CN106631019A - 一种温度稳定型陶瓷介质材料及其制备方法 - Google Patents
一种温度稳定型陶瓷介质材料及其制备方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000003989 dielectric material Substances 0.000 title abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 42
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 31
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 229910000027 potassium carbonate Inorganic materials 0.000 claims abstract description 20
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims abstract description 19
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims description 23
- 238000010792 warming Methods 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 6
- 230000000977 initiatory effect Effects 0.000 claims description 6
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- 235000015320 potassium carbonate Nutrition 0.000 abstract 2
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- 238000011056 performance test Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- CZFMLDUNXATLOW-XKZIYDEJSA-N (5z)-5-[[3-(2-hydroxyethoxymethyl)thiophen-2-yl]methylidene]-10-methoxy-2,2,4-trimethyl-1h-chromeno[3,4-f]quinolin-9-ol Chemical class C1=CC=2NC(C)(C)C=C(C)C=2C2=C1C=1C(OC)=C(O)C=CC=1O\C2=C/C=1SC=CC=1COCCO CZFMLDUNXATLOW-XKZIYDEJSA-N 0.000 description 1
- QQGISFDJEJMKIL-JAIQZWGSSA-N (5z)-5-[[3-(hydroxymethyl)thiophen-2-yl]methylidene]-10-methoxy-2,2,4-trimethyl-1h-chromeno[3,4-f]quinolin-9-ol Chemical class C1=CC=2NC(C)(C)C=C(C)C=2C2=C1C=1C(OC)=C(O)C=CC=1O\C2=C/C=1SC=CC=1CO QQGISFDJEJMKIL-JAIQZWGSSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- SEGBQNJGOCXIGC-FHERZECASA-N benzyl n-[(2s)-1-[(4-hydroxyoxolan-3-yl)amino]-4-methyl-1-oxopentan-2-yl]carbamate Chemical class N([C@@H](CC(C)C)C(=O)NC1C(COC1)O)C(=O)OCC1=CC=CC=C1 SEGBQNJGOCXIGC-FHERZECASA-N 0.000 description 1
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Abstract
本发明公开一种温度稳定型陶瓷介质材料及其制备方法，主要化学组成是K2CO3‑SrCO3‑R2O3‑Ta2O5(R＝Pr、Ce)，K2CO3、SrCO3、R2O3和Ta2O5的摩尔比例为0.5：3：0.5：5，并掺入V2O5和CuO的混合物，混合物质量占原料总量的0.2‑0.5％。所述的制备方法包括将K2CO3等原料按摩尔比进行配料混合后按质量比加入V2O5和CuO混合物充分搅拌，通过球磨、烘干后预烧，然后进行造粒并烧结，即得。本发明提供的电容器介质材料具有优良的温度稳定性好，有效的增大了储能应用面积，具有良好的节能环保效应和广阔的应用前景。
Description
技术领域
本发明涉及电容器材料技术领域，具体涉及一种温度稳定型陶瓷介质材料及其制备方法。
背景技术
在高速发展的当今社会，人们对能源的需求日渐增多，而日益消耗的不可再生能源给整个人类的生存环境带来了巨大的压力，因此寻求并使用清洁能源便成为了环境对人类提出的新课题。近年来，随着科学技术的不断发展，太阳能、风能、热能以及核能都逐步被开发和使用，使得传统能源的占比显著降低。而另一方面，在新能源进行开发和挖掘的同时，能源的有效储存也随之成为了又一研究方向。
在能源转化过程中，可以通过将不同形式的能源转换为电能进行储存，这就意味着储能介质材料对环境的适应能力尤为重要。因此，如何增加介质材料的储能应用面积已达到最大程度的电能储存效率成为了当下亟待解决的问题。
发明内容
针对现有技术的不足，本发明提供了一种温度稳定型陶瓷介质材料及其制备方法。
为实现上述目的，本发明通过以下技术方案实现：
一种温度稳定型陶瓷介质材料，主要化学组成是K2CO3-SrCO3-R2O3-Ta2O5(R＝Pr、Ce)，K2CO3、SrCO3、R2O3和Ta2O5的摩尔比例为0.5：3：0.5：5，并掺入V2O5和CuO的混合物，混合物质量占原料总量的0.2-0.5％。
优选的，所述主要化学组成K2CO3、SrCO3、R2O3和Ta2O5的纯度大于99％。
优选的，所述混合物质量占原料总量的0.4％。
优选的，所述V2O5和CuO的质量比为1:3-1:5。
所述温度稳定型陶瓷介质材料的制备步骤如下：
1)将K2CO3、SrCO3、R2O3和Ta2O5为起始原料按摩尔比进行配料，混合后按质量比加入V2O5和CuO混合物充分搅拌，并加入无水乙醇混合球磨12-48小时，烘干得到粉末A；
2)将步骤1)中制得的粉末A放入马弗炉中，升温至1050～1200℃预烧4-10小时得到前驱体B；
3)将步骤2)中制得的前驱体B研碎后加入无水乙醇，球磨8-15小时混合均匀，烘干得到粉末C；
4)向步骤3)中制得的粉末C中加入5～10wt％聚乙烯醇水溶液造粒，过60目筛后压制成型，放入高温炉中升温至1250～1400℃烧结8-12小时后自然冷却至室温，即得。
优选的，所述步骤2)中预烧温度为1180℃，时间为4小时。
优选的，所述步骤4)中烧结温度为1300℃，时间为10小时。
本发明有益效果：本发明提供了一种温度稳定型陶瓷介质材料及其制备方法，原料各组分混合性较好，通过高温固相合成工艺，使得混合均匀后的原料在高温作用下可以得到KSr3RTa10O30(R＝Pr、Ce)。本发明提供的电容器介质材料在-50-200℃温度范围内具有优良的温度稳定性好，均满足电容变化率ΔC/C25≤±15％，有效的增加了电容器的工作范围，使其在多种温度情况下仍然可以发挥储能作用，有效的增大了储能应用面积，具有良好的节能环保效应。本发明提供的电容器介质材料及其制备方法，具有广阔的应用前景。
具体实施方式
实施例1：
一种温度稳定型陶瓷介质材料，主要化学组成是K2CO3-SrCO3-R2O3-Ta2O5(R＝Pr、Ce)，K2CO3、SrCO3、R2O3和Ta2O5的摩尔比例为0.5：3：0.5：5，并掺入V2O5和CuO的混合物，混合物质量占原料总量的0.4％。
其中，主要化学组成K2CO3、SrCO3、R2O3和Ta2O5的纯度大于99％。
其中，V2O5和CuO的质量比为1:3。
所述温度稳定型陶瓷介质材料的制备步骤如下：
1)将K2CO3、SrCO3、R2O3和Ta2O5为起始原料按摩尔比进行配料，混合后按质量比加入V2O5和CuO混合物充分搅拌，并加入无水乙醇混合球磨16小时，烘干得到粉末A；
2)将步骤1)中制得的粉末A放入马弗炉中，升温至1180℃预烧4小时得到前驱体B；
3)将步骤2)中制得的前驱体B研碎后加入无水乙醇，球磨11小时混合均匀，烘干得到粉末C；
4)向步骤3)中制得的粉末C中加入6wt％聚乙烯醇水溶液造粒，过60目筛后压制成型，放入高温炉中升温至1300℃烧结10小时后自然冷却至室温，即得。
通过以上实施例分别合成KSr3PrTa10O30和KSr3CeTa10O30，并在-50-200℃内进行介电性能测试，测试结果如表1：
表1
实施例2：
一种温度稳定型陶瓷介质材料，主要化学组成是K2CO3-SrCO3-R2O3-Ta2O5(R＝Pr、Ce)，K2CO3、SrCO3、R2O3和Ta2O5的摩尔比例为0.5：3：0.5：5，并掺入V2O5和CuO的混合物，混合物质量占原料总量的0.2％。
其中，主要化学组成K2CO3、SrCO3、R2O3和Ta2O5的纯度大于99％。
其中，V2O5和CuO的质量比为1:4。
所述温度稳定型陶瓷介质材料的制备步骤如下：
1)将K2CO3、SrCO3、R2O3和Ta2O5为起始原料按摩尔比进行配料，混合后按质量比加入V2O5和CuO混合物充分搅拌，并加入无水乙醇混合球磨12小时，烘干得到粉末A；
2)将步骤1)中制得的粉末A放入马弗炉中，升温至1050℃预烧10小时得到前驱体B；
3)将步骤2)中制得的前驱体B研碎后加入无水乙醇，球磨8小时混合均匀，烘干得到粉末C；
4)向步骤3)中制得的粉末C中加入5wt％聚乙烯醇水溶液造粒，过60目筛后压制成型，放入高温炉中升温至1400℃烧结8小时后自然冷却至室温，即得。
通过以上实施例分别合成KSr3PrTa10O30和KSr3CeTa10O30，并在-50-200℃内进行介电性能测试，测试结果如表2：
表2
实施例3：
一种温度稳定型陶瓷介质材料，主要化学组成是K2CO3-SrCO3-R2O3-Ta2O5(R＝Pr、Ce)，K2CO3、SrCO3、R2O3和Ta2O5的摩尔比例为0.5：3：0.5：5，并掺入V2O5和CuO的混合物，混合物质量占原料总量的0.3％。
其中，主要化学组成K2CO3、SrCO3、R2O3和Ta2O5的纯度大于99％。
其中，V2O5和CuO的质量比为1:5。
所述温度稳定型陶瓷介质材料的制备步骤如下：
1)将K2CO3、SrCO3、R2O3和Ta2O5为起始原料按摩尔比进行配料，混合后按质量比加入V2O5和CuO混合物充分搅拌，并加入无水乙醇混合球磨30小时，烘干得到粉末A；
2)将步骤1)中制得的粉末A放入马弗炉中，升温至1100℃预烧8小时得到前驱体B；
3)将步骤2)中制得的前驱体B研碎后加入无水乙醇，球磨13小时混合均匀，烘干得到粉末C；
4)向步骤3)中制得的粉末C中加入8wt％聚乙烯醇水溶液造粒，过60目筛后压制成型，放入高温炉中升温至1250℃烧结9小时后自然冷却至室温，即得。
通过以上实施例分别合成KSr3PrTa10O30和KSr3CeTa10O30，并在-50-200℃内进行介电性能测试，测试结果如表3：
表3
实施例4：
一种温度稳定型陶瓷介质材料，主要化学组成是K2CO3-SrCO3-R2O3-Ta2O5(R＝Pr、Ce)，K2CO3、SrCO3、R2O3和Ta2O5的摩尔比例为0.5：3：0.5：5，并掺入V2O5和CuO的混合物，混合物质量占原料总量的0.5％。
其中，主要化学组成K2CO3、SrCO3、R2O3和Ta2O5的纯度大于99％。
其中，V2O5和CuO的质量比为1:3。
所述温度稳定型陶瓷介质材料的制备步骤如下：
1)将K2CO3、SrCO3、R2O3和Ta2O5为起始原料按摩尔比进行配料，混合后按质量比加入V2O5和CuO混合物充分搅拌，并加入无水乙醇混合球磨48小时，烘干得到粉末A；
2)将步骤1)中制得的粉末A放入马弗炉中，升温至1200℃预烧6小时得到前驱体B；
3)将步骤2)中制得的前驱体B研碎后加入无水乙醇，球磨15小时混合均匀，烘干得到粉末C；
4)向步骤3)中制得的粉末C中加入10wt％聚乙烯醇水溶液造粒，过60目筛后压制成型，放入高温炉中升温至1350℃烧结12小时后自然冷却至室温，即得。
通过以上实施例分别合成KSr3PrTa10O30和KSr3CeTa10O30，并在-50-200℃内进行介电性能测试，测试结果如表4：
表4
当然，上面只是本发明优选的具体实施方式作了详细描述，并非以此限制本发明的实施范围，凡依本发明的原理、构造以及结构所作的等效变化，均应涵盖于本发明的保护范围内。
Claims (7)
1.一种温度稳定型陶瓷介质材料，其特征在于，主要化学组成是K2CO3-SrCO3-R2O3-Ta2O5(R＝Pr、Ce)，K2CO3、SrCO3、R2O3和Ta2O5的摩尔比例为0.5：3：0.5：5，并掺入V2O5和CuO的混合物，混合物质量占原料总量的0.2-0.5％。
2.根据权利要求1所述温度稳定型陶瓷介质材料，其特征在于，所述主要化学组成K2CO3、SrCO3、R2O3和Ta2O5的纯度大于99％。
3.根据权利要求1所述温度稳定型陶瓷介质材料，其特征在于，所述混合物质量占原料总量的0.4％。
4.根据权利要求1所述温度稳定型陶瓷介质材料，其特征在于，所述V2O5和CuO的质量比为1:3-1:5。
5.根据权利要求1-4任一所述温度稳定型陶瓷介质材料的制备方法，其特征在于，步骤如下：
1)将K2CO3、SrCO3、R2O3和Ta2O5为起始原料按摩尔比进行配料，混合后按质量比加入V2O5和CuO混合物充分搅拌，并加入无水乙醇混合球磨12-48小时，烘干得到粉末A；
2)将步骤1)中制得的粉末A放入马弗炉中，升温至1050～1200℃预烧4-10小时得到前驱体B；
3)将步骤2)中制得的前驱体B研碎后加入无水乙醇，球磨8-15小时混合均匀，烘干得到粉末C；
4)向步骤3)中制得的粉末C中加入5～10wt％聚乙烯醇水溶液造粒，过60目筛后压制成型，放入高温炉中升温至1250～1400℃烧结8-12小时后自然冷却至室温，即得。
6.根据权利要求5所述温度稳定型陶瓷介质材料的制备方法，其特征在于，所述步骤2)中预烧温度为1180℃，时间为4小时。
7.根据权利要求5所述温度稳定型陶瓷介质材料的制备方法，其特征在于，所述步骤4)中烧结温度为1300℃，时间为10小时。
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