CN110818407A - 一种x7r特性mlcc介质材料及其制备方法 - Google Patents
一种x7r特性mlcc介质材料及其制备方法 Download PDFInfo
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- 239000003989 dielectric material Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 42
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 150000001875 compounds Chemical class 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 30
- 239000011777 magnesium Substances 0.000 claims abstract description 23
- 238000010532 solid phase synthesis reaction Methods 0.000 claims abstract description 20
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 13
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 13
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 13
- 239000011572 manganese Substances 0.000 claims abstract description 13
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 12
- 239000011575 calcium Substances 0.000 claims abstract description 12
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 4
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 claims description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 4
- 239000011656 manganese carbonate Substances 0.000 claims description 3
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 3
- 230000005855 radiation Effects 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 3
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims description 2
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 2
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 2
- 239000004576 sand Substances 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims 3
- 238000003756 stirring Methods 0.000 claims 1
- 239000000919 ceramic Substances 0.000 description 14
- 239000000843 powder Substances 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 239000003607 modifier Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 239000007791 liquid phase Substances 0.000 description 6
- 229910052573 porcelain Inorganic materials 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 239000007790 solid phase Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 229910052727 yttrium Inorganic materials 0.000 description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229940043430 calcium compound Drugs 0.000 description 2
- 150000001674 calcium compounds Chemical class 0.000 description 2
- 239000003985 ceramic capacitor Substances 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- ZXGIFJXRQHZCGJ-UHFFFAOYSA-N erbium(3+);oxygen(2-) Chemical class [O-2].[O-2].[O-2].[Er+3].[Er+3] ZXGIFJXRQHZCGJ-UHFFFAOYSA-N 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 2
- 238000007603 infrared drying Methods 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 2
- 229910001954 samarium oxide Inorganic materials 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 2
- 229910003454 ytterbium oxide Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000011324 bead Substances 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
- 239000002131 composite material Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000002681 magnesium compounds Chemical class 0.000 description 1
- 150000002697 manganese compounds Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- 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
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Abstract
本发明公开了一种X7R特性MLCC介质材料，所述介质材料由以下成分组成：固相法钛酸钡100摩尔份、SiO2 2.1‑2.9摩尔份、含镁化合物5.5‑7.0摩尔份、含锰化合物0.51‑1.0摩尔份、含钙化合物2.5‑4.0摩尔份和稀土氧化物0.51‑1.3摩尔份。该介质材料的介电常数为2200‑3800，符合X7R特性，可应用于厚度为2～10um的BME‑MLCC介质层的制备。本发明还公开了所述X7R特性MLCC介质材料的制备方法。
Description
技术领域
本发明涉及一种介质材料及其制备方法，尤其是一种BME-MLCC用X7R特性介质材料及其制备方法。
背景技术
随着MLCC大容量、小尺寸化的进一步发展，介质层厚度的降低，对陶瓷介质材料用主晶相原料的纯度、小粒径化、颗粒大小一致性、局部组分均匀性、分散性以及介质瓷料的制备工艺提出了更加严格的要求。
固相法钛酸钡成本低，其生产过程中环境污染小，但其组分均一性、分散性不如水热法钛酸钡。目前以固相法钛酸钡为主成分生产的X7R特性MLCC用介质材料，只能应用于厚度为8um以上的介质层，且添加的辅助成分品种多，为了得到良好的电性能，添加了RoHS指令中有控制限的金属元素。例如铅镁铌系铅基复合钙钛矿型弛豫铁电体材料。又例如我国专利CN 106747419A，以固相法掺钇钛酸钡为主要成分，生产中高压X7R特性MLCC用介质材料。该专利指出，固相合成钛酸钡时掺杂部分钇，使其具有钛酸钡高的结晶性外还有无孔洞、缺陷少等特点，保证介质材料高的可靠性；添加氧化物Cr2O3可以改善绝缘电阻及IR耐久性，含量过少，不能得到充分的效果。三价铬在有氧化剂(即氧化性大于六价铬)存在的条件下，温度高于30摄氏度就有可能被氧化成六价铬。
液相法制备钛酸钡，不同组分原材料可以在液态下进行分子级别的均匀混合，合成的钛酸钡在颗粒大小及组分的均一性方面，比固相法更有优势，尤其是水热法钛酸钡粉体。水热法钛酸钡纯度高、粒径小、颗粒大小均匀、分散性好、组分均一性好，更适合用于薄介质介电陶瓷的制备。但参与液相反应的各酸性或碱性原料遗留的大量可溶性杂质，需要用大量水或溶剂洗涤净化，排放的废水废气污染环境，且水热法钛酸钡生产工艺过程复杂，成本较高。
目前的X7R特性MLCC薄介质多采用液相法生产的钛酸钡为基础粉料。例如我国专利CN 101333105B(介质层厚度为1～3um)指出，为了使介质层尽可能薄，选用平均粒径为0.08～0.18um的液相法生产BaTiO3为主成分；并且，为了将主成分和辅助成分混合均匀，采用了复杂的介质材料制备工艺，包括①烧结助剂玻璃粉的球磨、烘干、过筛、烧结、后处理；②主成分与辅助成分的球磨混合、烘干、过筛、煅烧；③所有成分的球磨混合、烘干、过筛。这样操作过程繁琐，且烧结助剂玻璃粉烧结处理后降低了反应活性，不利于介质陶瓷的致密化。又例如我国专利CN 107840654A指出,一种用于陶瓷电容器的介质材料，其特征在于，BaTiO3采用水热法生产。水热法钛酸钡生产过程中排放的废水污染环境，且成本较高，从而推高了介质瓷料的生产成本。
发明内容
基于此，本发明的目的在于克服上述现有技术的不足之处而提供一种X7R特性MLCC介质材料。该介质材料以固相法钛酸钡为原料，添加的改性剂种类少，介质瓷料制备工艺简单，得到的介质材料可应用于薄介质BME-MLCC领域。
为实现上述目的，本发明所采取的技术方案为：一种X7R特性MLCC介质材料，所述介质材料由以下成份组成：固相法钛酸钡100摩尔份、SiO2 2.1-2.9摩尔份、含镁化合物5.5-7.0摩尔份、含锰化合物0.51-1.0摩尔份、含钙化合物2.5-4.0摩尔份和稀土氧化物0.51-1.3摩尔份。
纯钛酸钡不同温度时的介电性能变化很大，常温下介电常数随温度变化比较平坦，高温区介电常数随温度变化幅度很大，在居里点(120℃)出现峰值，容量温度稳定性差，需引入改性添加剂改善容量温度稳定性；在上述固相法合成的钛酸钡中添加少量亚微米级或纳米级的硅、镁、锰、钙的化合物，以及钇、镧、钐、镱、钬、铒元素氧化物中的两种或多种，湿法混合均匀并干燥后得到MLCC用介质瓷料，改善了陶瓷介质的温度特性，其温度稳定性符合美国电子工业协会制定的X7R介质材料标准；解决了钛酸钡瓷料抗还原性差的问题；解决了固相法钛酸钡制备的介电瓷料晶粒大、只能用于生产介质层较厚的MLCC的问题。
介电陶瓷在煅烧过程中，部分添加剂的软化温度低先溶为液相，随温度升高液相增多，逐渐包裹着还没有来得及长大的固相BaTiO3晶粒，形成壳-芯结构，抑制了钛酸钡晶粒的进一步长大，最终固溶成细晶的介电陶瓷，改善了介电陶瓷的温度特性。钛酸钡在还原气氛中烧结时易高温失氧而变成半导体，镁、钙、锰等化合物在瓷介的煅烧过程中起受主作用，所引起的氧空位浓度大于因氧挥发而形成的氧空位浓度，使钛酸钡在还原气氛中烧结时也能保持高电绝缘电阻率。
优选地，所述固相法钛酸钡呈球形或类球形，所述固相法钛酸钡的颗粒尺寸为150～500nm。
优选地，所述含镁化合物、含锰化合物、含钙化合物、稀土氧化物呈球形或类球形，所述含镁化合物、含锰化合物、含钙化合物、稀土氧化物的颗粒尺寸为亚微米级或纳米级。
更优选地，所述含镁化合物、含锰化合物、含钙化合物、稀土氧化物的颗粒尺寸为50～400nm。
优选地，所述含镁化合物为Mg(OH)2、Mg2CO3中的至少一种；所述含锰化合物为MnCO3、MnO2、Mn3O4中的至少一种；所述含钙化合物为CaCO3、CaO中的至少一种；所述稀土氧化物为Y2O3、La2O3、Sm2O3、Dy2O3、Ho2O3、Er2O3中的至少两种。
同时，本发明还公开一种上述X7R特性MLCC介质材料的应用，用于制备厚度为2～10um的BME-MLCC介质层。
再次，本发明还公开一种上述X7R特性MLCC介质材料制备得到的BME-MLCC介质层，所述BME-MLCC介质层的介电常数为2200-3800，直流耐压在5KV以上。
此外，本发明还公开一种所述X7R特性MLCC介质材料的制备方法，包括以下步骤：
将全部原料一起湿法混合，干燥后即得到所述X7R特性MLCC介质材料。
优选地，所述湿法混合方法包括搅拌磨、振动磨、球磨或砂磨。
更优选地，所述湿法混合方法为砂磨。
优选地，所述砂磨的研磨介质为0.1-1.2mm氧化锆珠。
优选地，所述干燥方法包括热辐射干燥、微波干燥或喷雾干燥。
更优选地，所述干燥方法为：在100-120℃下远红外热辐射干燥，或微波干燥，或喷雾干燥。
本发明通过简化介质材料的配方，优化介质材料的制备工艺，系统调节各改性添加剂的使用量，得到了温度稳定性好、抗还原性好、成瓷后晶粒细的介质材料，所制备的X7R瓷料制成BME-MLCC后具有高介电常数、高绝缘电阻、高耐压、容量温度特性符合X7R介质材料温度特性，可应用于厚度为2～10um的BME-MLCC介质层的制备。制成BME-MLCC后温度系数：-15％≤△C/C≤+15％(-55℃～+125℃)，室温介电常数：2200～3800，直流耐压在5KV以上。
相对于现有技术，本发明的有益效果为：
1、以固相法钛酸钡为主要成分，添加改性剂制成的介质材料温度特性符合X7R特性，既可制备成厚度为2～3um的薄层BME-MLCC用电介质，又可应用于厚度为4～10um的MLCC电介质的制备。
2、不添加RoHS指令受限物质，不添加铅、镉、铬等金属元素，为环保型介质材料；添加少量二氧化硅、镁化合物、锰化合物、钙化合物，以及钇、镧、钐、镱、钬、铒元素氧化物中的两种或多种对钛酸钡进行改性，所制备的X7R瓷料介电常数在2200-3800，直流耐压在5KV以上，可靠性好，可应用于瓷膜厚度为2～10um的BME-MLCC介质层的制备。
3、制备工艺简单，所使用的改性添加剂种类少，材料组份均匀性好，电性能优良，可用于中高压X7R特性MLCC的制备。
附图说明
图1为实施例2中制备的X7R特性介质粉体的扫描电镜图；
图2为实施例1中制备的介质材料制成MLCC后的瓷体表面扫描电镜图。
具体实施方式
为更好的说明本发明的目的、技术方案和优点，下面将结合附图和具体实施例对本发明作进一步说明。
实施例1
本发明所述X7R特性MLCC介质材料的一种实施例，本实施例所述X7R特性MLCC介质材料通过以下方法制备所得：
(1)将固相法钛酸钡粉体、二氧化硅粉体、含镁化合物粉体、含锰化合物粉体、含钙化合物粉体、稀土氧化物粉体，与去离子水一起湿法混合均匀，得到浆状介质材料；
(2)将上述浆状介质材料干燥后即得到所述X7R特性MLCC介质材料。
具体来说，按表1中的选材，取100mol固相法钛酸钡，按表2加入改性剂，与去离子水一起砂磨4-8小时，然后用微波炉干燥，得到所述X7R特性MLCC介质材料，制成介质厚度为2um的薄层BME-MLCC，电性能测试如表3。
表1试验选材(用于厚度为2～4um的BME-MLCC介质)
表2试验配料
表3电性能测试1
从表3可以看出，本发明所述X7R特性MLCC介质材料，制成介质厚度为2um的薄层BME-MLCC，-55℃至+125℃容量偏差不超过15％，介电常数在2200以上，介电损耗低，绝缘电阻高、耐压高，符合X7R介质材料标准。
实施例2
本发明所述X7R特性MLCC介质材料的一种实施例，本实施例所述X7R特性MLCC介质材料通过以下方法制备所得：
按表1选材，取100mol固相法钛酸钡，按表2加入改性剂，与去离子水一起球磨8-16小时，然后用远红外线干燥炉干燥，得到介质材料。
实施例3
本发明所述X7R特性MLCC介质材料的一种实施例，本实施例所述X7R特性MLCC介质材料通过以下方法制备所得：
按表1选材，取100mol固相法钛酸钡，按表2加入改性剂，与去离子水一起用振动磨磨15-24小时，然后用喷雾塔干燥，得到介质材料。
实施例4
本发明所述X7R特性MLCC介质材料的一种实施例，本实施例所述X7R特性MLCC介质材料通过以下方法制备所得：
按表1选材，取100mol固相法钛酸钡，按表2中的摩尔量加入改性剂，将Mg(OH)2换成Mg2CO3，将MnO2换成MnCO3，将CaCO3换成CaO，与去离子水一起砂磨4-8小时，然后用喷雾塔干燥，得到介质材料。
实施例5
本发明所述X7R特性MLCC介质材料的一种实施例，本实施例所述X7R特性MLCC介质材料通过以下方法制备所得：
按表1选材，取100mol固相法钛酸钡，按表2中的摩尔量加入改性剂，将Mg(OH)2换成Mg2CO3，将MnO2换成Mn3O4，将CaCO3换成CaO，与去离子水一起球磨8-16小时，然后用远红外线干燥炉干燥，得到介质材料。
实施例6
本发明所述X7R特性MLCC介质材料的一种实施例，本实施例所述X7R特性MLCC介质材料通过以下方法制备所得：
按表4选材，取100mol固相法钛酸钡，按表2中的摩尔量加入改性剂，将Mg(OH)2换成Mg2CO3，将MnO2换成Mn3O4，将CaCO3换成CaO，与去离子水一起砂磨4-8小时，然后在用微波炉干燥，得到介质材料，制成介质厚度为10um的BME-MLCC，电性能测试如表5。
表4试验选材(用于厚度为5～10um的BME-MLCC介质)
表5电性能测试2
从表5可以看出，本发明所述X7R特性MLCC介质材料，制成介质厚度为10um的BME-MLCC，-55℃至+125℃容量偏差不超过15％，介电损耗低，绝缘电阻高、耐压高，符合X7R介质材料标准。
附图1为实施例2中制备的X7R特性介质粉体的微观形貌。从附图1可以看出，介质粉体晶粒尺寸小，呈球形或类球形，有利于在烧结过程中形成致密的细晶介电陶瓷。
附图2为实施例1中制备的介质材料制成MLCC后的瓷体表面形貌。从附图2可以看出，烧结成瓷后晶粒尺寸较小，晶粒大小较为均匀。本发明中的改性剂有效地抑制了钛酸钡晶粒在烧结成瓷过程中的进一步长大，MLCC介质层厚度可以做得很薄。
最后所应当说明的是，以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的实质和范围。
Claims (9)
1.一种X7R特性MLCC介质材料，其特征在于，所述介质材料由以下成份组成：
固相法钛酸钡100摩尔份、SiO2 2.1-2.9摩尔份、含镁化合物5.5-7.0摩尔份、含锰化合物0.51-1.0摩尔份、含钙化合物2.5-4.0摩尔份和稀土氧化物0.51-1.3摩尔份。
2.如权利要求1所述的X7R特性MLCC介质材料，其特征在于，所述固相法钛酸钡呈球形或类球形，所述固相法钛酸钡的颗粒尺寸为150～500nm。
3.如权利要求1所述的X7R特性MLCC介质材料，其特征在于，所述含镁化合物、含锰化合物、含钙化合物、稀土氧化物呈球形或类球形，所述含镁化合物、含锰化合物、含钙化合物、稀土氧化物的颗粒尺寸为亚微米级或纳米级。
4.如权利要求3所述的X7R特性MLCC介质材料，其特征在于，所述含镁化合物为Mg(OH)2、Mg2CO3中的至少一种；所述含锰化合物为MnCO3、MnO2、Mn3O4中的至少一种；所述含钙化合物为CaCO3、CaO中的至少一种；所述稀土氧化物为Y2O3、La2O3、Sm2O3、Dy2O3、Ho2O3、Er2O3中的至少两种。
5.一种权利要求1～4任一项所述X7R特性MLCC介质材料的应用，其特征在于，所述介质材料用于制备厚度为2～10um的BME-MLCC介质层。
6.一种由权利要求1～4任一项所述的X7R特性MLCC介质材料制备得到的BME-MLCC介质层，其特征在于，所述BME-MLCC介质层的介电常数为2200-3800、直流耐压为5KV以上。
7.一种如权利要求1～4任一项所述X7R特性MLCC介质材料的制备方法，其特征在于，所述方法为：
将全部原料一起湿法混合，干燥后即得到所述X7R特性MLCC介质材料。
8.如权利要求7所述的X7R特性MLCC介质材料的制备方法，其特征在于，所述湿法混合方法包括搅拌磨、振动磨、球磨或砂磨。
9.如权利要求7所述的X7R特性MLCC介质材料的制备方法，其特征在于，所述干燥方法包括热辐射干燥、微波干燥或喷雾干燥。
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| CN105174941A (zh) * | 2015-09-08 | 2015-12-23 | 山东国瓷功能材料股份有限公司 | 一种高可靠x8r型多层陶瓷电容器用介质材料及其制备方法 |
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