CN109626989B - 一种无污染环保型多功能陶瓷材料的制备方法 - Google Patents

一种无污染环保型多功能陶瓷材料的制备方法 Download PDF

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CN109626989B
CN109626989B CN201910139005.5A CN201910139005A CN109626989B CN 109626989 B CN109626989 B CN 109626989B CN 201910139005 A CN201910139005 A CN 201910139005A CN 109626989 B CN109626989 B CN 109626989B
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Abstract

本发明涉及一种无污染环保型多功能陶瓷材料的制备方法，所述陶瓷材料是以BaCO3和TiO2为主要原料，以钙相、锆相、钴相和镨相作为掺杂剂制备而成；所述钙相、锆相、钴相和镨相分别是CaCO3、ZrO2、Co2O3和Pr6O11；BaCO3、TiO2、CaCO3、ZrO2的摩尔比为(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3，Co2O3的质量百分比含量为0.025wt％；Pr6O11的质量百分比含量为0.025wt％。本发明的陶瓷材料具有介电损耗低，压电系数高等特点，可广泛用于手机、电视、电脑、冶金、石油、化工等行业。

Description

一种无污染环保型多功能陶瓷材料的制备方法
技术领域
本发明涉及一种无污染环保型多功能陶瓷材料的制备方法。
背景技术
材料是人类赖以生存、发展的物质基础。它既是人类社会发展的先导，又是人类进步的里程碑。自1970年以来，以材料为基础，信息技术作为载体的高新技术领域群不断向发达国家的社会各方面渗透。这种变化不仅促使了人们的生活水平和生活方式发生大的变化，也使世界各国的生产力产生了新的飞跃。而伴随着这种变化，各国的经济结构，产业结构和劳动就业结构等也发生了新的巨大变化。这致使国家之间的基本竞争焦点也发生了根本的转变。世界各国因此逐渐的对新材料的研究与开发重视起来。而近些年来，美国、欧盟共同体和日本都把发展新材料技术放在国家科技发展关键技术的首位。
信息功能陶瓷材料是新材料领域的一个重要分支，而它被划分为电子功能材料。现在，它被广泛地应用于军用(战斗机、鱼雷、雷达等)和民用(手机、电视、电脑、冶金、石油、化工等)。自居里兄弟发现压电效应及逆压电效应以来，压电材料得到了迅猛发展，各种具有优异性能的压电陶瓷及单晶相继被科研工作者发明和发现。而与压电材料相关的应用器件的研究和生产也得到了飞速的发展。随着经济的发展，生活水平的不断提高，人们对于在一些高温领域工作的自动化设备的需求迅速增长。而对其中的超声探伤应用，高温物体的加速度、振动检测等需求则是显得尤为突出。但是要使压电材料能够在高温环境中保持性能稳定一直以来都是压电方向的难题。因此对高温压电材料尤其是高温压电陶瓷的研究成为了当务之急。
压电体材料受到机械外力的作用导致压电体两端表面内出现符号相反的束缚电荷，其电荷密度与外机械力成正比，这种现象称为正压电效应。与此现象相反的则称为逆压电效应。正逆压电效应是相生的，具有正压电效应的材料必然也具有逆压电效应。某些材料受到机械应力作用下发生相变时，内部会引起正负电荷中心移动而产生极化，表面出现感应电荷，称为正压电效应，反之，若将正压电效应的材料放到电场中，电场使材料正负电荷移动称为逆压电效应。不管是哪种压电效应，原因在于对称中心的晶体中正负离子的相对移动才引起的。压电材料种类可以分为：晶体(如石英、铌酸锂(LiNbO3)、碘酸锂等)、半导体(如CdS、CdSe、ZnO、ZnS,、ZnTe、ZdTe、GaAs、GaSb等)、压电陶瓷(如BaTiO3、PbTiO3)。材料的压电效应可以应用于滤波器、换能器、谐振器、传感器、扩音器、压电点火器、石英电子表、微位移控制等多个方面。
在一定外加电场范围内，介电系数与外加电场强度变化呈现线性关系，其介电系数不会随着外加电场的变化而变化，这是线性介质材料的重要特点。尽管线性电介质材料通常具有很高的击穿场强和高的储能效率，但是其往往具有较低的相对介电常数，导致其储能密度数值很低。非线性介质材料分为铁电体和反铁电体两种类型，铁电体自发形成的偶极矩能够在外加电场的作用下扭转方向，因偶极矩而产生储能效果。但由于实验条件的限制，制备出电容器器件还是比较困难的；而反铁电储能材料，具有小体积、大容量、超高耐压的储能特性，是材料研究领域一个新的研究热点之一。
虽然CN201510925007.9公开了一种钛酸钡压电陶瓷及其制备方法，本发明的陶瓷是以BaCO3和TiO2为主要原料，以钙相、锆相和钴相作为掺杂剂制备而成。其制备方法是先取所述主要原料和掺杂剂，分别烘干；将烘干的主要原料和掺杂剂混合，拌匀，得混合物；将混合物在1160-1280℃的环境中煅烧，得合成物；将合成物粉碎，得粉末，然后将粉末烘干，得烘干的粉末；在烘干的粉末中加入粘结剂，使其粘合，然后在20Mpa的压力下压成圆片；将圆片在1350-1500℃下保温四小时，冷却后取出，得烧结物；最后将烧结物进行被电极和极化处理，得钛酸钡压电陶瓷。但该发明的压电陶瓷介电损耗低仍然很高，无法满足要求。
因此，如何制备低介电损耗，高介电常数及压电系数高的陶瓷材料是本领域需要解决的技术问题。
发明内容
为了解决现有技术中无法制备低介电损耗，高介电常数及压电系数高的陶瓷材料的技术问题，本发明提出了如下技术方案：
一种无污染环保型多功能陶瓷材料，所述陶瓷材料是以BaCO3和TiO2为主要原料，以钙相、锆相、钴相和镨相作为掺杂剂制备而成；所述钙相、锆相、钴相和镨相分别是CaCO3、ZrO2、Co2O3和Pr6O11；BaCO3、TiO2、CaCO3、ZrO2的摩尔比为(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3，Co2O3的质量百分比含量为0.025wt％；Pr6O11的质量百分比含量为0.025wt％。
一种根据权利要求1所述的所述陶瓷材料的制备方法，所述陶瓷材料通过如下方法制备：
(1)配料：取所述主要原料和掺杂剂，分别在100℃的烘箱里烘8h，烘干，备用；
(2)混料：将烘干的主要原料和掺杂剂混合，拌匀，得混合物；
(3)合成：将混合物在1200-1250℃的环境中煅烧3-4h，然后随炉自然冷却，得合成物；
(4)粉碎：将合成物粉碎，得粉末，然后将粉末烘干，得烘干的粉末，所述粉末的粒度为10μm；
(5)成型：在烘干的粉末中加入石蜡，使其粘合，然后在20MPa的压力下压成直径为13mm的圆片；
(6)烧结：烧结过程采用二段式烧结工艺，所述二段式烧结工艺的具体过程包括：在1400℃下保温2小时，然后升温至1550℃保温2小时，随炉自然冷却后取出，得烧结物；
(7)被电极及极化处理：将烧结物进行被电极和极化处理，得钛酸钡压电陶瓷；其中，所述的被电极及极化处理是先在烧结物的两面涂上银浆，然后施行电极进行极化。
本发明的技术方案具有如下由益效果：
本发明通过优化掺杂相和烧结工艺能够在充分保证压电常数在合理范围的基础上，进一步降低介电损耗，即在保证压电常数在300～350范围内的基础上，介电损耗可以降低至1.0％。与传统的BCZT基压电陶瓷相比，本发明的陶瓷具有介电损耗低，且压电常数较高的有益效果。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例和对比例，对本发明进行进一步详细说明。
实施例1
一种无污染环保型多功能陶瓷材料，所述陶瓷材料是以BaCO3和TiO2为主要原料，以钙相、锆相、钴相和镨相作为掺杂剂制备而成；所述钙相、锆相、钴相和镨相分别是CaCO3、ZrO2、Co2O3和Pr6O11；BaCO3、TiO2、CaCO3、ZrO2的摩尔比为(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3，Co2O3的质量百分比含量为0.025wt％；Pr6O11的质量百分比含量为0.025wt％。
所述陶瓷材料通过如下方法制备：
(1)配料：取所述主要原料和掺杂剂，分别在100℃的烘箱里烘8h，烘干，备用；
(2)混料：将烘干的主要原料和掺杂剂混合，拌匀，得混合物；
(3)合成：将混合物在1200℃的环境中煅烧3h，然后随炉自然冷却，得合成物；
(4)粉碎：将合成物粉碎，得粉末，然后将粉末烘干，得烘干的粉末，所述粉末的粒度为10μm；
(5)成型：在烘干的粉末中加入石蜡，使其粘合，然后在20MPa的压力下压成直径为13mm的圆片；
(6)烧结：烧结过程采用二段式烧结工艺，所述二段式烧结工艺的具体过程包括：在1400℃下保温2小时，然后升温至1550℃保温2小时，随炉自然冷却后取出，得烧结物；
(7)被电极及极化处理：将烧结物进行被电极和极化处理，得钛酸钡压电陶瓷；其中，所述的被电极及极化处理是先在烧结物的两面涂上银浆，然后施行电极进行极化。
实施例2
一种无污染环保型多功能陶瓷材料，所述陶瓷材料是以BaCO3和TiO2为主要原料，以钙相、锆相、钴相和镨相作为掺杂剂制备而成；所述钙相、锆相、钴相和镨相分别是CaCO3、ZrO2、Co2O3和Pr6O11；BaCO3、TiO2、CaCO3、ZrO2的摩尔比为(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3，Co2O3的质量百分比含量为0.025wt％；Pr6O11的质量百分比含量为0.025wt％。
所述陶瓷材料通过如下方法制备：
(1)配料：取所述主要原料和掺杂剂，分别在100℃的烘箱里烘8h，烘干，备用；
(2)混料：将烘干的主要原料和掺杂剂混合，拌匀，得混合物；
(3)合成：将混合物在1225℃的环境中煅烧3.5h，然后随炉自然冷却，得合成物；
(4)粉碎：将合成物粉碎，得粉末，然后将粉末烘干，得烘干的粉末，所述粉末的粒度为10μm；
(5)成型：在烘干的粉末中加入石蜡，使其粘合，然后在20MPa的压力下压成直径为13mm的圆片；
(6)烧结：烧结过程采用二段式烧结工艺，所述二段式烧结工艺的具体过程包括：在1400℃下保温2小时，然后升温至1550℃保温2小时，随炉自然冷却后取出，得烧结物；
(7)被电极及极化处理：将烧结物进行被电极和极化处理，得钛酸钡压电陶瓷；其中，所述的被电极及极化处理是先在烧结物的两面涂上银浆，然后施行电极进行极化。
实施例3
一种无污染环保型多功能陶瓷材料，所述陶瓷材料是以BaCO3和TiO2为主要原料，以钙相、锆相、钴相和镨相作为掺杂剂制备而成；所述钙相、锆相、钴相和镨相分别是CaCO3、ZrO2、Co2O3和Pr6O11；BaCO3、TiO2、CaCO3、ZrO2的摩尔比为(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3，Co2O3的质量百分比含量为0.025wt％；Pr6O11的质量百分比含量为0.025wt％。
所述陶瓷材料通过如下方法制备：
(1)配料：取所述主要原料和掺杂剂，分别在100℃的烘箱里烘8h，烘干，备用；
(2)混料：将烘干的主要原料和掺杂剂混合，拌匀，得混合物；
(3)合成：将混合物在1250℃的环境中煅烧4h，然后随炉自然冷却，得合成物；
(4)粉碎：将合成物粉碎，得粉末，然后将粉末烘干，得烘干的粉末，所述粉末的粒度为10μm；
(5)成型：在烘干的粉末中加入石蜡，使其粘合，然后在20MPa的压力下压成直径为13mm的圆片；
(6)烧结：烧结过程采用二段式烧结工艺，所述二段式烧结工艺的具体过程包括：在1400℃下保温2小时，然后升温至1550℃保温2小时，随炉自然冷却后取出，得烧结物；
(7)被电极及极化处理：将烧结物进行被电极和极化处理，得钛酸钡压电陶瓷；其中，所述的被电极及极化处理是先在烧结物的两面涂上银浆，然后施行电极进行极化。
对比例1
对比例1中Co2O3的质量百分比含量为0.05wt％；未掺杂Pr6O11，其它与实施例1完全一致。
对比例2
对比例2中Pr6O11的质量百分比含量为0.05wt％；未掺杂Co2O3，其它与实施例1完全一致。
对比例3
对比例3与实施例1有两点不同：(1)中Co2O3的质量百分比含量为0.05wt％；未掺杂Pr6O11；(2)烧结过程采用一段式烧结工艺，即：在1400℃下保温四小时，随炉自然冷却后取出，得烧结物。其它与实施例1完全一致。
为了验证实施例1-3及对比例1-3的技术效果，将实施例1-3及对比例1-3的样品进行效果检测，效果检测采用GB/T3389-2008，利用介电损耗、压电常数表征，结果如下：
Figure BDA0001977943710000061
上述结果表明，本发明通过优化掺杂相和烧结工艺能够在充分保证压电常数在合理范围的基础上，进一步降低介电损耗，即在保证压电常数在300～350范围内的基础上，介电损耗可以降低至1.0％。与传统的BCZT基压电陶瓷相比，本发明的陶瓷材料具有介电损耗低，且压电常数较高的有益效果。

Claims (1)

1.一种无污染环保型多功能陶瓷材料的制备方法，其特征在于，所述陶瓷材料是以BaCO3和TiO2为主要原料，以钙相、锆相、钴相和镨相作为掺杂剂制备而成；所述钙相、锆相、钴相和镨相分别是CaCO3、ZrO2、Co2O3和Pr6O11；BaCO3、TiO2、CaCO3、ZrO2的摩尔比为(Ba0.85Ca0.15)(Zr0.1Ti0.9)O3，Co2O3的质量百分比含量为0.025wt％；Pr6O11的质量百分比含量为0.025wt％；
所述陶瓷材料通过如下方法制备：
(1)配料：取所述主要原料和掺杂剂，分别在100℃的烘箱里烘8h，烘干，备用；
(2)混料：将烘干的主要原料和掺杂剂混合，拌匀，得混合物；
(3)合成：将混合物在1200℃的环境中煅烧3h，然后随炉自然冷却，得合成物；
(4)粉碎：将合成物粉碎，得粉末，然后将粉末烘干，得烘干的粉末，所述粉末的粒度为10μm；
(5)成型：在烘干的粉末中加入石蜡，使其粘合，然后在20MPa的压力下压成直径为13mm的圆片；
(6)烧结：烧结过程采用二段式烧结工艺，所述二段式烧结工艺的具体过程包括：在1400℃下保温2小时，然后升温至1550℃保温2小时，随炉自然冷却后取出，得烧结物；
(7)被电极及极化处理：将烧结物进行被电极和极化处理，得钛酸钡压电陶瓷；其中，步骤(7)中，所述的被电极及极化处理是先在烧结物的两面涂上银浆，然后施行电极进行极化；
所述陶瓷材料的介电损耗低且压电常数较高，经GB/T3389-2008检测，所述陶瓷材料的介电损耗为1.0％，压电常数为320。
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