CN113149640B - 一种高温高能高效车用逆变电容器核心材料的制备方法 - Google Patents
一种高温高能高效车用逆变电容器核心材料的制备方法 Download PDFInfo
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000007599 discharging Methods 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
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- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 claims description 12
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 5
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- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 6
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Abstract
本发明涉及一种高温高能高效车用逆变电容器核心材料的制备方法依次包括以下步骤：1)制备二维BN：2)制备车用逆变电容器的核心材料：在原料中加入氧化锆球和无水乙醇进行第一次球磨，球磨后干燥后得到干燥的瓷料粉体，将干燥的瓷料粉体压实进行第一次预烧结；第一次预烧结后的粉体进行第二次球磨，待球磨后烘干后进行第二次烧结；随后将二维BN纳米材料无机填料放入第二次烧结后的粉体中进行第三次球磨，待球磨烘干得到坯体；将坯体放入研钵进行研碎后，向粉碎后的粉体中加入粘结剂进行造粒，造粒后的粉体陈腐后压制成样品；将样品进行排胶；将排胶后的生胚进行第三次烧结。降低烧结温度，在室温～200℃下兼具高储能密度和效率。
Description
技术领域
本发明属于电子元器件制备技术领域，具体涉及一种高温高能高效车用逆变电容器核心材料的制备方法。
背景技术
新能源汽车的电力系统由电池和逆变器构成，其中电池组输出的低压直流电经逆变器中的绝缘栅双极晶体管开关阵列转换成大功率高压交流电，为电动机提供电能。然而电池组不能直接与逆变器中的绝缘栅双极晶体管相连，否则由电动机的电感耦合和晶体管的开关跳变所引起的大功率反馈将直接冲击电池(冲击电压和电流超过1000V和250A)，导致电池组烧毁甚至引起爆炸。目前解决这一问题的有效途径是在逆变器的输入总线上并联大功率储能电容器，将冲击能量快速存储到电容器中，实现对电池组的保护。
目前，车用逆变储能电容器介质材料主要有：聚合物有机材料、陶瓷材料以及陶瓷与聚合物复合材料。聚合物材料具有抗击穿场强极高的优势，但聚合物介电常数小、高温下介电损耗大的缺点严重制约了聚合物的应用。复合电介质材料可一定程度上综合有机与无机材料的优势，但其使用温区依然受到严重限制，且批量生产技术不成熟。不同于聚合物及其复合材料，陶瓷材料及其电容器耐高温能力强、生产技术成熟。与铁电陶瓷相比，弛豫性铁电陶瓷更具独特的优势具有高的饱和极化及低的剩余极化，导致其储能密度和效率更高。
现阶段，国内外高储能密度弛豫性铁电材料的主要研究对象为钛酸铋钠(BNT)材料。BNT具有高的极化强度、剩余极化低，通常被研究人员制成块体陶瓷进行研究，相关报道主要集中在工艺技术改进、组分配比调整及掺杂改性方面，并未涉及畴壁导电及晶界电缺陷聚集效应等。受限于该体系材料相变电场较小的缺点，制得的材料储能密度一般在2J/cm3以下。此外，混合动力汽车电控系统使用冷却系统将环境温度从120-140℃降至70-80℃。然而，冷却系统的存在无疑会增加动力系统的质量和体积，降低燃料使用效率。
因此，能够在高温(≥150℃)环境中稳定工作并兼具高的储能密度的车用逆变电容器核心材料，是高新技术领域急需解决的问题。
发明内容
本发明所要解决的技术问题是针对上述现有技术的现状，提供一种在高温条件下稳定工作且储能密度和效率均高的高温高能高效的车用逆变电容器核心材料的制备方法。
本发明解决上述技术问题所采用的技术方案为：一种高温高能高效车用逆变电容器核心材料的制备方法，其特征在于，依次包括以下步骤：
1)制备二维BN：
将BN粉体在250～350mA的振幅下搅拌20～25h；随后，放置于离心管内，并在转速n1为2000～4000rpm下离心20～40min，收集上清液以分离未剥离的粉末；然后，将上清液以转速n2为9000～11000rpm下离心20～40min，并收集离心管壁上的沉积物，该沉积物为二维BN纳米材料无机填料；
2)制备车用逆变电容器的核心材料：
S1：先将核心材料钛酸铋钠基、钛酸钡基、铌酸钾钠基、铌酸钠基、铌酸银基和钛酸铋基中的一种核心材料的原料进行干燥，随后将所需要的原料量置于球磨罐中进行研磨，按照质量百分比为原料量：锆球：无水乙醇＝1:5:2，在原料中加入氧化锆球和无水乙醇进行第一次球磨，球磨后将得到的浆料进行干燥，从而得到干燥的瓷料粉体，随后将干燥的瓷料粉体放入坩埚中压实并进行第一次预烧结；
S2：随后将第一次预烧结后的粉体进行第二次球磨，待球磨后进行烘干，在烘干后进行第二次烧结；随后将二维BN纳米材料无机填料放入第二次烧结后的粉体中进行第三次球磨，待球磨后进行烘干得到坯体；
S3：将坯体放入研钵进行研碎后，向粉碎后的粉体中加入粘结剂聚乙烯醇溶液进行造粒，造粒后的粉体在空气中陈腐后压制成样品；
S4：将样品进行排胶处理；
S5：将排胶后的生胚在800～1200℃温度下进行第三次烧结，从而制备出所需的核心材料。
上述烧结过程中引入烧结助剂二维BN纳米片，使材料的烧结成型的温度低、晶粒尺寸小，有利于车用逆变电容器的核心材料储能密度、效率及温度稳定性的提高。
优选地，所述二维BN纳米片的厚度为2～300nm，直径为0.1～10um。厚度越薄越有利于分散在整个样品，有利于储能密度、效率的提高。
其中，所述钛酸铋钠基材料的原料为碳酸钠、二氧化钛和三氧化二铋，且在配料中加入多加入3mol％的三氧化二铋。
上述钛酸铋钠基、钛酸钡基、铌酸钾钠基、铌酸钠基、铌酸银基和钛酸铋基的原料均采用现有技术中的原料制备而成。
优选地，第一次球磨的时间为12h，第二次球磨的时间为24h，第三次球磨的时间为12h。为了更好的把原料混合均匀，有利于成相。
在步骤S1中，首次干燥的温度为90～110℃，保温时间为11～13h。具体地，在步骤S1中，首次干燥的温度为100℃，保温时间为12h。
优选地，在步骤S3中，在压力为190～210MPa下，得到厚度为2mm、直径为10mm的圆片样品。具体地，在步骤S3中，压力为200MPa。
优选地，所述排胶处理为在温度为540～560℃下，保温时间为11～13h，升温速度为0.9～1.1℃/min下进行排出粘结剂。具体地，排胶处理的温度为550℃，保温时间为12h，升温速度为1℃/min。
优选地，在步骤S5中，第三次烧结时的升温速度为3℃/min，保温时间为2h。如此，更好的烧结成型。
与现有技术相比，本发明的优点在于：通过二维BN的引入，以液相润湿作用而降低了陶瓷的烧结温度以及致密性，而烧结温度越低，越有利于陶瓷晶粒的长大，有利于击穿场强的提升，从而导致储能密度和效率的提高。因此，采用上述引入二维BN的制备方法，大幅度地降低了烧结温度，使该材料的储能密度、效率以及在室温～200℃下均可以稳定工作。此外，上述的制备方法成本低，性能优异，可达到量产，从而满足需求。
附图说明
图1为实施例1～8的烧结样品对应的储能密度示意图；
图2为实施例1～8的烧结样品的效率示意图；
图3为实施例3的核心材料样品在不同温度下的储能密度的示意图；
图4为实施例3的核心材料样品在不同温度下的效率的示意图。
具体实施方式
以下结合附图实施例对本发明作进一步详细描述。
实施例1：
上述逆变电容器核心材料的制备方法包括以下步骤：
1)制备二维BN：
将二维BN纳米片在250mA的振幅下搅拌20h；随后，放置于离心管内，并在转速n1为2000rpm下离心20min，收集上清液以分离未剥离的粉末；然后，将上清液以转速n2为9000rpm下离心20min，并收集离心管壁上的沉积物，该沉积物为二维BN纳米材料无机填料；
2)制备车用逆变电容器的钛酸铋钠基材料：
首先将钛酸铋钠基的原料如碳酸钠、二氧化钛和三氧化二铋置于鼓风干燥箱内，并在100℃下保温12h以去除原料中的水分。随后根据实际所需原料的质量，并在配料时过量加入3mol％的Bi2O3，防止其在烧结时发生挥发，从而产生质量损失。将所需的原料放置于尼龙球磨罐中，按照质量百分比为原料：锆球：无水乙醇＝1:5:2，在原料中加入氧化锆球和无水乙醇，进行第一次球磨，第一次球磨时间为12h，随后将球磨后得到的浆料放置于烧杯中，然后放入恒温鼓风干燥箱中干燥24h，而得到干燥的瓷料粉体，随后将干燥的瓷料粉体放入坩埚中压实进行第一次预烧结。
将第一次预烧结后的粉体进行第二次球磨，第二次球磨时间为24h，待烘干再进行第二次烧结；随后将二维BN纳米材料无机填料放入第二次烧结的样品中进行第三次球磨，第三次球磨时间为12h，并进行烘干而得到坯体。
将烘干的坯体放入研钵中进行研碎后，接着向烘干后的粉体中加入5wt.％的PVA溶液作为粘结剂进行造粒；造粒后的粉体需要在空气中陈腐24h，然后在200MPa的压力下成型得到厚度为2mm、直径为10mm直径的圆片样品。将成型得到的圆片样品作排胶处理，即在温度为550℃下保温时间为12h，升温速度为1℃/min，从而缓慢排出样品中的粘结剂。将排胶后的生胚放入硅钼炉内进行第三次烧结，烧结温度为850℃，升温速度设置为3℃/min，保温时间为2h，从而得到最后样品。
上述第一次烧结、第二次烧结的温度和时间为与第三次烧结的温度和时间相同。
实施例2：
本实施例与上述实施例1的区别仅在于：第三次烧结温度为900℃。
实施例3：
本实施例与上述实施例1的区别仅在于：第三次烧结温度为950℃。
实施例4：
本实施例与上述实施例1的区别仅在于：第三次烧结温度为1000℃。
实施例5：
本实施例与上述实施例1的区别仅在于：第三次烧结温度为1050℃。
实施例6：
本实施例与上述实施例1的区别仅在于：第三次烧结温度为1100℃。
实施例7：
本实施例与上述实施例1的区别仅在于：第三次烧结温度为1150℃。
实施例8：
本实施例与上述实施例1的区别仅在于：第三次烧结温度为1200℃。
上述实施例1～8在烧结样品的储能密度参见图1所示，由图1可知，在烧结温度为950℃下的储能密度为4.5J/cm3，效率为89％；在烧结温度为1000℃下的储能密度为4J/cm3，效率为90％；在1050℃下的储能密度约为3.6J/cm3，效率为92％。且由图1和图2可知，核心材料在烧结温度为850～950℃下即可烧结而成，与现有烧结温度通常在1050～1150℃下相比，烧结温度明显降低。
性能最好的样品为实施例3，实施例3所制备出的核心材料在室温～200℃下的储能密度和效率均较为稳定，储能密度在2.9～3.2J/cm3，效率为80～90％，如此，采用本实施例的制备方法所制备出的核心材料在室温～200℃下均可稳定工作。
实施例9：
1)制备二维BN：
将二维BN纳米片在350mA的振幅下搅拌25h；随后，放置于离心管内，并在转速n1为4000rpm下离心40min，收集上清液以分离未剥离的粉末；然后，将上清液以转速n2为1000rpm下离心40min，并收集离心管壁上的沉积物，该沉积物为二维纳米材料无机填料；
2)制备车用逆变电容器的钛酸铋钠基材料：
首先将钛酸铋钠基的原料如碳酸钠、二氧化钛和三氧化二铋置于鼓风干燥箱内，并在90℃下保温13h以去除原料中的水分。随后根据实际所需原料的质量，并在配料时过量加入3mol％的Bi2O3，防止其在烧结时发生挥发，从而产生质量损失。将所需的原料放置于尼龙球磨罐中，按照质量百分比为原料：锆球：无水乙醇＝1:5:2，在原料中加入氧化锆球和无水乙醇，进行第一次球磨，第一次球磨时间为12h，随后将球磨后得到的浆料放置于烧杯中，然后放入恒温鼓风干燥箱中干燥24h，而得到干燥的瓷料粉体，随后将干燥的瓷料粉体放入坩埚中压实进行第一次预烧结。
将第一次预烧结后的粉体进行第二次球磨，第二次球磨时间为24h，待烘干再进行第二次烧结；随后将二维BN纳米材料无机填料放入第二次烧结的样品中进行第三次球磨，第三次球磨时间为12h，并进行烘干而得到坯体。
将烘干的坯体放入研钵中进行研碎后，接着向烘干后的粉体中加入5wt.％的PVA溶液作为粘结剂进行造粒；造粒后的粉体需要在空气中陈腐24h，然后在190MPa的压力下成型得到厚度为2mm、直径为10mm直径的圆片样品。将成型得到的圆片样品作排胶处理，即在温度为540℃下保温时间为13h，升温速度为1.1℃/min，从而缓慢排出样品中的粘结剂。将排胶后的生胚放入硅钼炉内进行第三次烧结，烧结温度为900℃，升温速度设置为3℃/min，保温时间为2h，从而得到最后样品。
实施例10：
1)制备二维BN：
将二维BN纳米片在300mA的振幅下搅拌22h；随后，放置于离心管内，并在转速n1为3000rpm下离心30min，收集上清液以分离未剥离的粉末；然后，将上清液以转速n2为10000rpm下离心30min，并收集离心管壁上的沉积物，该沉积物为二维纳米材料无机填料；
2)制备车用逆变电容器的钛酸铋钠基材料：
首先将钛酸铋钠基的原料如碳酸钠、二氧化钛和三氧化二铋置于鼓风干燥箱内，并在110℃下保温11h以去除原料中的水分。随后根据实际所需原料的质量，并在配料时过量加入3mol％的Bi2O3，防止其在烧结时发生挥发，从而产生质量损失。将所需的原料放置于尼龙球磨罐中，按照质量百分比为原料：锆球：无水乙醇＝1:5:2，在原料中加入氧化锆球和无水乙醇，进行第一次球磨，第一次球磨时间为12h，随后将球磨后得到的浆料放置于烧杯中，然后放入恒温鼓风干燥箱中干燥24h，而得到干燥的瓷料粉体，随后将干燥的瓷料粉体放入坩埚中压实进行第一次预烧结。
将第一次预烧结后的粉体进行第二次球磨，第二次球磨时间为24h，待烘干再进行第二次烧结；随后将二维BN纳米材料无机填料放入第二次烧结的样品中进行第三次球磨，第三次球磨时间为12h，并进行烘干而得到坯体。
将烘干的坯体放入研钵中进行研碎后，接着向烘干后的粉体中加入5wt.％的PVA溶液作为粘结剂进行造粒；造粒后的粉体需要在空气中陈腐24h，然后在210MPa的压力下成型得到厚度为2mm、直径为10mm直径的圆片样品。将成型得到的圆片样品作排胶处理，即在温度为560℃下保温时间为11h，升温速度为0.9℃/min，从而缓慢排出样品中的粘结剂。将排胶后的生胚放入硅钼炉内进行第三次烧结，烧结温度为950℃，升温速度设置为3℃/min，保温时间为2h，从而得到最后样品。
实施例11：
本实施例与上述实施例1的区别仅在于：核心材料不同，具体地，核心材料选用钛酸钡基。钛酸钡基为现有的钛酸钡基，所制备出的为钛酸钡基材料。
实施例12：
本实施例与上述实施例1的区别仅在于：核心材料不同，具体地，核心材料选用铌酸钾钠基。铌酸钾钠基为现有的铌酸钾钠，所制备出的为铌酸钾钠基材料。
实施例13：
本实施例与上述实施例1的区别仅在于：核心材料不同，具体地，核心材料选用铌酸钠基。铌酸钠基为现有的铌酸钠，所制备出的为铌酸钠基材料。
实施例14：
本实施例与上述实施例1的区别仅在于：核心材料不同，具体地，核心材料选用铌酸银基。铌酸银基为现有的铌酸银，所制备出的为铌酸银基材料。
实施例15：
本实施例与上述实施例1的区别仅在于：核心材料不同，具体地，核心材料选用钛酸铋基。钛酸铋基为现有的钛酸铋，所制备出的为钛酸铋基材料。
Claims (7)
1.一种高温高能高效车用逆变电容器核心材料的制备方法，其特征在于，依次包括以下步骤：
1）制备二维BN：
将BN粉体在250~350mA的振幅下搅拌20~25h；随后，放置于离心管内，并在转速n1为2000~4000rpm下离心20~40min，收集上清液以分离未剥离的粉末；然后，将上清液以转速n2为9000~11000rpm下离心20~40min，并收集离心管壁上的沉积物，该沉积物为二维BN纳米材料无机填料；
2）制备车用逆变电容器的核心材料：
S1：先将核心材料钛酸铋钠基的原料进行干燥，随后将所需要的原料量置于球磨罐中进行研磨，按照质量百分比为原料量：锆球：无水乙醇 = 1: 5: 2，在原料中加入氧化锆球和无水乙醇进行第一次球磨，球磨后将得到的浆料进行干燥，从而得到干燥的瓷料粉体，随后将干燥的瓷料粉体放入坩埚中压实并进行第一次预烧结；所述钛酸铋钠基材料的原料为碳酸钠、二氧化钛和三氧化二铋，且在配料中多加入3 mol%的三氧化二铋；
S2：随后将第一次预烧结后的粉体进行第二次球磨，待球磨后进行烘干，在烘干后进行第二次烧结；随后将二维BN纳米材料无机填料放入第二次烧结后的粉体中进行第三次球磨，待球磨后进行烘干得到坯体；
S3：将坯体放入研钵进行研碎后，向粉碎后的粉体中加入粘结剂聚乙烯醇溶液进行造粒，造粒后的粉体在空气中陈腐后压制成样品，在步骤S3中，在压力为190~210MPa下，得到厚度为2 mm、直径为10 mm的圆片样品；
S4：将样品进行排胶处理；
S5：将排胶后的生胚在800~1200°C温度下进行第三次烧结，从而制备出所需的核心材料。
2.根据权利要求1所述的制备方法，其特征在于：第一次球磨的时间为12h，第二次球磨的时间为24h，第三次球磨的时间为12h。
3.根据权利要求1所述的制备方法，其特征在于：在步骤S1中，首次干燥的温度为90~110℃，保温时间为11~13h。
4.根据权利要求3所述的制备方法，其特征在于：在步骤S1中，首次干燥的温度为100℃，保温时间为12h。
5.根据权利要求1所述的制备方法，其特征在于：所述排胶处理为在温度为540~560°C下，保温时间为11~13h，升温速度为0.9~1.1 °C /min下进行排出粘结剂。
6.根据权利要求5所述的制备方法，其特征在于：排胶处理的温度为550°C，保温时间为12h，升温速度为1°C /min。
7.根据权利要求1所述的制备方法，其特征在于：在步骤S5中，第三次烧结时的升温速度为3 ℃/min，保温时间为 2h。
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