CN106187107A - 一种高可靠ag特性微波介质材料及其制备方法 - Google Patents
一种高可靠ag特性微波介质材料及其制备方法 Download PDFInfo
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- CN106187107A CN106187107A CN201610586467.8A CN201610586467A CN106187107A CN 106187107 A CN106187107 A CN 106187107A CN 201610586467 A CN201610586467 A CN 201610586467A CN 106187107 A CN106187107 A CN 106187107A
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- 239000003989 dielectric material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 238000000498 ball milling Methods 0.000 claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000470 constituent Substances 0.000 claims abstract description 15
- 239000000654 additive Substances 0.000 claims abstract description 11
- 230000000996 additive effect Effects 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 9
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 9
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 9
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 9
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 8
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 7
- 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 5
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 5
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 5
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 5
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 4
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 3
- 239000011230 binding agent Substances 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 229910007156 Si(OH)4 Inorganic materials 0.000 claims description 2
- 229910011011 Ti(OH)4 Inorganic materials 0.000 claims description 2
- 239000001095 magnesium carbonate Substances 0.000 claims description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 239000012752 auxiliary agent Substances 0.000 claims 1
- 238000009413 insulation Methods 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 238000000280 densification Methods 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 238000007873 sieving Methods 0.000 abstract 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 10
- 238000004891 communication Methods 0.000 description 8
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 6
- 239000003990 capacitor Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052763 palladium Inorganic materials 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000003985 ceramic capacitor Substances 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000005540 biological transmission 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
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000007766 curtain coating Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005433 ionosphere Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002365 multiple layer Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 231100000701 toxic element Toxicity 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种高可靠AG特性微波介质材料及其制备方法。其配方包括主成分Mg2(SixTi1‑x)O4，0.1≤x≤0.4；改性添加剂为MnO、Al2O3、CoO、CeO2、Nb2O5中的一种或几种；烧结助剂为B2O3、SiO2、ZnO、Li2CO3、Bi2O3中的一种或几种。主成分、改性添加剂和烧结助剂按比例混合，球磨，烘干，过筛后获得。采用本发明的微波介质材料制备的微波介质陶瓷材料，瓷体粒度分布均匀、分散性好、致密、无杂质和少缺陷，成型性工艺好，相对介电常数在10～20系列变化，室温损耗＜4×10‑4，绝缘电阻>1012Ω，容量温度特性稳定，品质因数Q·f很高，且符合环保要求。
Description
技术领域
本发明属于微波介质材料技术领域，特别涉及一种高可靠AG特性微波介质材料及其制备方法。
背景技术
微波介质陶瓷是应用于微波频段(300MHz～300GHz)电路中完成对电磁波的传输、反射、吸收，从而达到对微波的调制作用的微波电介质材料，是近二三十年来发展起来的一种新型功能陶瓷材料。微波介质材料可用于制造射频微波MLCC，广泛应用于微波功率放大器、混频器、振荡器、低噪声放大器、滤波网络、计时电路、延时线、天线调谐、磁共振成像仪，发射机等线路中，起阻抗匹配、调谐、耦合、隔直、滤波、旁路等作用。
随着现代通信和雷达技术的迅速发展，微波通讯己成为现代通信技术的重要组成部分。与普通无线电波相比，微波具有频率高、波长短、抗干扰能力强、能穿透电离层等特点，适合作大容量、高质量、远距离通信的信号载体。另一方面，由于微波通信采用的是无线通信方式，无需铺设线路、资金投入少、建设周期短、受自然环境和地形条件的影响小、抗灾害性能强，与其它通信方式相比具有明显的优越性。近年来，便携式移动电话、车载电话、卫星直播电视、3G/4G通信系统、蓝牙技术、全球卫星定位系统和军用制导系统等微波通信系统得到了迅速发展，小型化、频率高端化、集成化、高质量化和低成本化已成为微波技术发展的必然趋势。
微波介质材料虽在不断发展之中，但是高可靠AG特性的微波介质材料仍然是无相关的工业化应用。
发明内容
针对现有技术不足，本发明提供了一种高可靠AG特性微波介质材料及其制备方法。
一种高可靠AG特性微波介质材料，其配方由主成分、改性添加剂和烧结助剂组成，其中，
所述主成分为Mg2(SixTi1-x)O4，0.1≤x≤0.4；
所述改性添加剂为MnO、Al2O3、CoO、CeO2、Nb2O5中的一种或几种；
所述烧结助剂为B2O3、SiO2、ZnO、Li2CO3、Bi2O3中的一种或几种。
优选地，其配方以摩尔百分量计，含有：
主成分Mg2(SixTi1-x)O4 76～85mol％；
改性添加剂：MnO 0.1～0.5mol％、Al2O3 12～18mol％、CoO 0.1～0.5mol％，CeO20～0.5mol％、Nb2O5 0～2mol％；
烧结助剂共1～4mol％。
一种高可靠AG特性微波介质材料的制备方法，包括如下步骤：
(1)主成分Mg2(SixTi1-x)O4的制备：将MgO的前身物、TiO2的前身物、SiO2的前身物按比例混合，加入氧化锆球进行球磨，球磨时间5～8小时，在100～120℃烘干，过40目筛后，在1050℃～1220℃温度下煅烧2.5～5小时后获得；其中所述MgO的前身物为MgO、Mg(OH)2、MgCO3中的一种或几种；TiO2的前身物为TiO2、Ti(OH)4中的一种或两种；Si的前身物为SiO2、Si(OH)4、Si(CO3)2中的一种或几种；
(2)将上述步骤(1)制备的主成分与烧结助剂和改性添加剂按比例混合，加入氧化锆球进行球磨，球磨时间3～6小时，在120℃烘干，过100目筛后获得。
所述烧结助剂经预处理：将几种原料按比例混合，加入氧化锆球进行球磨，球磨时间为3～6小时，在60～80℃烘干，过100目筛后，在500～800℃煅烧2.5～5小时后获得。
一种高可靠AG特性微波介质材料制备微波介质陶瓷材料的方法，包括以下步骤：
将微波介质材料造粒，在4～6MPa压力下制成坯体；将坯体排胶，排胶温度为500℃，升温速率为2℃/min，保温1小时；再以3～8℃/min升温至1300±30℃对排胶后的坯体进行烧结，保温2～5小时，随炉自然冷却至室温。
一种高可靠AG特性微波介质材料制备MLCC的方法，包括瓷浆制备、制作介质膜片、交替叠印内电极和介质层、坯块干燥、层压、切割、排胶、烧结、倒角、封端、烧端工序；其特征在于，
所述排胶的温度为280～400℃；
所述烧结的温度为1300±30℃，烧结时间为2.5～5小时；
所述烧端的温度为750～850℃。
本发明的有益效果为：
采用本发明的微波介质材料制备微波介质陶瓷材料，能够在较高温度(1300±30℃)下烧结，瓷体具备材料均一、粒度分布均匀、分散性好、致密、无杂质和少缺陷，成型性工艺好，相对介电常数在10～20系列变化，室温损耗＜4×10-4，绝缘电阻>1012Ω，在-55～125℃范围内电容温度系数为100±30ppm/℃，容量温度特性稳定，品质因数Q·f很高。该微波介质材料不含铅Pb、镉Cd、汞Hg、铬Cr等有毒元素，符合环保要求。
本发明的微波介质材料可应用于微波陶瓷电容器、GPS天线、介质滤波器、谐振器等微波元器件的制造，广泛应用于几个至几十GHz微波区域，微波元器件在高功率条件下发热低，可长时间使用。
尤其与钯电极匹配制备的微波电容器FSR(串联谐振频率)高，ESR(等效串联电阻)低，Q值高，击穿电压高，且瓷体致密，适用于高温高湿的恶劣环境。其用钯电极做内电极，避免了银离子迁移引起的介电性能恶化，从而提高了电容器的可靠性。
具体实施方式
下面结合具体实施方式对本发明做进一步说明。应该强调的是，下述说明仅仅是示例性的，而不是为了限制本发明的范围及其应用。
主成分Mg2(Si0.3Ti0.7)O4的制备方法：将纯度均为99.0％以上的Mg(OH)20.2mol、TiO2 0.07mol和SiO2 0.03mol混合，加入氧化锆球进行球磨均匀，球磨时间7小时，在120℃烘6小时至干燥，过40目筛后，在1180±30℃煅烧混合物2.5h，即得主成分Mg2(Si0.3Ti0.7)O4。
烧结助剂的制备方法：按质量比例为1:0.08:4:0.05称取原料B2O3、SiO2、ZnO、Li2CO3混合，加入氧化锆球进行球磨，球磨时间为5小时，在80℃烘10小时至干燥，过100目筛后，在650℃煅烧4小时后获得。
高可靠AG特性微波介质材料的制备方法：配方如表1所示，按设计比例在主成分中添加烧结助剂和改性添加剂，加入氧化锆球进行球磨，球磨时间为5小时，在120℃烘6小时至干燥，过100目筛后获得。
微波介质陶瓷材料的制备：将微波介质材料加入6.5wt％的PVA(聚乙烯醇)水溶液粘合造粒；分别在4MPa、6MPa压力下压制成圆片和圆柱坯体，将坯体排胶，排胶温度为500℃，升温速率为2℃/min，保温1小时，去除粘合剂；将排胶后的坯体在1300±30℃下烧结，保温2～5小时，随炉自然冷却降至室温，制得微波介质陶瓷材料。
将烧制完的圆片两表面涂覆银浆、烧制银电极，制成电容器后测试其室温电学性能，结果见表2：相对介电常数13±3，损耗＜4×10-4，绝缘电阻>1012Ω，在-55～125℃范围内电容温度系数为90～110ppm/℃。
所述圆柱样品的直径为8.5mm，厚度为5mm，圆柱样品的Q·f值为25000～94800。
表1高可靠AG特性微波介质材料配方(mol％)
表2微波介质陶瓷材料的性能
选择配方9，按瓷料生产工艺流程制备一批瓷料，然后按MLCC的制作流程加入有机粘合剂和乙醇等溶剂，从而形成浆料，把浆料流延制作成薄膜片，在膜片上印刷钯内电极，交替层叠所需层数，形成生坯电容器芯片，然后在280～400℃温度热处理生坯电容器芯片，以排除有机粘合剂和溶剂，在1300±30℃烧结2.5～5小时，然后经表面抛光处理，再在电容器芯片的两端封上一对外部银电极，使外部电极与内部电极连接，在750～850℃温度范围内热处理外电极，再经电镀处理等工艺，即可得到多层片式陶瓷电容器。
获得的MLCC满足AG特性要求(在-55～125℃范围内，电容温度系数变化为100±30ppm/℃)，室温损耗≤1×10-4、ESR(1050MHz测试)可低至46mΩ，按照国军标GJB 192A-1998鉴定电容器合格可用。
表3两种规格微波MLCC的性能
Claims (6)
1.一种高可靠AG特性微波介质材料，其特征在于，其配方由主成分、改性添加剂和烧结助剂组成，其中，
所述主成分为Mg2(SixTi1-x)O4，0.1≤x≤0.4；
所述改性添加剂为MnO、Al2O3、CoO、CeO2、Nb2O5中的一种或几种；
所述烧结助剂为B2O3、SiO2、ZnO、Li2CO3、Bi2O3中的一种或几种。
2.根据权利要求1所述一种高可靠AG特性微波介质材料，其特征在于，其配方以摩尔百分量计，含有：
主成分Mg2(SixTi1-x)O4 76～85mol％；
改性添加剂：MnO 0.1～0.5mol％、Al2O3 12～18mol％、CoO 0.1～0.5mol％，CeO2 0～0.5mol％、Nb2O5 0～2mol％；
烧结助剂共1～4mol％。
3.权利要求1或2所述一种高可靠AG特性微波介质材料的制备方法，其特征在于，包括如下步骤：
(1)主成分Mg2(SixTi1-x)O4的制备：将MgO的前身物、TiO2的前身物、SiO2的前身物按比例混合，进行球磨、烘干、过筛后，在1050℃～1220℃温度下煅烧2.5～5小时后获得；其中所述MgO的前身物为MgO、Mg(OH)2、MgCO3中的一种或几种；TiO2的前身物为TiO2、Ti(OH)4中的一种或两种；Si的前身物为SiO2、Si(OH)4、Si(CO3)2中的一种或几种；
(2)将上述步骤(1)制备的主成分与烧结助剂和改性添加剂按比例混合，球磨、烘干、过筛后获得。
4.根据权利要求3所述的制备方法，其特征在于，所述烧结助剂经预处理：将几种原料按比例混合，进行球磨、烘干、过筛后，在500～800℃煅烧2.5～5小时后获得。
5.权利要求1或2所述一种高可靠AG特性微波介质材料制备微波介质陶瓷材料的方法，其特征在于，包括以下步骤：
将微波介质材料造粒，在4～6MPa压力下制成坯体；将坯体排胶，排胶温度为500℃，升温速率为2℃/min，保温1小时；再以3～8℃/min升温至1300±30℃对排胶后的坯体进行烧结，保温2～5小时，随炉自然冷却至室温。
6.权利要求1或2所述一种高可靠AG特性微波介质材料制备MLCC的方法，包括瓷浆制备、制作介质膜片、交替叠印内电极和介质层、坯块干燥、层压、切割、排胶、烧结、倒角、封端、烧端工序；其特征在于，
所述排胶的温度为280～400℃；
所述烧结的温度为1300±30℃，烧结时间为2.5～5小时；
所述烧端的温度为750～850℃。
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