CN109553411B - 一种高击穿场强钛酸铜锶钙介电陶瓷材料及其制备方法 - Google Patents

一种高击穿场强钛酸铜锶钙介电陶瓷材料及其制备方法 Download PDF

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CN109553411B
CN109553411B CN201910095081.0A CN201910095081A CN109553411B CN 109553411 B CN109553411 B CN 109553411B CN 201910095081 A CN201910095081 A CN 201910095081A CN 109553411 B CN109553411 B CN 109553411B
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张建花
吝伶艳
刘玉倩
李卓晓
郑杰诚
宋建成
李媛媛
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Abstract

本发明公开一种高击穿场强钛酸铜锶钙(CSCTO)介电陶瓷材料及其制备方法。本陶瓷材料的组成为Ca1‑xSrxCu3Ti4O12(0<x<1)。CSCTO粉体用溶胶凝胶法合成。具体工艺为：以硝酸铜、硝酸钙、硝酸锶、钛酸四丁酯为原料，按照各化学元素的计量比进行称量配料；以无水乙醇为溶剂；调节溶液的pH值为3~5；将上述溶胶置于水浴锅中，不断搅拌至形成干凝胶；利用电炉和马弗炉除去干凝胶中的有机物，形成CSCTO前驱体粉末；之后进行加胶、研磨、造粒、压片，制成陶瓷胚体，再把胚体放入马弗炉内烧结；在炉内自然冷却至室温，得到CSCTO介电陶瓷。该CSCTO陶瓷的击穿场强可提高至52.50 kV/cm，在高压电容等领域具有广泛的应用前景。

Description

一种高击穿场强钛酸铜锶钙介电陶瓷材料及其制备方法
技术领域
本发明属于电介质陶瓷合成技术领域，具体涉及一种高击穿场强钛酸铜锶钙介电陶瓷材料及其制备方法。
背景技术
目前，随着电子技术对器件高集成度和高可靠性要求的进一步提高，高介电常数材料成为人们关注的热点。钛酸铜钙（CaCu3Ti4O12，简称CCTO）为钙钛矿立方晶系结构，是近年来最具有代表性的新型高介电常数材料，该材料的介电常数高达到104~105，在很宽的温度和频率范围内保持稳定，且CCTO不会出现铁电-顺电相变；另外，CCTO制备工艺简单，烧结温度不高，具有工业化生产的潜在优势。良好的综合性能，使CCTO很有希望替代传统的介电陶瓷材料，在高密度能量存储、高介电电容器等一系列高新技术领域中具有很好的应用前景。
目前，国内外的许多研究结果表明：室温下，CCTO的击穿场强较低，普遍在2 kV/cm以下。(B. Cheng, Y.H. Lin, W. Deng, J.N. Cai, J.L. Lan, C.W. Nan, X. Xiao,J.L. He, Dielectric and nonlinear electrical behaviors of Ce-doped CaCu3Ti4O12ceramics, J Electroceram (2012) 29:250-253.)。国内外的学者的相关研究中，一种钛酸锆铜镉巨介电陶瓷材料CdCu3Zr0.05Ti3.95O12的击穿场强达到1530 V/cm，同时1 kHz下，其相对介电常数为15082 (晁小练,彭战辉,杨祖培,梁朋飞.一种高击穿场强钛酸锆铜镉巨介电陶瓷材料及其制备方法:中国, 201710593564.4 [P].2017.09.29.)。另外，一种双钙钛矿复相陶瓷Y2x/3Ca1-xCu3Ti4O12的击穿场强达到了11.24 kV/cm(J.Y. Li, K.N. Wu, R.Jia, L.L. Hou, L. Gao, S.T. Li, Towards enhanced varistor property and lowerdielectric loss of CaCu3Ti4O12 based ceramics, Mater. Des. (2016) 92：546-551.)。而固相烧结法制备的Ca0.5Sr0.5Cu3Ti4O12陶瓷的击穿场强达到了24.52 kV/cm，但其介电常数1kHz下大幅度下降至1000以下 (Z. Tang, Y. Huang, K.N. Wu, J.Y. Li,Significantly enhanced breakdown field in Ca1-xSrxCu3Ti4O12 ceramics bytailoring donor densities, J. Eur. Ceram. Soc. (2018) 38：1569-1575. )。
然而，在实际应用中，电介质材料的击穿场强一般需要控制在10 kV/cm以上。过低的击穿场强必然会限制CCTO陶瓷的应用范围，严重制约CCTO 陶瓷的应用前景。因此，在保持高介电常数的同时，如何有效地提高击穿场强成为目前CCTO材料研究领域一个亟待解决的问题。
发明内容
针对上述现有CCTO产品击穿场强较低的技术问题，本发明提供了一种高击穿场强钛酸铜锶钙(CSCTO)介电陶瓷材料，并且提供了该CSCTO介电陶瓷的制备方法，可在保持介电常数仍处于较高水平时，显著提高CCTO陶瓷的击穿场强。
为达到以上目的，本发明是采取如下技术方案予以实现：
(1) 一种高击穿场强CSCTO巨介电陶瓷材料，其化学式为Ca1-xSrxCu3Ti4O12，其中0＜x＜1。优选的，0.3≤x≤0.6。更优选的，x=0.5。
(2) 上述CSCTO材料的制备步骤为：
A.CSCTO陶瓷前驱体粉末的制备。根据Ca1-xSrxCu3Ti4O12的化学计量比称取硝酸铜、硝酸钙、硝酸锶与柠檬酸等原料，倒入无水乙醇中，不断搅拌使原料充分溶解，形成A溶液。将钛酸四丁酯倒入无水乙醇中，不断搅拌使其充分溶解，形成B溶液。保持A溶液不断搅拌的同时，将B溶液缓慢倒入A溶液中，形成溶胶。将聚乙二醇加入到溶胶中，搅拌至完全溶解；把溶液放入恒温80 ℃的水浴锅中不断搅拌，加入氨水调节溶液的pH值为3~5，后使之形成凝胶。将凝胶放入到蒸发皿中，用电炉对其进行去除有机物处理，形成CSCTO陶瓷前驱体粉末；所述柠檬酸物质的量为硝酸铜、硝酸钙、硝酸锶和钛酸四丁酯中金属阳离子(Ca2+、Cu2+、Ti4 +，Sr2+)摩尔数之和。经试验测量，前述氨水调节溶液pH值下的CSCTO陶瓷具有最小损耗。柠檬酸的用量是经过大量实验总结出的，确保CSCTO陶瓷具有较高的击穿场强；柠檬酸不足或者过量均可导致CSCTO陶瓷击穿场强下降。
B. CSCTO陶瓷的制备。把前驱体粉末倒入玛瑙研钵中，并加入前驱体粉末3%质量的PVA粘合剂，充分研磨，过筛造粒，后放入干燥箱中干燥。称取制得的适量粉末放入模具中压片，制得CSCTO陶瓷胚体。陶瓷胚体放入马弗炉中，在1000~1100 ℃保温烧结。烧结结束后，在炉内自然冷却至室温。所述烧结温度既能使得晶粒开始均匀生长，又不会使得晶粒过度长大或者熔融。
本发明采用溶胶凝胶法制备与CCTO结构及性能相近的CSCTO介电陶瓷，制备方法操作简单、重复性好、成品率高，且所制备的CSCTO陶瓷的击穿场强可提高至11~52 kV/cm，同时室温下介电常数在1kHz时为3900~6200，具有高击穿场强与高介电常数的特点，综合性能优良，可以实现电容元器件的小型化，也可以用于过电压保护装置，在高压电容等领域具有广泛的应用前景。
附图说明
图1为不同配比的CSCTO介电陶瓷试样的XRD图；
图2为不同配比的CSCTO介电陶瓷试样的J-E曲线；
图3为不同配比的CSCTO介电陶瓷试样的介电常数频谱图；
图4为不同配比的CSCTO介电陶瓷试样的介电损耗频谱图。
具体实施方式
下面结合具体实施方式对本发明进一步说明。下述说明仅仅是实例性的，而不限制本发明的范围。
实施例1
根据Ca1-xSrxCu3Ti4O12中，x取值0.3，称取硝酸钙、硝酸锶、硝酸铜、柠檬酸分别为6.6790 g、2.5398 g、29.2848 g、67.5827 g，将其倒入装有300 ml无水乙醇的烧杯中，不断搅拌使其充分溶解，形成A液。用烧杯称取55.0012 g钛酸四丁酯，然后向此烧杯中加入100ml的无水乙醇，搅拌使其充分溶解，形成B液。在不断搅拌A液的同时，沿着玻璃棒缓慢加入B液，形成溶胶；待其混合均匀后，加入1.8 ml的聚乙二醇；然后把溶胶放到80 ℃的水浴锅中，保持搅拌棒150~200 rpm进行搅拌，形成凝胶。在此期间加入氨水调节溶液的pH值为3~5。把凝胶倒入蒸发皿中再放到电炉上保持300~400 ℃除去凝胶中的有机物；然后再放入到马弗炉中750 ℃高温预烧2 h，形成CSCTO陶瓷前驱体粉末。
把CSCTO陶瓷前驱体粉末放入玛瑙研钵中，并加入前驱体粉末3%质量的PVA粘合剂，研磨2~3 h，再把其过120目筛，最后将其放入120℃干燥箱中干燥10 min；称取3.2 g粉体放入模具中，用300 MPa压强压制成圆片。把压好的圆片放入马弗炉中内，先以2 ℃/min的升温速率上升到100 ℃保温10 min进行除湿干燥，然后以5 ℃/min的升温速率上升到600 ℃保温1 h进行排胶，最后以10 ℃/min的升温速率上升到1050 ℃保温12 h进行烧结。烧结结束后，在炉内自然冷却至室温，得到CSCTO陶瓷。
在烧结好的CSCTO陶瓷样品表面涂上银浆，然后在马弗炉内500℃保温0.5 h完成镀银，最后进行介电性能的测量。得到了高击穿场强CSCTO介电陶瓷材料，其击穿场强可提高至11.50 kV/cm，同时室温下介电常数在1kHz时为6200。如表1所示。
实施例2
根据Ca1-xSrxCu3Ti4O12中，x取值0.4，称取硝酸钙、硝酸锶、硝酸铜、柠檬酸分别为5.7248 g、3.3864 g、29.2848 g、67.5827 g，其他步骤与实施例1相同，得到高击穿场强CSCTO介电陶瓷材料，其击穿场强可提高至26.00 kV/cm，同时室温下介电常数在1kHz时为4892。如表1所示。
实施例3
根据Ca1-xSrxCu3Ti4O12中，x取值0.5，称取硝酸钙、硝酸锶、硝酸铜、柠檬酸分别为4.7707g、4.2330 g、29.2848 g、67.5827 g，其他步骤与实施例1相同，得到高击穿场强CSCTO介电陶瓷材料，其击穿场强可提高至52.50 kV/cm，同时室温下介电常数在1kHz时为3902。如表1所示。
实施例4
根据Ca1-xSrxCu3Ti4O12中，x取值0.6，称取硝酸钙、硝酸锶、硝酸铜、柠檬酸分别为3.8166g、5.0796 g、29.2848g、67.5827g，其他步骤与实施例1相同，得到高击穿场强CSCTO介电陶瓷材料，其击穿场强可提高至91.40 kV/cm，同时室温下介电常数在1kHz时为2045。如表1所示。
Figure 686088DEST_PATH_IMAGE001
。

Claims (1)

1.一种高击穿场强钛酸铜锶钙介电陶瓷材料的制备方法，用于制备一种高击穿场强钛酸铜锶钙介电陶瓷材料，其化学式为：Ca1-xSrxCu3Ti4O12，其中x=0.5；其特征在于，所述制备方法具体包括以下步骤：
（1）根据Ca1-xSrxCu3Ti4O12的化学计量比称取硝酸铜、硝酸钙、硝酸锶与柠檬酸原料，倒入无水乙醇中，不断搅拌使其充分溶解，形成A溶液；将钛酸四丁酯倒入无水乙醇中，不断搅拌使其溶解均匀，形成B溶液；保持A溶液不断搅拌的同时，将B溶液缓慢倒入A溶液中，形成溶胶；将聚乙二醇加入到溶胶中，搅拌至完全溶解；把溶液放入恒温水浴锅中不断搅拌，加入氨水调节溶液的pH值为3~5，使之形成凝胶；将凝胶放入到蒸发皿中，用电炉保持300~400℃对其进行去除有机物处理，再用马弗炉进行750 ℃高温预烧2 h，形成CSCTO陶瓷前驱体粉末；所述柠檬酸物质的量为硝酸铜、硝酸钙、硝酸锶和钛酸四丁酯中金属阳离子摩尔数之和；
（2）把前驱体粉末倒入玛瑙研钵中，并加入前驱体粉末3%质量的PVA粘合剂，充分研磨2~3 h，再把研磨产物过120目筛，最后将过筛后的粉体放入120℃干燥箱中干燥10 min；称取制得的适量粉末放入模具中用300 MPa压强压制成圆片，制得CSCTO陶瓷胚体；陶瓷胚体放入马弗炉中先以2 ℃/min的升温速率上升到100 ℃保温10 min进行除湿干燥，然后以5℃/min的升温速率上升到600 ℃保温1 h进行排胶，最后以10 ℃/min的升温速率上升到1050 ℃保温12 h进行烧结；在烧结结束后，在炉内自然冷却至室温，得到Ca1-xSrxCu3Ti4O12，x=0.5的介电陶瓷。
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