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CN114874009B - 一种近室温弛豫铁电材料Ba4SrBiTi3Nb7O30及其制备方法和应用 - Google Patents

一种近室温弛豫铁电材料Ba4SrBiTi3Nb7O30及其制备方法和应用 Download PDF

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CN114874009B
CN114874009B CN202210647586.5A CN202210647586A CN114874009B CN 114874009 B CN114874009 B CN 114874009B CN 202210647586 A CN202210647586 A CN 202210647586A CN 114874009 B CN114874009 B CN 114874009B
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苏玉玲
左寓英
龚高尚
周进
段亚然
王永强
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Zhengzhou University of Light Industry
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Abstract

本发明属于弛豫性铁电材料技术领域，具体涉及一种近室温弛豫铁电材料Ba4SrBiTi3Nb7O30及其制备方法和应用。本发明克服了现有技术铅基铁电材料中存在的铅毒性问题，也克服了现有技术低温弛豫铁电材料较低的应用温度缺陷，提供了一种无铅的Ba4SrBiTi3Nb7O30铁电材料，且制得的Ba4SrBiTi3Nb7O30材料近室温表现出明显的弛豫性铁电特征，制得的Ba4SrBiTi3Nb7O30材料能够被应用于制备计算机存储元件、微位移器、传感器、储能器中。

Description

一种近室温弛豫铁电材料Ba4SrBiTi3Nb7O30及其制备方法和 应用
技术领域
本发明属于弛豫性铁电材料技术领域，具体涉及一种近室温弛豫铁电材料Ba4SrBiTi3Nb7O30及其制备方法和应用。
背景技术
在铁电体中，有一类称之为弛豫铁电体，该类材料由于介电常数高、电致伸缩效应大，从而在微定位器、致动器及机敏结构等领域有着广阔的应用前景；另外，弛豫性铁电材料优异的热释电性能使其应用于红外探测器等方面，而其压电性能使该材料能够应用于高频声纳设备中，作为接收换能器使用。这类材料本身的介电性也在大容量电容、可调谐微波器件、热敏元件等方面有着广泛应用。
但是目前具有弛豫性铁电特征的材料要么为铅基单晶或陶瓷，要么弛豫性铁电相变温度低；铅基材料中铅的毒性对环境和人类带来极大危害并威胁人类健康，低温弛豫铁电材料较低的应用温度又限制了其室温下的应用，因此寻找新型无铅、近室温弛豫性铁电材料具有重要意义。
发明内容
针对上述现有技术存在的不足，本发明提供了一种近室温弛豫铁电材料Ba4SrBiTi3Nb7O30及其制备方法和应用；本发明提供了一种无铅的Ba4SrBiTi3Nb7O30铁电材料，且制得的Ba4SrBiTi3Nb7O30材料近室温表现出明显的弛豫性铁电特征。
为实现上述目的，本发明的技术方案如下：
一种近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的制备方法，包括如下步骤：
(1)按照化学式Ba4SrBiTi3Nb7O30称取原料BaCO3、SrCO3、Bi2O3、TiO2和Nb2O5，将各原料共同研磨，直至原料均匀混合，得到混合物；
其中，BaCO3、SrCO3、Bi2O3、TiO2和Nb2O5的化学计量之比为8:2:1:3:7；
(2)将步骤(1)的混合物先预烧，冷却至室温，得到一段烧结物；再研磨至无颗粒感的粉体，得到坯料；然后将坯料进行烧结，冷却至室温，得到近室温弛豫铁电材料Ba4SrBiTi3Nb7O30。
优选的，所述步骤(1)的研磨时间为6-10h，所述步骤(2)的研磨时间为2-4h。
优选的，所述步骤(2)中预烧的条件为：将步骤(1)的混合物在 1000-1200℃下预烧3-7h后，冷却至室温，得到一段烧结物。
优选的，所述步骤(2)中烧结的条件为：将坯料在1250-1350℃下烧结 4-6h后，冷却至室温，得到近室温弛豫铁电材料Ba4SrBiTi3Nb7O30。
优选的，所述步骤(2)中，将坯料在1300℃下烧结5h。
本发明还保护了制备方法制得的近室温弛豫铁电材料Ba4SrBiTi3Nb7O30，所述近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的结晶为钨青铜结构，在250K近室温表现出弛豫铁电特性。
本发明还保护了近室温弛豫铁电材料Ba4SrBiTi3Nb7O30在制备计算机存储元件、微位移器、传感器、储能器中的应用。
与现有技术相比，本发明的有益效果：
1、现有技术中尚无技术制备出Ba4SrBiTi3Nb7O30材料弛豫铁电材料，而其他目前应用的弛豫铁电材料含有铅元素，铅有毒对人体和环境带来极大危害。
2、本发明所制备的新型近室温弛豫铁电材料Ba4SrBiTi3Nb7O30，结晶为钨青铜结构，250K展现弛豫铁电特性，因此成功制备出了一种相变温度接近室温的弛豫性铁电材料；此外本发明的制备工艺简单，成本低，可实现大批量制备生产。
3、实验结果表明，本发明的近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的制备中，BaCO3、SrCO3、Bi2O3、TiO2、Nb2O5的化学计量比必须为8:2:1:3:7，原料必须为BaCO3、SrCO3、Bi2O3、TiO2和Nb2O5，否则无法制得结构与性能相同或相近的近室温弛豫铁电材料。
附图说明
图1为本发明实施例1制得的近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的 XRD图谱；
图2为本发明实施例1制得的近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的(a) 图为Ba4SrBiTi3Nb7O30的介电常数-温度图，(b)图为Ba4SrBiTi3Nb7O30的介电损耗-温度图；
图3为本发明实施例1制得的近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的铁电极化图。
具体实施方式
下面对本发明的具体实施方式进行详细描述，但应当理解本发明的保护范围并不受具体实施方式的限制。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的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。本发明各实施例中所述实验方法，如无特殊说明，均为常规方法。
下述实验方法和检测方法，如没有特殊说明，均为常规方法；下述试剂和原料，如没有特殊说明，均为市售。
实施例1
一种近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的制备方法，包括以下步骤：
(1)按照计量比为8:2:1:3:7称量BaCO3、SrCO3、Bi2O3、TiO2、Nb2O5；
(2)将步骤(1)中的各原料置于玛瑙研钵共同研磨8h，直至原料均匀混合，得到混合物；
(3)将步骤(2)的混合物放入Al2O3材质坩埚并置于马弗炉内，以 5℃/min升温速率升温至1100℃，保温5h，冷却至室温，得到一段烧结物；
(4)将步骤(3)的一段烧结物继续研磨4h，至无颗粒感的粉体，得到坯料；
(5)将步骤(4)的坯料以3℃/min速率升温至1300℃，保温5h，然后以1℃/min的速率冷却至室温，得到Ba4SrBiTi3Nb7O30近室温弛豫铁电材料。
实施例2
一种近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的制备方法，包括以下步骤：
(1)按照计量比为8:2:1:3:7称量BaCO3、SrCO3、Bi2O3、TiO2、Nb2O5；
(2)将步骤(1)中的各原料置于玛瑙研钵共同研磨10h，直至原料均匀混合，得到混合物；
(3)将步骤(2)的混合物放入Al2O3材质坩埚并置于马弗炉内，以5℃/min 升温速率升温至1100℃，保温7h，冷却至室温，得到一段烧结物；
(4)步骤(3)的一段烧结物继续研磨2h，至无颗粒感的粉体，得到坯料；
(5)将步骤(4)的坯料以3℃/min速率升温至1250℃，保温5h，然后自然降温至室温，得到近室温弛豫铁电材料Ba4SrBiTi3Nb7O30。
实施例3
一种近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的制备方法，包括以下步骤：
(1)按照计量比为8:2:1:3:7称量BaCO3、SrCO3、Bi2O3、TiO2、Nb2O5；
(2)将步骤(1)中的各原料置于玛瑙研钵共同研磨6h，直至原料均匀混合，得到混合物；
(3)将步骤(2)的混合物放入Al2O3材质坩埚并置于马弗炉内，以5℃/min 升温速率升温至1100℃，保温5h，冷却至室温，得到一段烧结物；
(4)将步骤(3)的一段烧结物继续研磨4h，至无颗粒感的粉体，得到坯料；
(5)将步骤(4)的坯料以3℃/min速率升温至1350℃，保温5h，然后以5℃/min速率冷却至室温，得到近室温弛豫铁电材料Ba4SrBiTi3Nb7O30。
实施例4
近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的制备方法，包括以下步骤：
(1)按照计量比为8:2:1:3:7称量BaCO3、SrCO3、Bi2O3、TiO2、Nb2O5；
(2)将步骤(1)中的各原料置于玛瑙研钵共同研磨8h，直至原料均匀混合，得到混合物；
(3)将步骤(2)的混合物放入Al2O3材质坩埚并置于马弗炉内，以5℃/min 升温速率升温至1100℃，保温5h，冷却至室温，得到一段烧结物；
(4)将步骤(3)的一段烧结物继续研磨4h，至无颗粒感的粉体，得到坯料；
(5)将步骤(4)的坯料以3℃/min速率升温至1320℃，保温5h，然后以1℃/min速率冷却至室温，得到近室温弛豫铁电材料Ba4SrBiTi3Nb7O30。
实施例5
近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的制备方法，包括以下步骤：
(1)按照计量比为8:2:1:3:7称量BaCO3、SrCO3、Bi2O3、TiO2、Nb2O5；
(2)将步骤(1)中的各原料置于玛瑙研钵共同研磨8h，直至原料均匀混合，得到混合物；
(3)将步骤(2)的混合物放入Al2O3材质坩埚并置于马弗炉内，以5℃/min 升温速率升温至1000℃，保温7h，冷却至室温，得到一段烧结物；
(4)将步骤(3)的一段烧结物继续研磨4h，至无颗粒感的粉体，得到坯料；
(5)将步骤(4)的坯料以3℃/min速率升温至1320℃，保温4h，然后以1℃/min速率冷却至室温，得到近室温弛豫铁电材料Ba4SrBiTi3Nb7O30。
实施例6
近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的制备方法，包括以下步骤：
(1)按照计量比为8:2:1:3:7称量BaCO3、SrCO3、Bi2O3、TiO2、Nb2O5；
(2)将步骤(1)中的各原料置于玛瑙研钵共同研磨8h，直至原料均匀混合，得到混合物；
(3)将步骤(2)的混合物放入Al2O3材质坩埚并置于马弗炉内，以5℃/min 升温速率升温至1200℃，保温3h，冷却至室温，得到一段烧结物；
(4)将步骤(3)的一段烧结物继续研磨4h，至无颗粒感的粉体，得到坯料；
(5)将步骤(4)的坯料以3℃/min速率升温至1280℃，保温6h，然后以1℃/min速率冷却至室温，得到近室温弛豫铁电材料Ba4SrBiTi3Nb7O30。
本发明实施例1-6均制得具有近室温表现出明显弛豫性铁电特征的铁电材料Ba4SrBiTi3Nb7O30，且效果平行，下面以实施例1制得的近室温弛豫铁电材料Ba4SrBiTi3Nb7O30为例进行研究，具体研究结果如下所示：
对实施例1中制得的Ba4SrBiTi3Nb7O30材料样品微观结构进行表征，采用 X射线衍射仪(XRD)对其物相分析；从图1可看出，样品衍射峰尖锐，结晶良好，无其他杂质生成。
图2给出了近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的介电-温度谱图；从图2中可以看出Ba4SrBiTi3Nb7O30在250K附近存在铁电转变，且随测试频率的增加，样品的介电常数和介电损耗峰均向高温方向偏移，显现出明显的弛豫特征。
图3给出了本发明实施例1的近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的铁电极化曲线，可以看到当温度降低到250K左右，Ba4SrBiTi3Nb7O30由顺电相进入铁电相，开始出现自发铁电极化(电极化强度不再为零)，证实了其铁电性。
显然，本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发明的精神和范围。这样，倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内，则本发明也意图包含这些改动和变型在内。

Claims (6)

1.一种近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的制备方法，其特征在于，包括如下步骤：
(1)按照化学式Ba4SrBiTi3Nb7O30称取原料BaCO3、SrCO3、Bi2O3、TiO2和Nb2O5，将各原料共同研磨，直至原料均匀混合，得到混合物；
其中，BaCO3、SrCO3、Bi2O3、TiO2和Nb2O5的化学计量之比为8:2:1:3:7；
(2)将步骤(1)的混合物先预烧，冷却至室温，得到一段烧结物；再研磨至无颗粒感的粉体，得到坯料；然后将坯料进行烧结，冷却至室温，得到近室温弛豫铁电材料Ba4SrBiTi3Nb7O30；
所述步骤(2)中烧结的条件为：将坯料在1250-1350℃下烧结4-6h后，冷却至室温，得到近室温弛豫铁电材料Ba4SrBiTi3Nb7O30。
2.根据权利要求1所述的近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的制备方法，其特征在于，所述步骤(1)的研磨时间为6-10h，所述步骤(2)的研磨时间为2-4h。
3.根据权利要求1所述的近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的制备方法，其特征在于，所述步骤(2)中预烧的条件为：将步骤(1)的混合物在1000-1200℃下预烧3-7h后，冷却至室温，得到一段烧结物。
4.根据权利要求1所述的近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的制备方法，其特征在于，所述步骤(2)中，将坯料在1300℃下烧结5h。
5.一种权利要求1-4任一项所述制备方法制得的近室温弛豫铁电材料Ba4SrBiTi3Nb7O30，其特征在于，所述近室温弛豫铁电材料Ba4SrBiTi3Nb7O30的结晶为钨青铜结构，在250K近室温表现出弛豫铁电特性。
6.一种权利要求5所述的近室温弛豫铁电材料Ba4SrBiTi3Nb7O30在制备计算机存储元件、微位移器、传感器、储能器中的应用。
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