JPS58159306A - Manufacture of metallic magnetic powder - Google Patents
Manufacture of metallic magnetic powderInfo
- Publication number
- JPS58159306A JPS58159306A JP57042373A JP4237382A JPS58159306A JP S58159306 A JPS58159306 A JP S58159306A JP 57042373 A JP57042373 A JP 57042373A JP 4237382 A JP4237382 A JP 4237382A JP S58159306 A JPS58159306 A JP S58159306A
- Authority
- JP
- Japan
- Prior art keywords
- iron
- magnetic powder
- metallic
- metallic magnetic
- polyhydric alcohol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000006247 magnetic powder Substances 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229910052742 iron Inorganic materials 0.000 claims abstract description 28
- 239000002184 metal Substances 0.000 claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 claims abstract description 26
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 17
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 11
- 150000003839 salts Chemical class 0.000 claims abstract description 11
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 10
- 239000010941 cobalt Substances 0.000 claims abstract description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000006104 solid solution Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 abstract description 8
- 238000007254 oxidation reaction Methods 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 abstract description 6
- 150000002739 metals Chemical class 0.000 abstract description 4
- 238000009835 boiling Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract 1
- 150000004820 halides Chemical class 0.000 abstract 1
- 229910017053 inorganic salt Inorganic materials 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 230000005415 magnetization Effects 0.000 description 9
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 150000001868 cobalt Chemical class 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000003463 sulfur Chemical class 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 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
- H01F1/032—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 hard-magnetic materials
- H01F1/04—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 hard-magnetic materials metals or alloys
- H01F1/06—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 hard-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/061—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 hard-magnetic materials metals or alloys in the form of particles, e.g. powder with a protective layer
Abstract
Description
【発明の詳細な説明】
この発明は鉄を主体とする金属磁性粉末の製造方法に関
し、その目的とするところは酸化安定性に優れる前記の
金属磁性粉１ｅ製造方法を提供することｋある。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a metal magnetic powder mainly composed of iron, and an object thereof is to provide a method for producing the metal magnetic powder 1e described above which has excellent oxidation stability.
鉄を主体とする金属磁性粉末は従来の一化物系磁性粉末
に比較して優れた磁気特性を有して埴るが、反面空気中
で非常に酸化を受は易く、飽和磁化量が経時的に低下し
、貯蔵安定性に欠けるという間層がある・
このため、この種の金属磁性粉末を有機溶剤中あるいは
窒素Ｗ囲気中で微量の溶存酸素あるいは低濃度の酸素含
有ガス亀どｋより酸化して粒子表ｒｆＩＪに酸化物被膜
を形成するなどの方法で酸化安定性の改善が図られてい
るが、このようｋして形成された酸化物被膜は未だ充分
に安定したものではなくまたそれほど緻密なものでもな
い丸め充分に満足できる結果は得られていない＠
この発明者らはかかる現吠に鐙み種々検討を行なった結
果、既Ｋｌｌ！化物被膜を形成し丸鉄を主体とする金属
磁性粉末を、鉄、コバルト、ニッケルから選ばれる少な
くとも一種を含も金属塩を含む多価アルコール中に分散
し、次いでこれを加熱すると既に前記磁性粉末の粒子表
面に形成された酸化物被−中に鉄、コバルト、ニッケル
から選ばれる少亀くとも一種の金属が固溶されて酸化物
被膜が安定化すると同時に駿密化され、その結果酸化安
定性が充分に向上されることを晃いだし、この発明をな
すに至った。Metallic magnetic powders mainly composed of iron have superior magnetic properties compared to conventional monide-based magnetic powders, but on the other hand, they are highly susceptible to oxidation in the air, and the amount of saturation magnetization decreases over time. Therefore, this type of metal magnetic powder is oxidized in an organic solvent or in a nitrogen atmosphere using a trace amount of dissolved oxygen or a low concentration of oxygen-containing gas. The oxidation stability has been improved by methods such as forming an oxide film on the particle surface rfIJ, but the oxide film formed in this way is still not sufficiently stable and The rounding is not very precise.A fully satisfactory result has not been obtained.The inventors of the present invention have made various studies based on the current situation. When a metal magnetic powder that forms a compound film and is mainly made of round iron is dispersed in a polyhydric alcohol containing a metal salt containing at least one selected from iron, cobalt, and nickel, and then heated, the magnetic powder is already formed. At least a small amount of metal selected from iron, cobalt, and nickel is dissolved in the oxide coating formed on the surface of the particles, and the oxide coating is stabilized and densified, resulting in oxidation stability. The present inventors have found that the properties can be sufficiently improved, and have come up with this invention.
この発明において使用する多価アルコールとしては、沸
点が１５０℃以上の、たとえばエチレンクリコール、ポ
リエチレングリコール、プロピレングリコール、グリセ
リンなどが好適なものとして使用され、これら高沸点の
多価アルコール中に鉄塩また社コバルト塩もしくはニッ
ケル塩等を溶解してできたアルコラード溶液中に１既に
酸化物被膜を形成した鉄を主体とする金属磁性粉末を分
散した後、１５０℃以上の温度で加熱すると、多価アル
コールの作用で既に前記金属磁性粉末の粒子表面に形成
された一−Ｆｅ２Ｏ，などの拳化鉄被膜が還元されると
同時に仁の被膜中に鉄、コバルト、ニッケルなどの金属
が導入拡散され、これらの金属を！ＨＩＬした安定で緻
密なマグネタイト被膜が形成されて酸化安定性が向上す
る。このような酸化物被膜の還元と、被膜中への金属の
導入拡散は、１５０℃以下の加熱処理ではおこ抄Ｋ＜＜
、高温になるほど促進されて酸化安定性が向上するが、
還元されると同時に金属の被膜中への導入拡散も充分に
打電われるため３００”Ｃ以上の１１度で加熱処理する
必要はない・
多価アルコール申に溶解する金属塩としては、鉄または
コバルシもしくはニッケル〇へロゲン化物、水酸化物、
炭醗塩、硫讃塩などの無機塩の他、これらの金属の有機
金属塩等が好適なものとして使用され、これらの金属塩
が多価アルコール中に溶解されると多価アルコールと反
応して金属アルコラードが生成される〇
粒子表面に酸化物被膜を形成する前の鉄を主体とする金
属磁性粉末としては、金属鉄粉末の他、鉄にＣｏｓ Ｎ
ｉＮ Ａｌ 、Ｃｒｓ Ｍｎ％Ｓｉ 、Ｚｎなどを含有
させた金属磁性粉末が広く包含され、液中還元法、気相
還元法、電解法のいかんを問わずあらゆる方法で製造さ
れえ従来の鉄を主体とする金属磁性粉末がいずれも用い
られる。As the polyhydric alcohol used in this invention, those having a boiling point of 150°C or higher, such as ethylene glycol, polyethylene glycol, propylene glycol, and glycerin, are preferably used. In addition, after dispersing metal magnetic powder mainly composed of iron on which an oxide film has already been formed in an Alcolade solution made by dissolving cobalt salt or nickel salt, etc., and heating it at a temperature of 150°C or higher, polyvalent Due to the action of alcohol, the Fe2O film already formed on the surface of the metallic magnetic powder particles is reduced, and at the same time, metals such as iron, cobalt, and nickel are introduced and diffused into the film. These metals! A stable and dense magnetite film with HIL is formed, improving oxidation stability. Such reduction of the oxide film and the introduction and diffusion of metal into the film are caused by heat treatment below 150°C.
, the higher the temperature, the faster the oxidation stability improves,
At the same time as the reduction, the introduction and diffusion of the metal into the film is sufficiently electrified, so there is no need for heat treatment at 11 degrees above 300"C. Metal salts that dissolve in polyhydric alcohol include iron, cobalt, or Nickel 〇 herogenide, hydroxide,
In addition to inorganic salts such as charcoal salts and sulfur salts, organic metal salts of these metals are preferably used, and when these metal salts are dissolved in a polyhydric alcohol, they react with the polyhydric alcohol. Metallic magnetic powder containing iron as a main component before forming an oxide film on the particle surface includes metallic iron powder as well as CosN on iron.
It includes a wide range of metal magnetic powders containing iNAl, CrsMn%Si, Zn, etc., and can be produced by any method, including liquid reduction, vapor phase reduction, and electrolytic methods. Both metal magnetic powders are used.
次に、この発明の実施例について説明する。Next, embodiments of the invention will be described.
実施例１
粒径０．３μ、軸比（長軸／短軸）１０／１、飽和磁化
量σｓ １６５ ｅｍｕ／ｇ、保磁力１４００！ルステ
ツドの金属鉄粉末１１ｆをトルエン１（ｌ中に分散させ
、流速５／／分の空気を分散液中にバブリングさせなが
ら５時間攪拌処理して瞭化鉄からなる酸化物被膜で覆わ
れた粒径０．３μ、軸比（長軸／短軸）１０／１．飽和
磁化量ｇ ｓ １３６ ｅｍｕ／９、保磁力１４１０エ
ルステツドの金属鉄粉末を得た。Example 1 Particle size 0.3μ, axial ratio (major axis/minor axis) 10/1, saturation magnetization σs 165 emu/g, coercive force 1400! Rusted's metallic iron powder 11f was dispersed in 1 l of toluene and stirred for 5 hours while bubbling air at a flow rate of 5/min into the dispersion to form particles covered with an oxide film made of iron. A metallic iron powder was obtained with a diameter of 0.3 μ, an axial ratio (major axis/minor axis) of 10/1, a saturation magnetization g s of 136 emu/9, and a coercive force of 1410 oersted.
次いでこの酸化物被膜で覆われた金属鉄粉末１００重量
部を、ポリエチレングリコール（平均分子量６００）２
００重量部に塩化ニッケル（ＮｉＣ１２・６ Ｈ２Ｏ）
８重量部を溶かしてできたアルコラード溶液中に分散
させ、常圧下２５０°Ｇで４時間反応させた。これを水
洗、乾燥し、ニッケルを固溶したマグネタイトからなる
酸化物被膜を粒子表面に形成した金属鉄粉末を得え。得
られた金属鉄粉末は粒径が０．３μ、軸比（長軸／短軸
）が１０／１、飽和磁化量σＳが１２８ｅｍｕ／９で、
保磁力は１４２０エルステツドであった。Next, 100 parts by weight of the metallic iron powder covered with this oxide film was mixed with polyethylene glycol (average molecular weight 600) 2
00 parts by weight of nickel chloride (NiC12.6 H2O)
It was dispersed in an Alcolade solution prepared by dissolving 8 parts by weight, and reacted at 250°G under normal pressure for 4 hours. This is washed with water and dried to obtain metallic iron powder with an oxide film made of magnetite in which nickel is dissolved as a solid solution formed on the particle surface. The obtained metallic iron powder had a particle size of 0.3μ, an axial ratio (major axis/minor axis) of 10/1, and a saturation magnetization σS of 128 emu/9.
The coercive force was 1420 oersted.
実施例２
実施例ＩＫ、おいて塩化ニッケルに代えて塩化コバル）
（ＣｏＣｌ２．６ Ｈ２Ｏ）を同量使用した以外は実
施例１と同様にしてコバルトを固溶したマグネタイトか
らなる酸化物被膜を粒子表面に形成した粒径０．３μ、
軸比（長軸／短軸）１Ｇ／１、飽和磁化量ｇｓ １３１
ｅｍｕ／ ９、保磁力１４５０エルステツドの金属鉄
粉末を得た。Example 2 Cobal chloride instead of nickel chloride in Example IK)
A particle size of 0.3 μ, in which an oxide film made of magnetite containing cobalt as a solid solution was formed on the particle surface in the same manner as in Example 1 except that the same amount of (CoCl2.6 H2O) was used.
Axial ratio (major axis/minor axis) 1G/1, saturation magnetization gs 131
Metallic iron powder with emu/9 and coercive force of 1450 oersted was obtained.
実施例３
実施例１において塩化ニッケルに代えて塩化鉄（ＦｅＣ
ｌ、 、 Ｈ２Ｏ）を同量使用した以外は実施例１と同
様にして鉄を固溶したマグネタイトからなる酸化物被膜
を粒子表面に形成した粒径０．３μ、軸比（長軸／短軸
）１０／１、飽和磁化量σｓ１３０ｅｍｕ／９、保磁力
１３９０エルステツドの金属鉄粉末を得た。Example 3 In Example 1, iron chloride (FeC) was used instead of nickel chloride.
An oxide film made of magnetite containing iron as a solid solution was formed on the surface of the particles in the same manner as in Example 1, except that the same amount of H2O was used. ) 10/1, a saturation magnetization σs of 130 emu/9, and a coercive force of 1390 oersted.
各実施例で得られた金属鉄粉末および実施例１のニッケ
ル固溶処理前の酸化鉄からなる酸化物被膜で覆われた金
属鉄粉末（比較例）を、６０℃、９ｏＩＲｕの条件下で
２４時間空気中に放置し、放置後の飽和磁化量を測定し
て放置前の飽和磁化量からの低下率を調べた。The metallic iron powder obtained in each example and the metallic iron powder covered with an oxide film made of iron oxide before the nickel solid solution treatment of Example 1 (comparative example) were heated at 60°C and 9oIRu for 24 hours. The sample was left in the air for an hour, and the saturation magnetization after being left was measured to examine the rate of decrease from the saturation magnetization before being left.
下表はその結果である。The table below shows the results.
表
上表から明らかなように、この発明で得られた金属鉄粉
末（実施例１〜３）はいずれも従来の拳化物被膜を有す
る金属鉄粉末（比較例）Ｋ比し、飽和磁化量Ｃ８の低下
率が小さく、このことからこの発明の製造方法によれば
酸化安定性に優れた鉄を主体とする金属磁性粉末が得ら
れることがわかる。As is clear from the above table, all of the metallic iron powders obtained by the present invention (Examples 1 to 3) have a saturation magnetization amount of C8 The rate of decrease in is small, which indicates that the production method of the present invention yields a metal magnetic powder mainly composed of iron with excellent oxidation stability.
Claims (1)
する金属磁性粉末を、鉄、コバルト、ニッケルから選ば
れる少なくとも一種を含も金属塩を溶解した多価アルコ
ール中に分散し、これを加熱して鉄を主体とする金属磁
性粉末の粒子表面に１鉄、コバルト、ニッケルから迩ば
れる少なくとも一種の金属を固溶した酸化物被膜を形成
することを特徴とする金属磁性粉末の製造方法1. A metal magnetic powder mainly composed of iron with an oxide film formed on the surface of the powder particles is dispersed in a polyhydric alcohol containing a metal salt containing at least one selected from iron, cobalt, and nickel. A method for producing a metal magnetic powder, which comprises heating the powder to form an oxide film containing at least one metal selected from iron, cobalt, and nickel as a solid solution on the particle surface of a metal magnetic powder mainly composed of iron.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57042373A JPS58159306A (en) | 1982-03-17 | 1982-03-17 | Manufacture of metallic magnetic powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP57042373A JPS58159306A (en) | 1982-03-17 | 1982-03-17 | Manufacture of metallic magnetic powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58159306A true JPS58159306A (en) | 1983-09-21 |
| JPH0447962B2 JPH0447962B2 (en) | 1992-08-05 |
Family
ID=12634236
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP57042373A Granted JPS58159306A (en) | 1982-03-17 | 1982-03-17 | Manufacture of metallic magnetic powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58159306A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS644001A (en) * | 1987-06-26 | 1989-01-09 | Taiyo Yuden Kk | Manufacture of magnetic powder for magnetic recording medium |
| KR101016560B1 (en) | 2003-09-09 | 2011-02-22 | 도와 홀딩스 가부시키가이샤 | Metal magnetic powder and process for producing the same |
-
1982
- 1982-03-17 JP JP57042373A patent/JPS58159306A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS644001A (en) * | 1987-06-26 | 1989-01-09 | Taiyo Yuden Kk | Manufacture of magnetic powder for magnetic recording medium |
| KR101016560B1 (en) | 2003-09-09 | 2011-02-22 | 도와 홀딩스 가부시키가이샤 | Metal magnetic powder and process for producing the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0447962B2 (en) | 1992-08-05 |
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