CN106587996B - 一种高频晶界层陶瓷电容器介质 - Google Patents
一种高频晶界层陶瓷电容器介质 Download PDFInfo
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 26
- 239000011521 glass Substances 0.000 claims abstract description 18
- 229910008621 Li2O—Bi2O3 Inorganic materials 0.000 claims abstract description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910010252 TiO3 Inorganic materials 0.000 claims abstract description 12
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 7
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 7
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 7
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000003292 glue Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 238000010532 solid phase synthesis reaction Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 2
- 239000013064 chemical raw material Substances 0.000 claims description 2
- 229910000001 cobalt(II) carbonate Inorganic materials 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- 238000003746 solid phase reaction Methods 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims 1
- 229910021641 deionized water Inorganic materials 0.000 claims 1
- 238000003466 welding Methods 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 7
- 239000010410 layer Substances 0.000 description 17
- 238000005245 sintering Methods 0.000 description 10
- 239000000919 ceramic Substances 0.000 description 6
- 229910010293 ceramic material Inorganic materials 0.000 description 6
- 238000007599 discharging Methods 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 239000002356 single layer Substances 0.000 description 6
- 238000011161 development Methods 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011177 media preparation Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
本发明涉及无机非金属材料技术领域，特指一种高频晶界层陶瓷电容器介质。介质配方组成，按照重量百分比计算：(Sr0.96Ba0.04)TiO3 88‑96％，Co(Li1/4Nb3/4)O30.1‑3％，Dy2O3 0.1‑4％，SiO2 0.1‑2.0％,Al2O30.1‑2.5％,Co(Zr1/2Mg1/2)O30.03‑2.0％，ZnO‑Li2O‑Bi2O3玻璃粉(ZLB)0.1‑2.0％，CuO0.01‑2％。本介质的介电常数高，为50000以上；耐电压高，直流耐电压可达8kV/mm以上；介质损耗小，小于0.6％；色散频率(fm)高，色散频率(fm)高达2GHz以上；本介质的介电常数高，能实现陶瓷电容器的小型化和大容量,同样能降低成本。
Description
技术领域
本发明涉及无机非金属材料技术领域，特指一种高频晶界层陶瓷电容器介质。它采用常规的陶瓷电容器介质制备方法和一次烧结工艺方法，利用电容器陶瓷普通化学原料，制备得到无铅、无镉的高频晶界层陶瓷电容器介质，还能降低电容器陶瓷的烧结温度，该介质适合于制备单片陶瓷电容器和单层片式陶瓷电容器，能大大降低陶瓷电容器的成本，该介质介电常数较高，容易实现陶瓷电容器的小型化，而且温度特性好，同时能提高耐电压和色散频率高以扩大晶界层陶瓷电容器的应用范围，并且在制备和使用过程中不污染环境、安全性高。
背景技术
随着表面安装技术的迅速发展与普及,表面安装元件(SMC)在电子设备中的占有率稳步提高。1997年,世界发达国家电子元器件片式化率已达70％以上，全世界平均40％以上。2000年，全世界电子元器件片式化率达70％。2002年，片式化率已经超过85％。特别是为适应信息领域和航空航天等国防尖端领域对小型多功能电子装置日益紧迫的需求，顺应通信与信息终端的便携化、小型化与多功能化发展潮流，片式电子元件进入了全面发展的新时期。单层片式半导体陶瓷材料分为表面层型和晶界层型两类，其特点是体积小、容量大。此外，晶界层半导体陶瓷材料还具有温度特性好、频率特性好、工作频率高等优点。目前在全球范围内，只有AVX、JOHANSON等不到十家公司能提供单层片式半导体陶瓷材料。全球对单层片式半导体陶瓷材料元件的市场总需求高达45亿只/年。为适应电子元器件微型化、轻型化、复合化、高频化和高性能化的日益迫切要求,半导体陶瓷材料在小型化,高介电常数化,高精度化和高频化方面得到迅速发展,单层片式半导体陶瓷材料为发展的趋势。一般单片晶界层陶瓷电容器介质和单层片式晶界层陶瓷电容器介质的烧结温度为1350～1430℃，同时存在如下问题：要么耐压较低，要么温度系数较大，要么介电常数较低，烧结工艺基本上都是采用二次烧结方法，即：先高温还原，然后涂覆绝缘氧化物在中温进行氧化热处理，工艺较复杂，成本较高；有些采用涂覆法，工艺较复杂，原料较昂贵，成本也较高；而本发明的晶界层陶瓷电容器介质烧结温度为1250-1270℃左右，同时采用一次烧结工艺(先在氮气中500℃以前排胶，然后在高于1000℃后以慢速升温(30-50℃/小时)，然后于1250-1270℃保温3-5小时烧结，然后缓慢冷却到900-950℃左右于空气中保温2-3小时处理，最后随炉冷却))，这样能大大降低晶界层陶瓷电容器的成本，同时本专利电容器陶瓷介质不含铅和镉，电容器陶瓷在制备和使用过程中不污染环境。另外，本发明的电容器陶瓷的介电常数高，这样会提高陶瓷电容器的容量并且小型化，符合陶瓷电容器的发展趋势,同样也会降低陶瓷电容器的成本。本发明的晶界层陶瓷电容器介质耐电压高、色散频率高，容温特性符合X7R的要求等有利于扩大晶界层陶瓷电容器的使用范围和安全性。
发明内容
本发明的目的是提供一种高频晶界层陶瓷电容器介质。
本发明的目的是这样来实现的：
高频晶界层陶瓷电容器介质配方组成，按照重量百分比计算：(Sr0.96Ba0.04)TiO388-96％，Co(Li1/4Nb3/4)O30.1-3％，Dy2O3 0.1-4％，SiO2 0.1-2.0％,Al2O30.1-2.5％,Co(Zr1/2Mg1/2)O30.03-2.0％，ZnO-Li2O-Bi2O3玻璃粉(ZLB)0.1-2.0％，CuO0.01-2％；其中(Sr0.96Ba0.04)TiO3、Co(Li1/4Nb3/4)O3、ZnO-Li2O-Bi2O3玻璃粉分别是采用常规的化学原料以固相法合成。
本发明的介质中所用的Co(Li1/4Nb3/4)O3是采用如下工艺制备的：将常规的化学原料CoCO3和Li2CO3和Nb2O5按1：1/8：3/8摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于830℃保温120分钟，固相反应合成Co(Li1/4Nb3/4)O3，冷却后研磨过200目筛，备用。
本发明的介质中所用的Co(Zr1/2Mg1/2)O3是采用如下工艺制备的：Co(Zr1/2Mg1/2)O3的制备过程包括：Co2O3和ZrO2和MgO按1/2：1/2：1/2摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于1100-1150℃保温120分钟，冷却后得到Co(Zr1/2Mg1/2)O3，研磨过200目筛，备用。
本发明的介质中所用的ZnO-Li2O-Bi2O3玻璃粉(ZLB)是采用如下工艺制备的：将常规的化学原料ZnO和Li2CO3和Bi2O3按1：0.5：0.5摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于600-650℃保温120分钟，然后在水中淬冷，冷却后得到ZnO-Li2O-Bi2O3玻璃粉,研磨过200目筛，备用。
本发明采用如下的高频晶界层陶瓷介质制备工艺：首先采用常规的化学原料用固相法分别合成(Sr0.96Ba0.04)TiO3、Co(Li1/4Nb3/4)O3、Co(Zr1/2Mg1/2)O3、ZnO-Li2O-Bi2O3玻璃粉(ZLB)，然后按配方配料将配合料球磨粉碎混合，进行烘干后，加入粘合剂造粒，再压制成生坯片，然后在空气中进行排胶和烧结(先在氮气中500℃以前排胶，然后在高于1000℃后以慢速升温(30-50℃/小时)，然后于1250-1270℃保温3-5小时烧结，然后缓慢冷却到900-950℃于空气中保温2-3小时处理，最后随炉冷却)，获得高频晶界层陶瓷电容器介质，在介质上被电极即成。
上述陶瓷介质的配方最好采用下列二种方案(重量百分比)：
(Sr0.96Ba0.04)TiO3 89-94％，Co(Li1/4Nb3/4)O30.3-2.5％，Dy2O3 0.3-2.5％，SiO20.1-1.5％,Al2O30.1-2％,Co(Zr1/2Mg1/2)O30.05-1.6％，ZnO-Li2O-Bi2O3玻璃粉(ZLB)0.2-1.8％，CuO0.06-2％。
(Sr0.96Ba0.04)TiO3 90-94％，Co(Li1/4Nb3/4)O3 0.3-2.0％，Dy2O3 0.3-2.0％，SiO20.1-1.3％,Al2O30.1-1.6％,Co(Zr1/2Mg1/2)O30.08-1.5％，ZnO-Li2O-Bi2O3玻璃粉(ZLB)0.3-1.5％，CuO0.1-1.8％。
本发明与现有技术相比，具有如下优点：
1、本专利的介质采用如下的一次烧结工艺：先在氮气中500℃以前排胶，然后在高于1000℃后以慢速升温(30-50℃/小时)，然后于1250-1270℃保温3-5小时烧结，然后缓慢冷却到900-950℃于空气中保温2-3小时处理，最后随炉冷却。这样能大大降低陶瓷电容器的成本，本专利的介质组分中不含铅和镉，对环境无污染。
2、本介质的介电常数高，为50000以上；耐电压高，直流耐电压可达8kV/mm以上；介质损耗小，小于0.6％；色散频率(fm)高，色散频率(fm)高达2GHz以上；本介质的介电常数高，能实现陶瓷电容器的小型化和大容量,同样能降低成本。
3、本介质的温度系数低，电容温度变化率小，符合X7R特性的要求。介质损耗小于0.6％,使用过程中性能稳定性好，安全性高。
4、主要原料采用陶瓷电容器级纯即可制造出本发明的陶瓷介质。
5、本介质采用常规的固相法陶瓷电容器介质制备工艺和一次还原氧化烧结工艺即可进行制备。
具体实施方式
现在结合实施例对本发明作进一步的描述。表1给出本发明的实施例共4个试样的配方。
本发明的实施例共4个试样的配方的主要原料采用陶瓷电容器级纯,在制备时首先采用常规的化学原料用固相法分别合成(Sr0.96Ba0.04)TiO3、Co(Li1/4Nb3/4)O3、Co(Zr1/ 2Mg1/2)O3、ZnO-Li2O-Bi2O3玻璃粉(ZLB)，然后按上述配方配料,将配好的料用蒸馏水或去离子水采用行星球磨机球磨混合,料:球:水＝1:3:(0.6～1.0)(质量比),球磨4～8小时后，烘干得干粉料，在干粉料中加入占其重量8～10％的浓度为10wt％的聚乙烯醇溶液，进行造粒，混研后过40目筛，再在20～30Mpa压力下进行干压成生坯片，然后在温度为1250-1270℃下保温3～5小时进行排胶和烧结(先在氮气中500℃以前排胶，然后在高于1000℃后以慢速升温(30-50℃/小时)，然后于1250-1270℃保温3-5小时烧结，然后缓慢冷却到900-950℃于空气中保温2-3小时处理，最后随炉冷却)，再在780～800℃下保温15分钟进行烧银，形成银电极，再焊引线，进行包封，即得晶界层陶瓷电容器，测试其介电性能。上述各配方试样的介电性能列于表2。从表2可以看出所制备的电容器陶瓷耐电压较高，直流耐电压可达8kV/mm以上；介电常数高，为50000以上；色散频率(fm)高达2GHz以上；介质损耗小于0.6％；电容温度变化率小，符合X7R特性的要求。
表1本发明的实施例共9个试样的配方(重量百分比)
表2各配方试样的介电性能
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (6)
1.一种高频晶界层陶瓷电容器介质，其特征在于：介质配方组成，按照重量百分比计算：(Sr0.96Ba0.04)TiO3 88-96%，Co(Li1/4Nb3/4)O30.1-3%，Dy2O3 0.1-4%，SiO2 0.1-2.0%,Al2O30.1-2.5%, Co(Zr1/2Mg1/2)O30.03-2.0%，ZnO-Li2O-Bi2O3玻璃粉0.1-2.0%，CuO0.01-2%;其中(Sr0.96Ba0.04)TiO3、Co(Li1/4Nb3/4)O3、ZnO-Li2O-Bi2O3玻璃粉分别是采用常规的化学原料以固相法合成；所述高频晶界层陶瓷电容器介质的制备方法如下：
首先采用常规的化学原料用固相法分别合成(Sr0.96Ba0.04)TiO3、Co(Li1/4Nb3/4)O3、Co(Zr1/2Mg1/2)O3、ZnO-Li2O-Bi2O3玻璃粉，然后按上述配方配料，将配好的料用蒸馏水或去离子水采用行星球磨机球磨混合,料、球和水的质量比=1:3:(0.6~1.0),球磨4~8小时后，烘干得干粉料，在干粉料中加入占其重量8~10%的浓度为10wt%的聚乙烯醇溶液，进行造粒，混研后过40目筛，再在20~30Mpa压力下进行干压成生坯片，先在氮气中500℃以前排胶，然后在高于1000℃后以慢速升温，升温速率30-50℃/小时，然后于1250-1270℃保温3-5小时烧结，然后缓慢冷却到900-950℃于空气中保温2-3小时处理，最后随炉冷却，再在780~800℃下保温15分钟进行烧银，形成银电极，再焊引线，进行包封，即得晶界层陶瓷电容器介质。
2.如权利要求1所述的一种高频晶界层陶瓷电容器介质，其特征在于：所述的Co(Li1/ 4Nb3/4)O3是采用如下工艺制备的：将常规的化学原料CoCO3和Li2CO3和Nb2O5按1：1/8：3/8摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于830℃保温120分钟，固相反应合成Co(Li1/ 4Nb3/4)O3，冷却后研磨过200目筛，备用。
3.如权利要求1所述的一种高频晶界层陶瓷电容器介质，其特征在于：所述的Co(Zr1/ 2Mg1/2)O3是采用如下工艺制备的：Co(Zr1/2Mg1/2)O3的制备过程包括：Co2O3和ZrO2和MgO按1/2：1/2：1/2摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于1100-1150℃保温120分钟，冷却后得到Co(Zr1/2Mg1/2)O3，研磨过200目筛，备用。
4.如权利要求1所述的一种高频晶界层陶瓷电容器介质，其特征在于：所述的ZnO-Li2O-Bi2O3玻璃粉是采用如下工艺制备的：将常规的化学原料ZnO和Li2CO3和Bi2O3按1：0.5：0.5摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于600-650℃保温120分钟，然后在水中淬冷，冷却后得到ZnO-Li2O-Bi2O3玻璃粉,研磨过200目筛，备用。
5.如权利要求1所述的一种高频晶界层陶瓷电容器介质，其特征在于：介质配方组成，按照重量百分比计算： (Sr0.96Ba0.04)TiO3 89-94%，Co(Li1/4Nb3/4)O30.3-2.5%，Dy2O3 0.3-2.5%，SiO2 0.1-1.5%, Al2O30.1-2%, Co(Zr1/2Mg1/2)O30.05-1.6%，ZnO-Li2O-Bi2O3玻璃粉0.2-1.8%，CuO0.06-2%。
6.如权利要求1所述的一种高频晶界层陶瓷电容器介质，其特征在于：介质配方组成，按照重量百分比计算：(Sr0.96Ba0.04)TiO3 90-94%，Co(Li1/4Nb3/4)O3 0.3-2.0%，Dy2O3 0.3-2.0%，SiO2 0.1-1.3%, Al2O30.1-1.6%, Co(Zr1/2Mg1/2)O30.08-1.5%，ZnO-Li2O-Bi2O3玻璃粉0.3-1.5%，CuO0.1-1.8%。
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