来源:塑料托盘 发布时间:2010年7月25日
塑料托盘BaTiO3基陶瓷实现低阻化的途径有多种:通过施主、受主掺杂;改进制备工艺,包括湿法制备超细BaTiO3基粉体;采取与低阻相复合的办法,等等。就高性能PTCR陶瓷低阻化问塑料托盘题,本文从多个方面着手进行了研究。BaTiO3基PTCR陶瓷粉体的湿法制备。采用了柠檬酸盐溶胶-凝胶二步合成法来制备PTCR陶瓷粉体,对溶液的pH值、溶胶反应中溶液的含水量、凝胶化温度、共沉淀反应物的加入顺序等因素进行了分析。大量的研究结果表明:(1)在凝塑料托盘胶化反应中,适合的pH值区间为6.5~7.5,使溶胶凝胶反应充分进行的溶液含水量范围R=[H2O]/[[Ba2+](mol)在70~80,使凝胶化络合反应完全进行的温度在80℃左右。(塑料托盘2)采用柠檬酸盐溶胶-凝胶二步合成法,在600℃即可得到粒径分布在30~70nm之间的施主掺杂BaTiO3粉体,通过二次合成掺杂受主杂质和烧结助剂,不但使粉体的“软团聚”状态得以分散,而且还有利于二次掺杂物均匀地分布在晶界上。(3)柠檬酸盐溶胶-凝胶二次合塑料托盘成法得到的PTC粉体化学组成更为均匀、晶型发育更为完全,更符合理想PTC粉体要求。基于湿法合成BaTiO3基粉体的PTCR陶瓷的制备。采用柠檬酸盐溶胶-凝胶法制备性能优良的BaTiO3基PTC前驱粉体,以Y2O3+Nb2O5双施主掺杂,AST+B塑料托盘N复合烧结,采用二次合成工艺制备了室温电阻率为147Ω·cm、升阻比达5个数量级的PTC陶瓷材料。基于湿法合成的BaTiO3基粉体Ni、Mn掺杂PTCR的制备。采用高纯原料,利用溶胶-凝胶法制备化学组成均匀、颗粒细小的BaTiO3粉体,在此基础上分别加入施主、受塑料托盘主掺杂物质,从而在很大程度上提高和改善了PTC效应。通过复合掺杂金属Ni以降低室温电阻率塑料托盘。系统地考虑了金属Ni的掺入量,烧成气氛,氧化处理温度和氧化处理保温时间对PTC材料性能的影响。将金属具有的良好导电性与BaTiO3瓷特有的电特性相结合,制备出了性能良好的金属/PTCR陶瓷复合材料。基于固相合成法的Ni、Mn掺杂BaTiO3基PTCR的制塑料托盘备。以传统固相法合成BaTiO3基PTC粉体,加入施主物质,以及金属Ni、Mn,在还原气氛烧成及空气气氛处理,制备PTCR陶瓷复合材料,研究和讨论了金属与BaTiO3基PTC材料复合以及后期工艺过程对其室温电阻率、升阻比等性能的影响。通塑料托盘过掺杂金属Mn使其氧化为Mn离子而一方面起到受主作用提高升阻比,一方面在一定程度上对金属Ni起保护作用。研究表明,在还原气氛下烧成(1250℃,保温20min),室温电阻率较低,但只有很弱的PTC效应,再通过适当的后期热处理工艺(空气气氛,780℃,保温60min)PTC效应可塑料托盘得到部分恢复。最终获得了具有低室温电阻率(ρ25℃=10.2Ω·cm)和较高升阻比(ρmax/ρmin=1.42×103)的PTCR复合材料。Ni、Mn掺杂多孔BaTiO3基PTC复合材料的研制。以传统固相法反应法合成双施主掺杂的BaTiO3基PTC粉体,从与低阻相复合降低PTCR材料室温电阻率,多孔可有利于氧吸附,增大表面受态,提高升阻比的角度着手,通过复合Ni、Mn来降低室温电阻率,通过加入淀粉来制造多孔PTCR。复合体在空气和还原气氛下烧结,结果表明还原气氛下烧结的复合体有低的室温电阻率,空气气氛下的室温电阻率达3个数量级。塑料托盘Ni及淀粉加入量对室温电阻率有很大的影响,当淀粉加入量为15wt%,Ni加入量为10wt%时室温电阻率最低,其电阻率是9.9Ω·cm。氧化处理温度及时间对复合材料的性能也有影响,通过对比实验分析可得,850℃50min是最好的氧化处理参数,Ni此时能在淀粉的保护下不被氧化,淀粉燃烧掉形成的孔形成表面受主态,氧被吸附到晶界上而提高了升阻比。根据实验结果结合分析,说明通过柠檬酸盐溶胶-凝胶法可以制备超细BaTiO3基粉体。以传统固相法反应法合成PTC粉体,采取复合Ni、Mn,以及加入淀粉制造多孔,氧化烧成,还原处理等多种工艺措施,可以有效降低BaTiO3基PTCR复合材料的室温电阻率,并获得较高的升阻比。【Abstract】 There are many means in preparing lower resistivity BaTiO3–based PTCR ceramics, such as doping donors and acceptors, improving technics process (include synthesizing BaTiO3-based fine particle powder by wet chemical method), composited with low resistivity materals, etc. On the aim of reducing the resistivity of high performance PTCR, some methods were investigated systemically.Citrate sol-gel twice-through method was used to prepare BaTiO3–based powder. Some factors, such as the value of pH, H2O content, the temperature of gelation, the added sequence of coprecipiting reactor were analysized. The results illuminated that: (1) At the process of citrate sol-gel method, the interval of pH value is 6.57.5, the water-content value (R=[H2O]/[[Ba2+](mol)] is 70~80, and the temperature of gelation is 80℃. (2) The donor-doped BaTiO3 powder which particle size is 3070 nm can be prepared at 600℃by citrate sol-gel method. Through adding acceptor impurities and sintering fluxs with twice-through method, not only the powder have been well distributed, but also the dopants can be good dispersed on the grain boundary. (3) The BaTiO3–based powder, which chemical composition more uniformity and the crystals more completeness, can be prepared by citrate sol-gel twice-through method.Preparation of PTCR ceramics based on BaTiO3-based powder was synthesized with wet chemical method. The PTC powder was prepared by citrate sol-gel method at first. Then by adding Y2O3+Nb2O5 double donor doping and AST+BN sintering fluxs with twice-through method, PTCR ceramics, which under room temperatureρis 147Ω·cm, ratio of lg(Rmax/Rmin) reach to 5, were prepared.Preparation of Ni, Mn dopened PTCR ceramics based on BaTiO3-based powder synthesized with wet chemical method. Using fine purity materials, At first, the PTC powder which has homogeneous chemical composition and fine size particle were prepared by citrate sol-gel method. Then the PTCR ceramics were prepared on the base of adding donor dopants and acceptor dopant to improve PTC effect. The aim of adding Ni is to reduce the resistivity of the PTCR composites. The effect of the content of Ni,sintered atmosphere,heat-treated temperature and heat preservation time were considered. The results shows that when adulterating Ni、Mn into it,more ideal PTCR material can be prepared.Preparation of Ni, Mn dopened PTCR ceramics based on BaTiO3-based powdersynthesized with traditional solid phase method. In order to obtain low resistivity and high PTC effect, Ni/Mn/BaTiO3 PTCR ceramics were prepared by traditional solid phase sintering method. Adding Mn was not only to improve the PTC effect but also to keep Ni from oxygenated. Prepared composite that sintered at deoxidizing atmosphere(1250℃, 20min) had very weak PTC effect, which was renewed effectively by heat-treatment in air(780℃, 60min). The composite showed low room-temperature resistivity(ρ25℃=10.2Ω·cm) and obvious PTC effect(ρmax/ρmin =1.42×103).Preparation of Ni, Mn dopened porous PTCR ceramics based on BaTiO3-based powder synthesized with traditional solid phase method. The double donor-doped BaTiO3-based powder was prepared by the solid phase reaction. In order to get porous Ni/Mn/BaTiO3 PTCR composites, the additions containing Ni, Mn and starch were mixed into the prepared powder. The composites were sintered in air and reducing atmosphere. Research showed that the composites sintered in reducing atmosphere have lower room temperature resistivity. However, the resistivity of samples that sintered in air, achived to 3 orders. By analysising the contents of Ni and starch, it shows that the contents have effect on the room temperature resistivities. The composites that with the contents of Ni 10wt% and starch 15wt% have the lowest room temperature resistivity about 9.9Ω·cm. Reoxidating and holding time affect the composites characteristic. By analysis, 850℃, 50min were considered the best parameters. At such temperature Ni was not oxidated, because of the existing of the starch. The porous ceramics were more favorable to form surface acceptor states compared with ordinary dense ceramics. Oxygen irons can be easily absorbed at the grain boundaries and result in a high PTC jumps.By analyzing the results and data of the experiments, it showed that BaTiO3–based PTCR composite which has lower room temperature resistivity and high PTC jump could be prepared by some ways and means, such as BaTiO3-based powder synthesized by wet chemical method, adding Ni, Mn and starch, sintered in air and reducing treatment, etc

