CN113831123A - 钛酸钡基芯片电容器用介质陶瓷材料及其制备方法和应用 - Google Patents
钛酸钡基芯片电容器用介质陶瓷材料及其制备方法和应用 Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 69
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 58
- 239000003990 capacitor Substances 0.000 title claims abstract description 51
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000000919 ceramic Substances 0.000 claims abstract description 33
- 239000011521 glass Substances 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 17
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 9
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 9
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 9
- 239000000654 additive Substances 0.000 claims abstract description 6
- 230000000996 additive effect Effects 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 6
- 229910052681 coesite Inorganic materials 0.000 claims description 9
- 229910052906 cristobalite Inorganic materials 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
- 229910052682 stishovite Inorganic materials 0.000 claims description 9
- 229910052905 tridymite Inorganic materials 0.000 claims description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 4
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 230000000052 comparative effect Effects 0.000 description 10
- 230000008859 change Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000012188 paraffin wax Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 230000010287 polarization Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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Abstract
本发明提供了钛酸钡基芯片电容器用介质陶瓷材料及其制备方法和应用,涉及电容器陶瓷材料技术领域。钛酸钡基芯片电容器用介质陶瓷材料,以BaTiO3的重量百分比为100%计,添加以下重量百分比的组分:0~1.70%的La2O3、0~1.60%的Nb2O5、0~0.40%的CeO2、0~0.12%的MnO2、0~0.50%MgCO3和0.3~1.3%的玻璃粉。其制备方法包括以下步骤:S1:将玻璃粉组分按比例混合制备玻璃粉;S2:将制得的玻璃粉和BaTiO3及其余组分按比例混合制备得到介质陶瓷材料。本发明还提供了由上述方法制备的钛酸钡基芯片电容器用介质陶瓷材料,其生产X7R‑502介质陶瓷中的应用。本发明可以制得在符合X7R的温度特性基础上,具有较高的介电常数,在1MHz下具有较小的介质损耗的钛酸钡基芯片电容器用介质陶瓷材料。
Description
技术领域
本发明涉及电容器陶瓷材料技术领域,具体而言,涉及钛酸钡基芯片电容器用介质陶瓷材料及其制备方法和应用。
背景技术
芯片电容器具有体积小、电气性能稳定、可靠性高等优点,适用于金丝键合工艺的高频电子线路中;此类芯片电容器生产用的支撑材料须满足在高频(1MHz)条件下介电常数高、介质损耗低等条件;此类芯片电容器生产用的支撑材料一般使用具有X7R特性的介质陶瓷材料。
目前,现有的具有X7R特性的介质陶瓷材料的介电常数较低,一般难以达到5000,介质损耗也较高,无法满足芯片电容器最高端型号产品的生产要求。
发明内容
本发明的第一个目的在于提供钛酸钡基芯片电容器用介质陶瓷材料,其可以在符合X7R的温度特性基础上,具有较高的介电常数,在1MHz下具有较小的介质损耗;可以满足芯片电容器最高端型号产品的生产需要。
本发明的第二个目的在于提供钛酸钡基芯片电容器用介质陶瓷材料的制备方法,通过制备方法制得的具有较高的介电常数和在1MHz下具有较小的介质损耗的钛酸钡基芯片电容器用介质陶瓷材料。
本发明的第三个目的在于提供钛酸钡基芯片电容器用介质陶瓷材料的应用,其可有效应用于生产X7R-502介质陶瓷。
本发明的实施例通过以下技术方案实现:
钛酸钡基芯片电容器用介质陶瓷材料,以BaTiO3的重量百分比为100%计,添加以下重量百分比的组分:0~1.70%的La2O3、0~1.60%的Nb2O5、0~0.40%的CeO2、0~0.12%的MnO2、0~0.50%MgCO3和0.3~1.3%的玻璃粉。
进一步地,所述玻璃粉包括以下重量百分比的组分:10~20%的Nd2O3、35~45%的ZnO、15~25%的SiO2和15~25%的B2O3。
芯片电容器产品会应用在高频的线路当中,在1MHz下钛酸钡***的介质陶瓷材料的介质损耗会成倍的增加,就会导致产品的发热失效,为了降低1MHz下介质陶瓷材料的介质损耗,本发明的钛酸钡基芯片电容器用介质陶瓷材料选用相应的组分及含量配比,在主晶相***中添加改性物质MnO2、MgCO3及稀土元素(La3+、Nd3+)等,可在保证BaTiO3自发极化的同时抑制BaTiO3晶粒异常生长,减少空间电荷极化引起的松弛极化,获得致密的瓷体结构,使钛酸钡基芯片电容器用介质陶瓷材料的介电常数达到5000的同时,降低高频(1MHz)下钛酸钡基芯片电容器用介质陶瓷材料的介质损耗;
同时,本发明的钛酸钡基芯片电容器用介质陶瓷材料中加入一定组分和含量配比形成的玻璃粉,其各组分可以起移峰压峰的作用,又可以起到各组分相互键联的作用,从而增加钛酸钡基芯片电容器用介质陶瓷材料的致密度,从而增大钛酸钡基芯片电容器用介质陶瓷材料的介电常数,减小钛酸钡基芯片电容器用介质陶瓷材料的介质损耗。
另外,BaTiO3的晶型会随着温度的改变而发生变化,导致其介电常数呈非线性变化,在-55~125℃温度范围内难以达到X7R特性,在BaTiO3中引入Nd2O3、ZnO、SiO2和B2O3组成的玻璃粉,La2O3、CeO2、Nb2O5和SiO2属于移峰剂、展宽剂物质,在不过分抑制其铁电性的同时,使BaTiO3居里峰弥散并向中部移动,使介电常数高且平缓;在钛酸钡基芯片电容器用介质陶瓷材料获得5000以上介电常数的同时,优化了电容量随温度变化率,从而达到X7R特性。
钛酸钡基芯片电容器用介质陶瓷材料的制备方法,包括以下步骤:
S1:将玻璃粉的各组分按比例混合制备玻璃粉;
S2:将制得的玻璃粉和BaTiO3及其余各组分按比例混合制备得到介质陶瓷材料。
进一步地,所述步骤S1中将Nd2O3、ZnO、SiO2和B2O3按照比例混合,过200目筛4~5遍后置于氧化锆匣钵中,在900~970℃条件下煅烧,再用搅拌磨以去离子水为介质研磨1~2h,再于100~140℃烘干并过200目筛网,制得玻璃粉。
进一步地,所述步骤S2中将制得的玻璃粉和BaTiO3、CeO2、La2O3、Nb2O5、MnO2、MgCO3按比例从大到小依次加入立式振动磨,按照粉料:去离子水:球磨介质=1:1.4:5的质量比例振动研磨15~20h,研磨后经320目筛处理得到陶瓷浆料,将陶瓷浆料于100~140℃烘干,过200目筛网,制得介质陶瓷材料。
一种根据权利要求9所述的钛酸钡基芯片电容器用介质陶瓷材料,在生产X7R-502介质陶瓷中的应用,将制得的介质陶瓷材料瓷料加入7~8wt%的石蜡进行造粒,使用液压机制成直径为15mm,厚度为1.3~1.7mm的圆片,然后将温度以1.5℃/min的速度升至450℃排出石蜡,再将温度以3℃/min的速度升至1350~1390℃,进行烧结3h后随炉冷却,制得X7R-502介质陶瓷。
本发明实施例的技术方案至少具有如下优点和有益效果:
1.本发明选用相应的组分及含量配比组成的钛酸钡基芯片电容器用介质陶瓷材料,其在达到X7R特性的基础上,介电常数较高,可以达到5000以上,同时在高频(1MHz)下介质损耗较低。
2.本发明可以制得具有较高的介电常数和在1MHz下具有较小的介质损耗的钛酸钡基芯片电容器用介质陶瓷材料。
3.本发明制得的具有较高的介电常数和在1MHz下具有较小的介质损耗的钛酸钡基芯片电容器用介质陶瓷材料,可以应用于生产X7R-502介质陶瓷。
4.本发明的钛酸钡基芯片电容器用介质陶瓷材料中未选用Pb、Cr、Hg等有毒有害物质,符合欧盟ROHS指令环保要求。
附图说明
图1为实施例1制得的介质陶瓷材料的扫描电镜(SEM)图。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将对本发明实施例中的技术方案进行清楚、完整地描述。实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市售购买获得的常规产品。
下面对本发明实施例提供的钛酸钡基芯片电容器用介质陶瓷材料及其制备方法和应用进行具体说明。
实施例1~10
实施例1~10提供了钛酸钡基芯片电容器用介质陶瓷材料,以BaTiO3的重量百分比为100%计,添加重量百分比的组分如表1和表2所示。
表1玻璃粉组分
表2钛酸钡基芯片电容器用介质陶瓷材料组分
实施例1~10还提供了钛酸钡基芯片电容器用介质陶瓷材料的制备方法,包括以下步骤:
S1:将Nd2O3、ZnO、SiO2和B2O3按照比例混合,过200目筛4~5遍后置于氧化锆匣钵中,在900~970℃条件下煅烧,再用搅拌磨以去离子水为介质研磨1~2h,再于100~140℃烘干并过200目筛网,制得玻璃粉;
S2:将制得的玻璃粉和BaTiO3、CeO2、La2O3、Nb2O5、MnO2、MgCO3按比例从大到小依次加入立式振动磨,按照粉料:去离子水:球磨介质=1:1.4:5的质量比例振动研磨15~20h,研磨后经320目筛处理得到陶瓷浆料,将陶瓷浆料于100~140℃烘干,过200目筛网,制得介质陶瓷材料。实施例1制得的介质陶瓷材料的扫描电镜(SEM)图如图1所示。
实施例1~10还提供了钛酸钡基芯片电容器用介质陶瓷材料在生产X7R-502介质陶瓷中的应用,将制得的介质陶瓷材料瓷料加入7~8wt%的石蜡进行造粒,使用液压机制成直径为15mm,厚度为1.3~1.7mm的圆片,然后将温度以1.5℃/min的速度升至450℃排出石蜡,再将温度以3℃/min的速度升至1350~1390℃,进行烧结3h后随炉冷却,制得X7R-502介质陶瓷。
对比例1~8
对比例1~8提供了一种介质陶瓷材料,以BaTiO3的重量百分比为100%计,添加重量百分比的组分如表3和表4所示。
表3玻璃粉组分
表4介质陶瓷材料组分
对比例1~8提供的一种介质陶瓷材料的制备方法与实施例1~10的制备方法相同,并以实施例1~10相同的制备方法制得介质陶瓷。
实验例1
将实施例1分别于1350℃、1370℃和1390℃烧结温度下制得的X7R-502介质陶瓷A1、A2、A3和分别于1350℃、1370℃和1390℃烧结温度下制得的美国FerroX7R-502介质陶瓷B1、B2、B3分别通过介电温谱仪进行介电性能测试,结果如表5所示。
表5介电性能表
由表5可以看出,本发明制得的X7R-502介质陶瓷比美国FerroX7R-502介质陶瓷的介电常数高,高于5000以上;比美国FerroX7R-502介质陶瓷的介质损耗小,在1KHz下介质陶瓷的介质损耗小于0.6%,在1MHz下介质损耗小于1.8%;在-55~125℃的温度范围内,电容量随温度变化率小,符合X7R的温度特性。
实验例2
将实施例1~10制得的X7R-502介质陶瓷和对比例1~8制得的介质陶瓷分别通过介电温谱仪进行介电性能测试,结果如表6所示。
表6介电性能表
由表6可以看出,对比例1的介质陶瓷材料中无玻璃粉,对比例2的介质陶瓷材料中无玻璃粉且各组分不同,对比例3的介质陶瓷材料中无玻璃粉且各组分不同,对比例4的介质陶瓷材料中玻璃粉的组分不同,对比例5的介质陶瓷材料中所有组分均不同,对比例6~8的介质陶瓷材料中各组分的含量配比不在本发明的范围内;使用本发明提供的介质陶瓷材料制得的X7R-502介质陶瓷的介电常数高,高于5000以上;介质损耗小,在1KHz下介质陶瓷的介质损耗小于0.6%,在1MHz下介质损耗小于1.8%;在-55~125℃的温度范围内,电容量随温度变化率小,符合X7R的温度特性。
综上,本申请提供的钛酸钡基芯片电容器用介质陶瓷材料,其制备的X7R-502介质陶瓷在符合X7R的温度特性基础上,具有较高的介电常数,在1MHz下具有较小的介质损耗;可以满足芯片电容器最高端型号产品的生产需要。
以上所述仅为本发明的优选实施例而已,并不用于限制本发明,对于本领域的技术人员来说,本发明可以有各种更改和变化。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.钛酸钡基芯片电容器用介质陶瓷材料,其特征在于,以BaTiO3的重量百分比为100%计,添加以下重量百分比的组分:0~1.70%的La2O3、0~1.60%的Nb2O5、0~0.40%的CeO2、0~0.12%的MnO2、0~0.50%MgCO3和0.3~1.3%的玻璃粉。
2.根据权利要求1所述的钛酸钡基芯片电容器用介质陶瓷材料,其特征在于,所述玻璃粉包括以下重量百分比的组分:10~20%的Nd2O3、35~45%的ZnO、15~25%的SiO2和15~25%的B2O3。
3.根据权利要求2所述的钛酸钡基芯片电容器用介质陶瓷材料,其特征在于,所述玻璃粉包括以下重量百分比的组分:16%的Nd2O3、42%的ZnO、18%的SiO2和24%的B2O3。
4.根据权利要求2所述的钛酸钡基芯片电容器用介质陶瓷材料,其特征在于,所述玻璃粉包括以下重量百分比的组分:13%的Nd2O3、40%的ZnO、24%的SiO2和23%的B2O3。
5.根据权利要求1~4任一项所述的钛酸钡基芯片电容器用介质陶瓷材料,其特征在于,以BaTiO3的重量百分比为100%计,添加以下重量百分比的组分:0.61%的La2O3、0.54%的Nb2O5、0.05%的CeO2、0.09%的MnO2、0.03%MgCO3和0.5%的玻璃粉。
6.根据权利要求1~4任一项所述的钛酸钡基芯片电容器用介质陶瓷材料,其特征在于,以BaTiO3的重量百分比为100%计,添加以下重量百分比的组分:0.87%的La2O3、0.9%的Nb2O5、0.34%的CeO2、0.11%的MnO2、0.28%MgCO3和0.8%的玻璃粉。
7.一种由权利要求1~6任一项所述的钛酸钡基芯片电容器用介质陶瓷材料的制备方法,其特征在于,包括以下步骤:
S1:将玻璃粉的各组分按比例混合制备玻璃粉;
S2:将制得的玻璃粉和BaTiO3及其余各组分按比例混合制备得到介质陶瓷材料。
8.根据权利要求7所述的钛酸钡基芯片电容器用介质陶瓷材料的制备方法,其特征在于,所述步骤S1中将Nd2O3、ZnO、SiO2和B2O3按照比例混合,过200目筛4~5遍后置于氧化锆匣钵中,在900~970℃条件下煅烧,再用搅拌磨以去离子水为介质研磨1~2h,再于100~140℃烘干并过200目筛网,制得玻璃粉。
9.根据权利要求7所述的钛酸钡基芯片电容器用介质陶瓷材料的制备方法,其特征在于,所述步骤S2中将制得的玻璃粉和BaTiO3、CeO2、La2O3、Nb2O5、MnO2、MgCO3按比例从大到小依次加入立式振动磨,按照粉料:去离子水:球磨介质=1:1.4:5的质量比例振动研磨15~20h,研磨后经320目筛处理得到陶瓷浆料,将陶瓷浆料于100~140℃烘干,过200目筛网,制得介质陶瓷材料。
10.一种由权利要求1~6任一项所述的钛酸钡基芯片电容器用介质陶瓷材料或由权利要求7~9任一项所述的制备方法制得的钛酸钡基芯片电容器用介质陶瓷材料,在生产X7R-502介质陶瓷中的应用。
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