CN106565240A - 一种铁基陶瓷电容器材料及其制备方法 - Google Patents
一种铁基陶瓷电容器材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 32
- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 25
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 9
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 8
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 10
- 229910052721 tungsten Inorganic materials 0.000 claims description 7
- 239000010937 tungsten Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 230000000977 initiatory effect Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 150000002085 enols Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000003746 solid phase reaction Methods 0.000 abstract 1
- 239000010955 niobium Substances 0.000 description 12
- 239000000919 ceramic Substances 0.000 description 6
- 229910010293 ceramic material Inorganic materials 0.000 description 6
- 239000003990 capacitor Substances 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- -1 tungsten bronze series compound Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910000906 Bronze Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 230000010365 information processing Effects 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 230000005616 pyroelectricity Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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Abstract
本发明公开了一种铁基陶瓷电容器材料及其制备方法。将BaCO3、Nb2O5、Fe2O3和Pr2O3预先球磨，细化原料，根据化学计量比Ba4PrFe0.5Nb9.5O30进行配料，经过预烧、二次球磨等工序，利用固相反应制备得到陶瓷电容器材料Ba4PrFe0.5Nb9.5O30。本发明方法可获得性能优良的陶瓷电容器材料，在‑160℃～200℃其介电性能稳定；本发明方法简单，节能减排，成本适中，适合批量生产。
Description
技术领域
本发明涉及一种铁基陶瓷电容器材料Ba4PrFe0.5Nb9.5O30及其制备方法，属于电子元器件的陶瓷材料技术领域。
背景技术
陶瓷电容器是电子信息技术的重要基础器件，随着电子器件的飞速发展，要求陶瓷电容器材料能够更多元化。大多数陶瓷电容器基于钙钛矿结构，本发明采用钨青铜结构，有助于扩展电容器陶瓷的材料类型。目前对于钨青铜的研究和报道还是相对较少的，因此对钨青铜系列化合物的研究和应用,将具有十分良好的应用前景。钨青铜系列化合物亦可像钙钛矿结构化合物在铁电、压电、热释电、非线性光学等方面具有独特而优异的性能，在激光倍频、电光调制、光学信息处理、超导、湿度传感器、固体燃料电池等技术领域都有应用。
发明内容
1.本发明的目的是提供一种铁基陶瓷电容器材料及其制备方法。
2.本发明提供材料的化学组成式为Ba4PrFe0.5Nb9.5O30。
3.上述温度稳定型铁基陶瓷电容器材料的制备方法具体步骤为：
(1)将纯度大于99.9％的BaCO3，Pr2O3，Nb2O5和Fe2O3为起始原料，按照BaCO3：Pr2O3：Fe2O3：Nb2O5＝4:0.5：0.25:4.75的摩尔比进行配料，加入无水乙醇中，混合球磨8小时，烘干制得混合均匀的粉料；
(2)把按照步骤(1)制得的粉料样品在1250℃预烧结4小时，制得预烧后的粉体；
(3)将步骤(2)预烧后的粉体，在无水乙醇中球磨4小时混合均匀，烘干；加入7wt％聚乙烯醇水溶液进行造粒，过60目筛后压制成型，然后置于高温炉空气气氛中，在1300℃烧结10小时后自然冷却至室温，得到所述新型陶瓷电容器材料Ba4PrFe0.5Nb9.5O30；
所述的聚乙烯醇水溶液的浓度为7wt％。
4.本发明提供的新型陶瓷电容器材料及其制备方法，采用钨青铜结构，有助于扩展电容器陶瓷的材料类型。本发明采用传统的固相法制备陶瓷材料，在中温下烧结即可获得性能较为优良的新型陶瓷材料，且工艺简单，成本低廉，对环境无害。在我国，介质陶瓷材料正处在不断发展之中，所以寻找出新型结构的制备方法，扩展电容器陶瓷的材料类型是目前时代所需。因而，本发明所提供的陶瓷电容器介质材料及其制备方法，具有良好的产业化前景。
附图说明
1.图1为Ba4PrFe0.5Nb9.5O30陶瓷样品的X射线图谱；
2.图2为Ba4PrFe0.5Nb9.5O30陶瓷电容器材料的表面显微形貌照片；
3.图3为Ba4PrFe0.5Nb9.5O30陶瓷电容器材料的常温频谱图；
4.图4表示Ba4PrFe0.5Nb9.5O30陶瓷电容器材料的介电常数和损耗随温度的变化。
具体实施方式
将五氧化二铌、碳酸钡、三氧化二铁和三氧化二镨原料按化学计量比为Ba4PrFe0.5Nb9.5O30配料放入球磨罐中；选择氧化锆球和尼龙罐；所加粉体质量为磨球质量的8％；球磨时间为10个小时，转速为350转/分钟，球磨介质为无水乙醇。所得产物置于100℃的烘箱中烘干5小时，先以5℃/分的升温速率升至1250℃预烧4小时；取出预烧后的粉体研碎，再次球磨4小时，烘干后研磨成粉状，用质量百分浓度为7％的聚乙醇水溶液(PVA)作为有机粘结剂造粒，均匀混合后，过60目的筛子后在100MPa压强下压成直径为12mm，厚度为1mm的圆片状生坯，将圆片状生坯以1.5℃/分的升温速率升至550℃，保温4小时排出胶体再以5℃/分的升温速率升至1300℃，保温10小时，随炉自然冷却至室温。得到铁基陶瓷材料Ba4PrFe0.5Nb9.5O30。
图1为样品的X射线衍射谱图，图2为样品的表面微观形貌，X射线衍射谱图以及表面微观形貌均表明了Ba4PrFe0.5Nb9.5O30为未填满型钨青铜结构。
将本实施例制得的陶瓷电容器材料两侧均烧上银电极，制成圆片电容器，然后测试并计算该陶瓷电容器材料的介电性能。附图3给出了该介电陶瓷电容器材料的介电常数和损耗随频率变化的关系。附图4给出了Ba4PrFe0.5Nb9.5O30陶瓷电容器材料的介电常数和损耗随温度的变化，表明Ba4PrFe0.5Nb9.5O30陶瓷材料在-160℃～200℃介电常数保持在470-510，损耗低于0.1，进一步证明其可作为陶瓷电容器材料。
Claims (2)
1.一种铁基陶瓷电容器材料，其特征在于所述陶瓷电容器材料的化学组成式为Ba4PrFe0.5Nb9.5O30；
所述陶瓷电容器材料的结构为未填满型钨青铜结构，且在-160℃～200℃之间的介电常数保持在470-510，损耗低于0.1。
2.一种制备根据权利要求1所述的陶瓷电容器材料的制备方法，包括以下具体步骤：
(1)将纯度大于99.9％的BaCO3，Pr2O3，Nb2O5和Fe2O3为起始原料，按照BaCO3：Pr2O3：Fe2O3：Nb2O5＝4:0.5：0.25:4.75的摩尔比进行配料，加入无水乙醇中，混合球磨8小时，烘干制得混合均匀的粉料；
(2)把按照步骤(1)制得的粉料在1250℃预烧结4小时，制得预烧后的粉体；
(3)将步骤(2)预烧后的粉体，在无水乙醇中球磨4小时混合均匀，烘干；加入7wt％聚乙烯醇水溶液进行造粒，过60目筛后压制成型，然后置于高温炉空气气氛中，在1300℃烧结10小时后自然冷却至室温，得到所述铁基陶瓷电容器材料Ba4PrFe0.5Nb9.5O30。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108218423A (zh) * | 2018-01-11 | 2018-06-29 | 桂林理工大学 | 一种x8r型陶瓷电容器介质材料及其制备方法 |
| CN110511026A (zh) * | 2019-07-24 | 2019-11-29 | 桂林理工大学 | 一种x8r型陶瓷电容器介质材料及其制备方法 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926300A (zh) * | 2015-04-20 | 2015-09-23 | 桂林理工大学 | 温度稳定型电容器Sr4SmTiNb9O30陶瓷及其制备方法 |
| CN105884352A (zh) * | 2016-04-12 | 2016-08-24 | 桂林理工大学 | 一种新型陶瓷电容器材料Ba4RFe0.5Nb9.5O30（R=La，Eu，Gd）及其制备方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104926300A (zh) * | 2015-04-20 | 2015-09-23 | 桂林理工大学 | 温度稳定型电容器Sr4SmTiNb9O30陶瓷及其制备方法 |
| CN105884352A (zh) * | 2016-04-12 | 2016-08-24 | 桂林理工大学 | 一种新型陶瓷电容器材料Ba4RFe0.5Nb9.5O30（R=La，Eu，Gd）及其制备方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108218423A (zh) * | 2018-01-11 | 2018-06-29 | 桂林理工大学 | 一种x8r型陶瓷电容器介质材料及其制备方法 |
| CN110511026A (zh) * | 2019-07-24 | 2019-11-29 | 桂林理工大学 | 一种x8r型陶瓷电容器介质材料及其制备方法 |
| CN110511026B (zh) * | 2019-07-24 | 2022-01-04 | 桂林理工大学 | 一种x8r型陶瓷电容器介质材料及其制备方法 |
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