电容器用钽铌粉的研究进展

概括介绍了电容器用钽铌粉的研究进展,介绍了钽粉的3种钠还原制备方法的化学反应机理并进行了比较,同时还介绍了铌粉的制备方法,包括铝热还原法、电解还原法、蒸气还原法、钠还原法和金属热还原法;阐述了钽铌粉中杂质的测定方法以及有关钽铌粉的其它研究进展.     

电容器用铌粉和钽粉制备技术的进展

综述了铌粉和钽粉的现行生产工艺及几种新的还原方法,介绍了金属热还原反应中的电化学反应机理.钽粉的现行生产工艺几乎都用亨特法,铌粉则大部分采用铝热还原法生产.通过对亨特法还原条件、稀释剂组成等各种工艺参数的改进,已经可以制备纯度高、形态可控的金属钽粉.铌粉新还原方法的研究主要包括金属预成形热还原法、镁等蒸气还原预成形氧化物粉末的方法、镁或钠的蒸气还原氯化物蒸气的气相还原法、以液氨为介质在低温液相中均相还原铌或钽的氯化物的方法、反应媒介熔盐在强搅拌条件下的液体镁热还原金属氧化物的方法等.     

还原氧化钽制备钽粉工艺研究进展

评述了几种由氧化钽还原制取钽粉的新工艺。并阐述了不同方法的工艺原理、特点和产品特性。钠还原法反应时间短,还原温度范围广,能过得到高纯度高比表面的钽粉。FFC法具有工艺简单,污染小,成本低的特点,可以用来制备电容器级粉末。SOM法电解速度快,具有很好的发展前景。采用镁蒸汽还原能够得到性能好的钽粉,但是还原时间长,还原装置复杂。     

几家公司的钽工艺开发

1美国扇钢(Fansteel)公司 1922年,Fansteel公司开发了钠热还原工艺生产钽粉,并取得了专利,但直到20世纪50年代后半期才得到商业化应用,当时,竞争压力使该公司必须大大改善金属钽粉技术工艺,尤其是用于电容器的钽粉工艺.     

金属钛粉的制备工艺

钛粉作为钛粉末冶金的主要原料,其品质及生产成本限制了钛及钛合金粉末冶金的发展.综述了机械合金化法、氢化脱氢法(HDH)、雾化法、金属热还原法、熔盐电解法制备钛粉的基本原理和工艺现状.新兴的生产技术有望降低钛粉生产成本,从而推动钛及钛合金粉末冶金的发展,扩大其应用范围.     

钽铌电子材料新进展(Ⅰ)

代表中国钽铌工业整体水平的宁夏东方有色金属集团有限公司,近年来,研究了钽粉的微观结构,开发出降低杂质含量,改善物理性能等新技术以及Ta2O5钠还原制取高比容钽粉、TaCl5低温钠还原制取纳米级钽粉的新工艺方法;研制并生产出性能优良的、适用于钽电容器的高比容钽粉,同时也开发了高比容铌粉、一氧化铌粉的制造新技术,制得高性能的电容器级铌粉和一氧化铌粉,为铌电容器作为一种新型电容器产业参与竞争提供了优质的基础材料.     

钽铌电子材料新进展(Ⅱ)

代表中国钽铌工业整体水平的宁夏东方有色金属集团有限公司,近年来,研究了钽粉的微观结构,开发出降低杂质含量、改善物理性能等新技术以及钠还原Ta2O5制取高比容钽粉、低温钠TaCl5还原制取纳米级钽粉的新工艺方法;研制并生产出性能优良的、适用于钽电容器的高比容钽粉,同时也开发了高比容铌粉、一氧化铌粉的制造新技术,制得高性能的电容器级铌粉和一氧化铌粉,为铌电容器作为一种新型电容器产业参与竞争提供了优质的基础材料.     

纳米银的制备及其应用

综述了制备纳米银粒子的方法,主要包括物理法、液相化学还原法、电化学还原法、光化学还原法等,论述了纳米银在催化反应、抗菌领域及导电等领域的应用,并展望了纳米银粉制备技术的研究发展方向.     

热处理温度对钽粉性能的影响

用钠还原氟钽酸钾得到的原粉分别在1 350,1 400,1 450℃温度下进行热处理,得到的3种钽粉按照相同的条件进行镁还原脱氧处理,测试钽粉的化学成分、物理性能和电性能.表明提高热处理温度:可降低钽粉氧,钾,钠杂质含量,平均粒径和松装密度增大,细粉比例和收缩率降低,颗粒强度和坯块强度提高;在条件I下赋能的钽粉比容、漏电流、损耗降低;在条件Ⅱ下赋能的钽粉漏电流和损耗降低,比容提高.因此,热处理温度低的钽粉适合在较低温度下烧结、低压赋能制作电容器;而热处理温度高的钽粉适合于较高温度烧结和较高电压赋能制作电容器.     

钽粉颗粒强度的研究

研究了采用激光粒度分布仪测试电容器级团化钽粉粒度分布及强度的方法.其中心内容是:先采用3种不同比表面积、松装密度和费氏平均粒径的钠还原原粉,按3种烧结工艺制得团化钽粉.然后把烧结得到的6种试样加入纯水中,以200～300 r/min进行高速搅拌并以40 W,42 kHz超声波振动.将激光衍射分析仪的激光束穿过经不同搅拌时间的悬浊钽粉,测得不同时间的钽粉粒径分布曲线.分析分布曲线可以获得团化钽粉的一系列信息,包括:①几种团化钽粉颗粒的相对强度;②影响团化钽粉颗粒强度的因素;③钽粉强度和其他性能如介电损耗、流动性,平均粒径及密度的关系等.     

电容器级钽粉关键技术与开发研究

引述了Ta电容器与Al电容器、多层陶瓷电容器相比突出的性能与应用特征，分析了Ta电容器片式化、小型化促进电容器级Ta粉高比容化发展的新趋势，叙述了航空、航天和军工领域对高压电容器高可靠性能的需求，以及对中高压Ta粉向更高电压、更低SER方向发展的引领，回顾了电容器用高比容Ta粉、中高压Ta粉发展应用进程，介绍了经典氟钽酸钾（K2TaF7）金属Na还原法、电子束熔炼法、球磨片式化法生产的高比容Ta粉、高压Ta粉、中压（片状）Ta粉的性能、产品品级及关键技术，分析了30～80kμFV／gTa粉耐压性能影响因素，介绍了Ta粉高比容化、高压化新技术、装置、产品形貌、性能及优缺点，在此基础上提出了电容器级Ta粉高比容化、高压化创新进步的思路。     

世界钽粉生产工艺的发展

论述了国内外电容器级高压钽粉、中压钽粉、高比容钽粉的生产工艺发展过程。在钽粉生产工艺发展过程中,各种先进的装备被应用,各钽粉生产厂家围绕着钽粉比容的提高,杂质含量的降低,物理性能的优化等综合性能的改善,不断开发出新工艺、新技术,使钽粉适应并推动着钽电容器的发展。     

X-ray diffraction study of sodium metal reduction tantalum powders

This paper examines the effect of sodiothermic reduction conditions on the crystal structure of tantalum and the structural changes induced by subsequent modification of the tantalum powder.     

基于高比容钽粉的聚合物片式电容器制备工艺研究

针对比容为50000～70000μF.V/g的较高比容钽粉,研究了导电聚合物聚3,4-乙烯基二氧噻吩(PE-DOT)作为阴极材料的有机片式固体钽电解电容器的制备工艺,通过调整阳极体制备及阴极被覆工艺等参数实现了PEDOT在高比容钽块表面的有效被覆,获得了各项性能参数良好的聚合物片式钽电解电容器。重点研究了压制密度、形成电流密度等参数及分段被膜工艺对聚合物片式固体钽电容器容量引出、等效串联电阻、漏电流等性能的影响,并讨论了相应的电容器工作机理。     

溅射钽靶材用高纯钽粉工艺研究

分析了高纯钽粉生产的技术特点,介绍了一种改进的钽靶材用高纯钽粉的生产方法。采用高温脱氢(900~950℃)和低温脱氧(700~800℃)分步进行的工艺,有利于钽粉氧、氢、镁含量及粒度的控制,所得样品兼具低氧和小粒度的特点。采用真空热处理(700~800℃)工艺可以有效除去脱氧后残余的金属镁、酸洗带入的H、F等杂质,确保颗粒不长大,同时使杂质含量得到了很好的控制。     

Controlling the synthesis of TaC nanopowders by injecting liquid precursor into RF induction plasma

Thermal plasma processing has been used to synthesize nano-size powders through the condensation of reactant species from a vapor phase. Further development of this synthesis method will require the careful selection of an appropriate precursor and precise control of products species and their particle sizes. Direct introduction of liquid mist into thermal plasma gives us a wider choice of precursors than does vapor-phase precursor injection and lets us inject the precursors in larger amounts. In the present work, nano-size tantalum carbide powder was prepared from a liquid precursor, tantalum ethoxide Ta(OC₂H₅)₅, by using r.f. thermal plasma. The liquid precursor was atomized to generate micron-sized mist droplets, and the mist was introduced into plasma. This atomized precursor evaporated quickly in the high-temperature plasma flame, and nanoparticles were formed as temperature decreased. The process was controlled by changing the hydrogen addition, process pressure, carrier gas flow rate for mist injection, and quenching condition. Adding hydrogen improved the powder quality by removing solid carbon, but excess hydrogen suppressed the formation of tantalum carbide. The quenching conditions gave significant effects on the reduction of particles size by two thirds and yielded average particle sizes as small as 8 nm.     

Synthesis of boride and nitride ceramics in molten aluminium by reactive infiltration

The infiltration of solid powder mixtures with molten aluminium has been investigated as a potential route for the synthesis of ceramic/metal composites. Either titanium or tantalum powder was mixed with boron nitride flakes for the reaction powder mixture. The infiltration occurred spontaneously at 1473K for both [Ti+BN] and [Ta+BN] powder mixtures. Owing to reactions between the starting materials, both boride and nitride ceramics were produced in molten aluminium. TiB2 and AlN were produced from the [Ti+BN] powder mixture, and TaB2 and AlN were produced from the [Ta+BN] powder mixture. When the [Ti+BN] powder mixture was used, a reaction producing Al3Ti took place immediately after the infiltration of the molten aluminium, and a subsequent reaction producing TiB2 and AlN proceeded gradually. The time required to convert BN flakes to TiB2 and AlN particles at 1473K was in the range of 1800–3600 s. On the other hand, when the [Ta+BN] powder mixture was used, there was an initial incubation period to allow the tantalum and molten aluminium to react with each other. The reaction between tantalum, BN and aluminium took place after this incubation period. This revised version was published online in November 2006 with corrections to the Cover Date.     

Electro-deoxidation of Ta2O5 in calcium chloride–calcium oxide melts

Tantalum oxide has been electro-deoxidised in a bath of CaCl₂-1wt%CaO to form tantalum. It was found that the reaction between the calcium oxide in the melt and the tantalum oxide takes precedence over any reduction process so that until the calcium tantalum oxide Ca₃(CaTa₂O₉) (equivalent to 4CaO·Ta₂O₅ or Ca₄Ta₂O₁₀) is formed, calcium ions are reduced to either form calcium metal or reduced calcium species. This eventually results in high electronic conductivity in the melt which means that, compared to the electro-deoxidation of oxides of similar stability to Ta₂O₅, the energy and current efficiencies are low. In addition, the vast changes in microstructure result in a structure that is extremely fragile so that the resulting tantalum can only be harvested as a fine powder.