CN107879736A - 铁氧体组合物及电子部件 - Google Patents
铁氧体组合物及电子部件 Download PDFInfo
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- CN107879736A CN107879736A CN201710879832.9A CN201710879832A CN107879736A CN 107879736 A CN107879736 A CN 107879736A CN 201710879832 A CN201710879832 A CN 201710879832A CN 107879736 A CN107879736 A CN 107879736A
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 60
- 239000000203 mixture Substances 0.000 title claims abstract description 52
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 150000003377 silicon compounds Chemical class 0.000 claims abstract description 24
- 239000004615 ingredient Substances 0.000 claims abstract description 22
- 150000001869 cobalt compounds Chemical class 0.000 claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011787 zinc oxide Substances 0.000 claims abstract description 14
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 13
- 150000001622 bismuth compounds Chemical class 0.000 claims abstract description 11
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 11
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 11
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 11
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 11
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims abstract description 10
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 9
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 6
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims 1
- 229910052802 copper Inorganic materials 0.000 claims 1
- 230000035699 permeability Effects 0.000 abstract description 46
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 abstract description 24
- 229960004643 cupric oxide Drugs 0.000 abstract description 11
- 239000000463 material Substances 0.000 description 15
- 230000000630 rising effect Effects 0.000 description 15
- 230000004523 agglutinating effect Effects 0.000 description 12
- 239000002994 raw material Substances 0.000 description 12
- 150000001875 compounds Chemical class 0.000 description 11
- 238000000034 method Methods 0.000 description 11
- 239000000843 powder Substances 0.000 description 8
- 238000001354 calcination Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- 239000004020 conductor Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000012298 atmosphere Substances 0.000 description 5
- 229910017052 cobalt Inorganic materials 0.000 description 5
- 239000010941 cobalt Substances 0.000 description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000000605 extraction Methods 0.000 description 5
- 238000009766 low-temperature sintering Methods 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- 241000656145 Thyrsites atun Species 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 229910001252 Pd alloy Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 229910000428 cobalt oxide Inorganic materials 0.000 description 2
- 230000002508 compound effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002902 organometallic compounds Chemical class 0.000 description 2
- 150000003891 oxalate salts Chemical class 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910001020 Au alloy Inorganic materials 0.000 description 1
- 229910017518 Cu Zn Inorganic materials 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910017752 Cu-Zn Inorganic materials 0.000 description 1
- 229910017943 Cu—Zn Inorganic materials 0.000 description 1
- 206010022971 Iron Deficiencies Diseases 0.000 description 1
- 229910018054 Ni-Cu Inorganic materials 0.000 description 1
- 229910018481 Ni—Cu Inorganic materials 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
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Abstract
本发明提供一种初始磁导率、比电阻、频率特性及温度特性良好的铁氧体组合物以及使用了上述铁氧体组合物的电子部件。本发明为一种具有主成分和副成分的铁氧体组合物。主成分由以Fe2O3换算为18~30摩尔%的氧化铁、以CuO换算为4~14摩尔%的氧化铜、以ZnO换算为0~6摩尔%的氧化锌、余量为氧化镍构成。相对于主成分100重量份,作为副成分,含有以SiO2换算为0.30~1.83重量份的硅化合物、以Co3O4换算为2.00~10.00重量份的钴化合物、以Bi2O3换算为1.00~3.00重量份的铋化合物。用以Co3O4换算的钴化合物的含量除以以SiO2换算的硅化合物的含量所得的值为5.5~30.0。
Description
技术领域
本发明涉及一种适于叠层型电感器等的制造的铁氧体组合物、以及具有由该组合物构成的铁氧体烧结体的电子部件。
背景技术
近年来,DC-DC转换器在向小型化、高频化发展,以数十MHz~数百MHz左右的频率驱动的DC-DC转换器也出现。作为适用于小型化、高频化后的DC-DC转换器的电感器,要求即使在高频区域下也能够作为电感器工作的频率特性、以及即使施加大电流、工作也几乎没有变化的直流叠加特性。
作为适用于DC-DC转换器的电感器所使用的铁氧体组合物,以往提出了添加有钴的NiCuZn铁氧体。正在探讨通过对NiCuZn铁氧体进行钴添加而提高磁各向异性、提高磁导率的频率特性的方法。
但是,以往已知添加有钴的NiCuZn铁氧体与未添加钴的NiCuZn铁氧体相比,有烧结性降低、温度特性变差的倾向。作为克服上述的钴添加的缺点的方法,提出了以下所示的方法。
专利文献1中,通过在NiCuZn铁氧体中与钴化合物一起添加氧化铋等铋化合物而克服烧结性降低。进一步,通过添加锆化合物而改善温度特性。
专利文献2中,通过在NiCuZn铁氧体中添加Co3O4、SiO2、Bi2O3,得到高的Q值、良好的温度特性和高的抗应力特性。
专利文献3中,通过使NiCuZn铁氧体中的Fe2O3量和ZnO量比较少,进而通过添加CoO而得到频率特性优异的铁氧体组合物。
但是,专利文献1的实施例中,虽然显示初始磁导率μi的值,但是,没有记载保持磁导率的值至何种程度的高频率。根据Snoek极限,一般而言,初始磁导率μi的值越低,越保持磁导率的值至高的频率。但是,在添加有添加物的情况下,在Snoek极限以上保持磁导率至高频率,相反,在Snoek极限以下的低频率磁导率降低。因此,初始磁导率μi成为频率特性的标准,但作为频率特性的评价基准,根据不足。因此,在专利文献1的实施例中,频率特性不清楚。
此外,Snoek极限通过以下的式(1)表示。此外,fr为旋转磁化共振频率,μi为初始磁导率,γ为回转磁常数(gyromagnetic constant),Ms为饱和磁化。
fr(μi-1)=|γ|×(Ms/3π)……式(1)
另外,专利文献1中,关于添加有氧化锆的情况下的磁导率的温度变化,示出了20℃下的初始磁导率和85℃下的初始磁导率之比。但是,在专利文献1的实施例所示的20℃下的初始磁导率和85℃下的初始磁导率之比中最小的为1.45倍。其结果,对于抑制初始磁导率相对于温度变化的变化的效果过大。
另外,在专利文献2中,没有显示初始磁导率的值,频率特性不清楚。在专利文献3中,温度特性不清楚。进一步,专利文献1~3中,直流叠加特性均不清楚。
由以上可知,并不清楚专利文献1~3的NiCuZn铁氧体是否频率特性、直流叠加特性以及温度特性全部都优异。
专利文献1:日本特开2000-252112号公报
专利文献2:日本特开2006-206347号公报
专利文献3:日本特开2008-300548号公报
发明内容
本发明是鉴于这样的实际情况而完成的,其目的在于,提供一种初始磁导率、比电阻、频率特性及温度特性良好的铁氧体组合物、以及使用了上述铁氧体组合物的电子部件。
为了实现上述目的,本发明所涉及的铁氧体组合物为具有主成分和副成分的铁氧体组合物,其特征在于,所述主成分由以Fe2O3换算为18~30摩尔%的氧化铁、以CuO换算为4~14摩尔%的氧化铜、以ZnO换算为0~6摩尔%的氧化锌、余量为氧化镍所构成,相对于上述主成分100重量份,作为上述副成分,含有以SiO2换算为0.30~1.83重量份的硅化合物、以Co3O4换算为2.00~10.00重量份的钴化合物、以Bi2O3换算为1.00~3.00重量份的铋化合物,用以Co3O4换算后的上述钴化合物的含量除以以SiO2换算的上述硅化合物的含量所得的值为5.5~30.0。
本发明的铁氧体组合物通过将构成主成分的氧化物的含量设为上述的范围,进一步作为副成分在上述的范围内含有硅化合物、钴化合物以及铋化合物,从而烧结后的初始磁导率μi、比电阻ρ、频率特性以及初始磁导率μi的温度特性良好。
认为可得到这种效果的理由是通过将主成分设为规定范围、进一步将各成分的含量设为特定的范围所得到的复合的效果。
本发明的电子部件具有由上述的铁氧体组合物构成的铁氧体烧结体。
此外,由本发明的铁氧体组合物构成的铁氧体烧结体优选用于叠层型电感器、叠层型L-C滤波器、叠层型共模滤波器、利用其它的叠层方法的复合电子部件等。例如在LC复合电子部件、NFC线圈、叠层型阻抗元件、叠层型变压器中也适合使用本发明的铁氧体组合物。
附图说明
图1是本发明的一个实施方式的叠层型电感器的剖面图。
图2是本发明的一个实施方式的LC复合电子部件的剖面图。
图3是NiCuZn铁氧体中的磁导率的频率特性的示意图。
符号说明
1……叠层型电感器
2……元件
3……端子电极
4……叠层体
5……线圈导体
5a、5b……引出电极
10……LC复合电子部件
12……电感器部
14……电容器部
具体实施方式
以下,基于附图所示的实施方式说明本发明。
如图1所示,本发明的一个实施方式的叠层型电感器1具有元件2和端子电极3。元件2通过经由铁氧体层4而3维且螺旋状地形成有线圈导体5的生坯叠层体进行烧成而得到。铁氧体层4由本发明的一个实施方式的铁氧体组合物构成。通过在元件2的两端形成端子电极3,并且经由引出电极5a、5b与端子电极3接续从而得到叠层型电感器1。对元件2的形状没有特别限制,通常设为长方体状。另外,对其尺寸也没有特别限制,根据用途设为适当的尺寸即可。
作为线圈导体5及引出电极5a、5b的材质,没有特别限定,可使用Ag、Cu、Au、Al、Pd、Pd/Ag合金等。此外,也可以添加Ti化合物、Zr化合物、Si化合物等。
本实施方式的铁氧体组合物为Ni-Cu系铁氧体或Ni-Cu-Zn系铁氧体,作为主成分,可以含有氧化铁、氧化铜及氧化镍,进一步可以含有氧化锌。
主成分100摩尔%中,氧化铁的含量以Fe2O3换算为18.0~30.0摩尔%。无论氧化铁的含量过多还是过少,都存在烧结性变差、特别是低温烧结时的烧结密度降低的倾向。另外,在氧化铁过少的情况下,存在初始磁导率μi降低的倾向。在氧化铁过多的情况下,存在频率特性变差、后述的μ”上升频率降低的倾向。进而,存在初始磁导率μi的温度特性也变差的倾向。
主成分100摩尔%中,氧化铜的含量以CuO换算为4~14摩尔%。氧化铜的含量过少时,存在烧结性变差、特别是低温烧结时的烧结密度降低的倾向。其结果,存在比电阻ρ及初始磁导率μi的温度特性变差的倾向。其过多时,存在初始磁导率μi降低的倾向。
主成分100摩尔%中,氧化锌的含量以ZnO换算为0~6.0摩尔%。即,可以含有氧化锌作为主成分,也可以不含有。此外,存在氧化锌的含量越多、初始磁导率越上升的倾向,初始磁导率越升高,越适于电感器。但是,氧化锌的含量过多时,存在居里温度及μ”上升频率降低的倾向。
主成分的余量由氧化镍构成。
本实施方式的铁氧体组合物除上述的主成分之外,含有硅化合物、钴化合物及铋化合物作为副成分。此外,作为各化合物的种类,除氧化物之外,只要是在烧成后会成为氧化物的化合物,就没有特别限定。
相对于主成分100重量份,硅化合物的含量以SiO2换算为0.30~1.83重量份。如果在特定的范围内含有硅化合物时,铁氧体组合物的温度特性提高。硅化合物的含量过少时,存在初始磁导率μi的温度特性降低的倾向。其过多时,存在烧结性变差、特别是低温烧结时的烧结密度降低的倾向。进而,存在初始磁导率μi及比电阻ρ降低的倾向。
对通过硅化合物的添加而提高温度特性的理由进行说明。氧化硅等硅化合物与NiCuZn铁氧体颗粒相比,线膨胀系数小。即,在NiCuZn铁氧体中添加硅化合物而形成铁氧体组合物的情况下,所添加的硅化合物对NiCuZn铁氧体预先施加应力。本发明人等认为,通过硅化合物的存在而产生的应力存在,因此通过温度变化而产生的应力的影响得以缓和,温度特性提高。
相对于主成分100重量份,铋化合物的含量以Bi2O3换算为1.00~3.00重量份。前述的硅化合物及后述的钴化合物具有使烧结性降低的效果。与此相对,铋化合物可以提高烧结性,并且能够在900℃以下的温度下进行烧成。铋化合物的含量过少时,存在烧结性变差、特别是低温烧结时的烧结密度降低的倾向。进而,存在伴随烧结性的变差、比电阻ρ也降低的倾向。铋化合物的含量过多时,存在比电阻ρ降低的倾向。
相对于主成分100重量份,钴化合物的含量以Co3O4换算为2.00~10.00重量份。在特定的范围内含有钴化合物时,频率特性提高,μ”上升频率提高。进而,直流叠加特性也提高。即,直流电流叠加时的感应系数降低变小。钴化合物的含量过少时,存在频率特性变差、μ”上升频率降低的倾向。进而,存在比电阻ρ也降低的倾向。其过多时,存在烧结性变差,特别是低温烧结时的烧结密度降低的倾向。其结果,存在初始磁导率μi也降低的倾向。进而,存在初始磁导率μi的温度特性变差的倾向。
进而,在本实施方式的铁氧体组合物中,按重量基准计以Co3O4换算的钴化合物的含量除以按重量基准计以SiO2换算的硅化合物的含量所得的值(以下,记为Co/Si)为5.5~30.0。
上述的Co/Si的限定显示钴化合物的含量的允许范围根据硅化合物的含量而增减。即使钴化合物的含量为10.0重量份以下,由于硅化合物的添加量也少,因此,在Co/Si超过30.0的情况下,存在初始磁导率μi的温度特性变差的倾向。另外,即使钴化合物的含量为2.0重量份以上,在Co/Si低于5.5的情况下,也存在比电阻ρ及初始磁导率μi降低的倾向。进而,与具有同等磁导率的试样相比,频率特性降低,μ”上升频率降低。
在本实施方式的铁氧体组合物中,除主成分的组成范围被控制在上述的范围之外,还作为副成分,全部在本发明的范围内含有上述的硅化合物、铋化合物及钴化合物。其结果,可以使烧结温度降低,作为一体烧成的内部导体,例如可以使用Ag等比较的低熔点的金属。进而,通过低温烧成而得到的铁氧体烧结体,其初始磁导率高,频率特性良好,比电阻ρ高,直流叠加特性良好,温度特性良好。特别是通过钴化合物和硅化合物的相互作用从而μ”上升频率及初始磁导率μi的温度特性变得良好。
此外,硅化合物、铋化合物及钴化合物中,在任一个不含有一个以上的情况、或者含量为本发明的范围外的情况下,不能充分地得到上述的效果。即,认为上述的效果是在同时含有特定量的硅化合物、铋化合物及钴化合物的情况下首次得到的复合的效果。
另外,本实施方式的铁氧体组合物在上述副成分之外,可以进一步在不阻碍本发明的效果的范围内含有Mn3O4等锰氧化物、氧化锆、氧化锡、氧化镁、玻璃化合物等附加的成分。这些附加的成分的含量没有特别限定,例如为0.05~10重量%左右。
进而,在本实施方式的铁氧体组合物中,可含有不可避免的杂质元素的氧化物。
具体而言,作为不可避免的杂质元素,可列举C、S、Cl、As、Se、Br、Te、I、或Li、Na、Mg、Al、Ca、Ga、Ge、Sr、Cd、In、Sb、Ba、Pb等的典型金属元素、或Sc、Ti、V、Cr、Y、Nb、Mo、Pd、Ag、Hf、Ta等过渡金属元素。另外,不可避免的杂质元素的氧化物可以在铁氧体组合物中含有0.05重量%以下左右。
本实施方式的铁氧体组合物具有铁氧体颗粒和存在于相邻的晶体颗粒间的结晶晶界。晶体颗粒的平均晶体粒径优选为0.2~1.5μm。
下面,针对本发明的铁氧体组合物的频率特性进行说明。
本发明的铁氧体组合物的频率特性表示是否可以保持磁导率至高频率。
为了对本发明的铁氧体组合物的频率特性进行说明,对一般的NiCuZn铁氧体,将以频率为横轴、以复数磁导率的实部μ’和虚部μ”为纵轴时的示意图示于图3。
在低频率区域,即使使频率变化,μ’也大致为一定,μ”在0附近且大致为一定。在使频率上升并设为特定的频率以上时,μ”显示从0上升的行为。本申请中,将成为μ”>0.1的频率设为μ”上升频率。
在μ”上升频率以上的频率的区域,Q值降低,作为电感器使用变得困难。因此,就本发明的铁氧体组合物而言,μ”上升频率越高,可以作为电感器使用的频率的上限越升高。就本发明的铁氧体组合物而言,μ”上升频率越高,频率特性越良好。以下,有时将μ”上升频率记为f。
接下来,对本实施方式的铁氧体组合物的制造方法的一例进行说明。首先,以成为规定的组成比的方式称量并混合起始原料(主成分的原料及副成分的原料),得到原料混合物。作为混合的方法,例如可列举使用球磨机进行的湿式混合、或使用干式混合机进行的干式混合。此外,优选使用平均粒径为0.05~1.0μm的起始原料。
作为主成分的原料,可以使用氧化铁(α-Fe2O3)、氧化铜(CuO)、氧化镍(NiO)、根据需要的氧化锌(ZnO)、或复合氧化物等。进而,此外,可以使用通过烧成而成为上述的氧化物或复合氧化物的各种化合物等。作为通过烧成而成为上述的氧化物的物质,可列举例如:金属单质、碳酸盐、草酸盐、硝酸盐、氢氧化物、卤化物、有机金属化合物等。
作为副成分的原料,可以使用氧化硅、氧化铋及氧化钴。对成为副成分的原料的氧化物没有特别限定,可以使用复合氧化物等。进而,此外,可以使用通过烧成而成为上述的氧化物或复合氧化物的各种化合物等。作为通过烧成而成为上述的氧化物的物质,可列举例如:金属单质、碳酸盐、草酸盐、硝酸盐、氢氧化物、卤化物、有机金属化合物等。
此外,作为氧化钴的一个实施方式的Co3O4由于容易保管或处理,在空气中价数稳定,因此,优选作为氧化钴的原料。
接着,进行原料混合物的煅烧,得到煅烧材料。煅烧是为了引起原料的热分解、成分的均质化、铁氧体的生成、由烧结导致的超微粉的消失和晶粒成长为适当的颗粒尺寸,并将原料混合物变换为适于后工序的形态而进行。这样的煅烧优选在500~900℃的温度下通常进行2~15小时左右。煅烧通常在大气(空气)中进行,但也可以在比大气中氧分压低的气氛下进行。此外,主成分的原料和副成分的原料的混合可以在煅烧之前进行,也可以在煅烧后进行。
接下来,进行煅烧材料的粉碎,得到粉碎材料。粉碎是为了粉碎煅烧材料的凝集而制成具有适当的烧结性的粉体而进行。在煅烧材料形成大的块体时,在进行粗粉碎后,使用球磨机或超微磨碎机等进行湿式粉碎。湿式粉碎优选进行至粉碎材料的平均粒径成为0.1~1.0μm左右。
使用所得到的粉碎材料,制造本实施方式的叠层型电感器。对制造该叠层型电感器的方法没有限制,以下使用片材法。
首先,将得到的粉碎材料与溶剂或粘合剂等添加剂一起进行浆料化,制作膏体。而且,使用该膏体形成生坯片材。接着,将所形成的生坯片材加工成规定的形状,经过脱粘合剂工序、烧成工序,可得到本实施方式的叠层型电感器。烧成在线圈导体5及引出电极5a、5b的熔点以下的温度下进行。例如,线圈导体5及引出电极5a、5b为Ag(熔点962℃)时,优选在850~920℃的温度下进行。就烧成时间而言,通常进行1~5小时左右。另外,烧成可以在大气(空气)中进行,也可以在比大气中氧分压低的气氛下进行。这样得到的叠层型电感器由本实施方式的铁氧体组合物构成。
以上,对本发明的实施方式进行了说明,但本发明并不受这样的实施方式的任何限定,显然可以在不脱离本发明的主旨的范围内以各种方式实施。例如,作为图2所示的LC复合电子部件10中的铁氧体层4,可以使用本发明的铁氧体组合物。此外,图2中,符号12所示的部分为电感器部,符号14所示的部分为电容器部。
实施例
以下,进一步基于详细的实施例说明本发明,但本发明并不限定于这些实施例。
首先,作为主成分的原料,准备了Fe2O3、NiO、CuO、ZnO。作为副成分的原料,准备了SiO2、Bi2O3、Co3O4。
接下来,以作为烧结体成为表1~表4所记载的组成的方式称量了所准备的主成分之后,用球磨机进行湿式混合16小时从而得到原料混合物。
接着,将得到的原料混合物进行干燥之后,在空气中在500℃~900℃下进行煅烧而制成煅烧粉。将煅烧粉及副成分的原料粉末用钢铁制球磨机进行湿式粉碎72小时从而得到粉碎粉。
接下来,将该粉碎粉进行干燥之后,在粉碎粉100重量份中添加作为粘合剂的6wt%浓度的聚乙烯醇水溶液10.0重量份进行造粒而制成颗粒。将该颗粒进行加压成形,以成为成形密度3.20Mg/m3的方式得到了环形状(尺寸=外径13mm×内径6mm×高度3mm)的成形体、及盘形状(尺寸=外径12mm×高度2mm)的成形体。
接着,将这些各成形体在空气中、在作为Ag的熔点(962℃)以下的900℃下烧成2小时,从而得到作为烧结体的圆环磁芯样品。进一步对样品进行了以下的特性评价。将试验结果示于表1~表4。此外,表1~表4中记载的各成分的含量分别为以Fe2O3、NiO、CuO、ZnO、SiO2、Co3O4、Bi2O3换算的值。
初始磁导率μi
对圆环磁芯样品卷绕铜线10圈,使用阻抗分析仪(Agilent Technologies公司制的4991A)测定初始磁导率μi。作为测定条件,设为测定频率1MHz、测定温度25℃。在本实施例中,将初始磁导率μi为1.5以上的情况设为良好。
频率特性(μ”上升频率)
对测定了初始磁导率μi的圆环磁芯样品,一边使测定频率从1MHz增加,一边测定μ”。将μ”超过0.1时的频率设为μ”上升频率。将μ”上升频率f为600MHz以上的情况设为频率特性良好。
比电阻ρ
在盘样品的两面涂敷In-Ga电极,测定直流电阻值,求出比电阻ρ(单位:Ω·m)。测定使用IR计(HEWLETT PACKARD公司制造的4329A)来进行。在本实施例中,将比电阻ρ为106Ω·m以上的情况设为良好。
初始磁导率μi的温度特性
以室温25℃为基准,求出25℃~125℃时的初始磁导率μi的变化率。在本实施例中,将μi的变化率为±30%以内的情况设为良好。
【表1】
*为比较例
表1的试样为将Co及Si以外的全部的组成在本发明的范围内设为相同,在以0.33、0.36或0.40重量份固定了Si的含量的基础上,仅使Co的含量变化的试样。
由表1可知:在全部的主成分及副成分的组成为本发明的范围内的情况下,初始磁导率μi、比电阻ρ、频率特性以及初始磁导率μi的温度特性变得良好。
与此相对,对于作为副成分的Co的含量过少的试样1、11及21而言,频率特性或比电阻ρ不优选。而Co的含量为本发明的范围内但Co/Si过小的试样22,也是比电阻ρ不优选。
另外,就Co的含量过多的试样7、17及27而言,初始磁导率μi的温度特性不优选。针对试样27而言,初始磁导率μi也不优选。进一步,Co的含量为本发明的范围内但Co/Si过大的试样6,也是初始磁导率μi的温度特性不优选。
【表2】
*为比较例
表2的试样为将Co及Si以外的全部的组成在本发明的范围内设为相同,在以2.00、4.80、9.00或10.00重量份固定了Co的含量的基础上,仅使Si的含量变化的试样。
由表2可知:在全部的主成分及副成分的组成为本发明的范围内的情况下,初始磁导率μi、比电阻ρ、频率特性及初始磁导率μi的温度特性变得良好。
与此相对,就作为副成分的Si的含量过少的试样31、36、41及46而言,初始磁导率μi的温度特性不优选。另外,Si的含量为本发明的范围内但Co/Si过大的试样47,也是初始磁导率μi的温度特性不优选。
另外,就Si的含量过多的试样50而言,初始磁导率μi及比电阻ρ不优选。进而,Si的含量为本发明的范围内,但Co/Si过小的试样22、40及45,比电阻ρ不优选。就试样40及45而言,初始磁导率μi也不优选。
【表3】
*为比较例
表3的试样为从试样12使主成分的含量变化的试样。
由表3可知:在全部的主成分及副成分的组成为本发明的范围内的情况下,初始磁导率μi、比电阻ρ、频率特性及初始磁导率μi的温度特性变得良好。
与此相对,就主成分的含量为本发明的范围外的比较例而言,比电阻ρ、频率特性、初始磁导率μi的温度特性和/或初始磁导率μi成为不优选的值。
【表4】
*为比较例
表4的试样91~95为将Bi以外的组成设为与试样12相同,仅使Bi的含量变化的试样。另外,关于表4的试样12及91~95,为了确认烧结性,也进行了相对密度的测定。
就相对密度的测定而言,对成形为盘形而得到的烧结体,由烧成后的烧结体的尺寸及重量算出烧结体密度,将相对于理论密度的烧结体密度作为相对密度来计算。在本实施例中,将相对密度为95%以上设为良好。
由表4可知:在全部的主成分及副成分的组成为本发明的范围内的情况下,初始磁导率μi、比电阻ρ、相对密度(烧结性)、频率特性及初始磁导率μi的温度特性变得良好。
与此相对,就Bi的含量过少的试样91而言,相对密度变低。即,试样91烧结性极度降低。其结果,初始磁导率μi及比电阻ρ成为了不优选的值。另外,就Bi的含量过多的试样95而言,比电阻ρ变差。
Claims (2)
1.一种铁氧体组合物,其特征在于,
该铁氧体组合物具有主成分和副成分,
所述主成分由以Fe2O3换算为18~30摩尔%的氧化铁、以CuO换算为4~14摩尔%的氧化铜、以ZnO换算为0~6摩尔%的氧化锌、余量为氧化镍构成,
相对于所述主成分100重量份,作为所述副成分,含有以SiO2换算为0.30~1.83重量份的硅化合物、以Co3O4换算为2.00~10.00重量份的钴化合物、以Bi2O3换算为1.00~3.00重量份的铋化合物,
用以Co3O4换算的所述钴化合物的含量除以以SiO2换算的所述硅化合物的含量所得的值为5.5~30.0。
2.一种电子部件,其具有由权利要求1所述的铁氧体组合物构成的铁氧体烧结体。
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CN115215642B (zh) * | 2021-03-31 | 2024-01-02 | Tdk株式会社 | 铁氧体组合物、电子部件和电源装置 |
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TW201814739A (zh) | 2018-04-16 |
US20180096768A1 (en) | 2018-04-05 |
KR101933320B1 (ko) | 2018-12-27 |
US10770210B2 (en) | 2020-09-08 |
TWI612539B (zh) | 2018-01-21 |
CN107879736B (zh) | 2020-12-01 |
JP6142950B1 (ja) | 2017-06-07 |
JP2018052793A (ja) | 2018-04-05 |
KR20180036578A (ko) | 2018-04-09 |
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