CN106554201A - 一种无铅高压陶瓷电容器材料 - Google Patents
一种无铅高压陶瓷电容器材料 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 40
- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 25
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 36
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000654 additive Substances 0.000 claims abstract description 23
- 230000000996 additive effect Effects 0.000 claims abstract description 23
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 14
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 9
- VKJLWXGJGDEGSO-UHFFFAOYSA-N barium(2+);oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[Ti+4].[Ba+2] VKJLWXGJGDEGSO-UHFFFAOYSA-N 0.000 claims abstract description 9
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 229960000892 attapulgite Drugs 0.000 claims description 11
- 229910052625 palygorskite Inorganic materials 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 229940125904 compound 1 Drugs 0.000 claims description 9
- 229940125782 compound 2 Drugs 0.000 claims description 9
- 239000004115 Sodium Silicate Substances 0.000 claims description 8
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 8
- 239000011656 manganese carbonate Substances 0.000 claims description 8
- 229940093474 manganese carbonate Drugs 0.000 claims description 8
- 235000006748 manganese carbonate Nutrition 0.000 claims description 8
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 8
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 6
- 239000011976 maleic acid Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 6
- PVGBHEUCHKGFQP-UHFFFAOYSA-N sodium;n-[5-amino-2-(4-aminophenyl)sulfonylphenyl]sulfonylacetamide Chemical compound [Na+].CC(=O)NS(=O)(=O)C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 PVGBHEUCHKGFQP-UHFFFAOYSA-N 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229940126214 compound 3 Drugs 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229960004756 ethanol Drugs 0.000 claims description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 3
- 238000003837 high-temperature calcination Methods 0.000 claims description 3
- 239000003595 mist Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052573 porcelain Inorganic materials 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims 2
- 229940068984 polyvinyl alcohol Drugs 0.000 claims 2
- VDGJOQCBCPGFFD-UHFFFAOYSA-N oxygen(2-) silicon(4+) titanium(4+) Chemical compound [Si+4].[O-2].[O-2].[Ti+4] VDGJOQCBCPGFFD-UHFFFAOYSA-N 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 8
- 239000003990 capacitor Substances 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000009472 formulation Methods 0.000 abstract description 2
- 229910052727 yttrium Inorganic materials 0.000 abstract description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229940088417 precipitated calcium carbonate Drugs 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—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
- C04B35/46—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 titanium oxides or titanates
- C04B35/462—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 titanium oxides or titanates based on titanates
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
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Abstract
发明公开了一种无铅高压陶瓷电容器材料，其特征在于，由以下成分制成：钛酸钡、二氧化钛、碳酸钙、二氧化锆、二氧化硅、改性添加料。与现有技术相比，对陶瓷电容材料的配方和制备工艺进行了优化改进，配方不含铅元素及稀有金属元素，绿色环保，成本低，通过添加了改性添加料极大的改善陶瓷材料的性能，大大提高陶瓷材料的介电常数与耐压值，并能达到较小的温度变化率，使电容器在工作过程中性能更加稳定。
Description
技术领域
本发明涉及电容器材料领域，特别是涉及一种无铅高压陶瓷电容器材料。
背景技术
目前广泛生产使用的高压陶瓷电容器材料中往往含有大量的铅，铅是一种强污染物范围的元素，它具有不可降解性，对人体和环境都会造成长期持久的伤害。且同时一般配方的无铅陶瓷电容器材料的介电常数较小，不能满足电子线路小型化的需求，且耐压值不够高。
发明内容
本发明的目的是提供一种无铅高压陶瓷电容器材料。
本发明通过以下技术方案实现：
一种无铅高压陶瓷电容器材料，按重量份由以下成分制成：钛酸钡78-84、二氧化钛15-18、碳酸钙4-6、二氧化锆3-5、二氧化硅4-7、改性添加料2-4；所述改性添加料按重量份计由以下成分制成：氧化铝6、二氧化锡4、硅酸钠2、碳酸锰1、凹凸棒土4。
进一步的，所述碳酸钙为轻质碳酸钙，并且所述碳酸钙经过265-270℃高温煅烧15min。
进一步的，所述二氧化硅经过预处理：将乙烯基三甲氧基硅烷与乙醇按3:85质量比例混合后得到混合溶液，将二氧化硅添加到混合溶液中浸泡8-10h，然后过滤，表面烘干，即可。
进一步的，所述改性添加料的制备方法为：①按重量份将6份氧化铝、4份二氧化锡与2份的凹凸棒土均匀混合到一起，得到混合料1，对混合料1加热至220-230℃，并加压至0.35MPa，保温保压15min后，添加混合料1质量20%的无水乙醇，搅拌均匀后进行研磨，研磨35min后除去无水乙醇，静置待用；②按重量份将2份硅酸钠、1份碳酸锰与2份的凹凸棒土均匀混合到一起，得到混合料2，对混合料2加热至132-135℃，并加压至0.6MPa，保温保压25min后，添加混合料2质量25%的异丙醇，搅拌均匀后进行研磨，研磨30min后除去异丙醇；
③将混合料1与混合料2均匀混合到一起，得到混合料3，添加混合料3质量2%的马来酸溶液，以250r/min转速搅拌20min后，再进行研磨，研磨40min后，除去马来酸溶液，然后进行干燥，即可。
进一步的，所述无铅高压陶瓷电容器材料的制备方法为：将钛酸钡、二氧化钛、碳酸钙、二氧化锆、二氧化硅、改性添加料按各自重量份均匀混合后得混合料，于820~920℃温度下第一次烧结，对混合料进行第一次球磨并烘干，然后于1120~1220℃温度下第二次烧结，接着进行第二次球磨，最后加入聚乙烯醇进行喷雾造粒形成粉体材料，将粉体材料干压成型后于1420~1450℃的温度下烧结，得无铅高压陶瓷电容器材料。
进一步的，聚乙烯醇的添加料为混合料质量的1.5%。
本发明的有益效果是：与现有技术相比，对陶瓷电容材料的配方和制备工艺进行了优化改进，配方不含铅元素及稀有金属元素，绿色环保，成本低，通过添加了改性添加料极大的改善陶瓷材料的性能，大大提高陶瓷材料的介电常数与耐压值，并能达到较小的温度变化率，使电容器在工作过程中性能更加稳定，并且还极大的降低了介质损耗；通过改性添加料与经过煅烧后的碳酸钙的协同作用，改善了陶瓷材料的温度特性，使得其晶粒尺寸均匀，进而提高了陶瓷材料的稳定性；通过本发明中改性添加料与其它成分的协同配合作用，制备的陶瓷材料，耐压强度提高到18.5KV/mm以上，介电常数达到4200±15，在频率为1±0.1KHz，交流有效值1±0.1V的范围内测试，介质损耗为19.5×10-4左右。
具体实施方式
实施例1
一种无铅高压陶瓷电容器材料，其特征在于，按重量份由以下成分制成：钛酸钡78、二氧化钛15、碳酸钙4、二氧化锆3、二氧化硅4、改性添加料2；所述改性添加料按重量份计由以下成分制成：氧化铝6、二氧化锡4、硅酸钠2、碳酸锰1、凹凸棒土4。
实施例2
一种无铅高压陶瓷电容器材料，其特征在于，按重量份由以下成分制成：钛酸钡84、二氧化钛18、碳酸钙6、二氧化锆5、二氧化硅7、改性添加料4；所述改性添加料按重量份计由以下成分制成：氧化铝6、二氧化锡4、硅酸钠2、碳酸锰1、凹凸棒土4。
实施例3
一种无铅高压陶瓷电容器材料，其特征在于，按重量份由以下成分制成：钛酸钡80、二氧化钛17、碳酸钙5、二氧化锆4、二氧化硅5、改性添加料3；所述改性添加料按重量份计由以下成分制成：氧化铝6、二氧化锡4、硅酸钠2、碳酸锰1、凹凸棒土4。
本发明实施例中：
进一步的，所述碳酸钙为轻质碳酸钙，并且所述碳酸钙经过265-270℃高温煅烧15min。
进一步的，所述二氧化硅经过预处理：将乙烯基三甲氧基硅烷与乙醇按3:85质量比例混合后得到混合溶液，将二氧化硅添加到混合溶液中浸泡8-10h，然后过滤，表面烘干，即可。
进一步的，所述改性添加料的制备方法为：①按重量份将6份氧化铝、4份二氧化锡与2份的凹凸棒土均匀混合到一起，得到混合料1，对混合料1加热至220-230℃，并加压至0.35MPa，保温保压15min后，添加混合料1质量20%的无水乙醇，搅拌均匀后进行研磨，研磨35min后除去无水乙醇，静置待用；②按重量份将2份硅酸钠、1份碳酸锰与2份的凹凸棒土均匀混合到一起，得到混合料2，对混合料2加热至132-135℃，并加压至0.6MPa，保温保压25min后，添加混合料2质量25%的异丙醇，搅拌均匀后进行研磨，研磨30min后除去异丙醇；
③将混合料1与混合料2均匀混合到一起，得到混合料3，添加混合料3质量2%的马来酸溶液，以250r/min转速搅拌20min后，再进行研磨，研磨40min后，除去马来酸溶液，然后进行干燥，即可。
进一步的，所述无铅高压陶瓷电容器材料的制备方法为：将钛酸钡、二氧化钛、碳酸钙、二氧化锆、二氧化硅、改性添加料按各自重量份均匀混合后得混合料，于820~920℃温度下第一次烧结，对混合料进行第一次球磨并烘干，然后于1120~1220℃温度下第二次烧结，接着进行第二次球磨，最后加入聚乙烯醇进行喷雾造粒形成粉体材料，将粉体材料干压成型后于1420~1450℃的温度下烧结，得无铅高压陶瓷电容器材料。
进一步的，聚乙烯醇的添加料为混合料质量的1.5%。
陶瓷电容器材料性能：
表1
| 耐压强度/KV/mm | 介电常数 | 介质损耗 | |
| 实施例1 | 18.6 | 4185 | 19.5×10-4 |
| 实施例2 | 18.8 | 4215 | 19.2×10-4 |
| 实施例3 | 18.7 | 4200 | 19.3×10-4 |
| 对比例1 | 11.8 | 3210 | 28.5×10-4 |
| 对比例2 | 16.5 | 3840 | 22.1×10-4 |
其中，对比例1为：将实施例2中添加料制备成分不变，不经过处理，直接添加到陶瓷材料制备中，其它成分与处理方法不变；
对比例2为：将实施例2中碳酸钙不经过煅烧处理，其它成分与处理方法不变。
由表1可知，采用不经过改性处理的添加料会极大的降低本发明陶瓷电容器材料的性能，不对碳酸钙进行煅烧处理会一定程度上降低本发明陶瓷电容器材料的性能。
本发明陶瓷电容器材料的使用寿命相较于普通陶瓷电容器材料的使用寿命提高了2-3倍。
Claims (6)
1.一种无铅高压陶瓷电容器材料，其特征在于，按重量份由以下成分制成：钛酸钡78-84、二氧化钛15-18、碳酸钙4-6、二氧化锆3-5、二氧化硅4-7、改性添加料2-4；所述改性添加料按重量份计由以下成分制成：氧化铝6、二氧化锡4、硅酸钠2、碳酸锰1、凹凸棒土4。
2.根据权利要求1所述的一种无铅高压陶瓷电容器材料，其特征在于，所述碳酸钙为轻质碳酸钙，并且所述碳酸钙经过265-270℃高温煅烧15min。
3.根据权利要求1所述的一种无铅高压陶瓷电容器材料，其特征在于，所述二氧化硅经过预处理：将乙烯基三甲氧基硅烷与乙醇按3:85质量比例混合后得到混合溶液，将二氧化硅添加到混合溶液中浸泡8-10h，然后过滤，表面烘干，即可。
4.根据权利要求1所述的一种无铅高压陶瓷电容器材料，其特征在于，所述改性添加料的制备方法为：①按重量份将6份氧化铝、4份二氧化锡与2份的凹凸棒土均匀混合到一起，得到混合料1，对混合料1加热至220-230℃，并加压至0.35MPa，保温保压15min后，添加混合料1质量20%的无水乙醇，搅拌均匀后进行研磨，研磨35min后除去无水乙醇，静置待用；②按重量份将2份硅酸钠、1份碳酸锰与2份的凹凸棒土均匀混合到一起，得到混合料2，对混合料2加热至132-135℃，并加压至0.6MPa，保温保压25min后，添加混合料2质量25%的异丙醇，搅拌均匀后进行研磨，研磨30min后除去异丙醇；
③将混合料1与混合料2均匀混合到一起，得到混合料3，添加混合料3质量2%的马来酸溶液，以250r/min转速搅拌20min后，再进行研磨，研磨40min后，除去马来酸溶液，然后进行干燥，即可。
5.根据权利要求1所述的一种无铅高压陶瓷电容器材料，其特征在于，所述无铅高压陶瓷电容器材料的制备方法为：将钛酸钡、二氧化钛、碳酸钙、二氧化锆、二氧化硅、改性添加料按各自重量份均匀混合后得混合料，于820~920℃温度下第一次烧结，对混合料进行第一次球磨并烘干，然后于1120~1220℃温度下第二次烧结，接着进行第二次球磨，最后加入聚乙烯醇进行喷雾造粒形成粉体材料，将粉体材料干压成型后于1420~1450℃的温度下烧结，得无铅高压陶瓷电容器材料。
6.根据权利要求4所述的一种无铅高压陶瓷电容器材料，其特征在于，聚乙烯醇的添加料为混合料质量的1.5%。
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