CN114573338B - 一种高储能密度介电陶瓷的制备方法及应用 - Google Patents

一种高储能密度介电陶瓷的制备方法及应用 Download PDF

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CN114573338B
CN114573338B CN202210175161.9A CN202210175161A CN114573338B CN 114573338 B CN114573338 B CN 114573338B CN 202210175161 A CN202210175161 A CN 202210175161A CN 114573338 B CN114573338 B CN 114573338B
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CN114573338A (zh
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叶宝华
张海波
姜礼
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Dongguan Pulom Electronic Co ltd
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Abstract

本发明公开了一种高储能密度介电陶瓷的制备方法及应用，包括以下步骤：S1：将Na0.5Bi0.5TiO3、BiFeO3和Sr0.7Bi0.2TiO3以一定比例进行配制，然后加ZrO2球和无水乙醇进行球磨；S2：将S1中的料放置于样品盘中于干燥箱中进行烘干；S3：将S2中的干料压制成直径为2cm、高2cm的圆柱体形状，然后放入马弗炉中进行预烧，排除CO2；S4：将S3中排除CO2后的圆柱体样品捣碎成粉末状，然后进行二次球磨，细节如S1所示；S5：将S4中的粉料在干燥箱中以70℃温度进行烘干；S6：将S5中的干料中一定量的PVA混合均匀，然后过400目筛，留下均匀的颗粒状料。本发明提供了一种Sr0.7Bi0.2TiO3掺杂Na0.5Bi0.5TiO3‑BiFeO3陶瓷的制备方法及应用，属于介电陶瓷领域，提供了一种成本低、工艺简单、环境友好的制备方法。

Description

一种高储能密度介电陶瓷的制备方法及应用
技术领域
本发明涉及介电陶瓷材料技术领域，尤其涉及一种高储能密度介电陶瓷的制备方法及应用。
背景技术
介质电容器虽然储能密度相对较低，但其充放电速度快、工作温度高、安全、易小型化等优点使其在脉冲功率技术、雷达等领域得到广泛应用。然而，已经应用于脉冲功率技术的电容器受大部分都含有铅，对环境和人体健康造成危害。因此，研究无铅铁电陶瓷并提高其储能密度显得至关重要。在许多非线性介电材料中，弛豫铁电体和反铁电体是实现优异储能性能的最佳候选材料，但是反铁电体在高电场下会发生铁电-反铁电相变，造成使用寿命短，所以难以应用于实际。相比之下，弛豫铁电体具有较大的饱和极化、较小的剩余极化和较大的击穿强度(BDS)，容易获得出色的储能性能。
因此，该发明专利研究了具有A位点缺陷的化合物Sr0.7Bi0.2TiO3掺杂Na0.5Bi0.5TiO3-BiFeO3陶瓷，并获得了高储能密度。
发明内容
为了弥补现有技术的缺点与不足，本发明的目的之一在于Sr0.7Bi0.2TiO3成功固溶于Na0.5Bi0.5TiO3-BiFeO3；目的之二在于提供一种成本低、工艺简单、环境友好的制备方法；目的之三在于提供一种在高场下可以获取高储能密度的介电陶瓷。
为了实现上述目的，本发明采用了如下技术方案：
一种高储能密度介电陶瓷的制备方法及应用，包括以下步骤：
S1：将Na0.5Bi0.5TiO3、BiFeO3和Sr0.7Bi0.2TiO3以一定比例进行配制，然后加ZrO2球和无水乙醇进行球磨；
S2：将S1中的料放置于样品盘中于干燥箱中进行烘干；
S3：将S2中的干料压制成直径为2cm、高2cm的圆柱体形状，然后放入马弗炉中进行预烧，排除CO2；
S4：将S3中排除CO2后的圆柱体样品捣碎成粉末状，然后进行二次球磨，细节如S1所示；
S5：将S4中的粉料在干燥箱中以70℃温度进行烘干；
S6：将S5中的干料中一定量的PVA混合均匀，然后过400目筛，留下均匀的颗粒状料；
S7：将S6中所得粒料成直径为10mm、厚度为1mm的生片，然后置于马弗炉中排尽生片中的胶量，最后随炉冷却至室温；
S8：将S7中样品进行烧结，最后随炉冷却至室温后得到成品。
优选的，所述S1中，Na0.5Bi0.5TiO3、BiFeO3和Sr0.7Bi0.2TiO3配制比例为147：3：100；料、无水乙醇、球之比为1：2：1；球磨时间为30小时。
优选的，所述S2中，干燥条件为70℃。
优选的，所述S3中，圆柱体样品预烧温度为850℃，升温速率为4℃/min，保温时间为2小时。
优选的，所述S4和S5中，料、无水乙醇、球之比为1：2：1；球磨时间为30小时，干燥温度为70℃。
优选的，所述S6中，PVA是由聚乙烯醇和去离子水以8：100的质量比混合均匀，每20g粉料加入约60滴PVA混合均匀后过400目筛留下下层样品。
优选的，所述S7中，压制生片使用8MPa压力，排胶温度为600℃，升温速率为4℃/min，保温2小时。
优选的，所述S7中样品烧结温度为1120℃，升温速率为4℃/min，保温2小时。
优选的，制备的Sr0.7Bi0.2TiO3掺杂Na0.5Bi0.5TiO3-BiFeO3陶瓷。
优选的，Sr0.7Bi0.2TiO3掺杂Na0.5Bi0.5TiO3-BiFeO3陶瓷应用于脉冲、雷达领域。
与现有技术相比，本发明提供了一种高储能密度介电陶瓷的制备方法及应用，具备以下有益效果：
本发明提供了一种Sr0.7Bi0.2TiO3掺杂Na0.5Bi0.5TiO3-BiFeO3陶瓷的制备方法及应用，属于介电陶瓷领域，提供了一种成本低、工艺简单、环境友好的制备方法，本发明提供的Sr0.7Bi0.2TiO3掺杂Na0.5Bi0.5TiO3-BiFeO3陶瓷在室温下呈现为三方相结构，掺杂后样品具有致密的微观结构，并且样品的介电温谱图在室温下出现频率扩散现象，转变为弛豫铁电体。此外，掺杂Sr0.7Bi0.2TiO3后的样品饱和将储能密度从0.18J/cm3提升至1.69J/cm3。
附图说明
图1为实施例1(NBT-BFO)，实施例2(NBT-BFO-SBT)的X射线粉末衍射图(XRD)；
图2为实施例1和实施例2的扫描电子显微镜图(SEM)；
图3为实施例1和实施例2的介电温谱图；
图4为实施例1和实施例2的电滞回线图(P-E)，并且计算出其储能密度。
具体实施方式
以下通过特定的具体实例说明本发明的实施方式，本领域技术人员可由本说明书所揭露的内容轻易地了解本发明的其他优点与功效。本发明还可以通过另外不同的具体实施方式加以实施或应用，本说明书中的各项细节也可以基于不同观点与应用，在没有背离本发明的精神下进行各种修饰或改变。
实施例一
制备0.98Na0.5Bi0.5TiO3-0.02BiFeO3(NBT-BFO)
1)将NBT-BFO以49：1的比例进行配制，通过球磨、预烧、二次球磨、造粒压片、排胶烧结等步骤制备样品；
2)将步骤1)中的成品覆盖银电极，进行电学性能测试。
实施例中，对NBT-BFO进行X射线粉末衍射分析，如图1中所示，在室温下表现为三方相；对NBT-BFO进行扫描电子显微镜，样品致密无明显气孔如图2(a)所示；对NBT-BFO进行介电温谱测试，在室温下没有出现频率色散和弥散相变，其在室温下为铁电相，如图3(a)所示；对NBT-BFO进行电滞回线测试，如图4(a)所示，其电滞回线呈现方形，储能密度只有0.18J/cm3。
实施例二
制备0.6(0.98Na0.5Bi0.5TiO3-0.02BiFeO3)-Sr0.7Bi0.2TiO(NBT-BFO-SBT)
1)将NBT-BFO和SBT以3：2的比例进行配制，其主要制备过程与实施例1基本一致。
实施例中，对NBT-BFO-SBT进行X射线粉末衍射分析，如图1中所示，其在室温下表现为三方相；对NBT-BFO-SBT的扫描电子显微镜测试如图2(b)所示，表现为致密无气孔结构；对NBT-BFO-SBT的介电温谱测试中，发生明显的频率扩散和弥散相变，转变为弛豫铁电体，如图3(b)所示；对NBT-BFO-SBT测试电滞回线，如图4(b)所示，电滞回线变得瘦细，储能密度大有改善，其储能密度可以达到1.69J/cm3。
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。

Claims (8)

1.一种高储能密度介电陶瓷的制备方法，其特征在于，所述高储能密度介电陶瓷为Sr0.7Bi0.2TiO3掺杂Na0.5Bi0.5TiO3-BiFeO3陶瓷，所述陶瓷的制备方法包括以下步骤：
S1：将Na0.5Bi0.5TiO3、BiFeO3和Sr0.7Bi0.2TiO3以147：3：100的比例进行配制，然后按照料、无水乙醇、球之比为1：2：1的比例加入ZrO2球和无水乙醇进行球磨30h；
S2：将S1中的料放置于样品盘中于干燥箱中进行烘干；
S3：将S2中的干料压制成直径为2 cm、高2 cm的圆柱体形状，然后放入马弗炉中进行预烧，排除CO2；
S4：将S3中排除CO2后的圆柱体样品捣碎成粉末状，然后进行二次球磨，细节如S1所示；
S5：将S4中的粉料在干燥箱中以70 °C温度进行烘干；
S6：将S5中的干料中一定量的PVA混合均匀，然后过400目筛，留下均匀的颗粒状料；
S7：将S6中所得粒料成直径为10 mm、厚度为1 mm的生片，然后置于马弗炉中排尽生片中的胶量，最后随炉冷却至室温；
S8：将S7中样品在1120 ℃温度下进行烧结，且升温速率为4℃/min，保温2小时，最后随炉冷却至室温后得到成品。
2.根据权利要求1所述的一种高储能密度介电陶瓷的制备方法，其特征在于，所述S2中，干燥条件为70 ℃。
3.根据权利要求1所述的一种高储能密度介电陶瓷的制备方法，其特征在于，所述S3中，圆柱体样品预烧温度为850℃，升温速率为4℃/min，保温时间为2小时。
4.根据权利要求1所述的一种高储能密度介电陶瓷的制备方法，其特征在于，所述S4和S5中，料、无水乙醇、球之比为1：2：1；球磨时间为30小时，干燥温度为70℃。
5.根据权利要求1所述的一种高储能密度介电陶瓷的制备方法，其特征在于，所述S6中，PVA是由聚乙烯醇和去离子水以8：100的质量比混合均匀，每20 g粉料加入60滴PVA混合均匀后过400 目筛留下下层样品。
6.根据权利要求1所述的一种高储能密度介电陶瓷的制备方法，其特征在于，所述S7中，压制生片使用8 MPa压力，排胶温度为600 °C，升温速率为4 °C/min，保温 2 小时。
7.根据权利要求1所述的一种高储能密度介电陶瓷的制备方法，其特征在于，所述S7中样品烧结温度为1120 °C，升温速率为4 °C/min，保温 2 小时。
8.根据权利要求1-7任一项所述的一种高储能密度介电陶瓷的制备方法，其特征在于，所述Sr0.7Bi0.2TiO3掺杂Na0.5Bi0.5TiO3-BiFeO3陶瓷应用于脉冲、雷达领域。
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