JP3556032B2 - Manufacturing method of metallic magnetic material for high frequency - Google Patents
Manufacturing method of metallic magnetic material for high frequency Download PDFInfo
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- JP3556032B2 JP3556032B2 JP34990395A JP34990395A JP3556032B2 JP 3556032 B2 JP3556032 B2 JP 3556032B2 JP 34990395 A JP34990395 A JP 34990395A JP 34990395 A JP34990395 A JP 34990395A JP 3556032 B2 JP3556032 B2 JP 3556032B2
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- Prior art keywords
- magnetic material
- oxide
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- metal
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- 239000000696 magnetic material Substances 0.000 title claims description 12
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000013078 crystal Substances 0.000 claims description 12
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 229910044991 metal oxide Inorganic materials 0.000 claims description 8
- 150000004706 metal oxides Chemical class 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 5
- 239000011812 mixed powder Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 2
- 239000007769 metal material Substances 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- 238000000034 method Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000004907 flux Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
- H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Magnetic Ceramics (AREA)
- Hard Magnetic Materials (AREA)
- Soft Magnetic Materials (AREA)
Description
【０００１】
【発明の属する技術分野】
本発明は、平滑チョークコイル、トランス等の高透磁率合金磁心等に用いられる高周波用金属磁性材料の製造方法に関するものである。
【０００２】
【従来の技術】
現在、平滑チョークコイル等は、小型化が著しく進んでいる。これは、高周波領域における磁気損失が小さいことを最も重要視していたためであり、従来は、その材料として、比抵抗の大きいフェライトが使用されてきた。
【０００３】
一般に、チョークコイル、トランス等に使用されているフェライトは、主成分に対して微量副成分であるＳｉＯ２，ＣａＯ，ＨｆＯ２，Ｎｂ２Ｏ５，Ｔａ２Ｏ５，Ｖ２Ｏ５，ＺｒＯ２等の酸化物を混合し、焼結を行っている。
【０００４】
混合されている微量副成分は、焼結の過程で粒界に析出し、高抵抗の粒界層を形成することによって、渦電流損失を小さくすることが知られている。
【０００５】
【発明が解決しようとする課題】
しかし、フェライトでは、飽和磁束密度が低く、３〜５ＫＧ程度しかない。このため、飽和を防ぐためには、チョークコイルを大型化しなければならないという問題点があった。
【０００６】
そこで、本発明の課題は、飽和磁束密度が高く、磁気損失の小さな、高周波用金属磁性材料の製造方法を提供することにある。
【０００７】
【課題を解決するための手段】
本発明によれば、結晶粒界が少なくとも１種以上の酸化物からなる高周波用金属磁性材料の製造方法であって、主成分となる金属酸化物の粉末にＳｉＯ２，ＣａＯ，ＨｆＯ２，Ｎｂ２Ｏ５，Ｔａ２Ｏ５，Ｖ２Ｏ５，ＺｒＯ２のうち少なくとも１つ以上の酸化物を混合する工程▲１▼、その混合粉末をプレスする工程▲２▼、プレスにて作製した成形体を焼結させる工程▲３▼、更にその焼結体を水素ガスと不活性ガスの雰囲気中にて熱処理する工程▲４▼からなることを特徴とする高周波用金属磁性材料の製造方法が得られる。
【０００８】
又、本発明によれば、前記主成分となる金属酸化物がＦｅ２Ｏ３であることを特徴とする上記高周波用金属磁性材料の製造方法が得られる。
【０００９】
主成分である金属酸化物の粉末に、ＳｉＯ２，ＣａＯ，ＨｆＯ２，Ｎｂ２Ｏ５，Ｔａ２Ｏ５，Ｖ２Ｏ５，ＺｒＯ２のうち少なくとも１つ以上の酸化物を混合し、得られた混合粉末を必要な形状にプレスし、成形体を作り、焼結する。
【００１０】
焼結過程において、混合したＳｉＯ２，ＣａＯ，ＨｆＯ２，Ｎｂ２Ｏ５，Ｔａ２Ｏ５，Ｖ２Ｏ５，ＺｒＯ２の酸化物は、粒界に析出し、高抵抗で安定な粒界層を形成する。そして、得られた焼結体を更に水素ガスと不活性ガスの雰囲気中で還元することによって、粒を形成している主成分の金属酸化物から酸素が奪われ、金属が生成される。
【００１１】
この時、粒界を形成している酸化物は、粒を形成している主成分の金属酸化物よりも安定であるため、還元されずに高抵抗な粒界層を形成したままである。即ち、粒内は金属、粒界層は酸化物によって形成される組織となる。
【００１２】
つまり、主成分である金属酸化物に、ＳｉＯ２，ＣａＯ，ＨｆＯ２，Ｎｂ２Ｏ５，Ｔａ２Ｏ５，Ｖ２Ｏ５，ＺｒＯ２のうち少なくとも１つ以上の酸化物を混合し、プレスし、焼結し、更に、その焼結体を水素ガスと不活性ガスの雰囲気中で熱処理することによって、平滑チョークコイル、トランス等の高透磁率合金磁芯等に用いられる高周波用金属磁性材料が得られる。
【００１３】
【発明の実施の形態】
以下、本発明の実施の形態について、実施例を用いて説明する。
【００１４】
（実施例１）
高純度のＦｅ２Ｏ３粉末１００ｇに対して、表１に示す酸化物をそれぞれ添加し、ボールミルにて湿式粉砕し、混合した。
【００１５】
この混合粉末にバインダーとしてポリビニルアルコールを加えて造粒した後、プレス機によって混合粉末の成形体を成形した。
【００１７】
この成形体を、１３５０℃にて焼結し、焼結体（試料１〜４）を作製した。その後、焼結体を７００℃×２時間、水素ガス雰囲気によって熱処理を行った。
【００１８】
このようにして得られた試料を樹脂埋め込みによって固定し、その断面を紙やすりの＃３２０〜＃１５００まで研磨し、最後にバフ研磨にて鏡面とした。そして、ナイタ−ル（エタノール＋５％硝酸）にて断面をエッチングした後、ＥＤＸにて結晶粒内及び結晶粒界について線分析等を行った結果を表２に示す。
【００１９】
結晶粒界については、それぞれに添加した酸化物を検出し、結晶粒内については、Ｆｅの組成を示し、その他の成分は検出されなかった。このことから、本発明方法によって、高周波用金属磁性材料の結晶粒界をＳｉＯ２，ＣａＯ，ＨｆＯ２，Ｎｂ２Ｏ５，Ｔａ２Ｏ５，Ｖ２Ｏ５，ＺｒＯ２のうち少なくとも１つ以上の酸化物によって形成することができることがわかる。
【００２１】
（実施例２）
高純度のＦｅ２Ｏ３粉末１００ｇに対して、表３に示す酸化物をそれぞれ添加し、実施例１と同一の条件で作製した焼結体を、８００℃×６時間、水素ガス５０Ｖｏｌ％＋Ａｒガス５０Ｖｏｌ％の雰囲気によって熱処理を行った。
【００２２】
このようにして得られた試料を樹脂埋め込みによって固定し、その断面を紙やすりの＃３２０〜＃１５００まで研磨し、最後にバフ研磨にて鏡面とした。そして、ナイタ−ル（エタノール＋５％硝酸）にて断面をエッチングした後、ＥＤＸにて結晶粒内及び結晶粒界について線分析等行った結果を表４に示す。
【００２４】
結晶粒界については、添加を行った酸化物を検出し、結晶粒内については、Ｆｅの組成を示し、その他の成分は検出されなかった。このことから、実施例１と同様に、本発明方法によって、高周波用金属磁性材料の結晶粒界をＳｉＯ２，ＣａＯ，ＨｆＯ２，Ｎｂ２Ｏ５，Ｔａ２Ｏ５，Ｖ２Ｏ５，ＺｒＯ２のうち少なくとも１つ以上の酸化物によって形成することができることがわかる。
【００２６】
（実施例３）
実施例１及び実施例２にて得られた試料の電気抵抗及び磁気特性を測定した。電気抵抗の測定は、室温で４端子法にて行った。比較例として、純鉄（純度：９９．９％）を挙げた。その結果を表５に示す。特性値は、比較品である純鉄の値を１として規格化した値で示した。
【００２７】
電気抵抗については、純鉄と発明品との比較において、発明品がかなりの電気抵抗の上昇が認められる。このことは、結晶粒界に高電気抵抗物質が均一に分散したことを示している。また、磁気特性については、ほぼ同等である。
【００２９】
【発明の効果】
以上、述べたように、金属の酸化物にＳｉＯ２，ＣａＯ，ＨｆＯ２，Ｎｂ２Ｏ５，Ｔａ２Ｏ５，Ｖ２Ｏ５，ＺｒＯ２のうち少なくとも１つ以上の酸化物を混合し、プレス、焼結を行ない、更に、その焼結体を水素ガスと不活性ガスの雰囲気中で還元することによって、飽和磁束密度が高く、磁気損失が小さい高周波用金属磁性材料が得られる。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a method for producing a high-frequency metallic magnetic material used for a high-permeability alloy core such as a smooth choke coil and a transformer.
[0002]
[Prior art]
At present, miniaturization of smooth choke coils and the like has been significantly advanced. This is because the emphasis was placed on the fact that the magnetic loss in the high frequency region is small. Conventionally, ferrite having a large specific resistance has been used as the material.
[0003]
In general, ferrites used in choke coils, transformers, and the like are composed of SiO 2 , CaO, HfO 2 , Nb 2 O 5 , Ta 2 O 5 , V 2 O 5 , and ZrO 2 which are minor auxiliary components with respect to the main component. And sintering.
[0004]
It is known that the mixed minor component precipitates at the grain boundary during the sintering process and forms a high-resistance grain boundary layer, thereby reducing eddy current loss.
[0005]
[Problems to be solved by the invention]
However, ferrite has a low saturation magnetic flux density and is only about 3 to 5 KG. For this reason, there is a problem that the choke coil must be enlarged in order to prevent saturation.
[0006]
Therefore, an object of the present invention is to provide a method for producing a high-frequency metal magnetic material having a high saturation magnetic flux density and a small magnetic loss.
[0007]
[Means for Solving the Problems]
According to the present invention, there is provided a method for producing a high-frequency metal magnetic material in which a crystal grain boundary is made of at least one or more oxides, wherein SiO 2 , CaO, HfO 2 , Nb are added to a metal oxide powder as a main component. A step (1) of mixing at least one oxide of 2 O 5 , Ta 2 O 5 , V 2 O 5 , and ZrO 2 , a step (2) of pressing the mixed powder, and a molding formed by pressing A method for producing a high-frequency metallic magnetic material, characterized by comprising a step (3) of sintering the body and a step (4) of heat-treating the sintered body in an atmosphere of hydrogen gas and an inert gas. Can be
[0008]
Further, according to the present invention, there is provided the method for producing a high-frequency metal magnetic material, wherein the metal oxide as the main component is Fe 2 O 3 .
[0009]
At least one oxide of SiO 2 , CaO, HfO 2 , Nb 2 O 5 , Ta 2 O 5 , V 2 O 5 , and ZrO 2 is mixed with the powder of the metal oxide as the main component to obtain a mixture. The obtained mixed powder is pressed into a required shape to form a molded body and sintered.
[0010]
In the sintering process, the mixed oxides of SiO 2 , CaO, HfO 2 , Nb 2 O 5 , Ta 2 O 5 , V 2 O 5 , and ZrO 2 precipitate at the grain boundaries, and have high resistance and stable grain boundaries. Form a layer. Then, the obtained sintered body is further reduced in an atmosphere of a hydrogen gas and an inert gas, whereby oxygen is deprived from the main metal oxide forming the grains, and a metal is generated.
[0011]
At this time, since the oxide forming the grain boundary is more stable than the metal oxide as the main component forming the grain, it is not reduced and the high-resistance grain boundary layer is still formed. That is, the inside of the grain has a structure formed of metal and the grain boundary layer has a structure formed of oxide.
[0012]
That is, at least one oxide of SiO 2 , CaO, HfO 2 , Nb 2 O 5 , Ta 2 O 5 , V 2 O 5 , and ZrO 2 is mixed with the metal oxide as the main component, and pressed. Then, the sintered body is heat-treated in an atmosphere of a hydrogen gas and an inert gas to obtain a high-frequency metal magnetic material used for high-permeability alloy magnetic cores such as smooth choke coils and transformers. Is obtained.
[0013]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, embodiments of the present invention will be described using examples.
[0014]
(Example 1)
The oxides shown in Table 1 were added to 100 g of high-purity Fe 2 O 3 powder, wet-ground with a ball mill, and mixed.
[0015]
After polyvinyl alcohol was added as a binder to the mixed powder and granulated, a compact of the mixed powder was formed by a press machine.
[0017]
This molded body was sintered at 1350 ° C. to produce a sintered body (samples 1 to 4). Thereafter, the sintered body was subjected to a heat treatment in a hydrogen gas atmosphere at 700 ° C. for 2 hours.
[0018]
The sample thus obtained was fixed by embedding with a resin, and its cross section was polished to sandpaper # 320 to # 1500, and finally a mirror surface was obtained by buff polishing. Table 2 shows the results of line analysis of the inside of the crystal grains and the crystal grain boundaries by EDX after etching the cross section with nitral (ethanol + 5% nitric acid).
[0019]
The oxide added to each of the crystal grain boundaries was detected, and within the crystal grains, the composition of Fe was shown, and no other components were detected. From this, according to the method of the present invention, the crystal grain boundary of the high-frequency metal magnetic material is formed by at least one of SiO 2 , CaO, HfO 2 , Nb 2 O 5 , Ta 2 O 5 , V 2 O 5 , and ZrO 2. It can be seen that it can be formed by the oxide of.
[0021]
(Example 2)
The oxides shown in Table 3 were added to 100 g of the high-purity Fe 2 O 3 powder, and the sintered bodies produced under the same conditions as in Example 1 were heated at 800 ° C. for 6 hours at 50 vol% hydrogen gas + Ar gas. The heat treatment was performed in an atmosphere of 50% by volume of gas.
[0022]
The sample thus obtained was fixed by embedding with a resin, and its cross section was polished to sandpaper # 320 to # 1500, and finally a mirror surface was obtained by buff polishing. Table 4 shows the results of line analysis and the like of crystal grains and grain boundaries by EDX after etching the cross section with nitral (ethanol + 5% nitric acid).
[0024]
As for the crystal grain boundaries, oxides added were detected, and within the crystal grains, the composition of Fe was shown, and no other components were detected. From this, similarly to the first embodiment, according to the method of the present invention, the crystal grain boundaries of the high-frequency metal magnetic material are formed of SiO 2 , CaO, HfO 2 , Nb 2 O 5 , Ta 2 O 5 , V 2 O 5 , and ZrO. it can be seen that can be formed by at least one or more oxides of 2.
[0026]
(Example 3)
The electrical resistance and magnetic properties of the samples obtained in Example 1 and Example 2 were measured. The electrical resistance was measured at room temperature by a four-terminal method. As a comparative example, pure iron (purity: 99.9%) was mentioned. Table 5 shows the results. The characteristic values are shown as values obtained by standardizing the value of pure iron as a comparative product as 1.
[0027]
Regarding the electric resistance, in comparison between the pure iron and the invention, a considerable increase in the electric resistance of the invention is observed. This indicates that the high electric resistance material was uniformly dispersed in the crystal grain boundaries. Further, the magnetic properties are almost the same.
[0029]
【The invention's effect】
As described above, at least one oxide of SiO 2 , CaO, HfO 2 , Nb 2 O 5 , Ta 2 O 5 , V 2 O 5 , and ZrO 2 is mixed with the metal oxide, By performing pressing and sintering, and further reducing the sintered body in an atmosphere of hydrogen gas and an inert gas, a high-frequency metallic magnetic material having a high saturation magnetic flux density and a small magnetic loss can be obtained.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34990395A JP3556032B2 (en) | 1995-12-20 | 1995-12-20 | Manufacturing method of metallic magnetic material for high frequency |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34990395A JP3556032B2 (en) | 1995-12-20 | 1995-12-20 | Manufacturing method of metallic magnetic material for high frequency |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09171919A JPH09171919A (en) | 1997-06-30 |
| JP3556032B2 true JP3556032B2 (en) | 2004-08-18 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34990395A Expired - Fee Related JP3556032B2 (en) | 1995-12-20 | 1995-12-20 | Manufacturing method of metallic magnetic material for high frequency |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3556032B2 (en) |
-
1995
- 1995-12-20 JP JP34990395A patent/JP3556032B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH09171919A (en) | 1997-06-30 |
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