CN107188564A - 一种高介电性能的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料及其制备方法 - Google Patents

一种高介电性能的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料及其制备方法 Download PDF

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CN107188564A
CN107188564A CN201710577430.3A CN201710577430A CN107188564A CN 107188564 A CN107188564 A CN 107188564A CN 201710577430 A CN201710577430 A CN 201710577430A CN 107188564 A CN107188564 A CN 107188564A
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ferroelectric ceramic
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魏灵灵
郝胜兰
杨祖培
晁小练
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Abstract

本发明公开了一种高介电性能的Eu3+掺杂铌酸锶钙钠钨青铜发光铁电陶瓷材料及其制备方法，该陶瓷材料的结构通式为Sr1.90Ca0.15Na0.90‑3xEuxNb5O15，其中x的取值为0.02～0.06。本发明通过配料、预烧、球磨、造粒、压片、烧结等传统固相的工艺步骤制备Sr1.90Ca0.15Na0.90‑3xEuxNb5O15陶瓷，制备方法成本低廉，操作方便。本发明通过在陶瓷材料中掺杂Eu3+，明显提高了其介电、铁电性能，其中x＝0.05时，其最大介电常数为1270、居里温度为263℃、剩余极化强度为6.6μC/cm2、室温介电常数达到1700。除此之外，本发明陶瓷材料还具有良好的光致发光性能，在395nm光激发都能在617nm处有很强的红光发射。

Description

一种高介电性能的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料及 其制备方法
技术领域
本发明属于材料技术领域，具体涉及一种高介电性能的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料及其制备方法。
背景技术
近年来，无铅压铁电材料除了研究提高压铁电性能以期替代含铅材料外，还在储能、应变、电卡、热电、光电、发光等方面发现新的功能特性，使其受到越来越多的关注。随着材料设计理论的发展和制备技术的创新，无机电子信息材料需向着高效能、高可靠、智能化和功能集成化方向发展，期待在同一种压铁电材料中实现多个功能响应，使其成为新型智能化材料是该领域的研究热点。
目前，钨青铜结构材料研究主要集中在两个方面，分别是碱土稀土金属铌酸盐和碱土金属铌酸盐。前者主要集中于研究其低温的介电异常和弛豫行为，但是其介电性能偏低，限制其应用；后者主要研究通过调节钨青铜结构不同的间隙填空情况，使结构从未充满向充满型转变，以期提高介电和铁电性能。其中以充满型Sr2-xCaxNaNb5O15体系研究较多且最具有代表性。R.R.Neurgaonkar等人报道，在Sr2-xCaxNaNb5O15单晶体系中，当x＝0.10时其压电常数d33可达270pC/N。发明人所在的研究小组采用传统固相法研究了(Sr0.925Ca0.075)2.5-0.5xNaxNb5O15体系，通过调节Na的含量使钨青铜结构从未充满型向充满型转变，结果发现随着填充程度的增大，其电学性能也随之增大，但是当x＝1.0时，虽然结构处于充满型，但会生成第二相，恶化其电学性能。
发明内容
本发明所要解决的技术问题在于提供一种具有高介电性能且同时具有发光性能的Eu3+掺杂铌酸锶钙钠铁电陶瓷材料，并为该陶瓷材料提供一种制备方法。
解决上述技术问题所采用的陶瓷材料的通式为Sr1.90Ca0.15Na0.90-3xEuxNb5O15，其中x的取值为0.02～0.06，优选x的取值为0.05，该陶瓷材料为钨青铜结构。
本发明Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料的制备方法由下述步骤组成：
1、按照Sr1.90Ca0.15Na0.90-3xEuxNb5O15的化学计量比分别称取纯度为99.00％以上的Na2CO3、SrCO3、Nb2O5、CaCO3、Eu2O3，充分混合球磨16～24小时，在80～100℃下干燥12～24小时，得到原料混合物。
2、将原料混合物在1180～1250℃下预烧5～8小时，得到预烧粉。
3、将预烧粉经造粒、压片、排胶后，在1300～1380℃下烧结3～6小时，得到Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料。
上述步骤2中，优选将原料混合物在1200℃下预烧6小时。
上述步骤3中，优选将预烧粉经造粒、压片、排胶后，在1320℃下烧结4小时。
本发明通过在Sr1.90Ca0.15Na0.90Nb5O15体系中掺入Eu3+，使所得陶瓷材料具有优异的介电、铁电性能，同时还具有良好的红色发光性能，实现了多功能响应的耦合。
附图说明
图1是对比例1制备的铌酸锶钙钠铁电陶瓷材料及实施例1～4制备的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料的XRD图。
图2是实施例1～4制备的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料的发射光谱图。
图3是对比例1制备的铌酸锶钙钠铁电陶瓷材料在不同测试频率下的介电温镨图。
图4是实施例1制备的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料在不同测试频率下的介电温镨图。
图5是实施例2制备的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料在不同测试频率下的介电温镨图。
图6是实施例3制备的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料在不同测试频率下的介电温镨图。
图7是实施例4制备的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料在不同测试频率下的介电温镨图。
图8是对比例1制备的铌酸锶钙钠铁电陶瓷材料及实施例1～4制备的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料在10kHz下居里温度和最大介电常数的对比图。
图9是对比例1制备的铌酸锶钙钠铁电陶瓷材料及实施例1～4制备的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料的陶瓷材料的电滞回线。
图10是对比例1制备的铌酸锶钙钠铁电陶瓷材料及实施例1～4制备的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料的剩余极化强度和矫顽场对比图。
具体实施方式
下面结合附图和实施例对本发明进一步详细说明，但本发明的保护范围不仅限于这些实施例。
实施例1
1、按照Sr1.90Ca0.15Na0.84Eu0.02Nb5O15的化学计量分别称取纯度为99.80％的Na2CO30.8822g、纯度为99.00％的SrCO3 5.6038g、纯度为99.99％的Nb2O5 13.1445g、纯度为99.00％的CaCO3 0.3000g、纯度为99.99％的Eu2O3 0.0696g，装入尼龙罐中，以锆球为磨球、无水乙醇为球磨介质，用球磨机充分混合球磨24小时，置于干燥箱内在80℃下干燥15小时，用研钵研磨30分钟，得到原料混合物。
2、将原料混合物置于氧化铝坩埚内，用玛瑙棒压实，使其压实密度为1.5g/cm3，加盖，置于电阻炉内，以3℃/分钟的升温速率升温至1200℃预烧6小时，自然冷却至室温，用研钵研磨10分钟，得到预烧粉。
3、向预烧粉中加入质量分数为5％的聚乙烯醇水溶液，聚乙烯醇水溶液的加入量为预烧粉质量的50％，造粒，过120目筛，制成球状粉粒，将球状粉粒放入直径为15mm的不锈钢模具内，用粉末压片机在300MPa的压力下将其压制成厚度为1.5mm的圆柱状坯件；将圆柱状坯件放在氧化锆平板上，将氧化锆平板置于氧化铝密闭匣钵中，先升温至500℃，保温2小时排胶，冷却至室温；然后以10℃/分钟的升温速率升温至1000℃，再以3℃/分钟的升温速率升温至1320℃，烧结4小时，随炉自然冷却至室温，得到Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料。
实施例2
本实施例的步骤1中，按照Sr1.90Ca0.15Na0.81Eu0.03Nb5O15的化学计量分别称取纯度为99.80％的Na2CO3 0.8506g、纯度为99.00％的SrCO3 5.6028g、纯度为99.99％的Nb2O513.1423g、纯度为99.00％的CaCO3 0.2999g、纯度为99.99％的Eu2O3 0.1044g，其他步骤与实施例1相同，得到Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料。
实施例3
本实施例的步骤1中，按照Sr1.90Ca0.15Na0.75Eu0.05Nb5O15的化学计量分别称取纯度为99.80％的Na2CO3 0.7873g、纯度为99.00％的SrCO3 5.6010g、纯度为99.99％的Nb2O513.1380g、纯度为99.00％的CaCO3 0.2998g、纯度为99.99％的Eu2O3 0.1739g，其他步骤与实施例1相同，得到Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料。
实施例4
本实施例的步骤1中，按照Sr1.90Ca0.15Na0.72Eu0.06Nb5O15的化学计量分别称取纯度为99.80％的Na2CO3 0.7557g、纯度为99.00％的SrCO3 5.6001g、纯度为99.99％的Nb2O513.1358g、纯度为99.00％的CaCO3 0.2997g、纯度为99.99％的Eu2O3 0.2087g，其他步骤与实施例1相同，得到Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料。
对比例1
按照Sr1.90Ca0.15Na0.90Nb5O15的化学计量分别称取纯度为99.80％的Na2CO30.9455g、纯度为99.00％的SrCO3 5.6056g、纯度为99.99％的Nb2O5 13.1488g、纯度为99.00％的CaCO3 0.3000g，其他步骤与实施例1相同，得到铌酸锶钙钠铁电陶瓷材料。
上述实施例1～4制备的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料以及对比例1制备的铌酸锶钙钠铁电陶瓷材料分别采用D/max-2200X型射线衍射仪(由日本理学公司生产)进行XRD测试、采用F-4600型荧光分光光度计进行荧光性能激发光谱和发射光谱测试，结果见图1和图2。由图1可见，实施例1～4以及对比例1制备的陶瓷材料均为纯的四方钨青铜相。由图2可见，实施例1～4制备的陶瓷材料在395nm的紫外光激发下能够在617nm处具有较强的红光发射。
将上述实施例1～4制备的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料以及对比例1制备的铌酸锶钙钠铁电陶瓷材料表面依次用320目、800目、1500目的砂纸抛光至0.5～0.6mm厚，然后在陶瓷上下表面涂覆厚度为0.02mm的银浆，置于电阻炉中840℃保温30分钟。采用HIOKI3532-50和Agilient4980A型精密阻抗分析仪(由安捷伦科技有限公司生产)对烧银后的陶瓷材料进行介电铁电性能测试，结果见图3～10。由图3～10可见，对比例1中未掺杂Eu3+的陶瓷材料，其最大介电常数仅为1050、室温介电常数为1640、剩余极化强度为5.7μC/cm2，而本发明通过在铌酸锶钙钠铁电陶瓷材料中掺杂Eu3+，不但使陶瓷材料具有了发光性能，同时还显著提高了陶瓷材料的介电性能，实现了介电铁电和发光的耦合，进一步实现了多功能化集成材料，其中Eu3+的掺杂量为0.05时，陶瓷材料的电学性能最佳，其最大介电常数达到1270、居里温度为263℃、室温介电常数达到1700、剩余极化强度为6.6μC/cm2。

Claims (5)

1.一种高介电性能的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料，其特征在于：该陶瓷材料的通式为Sr1.90Ca0.15Na0.90-3xEuxNb5O15，其中x的取值为0.02～0.06，该陶瓷材料为钨青铜结构。
2.根据权利要求1所述的高介电性能的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料，其特征在于：所述x的取值为0.05。
3.一种权利要求1所述的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料的制备方法，其特征在于它由下述步骤组成：
(1)按照Sr1.90Ca0.15Na0.90-3xEuxNb5O15的化学计量比分别称取纯度为99.00％以上的Na2CO3、SrCO3、Nb2O5、CaCO3、Eu2O3，充分混合球磨16～24小时，在80～100℃下干燥12～24小时，得到原料混合物；
(2)将原料混合物在1180～1250℃下预烧5～8小时，得到预烧粉；
(3)将预烧粉经造粒、压片、排胶后，在1300～1380℃下烧结3～6小时，得到Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料。
4.根据权利要求3所述的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料的制备方法，其特征在于：在步骤(2)中，将原料混合物在1200℃下预烧6小时。
5.根据权利要求3所述的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料的制备方法，其特征在于：在步骤(3)中，将预烧粉经造粒、压片、排胶后，在1320℃下烧结4小时。
CN201710577430.3A 2017-07-14 2017-07-14 一种高介电性能的Eu3+掺杂铌酸锶钙钠发光铁电陶瓷材料及其制备方法 Active CN107188564B (zh)

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