JP4823531B2 - Magnetic oxide material - Google Patents
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- JP4823531B2 JP4823531B2 JP2005017219A JP2005017219A JP4823531B2 JP 4823531 B2 JP4823531 B2 JP 4823531B2 JP 2005017219 A JP2005017219 A JP 2005017219A JP 2005017219 A JP2005017219 A JP 2005017219A JP 4823531 B2 JP4823531 B2 JP 4823531B2
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- 239000000463 material Substances 0.000 title description 10
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 title description 2
- 239000000696 magnetic material Substances 0.000 claims description 23
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 20
- 229910000859 α-Fe Inorganic materials 0.000 claims description 18
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 15
- 229910020599 Co 3 O 4 Inorganic materials 0.000 claims description 13
- 239000000654 additive Substances 0.000 claims description 9
- 230000000996 additive effect Effects 0.000 claims description 9
- 229910007565 Zn—Cu Inorganic materials 0.000 claims description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 33
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 17
- 239000011787 zinc oxide Substances 0.000 description 17
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 16
- 230000035699 permeability Effects 0.000 description 13
- 230000002180 anti-stress Effects 0.000 description 12
- 239000000395 magnesium oxide Substances 0.000 description 9
- 238000010304 firing Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910000428 cobalt oxide Inorganic materials 0.000 description 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 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
- 239000011521 glass Substances 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 1
- 229910017518 Cu Zn Inorganic materials 0.000 description 1
- 229910017752 Cu-Zn Inorganic materials 0.000 description 1
- 229910017943 Cu—Zn Inorganic materials 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006355 external stress Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- -1 mol% Substances 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Magnetic Ceramics (AREA)
- Soft Magnetic Materials (AREA)
Description
本発明は、フィルター、固定コイル等のインダクタンス素子として利用できるＮｉ−Ｚｎ−Ｃｕ系フェライトからなる酸化物磁性材料に関する。 The present invention relates to an oxide magnetic material made of Ni—Zn—Cu ferrite that can be used as an inductance element such as a filter and a fixed coil.
Ｆｅ2Ｏ3、ＮｉＯ、ＺｎＯ、ＣｕＯを主成分とする酸化物磁性材料に、Ｃｏ3Ｏ4、ＳｉＯ2、Ｂｉ2Ｏ3等を添加して、種々の特性を改善した酸化物磁性材料は周知である（例えば、特許文献１〜６参照）が、いずれも、高いＱ値、良好な温度特性（温度変化に対する透磁率変化が小さい）、高い抗応力特性を兼ね備えたものではなかった。
特許文献１には、「Ｎｉを必須成分として含有する磁性酸化物フェライト材料に添加物としてＢｉ2Ｏ3、Ｖ2Ｏ5の少なくとも１種を０．５〜５重量％含有させた焼結体からなることを特徴とする、外部応力下に使用されるインダクタ用磁心。」（特許請求の範囲請求項１）の発明が記載されており、抗応力特性を改善するために、Ｂｉ2Ｏ3を含有させるものである（第２頁右上欄第６行〜第１６行）。 Patent Document 1 states that “a sintered body containing 0.5 to 5% by weight of at least one of Bi 2 O 3 and V 2 O 5 as an additive in a magnetic oxide ferrite material containing Ni as an essential component. In order to improve the anti-stress characteristic, Bi 2 O 3 is described, which describes an inductor magnetic core used under an external stress. (The second page, upper right column, lines 6 to 16).
特許文献２には、「主成分としてＦｅ2Ｏ3が４７．０〜５０．０モル％、Ｍｎ2Ｏ3が０．０１〜３．０モル％、ＣｕＯが０．５〜４．９モル％、ＺｎＯが１．０〜２３．０モル％、ＮｉＯが残部モル％含有されて構成されるＮｉＣｕＺｎ系のフェライト材料であって、この主成分に対して、ＣｏＯが０．０２〜１．０重量％、Ｂｉ2Ｏ3が０．５〜１０．０重量％、ＳｉＯ2が０．１〜２．０重量％、ＭｇＯが０．０５〜１．０重量％添加されてなることを特徴とするフェライト材料。」（特許請求の範囲請求項１）の発明が記載されており、「極めて温度特性が良好（温度変化に対する透磁率の変化率が小さい）で、品質係数Ｑが高く、高強度のＮｉＣｕＺｎ系フェライト材料が得られる。」（段落［００４６］）ことが示されているが、Ｑ値を向上させるために、Ｍｎ2Ｏ3、ＭｇＯを必須成分とする（段落［００１８］、［００２４］）ものである。 Patent Document 2 states that “Fe 2 O 3 as a main component is 47.0 to 50.0 mol%, Mn 2 O 3 is 0.01 to 3.0 mol%, and CuO is 0.5 to 4.9 mol. %, ZnO is 1.0 to 23.0 mol%, NiO is the remaining mol% NiCuZn-based ferrite material, CoO is 0.02 to 1.0 with respect to this main component It is characterized in that 0.5% to 10.0% by weight of Bi 2 O 3, 0.1 to 2.0% by weight of SiO 2 and 0.05 to 1.0% by weight of MgO are added. "The ferrite material to be used." (Claim 1) is described, "It has extremely good temperature characteristics (small change rate of magnetic permeability with respect to temperature change), high quality factor Q, and high strength. Of NiCuZn-based ferrite material is obtained ”(paragraph [0046]). To improve the Q value, Mn 2 O 3, MgO and as essential components (paragraph [0018], [0024]) is intended.
特許文献３には、「Ｆｅ2Ｏ3 ４６．５〜４９．５モル％、ＣｕＯ ５〜１０モル％、ＺｎＯ ２〜３０モル％、および残部ＮｉＯからなる、Ｎｉ−Ｚｎ−Ｃｕ系フェライト材料に、Ｃｏ3Ｏ4 ０．０５〜０．６０重量％、Ｂｉ2Ｏ3 ３〜５重量％、およびＳｉＯ2 ０．１０〜２．０重量％を添加した、フェライトコア焼成用材料。」（特許請求の範囲）の発明が記載されているが、ＣｕＯの含有量が多いものであり、高いＱ値のものを得ることは示されていない。 Patent Document 3 states that “a Ni—Zn—Cu ferrite material composed of 46.5 to 49.5 mol% of Fe 2 O 3 , 5 to 10 mol% of CuO, 2 to 30 mol% of ZnO, and the balance NiO is used. , Co 3 O 4 0.05 to 0.60 wt%, Bi 2 O 3 3 to 5 wt%, and SiO 2 0.10 to 2.0 wt% were added. The invention of claim (Claims) is described, but the content of CuO is large, and it is not shown to obtain a high Q value.
特許文献４には、「酸化鉄の含有量がＦｅ2Ｏ3換算で４５．０〜５１．０モル％の範囲、酸化銅の含有量がＣｕＯ換算で０．５〜１５．０モル％の範囲、酸化亜鉛の含有量がＺｎＯ換算で０〜３３．０モル％の範囲、酸化マグネシウムの含有量がＭｇＯ換算で０．１〜５．０モル％、および、残部酸化ニッケルからなる主成分を含有し、さらに、該主成分に対して副成分として酸化コバルトをＣｏ3Ｏ4換算で０．０５〜１．０重量％の範囲、酸化ビスマスをＢｉ2Ｏ3換算で０．５〜７．０重量％の範囲、酸化ケイ素をＳｉＯ2換算で０〜５．０重量％の範囲で含有することを特徴とする磁性材料。」（特許請求の範囲請求項１）の発明が記載されており、Ｑ値、抗応力特性の向上を目的とする（段落［００１２］）ことが示されているが、高周波領域におけるＱ特性を向上させるためにＭｇＯを必須成分とする（段落［００２０］）ものである。 Patent Document 4 states that “the content of iron oxide is in the range of 45.0 to 51.0 mol% in terms of Fe 2 O 3 , and the content of copper oxide is 0.5 to 15.0 mol% in terms of CuO. The main component of the range, the content of zinc oxide in the range of 0 to 33.0 mol% in terms of ZnO, the content of magnesium oxide in the range of 0.1 to 5.0 mol% in terms of MgO, and the remaining nickel oxide And cobalt oxide as a subcomponent in the range of 0.05 to 1.0% by weight in terms of Co 3 O 4 and bismuth oxide in the range of 0.5 to 7 in terms of Bi 2 O 3 . A magnetic material characterized in that it contains 0% by weight and silicon oxide in the range of 0 to 5.0% by weight in terms of SiO 2 ”(Claim 1). It is shown that the purpose is to improve the Q value and the anti-stress characteristic (paragraph [0012]). MgO and as essential components in order to improve the Q characteristic in a high frequency region (paragraph [0020]) is intended.
特許文献５には、「Ｎｉ−Ｃｕ−Ｚｎ系高周波軟磁性材料において、モル％で、Ｆｅ2Ｏ3が４０．０〜５１．０％、ＣｕＯが１．０〜１００％、ＮｉＯが３８．０〜４８．０％、およびＺｎＯが１．０〜１０．０％からなる磁性粉末にＢ2Ｏ3−Ｂｉ2Ｏ3−ＺｎＯ系ガラスが１〜２５ｗｔ％含有することを特徴とする低温焼成用高周波軟磁性材料。」（特許請求の範囲請求項１）の発明が記載されているが、焼成温度を下げ、焼成に起因する母材と内部電極間の収縮時に生ずる応力を減少させ、内部電極の安定化を図る（段落［００１９］ために、Ｂ2Ｏ3を必須成分とするガラスを含有させるものである。 Patent Document 5 states that “in a Ni—Cu—Zn high-frequency soft magnetic material, mol%, Fe 2 O 3 is 40.0 to 51.0%, CuO is 1.0 to 100%, and NiO is 38.%. Low-temperature firing characterized by containing 1 to 25 wt% of B 2 O 3 —Bi 2 O 3 —ZnO-based glass in a magnetic powder comprising 0 to 48.0% and ZnO of 1.0 to 10.0% High-frequency soft magnetic material for use "(Claim 1) is described, but the firing temperature is lowered to reduce the stress generated during shrinkage between the base material and the internal electrode due to firing, Stabilize the electrode (for paragraph [0019], glass containing B 2 O 3 as an essential component is contained).
特許文献６には、「Ｆｅ2Ｏ3 ４６．０〜５１．０ｍｏｌ％、ＣｕＯ ０．５〜１５．０ｍｏｌ％、残部ＮｉＯからなる主成分１００重量部に対し、添加物として、酸化ビスマスをＢｉ2Ｏ3換算で４．０〜１０．０重量部、酸化マグネシウムをＭｇＯ換算で１．０〜５．０重量部、酸化シリコンをＳｉＯ2換算で２．０〜８．０重量部、酸化コバルトをＣｏＯ換算で０．２〜０．５重量部添加してなることを特徴とする磁性材料。」（特許請求の範囲請求項１）の発明が記載されており、抗応力特性の向上を目的とする（段落［００１１］）ことが示されているが、初透磁率の温度係数を負とする温度特性に改善するために、ＭｇＯを必須成分とする（段落［００１８］）ものである。 Patent Document 6 discloses that “bismuth oxide is added as an additive to 100 parts by weight of a main component composed of 46.0 to 51.0 mol% of Fe 2 O 3, 0.5 to 15.0 mol% of CuO, and the balance NiO. 4.0 to 10.0 parts by weight in terms of 2 O 3 , magnesium oxide to 1.0 to 5.0 parts by weight in terms of MgO, silicon oxide to 2.0 to 8.0 parts by weight in terms of SiO 2 , cobalt oxide Is added in an amount of 0.2 to 0.5 parts by weight in terms of CoO. "(Claim 1) is described, and the object is to improve the anti-stress characteristics. (Paragraph [0011]), but MgO is an essential component (paragraph [0018]) in order to improve temperature characteristics in which the temperature coefficient of initial permeability is negative.
本発明は、Ｎｉ−Ｚｎ−Ｃｕ系フェライト材料（酸化物磁性材料）において、上記従来技術のようにＭｎ2Ｏ3、ＭｇＯ等を含有させることなく、Ｆｅ2Ｏ3、ＮｉＯ、ＺｎＯ、ＣｕＯ、Ｃｏ3Ｏ4、ＳｉＯ2、Ｂｉ2Ｏ3の含有量を調整することにより、高いＱ値、良好な温度特性（温度変化に対する透磁率変化が小さい）、高い抗応力特性を兼ね備えた酸化物磁性材料を提供することを課題とする。 In the Ni—Zn—Cu based ferrite material (oxide magnetic material), the present invention does not contain Mn 2 O 3 , MgO or the like as in the above-described conventional technique, and Fe 2 O 3 , NiO, ZnO, CuO, By adjusting the content of Co 3 O 4 , SiO 2 , Bi 2 O 3 , oxide magnetism that combines high Q-value, good temperature characteristics (small permeability change with temperature change), and high anti-stress characteristics It is an object to provide materials.
本発明は、上記の課題を解決するために、以下の手段を採用する。
（１）主成分として、（ａ）Ｆｅ2Ｏ3が４６．０〜５０．０ｍｏｌ％、（ｂ）ＺｎＯが０〜１８．０ｍｏｌ％、（ｃ）ＣｕＯが０．５〜５．０ｍｏｌ％未満、残部（ｄ）ＮｉＯで構成されるＮｉ−Ｚｎ−Ｃｕ系フェライトからなる酸化物磁性材料において、その主成分１００ｗｔ％に対し、添加成分として、（ｅ）Ｃｏ3Ｏ4が０．２〜１．０ｗｔ％、（ｆ）ＳｉＯ2が０．２〜２．０ｗｔ％、（ｇ）Ｂｉ2Ｏ3 が２．０〜１２．０ｗｔ％の範囲で構成されることを特徴とする酸化物磁性材料である。
（２）主成分として、（ａ）Ｆｅ2Ｏ3が４６．０〜５０．０ｍｏｌ％、（ｂ）ＺｎＯが０〜１８．０ｍｏｌ％、（ｃ）ＣｕＯが０．５〜４．０ｍｏｌ％、残部（ｄ）ＮｉＯで構成されるＮｉ−Ｚｎ−Ｃｕ系フェライトからなることを特徴とする前記（１）の酸化物磁性材料である。
（３）添加成分として、（ｇ）Ｂｉ2Ｏ3 が４．０〜１０．０ｗｔ％の範囲で構成されることを特徴とする前記（１）又は（２）の酸化物磁性材料である。
（４）添加成分として、（ｇ）Ｂｉ2Ｏ3 が５．０超〜１０．０ｗｔ％の範囲で構成されることを特徴とする前記（３）の酸化物磁性材料である。
The present invention employs the following means in order to solve the above problems.
(1) as a main component, (a) Fe 2 O 3 is 46.0~50.0mol%, (b) ZnO is 0~18.0mol%, (c) CuO is less than 0.5～5.0Mol% In the oxide magnetic material made of Ni—Zn—Cu ferrite composed of the balance (d) NiO, (e) Co 3 O 4 is 0.2 to 1 as an additive component with respect to 100 wt% of the main component. .0wt%, (f) SiO 2 is 0.2~2.0wt%, oxide magnetic material characterized Rukoto consists of (g) range Bi 2 O 3 is 2.0～12.0Wt% It is.
(2) As main components, (a) Fe 2 O 3 is 46.0 to 50.0 mol%, (b) ZnO is 0 to 18.0 mol%, (c) CuO is 0.5 to 4.0 mol%, The balance (d) is the oxide magnetic material according to (1) above, which is made of Ni—Zn—Cu ferrite composed of NiO.
(3) as an additive component, an oxide magnetic material of (1) or (2), wherein the Rukoto consists of range (g) Bi 2 O 3 of 4.0~10.0wt%.
(4) as an additive component, an oxide magnetic material of (3), wherein the Rukoto consists of (g) Range Bi 2 O 3 is 5.0 super ~10.0wt%.
本発明は、酸化物磁性材料において、主成分である（ａ）Ｆｅ2Ｏ3、（ｂ）ＺｎＯ、（ｃ）ＣｕＯの各成分の含有量（残部であるＮｉＯの含有量）、添加成分である（ｅ）Ｃｏ3Ｏ4、（ｆ）ＳｉＯ2、（ｇ）Ｂｉ2Ｏ3の各成分の含有量を厳密に調整することにより、高いＱ値、良好な温度特性（温度変化に対する透磁率変化が小さい）、高い抗応力特性を兼ね備えた酸化物磁性材料を得ることができる。 In the oxide magnetic material, the content of each component of (a) Fe 2 O 3 , (b) ZnO, and (c) CuO as the main components (the content of NiO as the balance) and additive components By strictly adjusting the content of each component of (e) Co 3 O 4 , (f) SiO 2 , and (g) Bi 2 O 3 , high Q value, good temperature characteristics (permeability with respect to temperature change) It is possible to obtain an oxide magnetic material having a high anti-stress characteristic.
本発明は、上記のように、各成分の含有量を厳密に調整することにより、高いＱ値、良好な温度特性（温度変化に対する透磁率変化が小さい）、高い抗応力特性を兼ね備えた酸化物磁性材料を得ることができるものであるが、以下、本発明における各成分の含有量の限定理由について具体的に述べる。 As described above, the present invention strictly adjusts the content of each component to provide a high Q value, good temperature characteristics (small permeability change with respect to temperature change), and high anti-stress characteristics. Although a magnetic material can be obtained, the reasons for limiting the content of each component in the present invention will be specifically described below.
（ａ）Ｆｅ2Ｏ3について
Ｆｅ2Ｏ3の含有量は、４６．０〜５０．０ ｍｏｌ％で望ましいフェライト特性が得られる。
少なすぎると磁気特性（Ｑ値）が低下し、多すぎると過剰Ｆｅの析出により焼結阻害、比抵抗低下、磁気特性（Ｑ値）低下が起こるので、上記のように規定した。
The content of Fe 2 O 3 for (a) Fe 2 O 3 is obtained is preferable ferrite properties 46.0-50.0 mol%.
If the amount is too small, the magnetic property (Q value) is lowered. If the amount is too large, sintering is inhibited, specific resistance is lowered, and magnetic property (Q value) is lowered due to precipitation of excess Fe.
（ｂ）ＺｎＯについて
ＺｎＯの含有量は、０〜１８．０ ｍｏｌ％で望ましいフェライト特性が得られる。
多すぎると高いＱ値が得られないので、上記のように規定した。
(B) About ZnO A desirable ferrite characteristic is obtained when the content of ZnO is 0 to 18.0 mol%.
If the amount is too large, a high Q value cannot be obtained.
（ｃ）ＣｕＯについて
ＣｕＯの含有量は、０．５〜５．０ｍｏｌ％未満で望ましいフェライト特性が得られる。特に、高いＱ値を得るためには、０．５〜４．０ｍｏｌ％が好ましい。
少なすぎると透磁率温度変化が大きくなってしまい、多すぎると高いＱ値が得られないので、上記のように規定した。
(C) About CuO A desirable ferrite characteristic is obtained when the CuO content is less than 0.5 to 5.0 mol%. In particular, in order to obtain a high Q value, 0.5 to 4.0 mol% is preferable.
If the amount is too small, the change in permeability temperature becomes large. If the amount is too large, a high Q value cannot be obtained.
（ｅ）Ｃｏ3Ｏ4について
Ｃｏ3Ｏ4の含有量は、０．２〜１．０ｗｔ％で望ましいフェライト特性が得られる。
少なすぎると透磁率温度変化が大きくなってしまい、多すぎると高いＱ値が得られないので、上記のように規定した。
(E) Co 3 O 4 The desired ferrite characteristics can be obtained when the content of Co 3 O 4 is 0.2 to 1.0 wt%.
If the amount is too small, the change in permeability temperature becomes large. If the amount is too large, a high Q value cannot be obtained.
（ｆ）ＳｉＯ2について
ＳｉＯ2の含有量は、０．２〜２．０ｗｔ％で望ましいフェライト特性が得られる。
少なすぎると温度特性（透磁率温度変化）と抗応力特性に改善効果が見られず、多すぎると焼結不足の不具合を起こすので、上記のように規定した。
(F) the content of SiO 2 for SiO 2 is desirable ferrite properties are obtained in 0.2~2.0wt%.
If the amount is too small, the effect of improving the temperature characteristics (permeability temperature change) and the anti-stress property is not observed. If the amount is too large, the problem of insufficient sintering is caused.
（ｇ）Ｂｉ2Ｏ3について
Ｂｉ2Ｏ3の含有量は、２．０〜１２．０ｗｔ％で望ましいフェライト特性が得られる。特に、高いＱ値を得るためには、４．０〜１０．０ｗｔ％が好ましい。５．０超〜１０．０ｗｔ％がより好ましい。
少なすぎると焼結不足の不具合を起こし、高いＱ値、良好な抗応力特性も得られず、多すぎるとＱ値が低下してくるので、上記のように規定した。
The content of the (g) the Bi 2 O 3 Bi 2 O 3 is ferrite properties can be obtained desirable 2.0~12.0wt%. In particular, in order to obtain a high Q value, 4.0 to 10.0 wt% is preferable. More than 5.0 to 10.0 wt% is more preferable.
If the amount is too small, the problem of insufficient sintering is caused, a high Q value and good antistress characteristics cannot be obtained, and if the amount is too large, the Q value is lowered.
以上のような組成範囲（各成分の含有量）からなる本発明の酸化物磁性材料は、例えば、以下のようにして製造することができる。
まず、焼成後の組成が上記の範囲となるように秤量したＦｅ2Ｏ3、ＮｉＯ、ＺｎＯ、ＣｕＯ、Ｃｏ3Ｏ4、ＳｉＯ2、Ｂｉ2Ｏ3を含有した原料を、ボールミル、サンドミル、振動ミル、湿式メディア攪拌型ミル等を用いて混合粉砕した後、仮焼（湿式の場合は乾燥後に仮焼）して仮焼粉を得る。その後、この仮焼粉を更にボールミル、サンドミル、振動ミル、湿式メディア攪拌型ミル等を用いて粉砕し、湿式の場合は更に乾燥する。この完成粉体にバインダーを加えて所望の形状に成形加工し、空気中で焼成して酸化物磁性材料を得る。
The oxide magnetic material of the present invention having the above composition range (content of each component) can be produced, for example, as follows.
First, a raw material containing Fe 2 O 3 , NiO, ZnO, CuO, Co 3 O 4 , SiO 2 , Bi 2 O 3 weighed so that the composition after firing is in the above range is used as a ball mill, sand mill, vibration After mixing and pulverizing using a mill, a wet media stirring type mill, etc., calcining (in the case of wet, calcining after drying), calcined powder is obtained. Thereafter, the calcined powder is further pulverized using a ball mill, a sand mill, a vibration mill, a wet media stirring mill, or the like, and further dried in the case of a wet type. A binder is added to the finished powder to form it into a desired shape and fired in air to obtain an oxide magnetic material.
各金属酸化物原料Ｆｅ2Ｏ3、ＮｉＯ、ＺｎＯ、ＣｕＯ、Ｃｏ3Ｏ4、ＳｉＯ2、Ｂｉ2Ｏ3を実施例表のように秤量し、ボールミルで５時間湿式混合した。その後、得られた原料混合粉末を空気中で８００〜９００℃で２ｈｒ仮焼し、この仮焼粉をボールミルで１８ｈｒ湿式粉砕した。
この完成粉体にバインダーとして有機物（ポリビニルアルコール）を少量混合した後加圧プレス機で約１００Ｍｐａの圧力で寸法が７ｍｍφ×１５ｍｍの円柱状成型体を得、この成型体を空気中で実施例表の設定温度で２ｈｒ焼成を行った。
Each metal oxide raw material Fe 2 O 3 , NiO, ZnO, CuO, Co 3 O 4 , SiO 2 , Bi 2 O 3 was weighed as shown in the example table, and wet mixed by a ball mill for 5 hours. Thereafter, the obtained raw material mixed powder was calcined in the air at 800 to 900 ° C. for 2 hr, and this calcined powder was wet pulverized by a ball mill for 18 hr.
A small amount of an organic substance (polyvinyl alcohol) as a binder is mixed with the finished powder, and then a cylindrical molded body having a size of 7 mmφ × 15 mm is obtained with a pressure press machine at a pressure of about 100 Mpa. Was baked for 2 hours at the set temperature.
次にこのコアサンプル中央部にワイヤを２０回巻き回し、コアサンプル両端面に一定圧力で一軸圧縮力１ｔ／ｃｍ2（９８ＭＰａ）を印加し、インダクタンス値をＬＣＲメーターで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した。Ｑは上記コアサンプルをＪＩＳコイル６φ用に入れＬＣＲメーターで５０ＭＨｚのＱ値を測定した。
結果を表１に示す。
Next, a wire is wound around the center of the core sample 20 times, a uniaxial compression force of 1 t / cm 2 (98 MPa) is applied to both ends of the core sample at a constant pressure, and the inductance value can be continuously measured with an LCR meter. The inductance change rate was calculated from the measured values. For Q, the core sample was put into a JIS coil 6φ, and the Q value at 50 MHz was measured with an LCR meter.
The results are shown in Table 1.
表１より、各成分の含有量が本発明の範囲内にある試料Ｎｏ．２〜４、６〜９、１２、１３、１９、２２〜２４、２７〜２９のＮｉ−Ｚｎ−Ｃｕ系フェライト材料は、Ｑ値が高く、温度変化に対する透磁率変化率が小さくて良好な温度特性のものであり、インダクタンス値変化率△Ｌ1／Ｌが小さくて高い抗応力特性のものであることが分かる。 From Table 1, sample No. in which the content of each component is within the scope of the present invention. Ni-4Zn-Cu ferrite materials of 2-4, 6-9, 12, 13, 19, 22, 24, 27-29 have a high Q value and a low rate of change in magnetic permeability with respect to temperature change, and good temperature. It can be seen that the inductance value change rate ΔL 1 / L is small and has high anti-stress characteristics.
試料Ｎｏ．１のものは、Ｆｅ2Ｏ3の含有量が本発明の下限（４６．０ｍｏｌ％）よりも少ないために、Ｑ値が低い。 Sample No. No. 1 has a low Q value because the content of Fe 2 O 3 is less than the lower limit (46.0 mol%) of the present invention.
試料Ｎｏ．５のものは、Ｆｅ2Ｏ3の含有量が本発明の上限（５０．０ｍｏｌ％）よりも多いために、焼成温度が高くなり焼結不足の不具合を起こすとともに、Ｑ値も低い。 Sample No. In No. 5, since the content of Fe 2 O 3 is higher than the upper limit (50.0 mol%) of the present invention, the firing temperature becomes high, causing the problem of insufficient sintering, and the Q value is also low.
試料Ｎｏ．１０のものは、ＺｎＯの含有量が本発明の上限（１８．０ｍｏｌ％）よりも多いために、Ｑ値が低い。 Sample No. No. 10 has a low Q value because the ZnO content is higher than the upper limit (18.0 mol%) of the present invention.
試料Ｎｏ．１１のものは、ＣｕＯの含有量が本発明の下限（０．５ｍｏｌ％）よりも少ない（０％）ために、温度変化に対する透磁率変化率が大きい。 Sample No. In No. 11, the content of CuO is less (0%) than the lower limit (0.5 mol%) of the present invention, and therefore the permeability change rate with respect to temperature change is large.
試料Ｎｏ．１４〜１７のものは、ＣｕＯの含有量が本発明の上限（５．０ｍｏｌ％）よりも多いために、Ｑ値が低い。
試料Ｎｏ．１６のものは、ＣｕＯの含有量とともにＺｎＯの含有量も本発明の上限（１８．０ｍｏｌ％）よりも多いために、Ｑ値が極端に低くなっている。
Sample No. Since the thing of 14-17 has more content of CuO than the upper limit (5.0 mol%) of this invention, Q value is low.
Sample No. In No. 16, since the content of ZnO as well as the content of CuO is larger than the upper limit (18.0 mol%) of the present invention, the Q value is extremely low.
試料Ｎｏ．１８のものは、Ｃｏ3Ｏ4の含有量が本発明の下限（０．２ｍｏｌ％）よりも少ない（０％）ために、温度変化に対する透磁率変化率が大きい。 Sample No. In No. 18, the content of Co 3 O 4 is less (0%) than the lower limit (0.2 mol%) of the present invention, and therefore the permeability change rate with respect to temperature change is large.
試料Ｎｏ．２０のものは、Ｃｏ3Ｏ4の含有量が本発明の上限（１．０ｍｏｌ％）よりも多いために、Ｑ値が低い。 Sample No. No. 20 has a low Q value because the content of Co 3 O 4 is higher than the upper limit (1.0 mol%) of the present invention.
試料Ｎｏ．２１のものは、ＳｉＯ2の含有量が本発明の下限（０．２ｍｏｌ％）よりも少ない（０％）ために、温度変化に対する透磁率変化率が大きく、インダクタンス値変化率も大きい。 Sample No. In No. 21, since the content of SiO 2 is less (0%) than the lower limit (0.2 mol%) of the present invention, the magnetic permeability change rate with respect to the temperature change is large, and the inductance value change rate is also large.
試料Ｎｏ．２５のものは、ＳｉＯ2の含有量が本発明の上限（２．０ｍｏｌ％）よりも多いために、焼成温度がやや高くなり焼結不足の不具合を起こす。 Sample No. In the case of No. 25, since the content of SiO 2 is higher than the upper limit (2.0 mol%) of the present invention, the firing temperature becomes slightly high, causing a problem of insufficient sintering.
試料Ｎｏ．２６のものは、Ｂｉ2Ｏ3の含有量が本発明の下限（０．２ｍｏｌ％）よりも少ない（０％）ために、焼成温度が高くなり焼結不足の不具合を起こすとともに、Ｑ値も低く、インダクタンス値変化率も大きい。 Sample No. In No. 26, the content of Bi 2 O 3 is lower (0%) than the lower limit (0.2 mol%) of the present invention. Low and inductance value change rate is large.
以上のように、本発明の酸化物磁性材料は、いずれもが、Ｑ値が高く、良好な温度特性、高い抗応力特性のものであったが、比較例のものは、Ｑ値が低かったり、焼結不足の不具合を起こしたり、温度特性や抗応力特性に満足のいくものではなかった。
As described above, all of the oxide magnetic materials of the present invention had a high Q value, good temperature characteristics, and high anti-stress characteristics, but the comparative examples had low Q values. It was not satisfactory in terms of temperature characteristics and anti-stress characteristics.
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