JP6451742B2 - MnZn系フェライトおよびその製造方法 - Google Patents
MnZn系フェライトおよびその製造方法 Download PDFInfo
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- JP6451742B2 JP6451742B2 JP2016545661A JP2016545661A JP6451742B2 JP 6451742 B2 JP6451742 B2 JP 6451742B2 JP 2016545661 A JP2016545661 A JP 2016545661A JP 2016545661 A JP2016545661 A JP 2016545661A JP 6451742 B2 JP6451742 B2 JP 6451742B2
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- 229910000859 α-Fe Inorganic materials 0.000 title claims description 61
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 23
- 229910052760 oxygen Inorganic materials 0.000 claims description 23
- 239000001301 oxygen Substances 0.000 claims description 23
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 20
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 17
- 238000010304 firing Methods 0.000 claims description 17
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 15
- 229910052718 tin Inorganic materials 0.000 claims description 15
- 230000008859 change Effects 0.000 claims description 14
- 229910052758 niobium Inorganic materials 0.000 claims description 14
- 230000004907 flux Effects 0.000 claims description 13
- 229910052715 tantalum Inorganic materials 0.000 claims description 12
- 229910020599 Co 3 O 4 Inorganic materials 0.000 claims description 11
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 11
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 4
- 229910052797 bismuth Inorganic materials 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000013078 crystal Substances 0.000 description 27
- 238000000034 method Methods 0.000 description 16
- 239000000203 mixture Substances 0.000 description 16
- 230000008569 process Effects 0.000 description 12
- 229910021645 metal ion Inorganic materials 0.000 description 11
- 239000011029 spinel Substances 0.000 description 11
- 229910052596 spinel Inorganic materials 0.000 description 11
- 230000001747 exhibiting effect Effects 0.000 description 6
- -1 CaCO 3 Inorganic materials 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 230000035699 permeability Effects 0.000 description 5
- 238000004804 winding Methods 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000002123 temporal effect Effects 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 230000036962 time dependent Effects 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 230000005381 magnetic domain Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000011802 pulverized particle Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Description
Ps(%)=〔(Pcv130B−Pcv130A)/Pcv130A〕×100
所望の温度での磁心損失Pcvを低減するには組成を適正化して、スピネルを構成する正の結晶磁気異方性定数K1を示す金属イオンと負の結晶磁気異方性定数K1を示す金属イオンの量を適宜調整することが必要である。しかしながら飽和磁束密度Bs、キュリー温度Tc、初透磁率μiなどの磁心損失Pcv以外の要求磁気特性による制限から、組成選択の自由度は少ない。またFe2O3が多い組成では、外部磁場印加によって得られる磁化曲線が原点付近でくびれ、いわゆるパーミンバー型となりやすく、磁心損失が増加する。そこで以上の観点から、磁心損失の極小温度が110℃から150℃の間にあるように、本発明では、主成分としてFe2O3が53.25モル%以上54.00モル%以下、ZnOが2.50モル%以上8.50モル%以下、残部がMnOの組成範囲を選択した。なお本発明においては、主成分とは主としてスピネルフェライトを構成する元素、化合物を言い、対して副成分とはその形成に補助的に用いられる元素、化合物を言い、一部がスピネルフェライトに固溶する元素を含む。また、Coのようにスピネルフェライトを構成するものも、前記主成分と比べて含有量が少なく副成分としている。
MnZn系フェライトとして所定の組成量となるように原料を秤量した後、主成分であるFe2O3、MnO(Mn3O4を使用)、ZnOを仮焼成し、解砕した後、副成分であるSiO2、CaCO3、Co3O4、Bi2O3と、Ta2O5又はNb2O5と、TiO2又はSnO2とを適宜添加混合し、バインダを加えて造粒、成形の後、焼成に供する。本発明においては焼成後のMnZn系フェライトをフェライト焼結体と呼ぶ場合がある。
log(PO2)=a−b/(T+273) ・・・式
なお、a、bは定数であり、aは3.1〜12.8、bは6000〜20000であるのが好ましい。aは高温保持工程の温度と酸素濃度から規定される。また、bが所定の範囲よりも小さいと温度が下がっても酸素濃度が高く酸化が進み、スピネルからヘマタイトが析出する場合がある。また、bが大きいと酸素濃度が低下しウスタイトが析出したりして、結晶粒や粒界層とも十分に酸化されずに抵抗が小さくなる。より好ましくは、aは6.4〜11.5、bは10000〜18000であり、高温保持工程における酸素濃度を0.7%以下、1200℃における酸素濃度を0.5%以下、1100℃における酸素濃度を0.1%以下に制御することにより、高温環境下での磁気特性の経時変化をより一層低減することが可能となる。
磁心損失Pcvは岩崎通信機株式会社製のB−Hアナライザ(SY−8232)を用い、磁心に一次側巻線と二次側巻線とをそれぞれ5ターン巻回し、周波数100kHz、最大磁束密度200mTで、室温(23℃)〜150℃における磁心損失を測定した。
更に高温槽にて200℃の雰囲気で96時間保持して高温環境に放置し、その後、高温槽から取り出して磁心の温度が室温まで下がってから、磁心損失を同様の条件で130℃にて評価し、高温環境放置前後の130℃における磁心損失から次式にて磁心損失の変化率Psを算出した。
Ps(%)=〔(Pcv130B−Pcv130A)/Pcv130A〕×100
なおPcv130Aは高温環境放置前の130℃における磁心損失であり、Pcv130Bは高温環境放置後の130℃における磁心損失である。なお、高温環境放置前の磁心損失の測定においては、磁心の温度が安定する10分から15分程度、磁心を最高で150℃の雰囲気に調整された恒温槽内におくが、以降の実施例の磁心を含めて磁気特性の経時変化は実質的に生じなかった。
飽和磁束密度(Bs)は、磁心に一次側巻線と二次側巻線とをそれぞれ40回巻回し、1.2kA/mの磁場を印加し、直流磁化測定試験装置(メトロン技研株式会社製SK−110型)を用いて130℃において測定した。
平均結晶粒径は、 フェライト焼結体の鏡面研磨面にて結晶粒界をサーマルエッチング(1100℃×1hr、N2中処理)し、その表面を光学顕微鏡で400倍にて写真撮影し、この写真上の140μm×105μm長方形領域において求積法により算出した。
Claims (5)
- 主成分としてFe、Mn及びZnと、副成分としてSi、Ca、Co、及びBiと、Ta又はNbの少なくとも一種と、Ti又はSnの少なくとも一種とを含み、
前記主成分がそれぞれFe2O3、ZnO、MnOで構成されるとしたときの総量を100モル%として、FeをFe2O3換算で53.25モル%以上54.00モル%以下、ZnをZnO換算で2.50モル%以上8.50モル%以下、及びMnをMnO換算で残部とし、
SiをSiO2換算で0.001質量%超0.02質量%未満、CaをCaCO3換算で0.04質量%超0.4質量%未満、CoをCo3O4換算で0.5質量%未満(0は含まず)、BiをBi2O3換算で0.05質量%未満(0は含まず)、TaをTa2O5換算で0.05質量%未満(0を含む)、NbをNb2O5換算で0.05質量%未満(0を含む)、TiをTiO2換算で0.3質量%未満(0を含む)、SnをSnO2換算で0.3質量%未満(0を含む)を満たし、ただし換算されたTa2O5とNb2O5の総量は0.05質量%未満(0は含まず)であり、換算されたTiO2とSnO2の総量は0.3質量%未満(0は含まず)であって、
周波数100kHzで最大磁束密度が200mTにおいて130℃での磁心損失(Pcv130A)が400kW/m3以下であり、200℃にて96時間保持した後の130℃での磁心損失(Pcv130B)を用いて下記式で表される磁心損失の変化率Psが5%以下であることを特徴とするMnZn系フェライト。
Ps(%)=〔(Pcv130B−Pcv130A)/Pcv130A〕×100 - 請求項1に記載のMnZn系フェライトであって、
SiをSiO2換算で0.003質量%以上0.015質量%以下、CaをCaCO3換算で0.06質量%以上0.3質量%以下、CoをCo3O4換算で0.16質量%以上0.4質量%以下、BiをBi2O3換算で0.0075質量%以上0.04質量%以下で、Ta又はNbを単独で含む場合、TaをTa2O5換算で0.015質量%以上0.04質量%以下、NbをNb2O5換算で0.015質量%以上0.04質量%以下、Ti又はSnを単独で含む場合、TiをTiO2換算で0.02質量%以上0.2質量%以下、SnをSnO2換算で0.02質量%以上0.2質量%以下含み、TaとNbとを両方含む場合、換算されたTa2O5とNb2O5の総量は0.04質量%以下であり、TiとSnとを両方含む場合、換算されたTiO2とSnO2の総量は0.2質量%以下であることを特徴とするMnZn系フェライト。 - 請求項1又は2に記載のMnZn系フェライトであって、
100℃から150℃の間での磁心損失が500kW/m3以下で、磁心損失の極小温度が110℃から150℃の間にあることを特徴とするMnZn系フェライト。 - 請求項3に記載のMnZn系フェライトであって、
200℃にて96時間保持した後の130℃での磁心損失(Pcv130B)が400kW/m3以下であることを特徴とするMnZn系フェライト。 - MnZn系フェライトの製造方法であって、
請求項1に規定する主成分及び副成分の酸化物粉末を成形して成形体とし、前記成形体を焼成する焼成工程を有し、前記焼成工程は昇温工程と高温保持工程と降温工程とを備え、高温保持工程における温度は1250℃から1400℃の間であり、高温保持工程における雰囲気中の酸素濃度を体積百分率で0.7%以下とし、前記降温工程において1200℃における酸素濃度を0.5%以下、1100℃における酸素濃度を0.1%以下としたことを特徴とするMnZn系フェライトの製造方法。
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