CN105884352A - 一种新型陶瓷电容器材料Ba4RFe0.5Nb9.5O30（R=La，Eu，Gd）及其制备方法 - Google Patents

一种新型陶瓷电容器材料Ba4RFe0.5Nb9.5O30（R=La，Eu，Gd）及其制备方法 Download PDF

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CN105884352A
CN105884352A CN201610226683.1A CN201610226683A CN105884352A CN 105884352 A CN105884352 A CN 105884352A CN 201610226683 A CN201610226683 A CN 201610226683A CN 105884352 A CN105884352 A CN 105884352A
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capacitor material
ceramic capacitor
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胡长征
朱其华
孙振
方亮
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Guilin University of Technology
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Abstract

本发明公开了一种新型电容器陶瓷材料Ba4RFe0.5Nb9.5O30（R=La，Eu，Gd）及其制备方法。将BaCO3，La2O3，Eu2O3，Gd2O3，Fe2O3和Nb2O5为起始原料，根据化学计量比Ba4RFe0.5Nb9.5O30（R=La，Eu，Gd）进行配料，经过预烧、二次球磨工序，利用固相反应法制备陶瓷电容器材料Ba4RFe0.5Nb9.5O30（R=La，Eu，Gd）。本发明方法可获得优良的新稳定型陶瓷电容器材料；本发明方法简单，节能减排，成本适中，适合批量生产。

Description

一种新型陶瓷电容器材料 Ba4RFe0.5Nb9.5O30 （ R=La ， Eu ， Gd ）及其制备方法
技术领域
本发明涉及一种新型陶瓷电容器材料Ba4RFe0.5Nb9.5O30（R= La，Eu， Gd）及其制备方法,属于电子元器件的陶瓷材料技术领域。
背景技术
陶瓷电容器材料是电子信息技术的重要基础器件，随着电子器件的飞速发展，要求陶瓷电容器材料能够在更宽的温度范围内保持稳定的介电性能。在军工、航天航空以及勘探等领域里，对于能承受高温的电子元器件有很大需求。目前大多数陶瓷电容器材料容量温度特性具有一定的局限性。因此，研发具有较宽温度稳定性的陶瓷电容器材料，具有重要的实际应用价值。另外，大多数陶瓷电容器材料基于钙钛矿结构，本发明采用钨青铜结构，有助于扩展电容器陶瓷的材料类型。
发明内容
1.本发明的目的是提供一种新型陶瓷电容器材料Ba4RFe0.5Nb9.5O30（R= La，Eu，Gd）及其制备方法。
2.本发明涉及的新型陶瓷电容器材料的化学组成式为：Ba4RFe0.5Nb9.5O30（R= La，Eu，Gd）。
3.上述新型陶瓷电容器材料的方法具体步骤为：
（1）将纯度大于99.9%的BaCO3，La2O3，Eu2O3，Gd2O3，Fe2O3和Nb2O5为起始原料，按照BaCO3：R2O3：Fe2O3：Nb2O5 =4:0.5：0.25:4.75（R= La，Eu，Gd）的摩尔比进行配料，加入无水乙醇中，混合球磨48小时，烘干制得混合均匀的物料；
（2）将步骤（1）的粉料在1280℃预烧4个小时，制得预烧后的粉体；
（3）将步骤（2）预烧后的粉体，在无水乙醇中球磨48小时混合均匀，烘干；加入5~10wt%聚乙烯醇水溶液进行造粒，过60目筛后压制成型，然后置于高温炉空气气氛中，在1280℃烧结4～10小时后自然冷却至室温，即得到所述新型陶瓷电容器材料Ba4RFe0.5Nb9.5O30（R= La，Eu， Gd）。
所述的聚乙烯醇水溶液的优选浓度为8wt%。
4.本发明提供所述新型陶瓷电容器材料，低温时稳定性好。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新型陶瓷电容器材料，且工艺简单，成本低廉，对环境无害。在我国，介质陶瓷材料正处在不断发展之中，尤其是像很多此类温度较为稳定的特种介质陶瓷，研究尚未完善，仍未实现规模化产业化。因而，本发明所提供的陶瓷电容器材料及其制备方法，具有良好的产业化前景。
附图说明
图1为本发明实施例1制得的样品Ba4LaFe0.5Nb9.5O30陶瓷电容器材料的X射线图谱；
图2为本发明实施例1制得的Ba4LaFe0.5Nb9.5O30陶瓷电容器材料的表面显微形貌照片；
图3为本发明实施例1制得的Ba4LaFe0.5Nb9.5O30陶瓷电容器材料的介电常数随温度变化规律；
图4为本发明实施例1制得的Ba4LaFe0.5Nb9.5O30陶瓷电容器材料的电容变化率与温度关系；
图5为本发明实施例2制得的Ba4EuFe0.5Nb9.5O30陶瓷电容器材料的X射线图谱；
图6为本发明实施例2制得的Ba4EuFe0.5Nb9.5O30陶瓷电容器材料的表面显微形貌照片；
图7为本发明实施例2制得的Ba4EuFe0.5Nb9.5O30陶瓷电容器材料的介电常数随温度变化规律；
图8为本发明实施例2制得的Ba4EuFe0.5Nb9.5O30陶瓷电容器材料的温度与电容变化率关系；
图9为本发明实施例3制得的Ba4GdFe0.5Nb9.5O30陶瓷电容器材料的X射线图谱；
图10为本发明实施例3制得的Ba4GdFe0.5Nb9.5O30陶瓷电容器材料的表面显微形貌照片；
图11为本发明实施例3制得的Ba4GdFe0.5Nb9.5O30陶瓷电容器材料的介电常数随温度变化规律；
图12为本发明实施例3制得的Ba4GdFe0.5Nb9.5O30陶瓷电容器材料的温度与电容变化率关系。
具体实施方式
本发明的新型陶瓷电容器材料的化学通式为Ba4RFe0.5Nb9.5O30，其中R为稀土元素，此处R= La，Eu，Gd。下列实施例中的稀土元素在La，Eu，Gd中变化。将纯度大于99.9%的BaCO3，R2O3，Fe2O3和Nb2O5为起始原料，按化学计量比为Ba4RFe0.5Nb9.5O30配料放入球磨罐中, 选择氧化锆球和尼龙罐；所加粉体质量为磨球质量的8%；球磨时间为48个小时，转速为350转/分钟，球磨介质为无水乙醇；所得产物置于120℃的烘箱中烘干4小时以上，先以5℃/min的升温速率升至1280℃预烧4小时；取出预烧后的粉体研碎，以无水乙醇为介质再次球磨48小时混合均匀，烘干后研磨成粉状，用质量百分浓度为8％的聚乙醇水溶液(PVA) 作为有机粘结剂造粒，过60目筛子后在6MPa 压强下压成直径为12mm，厚度为1mm 的圆片状生坯；将圆片生坯以3℃/min的升温速率升至550℃，保温4小时排出胶体再以5℃/min的升温速率升至1280℃，保温10小时，随炉自然冷却至室温，得到陶瓷电容器材料Ba4RFe0.5Nb9.5O30(R= La，Eu，Gd)。
实施例1
1.将纯度大于99.9%的BaCO3，La2O3，Fe2O3和Nb2O5为起始原料，按化学计量比为Ba4LaFe0.5Nb9.5O30配料放入球磨罐中，选择氧化锆球和尼龙罐；所加粉体质量为磨球质量的8%；球磨时间为48个小时，转速为350转/分钟，球磨介质为无水乙醇；所得产物置于120℃的烘箱中烘干4小时以上，先以5℃/min的升温速率升至1000℃预烧4小时；取出预烧后的粉体研碎，以无水乙醇为介质再次球磨48小时混合均匀，烘干后研磨成粉状，用质量百分浓度为8％的聚乙醇水溶液(PVA) 作为有机粘结剂造粒，过60目筛子后在6MPa 压强下压成直径为12mm，厚度为1mm 的圆片状生坯；将圆片生坯以3℃/min的升温速率升至550℃，保温4小时排出胶体再以5℃/min的升温速率升至1280℃，保温10小时，随炉自然冷却至室温，得到陶瓷电容器材料Ba4LaFe0.5Nb9.5O30。
将本实施例1制得的陶瓷电容器材料两侧均烧上银电极，制成圆片电容器，然后测试并计算该电容器材料的相对介电常数随温度的变化。如附图3所示样品的相对介电常数随温度的变化规律，图4直观的展示了Ba4LaFe0.5Nb9.5O30陶瓷材料在很宽的温度区间内具有平稳的温度特性，进一步证明其可作为一种温度稳定型陶瓷电容器材料。
实施例2
将纯度大于99.9%的BaCO3，Eu2O3，Fe2O3和Nb2O5为起始原料，按化学计量比为Ba4EuFe0.5Nb9.5O30配料放入球磨罐中，选择氧化锆球和尼龙罐；所加粉体质量为磨球质量的8%；球磨时间为48个小时，转速为350转/分钟，球磨介质为无水乙醇；所得产物置于120℃的烘箱中烘干4小时以上，先以5℃/min的升温速率升至1280℃预烧4小时；取出预烧后的粉体研碎，以无水乙醇为介质再次球磨48小时混合均匀，烘干后研磨成粉状，用质量百分浓度为8％的聚乙醇水溶液(PVA) 作为有机粘结剂造粒，过60目筛子后在6MPa 压强下压成直径为12mm，厚度为1mm 的圆片状生坯；将圆片生坯以3℃/min的升温速率升至550℃，保温4小时排出胶体再以5℃/min的升温速率升至1280℃，保温10小时，随炉自然冷却至室温，得到陶瓷电容器材料Ba4EuFe0.5Nb9.5O30。
将本实施例2制得的陶瓷电容器材料两侧均烧上银电极，制成圆片电容器，然后测试并计算该电容器材料的相对介电常数随温度的变化。如附图7所示样品的相对介电常数随温度的变化规律，图8直观的展示了Ba4EuFe0.5Nb9.5O30陶瓷材料在很宽的温度区间内具有平稳的温度特性，进一步证明其可作为一种温度稳定型陶瓷电容器材料。
实施例3
将纯度大于99.9%的BaCO3，Gd2O3，Fe2O3和Nb2O5为起始原料，按化学计量比为Ba4GdFe0.5Nb9.5O30配料放入球磨罐中，选择氧化锆球和尼龙罐；所加粉体质量为磨球质量的8%；球磨时间为48个小时，转速为350转/分钟，球磨介质为无水乙醇；所得产物置于120℃的烘箱中烘干4小时以上，先以5℃/min的升温速率升至1280℃预烧4小时；取出预烧后的粉体研碎，以无水乙醇为介质再次球磨48小时混合均匀，烘干后研磨成粉状，用质量百分浓度为8％的聚乙醇水溶液(PVA) 作为有机粘结剂造粒，过60目筛子后在6MPa 压强下压成直径为12mm，厚度为1mm 的圆片状生坯；将圆片生坯以3℃/min的升温速率升至550℃，保温4小时排出胶体再以5℃/min的升温速率升至1280℃，保温10小时，随炉自然冷却至室温，得到陶瓷电容器材料Ba4GdFe0.5Nb9.5O30。
将本实施例3制得的陶瓷电容器材料两侧均烧上银电极，制成圆片电容器，然后测试并计算该电容器材料的相对介电常数随温度的变化。如附图11所示样品的相对介电常数随温度的变化规律，图12直观的展示了Ba4GdFe0.5Nb9.5O30陶瓷材料在很宽的温度区间内具有平稳的温度特性，进一步证明其可作为一种温度稳定型陶瓷电容器材料。

Claims (2)

1.一种新型陶瓷电容器材料，其特征在于所述陶瓷电容器材料的化学组成式为Ba4RFe0.5Nb9.5O30（R=La，Eu，Gd）；
所述的陶瓷电容器材料的制备步骤为：
（1）将纯度大于99.9%的BaCO3，La2O3，Eu2O3，Gd2O3，Fe2O3和Nb2O5为起始原料，按照BaCO3：R2O3：Fe2O3：Nb2O5 =4:0.5：0.25:4.75（R=La，Eu，Gd）的摩尔比进行配料，加入无水乙醇中，混合球磨48小时，烘干制得混合均匀的物料；
（2）将步骤（1）制得的物料在1280℃预烧4个小时，制得预烧后的粉体；
（3）将步骤（2）预烧后的粉体，在无水乙醇中球磨48小时混合均匀，烘干；加入5~10wt%聚乙烯醇水溶液进行造粒，过60目筛后压制成型，然后置于高温炉空气气氛中，在1280℃烧结4～10小时后自然冷却至室温，即得到所述新型陶瓷电容器材料Ba4RFe0.5Nb9.5O30（R=La，Eu，Gd）。
2.根据权利要求1所述的新型陶瓷电容器材料的制备方法，其特征在于所述的聚乙烯醇水溶液的质量浓度为8wt%。
CN201610226683.1A 2016-04-12 2016-04-12 一种新型陶瓷电容器材料Ba4RFe0.5Nb9.5O30（R=La，Eu，Gd）及其制备方法 Pending CN105884352A (zh)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106565240A (zh) * 2016-11-05 2017-04-19 桂林理工大学 一种铁基陶瓷电容器材料及其制备方法
CN108101538A (zh) * 2017-12-29 2018-06-01 陕西科技大学 一种钨青铜型高储能密度陶瓷材料及其制备方法
CN108218423A (zh) * 2018-01-11 2018-06-29 桂林理工大学 一种x8r型陶瓷电容器介质材料及其制备方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106565240A (zh) * 2016-11-05 2017-04-19 桂林理工大学 一种铁基陶瓷电容器材料及其制备方法
CN108101538A (zh) * 2017-12-29 2018-06-01 陕西科技大学 一种钨青铜型高储能密度陶瓷材料及其制备方法
CN108218423A (zh) * 2018-01-11 2018-06-29 桂林理工大学 一种x8r型陶瓷电容器介质材料及其制备方法

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