CN110357612A - 一种石墨烯-ccto基陶瓷复合介电材料的制备方法 - Google Patents

一种石墨烯-ccto基陶瓷复合介电材料的制备方法 Download PDF

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CN110357612A
CN110357612A CN201910697433.XA CN201910697433A CN110357612A CN 110357612 A CN110357612 A CN 110357612A CN 201910697433 A CN201910697433 A CN 201910697433A CN 110357612 A CN110357612 A CN 110357612A
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China
Prior art keywords
graphene
base ceramic
ccto
ccto base
ceramic composite
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CN201910697433.XA
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曾和平
黄延伟
贺嘉杨
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East China Normal University
Chongqing Institute of East China Normal University
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East China Normal University
Chongqing Institute of East China Normal University
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Priority to CN201910697433.XA priority Critical patent/CN110357612A/zh
Publication of CN110357612A publication Critical patent/CN110357612A/zh
Priority to US16/910,781 priority patent/US11306030B2/en
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  • Compositions Of Oxide Ceramics (AREA)

Abstract

本发明公开了一种石墨烯‑CCTO基陶瓷复合介电材料的制备方法，其包括以下步骤：将金属离子源分溶解于溶剂中，混匀后，得到CCTO基陶瓷材料的前驱体溶胶；将所述CCTO基陶瓷材料的前驱体溶胶静置进行老化后，加入氧化石墨烯分散液，混匀后，干燥得到石墨烯‑CCTO基陶瓷材料的前驱体干粉，将所述石墨烯‑CCTO基陶瓷材料的前驱体干粉研磨成细粉后，在低功率激光下进行辐照，得到石墨烯‑CCTO基陶瓷复合粉末；将所述石墨烯‑CCTO基陶瓷复合粉末经过压实成型后，在高功率激光下进行合成，得到所述石墨烯‑CCTO基陶瓷复合介电材料。本发明所得复合介电材料颗粒细小、致密性较好，具有巨介电、低损耗的特点，且该制备方法成本低廉、快速高效，适合巨介电材料在高密度存储器件中的大范围应用。

Description

一种石墨烯-CCTO基陶瓷复合介电材料的制备方法
技术领域
本发明属于激光加工技术和能源材料领域，具体涉及一种快速激光烧结合成固态电解质及其制备方法。
背景技术
CCTO是一种巨介电常数陶瓷材料，在很宽的频率范围和温度范围内，介电常数可达到105以上，随着电子通讯行业以及新能源行业的快速发展，CCTO的巨介电性能的研究和开发越来越受到人们的关注，尤其是在高密度存储器件中，有着广泛的应用前景。CCTO属于ABO3型化合物，其中A位为Ca、Cu，B位为Ti，具有类钙钛矿结构。自2000年由Subramanian等人报道提出后[M.A.Subramanian,D.Li,N.Duan,B.A.Reisner,A.Sleight,Highdielectric constant inACaCu3Ti4O12andACaCu3Ti4O12phase.J.Solid State Chem.151(2),323-325(2000)]，引起了研究者们的巨大兴趣，CCTO从室温至600K其介电常数几乎保持不变，且在频率范围100Hz-1000MHz具有较高的介电常数值，CCTO陶瓷具有很多优良的特性，但是CCTO材料的介电常数在保持较高的同时，其介电损耗也很高，尤其是在低频阶段，长期以来，CCTO的低频介电损耗过高一直是人们倾力解决的问题，同时其巨介电性能也与合成原料和工艺制备过程有着密切的关系，这些问题严重阻碍了CCTO材料在电子元器件领域的应用，目前，针对CCTO陶瓷的介电性能的机理解释很多，其中得到广泛认可的是由Sinclair等人[Sinclair D C,Adams T B,Morrison F D,et al.CaCu3Ti4O12:One-stepinternal barrier layer capacitor.Applied Physics Letters,2002,80(12):2153-2155]提出的内部阻挡层电容器模型(IBLC)，该模型认为CCTO陶瓷超高的介电常数是由其内部存在的晶粒的半导化和晶界的绝缘性共同作用的结果，其中晶界的绝缘性与陶瓷的介电损耗有着直接的联系，因此，降低晶界的电导率即提高晶界的绝缘性可以有效降低介电损耗，目前，对CCTO的改性研究大部分集中在提高晶粒的半导性和提高晶界的绝缘性这两个方面，主要通过掺杂改性的方式，对CCTO进行A位掺杂或B位掺杂，A位掺杂离子一般为3价阳离子，如La3+、Bi3+、Nd3+等，这类掺杂取代A位上的Ca2+，在Ca2+位产生阳离子空位。B位掺杂离子一般为离子价为5价或6价的阳离子，如Nb5+、Ta5+、Sb5+、W6+等，则取代B位的Ti4+，在Ti4+位产生氧空位。但这些掺杂研究并没有达到改善CCTO材料的整体性能的目的，通常是在降低介电损耗的同时也降低了介电常数，或者在提高介电性能的同时，带来了更多工艺过程的复杂性问题。
石墨烯材料具有较高的电子迁移率、优良的热导性和高的比表面积，石墨烯结构稳定，具有很好的化学稳定性，对陶瓷材料进行石墨烯包覆不仅可以提高陶瓷材料的固有性质，还可以阻挡腐蚀介质的渗透形成物理阻隔，而且石墨烯的表面很大，应用较少的石墨烯就可以有效改善陶瓷材料的性能，且可以进一步提高材料的稳定性以适合在各种环境中应用。超薄的石墨烯不仅不会对基质材料的质量产生改变，同时还兼具高的强度和良好的摩擦学性能，由此可见石墨烯应用到介电材料中具有可行性。鉴于此，本发明采用激光催化合成包覆石墨烯的CCTO基复合介电陶瓷材料，介电陶瓷材料的制备方法很多，包括固相反应法、溶胶-凝胶法、共沉淀法、机械混合法等，这些合成方法大多需要长时间的高温煅烧和高温烧结过程，且烧结时长与目标样品的性能关系密切，本文针对这些问题中存在的不足之处，提出先采用类似溶胶-凝胶方法合成CCTO基陶瓷材料的先驱物，然后添加氧化石墨烯分散液，再用激光处理的方法来高效制备石墨烯-CCTO基陶瓷复合材料，采用激光催化法对样品实现快速高效的合成。
发明内容
本发明的目的在于提出一种石墨烯-CCTO基陶瓷复合介电材料的制备方法，以解决现有技术中所存在的上述问题。
本发明是通过以下技术方案实现的：
一种石墨烯-CCTO基陶瓷复合介电材料的制备方法，其包括以下步骤：
将金属离子源分溶解于溶剂中，混匀后，得到CCTO基陶瓷材料的前驱体溶胶；
将所述CCTO基陶瓷材料的前驱体溶胶静置进行老化后，加入氧化石墨烯分散液，混匀后，干燥得到石墨烯-CCTO基陶瓷材料的前驱体干粉，将所述石墨烯-CCTO基陶瓷材料的前驱体干粉研磨成细粉后，在低功率激光下进行辐照，得到石墨烯-CCTO基陶瓷复合粉末；
将所述石墨烯-CCTO基陶瓷复合粉末经过压实成型后，在高功率激光下进行合成，得到所述石墨烯-CCTO基陶瓷复合介电材料。
作为优选方案，所述CCTO基陶瓷材料包括钛酸铜钙，以及掺杂金属氧化物的钛酸铜钙。
作为优选方案，所述金属氧化物包括钇氧化物、镱氧化物、锌氧化物、锡氧化物、钽氧化物、铪氧化物、钆氧化物、锆氧化物中的至少一种。
作为优选方案，所述石墨烯与CCTO基陶瓷材料的质量比为1:3～1:100。
作为优选方案，所述干燥的温度为100～180℃。
作为优选方案，所述压实成型的方法包括直接压片成型、冷等静压成型或加PVA造粒成型。
与现有技术相比，本发明具有如下的有益效果：
本发明所得复合介电材料颗粒细小、致密性较好，具有巨介电、低损耗的特点，且该制备方法成本低廉、快速高效，适合巨介电材料在高密度存储器件中的大范围应用。
附图说明
通过阅读参照以下附图对非限制性实施例所作的详细描述，本发明的其它特征、目的和优点将会变得更明显：
图1为本发明中实施例2所合成的石墨烯的CCTO陶瓷复合材料的介电性能测试曲线。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明，但不以任何形式限制本发明。应当指出的是，对本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进。这些都属于本发明的保护范围。
在本发明中，以50W作为激光功率的界定，高于50W为高功率，低于50W为低功率。
实施例1
以钛酸四丁脂、硝酸铜、醋酸钙为先驱物原料，以无水乙醇、冰醋酸为溶剂，先称取0.04mol的钛酸四丁脂，溶于无水乙醇中，用玻璃棒搅拌均匀混合，加入冰醋酸，再用磁力搅拌器持续搅拌1小时配制含有钛离子的先驱物溶液，同时称取0.03mol的Cu(NO3)2·3H2O，溶于无水乙醇中，在磁力搅拌器上搅拌至澄清透明的蓝色溶液，然后将此蓝色溶液加入前述含钛离子的先驱物溶液，形成澄清透明的蓝绿色溶液，同理按配比制备含钙离子的溶液，即称取一定量的Ca(CH3COO)2·H2O，溶解于40ml去离子水中得到含钙离子的溶液。将此溶液慢慢滴加至前述蓝绿色含钛离子、铜离子的溶液中，在磁力搅拌器上搅拌1小时，得到蓝绿色的澄清透明的CCTO溶胶先驱体，即CCTO陶瓷材料的先驱物溶胶，将此溶胶静置24小时进行老化，然后加入一定比例的氧化石墨烯分散液，超声振荡混合60min，再在磁力搅拌器上混合搅拌3h，控制温度60℃，蒸发部分溶剂，然后干燥得石墨烯-CCTO基陶瓷复合材料先驱体干粉，将干粉研磨成细粉，得到细粉状石墨烯-CCTO基陶瓷材料先驱物，将所述粉状先驱物置于铜坩埚内，在真空气氛下进行低功率激光辐照，激光功率为25W，辐照时间20min，除去有机溶剂及溶阴离子，得到石墨烯-CCTO基陶瓷复合粉末，然后将此粉末经液压机压实成型，压力为15MPa，保持时间10s，然后进行高功率激光催化合成，控制激光功率为80W、作用时间5s。所得复合介电材料的致密性较未添加石墨烯的CCTO有所提高，介电常数可达104方及以上，介电损耗最低为0.2，材料微观颗粒大小在100nm以下。
实施例2
以钛酸四丁脂、硝酸铜、醋酸钙为先驱物原料，以无水乙醇、冰醋酸为溶剂，先称取0.04mol的钛酸四丁脂，溶于无水乙醇中，用玻璃棒搅拌均匀混合，加入冰醋酸，再用磁力搅拌器持续搅拌1小时配制含有钛离子的先驱物溶液，同时称取0.03mol的Cu(NO3)2·3H2O，溶于无水乙醇中，在磁力搅拌器上搅拌至澄清透明的蓝色溶液，然后将此蓝色溶液加入前述含钛离子的先驱物溶液，形成澄清透明的蓝绿色溶液，同理按配比制备含钙离子的溶液，即称取一定量的Ca(CH3COO)2·H2O，溶解于40ml去离子水中得到含钙离子的溶液。将此溶液慢慢滴加至前述蓝绿色含钛离子、铜离子的溶液中，在磁力搅拌器上搅拌1小时，得到蓝绿色的澄清透明的CCTO溶胶先驱体，即CCTO陶瓷材料的先驱物溶胶，将此溶胶静置36小时进行老化，然后加入一定比例的氧化石墨烯分散液，超声振荡混合30min，再在磁力搅拌器上混合搅拌2h，控制温度70℃，蒸发部分溶剂，然后干燥得石墨烯-CCTO基陶瓷复合材料先驱体干粉，将干粉研磨成细粉，得到细粉状石墨烯-CCTO基陶瓷材料先驱物，将所述粉状先驱物置于铜坩埚内，在真空气氛下进行低功率激光辐照，激光功率为20W，辐照时间30min，除去有机溶剂及溶阴离子，得到石墨烯-CCTO基陶瓷复合粉末，然后将此粉末经等静压压实成型，压力为80MPa，保持时间3min，然后进行高功率激光催化合成，控制激光功率为分别为78W、90W、102W、300W，作用时间5s，图1是激光催化合成包覆石墨烯的CCTO陶瓷复合材料的介电性能测试。所得复合介电材料的致密性较未添加石墨烯的CCTO有所提高，介电常数可达104方及以上，介电损耗最低为0.5，材料微观颗粒大小在100nm以下。
实施例3
以钛酸四丁脂、硝酸铜、醋酸钙为先驱物原料，以无水乙醇、冰醋酸为溶剂，先称取0.04mol的钛酸四丁脂，溶于无水乙醇中，用玻璃棒搅拌均匀混合，加入冰醋酸，再用磁力搅拌器持续搅拌1小时配制含有钛离子的先驱物溶液，同时称取0.03mol的Cu(NO3)2·3H2O，溶于无水乙醇中，在磁力搅拌器上搅拌至澄清透明的蓝色溶液，然后将此蓝色溶液加入前述含钛离子的先驱物溶液，形成澄清透明的蓝绿色溶液，同理按配比制备含钙离子的溶液，即称取一定量的Ca(CH3COO)2·H2O，溶解于40ml去离子水中得到含钙离子的溶液。将此溶液慢慢滴加至前述蓝绿色含钛离子、铜离子的溶液中，在磁力搅拌器上搅拌1小时，得到蓝绿色的澄清透明的CCTO溶胶先驱体，即CCTO陶瓷材料的先驱物溶胶，将此溶胶静置24小时进行老化，然后加入一定比例的氧化石墨烯分散液，超声振荡混合35min，再在磁力搅拌器上混合搅拌2h，控制适当温度，蒸发部分溶剂，然后干燥得石墨烯-CCTO基陶瓷复合材料先驱体干粉，将干粉研磨成细粉，得到细粉状石墨烯-CCTO基陶瓷材料先驱物，将所述粉状先驱物置于铜坩埚内，在空气气氛下进行低功率激光辐照，激光功率为15W，辐照时间20min，除去有机溶剂及溶阴离子，得到石墨烯-CCTO基陶瓷复合粉末，然后将此粉末经等静压压实成型，压力为80MPa，保持时间3min，然后进行高功率激光催化合成，控制激光功率为90W、作用时间5s，最终得到一种石墨烯-CCTO基陶瓷复合介电材料。所得复合介电材料的致密性较未添加石墨烯的CCTO有所提高，介电常数可达3×104方及以上，介电损耗最低为0.3，材料微观颗粒大小在100nm以下。
以上对本发明的具体实施例进行了描述。需要理解的是，本发明并不局限于上述特定实施方式，本领域技术人员可以在权利要求的范围内做出各种变形或修改，这并不影响本发明的实质内容。

Claims (6)

1.一种石墨烯-CCTO基陶瓷复合介电材料的制备方法，其特征在于，包括以下步骤：
将金属离子源分溶解于溶剂中，混匀后，得到CCTO基陶瓷材料的前驱体溶胶；
将所述CCTO基陶瓷材料的前驱体溶胶静置进行老化后，加入氧化石墨烯分散液，混匀后，干燥得到石墨烯-CCTO基陶瓷材料的前驱体干粉，将所述石墨烯-CCTO基陶瓷材料的前驱体干粉研磨成细粉后，在低功率激光下进行辐照，得到石墨烯-CCTO基陶瓷复合粉末；
将所述石墨烯-CCTO基陶瓷复合粉末经过压实成型后，在高功率激光下进行合成，得到所述石墨烯-CCTO基陶瓷复合介电材料。
2.如权利要求1所述的石墨烯-CCTO基陶瓷复合介电材料的制备方法，其特征在于，所述CCTO基陶瓷材料包括钛酸铜钙，以及掺杂金属氧化物的钛酸铜钙。
3.如权利要求2所述的石墨烯-CCTO基陶瓷复合介电材料的制备方法，其特征在于，所述金属氧化物包括钇氧化物、镱氧化物、锌氧化物、锡氧化物、钽氧化物、铪氧化物、钆氧化物、锆氧化物中的至少一种。
4.如权利要求1所述的石墨烯-CCTO基陶瓷复合介电材料的制备方法，其特征在于，所述石墨烯与CCTO基陶瓷材料的质量比为1:3～1:100。
5.如权利要求1所述的石墨烯-CCTO基陶瓷复合介电材料的制备方法，其特征在于，所述干燥的温度为100～180℃。
6.如权利要求1所述的石墨烯-CCTO基陶瓷复合介电材料的制备方法，其特征在于，所述压实成型的方法包括直接压片成型、冷等静压成型或加PVA造粒成型。
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Application publication date: 20191022