CN113443905A - 电介质陶瓷组合物及电子部件 - Google Patents
电介质陶瓷组合物及电子部件 Download PDFInfo
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- CN113443905A CN113443905A CN202110313873.8A CN202110313873A CN113443905A CN 113443905 A CN113443905 A CN 113443905A CN 202110313873 A CN202110313873 A CN 202110313873A CN 113443905 A CN113443905 A CN 113443905A
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- 239000000203 mixture Substances 0.000 title claims abstract description 96
- 239000000919 ceramic Substances 0.000 title claims abstract description 83
- 239000011521 glass Substances 0.000 claims abstract description 60
- 239000011575 calcium Substances 0.000 claims abstract description 33
- VAWSWDPVUFTPQO-UHFFFAOYSA-N calcium strontium Chemical compound [Ca].[Sr] VAWSWDPVUFTPQO-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052839 forsterite Inorganic materials 0.000 claims abstract description 32
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 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 10
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 10
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims description 36
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- 239000000843 powder Substances 0.000 description 38
- 238000010304 firing Methods 0.000 description 24
- 238000000034 method Methods 0.000 description 22
- 239000002994 raw material Substances 0.000 description 13
- 238000012360 testing method Methods 0.000 description 13
- 238000013001 point bending Methods 0.000 description 12
- 238000002156 mixing Methods 0.000 description 9
- 239000013078 crystal Substances 0.000 description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 8
- 238000010298 pulverizing process Methods 0.000 description 8
- 238000001354 calcination Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000011777 magnesium Substances 0.000 description 7
- 229910052719 titanium Inorganic materials 0.000 description 7
- 229910052791 calcium Inorganic materials 0.000 description 6
- 238000009766 low-temperature sintering Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 239000007858 starting material Substances 0.000 description 6
- 239000000395 magnesium oxide Substances 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052909 inorganic silicate Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000007580 dry-mixing Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000010295 mobile communication Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229910002971 CaTiO3 Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Inorganic materials [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 1
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 239000011656 manganese carbonate Substances 0.000 description 1
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 1
- 229910000473 manganese(VI) oxide Inorganic materials 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920001483 poly(ethyl methacrylate) polymer Polymers 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing 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
- 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
- C04B35/16—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 silicates other than clay
- C04B35/20—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 silicates other than clay rich in magnesium oxide, e.g. forsterite
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- C01B33/00—Silicon; Compounds thereof
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- C01B33/22—Magnesium silicates
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- C01G23/006—Alkaline earth titanates
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Abstract
本发明的目的在于,提供一种Q值、共振频率的温度特性及强度全部良好的电介质陶瓷组合物。作为主成分,包含镁橄榄石及钛酸锶钙。主成分中的镁橄榄石的含有比例为84.0摩尔份以上且92.5摩尔份以下,钛酸锶钙的含有比例为7.5摩尔份以上且16.0摩尔份以下。钛酸锶钙中的(Sr+Ca)/Ti以摩尔比计为1.03~1.20。该电介质陶瓷组合物是相对于主成分和除含Li玻璃以外的副成分的合计100质量份,添加2质量份以上且10质量份以下的含Li玻璃而得到的。含Li玻璃是Al2O3的含量为1质量%以上且10质量%以下的玻璃。
Description
技术领域
本发明涉及一种电介质陶瓷组合物及电子部件。
背景技术
近年来,在需求不断增加的智能手机等移动体通信设备中,使用着数百MHz至数GHz程度的称为所谓的准微波的高频段。因此,在用于移动体通信设备的电子部件中也要求适于高频段下的使用的诸多特性。而且,寻求适于高频段下的使用的优异的LTCC(低温共烧陶瓷)材料。特别是为了获得各种特性优异的LTCC材料,提出了各种各样的方法。
在专利文献1中提出有一种电介质陶瓷组合物,通过将主成分及副成分的种类及含量设为特定的范围内,从而低介电常数、高Qf值及频率的温度特性良好,机械强度也高。在专利文献2中提出了一种低温烧结陶瓷组合物,通过相对于陶瓷粉末在特定的范围内含有低软化点玻璃,从而提高陶瓷的低温下的烧结性,并且使热膨胀系数及Q值良好。在专利文献3中提出有一种电介质陶瓷,将镁橄榄石系晶相和由包含Ti的氧化物构成的晶相设为主成分,且各自的主成分具有特定范围内的组成,从而相对介电常数低,温度特性的调整容易。
现有技术文献
专利文献
专利文献1:日本专利第4506802号公报
专利文献2:日本专利第4868663号公报
专利文献3:日本专利第4650111号公报
发明内容
发明所要解决的问题
但是,目前,要求提供一种Q值及强度更高,共振频率的温度特性良好的电介质陶瓷组合物。
本发明的目的在于,提供一种Q值、共振频率的温度特性、及强度全部良好的电介质陶瓷组合物。
用于解决技术问题的手段
为了达成上述目的,本发明提供一种电介质陶瓷组合物,其中,
作为主成分包含镁橄榄石及钛酸锶钙,
主成分中的镁橄榄石的含有比例为84.0摩尔份以上且92.5摩尔份以下,钛酸锶钙的含有比例为7.5摩尔份以上且16.0摩尔份以下,
所述钛酸锶钙中的(Sr+Ca)/Ti以摩尔比计为1.03~1.20,
该电介质陶瓷组合物是相对于所述主成分和除含Li玻璃之外的副成分的合计100质量份,添加2质量份以上且10质量份以下的含Li玻璃而得到的,
其中,所述含Li玻璃是Al2O3的含量为1质量%以上且10质量%以下的玻璃。
本发明的电介质陶瓷组合物通过具有上述结构,成为Q值、共振频率的温度特性、及强度全部良好的电介质陶瓷组合物。
所述钛酸锶钙中的Ca/(Sr+Ca)以摩尔比计可以为0.60以上且1.00以下。
所述含Li玻璃的SiO2的含量可以为25质量%以上且45质量%以下,BaO的含量可以为20质量%以上且40质量%以下,CaO的含量可以为10质量%以上且30质量%以下,Li2O的含量可以为10质量%以上且30质量%以下。
所述含Li玻璃可以实际上不含有B2O3。
相对于所述主成分100质量份,作为副成分,可以包含:以CuO换算计为0.5质量份以上且3.0质量份以下的含Cu化合物,以B2O3换算计为0.2质量份以上且3.0质量份以下的含B化合物,以Al2O3换算计为0.3质量份以上且3.0质量份以下的含Al化合物,以MnO换算计为0.05质量份以上且1.5质量份以下的含Mn化合物。
本发明提供一种电子部件,其具有上述任一项的电介质陶瓷组合物。
具体实施方式
以下,对用于适当实施本发明的实施方式进行说明。
本实施方式的电介质陶瓷组合物中作为主成分包含镁橄榄石及钛酸锶钙。镁橄榄石是指由氧化镁及二氧化硅构成的化合物(Mg2SiO4)。镁橄榄石中的MgO:SiO2可设为以摩尔比计为1.9:1.1~2.1:0.9的范围内。另外,钛酸锶钙也可表示为(Sr1-xCax)yTiO2+y。本实施方式中,为0≤x≤1,1.03≤y≤1.20。即,钛酸锶钙也可以仅由钛酸锶构成,也可以仅由钛酸钙构成。
作为主成分包含镁橄榄石及钛酸锶钙是指将电介质陶瓷组合物整体设为100质量%,合计包含80质量%以上的镁橄榄石及钛酸锶钙。也可以包含主成分以外的成分作为副成分。
主成分中的镁橄榄石的含有比例为84.0摩尔份以上且92.5摩尔份以下,钛酸锶钙的含有比例为7.5摩尔份以上且16.0摩尔份以下。在主成分中的这些化合物的含有比例为上述的范围外的情况下,电介质陶瓷组合物的共振频率的温度依赖性过大。即,电介质陶瓷组合物的温度变化引起的共振频率的变化率的绝对值过大。另外,钛酸锶钙的含有比例越大,电介质陶瓷组合物的Q值越小。特别是后述的Ca/(Sr+Ca)越小,Q值越容易变小。
钛酸锶钙中的(Sr+Ca)/Ti以摩尔比计为1.03~1.20。在(Sr+Ca)/Ti过小的情况下,电介质陶瓷组合物的强度降低。在(Sr+Ca)/Ti过大的情况下,电介质陶瓷组合物的Q值降低。
钛酸锶钙中的Ca/(Sr+Ca)没有特别限制,以摩尔比计可以为0.60以上且1.00以下,也可以为0.80以上且1.00以下,也可以为0.89以上且1.00以下。即,也可以为0.60≤x≤1.00,也可以为0.80≤x≤1.00,也可以为0.89≤x≤1.00。Ca/(Sr+Ca)越大,电介质陶瓷组合物的Q值、强度均有变大的倾向。
另外,本实施方式的电介质陶瓷组合物是相对于上述主成分和除含Li玻璃以外的副成分的合计100质量份,添加2质量份以上且10质量份以下的含Li玻璃而得到的电介质陶瓷组合物。此外,将包含的Li2O的含量为5质量%以上的玻璃作为含Li玻璃。在含Li玻璃的添加量过少的情况下,难以低温烧结。在含Li玻璃的添加量过多的情况下,Q值降低且介电损耗变大。含Li玻璃的添加量优选为3质量份以上且7质量份以下。
本实施方式的含Li玻璃中,将含Li玻璃整体作为100质量%,包含1质量%以上且10质量%以下的Al2O3。
通过含Li玻璃中的Al2O3的含量为1质量%以上,可获得在制作含Li玻璃时难以结晶化且难以失透的含Li玻璃。另外,通过含Li玻璃中的Al2O3的含量为10质量%以下,从而在制作电介质陶瓷组合物时(烧成时),容易低温烧结。
本实施方式的含Li玻璃例如也可以为SiO2-BaO-CaO-Al2O3-Li2O系玻璃。而且,将含Li玻璃整体设为100质量%,SiO2的含量可以为25质量%以上且45质量%以下,BaO的含量可以为20质量%以上且40质量%以下,CaO的含量可以为10质量%以上且30质量%以下,Al2O3的含量可以为1质量%以上且10质量%以下,Li2O的含量可以为10质量%以上且30质量%以下。
本实施方式的含Li玻璃也可以实际上不含有B2O3。实际上不含有B2O3是指将含Li玻璃整体设为100质量%,B2O3的含量为0.1质量%以下(包含0质量%)。在本实施方式的电介质陶瓷组合物中,在含Li玻璃包含B2O3的情况下,Q值容易降低,介电损耗容易变大。另外,在含Li玻璃为SiO2-BaO-CaO-Al2O3-Li2O系玻璃的情况下,SiO2、BaO、CaO、Al2O3、Li2O、B2O3以外的成分的种类及含有比例没有特别限制。例如,也可以合计包含1质量%以下的SrO等。
本实施方式的电介质陶瓷组合物除了主成分及含Li玻璃之外,还包含副成分。副成分的种类及含量没有特别限制。例如,相对于主成分100质量份,可以包含以CuO换算计为0.5质量份以上且3.0质量份以下的含Cu化合物,包含以B2O3换算计为0.2质量份以上且3.0质量份以下的含B化合物,包含以Al2O3换算计为0.3质量份以上且3.0质量份以下的含Al化合物,包含以MnO换算计为0.05质量份以上且1.5质量份以下的含Mn化合物。此外,作为含各元素的化合物,可以示例各元素的氧化物、碳酸盐、硝酸盐、草酸盐、氢氧化物、硫化物、有机金属化合物等。
本实施方式的电介质陶瓷组合物通过包含含Cu化合物作为副成分,从而容易低温烧结,并且烧结体的Q值容易提高。另外,含Cu化合物的含量可以为相对于主成分100质量份以CuO换算计为0.5质量份以上且2.5质量份以下。含Cu化合物的含量越少,越难以低温烧结。含Cu化合物的含量越多,烧结体的Q值越容易降低。
本实施方式的电介质陶瓷组合物通过包含含B化合物作为副成分,从而容易低温烧结,并且烧结体的Q值容易提高。另外,含B化合物的含量也可以为相对于主成分100质量份以B2O3换算计为0.2质量份以上且2.5质量份以下。含B化合物的含量越少,越难以低温烧结。含B化合物的含量越多,Q值越容易降低。
本实施方式的电介质陶瓷组合物通过包含含Mn化合物作为副成分,从而容易低温烧结,且烧结体的Q值容易提高。另外,含Mn化合物的含量也可以为相对于主成分100质量份以MnO换算计为0.05质量份以上且1.0质量份以下。通过含Mn化合物的含量为上述的范围内,尤其是为0.05质量份以上,从而容易低温烧结。而且,Q值容易提高。
此外,本实施方式的电介质陶瓷组合物也可以包含上述以外的副成分,但优选实际上不含有含Zn化合物。实际上不含有含Zn化合物是指在对烧成后的烧结体进行XRD测定的情况下,观察不到ZnO的峰值,并且也观察不到由镁橄榄石及ZnO构成的化合物的峰值、由含Li玻璃及ZnO构成的化合物的峰值、及由各副成分及ZnO构成的化合物的峰值。另外,在该情况下,将主成分作为100质量份,含Zn化合物的含量以氧化物(ZnO)换算计大致低于0.05质量份。通过实际上不含有含Zn化合物,本实施方式的电介质陶瓷组合物的Q值及耐湿性提高。
另外,就本实施方式的电介质陶瓷组合物而言,上述以外的副成分的含量的合计没有特别限制,可以在不损坏本申请发明效果的范围内含有。例如,也可以将电介质陶瓷组合物整体设为100质量份,以氧化物换算计合计含有10质量份以下。
此外,在本实施方式中,烧成是指以烧结为目的的加热处理,烧成温度是在加热处理时将电介质陶瓷组合物暴露的气氛的温度。
本实施方式的电介质陶瓷组合物的介电特性能够根据该烧结体的Qf值、共振频率温度特性(温度变化引起的共振频率的变化率τf)、及相对介电常数εr进行评价。Qf值、相对介电常数εr能够根据日本工业标准“微波用精细陶瓷的介电特性的试验方法”(JIS R16271996年度)进行测定。
本实施方式的电介质陶瓷组合物中,作为主成分包含Mg2SiO4(镁橄榄石)。Mg2SiO4的单体中的Qf值为200000GHz以上,且介电损耗小,因此,具有降低电介质陶瓷组合物的介电损耗的功能。另外,Mg2SiO4的相对介电常数εr低至6~7左右,因此,还具有降低电介质陶瓷组合物的相对介电常数εr的功能。在此,介电损耗是高频的能量的一部分成为热而扩散的现象。介电损耗的大小由实际的电流和电压的相位差、与理想的电流和电压的相位差(90度)之差即损耗角度δ的正切tanδ的倒数Q(Q=1/tanδ)表示。电介质陶瓷组合物的介电损耗的评价使用该Q值和共振频率f的积即Qf值。如果介电损耗变小,则Qf值变大,如果介电损耗变大,则Qf值变小。介电损耗是指高频器件的功率损耗,因此,优选电介质陶瓷组合物的Qf值较大。但是,本实施方式中,将试验时的共振频率f看作大致一定,介电损耗的评价中使用Q值。
关于共振频率温度特性的评价,可以测定两个温度下的共振频率,并评价将一个温度设为基准温度的情况下的温度变化引起的共振频率的变化率τf。可以说τf的绝对值越小,共振频率温度特性越良好。
评价本实施方式的电介质陶瓷组合物的强度的方法没有特别限制。例如,可以评价三点弯曲强度。
以下,对本实施方式的电介质陶瓷组合物及烧结体的制造方法的一例进行说明。本实施方式的电介质陶瓷组合物及烧结体的制造方法包含以下的工序。
(a)镁橄榄石结晶粉末的制作工序:通过将氧化镁的原料粉末和二氧化硅的原料粉末混合并进行热处理,制作镁橄榄石结晶粉末;
(b)钛酸锶钙粉末的准备工序:准备钛酸锶钙粉末;
(c)含Li玻璃的准备工序:准备含Li玻璃;
(d)煅烧工序:向镁橄榄石结晶粉末及钛酸锶钙粉末中添加副成分的原料粉末并进行煅烧;
(e)电介质陶瓷组合物的制作工序:向煅烧后的粉末中添加含Li玻璃进行粉碎,从而获得电介质陶瓷组合物;
(f)烧成工序:烧成电介质陶瓷组合物,从而获得电介质陶瓷组合物的烧结体。
<镁橄榄石结晶粉末的制作工序>
镁橄榄石结晶粉末的准备方法没有特别限制。例如,首先,作为初始原料准备MgO、SiO2,以制作Mg2SiO4的方式进行称量。接着,对于称重的初始原料使用球磨机进行混合、粉碎之后,进行煅烧。煅烧后的粉末成为镁橄榄石粉末。另外,也可以将市售的镁橄榄石粉碎,获得镁橄榄石粉末。该镁橄榄石粉末被用作电介质陶瓷组合物的主成分粉末。
<钛酸锶钙粉末的准备工序>
钛酸锶钙粉末的准备方法没有特别限制。例如,作为初始原料准备SrCO3、CaCO3及TiO2,以(Sr+Ca)/Ti及Ca/(Sr+Ca)成为规定的范围内的方式组合并称重,并使用球磨机进行混合、粉碎,之后进行煅烧,从而合成钛酸锶钙粉末。另外,也可以将(Sr+Ca)/Ti及Ca/(Sr+Ca)为规定的范围内的市售的钛酸锶钙粉碎,获得钛酸锶钙粉末。该钛酸锶钙粉末可被用作电介质陶瓷组合物的主成分粉末。
<含Li玻璃的准备工序>
含Li玻璃的准备方法没有特别限制。例如,作为原料准备含Li玻璃中含有的各成分的初始原料,以成为期望的比例的方式称重并混合。混合的方法没有特别限制。例如也可以进行10小时以上且30小时以下的干式混合。接着,将该混合物以1500℃熔融,通过转出(roll out)获得约0.5mm厚的带状成形体。熔融中使用的炉没有特别限制。例如也可以是连续熔融炉。也可以将该带状成形体利用球磨机进行干式粉碎后,一边进行分级一边利用球磨机进行粉碎至平均粒径成为0.5μm以上且5μm以下。另外,也可以使用具有规定范围内的组成的市售的含Li玻璃。
<煅烧工序>
在煅烧工序中,将主成分的粉末及副成分的原料粉末称重规定量之后,将它们混合并进行热处理。作为副成分的原料,可使用通过在后述的煅烧等热处理中进行烧成而成为氧化物的化合物。作为通过烧成而成为上述氧化物的化合物,例如可示例:碳酸盐、硝酸盐、草酸盐、氢氧化物、硫化物、有机金属化合物等。此外,关于副成分,也可以作为主成分的粉末的杂质进行添加。此外,副成分的各原料的称重以电介质陶瓷组合物中的各副成分的含量(质量份)成为期望值的方式进行。煅烧条件没有特别限制。
混合能够通过干式混合或湿式混合等混合方式进行,例如,能够利用球磨机等混合分散机并通过使用了纯净水、乙醇等溶剂的混合方式进行。混合时间只要设为4小时以上且24小时以下程度即可。
优选以100℃以上且200℃以下,更优选为120℃以上且140℃以下的干燥温度,将原料混合粉末干燥12小时以上且36小时以下程度。
干燥的原料混合粉末例如以600℃以上且850℃以下进行热处理(煅烧)1小时以上且10小时以下。这样,通过以烧成温度以下的温度进行煅烧工序中的煅烧,从而能够抑制原料混合粉末中的镁橄榄石熔融,并且能够在电介质陶瓷组合物中以结晶的形式含有镁橄榄石。
<电介质陶瓷组合物的制作工序>
相对于煅烧后的粉末添加含Li玻璃并粉碎,制成电介质陶瓷组合物。具体的方法没有特别限制。例如,也可以在相对于煅烧后的粉末添加含Li玻璃并混合粉碎后,进行干燥。粉碎可以通过干式粉碎或湿式粉碎等粉碎方式来进行。粉碎时间只要设为4小时以上且24小时以下程度即可。粉碎后的粉末的干燥优选以80℃以上且200℃以下,更优选以100℃以上且140℃以下的处理温度进行12小时以上且36小时以下程度。
通过上述的方法,使电介质陶瓷组合物的主成分和副成分均匀地混合,能够获得材质均匀的电介质陶瓷组合物。
获得电介质陶瓷组合物之后,将电介质陶瓷组合物转移至烧成的烧成工序中。
<烧成工序>
在烧成工序中,将获得的电介质陶瓷组合物进行烧成,获得烧结体。烧成例如优选在空气中那样的氧气氛中进行。烧成温度没有特别限制。例如,也可以为800℃以上且1100℃以下,也可以为800℃以上且950℃以下。
使用本实施方式的电介质陶瓷组合物的制造方法获得的电介质陶瓷组合物即使以800℃以上且1100℃以下的低温进行烧成,也能够充分提高相对密度。因此,本实施方式的电介质陶瓷组合物能够在烧成工序中以低温烧成,并能够确保电介质陶瓷组合物的烧结性。然后,成为Q值、温度变化引起的共振频率的变化率τf以及强度全部优异的电介质陶瓷组合物。因此,本实施方式的电介质陶瓷组合物能够适用作构成过滤器、谐振器、电容器、电路基板等电子部件的一部分的电介质层。
以上,对本发明的电介质陶瓷组合物优选的实施方式进行了说明,但本发明未必限定于上述的实施方式。例如,也可以在不大幅度损坏介电特性及强度的范围内包含其它的化合物。
实施例
以下,举出实施例及比较例更具体地说明本发明,但本发明不限定于以下的实施例。
<电介质陶瓷组合物的制作>
关于镁橄榄石结晶粉末(Mg2SiO4粉末),分别进行称量作为原料的MgO及SiO2以使得Mg的摩尔数成为Si的摩尔数的2倍,并使用球磨机进行混合、粉碎后,进行煅烧,由此合成。
关于钛酸锶钙粉末,首先,作为初始原料,准备了高纯度的SrCO3、CaCO3及TiO2。接着,将这些初始原料以成为表1所示的(Sr+Ca)/Ti及Ca/(Sr+Ca)的方式组合并称量。使用球磨机进行混合、粉碎后,进行煅烧,由此合成钛酸锶钙粉末。
接着,将获得的镁橄榄石结晶粉末及钛酸锶钙粉末以加料组成成为表1所示的主成分组成的方式进行混合。然后,相对于主成分100质量份,作为副成分添加1.5质量份的CuO、1.0质量份的B2O3、以MnO换算计为0.3质量份的MnCO3、1.0质量份的Al2O3。然后,以800℃煅烧2小时,获得煅烧体。然后,以表1所示的添加量添加含Li玻璃。此外,MnCO3在前述的煅烧时及/或后述的烧成时变化成MnO。另外,表1所记载的含Li玻璃的添加量是将主成分和除含Li玻璃之外的副成分的合计以氧化物换算计设为100质量份的情况下的添加量。另外,作为含Li玻璃,制作并使用了表1所示的组成的SiO2-BaO-CaO-Al2O3-Li2O系玻璃。
含Li玻璃通过下述的方法制作。首先,作为含Li玻璃的原料,将SiO2、Al2O3、B2O3(仅实施例13)、CaCO3、BaCO3及Li2CO3以氧化物换算计成为表1所示的比例的方式称重,并进行2小时的干式混合。接着,获得的该混合物利用连续熔解炉以1500℃熔融后,通过转出(rollout),获得约0.5mm厚的带状成形体。将该带状成形体利用球磨机干式粉碎至100目以下后,一边进行风力分级,一边利用ZrO2球磨机进行粉碎至平均粒径成为3μm。然后,获得添加于煅烧后的主成分及副成分的含Li玻璃。
此外,想要制作比较例5所示的组成的含Li玻璃,但结晶析出并失透,因此,对于比较例5不进行以下的试验。此外,认为假设在使用失透的含Li玻璃制作电介质陶瓷组合物的情况下烧结不足。
另外,向上述的混合物中添加10质量%的作为丙烯酸树脂的聚(甲基丙烯酸乙酯)作为有机粘合剂后,通过刮刀法进行片材成型,制作多个片材成型体。将多个片材成型体层叠后进行冲压,并成型为基板状,由此制作片材层叠成型体。将该片材层叠成型体以期望的尺寸切断,获得芯片。在进行芯片的倒角之后,以烧成温度900℃烧成2小时,从而制作了电介质陶瓷组合物的烧结体。有机粘合剂的混合量通过各实施例及比较例的组成适当变化。
测定获得的各实施例及比较例的电介质陶瓷组合物的烧结体的相对介电常数εr、Q值、温度变化引起的共振频率的变化率τf、及三点弯曲强度。
<烧结密度>
烧成后的试验片以大致成为4.5mm×3.2mm×0.8mm的方式切断加工,并利用测微计精密地测定各方向的尺寸。另外,将利用电子天平测定切断加工后的试验片的质量所得到的切断加工后的试验片的质量除以切断加工后的试验片的体积,由此测定了烧结密度。相对于根据将Mg2SiO4的密度设为3.2g/cm3,将CaTiO3的密度设为4.1g/cm3,将SrTiO3的密度设为5.1g/cm3的各化合物的含有比率算出的理论密度,在烧结密度为90%以下的情况下判定为差(不可)。烧结密度差(不可)的比较例6、7的烧结不足,因此,不能进行以下所记载的评价。
<相对介电常数εr,Q值>
烧结体的相对介电常数εr及Q值根据日本工业标准“微波用精细陶瓷的介电特性的试验方法(JIS R1627 1996年度)”进行测定。具体而言,制作了10mmφ×5mm的圆柱(粒料),通过两端短路形电介质谐振器法算出相对介电常数εr及介质损耗角正切(dissipation factor)tanδ。而且,设为1/tanδ=Q。在为Q≥1500的情况下,Q值良好。更优选Q≥1600的情况。
<温度变化引起的共振频率的变化率τf>
对于上述的粒料,根据日本工业标准“微波用精细陶瓷的介电特性的试验方法(JIS R1627 1996年度)”以25℃和85℃测定共振频率,将基准温度设为25℃的情况下的温度变化引起的共振频率的变化率设为τf。在τf的绝对值为20ppm/℃以下,即τf为-20ppm/℃以上且20ppm/℃以下的情况下,共振频率温度特性良好。
<三点弯曲强度(抗折强度)>
以各电介质陶瓷的试验片的厚度成为0.4mm左右,宽度成为2.6mm左右的方式进行切断加工,对获得的试验片测定三点弯曲强度。在三点弯曲强度的测定中使用了测定器(商品名:5543,Instron Corporation制造)。在测定三点弯曲强度时,支承试验片的两点间的距离(夹具距离)设为15mm,且三点弯曲强度的测定速度设为0.5mm/min。将对30个试验片测定三点弯曲强度而获得的值的平均值(单位:MPa)设为三点弯曲强度的测定值。此外,将三点弯曲强度的测定值为250MPa以上的情况设为良好。
根据表1,所有的组成为本申请发明的范围内的实施例中,即使以900℃的低温烧成,也能够获得充分的烧结密度。而且,Q值、τf及三点弯曲强度全部良好。
与之相对,任一副成分的组成为本申请发明的范围外的比较例1~4、8中,Q值、τf及三点弯曲强度的任一项以上都不好。
另外,实测并确认了实施例3中的煅烧后的含Li玻璃添加前的煅烧体的组成。具体而言,将煅烧体粉碎进行粉末化,使用理学电机制PrimusIV进行荧光X射线分析。将实施例3中的加料组成及煅烧体的分析值在表2中示出。此外,主成分组成的分析值、即镁橄榄石的含量的分析值(单位:摩尔%)及钛酸锶钙的含量的分析值(单位:摩尔%)根据煅烧体中的Mg的分析值及Ti的分析值来计算。(Sr+Ca)/Ti及Ca/(Sr+Ca)是根据Sr的分析值、Ca的分析值及Ti的分析值计算得到的摩尔比。
【表2】
根据表2能够确认到,本实施例中,在加料组成和煅烧体的分析值中,主成分组成、(Sr+Ca)/Ti及Ca/(Sr+Ca)大致一致。
此外,对于煅烧体的ZnO的含量,也同样通过荧光X射线分析进行了确认,结果能够确认到相对于上述主成分100质量份,低于0.05质量份,实际上不含有。
Claims (6)
1.一种电介质陶瓷组合物,其中,
作为主成分包含镁橄榄石及钛酸锶钙,
主成分中的镁橄榄石的含有比例为84.0摩尔份以上且92.5摩尔份以下,钛酸锶钙的含有比例为7.5摩尔份以上且16.0摩尔份以下,
所述钛酸锶钙中的(Sr+Ca)/Ti以摩尔比计为1.03~1.20,
所述电介质陶瓷组合物是相对于所述主成分和除含Li玻璃之外的副成分的合计100质量份,添加2质量份以上且10质量份以下的含Li玻璃而得到的,
其中,所述含Li玻璃为Al2O3的含量为1质量%以上且10质量%以下的玻璃。
2.根据权利要求1所述的电介质陶瓷组合物,其中,
所述钛酸锶钙中的Ca/(Sr+Ca)以摩尔比计为0.60以上且1.00以下。
3.根据权利要求1或2所述的电介质陶瓷组合物,其中,
所述含Li玻璃中,SiO2的含量为25质量%以上且45质量%以下,BaO的含量为20质量%以上且40质量%以下,CaO的含量为10质量%以上且30质量%以下,Li2O的含量为10质量%以上且30质量%以下。
4.根据权利要求1或2所述的电介质陶瓷组合物,其中,
所述含Li玻璃实际上不含有B2O3。
5.根据权利要求1或2所述的电介质陶瓷组合物,其中,
相对于所述主成分100质量份,作为所述副成分,包含:以CuO换算计为0.5质量份以上且3.0质量份以下的含Cu化合物,以B2O3换算计为0.2质量份以上且3.0质量份以下的含B化合物,以Al2O3换算计为0.3质量份以上且3.0质量份以下的含Al化合物,以MnO换算计为0.05质量份以上且1.5质量份以下的含Mn化合物。
6.一种电子部件,其具有权利要求1~5中任一项所述的电介质陶瓷组合物。
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