CN114956815A - 一种新型高应变高居里温度铌酸钾钠基铁电陶瓷的制备方法 - Google Patents

一种新型高应变高居里温度铌酸钾钠基铁电陶瓷的制备方法 Download PDF

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CN114956815A
CN114956815A CN202210626526.5A CN202210626526A CN114956815A CN 114956815 A CN114956815 A CN 114956815A CN 202210626526 A CN202210626526 A CN 202210626526A CN 114956815 A CN114956815 A CN 114956815A
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李敏
李康微
彭文泺
李雪阳
陈建兵
杨小红
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Chizhou University
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Abstract

本发明涉及铌酸钾钠基铁电陶瓷领域。公开了一种新型高应变高居里温度铌酸钾钠基铁电陶瓷的开发。所述陶瓷具有正交‑四方(O‑T)两相共存晶体结构，化学组成为0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3‑0.03SrTiO3。本发明制备的铌酸钾钠基铁电陶瓷具有良好的应变性能，在外电场40kV/cm下，应变达到0.22％，居里温度为280℃，制备简单，成本低廉。

Description

一种新型高应变高居里温度铌酸钾钠基铁电陶瓷的制备方法
技术领域
本发明涉及新型高应变高居里温度铌酸钾钠基铁电陶瓷的开发技术领域，具体为一种新型高应变高居里温度铌酸钾钠基铁电陶瓷的制备方法。
背景技术
铌酸钾钠基无铅铁电陶瓷成为近些年来最具讨论性和研究性的铁电陶瓷体系之一，传统的陶瓷工艺难以获得致密性良好的陶瓷体。因此，研究者常用掺杂改性调控结构来优化其铁电性能。铌酸钾钠(K0.5Na1-xNbO3)基陶瓷的高应变值引起了人们的广泛研究关注。应变是铁电陶瓷在传感器和执行器应用中的一个关键特性。目前，K0.5Na1-xNbO3(KNN)基铁电陶瓷在室温附近的多态相变相界(简称PPB)，例如菱形-正方(R-T)和正交-四方(O-T) 相边界，在PPB上的易极化开关产生了一个较高的应变响应。通过添加掺杂剂，将菱形-正交相变温度(TR-O)或正交四方转变温度(TO-T移动到室温下，得到了具有不同相边界的KNN基铁电陶瓷。
KNN基铁电陶瓷目前主要是通过掺杂构建多相共存，改变晶粒、改变畴的大小、使畴壁易转向、提高陶瓷致密度等方法提高应变。相界的构造可以有效的提高铁电陶瓷的电学性能。另外构建相界降低极化各向异性能量，利于极化转向提高其应变性能。
根据铅基PZT材料通过调节Zr和Ti的比例，可以大幅提高材料的压电性能，当Zr的含量为52％，PZT处于一种三方-四方铁电相共存的状态。因此本发明调节组分0.97(K0.48Na0.52)La0.0075(ZrxNb1-x)O3-0.03SrTiO3陶瓷的B位，当 x＝0.0025时，陶瓷具有O-T相界，在40kV/cm电场下产生0.21％的高应变。
现有技术，KNN铁电陶瓷具有O-T两相共存时，在40kV/cm下，应变S％达到0.1-0.2％，居里温度在250℃左右，决定陶瓷低于250℃使用才具有应变性能。
发明内容
本发明的目的在于提供一种新型高应变高居里温度铌酸钾钠基铁电陶瓷的制备方法，以解决上述背景技术中提出的问题。
为实现上述目的，本发明提供如下技术方案：一种新型高应变高居里温度铌酸钾钠基铁电陶瓷的制备方法，制备方法包括以下步骤：
步骤一，原料预处理；
步骤二，原料混合；
步骤三，原料烘干；
步骤四，混合料过筛；
步骤五，混合料的煅烧；
步骤六，煅烧料的球磨；
步骤七，排胶；
步骤八，烧结；
步骤九，打磨；
步骤十，烧银；
步骤十一，冷却；
步骤十二，得到制备化学式为 0.97(K0.48Na0.52)La0.0075(ZrxNb1-x)O3-0.03SrTiO3铁电陶瓷；
步骤十三，对0.97(K0.48Na0.52)La0.0075(ZrxNb1-x)O3-0.03SrTiO3铁电陶瓷结构和性能测试。
优选的，所述陶瓷化学组成为 0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3。
优选的，所述陶瓷化学组最大特点在于加入ZrO2、La2O3、SrTiO3三种物料共同配合，构建了正交-四方两相共存的结构，即(O-T)相界。
优选的，所述烧银后得到陶瓷，在外电场E为40kV/cm下，应变为0.22％，且居里温度高达280℃。
优选的，所述步骤十三，当x＝0.0025时，得出陶瓷物相：经XRD测试，陶瓷具有O-T两相共存结构，居里温度280℃；微观形貌：经微观形貌SEM 测试，平均晶粒尺寸在0.34μm；利用密度仪，测试密度为4.28g/cm3；铁电性：最大极化强度Pmax为17.08μC/cm2；应变性能：当E＝40kV/cm下，应变S％达到0.22％。
与现有技术相比，本发明的有益效果是：
本发明技术特点，KNN基铁电陶瓷具有O-T两相共存时，在40kV/cm 下，应变S％达到0.22％，一般应变性能高于0.1％就可以用于设备中。其居里温度高达280℃，决定陶瓷低于280℃使用具有应变性能，本发明制备的铌酸钾钠基压电陶瓷具有良好的应变性能，制备简单，成本低廉。
附图说明
图1为本发明的图1 0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3铁电陶瓷的微观形貌图.(a)SEM图；(b)粒径分布图；
图2为本发明的0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3铁电陶瓷的XRD图；
图3为本发明的0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3铁电陶瓷的介温谱图；
图4为本发明的0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3铁电陶瓷的测试.(a)P-E曲线，(b)S-E曲线
图5为本发明的工艺流程图。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
在本发明的描述中，需要说明的是，术语“上”、“下”、“内”、“外”“前端”、“后端”、“两端”、“一端”、“另一端”等指示的方位或位置关系为基于附图所示的方位或位置关系，仅是为了便于描述本发明和简化描述，而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为对本发明的限制。此外，术语“第一”、“第二”仅用于描述目的，而不能理解为指示或暗示相对重要性。
在本发明的描述中，需要说明的是，除非另有明确的规定和限定，术语“安装”、“设置有”、“连接”等，应做广义理解，例如“连接”，可以是固定连接，也可以是可拆卸连接，或一体的连接；可以是机械连接，也可以是电连接；可以是直接相连，也可以通过中间媒介间接相连，可以是两个元件内部的连通。对于本领域的普通技术人员而言，可以具体情况理解上述术语在本发明中的具体含义。
请参阅图1、图2、图3、图4和图5，本发明提供的一种实施例：一种新型高应变高居里温度铌酸钾钠基铁电陶瓷的制备方法，
实施例一，制备方法包括以下步骤：
步骤一，原料预处理；
步骤二，原料混合；
步骤三，原料烘干；
步骤四，混合料过筛；
步骤五，混合料的煅烧；
步骤六，煅烧料的球磨；
步骤七，排胶；
步骤八，烧结；
步骤九，打磨；
步骤十，烧银；
步骤十一，冷却；
步骤十二，得到制备化学式为 0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3铁电陶瓷；
步骤十三，对0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3铁电陶瓷结构和性能测试。
所述陶瓷化学组成为0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3
所述陶瓷化学组最大特点在于加入ZrO2、La2O3、SrTiO3三种物料共同配合，构建了正交-四方两相共存的结构，即(O-T)相界。
所述烧银后得到陶瓷，通过加工使其致密化，在外电场E为40kV/cm下，应变为0.21％，且居里温度高达280℃。
所述步骤十三，得出陶瓷物相：经XRD测试，陶瓷具有O-T两相共存结构，居里温度280℃；微观形貌：经微观形貌SEM测试，平均晶粒尺寸在0.34 μm；利用密度仪，测试密度为4.28g/cm3；铁电性：最大极化强度Pmax为17.08 μC/cm2；应变性能：当E＝40kV/cm下，应变S％达到0.21％。
实施例二，制备方法包括以下步骤：
步骤一，原料预处理；
步骤二，原料混合；
步骤三，原料烘干；
步骤四，混合料过筛；
步骤五，混合料的煅烧；
步骤六，煅烧料的球磨；
步骤七，排胶；
步骤八，烧结；
步骤九，打磨；
步骤十，烧银；
步骤十一，冷却；
步骤十二，得到制备化学式为 0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3铁电陶瓷；
步骤十三，对0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3铁电陶瓷结构和性能测试。
所述陶瓷化学组成为0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3。
所述陶瓷化学组最大特点在于加入ZrO2、La2O3、SrTiO3三种物料共同配合，构建了正交-四方两相共存的结构，即(O-T)相界。
所述烧银后得到陶瓷，通过加工使其致密化，在外电场E为40kV/cm下，应变为0.22％，且居里温度高达280℃。
所述步骤十三，当x＝0.0025时， 0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3铁电陶瓷结构和性能测试如下，
陶瓷物相：经XRD测试，陶瓷具有O-T两相共存结构，居里温度280℃。
微观形貌：经微观形貌SEM测试，平均晶粒尺寸在0.34μm。
利用密度仪，测试密度为4.28g/cm3
铁电性：最大极化强度Pmax为17.08μC/cm2
应变性能：当E＝40kV/cm下，应变S％达到0.21％。
实施例三，制备方法包括以下步骤：
步骤一，原料粉碎；
步骤二，原料混合；
步骤三，原料烘干；
步骤四，混合料过筛；
步骤五，混合料的煅烧；
步骤六，煅烧料球磨；
步骤七，排胶；
步骤八，烧结；
步骤九，烧结；
步骤十，打磨；
步骤十一，烧银；
这种铁电陶瓷，组分为 0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3，具有高的致密性和合适的晶粒尺寸，以及具有正交-四方两相共存的晶体结构，这种结构的压电陶瓷内部极化偶极子易转动，增加极化进而提高压电陶瓷在外电场下的应变性能。
具体证明如下图。
图1是陶瓷微观形貌图，图1(a)表明晶粒尺寸排布紧密，气孔少，陶瓷很致密；通过统计粒径尺寸如图1(b)，平均粒径为0.34μm；
图2是XRD测试，图2表明陶瓷具有钙钛矿结构，图中右上角小图是衍射角44-470放大图，(002)与(200)峰高接近，表明是陶瓷是正交-四方两相共存；
进一步通过介温谱分析图3，表明陶瓷在室温附近处于正交-四方相变处，就是说明陶瓷具有正交-四方两相共存的晶相；具有居里温度TC约280℃，是四方-立方相变温度；
图4(a)是陶瓷的电滞回线(P-E曲线)，表明陶瓷具有铁电性，铁电性的大小可用最大极化强度Pmax来表示，Pmax达到17.08μC/cm2；图4(b)是陶瓷的电致应变回线(S-E曲线)，表明陶瓷在电场(E)在40kV/cm下，应变量S％等于0.22％。
对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。不应将权利要求中的任何附图标记视为限制所涉及的权利要求。

Claims (5)

1.一种新型高应变高居里温度铌酸钾钠基铁电陶瓷的制备方法，其特征在于，制备方法包括以下步骤：
步骤一，原料预处理；
步骤二，原料混合；
步骤三，原料烘干；
步骤四，混合料过筛；
步骤五，混合料的煅烧；
步骤六，煅烧料的球磨；
步骤七，排胶；
步骤八，烧结；
步骤九，打磨；
步骤十，烧银；
步骤十一，冷却；
步骤十二，得到制备化学式为0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3铁电陶瓷；
步骤十三，对0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3铁电陶瓷结构和性能测试。
2.根据权利要求1所述的一种新型高应变高居里温度铌酸钾钠基铁电陶瓷的制备方法，其特征在于：所述陶瓷化学组成为0.97(K0.48Na0.52)La0.0075(Zr0.0025Nb0.9975)O3-0.03SrTiO3。
3.根据权利要求1所述的一种新型高应变高居里温度铌酸钾钠基铁电陶瓷的制备方法，其特征在于：所述陶瓷化学组最大特点在于加入ZrO2、La2O3、SrTiO3三种物料共同配合，构建了正交-四方两相共存的结构，即(O-T)相界。
4.根据权利要求1所述的一种新型高应变高居里温度铌酸钾钠基铁电陶瓷的制备方法，其特征在于：所述烧银后得到陶瓷，在外电场E为40kV/cm下，应变为0.22％，且居里温度高达280℃。
5.根据权利要求1所述的一种新型高应变高居里温度铌酸钾钠基铁电陶瓷的制备方法，其特征在于：所述步骤十三，当x＝0.0025时，得出陶瓷物相：经XRD测试，陶瓷具有O-T两相共存结构，居里温度280℃；微观形貌：经微观形貌SEM测试，平均晶粒尺寸在0.34μm；利用密度仪，测试密度为4.28g/cm3；铁电性：最大极化强度Pmax为17.08μC/cm2；应变性能：当E＝40kV/cm下，应变S％达到0.22％。
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