CN110423116B - 一种x7r型陶瓷电容器介质材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种X7R型陶瓷电容器介质材料及其制备方法。将碳酸钡、碳酸锶、三氧化二钐、三氧化二铁和五氧化二铌先球磨,细化原料,根据名义化学式按化学计量比配料,经预烧、二次球磨等工序,利用固相反应过程,最终制得X7R型陶瓷电容器介质材料Ba2Sr2SmFe0.5Nb9.5O30。本发明方法可获得优良的温度稳定性介电陶瓷材料,满足EIA X7R标准;本发明方法简单,节能减排,成本适中,适合批量生产。
Description
技术领域
本发明涉及一种X7R型陶瓷电容器介质材料及其制备方法,属于电子材料与器件技术领域。
背景技术
电容器是一类重要的无源电子器件,是电子、通信及信息产业中所不可或缺的器件,可以起到储存电荷、隔断直流、交流虑波、提供调谐及震荡等。近年来随着电子产业的不断发展,市场上对陶瓷电容器的要求也越来越高,既要小型化也要可靠性高。根据国际电子工业协会EIA(Electronic Industries Association)标准,X7R型MLCC是指以25℃的电容值为基准,在温度从-55℃到+125℃的范围内,电容变化率(ΔC/C25)≤±15%。X7R型MLCC在各种电子终端设备上已获得广泛应用的应用。当前铅基铁电X7R型陶瓷系统运用较为广泛,但是因为该系统中含铅,在生产和应用过程中会对人体和环境造成极大的危害。因此,研发具有X7R特性的无铅介电材料具有重要的意义与实际运用价值。本发明采用钨青铜结构,有助于拓展陶瓷电容器材料的结构类型,减少铅基陶瓷对人体和环境造成的危害。
发明内容
本发明的目的是提供一种X7R型陶瓷电容器介质材料及其制备方法。
本发明的X7R型陶瓷电容器介质材料的名义化学式为Ba2Sr2SmFe0.5Nb9.5O30。
制备上述的X7R型陶瓷电容器介质材料的方法的具体步骤为:
(1)将纯度大于99.9%的BaCO3、SrCO3、Sm2O3、Fe2O3和Nb2O5作为起始原料,按照BaCO3:SrCO3:Sm2O3:Fe2O3:Nb2O5=2:2:0.5:0.25:4.75的摩尔比进行配料,以无水乙醇为球磨介质,混合球磨24小时,于100℃下烘干4小时,制得烘干样品。
(2)把步骤(1)制得的烘干样品在1000~1150℃预烧结4小时,制得预烧后的粉体。
(3)将步骤(2)制得的预烧后的粉体研碎,再以无水乙醇为球磨介质球磨24小时混合均匀,于100℃下烘干4小时后研磨成粉状,加入8wt%的聚乙烯醇水溶液,造粒,然后过60目筛后压制成型,于400~600℃下保温3~5小时排出胶体,再在高温炉空气气氛中1100~1300℃烧结4~10小时后随炉自然冷却至室温,即制得X7R型陶瓷电容器介质材料。
本发明采用传统的固相法制备介质材料,在中温下烧结即可获得性能优良的X7R型陶瓷材料,工艺简单,成本低廉,对环境无害,且所制得的X7R型陶瓷电容器介质材料的温度稳定性好,能够在-55~125℃的范围内满足(ΔC/C25)≤±15%,满足EIA的X7R标准;本发明所提供的陶瓷电容器介质材料及其制备方法,具有良好的产业化前景。
附图说明
图1为本发明实施例制得的Ba2Sr2SmFe0.5Nb9.5O30陶瓷电容器介质材料的X射线衍射图谱。
图2为本发明实施例制得的Ba2Sr2SmFe0.5Nb9.5O30陶瓷电容器介质材料的表面显微形貌照片。
图3为本发明实施例制得的Ba2Sr2SmFe0.5Nb9.5O30陶瓷电容器介质材料的介电常数随温度变化的规律图。
图4为本发明实施例制得的Ba2Sr2SmFe0.5Nb9.5O30陶瓷电容器介质材料的电容变化率随温度变化的规律图,从图中看出,在室温时介电常数变化在±15%以内。
具体实施方式
实施例1:
将纯度均为99.99%的BaCO3、SrCO3、Sm2O3、Fe2O3和Nb2O5原料按化学计量比为Ba2Sr2SmFe0.5Nb9.5O30配料放入球磨罐中;选择氧化锆球和尼龙罐;所加原料质量为磨球质量的8%;混合球磨时间为24小时,转速为350转/分钟,球磨介质为无水乙醇;所得产物置于100℃的烘箱中烘干4小时,以5℃/分的升温速率升至1000℃预烧结4小时;取出预烧后的粉体研碎,再以无水乙醇为球磨介质球磨24小时混合均匀,于100℃下烘干4小时后研磨成粉状,用质量百分浓度为8%的聚乙烯醇水溶液作为粘结剂造粒,过60目的筛子后在100MPa压强下压成直径为10mm,厚度为1mm的圆片状生坯,以1.5℃/分的升温速率升至400℃,保温3小时排出胶体,再以5℃/分的升温速率升至1100℃于高温炉空气气氛中保温4小时进行烧结,最后随炉自然冷却至室温,即制得X7R型陶瓷电容器介质材料Ba2Sr2SmFe0.5Nb9.5O30。
实施例2:
将纯度均为99.99%的BaCO3、SrCO3、Sm2O3、Fe2O3和Nb2O5原料按化学计量比为Ba2Sr2SmFe0.5Nb9.5O30配料放入球磨罐中;选择氧化锆球和尼龙罐;所加原料质量为磨球质量的8%;混合球磨时间为24小时,转速为350转/分钟,球磨介质为无水乙醇;所得产物置于100℃的烘箱中烘干4小时,以5℃/分的升温速率升至1100℃预烧结4小时;取出预烧后的粉体研碎,再以无水乙醇为球磨介质球磨24小时混合均匀,于100℃下烘干4小时后研磨成粉状,用质量百分浓度为8%的聚乙烯醇水溶液作为粘结剂造粒,过60目的筛子后在100MPa压强下压成直径为10mm,厚度为1mm的圆片状生坯,以1.5℃/分的升温速率升至550℃,保温4小时排出胶体,再以5℃/分的升温速率升至1250℃于高温炉空气气氛中保温6小时进行烧结,最后随炉自然冷却至室温,即制得X7R型陶瓷电容器介质材料Ba2Sr2SmFe0.5Nb9.5O30。
实施例3:
将纯度均为99.99%的BaCO3、SrCO3、Sm2O3、Fe2O3和Nb2O5原料按化学计量比为Ba2Sr2SmFe0.5Nb9.5O30配料放入球磨罐中;选择氧化锆球和尼龙罐;所加原料质量为磨球质量的8%;混合球磨时间为24小时,转速为350转/分钟,球磨介质为无水乙醇;所得产物置于100℃的烘箱中烘干4小时,以5℃/分的升温速率升至1150℃预烧结4小时;取出预烧后的粉体研碎,再以无水乙醇为球磨介质球磨24小时混合均匀,于100℃下烘干4小时后研磨成粉状,用质量百分浓度为8%的聚乙烯醇水溶液作为粘结剂造粒,过60目的筛子后在100MPa压强下压成直径为10mm,厚度为1mm的圆片状生坯,以1.5℃/分的升温速率升至600℃,保温5小时排出胶体,再以5℃/分的升温速率升至1300℃于高温炉空气气氛中保温10小时进行烧结,最后随炉自然冷却至室温,即制得X7R型陶瓷电容器介质材料Ba2Sr2SmFe0.5Nb9.5O30。
将上述实施例制得的X7R型陶瓷电容器介质材料两侧均烧上银电极,制成圆片电容器,然后测试并计算该介质材料的相对介电常数随温度的变化情况,如附图3所示,Ba2Sr2SmFe0.5Nb9.5O30陶瓷材料在很宽的温度区间内具有平稳的温度特性,满足X7R标准,即电容变化率在-55~125℃范围内不超过±15%,能作为X7R型陶瓷电容器介质材料。
Claims (2)
1.一种X7R型陶瓷电容器介质材料,其特征在于该X7R型陶瓷电容器介质材料的名义化学式为Ba2Sr2SmFe0.5Nb9.5O30。
2.根据权利要求1所述的X7R型陶瓷电容器介质材料的制备方法,其特征在于具体步骤为:
(1)将纯度大于99.9%的BaCO3、SrCO3、Sm2O3、Fe2O3和Nb2O5作为起始原料,按照BaCO3:SrCO3:Sm2O3:Fe2O3:Nb2O5=2:2:0.5:0.25:4.75的摩尔比进行配料,以无水乙醇为球磨介质,混合球磨24小时,于100℃下烘干4小时,制得烘干样品;
(2)把步骤(1)制得的烘干样品在1000~1150℃预烧结4小时,制得预烧后的粉体;
(3)将步骤(2)制得的预烧后的粉体研碎,再以无水乙醇为球磨介质球磨24小时混合均匀,于100℃下烘干4小时后研磨成粉状,以8wt%的聚乙烯醇水溶液作为粘结剂造粒,然后过60目筛后压制成型,于400~600℃下保温3~5小时排出胶体,再在高温炉空气气氛中1100~1300℃烧结4~10小时后随炉自然冷却至室温,即制得X7R型陶瓷电容器介质材料。
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