CN110894160B - 电介质组合物及电子部件 - Google Patents
电介质组合物及电子部件 Download PDFInfo
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- CN110894160B CN110894160B CN201910840816.8A CN201910840816A CN110894160B CN 110894160 B CN110894160 B CN 110894160B CN 201910840816 A CN201910840816 A CN 201910840816A CN 110894160 B CN110894160 B CN 110894160B
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- dielectric composition
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- composite oxide
- oxide
- aluminum oxide
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- 239000000203 mixture Substances 0.000 title claims abstract description 92
- 239000002131 composite material Substances 0.000 claims abstract description 54
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 229910052735 hafnium Inorganic materials 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 229910052712 strontium Inorganic materials 0.000 claims description 4
- 239000010410 layer Substances 0.000 description 39
- 239000003985 ceramic capacitor Substances 0.000 description 34
- 239000000843 powder Substances 0.000 description 30
- 239000002245 particle Substances 0.000 description 28
- 239000002994 raw material Substances 0.000 description 19
- 238000010304 firing Methods 0.000 description 16
- 239000010955 niobium Substances 0.000 description 16
- 229910052788 barium Inorganic materials 0.000 description 12
- 239000007858 starting material Substances 0.000 description 12
- 230000005684 electric field Effects 0.000 description 11
- 239000010936 titanium Substances 0.000 description 11
- 239000011230 binding agent Substances 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 10
- 238000000034 method Methods 0.000 description 10
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 7
- 229910002113 barium titanate Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000013001 point bending Methods 0.000 description 7
- 239000002002 slurry Substances 0.000 description 7
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 239000003990 capacitor Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 239000004020 conductor Substances 0.000 description 5
- 239000011777 magnesium Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000003989 dielectric material Substances 0.000 description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 229910052758 niobium Inorganic materials 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 239000002612 dispersion medium Substances 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 229910016010 BaAl2 Inorganic materials 0.000 description 1
- 229910000807 Ga alloy Inorganic materials 0.000 description 1
- 229910001252 Pd alloy Inorganic materials 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000002003 electrode paste Substances 0.000 description 1
- 239000011267 electrode slurry Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910000449 hafnium oxide Inorganic materials 0.000 description 1
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000484 niobium oxide Inorganic materials 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000012856 weighed raw material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Abstract
一种电介质组合物，其中，含有：以通式AaBbC4O15+α表示的复合氧化物、和铝氧化物，A至少含有Ba，B至少含有Zr，C至少含有Nb，a为2.50以上且3.50以下，b为0.50以上且1.50以下。
Description
技术领域
本发明涉及电介质组合物及具备由该电介质组合物构成的电介质层的电子部件。
背景技术
装入电子设备的电子电路或电源电路中搭载有多个利用电介质体现的介电特性的层叠陶瓷电容器那样的电子部件。作为构成这种电子部件的电介质的材料(电介质材料)，广泛使用着钛酸钡系的电介质组合物。
但是，近年来，电子部件的用途扩大，即使在高电压的环境下，也要求电子部件充分发挥作用。但是，这种环境中，钛酸钡系的电介质组合物的介电特性降低，钛酸钡系的电介质组合物不能充分应对该环境。因此，要求即使在这种用途中也能够发挥较高的介电特性的电介质组合物。
作为钛酸钡系电介质组合物以外的电介质组合物，专利文献1公开有在以通式Ba6Ti2Nb8O30表示的强电介质材料中将Ba、Ti及Nb的一部分利用其它的元素置换的电介质组合物。
现有技术文献
专利文献
专利文献1：日本特开平3-274607号公报
发明内容
发明所要解决的技术问题
但是，专利文献1所记载的电介质组合物存在高电场强度下的相对介电常数较低的问题。
另外，搭载于电路基板的电子部件中，有时由于电路基板的挠曲等的变形而施加应力。因此，对电介质组合物要求机械强度高。
本发明是鉴于这种实际状况而研发的，其目的在于，提供一种电子部件，具备具有较高的机械强度且高电场强度下的相对介电常数较高的电介质组合物和由该电介质组合物构成的电介质层。
用于解决技术问题的技术方案
为了达成所述目的，本发明提供一种电介质组合物如下。
[1]一种电介质组合物，其中，
所述电介质组合物含有：以通式AaBbC4O15+α表示的复合氧化物、和Al的氧化物(铝氧化物)，
A至少含有Ba，B至少含有Zr，C至少含有Nb，
a为2.50以上且3.50以下，b为0.50以上且1.50以下。
[2]根据[1]所记载的电介质组合物，其中，
通式以(Ba1-xA1x)a(Zr1-yB1y)b(Nb1-zC1z)4O15+α表示，
A1含有选自Mg、Ca及Sr中的1种以上，B1含有选自Ti及Hf中的1种以上，C1含有Ta，
x为0.50以下，y为0.50以下，z为0.50以下。
[3]根据[1]或[2]所记载的电介质组合物，其中，
Al的氧化物(铝氧化物)为含有Ba的复合氧化物。
[4]根据[1]～[3]中任一项所记载的电介质组合物，其中，
密度为4.40g/cm3以上。
[5]一种电子部件，其中，
所述电子部件具备：含有[1]～[4]中任一项所记载的电介质组合物的电介质层、和电极层。
发明效果
根据本发明，能够提供具备具有较高的机械强度且高电场强度下的相对介电常数较高的电介质组合物和由该电介质组合物构成的电介质层的电子部件。
附图说明
图1是本发明一个实施方式的层叠陶瓷电容器的剖面图。
符号说明
1…层叠陶瓷电容器
10…元件主体
2…电介质层
3…内部电极层
4…外部电极
具体实施方式
以下，基于具体的实施方式，通过以下的顺序详细地说明本发明。
1.层叠陶瓷电容器
1.1层叠陶瓷电容器的整体结构
1.2电介质层
1.3内部电极层
1.4外部电极
2.电介质组合物
2.1复合氧化物
2.2 Al的氧化物(铝氧化物)
3.层叠陶瓷电容器的制造方法
4.本实施方式的效果
5.变形例
(1.层叠陶瓷电容器)
(1.1层叠陶瓷电容器的整体结构)
作为本实施方式的电子部件的一例的层叠陶瓷电容器1在图1中表示。层叠陶瓷电容器1具有电介质层2和内部电极层3交替层叠的结构的元件主体10。在该元件主体10的两端部形成有在元件主体10的内部交替配置的内部电极层3和分别导通的一对外部电极4。元件主体10的形状没有特别限制，但通常设为长方体状。另外，元件主体10的尺寸也没有特别限制，只要根据用途设为适当的尺寸即可。
(1.2电介质层)
电介质层2由后述的本实施方式的电介质组合物构成。其结果，具有电介质层2的层叠陶瓷电容器具有较高的机械强度，即使施加较高的电场强度(例如，25V/μm)，也能够呈现较高的相对介电常数(例如，200以上)。
电介质层2的每一层的厚度(层间厚度)没有特别限定，能够根据期望的特性或用途等任意设定。通常优选层间厚度为100μm以下，更优选为30μm以下。本实施方式中，另外，电介质层2的层叠数没有特别限定，但本实施方式中，例如优选为20以上。
(1.3内部电极层)
本实施方式中，内部电极层3以各端面交替露出于元件主体10的对置的两个端部的表面的方式层叠。
作为内部电极层3中含有的导电材料没有特别限定，但在与电介质层同时烧成的情况下，优选使用Pd、Pt、Ag-Pd合金等的公知的贵金属。另外，在通过溅射等形成内部电极层3的情况，或在电介质层的烧成后形成内部电极层3的情况下，作为导电材料，能够使用公知的贱金属。内部电极层3的厚度只要根据用途等适当决定即可。
(1.4外部电极)
外部电极4中含有的导电材料没有特别限定。例如只要使用Ni、Cu、Sn、Ag、Pd、Pt、Au或它们的合金、导电性树脂等公知的导电材料即可。外部电极4的厚度只要根据用途等适当决定即可。
(2.电介质组合物)
本实施方式的电介质组合物含有：至少含有Ba、Zr及Nb的复合氧化物和Al的氧化物(铝氧化物)。电介质组合物中，复合氧化物为主成分。具体而言，复合氧化物在本实施方式的电介质组合物100质量％中含有80质量％以上，优选含有90质量％以上。
另外，电介质组合物具有由上述复合氧化物构成的主成分颗粒和存在于主成分颗粒间的晶界。晶界中包含上述铝氧化物、从主成分扩散的成分等。
主成分颗粒的平均粒径优选为0.01～4μm的范围内。另外，主成分颗粒的平均粒径更优选为0.1μm以上。另一方面，主成分颗粒的平均粒径更优选为1μm以下。通过将主成分颗粒的平均粒径设为上述范围内，容易得到具有较高的机械强度的电介质组合物。
本实施方式中，主成分颗粒的平均粒径设为通过线法算出的线直径(corddiameter)的平均值。具体而言，在主成分颗粒出现的照片上任意画直线，利用该直线与晶界的交点的数去除该直线的长度，由此，算出线直径。对10条左右的直线算出线直径，并将其平均值设为主成分颗粒的平均粒径。
(2.1复合氧化物)
该复合氧化物中包含的氧以外的元素以价数为基准，分成3个元素组(“A”、“B”及“C”)，该复合氧化物以通式AaBbC4O15+α表示。
“A”为2价元素，并含有Ba。“B”为4价元素，并含有Zr。“C”为5价元素，并含有Nb。另外，上述通式中的“a”表示构成“C”的元素在通式中包含4个原子的情况下的“A”的原子数比例，上述通式中的“b”表示构成“C”的元素在通式中包含4个原子的情况下的“B”的原子数比例。
本实施方式中，该复合氧化物为弛豫强电介质，将以通式A3B1C4O15表示的复合氧化物设为基础。该复合氧化物中，价数不同的“B”和“C”以规定的比例占有结晶结构的规定的位点。认为起因于由此产生的局部的结构引起的不均质性，得到规定的介电特性。
以通式A3B1C4O15表示的复合氧化物的组成的自由度高，构成“A”、“B”及“C”的元素的原子数比例根据化学计量比进行某种程度变化。因此，以通式中的“C”的原子数4为基准时，“a”及“b”具有规定的范围。
本实施方式中，“a”为2.50以上，优选为2.70以上。另外，“a”为3.50以下，优选为3.30以下。
另外，本实施方式中，“b”为0.50以上，优选为0.70以上。另外，“b”为1.50以下，优选为1.30以下。
在“a”及“b”为上述范围内的情况下，以通式AaBbC4O15+α表示的复合氧化物呈现适当的介电特性。
此外，该复合氧化物中，氧(O)量有时根据“A”、“B”及“C”的结构比、氧缺陷等而变化。因此，本实施方式中，将以通式A3B1C4O15表示的复合氧化物中的化学计量比设为基准，将来自化学计量比的氧的偏差量以“α”表示。作为“α”的范围没特别限制，例如为-1以上1以下左右。
本实施方式中，“A”至少含有Ba，但也可以含有Ba以外的2价元素A1。“A1”优选含有选自Mg、Ca及Sr中的1种以上。除了Ba之外，在“A”中含有“A1”的情况下，本实施方式的复合氧化物能够以(Ba1-xA1x)aBbC4O15+α表示。式中，“x”优选为0.00以上。另一方面，“x”优选为0.50以下，更优选为0.25以下。即使“A”中含有“A1”，也可得到适当的介电特性。
此外，在作为“A1”含有Mg的情况下，存在相对介电常数降低的倾向。因此，从得到较高的相对介电常数的观点来看，在将构成“A”的原子总数设为1的情况下，Mg的原子数的比例优选为0.10以下，更优选为0.05以下。
另外，“B”至少含有Zr，但也可以含有Zr以外的4价元素B1。“B1”优选含有选自Ti及Hf中的1种以上。在除了Zr之外，“B”中还含有“B1”的情况下，本实施方式的复合氧化物能够以Aa(Zr1-yB1y)bC4O15+α表示。式中，“y”优选为0.00以上。另一方面，“y”优选为0.50以下，更优选为0.25以下。即使“B”中含有“B1”，也可得到适当的介电特性。
此外，在作为“B1”含有Ti的情况下，存在电阻率降低的倾向。因此，本实施方式中，优选Ti以得到本发明效果的程度而含有。具体而言，在将构成“B”的原子总数设为1的情况下，Ti的原子数的比例优选为0.20以下，更优选为0.10以下。从得到较高的电阻率的观点来看，优选实际上不含有Ti。在此，“实际上不含有Ti”是指，如果是不可避免的杂质所引起的量的程度，则也可以含有Ti。
另外，“C”至少含有Nb，但也可以含有Nb以外的5价元素C1。“C1”优选含有Ta。在除了Nb之外，“C”中还含有“C1”的情况下，本实施方式的复合氧化物能够以AaBb(Nb1-zC1z)4O15+α表示。式中，“z”优选为0.00以上。另一方面，“z”优选为0.50以下。
此外，在将构成“A”的原子总数设为1的情况下，优选Mg、Ca及Sr以外的2价元素A1的原子数的比例为0.10以下。在将构成“B”的原子总数设为1的情况下，优选Ti及Hf以外的4价元素B1的原子数的比例为0.10以下。在将构成“C”的原子总数设为1的情况下，优选Ta以外的5价元素C1的原子数的比例为0.10以下。
综上所述，通式AaBbC4O15+α能够以(Ba1-xA1x)a(Zr1-yB1y)b(Nb1-zC1z)4O15+α表示。“a”、“b”、“x”、“y”、“z”及“α”为上述范围。
(2.2Al的氧化物(铝氧化物))
本实施方式的电介质组合物除了上述复合氧化物以外，作为副成分，含有Al的氧化物(铝氧化物)。通过含有铝氧化物，电介质组合物的电阻率高，而且即使在施加较高的电场强度的情况下，也可得到良好的介电特性。另外，通过含有铝氧化物，能够缩小由上述复合氧化物构成的主成分颗粒的平均粒径。其结果，容易得到具有较高的机械强度的电介质组合物。作为铝氧化物，例如示例Al2O3。
铝氧化物主要具有作为烧结助剂的作用。即，通过在该电介质组合物的原料中含有铝氧化物的原料，在烧成时促进电介质组合物的烧结。因此，能够降低为了得到能够发挥充分的特性的程度的烧结性所需要的烧成温度。换言之，能够提高以相同的烧成温度烧成而得到的电介质组合物的密度。本实施方式中，电介质组合物的密度优选为4.40g/cm3，更优选为4.70g/cm3以上。
另外，随着电介质组合物的烧结性的提高，电介质组合物的特性也提高。因此，通过含有铝氧化物，即使烧成温度较低，电介质组合物的密度也变高，其结果，电阻率、相对介电常数等的介电特性提高。
本实施方式中，铝氧化物的含量相对于上述复合氧化物100质量％优选为0.5质量％以上，更优选为1质量％以上。另一方面，铝氧化物的含量相对于上述复合氧化物100质量％优选为20质量％以下，更优选为10质量％以下。
另外，氧化铝优选含有Ba，更优选为含有Al(铝)和Ba(钡)的复合氧化物。作为含有Al(铝)和Ba(钡)的复合氧化物，优选Ba(钡)的原子数比Al(铝)的原子数少。作为这种复合氧化物，例如，示例0.82BaO·6Al2O3、1.32BaO·6Al2O3、BaAl2O4，优选为1.32BaO·6Al2O3。
另外，本实施方式的电介质组合物也可以在实现本发明效果的范围内，除了上述复合氧化物及铝氧化物以外，含有其它的成分。其它的成分的含量优选为电介质组合物100质量％中20质量％以下，更优选为10质量％以下。特别是选自SiO2、MnO、CuO及Fe2O3中的1种以上的成分的含量优选合计为电介质组合物100质量％中0.5质量％以下。这是由于，这些成分降低电介质组合物的烧结性，其结果，电介质组合物的介电特性及物理特性降低。
(3.层叠陶瓷电容器的制造方法)
接着，以下说明图1所示的层叠陶瓷电容器1的制造方法的一例。
本实施方式的层叠陶瓷电容器1能够通过与现有的层叠陶瓷电容器同样的公知的方法制造。作为公知的方法，例如示例如下方法：使用包含电介质组合物的原料的浆料制作生坯芯片，将其烧成并制造层叠陶瓷电容器。以下，具体地说明制造方法。
首先，准备电介质组合物的初始原料。作为初始原料，能够使用构成上述电介质组合物的复合氧化物。另外，能够使用复合氧化物中包含的各金属的氧化物。另外，能够使用通过烧成而成为构成该复合氧化物的成分的各种化合物。作为各种化合物，例如示例：碳酸盐、草酸盐、硝酸盐、氢氧化物、有机金属化合物等。另外，作为铝氧化物的原料，与复合氧化物的原料一样，能够使用氧化物、各种化合物等。本实施方式中，上述初始原料优选为粉末。
准备的初始原料中，将复合氧化物的原料按规定的比例称重之后，使用球磨机等进行规定时间的湿式混合。将混合粉干燥后，在大气中以700～1300℃的范围进行热处理，得到复合氧化物的预烧粉末。另外，在铝氧化物为复合氧化物的情况下，优选将构成该复合氧化物的各成分的原料进行热处理并得到铝氧化物的预烧粉末。
接着，制备用于制作生坯芯片的浆料。将得到的预烧粉末、铝氧化物的原料粉末或铝氧化物的预烧粉末、粘合剂、溶剂混炼而涂料化，制备电介质层用浆料。粘合剂及溶剂只要使用公知的材料即可。另外，电介质层用浆料也可以根据需要含有增塑剂或分散剂等的添加物。
内部电极层用浆料通过将上述导电材料的原料、粘合剂、溶剂进行混炼而得到。粘合剂及溶剂只要使用公知的材料即可。内部电极层用浆料也可以根据需要含有常用材料或增塑剂或分散剂等的添加物。
外部电极用浆料能够与内部电极层用浆料同样地制备。
使用得到的各浆料，形成生坯片材及内部电极图案，将它们层叠而得到生坯芯片。
对于得到的生坯芯片，根据需要进行脱粘合剂处理。脱粘合剂处理条件只要设为公知的条件即可，例如，将保持温度优选设为200～350℃。
脱粘合剂处理后，进行生坯芯片的烧成，得到元件主体。本实施方式中，在空气中进行烧成。其它的烧成条件只要设为公知的条件即可，例如，优选将保持温度设为1200～1450℃。
构成上述那样得到的元件主体的电介质层的电介质组合物是上述电介质组合物。对该元件主体实施端面研磨，且涂布外部电极用浆料并烧接，形成外部电极4。然后，根据需要，在外部电极4的表面通过镀敷等形成包覆层。
这样，制造本实施方式的层叠陶瓷电容器。
(4.本实施方式的效果)
本实施方式中，电介质组合物含有具有上述组成的复合氧化物和铝氧化物。
该复合氧化物为弛豫强电介质，期待在较高的电场强度下，具有比钛酸钡系电介质高的相对介电常数。在含有复合氧化物作为主成分的电介质组合物致密的情况下，这种介电特性、物理特性等充分得到。但是，在电介质组合物不致密的情况下，即使具有相同的组成，它们的特性也存在恶化的倾向。
因此，促进复合氧化物的烧结的烧结助剂是重要的。作为烧结助剂，也可以使用SiO2、MnO等，但本实施方式中，通过电介质组合物含有铝氧化物，由此，电介质组合物充分烧结。其结果，特别是在高电场强度下得到较高的相对介电常数。另外，通过电介质组合物含有铝氧化物，能够缩小主成分颗粒的平均粒径。其结果，容易得到较高的机械强度。另一方面，即使本实施方式的电介质组合物含有SiO2、MnO等，该电介质组合物也未充分烧结，平均粒径也较大。其结果，电介质组合物的密度较低，介电特性及物理特性也不充分。
即，本发明效果是通过具有上述组成的复合氧化物与铝氧化物的组合而首先得到的效果。
为了得到这种效果，也可以将构成A的Ba利用上述2价元素A1以规定的比例置换，也可以将构成B的Zr利用上述4价元素B1以规定的比例置换，也可以将构成C的Nb利用上述5价元素C1以规定的比例置换。
另外，在铝氧化物为Al与Ba的复合氧化物的情况下，进一步提高上述效果。
(5.变形例)
上述实施方式中，说明了本发明的电子部件为层叠陶瓷电容器的情况，但本发明的电子部件不限定于层叠陶瓷电容器，只要是具有上述电介质组合物的电子部件均可。
另外，上述实施方式中，作为电子部件说明了以层叠陶瓷电容器为代表的层叠电子部件，但也可以是电介质层为1层的单层电子部件。
以上，说明了本发明的实施方式，但本发明不受上述实施方式的任何限定，也可以在本发明的范围内以各种方式改变。
实施例
以下，使用实施例及比较例更详细地说明本发明。但是，本发明不限定于以下的实施例。
(实验1)
首先，作为电介质组合物的主成分即复合氧化物的初始原料，准备碳酸钡(BaCO3)、碳酸钙(CaCO3)、碳酸锶(SrCO3)、氧化镁(MgO)、氧化锆(ZrO2)、氧化铪(HfO2)、氧化钛(TiO2)、氧化铌(Nb2O5)及氧化钽(Ta2O5)的粉末。另外，作为铝氧化物的初始原料，准备氧化铝(Al2O3)及碳酸钡(BaCO3)的粉末。以烧成后的电介质组合物具有表1所示的组成的方式，称重所准备的初始原料。此外，铝氧化物以相对于复合氧化物100质量％含有5质量％的方式称重。
另外，作为复合氧化物的比较例的初始原料，准备钛酸钡(BaTiO3)的粉末。另外，作为铝氧化物的比较例的初始原料，准备氧化硅(SiO2)、氧化锰(MnO)、氧化铜(CuO)及氧化铁(Fe2O3)的粉末。以烧成后的电介质组合物具有表1所示的组成的方式，称重所准备的初始原料。此外，SiO2等以相对于复合氧化物100质量％含有5质量％的方式称重。
接着，将称重的复合氧化物的初始原料的各粉末使用作为分散介质的离子交换水利用球磨机进行16小时湿式混合，将混合物干燥得到混合原料粉末。然后，将得到的混合原料粉末在大气中以保持温度900℃、保持时间2小时的条件进行热处理，得到复合氧化物的预烧粉末。
另外，在铝氧化物为Al与Ba的复合氧化物的情况下，将称重的Al2O3及BaCO3的各粉末使用作为分散介质的离子交换水利用球磨机进行16小时湿式混合，将混合物干燥，得到混合原料粉末。然后，将得到的混合原料粉末在大气中以保持温度1300℃、保持时间2小时的条件进行热处理，得到铝氧化物的预烧粉末。
向得到的复合氧化物的预烧粉末中，根据需要添加铝氧化物的预烧粉末或铝氧化物的原料粉末并称重，使用作为分散介质的离子交换水利用球磨机进行16小时湿式粉碎，并将粉碎物干燥。
相对于干燥的粉末100质量％，添加10质量％的含有6质量％的作为粘合剂的聚乙烯醇树脂的水溶液进行造粒，得到造粒粉。
将得到的造粒粉投入φ12mm的模具中，以0.6ton/cm2的压力进行预冲压成型，进一步以1.2ton/cm2的压力进行本冲压成型，得到圆盘状的生坯成型体。
将得到的生坯成型体在空气中烧成，得到圆盘状的烧结体。烧成条件中，将升温速度设为200℃/h，将保持温度设为1300℃，将保持时间设为2小时。
密度如以下测定。将烧成后的圆盘状的电容器试样的直径测定3个部位，得到直径R。接着，将圆盘状的电容器试样的厚度测定3个部位，得到厚度h。使用得到的R和h，算出圆盘状的电容器试样的体积V(＝1/4·π·R2·h)。这里的π表示圆周率。接着，测定圆盘状的电容器试样的质量m，并计算m/V，由此，得到圆盘状的电容器试样的密度。将对3个试样评价的密度的结果的平均值在表1中表示。
对得到的烧结体的表面进行镜面研磨，在空气中将升温速度设为200℃/h，将保持温度设为1200℃，将保持时间设为2小时，进行热蚀刻。在热蚀刻后通过SEM观察烧结体的表面，特定主成分颗粒，并如以下测定主成分颗粒的线直径。
在通过SEM拍摄的烧结体的表面的照片上画任意的线，计数横切线的晶界的数后，利用晶界的数去除线的长度，由此，计算线直径。线画10条，并在各个线中测定线直径。将测定的线直径的平均值设为主成分颗粒的平均粒径。将平均粒径在表1中表示。
向与测定线直径的烧结体不同的烧结体的两主面涂布In-Ga合金，形成一对电极，由此，得到圆盘状的陶瓷电容器的试样。
相对于圆盘状的陶瓷电容器试样，在基准温度(25℃)下，使用数字电阻仪表(ADVANTEST公司制造R8340)测定绝缘电阻。根据得到的绝缘电阻、有效电极面积、电介质层的厚度算出电阻率。电阻率越高越优选，本实施例中，将电阻率为1×109(Ω·m)以上的试样判断为良好。将结果在表1中表示。
接着，制作用于测定相对介电常数的试样。向上述中准备的复合氧化物的预烧粉末中，根据需要添加铝氧化物的预烧粉末或铝氧化物的原料粉末，得到电介质组合物的原料粉末。将得到的电介质组合物的原料粉末、粘合剂、溶剂混合，制作浆料。使用得到的浆料形成生坯片材，在其上印刷Pd电极，进行脱粘合剂处理，并在空气中进行烧成，制作层叠陶瓷电容器试样。Pd电极间的距离(电介质层的厚度)为5μm，电介质层的层数设为4层。
对于得到的层叠陶瓷电容器试样，在基准温度(25℃)下，在不施加直流电压的情况和施加直流电压的情况下，评价相对介电常数。首先，利用数字LCR仪表(YHP公司制造4284A)输出频率1kHz、输入信号电平(测定电压)1Vrms的信号，测定电容。然后，将未施加直流电压的情况，即，电场强度为0V/μm的情况的相对介电常数(无单位)基于电介质层的厚度、有效电极面积、通过测定得到的电容进行算出。接着，在以电场强度成为25V/μm的方式施加直流电压的状态下，通过上述测定条件测定电容。根据通过测定得到的电容，算出电场强度为25V/μm时的相对介电常数。相对介电常数越高越优选，本实施例中，将电场强度为25V/μm时的相对介电常数为200以上的试样判断为良好。将结果在表1中表示。
另外，如以下测定电介质组合物的机械强度。将得到的造粒粉投入5×53mm的模具，以0.6ton/cm2的压力进行预冲压成型，进一步以1.2ton/cm2的压力进行本冲压成型，制作生坯成型体。将得到的生坯成型体在空气中烧成，得到截面为长方形的棱柱的烧结体。烧成条件中，将升温速度设为200℃/h，将保持温度设为1300℃，将保持时间设为2小时。
将得到的烧结体以成为总长36mm以上且低于45mm、宽度4.0±0.1mm、厚度3.0±0.1mm的方式加工，进行倒角，并设为试验用的样品。相对于对各试样得到的10个样品，基于JIS R 1601中规定的试验方法进行3点弯曲试验。本实施例中，将3点弯曲强度的平均值为40MPa以上的试样判断为良好(○)，将低于40MPa的试样判断为不良(×)。将结果在表1中表示。
表1
“电阻率”的栏中的“aE+b”的记载表示“a×10b”。
根据表1能够确认到，将以组成式Ba3ZrNb4O15表示的复合氧化物的化学量论组成设为基准，含有以Ba及Zr的原子数相对于Nb的原子数的比例为上述范围的复合氧化物作为主成分，进一步与不含有铝氧化物的试样相比，含有铝氧化物的试样的电阻率、相对介电常数、密度及3点弯曲强度的任一项均良好。另外，能够确认到，作为铝氧化物，与Al2O3相比，Al与Ba的复合氧化物一方优选。
另一方面，能够确认到，与含有铝氧化物的试样相比，含有也可以用作烧结助剂的SiO2、MnO、CuO及Fe2O3的试样的电阻率、相对介电常数、密度及3点弯曲强度的任一项均差。另外，能够确认到，钛酸钡系电介质组合物不施加直流电压时的相对介电常数较大，但施加直流电压时的相对介电常数比含有铝氧化物的试样非常差。
(实验2)
除了以烧成后的电介质组合物具有表2所示的组成的方式，称重所准备的初始原料以外，通过与实验1相同的方法，制作圆盘状的陶瓷电容器试样。另外，对于制作的圆盘状的陶瓷电容器试样，通过与实验1相同的方法，评价电阻率、未施加直流电压时的相对介电常数、密度、平均粒径及3点弯曲强度。将结果在表2中表示。
表2
“电阻率”的栏中的“aE+b”的记载表示“a×10b”。
根据表2能够确认到，在使“a”及“b”在上述范围内变化的情况下，维持较高的电阻率及机械强度，且提高相对介电常数。
(实验3)
实施例3的试样中，除了以烧成后的电介质组合物具有表3所示的组成的方式，称重所准备的初始原料以外，通过与实验1相同的方法，制作圆盘状的陶瓷电容器试样。另外，相对于所制作的圆盘状的陶瓷电容器试样，通过与实验1相同的方法，评价密度、平均粒径及3点弯曲强度。将结果在表3中表示。
表3
根据表3能够确认到，即使将Ba、Zr及Nb利用上述元素以上述比例置换，密度也为同程度，且能够维持较高的机械强度。
(实验4)
除了以烧成后的电介质组合物具有表4所示的组成的方式，称重所准备的初始原料以外，通过与实验1相同的方法，制作圆盘状的陶瓷电容器试样及层叠陶瓷电容器试样。另外，对于所制作的圆盘状的陶瓷电容器试样及层叠陶瓷电容器试样，通过与实验1相同的方法，评价电阻率、不施加直流电压时的相对介电常数、密度、平均粒径及3点弯曲强度。将结果在表4中表示。
表4
“电阻率”的栏中的“aE+b”的记载表示“a×10b”。
根据表4能够确认到，在使“a”及“b”在上述范围内变化的情况下，或使Ba、Zr及Nb利用上述元素以上述比例置换的情况下，能够维持较高的电阻率及机械强度。
本实施例中，关于电阻率，对所谓的单层陶瓷电容器进行了评价，但对于层叠有电介质层和内部电极的层叠陶瓷电容器，也呈现与本实施例的电容器试样同样的电阻率。
Claims (4)
1.一种电介质组合物，其中，
所述电介质组合物含有：以通式AaBbC4O15+α表示的复合氧化物、和铝氧化物，
所述A至少含有Ba，所述B至少含有Zr，所述C至少含有Nb，
所述a为2.50以上且3.50以下，所述b为0.50以上且1.50以下，
所述铝氧化物为含有Ba的复合氧化物。
2.根据权利要求1所述的电介质组合物，其中，
所述通式以(Ba1-xA1x)a(Zr1-yB1y)b(Nb1-zC1z)4O15+α表示，
所述A1含有选自Mg、Ca及Sr中的1种以上，所述B1含有选自Ti及Hf中的1种以上，C1含有Ta，
所述x为0.50以下，所述y为0.50以下，所述z为0.50以下。
3.根据权利要求1或2所述的电介质组合物，其中，
密度为4.40g/cm3以上。
4.一种电子部件，其中，
所述电子部件具备：含有权利要求1～3中任一项所述的电介质组合物的电介质层、和电极层。
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| CN1790568A (zh) * | 2003-12-18 | 2006-06-21 | Tdk株式会社 | 电介质瓷器组合物、电子部件和它们的制造方法 |
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