CN112811902B - 一种高储能密度的钛酸铋钾基三元无铅铁电陶瓷材料及其制备 - Google Patents

一种高储能密度的钛酸铋钾基三元无铅铁电陶瓷材料及其制备 Download PDF

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CN112811902B
CN112811902B CN202110031606.1A CN202110031606A CN112811902B CN 112811902 B CN112811902 B CN 112811902B CN 202110031606 A CN202110031606 A CN 202110031606A CN 112811902 B CN112811902 B CN 112811902B
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朱满康
杨倩
位秋梅
张蔓琳
郑木鹏
侯育冬
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Abstract

一种高储能密度的钛酸铋钾基三元无铅铁电陶瓷材料及其制备，属于功能陶瓷材料技术领域。其化学通式为(1‑x‑y)Bi0.5K0.5TiO3‑xBiFeO3‑yNaTaO3，其中0.21≤x≤0.24，0.00<y≤0.08。采用传统固相法制备的三元无铅铁电陶瓷在150kV/cm的电场下，有效储能密度达到了2.88J/cm3，且具有优异的温度稳定性，可以满足储能电容器对材料的要求。

Description

一种高储能密度的钛酸铋钾基三元无铅铁电陶瓷材料及其 制备
技术领域
本发明涉及一种高储能密度无铅铁电陶瓷材料，属于功能陶瓷材料技术领域。
背景技术
储能介电电容以其超高功率密度、高温稳定性和超快充放电能力，广泛应用于电动汽车、高频逆变器、电磁脉冲发生器等脉冲电力***。然而，由于它们与超级电容器和电池相比的储能密度较低，介电电容器往往需要较大的体积和重量才能提供足够的功率，这不符合有关脉冲功率器件的重量和集成的要求。因此，迫切需要开发具有高可回收储能密度Wr的介电电容材料。通常，介电陶瓷的总储能密度W和有效储能密度Wr可以分别由方程
Figure BDA0002892483130000011
和
Figure BDA0002892483130000012
来计算，效率η则可以由方程η＝Wr/W来计算，其中W、Pr、Pm、和E分别是总储能密度、剩余极化强度、最大极化强度和外加电场。从这些方程出发，具有高Wr的介电电容材料期望其具有高Pm、低Pr以及高的外加电场。钙钛矿氧化物是最有前途的材料之一，它们的P-E电滞回线的形状可以通过形成固溶体来调整，以提高它们的储能性能。
近年来，为了探索无铅储能电容器的候选材料，对Bi0.5Na0.5TiO3(BNT)、K0.5Na0.5NbO3(KNN)、BiFeO3(BF)、AgNbO3(AN)、SrTiO3(ST)、BaTiO3(BT)等无铅钙钛矿氧化物进行了广泛的研究。而K0.5Bi0.5TiO3(KBT)因其高极化特性和强弛豫特性引起了我们的兴趣。根据第一原理计算，KBT具有较高的自发极化(Ps＝52μC/cm2)，这是实现高储能密度的必要条件。此外，KBT的固有弛豫特性使其可具有较低的Pr，有利于获得较高的η。李峰等采用热压烧结工艺制备了La(Mg0.5Ti0.5)O3和Ba(Mg1/3Nb2/3)O3改性Bi0.5K0.5TiO3基陶瓷，在180kV/cm和230kV/cm的电场下分别获得了2.08J/cm3和3.14J/cm3的Wr值，同时也具有优异的温度稳定性。这些结果表明，KBT陶瓷具有在较宽的温度范围内获得高储能性能的潜力。目前，KBT陶瓷作为储能应用主要存在两个方面的不足，一是纯KBT的晶粒尺寸小，只有300nm左右，畴的钉扎作用太强，难以在较低的电场下获得高的自发极化；二是常规烧结工艺中K和Bi容易挥发，难以获得致密的结构，击穿场强较低，难于满足介电储能的需要。而采用特殊的烧结工艺，如热压，由于其还原气氛使陶瓷必须在氧环境进行进一步的热处理，增加了工艺的复杂和可控性。
因此，本发明设计在KBT中加入钙钛矿铁电体BF，可使KBT陶瓷的晶粒尺寸增加，改善烧结性能的同时实现较高的自发极化，从而可以采用常规无压烧结工艺。同时，BF含量为25mol.％左右的KBT-BF二元体系可形成多相边界MPB，使体系具有多相共存现象。进而，通过引入先兆性铁电体NaTaO3(NT)，降低其电滞现象，减小剩余极化强度，并提高其击穿强度。特别是，NaTaO3(NT)的引入可以破坏KBT中铁电相的稳定性，并将介电最大值温度向低温移动，从而有利于获得良好的温度稳定性。其原因在于，Na+和Ta5+与KBT-BF的相应位置上的电荷和离子半径不同，会带来电荷不均匀性和局部随机场，从而增强了弛豫行为，获得高的储能密度。同时，NT的引入可以拓宽驰豫相弥散相变温度范围，使KBT基陶瓷的储能行为表现出良好的温度稳定性。
发明内容
本发明的目的是采用传统固相氧化物烧结法获得一种具有高储能密度的新型基无铅铁电陶瓷材料。为此，本发明采用的方法是在MPB附近的K0.5Bi0.5TiO3-BiFeO3二元体系中引入先兆性铁电体NaTaO3，形成化学计量比为(1-x-y)Bi0.5K0.5TiO3-xBiFeO3-yNaTaO3的三元无铅铁电陶瓷，0.21≤x≤0.24，0<y≤0.08，从而获得高的储能密度。
本发明制备的(1-x-y)Bi0.5K0.5TiO3-xBiFeO3-yNaTaO3[0.21≤x≤0.24，0<y≤0.08]陶瓷的步骤如下。首先根据化学化学计量比称量原料，将原料在乙醇中球磨以使原料充分混合均匀，将混合均匀的原料烘干后装入氧化铝坩埚内，在空气中800-890℃煅烧4h。最后将压制成型的坯体埋入KBT煅烧粉末中，在空气气氛中在1030-1070℃下烧结10h，得到致密的陶瓷。
本发明得到的(1-x-y)Bi0.5K0.5TiO3-xBiFeO3-yNaTaO3[0.21≤x≤0.24，0<y≤0.08]三元无铅铁电陶瓷，由于NT的加入削弱了长程铁电相形成了遍历弛豫相,在较低的电场(150kV/cm)下，获得了高达2.88J/cm3的Wr值，并且具有良好的温度稳定性(如20-160℃的温度范围内具有很好地稳定性)，实现了与热压烧结的KBT基陶瓷可比拟的储能性能。
附图简述
关于本发明的示例性实施方案的详述，表现在参考附图，其中：
图1为本发明组成为0.73Bi0.5K0.5TiO3-0.23BiFeO3-0.04NaTaO3陶瓷的XRD图，表明该陶瓷具有纯钙钛矿结构，并表现出赝立方结构特征。
图2为本发明组成为0.73Bi0.5K0.5TiO3-0.23BiFeO3-0.04NaTaO3陶瓷在10-150kV/cm的外加电场下的单极电致回线图。
图3为本发明组成为0.73Bi0.5K0.5TiO3-0.23BiFeO3-0.04NaTaO3陶瓷在10-150kV/cm的外加电场下的储能性能图。
图4为本发明组成为0.73Bi0.5K0.5TiO3-0.23BiFeO3-0.04NaTaO3陶瓷在20-160℃的范围内90kV/cm外加电场下的储能性能图。
符号和术语
在下列说明书和权利要求书各处使用某些术语。
术语“极化滞后”是指表现出代表由于无铅铁电陶瓷材料的非线性极化产生的电场上升和下降时极化强度不一致的现象。
术语“多相边界”是指在温度-成分相图上，在特定的成分范围和温度区间内出现多相结构共存的现象，该成分称之为多相边界。
术语“大约”在表示数值或范围时意在包括由于进行测量时发生的实验误差造成的更大或更小的值。这样的测量偏差通常在所列数值的±10％内。
无铅铁电材料中组成的相对量或比例以摩尔分数或摩尔％(mol.％)表示，例如，x≤0.06，x＝0.08或0.73Bi0.5K0.5TiO3-0.23BiFeO3-0.04NaTaO3。
温度、比例等其他数值数据可以以范围格式呈现。这样的范围格式仅为方便和简明使用，并且应灵活解释不仅包括作为该范围的明确列举的数值，还包括该范围内包含的所有独立数值或子范围。例如，20-160℃的温度范围内应被解释为不仅包括明确列举的数值20℃和160℃，还包括每一中间温度，如40℃、60℃、80℃、100℃、120℃、140℃和所有的子范围，如60-120℃,等等。
具体实施方式
下面结合实施例进一步说明本发明，但本发明并不限于以下实施例。
本发明的实施例是一种高储能密度的KBT-BF基无铅铁电陶瓷，通式为(1-x-y)Bi0.5K0.5TiO3-xBiFeO3-yNaTaO3，其中x代表BiFeO3的摩尔百分比，0.18≤x≤0.26，y代表NaTaO3的摩尔百分比，0.02≤y≤0.08。各组分以K2CO3(99.95％),Na2CO3(99.95％),Bi2O3(99.95％),TiO2(99.95％),Fe2O3(99.95％),Ta2O5(99.98％)为原料进行配料。本发明制备陶瓷是采用常规的氧化物陶瓷制备工艺，首先根据化学化学计量比称量原料，将原料在乙醇中球磨以使原料充分混合均匀，将混合均匀的原料烘干后装入氧化铝坩埚内，在空气中800-890℃煅烧4h。最后将压制成型的坯体埋入KBT煅烧粉末中，在空气气氛中在1030-1070℃下烧结10h，得到致密的陶瓷。
本发明各实施例的(1-x-y)Bi0.5K0.5TiO3-xBiFeO3-yNaTaO3陶瓷的配方和、煅烧及烧结工艺参数如表1所示。
表1本发明各实施例陶瓷的配方和烧结参数
Figure BDA0002892483130000051
对实施例2中的陶瓷样品进行X射线测试，所得XRD图显示在附图1中，表明该实施例具有纯的钙钛矿结构，没有第二相的痕迹。
附图2和附图3是本实施例2的陶瓷样品的电滞回线测量结果和所计算的储能性能。可以看到，随着电场的增加，最大极化强度呈线性增加，储能密度不断提高，最终在150kV/cm的工作电场下，有效储能密度达到2.88J/cm3。
附图4表示了本实施例2的陶瓷样品在20-160℃的温度范围内的储能性能，可以看到，该实施例具有良好的温度稳定性，有效储能密度的变化率低于12％，储能效率的变化率低于5％。
对比例及实施例性能表：
Figure BDA0002892483130000052
Figure BDA0002892483130000061

Claims (4)

1.一种高储能密度的钛酸铋钾基三元无铅铁电陶瓷材料，其特征在于，其组成为K0.5Bi0.5TiO3-BiFeO3-NaTaO3固溶体；其化学通式为(1-x-y)Bi0.5K0.5TiO3-xBiFeO3-yNaTaO3，其中0.21≤x≤0.24，0.00＜y≤0.08。
2.按照权利要求1所述的一种高储能密度的钛酸铋钾基三元无铅铁电陶瓷材料，其特征在于，所述陶瓷材料具有稳定钙钛矿结构。
3.按照权利要求1所述的一种高储能密度的钛酸铋钾基三元无铅铁电陶瓷材料，其特征在于，制备方法，包括以下步骤：首先根据化学计量比称量原料，将原料在乙醇中球磨以使原料充分混合均匀，将混合均匀的原料烘干后装入氧化铝坩埚内，在空气中800-890℃煅烧4h，最后将压制成型的坯体埋入KBT煅烧粉末中，在空气气氛中在1030-1070℃下烧结10h，得到致密的陶瓷。
4.按照权利要求1所述的一种高储能密度的钛酸铋钾基三元无铅铁电陶瓷材料，其特征在于，20-160℃的温度范围内储能稳定。
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