CN105967681B - 一种抗还原x9r型介质陶瓷材料 - Google Patents
一种抗还原x9r型介质陶瓷材料 Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 25
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 229910052689 Holmium Inorganic materials 0.000 claims abstract description 6
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 5
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 4
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 4
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000000498 ball milling Methods 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 13
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 239000004615 ingredient Substances 0.000 claims description 12
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910020489 SiO3 Inorganic materials 0.000 claims description 3
- 229910002113 barium titanate Inorganic materials 0.000 claims description 3
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 3
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- 239000011656 manganese carbonate Substances 0.000 claims description 3
- 229940093474 manganese carbonate Drugs 0.000 claims description 3
- 235000006748 manganese carbonate Nutrition 0.000 claims description 3
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 3
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 239000003985 ceramic capacitor Substances 0.000 abstract description 8
- 239000003814 drug Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
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Abstract
一种抗还原X9R型介质陶瓷材料，包括主材料和烧结助剂,所述主材料的化学通式为:(Bix1Mx1Nx2Ba1‑x1‑x2)(Mny1Mgy2Ny3Ti1‑y1‑y2‑y3)O3；所述主材料通式中的Ｍ为选自Li、Na和K中的一种；所述主材料通式中的Ｎ为选自Y、Dy、Ho和Er中的一种；其中,0.02＜x1＜0.10，0＜x2＜0.01，0.001＜y1＜0.01，0.003＜y2＜0.01,0＜y3＜0.01；所述烧结助剂的化学通式为:BazCa1‑zSiO3,其中0.4＜z＜0.6；所述烧结助剂与主材料的重量份配比为：1‑5：100。本发明有益效果是：本发明所述的X9R型介质陶瓷材料既满足X9R温度特性，又能在还原气氛烧结后得到高的电阻率，可以应用于制备镍电极X9R陶瓷电容器。
Description
技术领域
本发明涉及介质陶瓷材料，具体涉及一种抗还原X9R型介质陶瓷材料。
背景技术
在航空航天、勘探及军工等承受大温度差的应用中，对于能承受大温差的电子元器件有很大的需求。目前国际通行的标准为美国电子工业协会EIA标准，根据EIA标准，X9R是指从-55℃到+200℃的温度变化范围内，电容器容量相对25℃室温容量的变化率不超过15%。
在多层陶瓷电容器制造工业中，为了节省成本，绝大部分多层陶瓷电容器使用镍电极代替银-钯等贵金属电极。镍电极在烧结时需要还原气氛保护，以防止镍电极被氧化，因此要求介质陶瓷材料须具有抗还原的特性。
现已公开关于X9R的专利，均为在空气或氧化气氛中烧结的介质陶瓷材料，无法制备镍电极X9R型多层陶瓷电容器。本发明提供一种抗还原X9R型介质陶瓷材料，能在还原气氛中烧结而不被还原，从而能制备镍电极X9R型多层陶瓷电容器。
发明内容
本发明解决的技术问题在于提供一种抗还原X9R型介质陶瓷材料，从而能用于制备镍电极X9R型多层陶瓷电容器。
本发明解决的技术问题可以采用以下技术方案来实现：一种抗还原X9R型介质陶瓷材料，包括原材料和烧结助剂,所述主材料的化学通式为:
(Bix1Mx1Nx2Ba1-x1-x2)(Mny1Mgy2Ny3Ti1-y1-y2-y3)O3；
所述主材料通式中的Ｍ为选自Li、Na和K中的一种；
所述主材料通式中的Ｎ为选自Y、Dy、Ho和Er中的一种；
其中,0.02＜x1＜0.10，0＜x2＜0.01，0.001＜y1＜ 0.01，
0.003＜y2＜ 0.01, 0＜y3＜ 0.01；
所述烧结助剂的化学通式为:BazCa1-zSi O3,其中0.4＜z＜0.6；
所述烧结助剂与主材料的重量份配比为：1-5：100。
所述的一种抗还原X9R型介质陶瓷材料的制备方法，包括以下制备步骤：
a、主材料制备：选取分析纯钛酸钡、二氧化钛、氧化铋、碳酸钠、碳酸锰、氧化镁和氧化钬，按参数比例配料后加入乙醇，球磨3.5-4.5小时后，放入煅烧炉中煅烧1.5-2.5小时，煅烧温度为860℃-920℃，然后再加乙醇球磨1.5-2.5小时并烘干制得原料备用；
b、烧结助剂制备：选取分析纯碳酸钙、碳酸钡和二氧化硅，按Ba0.6Ca0.4SiO3的比例配料，加入纯水球磨7.5-8.5小时后，放入煅烧炉中煅烧1.5-2.5小时，煅烧温度为960-1100℃，然后加入乙醇球磨3.5-4.5小时并烘干制得烧结助剂备用；
c、按照烧结助剂和主材料成分的比例为2:100配料，加入乙醇球磨0.5-1.5小时并烘干，加入PVA造粒并压成φ10*2mm小圆片,在小圆片两边涂覆镍浆，于1300℃、氧分压为10-11Pa的还原气氛炉中烧结1.5-2.5小时，然后再于900℃、氧分压为10Pa的环境退火5小时，制得抗还原X9R型介质陶瓷材料；
d、测试该X9R 型介质陶瓷材料的介电性能。
本发明有益效果是：本发明所述的X9R型介质陶瓷材料既满足X9R温度特性，又能在还原气氛烧结后得到高的电阻率，可以应用于制备镍电极X9R陶瓷电容器。
具体实施方式
为了进一步理解本发明，下面结合实施例对本发明优选实施方案进行描述，但是应当理解，这些描述只是为进一步说明本发明的特征和优点，而不是对本发明权利要求的限制。
本发明提供的抗还原X9R型介质陶瓷材料，包括原材料和烧结助剂。所述主材料的化学通式为:
(Bix1Mx1Nx2Ba1-x1-x2)(Mny1Mgy2Ny3Ti1-y1-y2-y3)O3；
本发明对主材料的合成方法没有特殊限制，本领域技术人员可根据自身熟悉程度情况进行选择，可优选固相合成法。本发明对主成分的颗粒大小没有特殊限制，可优选为0.2-0.5微米。
本发明对烧结助剂的合成方法没有特殊限制，本领域技术人员可根据自身熟悉程度情况进行选择，可优选固相合成法。本发明对烧结助剂的颗粒大小没有特殊限制，可优选为0.2-0.5微米。
上述主材料通式中，M为具有+1价离子的物质，优选为以下物质的一种：Li、Na、K，更优选为Na；
上述主材料通式中，N为离子半径范围在0.087-0.094纳米的物质，从而既可以占据钙钛矿结构中的A位，也可占据钙钛矿结构中的B位，优选为以下物质的一种：Y、Dy、Ho、Er，更优选为Ho、Y；
为了进一步理解本发明，下面结合实施例对本发明提供的抗还原X9R型介质陶瓷材料进行说明，本发明的保护范围不受以下实施例的限制。
a、主材料制备：选取分析纯钛酸钡、二氧化钛、氧化铋、碳酸钠、碳酸锰、氧化镁和氧化钬，按表1参数比例配料后加入乙醇，球磨4小时后，放入煅烧炉中煅烧2小时，煅烧温度为900℃，然后再加乙醇球磨2小时并烘干制得原料备用；
b、烧结助剂制备：选取分析纯碳酸钙、碳酸钡和二氧化硅，按Ba0.6Ca0.4SiO3的比例配料，加入纯水球磨8小时后，放入煅烧炉中煅烧2时，煅烧温度为1000℃，然后加入乙醇球磨4小时并烘干制得烧结助剂备用；
c、按照烧结助剂和主材料成分的比例为2:100配料，加入乙醇球磨1小时并烘干，加入PVA造粒并压成φ10*2mm小圆片,在小圆片两边涂覆镍浆，于1300℃、氧分压为10-11Pa的还原气氛炉中烧结1.5-2.5小时，然后再于900℃、氧分压为10Pa的环境退火5小时，制得抗还原X9R型介质陶瓷材料；
d、测试该X9R 型介质陶瓷材料的介电性能见下表1。
表1 实施例参数及性能如下：
从上表可以看到，实施例2、4、5、6既满足X9R温度特性，又能在还原气氛烧结后得到高的电阻率，可以应用于制备镍电极X9R陶瓷电容器。
以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以对本发明进行若干改进和修饰，这些改进和修饰也落入本发明权利要求的保护范围内。
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (2)
1.一种抗还原X9R型介质陶瓷材料，其特征在于包括主材料和烧结助剂,所述主材料的化学通式为:
(Bix1Mx1Nx2Ba1-x1-x2)(Mny1Mgy2Ny3Ti1-y1-y2-y3)O3；
所述主材料通式中的Ｍ为选自Li、Na和K中的一种；
所述主材料通式中的Ｎ为选自Y、Dy、Ho和Er中的一种；
其中,0.02＜x1＜0.10，0＜x2＜0.01，0.001＜y1＜ 0.01，
0.003＜y2＜ 0.01, 0＜y3＜ 0.01；
所述烧结助剂的化学通式为:BazCa1-zSiO3,其中0.4＜z＜0.6；
所述烧结助剂与主材料的重量份配比为：1-5：100。
2.根据权利要求1 所述的一种抗还原X9R型介质陶瓷材料的制备方法，其特征在于，包括以下制备步骤：
a、主材料制备：选取分析纯钛酸钡、二氧化钛、氧化铋、碳酸钠、碳酸锰、氧化镁和氧化钬，按参数比例配料后加入乙醇，球磨3.5-4.5小时后，放入煅烧炉中煅烧1.5-2.5小时，煅烧温度为860℃-920℃，然后再加乙醇球磨1.5-2.5小时并烘干制得原料备用；
b、烧结助剂制备：选取分析纯碳酸钙、碳酸钡和二氧化硅，按Ba0.6Ca0.4SiO3的比例配料，加入纯水球磨7.5-8.5小时后，放入煅烧炉中煅烧1.5-2.5小时，煅烧温度为960-1100℃，然后加入乙醇球磨3.5-4.5小时并烘干制得烧结助剂备用；
c、按照烧结助剂和主材料成分的比例为2:100配料，加入乙醇球磨0.5-1.5小时并烘干，加入PVA造粒并压成φ10*2mm小圆片,在小圆片两边涂覆镍浆，于1300℃、氧分压为10- 11Pa的还原气氛炉中烧结1.5-2.5小时，然后再于900℃、氧分压为10Pa的环境退火5小时，制得抗还原X9R型介质陶瓷材料；
d、测试该X9R 型介质陶瓷材料的介电性能。
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