曼散射(SERS)分析了氟化处理前后基底对目标分子的检测能力.实验结果表明,具有超疏水性能的复合基底对R 6G分子的检出限为1 ×10-16 mol/L.以纳米银修饰的不锈钢网和聚纤维素酯两种复合材料为基底,对常用杀虫剂敌百虫的检出限分别为1×10-15 mol/L和1×10-16 mol/L.     

Hydrothermally assisted complex polymerization method for barium strontium titanate powder synthesis

Barium strontium titanate was obtained by hydrothermal treatment of barium strontium titanate citric precursor solution, previously prepared by complex polymerization method. The thermally induced phase evolution was followed at various temperatures up to 800 °C using thermogravimetric and differential thermal analysis, X-ray diffraction analysis, and Raman spectroscopy. Microstructural characterization of barium strontium titanate powders was performed by scanning and transmission electron microscopy. The proposed synthesis route has been proven as a better and faster method for barium strontium titanate powder preparation as compared to the conventional complex polymerization route. The method was found efficient for production of low agglomerated, fine, nanosized barium strontium titanate powder with well defined stoichiometry, and sub-micron particle size. The results of structural and microstructural characterization showed the complete crystallization of carbonate-free barium strontium titanate powder at 700 °C with an average size of crystallites below 50 nm.     

Enhanced electro-optical properties of a nematic liquid crystals in presence of BaTiO3 nanoparticles

Composites of nematic liquid crystals (NLCs) and ferroelectric barium titanate (BaTiO₃) nanoparticles (NPs) have been prepared. The alignments of NPs in the host medium have been demonstrated. Effect of NPs doping on various display parameters of NLCs, namely, threshold voltage, dielectric anisotropy and splay elastic constant has been studied using electro-optical and dielectric studies. The nematic ordering of host supports alignment of NPs parallel to the director which consequently improves electro-optical parameters in the composite system. The dielectric and electro-optic properties of LC–NPs composites have been discussed in frame of conventional theories of NLCs.     

Pyroelectricity and dielectric anisotropy in polarized and niobium modified barium titanate ceramics

The effect of time of soaking on bulk density and dielectric constant has been measured on pure and niobium-doped barium titanate pyroelectric specimens. The temperature dependence of the dielectric constant for both pure and niobium-doped barium titanate samples has been investigated before and after poling. The percentage dielectric anisotropy and ferroelectricity was also calculated for various pure and modified barium titanate pyroelectric materials. Our results can be explained in terms of the redistribution of the barium titanate lattice in a different crystallographic orientation, polarization, as well as the existence of lattice imperfection accompanying temperature, poling and niobium doping. The obtained results were in good conformity, and correlated with the increased proportion of the remnant 90° domains (induced electrically charged vacancies as a result of Nb³⁺ substitution of Ti⁴⁺ in octahedral lattice sites). It was concluded that poling of Nb-doped barium titanate samples produces the best quality ceramic pyroelectrics.     

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.     

The electrical properties of chemically obtained barium titanate improved by attrition milling

Barium titanate ceramics were prepared using the nanopowder resulting from a polymeric precursor method, a type of modified Pechini process. The obtained nanopowder was observed to agglomerate and in order to de-agglomerate the powder and enhance the properties of the barium titanate the material was attrition milled. The impact of this attrition milling on the electrical properties of the barium titanate was analysed. The temperature dependence of the relative dielectric permittivity showed three structural phase transitions that are characteristic for ferroelectric barium titanate ceramics. The relative dielectric permittivity at the Curie temperature was higher for the attrition-treated sample than for the non-treated barium titanate. The dielectric losses were below 0.04 in both barium titanate ceramics. The grain and grain-boundary contributions to the total resistivity were observed using impedance analyses for both ceramics. A well-defined ferroelectric hysteresis loop and piezoelectric coefficient d₃₃ = 150 pC/N were obtained for the ceramics prepared from the de-agglomerated powder. In this way we were able to demonstrate that by attrition milling of chemically obtained powders the ferroelectric and piezoelectric properties of the ceramics could be enhanced.     

Effect of nano-barium titanate on thermal stability of ferrite filled poly-ether-ether-ketone (PEEK) composites

The reinforcement of nano-barium titanate in ferrite filled poly-ether-ether-ketone (PEEK) composites caused a shift in the decomposition temperature, at which maximum mass loss occurred, to higher side and enhancement in char yield in thermogravimetric analysis. Loss tangent and glass transition temperature of ferrite filled PEEK composites were also found to be increased with the reinforcement of nano barium titanate. The effect of nano barium titanate on the melting behaviour of ferrite filled PEEK composites was negligible. This revised version was published online in August 2006 with corrections to the Cover Date.     

Liquid-phase synthesis of barium acetatotitanyl and barium oxalatotitanyl as intermediates for preparing nanosized barium titanate

Liquid-phase methods (an oxalate process in aqueous solution and a semialkoxide sol-gel process in anhydrous acetic acid) were used to prepare barium acetatotitanyl (BAT) and barium oxalatotitanyl (BOT), which are potential fillers for electrorheological liquids, and to prepare barium titanate during heat treatment of the aforementioned intermediates at 1200°C. The materials were characterized using electron microscopy, FTIR spectroscopy, and thermal analysis. The particle size was 80 to 100 nm for BAT powders and 20 to 50 nm for BOT powders. X-ray spectra of the powders dried at 120°C contain reflections from a barium titanate phase. The dielectric spectra of the materials synthesized were studied for suspensions in PMS-20 silicone oil over the frequency range from 25 to 10⁶ Hz up to 4 kV/mm. The dielectric parameters of BOT suspensions decrease hyperbolically with rising alternate current frequency, whereas BAT suspensions give rise to a relaxation dielectric spectrum with relaxation times on the order of 10⁻³ s.     

Preparation and Properties of Nb-Coated Barium Titanate Composite Particles by Surface Modification with Nb Alkoxide in Hydrophobic Solvent

Chemical processing for the preparation of Nb-coated barium titanate composite particles was investigated using surface modification technology, hydrolyzing Nb ethoxide on the surface of barium titanate particles dispersed in hydrophobic solvent.It was confirmed from the measurements of specific surface area and zeta potential as well as SEM, TEM and EDX observations of the resulting composite particles that the original barium titanate particles were coated uniformly with hydrolysis product of Nb ethoxide.Barium titanates coated with 1 wt% of Nb as oxide were well sintered at 1200–1300°C. The dielectric constants of the sintered barium titanates showed flattened temperature dependence, but it depended upon the average particle size of original barium titanate. The sintered bodies of Nb-coated barium titanate powders with average particle size of 0.2 m gave dielectric constants of 2000–3000 and those of barium titanate with average particle size of 0.5 m showed dielectric constants of 3000–4000 at room temperature.The microstructure of the sintered barium titanate coated with Nb oxide consisted of grains of about 1 m, smaller than those of sintered original barium titanate.     

Barium Titanate-reinforced Acrylonitrile-Butadiene Rubber: Synergy Effect of Carbon-based Secondary Filler

Acrylonitrile rubber(NBR) composites filled with barium titanate(BT) were prepared using an internal mixer and a two-roll mill. Also, a secondary filler, namely carbon nanotubes(CNT), was added in order to find a potential synergistic blend ratio of BT and CNT. The cure characteristics, tensile and dielectric properties(dielectric constant and dielectric loss) of the composites were determined. It was found that NBR/BT composites with CNT secondary filler, at a proper BT:CNT ratio, exhibited shorter scorch time(t_(s1)) and cure time(t_(c90)) together with superior tensile properties and reinforcement efficiency, relative to the one with only the primary filler. In addition, the NBR/BT-CNT composite with 80 phr BT and 1-2 phr CNT had dielectric constant of 100-500, dielectric loss of 12-100 and electrical conductivity below 10~(-4) S/m together with high thermal stability. Thus, with a proper BT:CNT mix and filler loading, we can produce mechanically superior rubber composites that are easy to process and low-cost, for flexible dielectric materials application.