JP4107667B2 - Ferrite material and inductor element - Google Patents
Ferrite material and inductor element Download PDFInfo
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- JP4107667B2 JP4107667B2 JP2004177292A JP2004177292A JP4107667B2 JP 4107667 B2 JP4107667 B2 JP 4107667B2 JP 2004177292 A JP2004177292 A JP 2004177292A JP 2004177292 A JP2004177292 A JP 2004177292A JP 4107667 B2 JP4107667 B2 JP 4107667B2
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- 239000000463 material Substances 0.000 title claims description 44
- 229910000859 α-Fe Inorganic materials 0.000 title claims description 42
- 230000035699 permeability Effects 0.000 claims description 20
- 230000002180 anti-stress Effects 0.000 claims description 16
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 6
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 238000005452 bending Methods 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 32
- 239000000843 powder Substances 0.000 description 25
- 239000011787 zinc oxide Substances 0.000 description 16
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 239000000203 mixture Substances 0.000 description 8
- 238000001354 calcination Methods 0.000 description 5
- 239000008187 granular material Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 238000013001 point bending Methods 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 238000004804 winding Methods 0.000 description 3
- 239000005751 Copper oxide Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 229910000431 copper oxide Inorganic materials 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 238000004519 manufacturing process 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
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
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- Compounds Of Iron (AREA)
- Magnetic Ceramics (AREA)
- Soft Magnetic Materials (AREA)
Description
本発明は、高い品質係数（以下、Ｑ値）を有し、かつ広い温度範囲で透磁率の変化が少ない、つまり温度係数の絶対値が小さいフェライト材料に関するものである。 The present invention relates to a ferrite material having a high quality factor (hereinafter referred to as Q value) and a small change in magnetic permeability over a wide temperature range, that is, a small absolute value of the temperature coefficient.
これまで、Ｑ値が高くかつ低温度係数を示すフェライト材料として特許文献１に開示されたものが知られている。このフェライト材料は、酸化鉄、酸化亜鉛、酸化ニッケルおよび酸化銅を主成分とする磁性フェライト材料であって、酸化鉄の含有量がＦｅ2Ｏ3換算で４０〜４６モル％の範囲、酸化亜鉛の含有量がＺｎＯ換算で２５．１〜３０モル％の範囲、酸化ニッケルの含有量がＮｉＯ換算で１０〜２５モル％の範囲、および、残部酸化銅を含有し、主成分に対して副成分として酸化ビスマスをＢｉ2Ｏ3換算で２重量％未満の範囲、酸化コバルトをＣｏ3Ｏ4換算で０．１重量％以下の範囲で含有することを特徴としている。 Until now, what was disclosed by patent document 1 is known as a ferrite material with a high Q value and showing a low temperature coefficient. The ferrite material, iron oxide, zinc oxide, a magnetic ferrite material mainly composed of nickel oxide and copper oxide, 40 to 46 mole% of the range the content of iron oxide in terms of Fe 2 O 3, zinc oxide Content of 20.1-30 mol% in terms of ZnO, content of nickel oxide in the range of 10-25 mol% in terms of NiO, and the balance copper oxide, the subcomponent for the main component And bismuth oxide in a range of less than 2% by weight in terms of Bi 2 O 3 and cobalt oxide in a range of 0.1% by weight or less in terms of Co 3 O 4 .
特許文献１のフェライト材料は、上記の組成を採用することにより、初透磁率の相対温度係数（以下、αμｉｒ）の絶対値が５ｐｐｍ／℃以下、周波数１ＭＨｚにおけるＱ値が１００以上という特性を得ることを可能にしている。ところが、特許文献１のαμｉｒは、２０〜６０℃における値であり、より広範囲な温度域、例えば−４０〜１６０℃において絶対値で３ｐｐｍ／℃以下という低αμｉｒを示し、かつ高いＱ値を得ることはできなかった。
本発明は、このような技術的課題に基づいてなされたもので、高いＱ値を有するとともに、−４０〜１６０℃という広範囲な温度域においてαμｉｒの絶対値が小さいフェライト材料の提供を課題とする。
By adopting the above composition, the ferrite material of Patent Document 1 has the characteristics that the absolute value of the relative temperature coefficient of initial permeability (hereinafter, αμir) is 5 ppm / ° C. or less and the Q value at a frequency of 1 MHz is 100 or more. Making it possible. However, αμir in Patent Document 1 is a value at 20 to 60 ° C., shows a low αμir of 3 ppm / ° C. or less in absolute value in a wider temperature range, for example, −40 to 160 ° C., and obtains a high Q value. I couldn't.
The present invention has been made based on such a technical problem, and an object thereof is to provide a ferrite material having a high Q value and a small absolute value of αμir in a wide temperature range of −40 to 160 ° C. .
かかる目的のもと、本発明はＦｅ２Ｏ３：４５．５〜４８ｍｏｌ％、ＣｕＯ：５〜１０ｍｏｌ％、ＺｎＯ:２６〜２９．５ｍｏｌ％、残部実質的にＮｉＯの主成分に対して副成分として酸化コバルトをＣｏＯ換算で０．００５〜０．０４５ｗｔ％の範囲で含有するフェライト材料により前記課題を解決した。
本発明のフェライト材料は、αμｉｒ−４０〜２０の絶対値及びαμｉｒ２０〜１６０の絶対値がともに３ｐｐｍ／℃以下、１００ｋＨｚにおけるＱ値が１７０以上という特性を有する。なお、αμｉｒ−４０〜２０及びαμｉｒ２０〜１６０は、以下に従って求められるものとする。
αμｉｒ−４０〜２０＝［（μｉ２０−μｉ−４０）／μｉ−４０ ２］×［１／（Ｔ２０−Ｔ−４０）］
αμｉｒ２０〜１６０＝［（μｉ１６０−μｉ２０）／μｉ２０ ２］×［１／（Ｔ１６０−Ｔ２０）］
μｉ−４０：−４０℃における初透磁率
μｉ２０：２０℃における初透磁率
μｉ１６０：１６０℃における初透磁率
For this purpose, the present invention provides Fe 2 O 3 : 45.5 to 48 mol%, CuO: 5 to 10 mol%, ZnO: 26 to 29.5 mol%, and the balance is substantially the main component of NiO. The above problems have been solved by a ferrite material containing cobalt oxide as a component in the range of 0.005 to 0.045 wt% in terms of CoO.
Ferrite material of the present invention are both 3 ppm / ° C. the absolute value of the absolute value and Arufamyuir 20 to 160 of αμir -40~20 below, Q values at 100kHz has the property that over 170. Note that αμir -40 to 20 and αμir 20 to 160 are obtained according to the following.
αμir -40~20 = [(μi 20 -μi -40) / μi -40 2] × [1 / (T 20 -T -40)]
αμir 20~160 = [(μi 160 -μi 20) / μi 20 2] × [1 / (T 160 -T 20)]
μi −40 : initial permeability at −40 ° C. μi 20 : initial permeability at 20 ° C. μi 160 : initial permeability at 160 ° C.
また、本発明のフェライト材料は、曲げ強度が２０ｋｇｆ／ｍｍ２以上、抗応力特性の絶対値が５％以下という特性を得ることができる。ただし、曲げ強度はＪＩＳ Ｒ１６０１により測定される値、抗応力特性は以下に従って求められる値とする。
抗応力特性＝（Ｌ１−Ｌ０）／Ｌ０×１００（％）
Ｌ１：一軸圧縮力（１ｔｏｎ／ｃｍ２）印加時のインダクタンス値
Ｌ０：一軸圧縮力（１ｔｏｎ／ｃｍ２）印加なしのインダクタンス値
本発明によるフェライト材料は抗応力特性が優れることから、Ｆｅ２Ｏ３：４５．５〜４８ｍｏｌ％、ＣｕＯ：５〜１０ｍｏｌ％、ＺｎＯ:２６〜２９．５ｍｏｌ％、残部実質的にＮｉＯの主成分に対して副成分として酸化コバルトをＣｏＯ換算で０．００５〜０．０４５ｗｔ％の範囲で含有し、αμｉｒ −４０〜２０ の絶対値及びαμｉｒ ２０〜１６０ の絶対値が３ｐｐｍ／℃以下、１００ｋＨｚにおける品質係数（Ｑ値）が１７０以上であるフェライト材料と、フェライト材料を被覆する樹脂モールドとを備えるインダクタ素子を提供することができる。
In addition, the ferrite material of the present invention can obtain the characteristics that the bending strength is 20 kgf / mm 2 or more and the absolute value of the anti-stress characteristic is 5% or less. However, the bending strength is a value measured according to JIS R1601, and the anti-stress characteristic is a value determined according to the following.
Anti-stress characteristics = (L 1 −L 0 ) / L 0 × 100 (%)
L 1 : Inductance value when uniaxial compression force ( 1 ton / cm 2 ) is applied L 0 : Inductance value without application of uniaxial compression force (1 ton / cm 2 ) Since the ferrite material according to the present invention has excellent anti-stress characteristics, Fe 2 O 3: 45.5~48mol%, CuO: 5~10mol%, ZnO: 26~ 29.5 mol%, cobalt oxide as a sub-component relative to the main component of the balance substantially being NiO in terms of CoO 0.005 contained in the range of ～0.045Wt%, a ferrite material having the absolute value of the absolute value and Arufamyuir 20 to 160 of αμir -40~20 is 3 ppm / ° C. or less, the quality factor (Q value) at 100kHz is 170 or more, An inductor element including a resin mold that covers a ferrite material can be provided.
本発明によれば、高いＱ値を有するとともに、−４０〜１６０℃という広範囲な温度域においてαμｉｒの絶対値が小さいフェライト材料が提供される。 According to the present invention, a ferrite material having a high Q value and a small absolute value of αμir in a wide temperature range of −40 to 160 ° C. is provided.
以下、本発明によるフェライト材料の組成限定理由について説明する。
本発明のフェライト材料の主成分を構成するＦｅ2Ｏ3の含有量が４５．５ｍｏｌ％未満だとＱ値が低く、キュリー点（以下、Ｔｃ）も低くなる。一方、Ｆｅ2Ｏ3の含有量が４８ｍｏｌ％を超えるとαμｉｒが大きくなる。したがって、本発明ではＦｅ2Ｏ3の含有量を４５．５〜４８ｍｏｌ％とする。望ましいＦｅ2Ｏ3の含有量は４６〜４７．８ｍｏｌ％、さらに望ましいＦｅ2Ｏ3の含有量は４６．５〜４７．５ｍｏｌ％である。
Hereinafter, the reasons for limiting the composition of the ferrite material according to the present invention will be described.
When the content of Fe 2 O 3 constituting the main component of the ferrite material of the present invention is less than 45.5 mol%, the Q value is low and the Curie point (hereinafter, Tc) is also low. On the other hand, the content of Fe 2 O 3 is αμir increases exceeds 48 mol%. Accordingly, the present invention is a 45.5～48Mol% content of Fe 2 O 3. The desirable Fe 2 O 3 content is 46 to 47.8 mol%, and the more desirable Fe 2 O 3 content is 46.5 to 47.5 mol%.
本発明のフェライト材料の主成分を構成するＣｕＯの含有量が５ｍｏｌ％未満だとＱ値が低くなるとともに、抗応力特性が大きくなる。一方、ＣｕＯの含有量が１０ｍｏｌ％を超えるとαμｉｒが大きくなる。したがって、本発明ではＣｕＯの含有量を５〜１０ｍｏｌ％とする。望ましいＣｕＯの含有量は５．５〜１０ｍｏｌ％、さらに望ましいＣｕＯの含有量は６〜９．５ｍｏｌ％である。 When the content of CuO constituting the main component of the ferrite material of the present invention is less than 5 mol%, the Q value decreases and the antistress characteristics increase. On the other hand, when the CuO content exceeds 10 mol%, αμir increases. Therefore, in this invention, content of CuO shall be 5-10 mol%. The desirable CuO content is 5.5 to 10 mol%, and the more desirable CuO content is 6 to 9.5 mol%.
本発明のフェライト材料の主成分を構成するＺｎＯの含有量が２６ｍｏｌ％未満だとαμｉｒが大きくなる。一方、ＺｎＯの含有量が３０ｍｏｌ％を超えるとＴｃが低くなる。したがって、本発明ではＺｎＯの含有量を２６〜３０ｍｏｌ％とする。望ましいＺｎＯの含有量は２６．５〜２９．５ｍｏｌ％、さらに望ましいＺｎＯの含有量は２７〜２９ｍｏｌ％である。
本発明のフェライト材料の主成分の残部が実質的にＮｉＯである。
When the content of ZnO constituting the main component of the ferrite material of the present invention is less than 26 mol%, αμir increases. On the other hand, when the ZnO content exceeds 30 mol%, Tc decreases. Therefore, in this invention, content of ZnO shall be 26-30 mol%. A desirable ZnO content is 26.5 to 29.5 mol%, and a more desirable ZnO content is 27 to 29 mol%.
The balance of the main component of the ferrite material of the present invention is substantially NiO.
本発明のフェライト材料は、上記の主成分に対して酸化コバルトをＣｏＯ換算で０．００５〜０．０４５ｗｔ％含有する。ＣｏＯは高いＱ値及び低いαμｉｒを得るために重要な成分であり、０．００５ｗｔ％未満だとＱ値が低くなり、０．０４５ｗｔ％を超えるとαμｉｒが大きくなる。望ましいＣｏＯの含有量は０．０１〜０．０３ｗｔ％、さらに望ましいＣｏＯの含有量は０．０１５〜０．０２５ｗｔ％である。 The ferrite material of the present invention contains 0.005 to 0.045 wt% of cobalt oxide in terms of CoO with respect to the above main component. CoO is an important component for obtaining a high Q value and a low αμir. If it is less than 0.005 wt%, the Q value decreases, and if it exceeds 0.045 wt%, αμir increases. The desirable CoO content is 0.01 to 0.03 wt%, and the more desirable CoO content is 0.015 to 0.025 wt%.
以上の組成を有するフェライト材料は、１００ｋＨｚにおけるＱ値が１７０以上を示すとともに、αμｉｒ-40〜20及びαμｉｒ20〜160が絶対値で３ｐｐｍ／℃以下という低い値を示す。
ところで、αμｉｒは一般に以下の通り定義される。
αμｉｒ＝［（μｉ2−μｉ1）／μｉ1 2］×［１／（Ｔ2−Ｔ1）］
μｉ1：温度Ｔ1のときの初透磁率
μｉ2：温度Ｔ2のときの初透磁率
本発明は、−４０〜１６０℃の温度範囲において低いαμｉｒを得ることを目的としているが、本発明のフェライト材料は室温近傍でμｉ（初透磁率）にピークが存在している。そのため、μi1を−４０℃の初透磁率、μi2を１６０℃の初透磁率としてαμｉｒを求めると、当該ピーク位置において初透磁率の温度係数が大きくなったとしても、それが反映されないおそれがある。そこで本発明では、−４０〜２０℃、２０℃〜１６０℃の２つの温度範囲に分けてαμｉｒを求め、その両者が３ｐｐｍ／℃以下であることを要件としている。
The ferrite material having the above composition exhibits a Q value at 100 kHz of 170 or more, and αμir −40 to 20 and αμir 20 to 160 have a low absolute value of 3 ppm / ° C. or less.
Incidentally, αμir is generally defined as follows.
αμir = [(μi 2 −μi 1 ) / μi 1 2 ] × [1 / (T 2 −T 1 )]
μi 1 : Initial permeability at temperature T 1 μi 2 : Initial permeability at temperature T 2 The present invention aims to obtain a low αμir in the temperature range of −40 to 160 ° C. This ferrite material has a peak in μi (initial permeability) near room temperature. Therefore, when αμir is obtained by setting μi 1 as an initial permeability of −40 ° C. and μi 2 as an initial permeability of 160 ° C., even if the temperature coefficient of the initial permeability increases at the peak position, it may not be reflected. There is. Therefore, in the present invention, αμir is obtained by dividing into two temperature ranges of −40 to 20 ° C. and 20 ° C. to 160 ° C., and both are required to be 3 ppm / ° C. or less.
また、本発明のフェライト材料は、以上の組成を採用することにより、Ｔｃを１６０℃以上とすることができる。高温度環境下における使用を確保する上でＴｃが高いことが要求され、本発明では１８０℃以上、さらには２００℃以上のＴｃを得ることができる。
さらに、本発明のフェライト材料は、機械的強度も優れている。具体的には、２０ｋｇｆ／ｍｍ2以上の３点曲げ強度を有している。なお、３点曲げ強度は角型サンプルを用いてＪＩＳ Ｒ１６０１に従って測定される値である。
Further, the ferrite material of the present invention can have a Tc of 160 ° C. or higher by adopting the above composition. A high Tc is required to ensure use in a high temperature environment, and in the present invention, a Tc of 180 ° C. or higher, or 200 ° C. or higher can be obtained.
Furthermore, the ferrite material of the present invention is also excellent in mechanical strength. Specifically, it has a three-point bending strength of 20 kgf / mm 2 or more. The three-point bending strength is a value measured according to JIS R1601 using a square sample.
さらに、本発明のフェライト材料は抗応力特性の絶対値を５％以下にすることができる。ここで、抗応力特性とは、圧縮応力に対するフェライト材料のインダクタンス値の変化の程度を言う。樹脂モールドタイプのインダクタ素子ではフェライト材料を樹脂モールドするが、樹脂硬化時にフェライト材料に圧縮応力が加わる。フェライト材料は圧縮応力の大きさに応じてインダクタンス値が変化するため、樹脂モールドタイプのインダクタンス素子では圧縮応力に対してインダクタンスの変化の少ない、抗応力に優れたフェライト材料であることが望まれる。絶対値で５％以下の抗応力特性を有している本発明のフェライト材料は、この要請に応え樹脂モールドタイプのインダクタ素子用フェライト材料として用いることができる。本発明のフェライト材料は、抗応力特性の絶対値を４％以下、さらには３％以下とすることができる。抗応力特性の具体的な算出方法は以下の通りである。
角型サンプルにワイヤを２０回巻線した後、これに一定速度で一軸圧縮力を印加し、このときのインダクタンス値を連続的に測定し、得られた測定値からインダクタンス変化率を算出する。このときの一軸圧縮応力は１ｔｏｎ／ｃｍ2とし、インダクタンス変化率は以下の式により求める。
（Ｌ1−Ｌ0）／Ｌ0×１００（％）
Ｌ1：一軸圧縮力印加時のインダクタンス値
Ｌ0：一軸圧縮力印加なしのインダクタンス値
Furthermore, the ferrite material of the present invention can make the absolute value of the antistress characteristic 5% or less. Here, the anti-stress characteristic refers to the degree of change in the inductance value of the ferrite material with respect to the compressive stress. In a resin mold type inductor element, a ferrite material is resin-molded, and compressive stress is applied to the ferrite material when the resin is cured. Since the inductance value of the ferrite material changes according to the magnitude of the compressive stress, it is desired that the resin mold type inductance element is a ferrite material having a small resistance change with respect to the compressive stress and excellent in the antistress. The ferrite material of the present invention having an anti-stress characteristic of 5% or less in absolute value can be used as a resin mold type ferrite material for an inductor element in response to this requirement. In the ferrite material of the present invention, the absolute value of the anti-stress characteristic can be 4% or less, further 3% or less. A specific calculation method of the anti-stress characteristic is as follows.
After winding a wire around a square sample 20 times, a uniaxial compressive force is applied thereto at a constant speed, the inductance value at this time is continuously measured, and the inductance change rate is calculated from the obtained measurement value. At this time, the uniaxial compressive stress is 1 ton / cm 2 , and the inductance change rate is obtained by the following equation.
(L 1 −L 0 ) / L 0 × 100 (%)
L 1 : Inductance value when uniaxial compression force is applied L 0 : Inductance value without application of uniaxial compression force
次に、本発明によるフェライト材料の好適な製造方法を工程順に説明する。
主成分をなす原料粉末として、例えば、Ｆｅ2Ｏ3粉末、ＣｕＯ粉末、ＺｎＯ粉末およびＮｉＯ粉末を用意する。これらの主成分をなす粉末に加えて、副成分をなすＣｏＯ粉末を用意する。
用意する各原料粉末の粒径は０.１〜１０μｍの範囲で適宜選択すればよい。また、用意された原料粉末は例えばボールミルを用いて湿式混合する。混合は、ボールミルの運転条件にも左右されるが、２０時間程度行なえば均一な混合状態を得ることができる。なお、副成分であるＣｏＯの添加は湿式混合時に限らず、後述する仮焼き粉の粉砕時であっても同様の効果を得ることができる。
なお、本発明では、上述の主成分の原料に限らず、２種以上の金属を含む複合酸化物の粉末を主成分の原料としてもよい。例えば、塩化鉄、塩化Ｎｉを含有する水溶液を酸化培焼することによりＦｅ、Ｎｉを含む複合酸化物の粉末が得られる。この粉末とＺｎＯ粉末を混合して主成分原料としてもよい。このような場合には、後述する仮焼きは不要である。
Next, the suitable manufacturing method of the ferrite material by this invention is demonstrated in order of a process.
For example, an Fe 2 O 3 powder, a CuO powder, a ZnO powder, and a NiO powder are prepared as raw material powders that constitute the main component. In addition to these main component powders, a CoO powder component is prepared.
What is necessary is just to select the particle diameter of each raw material powder to prepare suitably in the range of 0.1-10 micrometers. The prepared raw material powder is wet-mixed using, for example, a ball mill. The mixing depends on the operating conditions of the ball mill, but a uniform mixed state can be obtained if it is carried out for about 20 hours. The addition of CoO, which is a subcomponent, is not limited to wet mixing, and the same effect can be obtained even when calcining calcined powder described later.
In the present invention, not only the above-mentioned main component materials, but also a composite oxide powder containing two or more metals may be used as the main component materials. For example, a complex oxide powder containing Fe and Ni can be obtained by oxidizing and baking an aqueous solution containing iron chloride and Ni chloride. This powder and ZnO powder may be mixed and used as a main component material. In such a case, calcining described later is unnecessary.
原料粉末を混合した後、仮焼きを行なう。仮焼きは、保持温度を７００〜９５０℃の範囲とし、また、雰囲気を大気とすればよい。仮焼き後に、仮焼き粉は例えば平均粒径０．５〜２．０μｍ程度まで粉砕される。 After mixing the raw material powder, calcining is performed. In the calcining, the holding temperature may be in the range of 700 to 950 ° C., and the atmosphere may be air. After calcining, the calcined powder is pulverized to an average particle size of about 0.5 to 2.0 μm, for example.
主成分および副成分からなる粉砕粉末は、後の成形工程を円滑に実行するために顆粒に造粒することが望ましい。粉砕粉末に適当な結合材、例えばポリビニルアルコール（ＰＶＡ）を少量添加し、これをスプレードライヤで噴霧、乾燥することにより顆粒を得ることができる。得られる顆粒の粒径は６０〜２００μｍ程度とすることが望ましい。 It is desirable that the pulverized powder composed of the main component and the subcomponent is granulated into granules in order to smoothly perform the subsequent molding process. Granules can be obtained by adding a small amount of a suitable binder such as polyvinyl alcohol (PVA) to the pulverized powder, and spraying and drying it with a spray dryer. The particle size of the obtained granules is desirably about 60 to 200 μm.
得られた顆粒は、例えば所定形状の金型を有するプレスを用いて所望の形状に成形され、この成形体は焼成工程に供される。焼成における保持温度は、９００〜１１５０℃、望ましくは９５０〜１１００℃の範囲とすればよい。また、焼成は大気中で行えばよい。 The obtained granule is formed into a desired shape using, for example, a press having a mold having a predetermined shape, and this formed body is subjected to a firing step. The holding temperature in the firing may be 900 to 1150 ° C, preferably 950 to 1100 ° C. Moreover, what is necessary is just to perform baking in air | atmosphere.
以下、本発明を具体的な実施例に基づいて説明する。
主成分組成としてＦｅ2Ｏ3粉末、ＺｎＯ粉末、ＮｉＯ粉末およびＣｕＯ粉末を表１に示される最終組成（ｍｏｌ％）となるように秤量し、この主成分組成に対してＣｏＯを表１に示す量（ｗｔ％）だけ加えた。
次に、これらの原料を鋼鉄製のボールミルを用いて湿式混合し、得られた混合粉末を９００℃で２時間仮焼きし、この仮焼き粉を鋼鉄製のボールミルにて混合粉砕した。得られた粉砕粉末は、平均粒径が０．５μｍであった。
Hereinafter, the present invention will be described based on specific examples.
Fe 2 O 3 powder, ZnO powder, NiO powder and CuO powder as the main component composition are weighed so as to have the final composition (mol%) shown in Table 1, and CoO is shown in Table 1 for this main component composition. Only the amount (wt%) was added.
Next, these raw materials were wet-mixed using a steel ball mill, and the obtained mixed powder was calcined at 900 ° C. for 2 hours, and the calcined powder was mixed and ground in a steel ball mill. The obtained pulverized powder had an average particle size of 0.5 μm.
次いで、得られた各仮焼き粉に、バインダとしてポリビニルアルコール水溶液を添加して造粒した。こうして得られた平均粒径７０μｍの顆粒を用いて、電磁気特性評価用のトロイダル形状試料（外径２０ｍｍ、内径１０ｍｍ、高さ５ｍｍ）、および、機械的強度評価用の角柱試料（幅５ｍｍ、厚さ４ｍｍ、長さ５０ｍｍ）をプレス成形により得た。なお、成形密度が３．２０Ｍｇ／ｍ3となるように成形した。成形体を大気中、１０２０℃で２時間焼成し、表１に示す試料Ｎｏ．１〜２１を得た。 Subsequently, the obtained calcined powder was granulated by adding an aqueous polyvinyl alcohol solution as a binder. Using the granules having an average particle diameter of 70 μm thus obtained, a toroidal sample for evaluating electromagnetic properties (outer diameter 20 mm, inner diameter 10 mm, height 5 mm) and a prismatic sample for evaluating mechanical strength (width 5 mm, thickness) 4 mm in length and 50 mm in length) was obtained by press molding. In addition, it shape | molded so that a shaping | molding density might be 3.20Mg / m < 3 >. The molded body was fired at 1020 ° C. for 2 hours in the air, and sample No. 1-21 were obtained.
得られたトロイダル形状の試料にワイヤを２０回巻線した後、インピーダンスアナライザ（横河ヒューレットパッカード社製４１９２Ａ）にて１００ｋＨｚにおける透磁率を測定した。この測定結果に基づくμｉ、αμｉｒ-40〜20及びαμｉｒ20〜160を表１に示してある。なお、図１は、試料Ｎｏ．３のμｉの温度特性（−４０〜１６０℃）を示すグラフである。図１より室温近傍でμｉがピークをも持つことがわかる。ちなみに、−４０℃と１６０℃の初透磁率（μｉ）から求めた相対温度係数（αμｉｒ）は−０．２ｐｐｍ／℃である。
また、得られたトロイダル形状の試料にワイヤを２０回巻線した後、上述のインピーダンスアナライザにて１００ｋＨｚにおけるＲ値を測定し、式：Ｒ／２πｆＬ＝１／ＱよりＱ値を求めた。その結果を表１に示す。
さらに、得られたトロイダル形状の試料についてＴｃを測定した。Ｔｃの測定には、熱分析装置（真空理工社製ＴＡ７０００）を用いた。その結果を表１に示す。
After winding the wire 20 times on the obtained toroidal sample, the permeability at 100 kHz was measured with an impedance analyzer (Yokawa Hewlett-Packard 4192A). Table 1 shows μi, αμir −40 to 20, and αμir 20 to 160 based on the measurement results. Note that FIG. It is a graph which shows the temperature characteristic (-40-160 degreeC) of 3 of μi. FIG. 1 shows that μi also has a peak near room temperature. Incidentally, the relative temperature coefficient (αμir) obtained from the initial permeability (μi) at −40 ° C. and 160 ° C. is −0.2 ppm / ° C.
Further, after winding the wire 20 times on the obtained toroidal sample, the R value at 100 kHz was measured with the impedance analyzer described above, and the Q value was obtained from the formula: R / 2πfL = 1 / Q. The results are shown in Table 1.
Further, Tc was measured for the obtained toroidal sample. For the measurement of Tc, a thermal analyzer (TA7000 manufactured by Vacuum Riko Co., Ltd.) was used. The results are shown in Table 1.
次に、得られた角柱試料を用いて３点曲げ強度及び抗応力特性を測定した。その結果も表１に示した。 Next, the three-point bending strength and the anti-stress characteristic were measured using the obtained prism sample. The results are also shown in Table 1.
表１に示すように、Ｆｅ2Ｏ3：４５．５〜４８．０ｍｏｌ％、ＣｕＯ：５．０〜９．０ｍｏｌ％、ＺｎＯ:２６．０〜３０．０ｍｏｌ％、残部実質的にＮｉＯの主成分に対して副成分としてＣｏＯ：０．００５〜０．０４５ｗｔ％の範囲で含有する試料（Ｎｏ．２〜４、６〜９、１１〜１３、１６〜１８）は、−４０〜２０℃及び２０〜１６０℃におけるαμｉｒが３ｐｐｍ／℃以下、Ｑ値が１７０以上、Ｔｃが１６０℃以上の特性を有している。加えて、これら試料は、２０ｋｇｆ／ｍｍ2以上の曲げ強度及び５％以下の抗応力特性を有している。 As shown in Table 1, Fe 2 O 3: 45.5~48.0mol %, CuO: 5.0~9.0mol%, ZnO: 26.0~30.0mol%, balance substantially Lord NiO Samples (No. 2-4, 6-9, 11-13, 16-18) contained in the range of CoO: 0.005 to 0.045 wt% as subcomponents with respect to the components are -40 to 20 ° C and Αμir at 20 to 160 ° C. is 3 ppm / ° C. or less, Q value is 170 or more, and Tc is 160 ° C. or more. In addition, these samples have a 20 kgf / mm 2 or more flexural strength and 5% or less of the anti-stress properties.
以上を前提にして試料Ｎｏ．１〜５を参照すると、Ｆｅ2Ｏ3が４５．４ｍｏｌ％と少ないと品質係数（Ｑ値）が１７０未満となることがわかる。また逆にＦｅ2Ｏ3が４８．１ｍｏｌ％と多くなると、αμｉｒ-40〜20が３ｐｐｍ／℃を超えてしまう。
また、試料Ｎｏ．６〜１１を参照すると、ＺｎＯが２５．５ｍｏｌ％と少ないとαμｉｒ-40〜20が３ｐｐｍ／℃を超えてしまう。逆に、ＺｎＯが３０．５ｍｏｌ％Ｔｃが１６０℃未満と低くなることがわかる。
さらに、試料Ｎｏ．１２〜１６を参照すると、ＣｕＯが４．９ｍｏｌ％と少ないとＱ値が１７０未満と低い値を示すとともに、抗応力特性が−５．１％と低下することがわかる。また逆にＣｕＯが１１．０ｍｏｌ％と多くなると、αμｉｒ-40〜20が３ｐｐｍ／℃を超えるとともにＱ値が１７０未満となることがわかる。
さらにまた、試料Ｎｏ．１７〜２１を参照すると、ＣｏＯを添加しないとＱ値が１７０未満の低い値を示す。しかし、ＣｏＯの添加量が０．０５ｗｔ％と多くなるとαμｉｒ-40〜20が３ｐｐｍ／℃を超えることがわかる。
以上の通りであるが、本発明は主成分及び副成分の組成範囲を適切に設定することにより高いＱ値及び−４０〜１６０℃という広い温度範囲で温度係数の絶対値を小さくすることを可能としている。
Based on the above, sample no. Referring to 1 to 5, it can be seen that the quality factor (Q value) is less than 170 when Fe 2 O 3 is as small as 45.4 mol%. Further, when Fe 2 O 3 increases the 48.1Mol% Conversely, αμir -40 ~ 20 exceeds the 3 ppm / ° C..
Sample No. Referring to 6-11, and ZnO is small and 25.5mol% αμir -40 ~ 20 exceeds the 3 ppm / ° C.. Conversely, it can be seen that the ZnO 30.5 mol% Tc is as low as less than 160 ° C.
Furthermore, sample no. With reference to 12 to 16, it can be seen that when CuO is as low as 4.9 mol%, the Q value is as low as 170 and the anti-stress characteristic is reduced to −5.1%. Conversely, when CuO increases to 11.0 mol%, it can be seen that αμir −40 to 20 exceeds 3 ppm / ° C. and the Q value is less than 170.
Furthermore, sample no. Referring to 17 to 21, the Q value is a low value of less than 170 unless CoO is added. However, when the amount of CoO added is increased and 0.05wt% αμir -40 ~ 20 is seen to be greater than 3 ppm / ° C..
As described above, the present invention makes it possible to reduce the absolute value of the temperature coefficient in a wide temperature range of -40 to 160 ° C. by appropriately setting the composition range of the main component and the subcomponent. It is said.
Claims (4)
αμｉｒ −４０〜２０ の絶対値及びαμｉｒ ２０〜１６０ の絶対値が３ｐｐｍ／℃以下、１００ｋＨｚにおける品質係数（Ｑ値）が１７０以上であることを特徴とするフェライト材料。
ただし、
αμｉｒ −４０〜２０ ＝［（μｉ ２０ −μｉ −４０ ）／μｉ −４０ ２ ］×［１／（Ｔ ２０ −Ｔ −４０ ）］
αμｉｒ ２０〜１６０ ＝［（μｉ １６０ −μｉ ２０ ）／μｉ ２０ ２ ］×［１／（Ｔ １６０ −Ｔ ２０ ）］
μｉ −４０ ：−４０℃における初透磁率
μｉ ２０ ：２０℃における初透磁率
μｉ １６０ ：１６０℃における初透磁率 Fe 2 O 3: 45.5~48mol%, CuO: 5~10mol%, ZnO: 26~ 29.5 mol%, 0 cobalt oxide in terms of CoO as a sub-component relative to the main component of the balance substantially being NiO contain in the range of .005~0.045wt%,
A ferrite material having an absolute value of αμir −40 to 20 and an absolute value of αμir 20 to 160 of 3 ppm / ° C. or less and a quality factor (Q value) at 100 kHz of 170 or more.
However,
αμir -40~20 = [(μi 20 -μi -40) / μi -40 2] × [1 / (T 20 -T -40)]
αμir 20~160 = [(μi 160 -μi 20) / μi 20 2] × [1 / (T 160 -T 20)]
μi −40 : Initial permeability at −40 ° C.
μi 20 : Initial permeability at 20 ° C.
μi 160 : Initial permeability at 160 ° C.
ただし、曲げ強度はＪＩＳ Ｒ１６０１により測定される値、
抗応力特性＝（Ｌ１−Ｌ０）／Ｌ０×１００（％）
Ｌ１：一軸圧縮力（１ｔｏｎ／ｃｍ２）印加時のインダクタンス値
Ｌ０：一軸圧縮力（１ｔｏｎ／ｃｍ２）印加なしのインダクタンス値 2. The ferrite material according to claim 1 , wherein the ferrite material has a bending strength of 20 kgf / mm 2 or more and an absolute value of anti-stress characteristics of 5% or less.
However, the bending strength is a value measured according to JIS R1601,
Anti-stress characteristics = (L 1 −L 0 ) / L 0 × 100 (%)
L 1 : Inductance value when uniaxial compressive force ( 1 ton / cm 2 ) is applied L 0 : Inductance value without applying uniaxial compressive force (1 ton / cm 2 )
前記フェライト材料を被覆する樹脂モールドと、
を備え、
前記フェライト材料は、αμｉｒ −４０〜２０ の絶対値及びαμｉｒ ２０〜１６０ の絶対値が３ｐｐｍ／℃以下、１００ｋＨｚにおける品質係数（Ｑ値）が１７０以上であることを特徴とするインダクタ素子。
ただし、
αμｉｒ −４０〜２０ ＝［（μｉ ２０ −μｉ −４０ ）／μｉ −４０ ２ ］×［１／（Ｔ ２０ −Ｔ −４０ ）］
αμｉｒ ２０〜１６０ ＝［（μｉ １６０ −μｉ ２０ ）／μｉ ２０ ２ ］×［１／（Ｔ １６０ −Ｔ ２０ ）］
μｉ −４０ ：−４０℃における初透磁率
μｉ ２０ ：２０℃における初透磁率
μｉ １６０ ：１６０℃における初透磁率 Fe 2 O 3: 45.5~48mol%, CuO: 5~10mol%, ZnO: 26~ 29.5 mol%, 0 cobalt oxide in terms of CoO as a sub-component relative to the main component of the balance substantially being NiO A ferrite material contained in a range of 0.005 to 0.045 wt%;
A resin mold for coating the ferrite material;
Equipped with a,
The ferrite element has an absolute value of αμir −40 to 20, an absolute value of αμir 20 to 160 of 3 ppm / ° C. or less, and a quality factor (Q value) at 100 kHz of 170 or more.
However,
αμir -40~20 = [(μi 20 -μi -40) / μi -40 2] × [1 / (T 20 -T -40)]
αμir 20~160 = [(μi 160 -μi 20) / μi 20 2] × [1 / (T 160 -T 20)]
μi −40 : Initial permeability at −40 ° C.
μi 20 : Initial permeability at 20 ° C.
μi 160 : Initial permeability at 160 ° C.
Priority Applications (7)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2004177292A JP4107667B2 (en) | 2003-09-03 | 2004-06-15 | Ferrite material and inductor element |
| TW093122124A TWI303073B (en) | 2003-09-03 | 2004-07-23 | Ferrite material, ferrite sintered body, and inductor |
| KR1020040063191A KR100617494B1 (en) | 2003-09-03 | 2004-08-11 | Ferrite Material, Ferrite Sintering Material and Inductor Device |
| US10/931,299 US7034649B2 (en) | 2003-09-03 | 2004-08-31 | Ferrite material, ferrite sintered body, and inductor |
| CNB2004100751825A CN100339335C (en) | 2003-09-03 | 2004-09-02 | Ferrite material, ferrite sintered body, and inductor |
| EP04020904A EP1512668B1 (en) | 2003-09-03 | 2004-09-02 | Ferrite material, ferrite sintered body, and inductor |
| DE602004025886T DE602004025886D1 (en) | 2003-09-03 | 2004-09-02 | Ferritic material, sintered ferritic body and inductor |
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| JP2003311813 | 2003-09-03 | ||
| JP2004177292A JP4107667B2 (en) | 2003-09-03 | 2004-06-15 | Ferrite material and inductor element |
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| EP2234126B1 (en) | 2007-12-25 | 2019-09-04 | Hitachi Metals, Ltd. | Multilayer inductor and power converter comprising it |
| JP5580961B2 (en) * | 2010-07-15 | 2014-08-27 | Ｆｄｋ株式会社 | Oxidized magnetic material and manufacturing method thereof |
| JP5637152B2 (en) * | 2012-01-20 | 2014-12-10 | Tdk株式会社 | Ferrite sintered body and electronic parts |
| JP5765250B2 (en) * | 2012-01-20 | 2015-08-19 | Tdk株式会社 | Ferrite sintered body and electronic parts |
| US11380994B2 (en) | 2017-06-13 | 2022-07-05 | Hitachi Metals, Ltd. | Coil device and antenna |
| CN115073157B (en) * | 2022-06-16 | 2023-05-26 | 安徽锦华氧化锌有限公司 | Preparation method of ferrite powder containing zinc oxide, magnesium and zinc |
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