CN108863358B - 一种宽温度稳定型陶瓷电容器介质材料及其制备方法 - Google Patents
一种宽温度稳定型陶瓷电容器介质材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种宽温度稳定型陶瓷电容器介质材料及其制备方法，所述陶瓷组份的化学通式为(1‑x)(K0.5Na0.5)NbO3‑xSr(In0.5Nb0.5)O3，其中x表示摩尔分数，0.1≤x≤0.2。所述制备方法为固相反应烧结法，将K2CO3、Na2CO3、SrCO3、In2O3和Nb2O5按化学比例称料，然后多种粉体先后经过球磨、预烧、煅烧、造粒、成型和烧结，制备出具有宽温度稳定特性的铌酸钾钠基陶瓷电容器介质材料，在‑60℃至300℃具有稳定的介电性能，且具有制备方法简单、成本低和无铅环保等优势。
Description
技术领域
本发明属于介质陶瓷材料领域，具体涉及一种铌酸钾钠宽温度稳定型陶瓷电容器介质材料及其制备方法。
背景技术
片式多层陶瓷电容器(MLCC)在整个电容器领域中占据着第一大分支的地位，因其具有尺寸小、电容量大、介电损耗低、击穿场强高和耐腐蚀等诸多优点被广泛地应用于各种军、民用电子整机和电子设备领域，如电视、电脑、电话、手机、汽车等产品和设备，目前已经成为应用最广泛的被动元件产品。
随着科技的发展，军工、航天、汽车电子等领域的工作需要在更极端的温度环境下进行，因此要求MLCC不仅要有较大的温度使用范围和稳定的温度性能，而且要有材料环保、低成本的制备工艺。传统的X7R和X8R型陶瓷电容器工作温度上限分别为125℃和150℃已不能胜任，X9R型电容器具有更宽的温度区间。根据国际电子工业协会(EAI)所发布的标准，X9R型MLCC器件的工作温度在-55℃到200℃的范围内。目前，用于制造高介电常数MLCC器件的材料主要有铅基复合钙钛矿体系、钨青铜结构体系、BaTiO3体系三类。铅基复合钙钛矿体系因为含铅不符合环保要求而正在被法律、法规禁止并逐渐被取代，钨青铜结构体系具有介电常数高但损耗大且不稳定，BaTiO3体系是目前大部分商用MLCC所采用的介质材料，但其居里温度比较低且工作温区较窄。无铅(K0.5Na0.5)NbO3体系陶瓷材料具有较高的居里温度(420℃)，并且和BaTiO3体系一样具有钙钛矿结构，在以往的研究中被认为可以通过引入组分或掺杂改性，使其成为具有优异压电、铁电、介电、储能、应变等电学性能的新介质材料。
本发明对(K0.5Na0.5)NbO3陶瓷材料进行改性研究，通过引入其他组元与(K0.5Na0.5)NbO3形成固溶体，制备出了工作温度区间大、介电稳定性好的铌酸钾钠宽温度稳定型陶瓷电容器介质材料，在-60℃到300℃的范围内具有良好的介电稳定性。
发明内容
本发明的目的是提供一种介电稳定性高的铌酸钾钠基宽温度稳定型陶瓷电容器介质材料及其制备方法。
本发明所述陶瓷组份的化学通式为(1-x)(K0.5Na0.5)NbO3-xSr(In0.5Nb0.5)O3，其中x表示摩尔分数，0.1≤x≤0.2。
制备上述宽温度稳定型陶瓷电容器介质材料的具体步骤为：
(1)按照化学通式(1-x)(K0.5Na0.5)NbO3-xSr(In0.5Nb0.5)O3称量K2CO3、Na2CO3、SrCO3、In2O3和Nb2O5粉体原料进行配料，0.1≤x≤0.2。
(2)原料粉体加入无水乙醇球磨均匀混合，球磨浆料在90℃干燥，然后在950℃预烧5小时，冷却的预烧粉体研磨后再以950℃煅烧5小时。
(3)煅烧粉体用无水乙醇再次进行球磨破碎，90℃烘干后过筛，加入粘接剂造粒，用金属模具将粉体压制成圆片。
(4)将模压生坯放置在氧化铝承烧板上进行高温烧结，温度下降至600℃后停止加热，使炉温自然冷却至室温，然后取出陶瓷片。
附图说明
图1a、图1b、图1c分别是本发明实施例在x=0.10、x=0.15和x=0.20时制得的介质材料于-150℃～200℃温度范围内测试得到的介电温谱。
图2a、图2b、图2c分别是本发明实施例在x=0.10、x=0.15和x=0.20时制得的介质材料于室温到450℃温度范围内测试得到的介电温谱。
具体实施方式
实施例1：
(1)按照x=0.1的化学计量比称量K2CO3、Na2CO3、SrCO3、In2O3和Nb2O5原料粉体并倒入球磨罐中，加入无水乙醇后球磨24小时，在90℃干燥处理，过100目筛，放入坩埚中以950℃预烧5小时，取出预烧粉体进行研磨，再以950℃煅烧5小时，获得煅烧粉体。
(2)将煅烧粉体再次用无水乙醇球磨24小时，90℃烘干后过100目筛，添加浓度为5wt%的聚乙烯醇溶液为粘结剂造粒，将粉体放入金属模具以10MPa压力成型生坯。
(3)在氧化铝承烧板上铺垫氧化锆粉体，然后将生坯放在氧化锆粉体上，使用小尺寸的氧化铝坩埚倒扣罩住生坯，将小坩埚边缘用氧化锆粉体填充形成封闭式整体，最后以大尺寸的氧化铝坩埚倒扣罩住小坩埚。
(4)将放置有生坯的承烧板置于烧结炉中，采用1℃/min的升温度升温至1230℃并保温5小时，然后以1℃/min的速度降温至600℃后冷却至室温。
(5)烧结后的陶瓷抛光处理，加工成两面光滑、厚度为0.50mm的薄片，然后制备银电极制成圆片电容器，进行电学性能测试。
实施例2：
(1)按照x=0.15的化学计量比称量K2CO3、Na2CO3、SrCO3、In2O3和Nb2O5原料粉体并倒入球磨罐中，加入无水乙醇后球磨24小时，在90℃干燥处理，过100目筛，放入坩埚中以950℃预烧5小时，取出预烧粉体进行研磨，再以950℃煅烧5小时，获得煅烧粉体。
(2)将煅烧粉体再次用无水乙醇球磨24小时，90℃烘干后过100目筛，添加浓度为5wt%的聚乙烯醇溶液为粘结剂造粒，将粉体放入金属模具以10MPa压力成型生坯。
(3)在氧化铝承烧板上铺垫氧化锆粉体，然后将生坯放在氧化锆粉体上，使用小尺寸的氧化铝坩埚倒扣罩住生坯，将小坩埚边缘用氧化锆粉体填充形成封闭式整体，最后以大尺寸的氧化铝坩埚倒扣罩住小坩埚。
(4)将放置有生坯的承烧板置于烧结炉中，采用1℃/min的速度升温至1230℃并保温5小时，然后以1℃/min的速度降温至600℃后冷却至室温。
(5)烧结后的陶瓷抛光处理，加工成两面光滑、厚度为0.50mm的薄片，然后制备银电极制成圆片电容器，进行电学性能测试。
实施例3：
(1)按照x=0.2的化学计量比称量K2CO3、Na2CO3、SrCO3、In2O3和Nb2O5原料粉体并倒入球磨罐中，加入无水乙醇后球磨24小时，在90℃干燥处理，过100目筛，放入坩埚中以950℃预烧5小时，取出预烧粉体进行研磨，再以950℃煅烧5小时，获得煅烧粉体。
(2)将煅烧粉体再次用无水乙醇球磨24小时，90℃烘干后过100目筛，添加浓度为5wt%的聚乙烯醇溶液为粘结剂造粒，将粉体放入金属模具以10MPa压力成型生坯。
(3)在氧化铝承烧板上铺垫氧化锆粉体，然后将生坯放在氧化锆粉体上，使用小尺寸的氧化铝坩埚倒扣罩住生坯，将小坩埚边缘用氧化锆粉体填充形成封闭式整体，最后以大尺寸的氧化铝坩埚倒扣罩住小坩埚。
(4)将放置有生坯的承烧板置于烧结炉中，采用1℃/min的速度升温至1270℃并保温5小时，然后以1℃/min的速度降温至600℃后冷却至室温。
(5)烧结后的陶瓷抛光处理，加工成两面光滑、厚度为0.50mm的薄片，然后制备银电极制成圆片电容器，进行电学性能测试。
上述实施例制出的配方为(1-x)(K0.5Na0.5)NbO3-xSr(In0.5Nb0.5)O3的铌酸钾钠宽温度稳定型陶瓷电容器介质材料，在较宽的温度区间内具有稳定的温度特性，因此是制备宽温度稳定型陶瓷电容器潜在应用材料。
Claims (3)
1.一种宽温度稳定型陶瓷电容器介质材料，其特征在于所述材料的化学通式为
(1-x)(K0.5Na0.5)NbO3-xSr(In0.5Nb0.5)O3，0.1≤x≤0.2；所述材料的制备方法至少包括如下步骤：
（1）按照化学通式(1-x)(K0.5Na0.5)NbO3-xSr(In0.5Nb0.5)O3称量K2CO3、Na2CO3、SrCO3、In2O3和Nb2O5粉体原料进行配料，0.1≤x≤0.2；
（2）原料粉体加入无水乙醇球磨均匀混合，球磨浆料在90℃干燥，然后在950℃预烧5小时，冷却的预烧粉体研磨后再以950℃煅烧5小时；
（3）煅烧粉体用无水乙醇再次进行球磨破碎，90℃烘干后过筛，加入粘接剂造粒，用金属模具将粉体压制成圆片；
（4）将模压生坯放置在氧化铝承烧板上进行高温烧结，温度下降至600℃后停止加热，使炉温自然冷却至室温，然后取出陶瓷片；其中：用1℃/min的速度升温至烧结温度，烧结温度为1230~1270℃，保温时间为5小时，用1℃/min的速度降温至600℃。
2.根据权利要求1所述的介质材料，其特征在于：介质材料制备方法的步骤(4)中在氧化铝承烧板上铺垫一层氧化锆大颗粒粉体，防止烧结生坯与承烧板粘接。
3.根据权利要求1所述的介质材料，其特征在于：介质材料制备方法的步骤(4)中使用坩埚倒扣罩住生坯，形成压力气氛避免生坯中易挥发组分挥发逸出。
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