CN113185285A - 一种陶瓷介质材料及其独石电容器 - Google Patents
一种陶瓷介质材料及其独石电容器 Download PDFInfo
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- 239000003989 dielectric material Substances 0.000 title claims abstract description 33
- 239000000919 ceramic Substances 0.000 title claims abstract description 20
- 239000003990 capacitor Substances 0.000 title claims description 6
- 239000013078 crystal Substances 0.000 claims abstract description 42
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000000654 additive Substances 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 230000000996 additive effect Effects 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 7
- 239000012071 phase Substances 0.000 claims description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 229910052681 coesite Inorganic materials 0.000 claims description 11
- 229910052906 cristobalite Inorganic materials 0.000 claims description 11
- 239000011656 manganese carbonate Substances 0.000 claims description 11
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 229910052682 stishovite Inorganic materials 0.000 claims description 11
- 229910052905 tridymite Inorganic materials 0.000 claims description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- 229910052593 corundum Inorganic materials 0.000 claims description 10
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 10
- 229910002971 CaTiO3 Inorganic materials 0.000 claims description 9
- 229910017676 MgTiO3 Inorganic materials 0.000 claims description 9
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 6
- 238000010532 solid phase synthesis reaction Methods 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 3
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims description 3
- 239000012856 weighed raw material Substances 0.000 claims description 3
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910052689 Holmium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
- 239000011363 dried mixture Substances 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052759 nickel Inorganic materials 0.000 abstract description 5
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 6
- 238000009413 insulation Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Inorganic materials [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 229910011255 B2O3 Inorganic materials 0.000 description 1
- 230000003679 aging effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010344 co-firing Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
本发明属于陶瓷材料技术领域，具体涉及一种陶瓷介质材料，所述陶瓷介质材料的功能性成分包括主晶相、改性添加剂和烧结助剂；所述主晶相为(BaxCaySrz)m(ZrαTiβ)O3，其中0.01<x<0.2，0.4<y<0.8，0.1<z<0.4，0.95<m<1.01,0.7<α<1.0，0<β<0.1。本发明的介质材料符合EIA标准的COG特性，材料颗粒均一、粒度分布均匀、制备工艺简单、介电性能优良；该介质材料制作MLCC，匹配镍内电极，烧结晶粒小、均匀、致密，适合于制作薄介质、大容量、高可靠的MLCC产品。
Description
技术领域
本发明属于陶瓷材料技术领域，具体涉及一种陶瓷介质材料。
背景技术
MLCC是当前产量最大、发展最快的片式元器件之一，MLCC由内电极、陶瓷层和端电极三部分组成，陶瓷层介质材料与内电极以错位的方式堆叠，然后经过高温烧结烧制成形，再在芯片的两端封上金属层，得到了一个类似独石的结构体，故MLCC也常被称为“独石电容器”。
近年来，随着电子整机产品功能的扩大，对电子部件的要求；即使薄介质、大容量也要保证MLCC的可靠性；为了实现大容量，一方面介质材料具有高的介电常数；一方面烧结晶粒小，进而降低MLCC介质层的厚度和增加介质层数。
例如专利号为CN105174947A公报中提供了一种低温烧结薄介质多层陶瓷电容器用COG介质陶瓷材料，其含有主成分和添加剂，主成分为：(Ca1-xSrx)zZryO3，其中0.2≤x≤0.4，0.90≤y≤1.0，0.985≤z≤1.003；添加剂成分：Al2O3、MnCO3、MgO、TiO2、SiO2、BaCO3、ZnO中的至少二种或几种化合物；由于其烧后晶粒大，介质层不能薄层化，无法实现大容量。专利号为CN102964122A公报中提供了一种介电陶瓷组合物及其电子元器件制作方法，其介电陶瓷组合物包括主晶相、改性添加剂及烧结助剂，其主晶相的结构式为(MgγSrαCa(1-α-γ))m(TiβZr1-β)O3，其中0≤α≤1，0≤γ≤1,0≤β≤0.1,0.9≤m≤1.1，改性添加剂为MnCO3，MgCO3，Re2O3中的一种或几种，其中Re2O3为稀土氧化物，烧结助剂包括BaCO3，CaCO3，SiO2，Li2CO3，B2O3，Al2O3中的一种或几种，由于其介电常数只有20～30，偏低，不能实现大容量。
发明内容
为解决现有技术中的陶瓷材料在作为MLCC介质的过程中无法稳定地实现大容量的问题，本发明提供一种可用于MLCC的、稳定性可靠的陶瓷介质材料。
本发明所述陶瓷介质材料的功能性成分包括主晶相、改性添加剂和烧结助剂；所述主晶相为(BaxCaySrz)m(ZrαTiβ)O3，其中0.01<x<0.2，0.4<y<0.8，0.1<z<0.4，0.95<m<1.01,0.7<α<1.0，0<β<0.1。
本发明通过选择上述材料作为主晶相，可保证材料的介电常数维持在25-40之间，介电损耗低于10*10-4，25℃下绝缘电阻>10*1011Ω，-55℃～125℃温度范围内的温度变化率小且稳定。
作为优选的方案，所述主晶相为(BaxCaySrz)m(ZrαTiβ)O3，其中0.1<x<0.2，0.45<y<0.75，0.2<z<0.4，0.95<m<1.01,0.9<α<0.98，0.02<β<0.08。以上主晶相在应用的过程中取得了较好的效果。
优选的，按照物质的量计算，主晶相为100mol，改性添加剂为5～9.5mol，烧结助剂为4.5～7mol。在上述用量范围内，可保证主晶相的有效用量，进而保证材料的整体性能。
优选的，所述改性添加剂为MnCO3、MgTiO3、CaTiO3、Re2O3和RpOq中的一种或几种，其中Re是选自Y、Ho、Yb、Gd、Dy、Sm、Nd和Er中的至少一种稀土元素，R是选自W、Mo、V、Nb中的至少一种高价金属元素，其中p和q是正数，为保持电荷中性所需要。通过添加上述添加剂，可进一步保证材料的介电损耗低于4*10-4，125℃下绝缘电阻>1*1010Ω，-55℃～125℃温度范围内的温度特性满足EIA标准的COG特性，保证材料能与镍电极在还原气氛下共烧，且烧后的晶粒细、均匀。
优选的，所述改性添加剂的添加量为MnCO3 1.5～5.5mol，MgTiO3 0.2～0.45mol，CaTiO3 1.5～3.5mol，Re2O3 0～0.7mol，RpOq 0～0.08mol；其中，Re2O3和RpOq的添加量不同时为0。
优选的，所述烧结助剂是Al2O3、H3BO3和SiO2中的一种或多种。通过添加上述烧结助剂，可使材料在1200℃以下低温烧结，且瓷体致密。
优选的，所述烧结助剂的添加量为Al2O3 0.4～1.0mol，H3BO30.4～0.7mol，SiO22.5～5.5mol。
优选的，所述主晶相(BaxCaySrz)m(ZrαTiβ)O3采用固相法生产制得。
进一步优选的，对材料进行固相法生产的过程中煅烧的温度为1000℃～1100℃，这样可以维持材料的粒径在150-250nm之间。
优选的，所述固相法生产的过程中包括如下步骤：
选用纯度99.5％以上的BaCO3、CaCO3、SrCO3、ZrO2和TiO2，按照(BaxCaySrz)m(ZrαTiβ)O3，其中0.01<x<0.2，0.4<y<0.8，0.1<z<0.4，0.95<m<1.01,0.7<α<1.0，0<β<0.1组成的方式进行称量，之后将称量好的原材料进行湿式混合分散、干燥，再将干燥后的混合物进行煅烧，即得主晶相原料。
优选的，所述主晶相(BaxCaySrz)m(ZrαTiβ)O3的平均粒径为150-250nm，保证材料在烧结中的晶粒细，且具有高的耐压性能。
本发明的另一目的是保护一种独石电容器，所述独石电容器以本发明所述的陶瓷介质材料作为介质材料。
优选的，所述独石电容器的内电极为镍电极。
本发明具有如下有益效果：
1)本发明以低成本的固相法生产的(BaxCaySrz)m(ZrαTiβ)O3为主晶相，材料具有高的介电常数和优良的介电常数温度系数；以此为主晶相生产的介质材料符合COG特性要求，介电常数优异时可以保持在33-37之间，适合于制作介质层厚度小于5μm的薄介质大容量MLCC产品，电池容量可高达20nF以上，产品具有优异的介电性能和可靠性。
2)本发明进一步选择MnCO3、MgTiO3、CaTiO3、Re2O3、RpOq为改性添加剂，材料具有优良的介电性能和可靠性；选择Al2O3、H3BO3、SiO2为烧结助剂，材料可与镍电极匹配，可在还原气氛及低温度下烧结，有效抑制晶粒长大，使晶粒细小且均匀致密，具有高的介电强度；
3)本发明的材料不含有Pd等有害元素，满足欧盟ROHS要求。
具体实施方式
以下实施例用于说明本发明，但不用来限制本发明的范围。
实施例1～28
本实施例涉及陶瓷介质材料，所述介质材料以(Ba0.13Ca0.61Sr0.26)(Zr0.97Ti0.03)O3作为主晶相，按照表1中的比例加入所需的改性添加剂和烧结助剂；
表1：主晶相、改性添加剂和烧结助剂配方组成表
将实施例1～28中的混合物进行湿式混合分散、干燥过筛，即得介质材料粉末。
上述实施例中的主晶相材料由如下方法制备得到：选用纯度99.5％以上的BaCO3、CaCO3、SrCO3、ZrO2、TiO2原材料，按照(Ba0.13Ca0.61Sr0.26)(Zr0.97Ti0.03)O3组成的方式进行称量，之后将称量好的原材料进行湿式混合分散、干燥，再将干燥后的混合物在1050℃下进行煅烧，即得主晶相原料，颗粒的平均粒径约为200nm。
实施例29
本实施例涉及一种陶瓷介质材料，其主晶相为(Ba0.1Ca0.6Sr0.3)(Zr0.95Ti0.05)O3，其配方为主晶相100mol，MnCO3 3.5mol，MgTiO30.4mol，CaTiO3 2.5mol，Y2O3 0.7mol，Nb2O50.04mol，Al2O3 0.8mol，H3BO3 0.65mol，SiO2 4mol。
实施例30
本实施例涉及一种陶瓷介质材料，其主晶相为(Ba0.15Ca0.65Sr0.2)(Zr0.98Ti0.02)O3，其配方为主晶相100mol，MnCO3 3mol，MgTiO30.3mol，CaTiO3 2mol，Y2O3 0.6mol，V2O50.03mol，Al2O3 0.4mol，H3BO3 0.6mol，SiO2 5mol。
实施例31
本实施例涉及一种陶瓷介质材料，其主晶相为(Ba0.12Ca0.75Sr0.3)(Zr0.98Ti0.02)O3，其配方为主晶相100mol，MnCO3 3.5mol，MgTiO30.4mol，CaTiO3 2.5mol，Y2O3 0.7mol，Nb2O50.04mol，Al2O3 0.8mol，H3BO3 0.65mol，SiO2 4mol。
实施例32
本实施例涉及一种陶瓷介质材料，其主晶相为(Ba0.18Ca0.45Sr0.37)(Zr0.92Ti0.08)O3，其配方为主晶相100mol，MnCO3 3mol，MgTiO30.3mol，CaTiO3 2mol，Y2O3 0.6mol，V2O50.03mol，Al2O3 0.4mol，H3BO3 0.6mol，SiO2 5mol。
对比例1
与实施例1相比，其区别在于，所述主晶相为(Ba0.3Ca0.2Sr0.5)(Zr0.6Ti0.4)O3。
对比例2
与实施例1相比，其区别在于，所述主晶相为(Ba0.25Ca0.3Sr0.45)(Zr0.5Ti0.5)O3。
实验例
按照常用的MLCC制备工艺流程：浆料制备→流延→丝印→叠层→层压→切割→排胶→烧结→倒角→封端→烧端等进行MLCC制备；产品规格为0805C223J500N，介质层厚度为4μm，其丝印时使用镍内浆进行丝印，产品在1160℃的还原气氛下烧结，倒角后在产品的两端封上铜外电极，在800℃氮气保护气氛下对铜电极进行热处理，之后即可进行相关电性能的检测。
在室温25℃、45-65％RH条件下，利用Agilent 4284A电桥在1MHz、1Vrm下测试MLCC的容量C、介电损耗DF，根据介质层的厚度、有效电极面积、丝网系数、介质层数、容量计算介电常数；利用TH2683绝缘电阻测试仪在50VDC、60S条件下测试MLCC的绝缘电阻IR；利用CJ2671S耐压测试仪在充电电流＜20mA、施加电压速度200V/60S条件下测试MLCC的耐压BDV；利用高低温试验箱，在-55℃～125℃之间测试MLCC的温度系数TCC；利用老化试验箱在125℃、4倍工作电压条件下测试MLCC在500H下的老化性能HALT，每组测试40颗样品，将IR值为106Ω以下的样品设为失效，将每组40颗样品的失效颗数作为老化性能的评价结果；表2为由上述介质材料制得的MLCC性能参数表。
表2：介质材料制得的MLCC性能参数表
从表2可以看出，通过控制各成分的添加量，可以得出介电性能和老化性能优良的介质材料。
虽然，上文中已经用一般性说明、具体实施方式及试验，对本发明作了详尽的描述，但在本发明基础上，可以对之作一些修改或改进，这对本领域技术人员而言是显而易见的。因此，在不偏离本发明精神的基础上所做的这些修改或改进，均属于本发明要求保护的范围。
Claims (10)
1.一种陶瓷介质材料，其特征在于，所述陶瓷介质材料的功能性成分包括主晶相、改性添加剂和烧结助剂；所述主晶相为(BaxCaySrz)m(ZrαTiβ)O3，其中0.01<x<0.2，0.4<y<0.8，0.1<z<0.4，0.95<m<1.01,0.7<α<1.0，0<β<0.1。
2.根据权利要求1所述的介质材料，其特征在于，按照物质的量计算，主晶相为100mol，改性添加剂为5～9.5mol，烧结助剂为4.5～7mol。
3.根据权利要求1或2所述的介质材料，其特征在于，所述改性添加剂为MnCO3、MgTiO3、CaTiO3、Re2O3和RpOq中的一种或几种，其中Re是选自Y、Ho、Yb、Gd、Dy、Sm、Nd和Er中的至少一种稀土元素，R是选自W、Mo、V、Nb中的至少一种高价金属元素，其中p和q是正数，为保持电荷中性所需要。
4.根据权利要求3所述的介质材料，其特征在于，所述改性添加剂的添加量为MnCO3 1.5～5.5mol，MgTiO3 0.2～0.45mol，CaTiO3 1.5～3.5mol，Re2O3 0～0.7mol，RpOq 0～0.08mol；其中，Re2O3和RpOq的添加量不同时为0。
5.根据权利要求1或2所述的介质材料，其特征在于，所述烧结助剂是Al2O3、H3BO3和SiO2中的一种或多种。
6.根据权利要求5所述的介质材料，其特征在于，所述烧结助剂的添加量为Al2O3 0.4～1.0mol，H3BO3 0.4～0.7mol，SiO2 2.5～5.5mol。
7.根据权利要求1～4任一项所述的介质材料，其特征在于，所述主晶相(BaxCaySrz)m(ZrαTiβ)O3采用固相法生产制得，对材料进行固相法生产的过程中煅烧的温度为1000℃～1100℃。
8.根据权利要求7所述的介质材料，其特征在于，所述固相法生产的过程中包括如下步骤：
选用纯度99.5％以上的BaCO3、CaCO3、SrCO3、ZrO2和TiO2，按照(BaxCaySrz)m(ZrαTiβ)O3，其中0.01<x<0.2，0.4<y<0.8，0.1<z<0.4，0.95<m<1.01,0.7<α<1.0，0<β<0.1组成的方式进行称量，之后将称量好的原材料进行湿式混合分散、干燥，再将干燥后的混合物进行煅烧，即得主晶相原料。
9.根据权利要求1～8任一项所述的介质材料，其特征在于，所述主晶相(BaxCaySrz)m(ZrαTiβ)O3的平均粒径为150-250nm。
10.一种独石电容器，其特征在于，以权利要求1～9任一项所述的陶瓷介质材料作为介质材料。
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