JPH02197504A - Method for stabilizing metal powder for magnetic recording - Google Patents
Method for stabilizing metal powder for magnetic recordingInfo
- Publication number
- JPH02197504A JPH02197504A JP1016245A JP1624589A JPH02197504A JP H02197504 A JPH02197504 A JP H02197504A JP 1016245 A JP1016245 A JP 1016245A JP 1624589 A JP1624589 A JP 1624589A JP H02197504 A JPH02197504 A JP H02197504A
- Authority
- JP
- Japan
- Prior art keywords
- metal powder
- alcohol
- water
- magnetic recording
- magnetic
- 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.)
- Pending
Links
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 39
- 239000000843 powder Substances 0.000 title claims abstract description 27
- 239000002184 metal Substances 0.000 title claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims description 10
- 230000000087 stabilizing effect Effects 0.000 title claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000001590 oxidative effect Effects 0.000 claims abstract description 11
- 229910052742 iron Inorganic materials 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 10
- 238000007254 oxidation reaction Methods 0.000 abstract description 10
- 229920005989 resin Polymers 0.000 abstract description 8
- 239000011347 resin Substances 0.000 abstract description 8
- 239000007789 gas Substances 0.000 description 15
- 230000006641 stabilisation Effects 0.000 description 11
- 238000011105 stabilization Methods 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 229910001873 dinitrogen Inorganic materials 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 229920002433 Vinyl chloride-vinyl acetate copolymer Polymers 0.000 description 1
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical compound [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- -1 polyethylene terephthalate Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000009279 wet oxidation reaction Methods 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Hard Magnetic Materials (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、主として磁気テープ、磁気ディスク等の磁気
記録媒体に用いられる、通常針状形を有する、鉄を主体
とする金属粉の安定化方法に関するものである。[Detailed Description of the Invention] [Field of Industrial Application] The present invention is directed to the stabilization of iron-based metal powder, which usually has an acicular shape and is mainly used in magnetic recording media such as magnetic tapes and magnetic disks. It is about the method.
磁気記録用金属粉の安定化方法は従来より数多くの技術
が知られている０例えば、強磁性金属微粒子をトルエン
等の有機溶剤に懸濁し空気等の酸化性ガス或いは水蒸気
を含むガスを通気する湿式の酸化安定化処理、叉例えば
窒素ガス等の不活性ガスを通気し、徐々に酸素ガス等の
酸化性ガスの流量を増加していく乾式の酸化安定化処理
等の方法が提案されている。特開昭５５−１２５２０５
、同５６−６９３０１、同５６−１２７７０１ 、同
５２−８５０５４、同５５−１６４００１、同５７−８
５９０１、同５７−９３５０４、同５８−１１０４３３
、同５８−１５９３１１ 。Many techniques have been known for stabilizing metal powder for magnetic recording. For example, fine ferromagnetic metal particles are suspended in an organic solvent such as toluene, and an oxidizing gas such as air or a gas containing water vapor is aerated through the suspension. Methods such as wet oxidation stabilization treatment or dry oxidation stabilization treatment in which an inert gas such as nitrogen gas is aerated and the flow rate of oxidizing gas such as oxygen gas is gradually increased have been proposed. . Japanese Patent Publication No. 55-125205
, 56-69301, 56-127701, 52-85054, 55-164001, 57-8
5901, 57-93504, 58-110433
, 58-159311.
〔発明が解決しようとする課題］
然し、従来知られている技術は主として金属粉の表面を
安定化することに止まっており、磁気記録媒体が作成さ
れた場合の性能の安定性向上を直接に目標としたもので
はなかった。勿論、磁気記録媒体の性能の安定化にとっ
て、金属粉の安定性が重要であることは疑いない、然し
、本発明者等は金属粉と樹脂の結合性が不足し、その為
に磁気記録媒体にしたときの性能の安定化が不十分であ
ることに着目した。磁気記録媒体の性能の安定性は、金
属粉と樹脂が如何に均一に、強く結合しているかによっ
て当然左右され、この点に関して、従来の磁気記録媒体
は性能の安定性に於いて未だ充分とは言えなかった。[Problems to be Solved by the Invention] However, conventionally known techniques mainly focus on stabilizing the surface of metal powder, and it is difficult to directly improve the stability of performance when a magnetic recording medium is created. It wasn't the goal. Of course, there is no doubt that the stability of the metal powder is important for stabilizing the performance of magnetic recording media. We focused on the fact that performance was not sufficiently stabilized when The stability of performance of a magnetic recording medium naturally depends on how uniformly and strongly the metal powder and resin are bonded, and in this regard, conventional magnetic recording media still have insufficient stability of performance. I couldn't say it.
本発明者らは上記問題点に付、鋭意研究を行った結果、
本発明を完成したものである。The inventors of the present invention have conducted intensive research to solve the above problems, and as a result,
This completes the present invention.
即ち、本発明の磁気記録用金属粉の安定化方法は、鉄を
主体とする金属粉に酸化性ガスを用いて表面が安定化さ
れた磁気記録用金属粉を製造する方法に於いて、予め、
水及び／又はアルコールを含有させたガスを通気し、水
及び／又はアルコールを０．２〜５．０モルχ吸着させ
た後、酸化性ガスを通気して安定化させることを特徴と
するものである。That is, the method for stabilizing metal powder for magnetic recording of the present invention is a method for producing metal powder for magnetic recording whose surface is stabilized by using an oxidizing gas on metal powder mainly composed of iron. ,
A gas containing water and/or alcohol is aerated to adsorb 0.2 to 5.0 moles of water and/or alcohol, and then an oxidizing gas is aerated for stabilization. It is.
本発明における鉄を主体とする金属粉は通常針状形のオ
キシ水酸化鉄を出発点とし、それにＳｉ、 ＡＩ等の耐
熱成分を被着したのち、焼成還元したＳｉ、ＡＩを含を
する針状形金属粉が普通であるが、これに限定はされな
い０本発明において特にポイントになるのは酸化処理に
先立って水及び／又はアルコールを含有させたガスを通
気することにある。The metal powder mainly composed of iron in the present invention usually starts with needle-shaped iron oxyhydroxide, coats it with a heat-resistant component such as Si or AI, and then burns and reduces it into needles containing Si or AI. Although shaped metal powder is common, the present invention is not limited to this.A particular point in the present invention is to aerate a gas containing water and/or alcohol prior to the oxidation treatment.
水、アルコールを含有させる方法は、例えば、窒素ガス
中に磁気として含有させる。その濃度としては、金属粉
への吸着量との関係で適宜選択されるが、２０％以下の
低濃度が好ましい、叉通気する時の温度は、やはり金ｉ
粉への吸着量との関係で適宜選択されるが、通常５０°
Ｃ以下の低温が好ましい、アルコールとしては低級アル
コールが用いられる。一般式Ｒ−ＯＨで表される物のう
ちＲが１０以下の脂肪族飽和及び不飽和アルコールが含
まれる。For example, water and alcohol can be contained in nitrogen gas as magnetism. The concentration is appropriately selected in relation to the amount of adsorption to the metal powder, but a low concentration of 20% or less is preferable.
It is selected appropriately depending on the amount of adsorption to the powder, but usually 50°
A low temperature of C or lower is preferable, and a lower alcohol is used as the alcohol. Among those represented by the general formula R-OH, aliphatic saturated and unsaturated alcohols in which R is 10 or less are included.
吸着させる量は０．２〜５．０モルχの範囲が必要であ
る、０．２モルχより低い場合は本発明の効果は出ない
、叉５．０モルχを越えると後段で酸化性ガスを通気し
た時の酸化処理の効率が低下し良くない０Ｍ化性ガスと
しては通常空気が用いられるがこれに限定はされない、
酸化性ガスの通気は水及び／又はアルコールを通気した
後である。The amount to be adsorbed must be in the range of 0.2 to 5.0 mol χ. If it is lower than 0.2 mol χ, the effect of the present invention will not be obtained, and if it exceeds 5.0 mol χ, it will be oxidized in the subsequent stage. Air is usually used as the 0M-forming gas, which reduces the efficiency of oxidation treatment when gas is aerated, but is not limited to this.
The oxidizing gas is vented after water and/or alcohol is vented.
一定量以上の水及び／又はアルコールを通気した後、酸
化性ガスを通気するに当たり、引き続き水及び／又はア
ルコールを含むガスを同時に通気してもよい。After a given amount or more of water and/or alcohol is aerated, when oxidizing gas is aerated, a gas containing water and/or alcohol may be simultaneously aerated.
以下、本発明を実施例により更に詳細に説明する。 Hereinafter, the present invention will be explained in more detail with reference to Examples.
実施例１
平均軸比が１：１０の針状含水酸化鉄にケイ酸ソーダを
用いてＳｉ化合物を被着したのち、空気中８００℃で焼
成し、ついでＨ２を８ｏｚ含むガスで５００°Ｃで還元
をしてＳｉを含む針状形磁性鉄粉を得た。（此れをＰ−
１とする）
この磁性鉄粉を口径ＩＨのチューブ型反応器に入れ、先
ず最初に１０°Ｃに於いて水を５χ含有する窒素ガスを
３時間通気した。一部金属粉をサンプリングし水の含有
量を測定したところ１．３４モルχであった。ついで０
゛Ｃにて酸素を１χ含む窒素ガスで１０時間通気し、つ
いで２０χの酸素を含む窒素ガスを５時間通気して安定
化された磁性鉄粉を得た。このようにして得られた安定
化された磁性鉄粉（これをＡ−１とする）を用いて樹脂
として塩化ビニル−酢酸ビニール共重合樹脂を用い添加
剤を少量入れて混合して磁性塗料を得、これをポリエチ
レンテレフタレートフィルムに塗布し、磁場配向した後
乾燥し、カレンダー処理を経て磁気テープとした。Example 1 After depositing a Si compound on acicular hydrated iron oxide with an average axial ratio of 1:10 using sodium silicate, it was fired at 800°C in air, and then heated at 500°C with a gas containing 8 oz of H2. After reduction, acicular magnetic iron powder containing Si was obtained. (P-
1) This magnetic iron powder was placed in a tube reactor with a diameter of IH, and first, nitrogen gas containing 5χ of water was bubbled through the reactor at 10°C for 3 hours. When some metal powder was sampled and the water content was measured, it was found to be 1.34 mol χ. Then 0
Nitrogen gas containing 1x oxygen was aerated at °C for 10 hours, and then nitrogen gas containing 20x oxygen was aerated for 5 hours to obtain stabilized magnetic iron powder. Using the thus obtained stabilized magnetic iron powder (this will be referred to as A-1), a magnetic paint is made by mixing a small amount of additives and using vinyl chloride-vinyl acetate copolymer resin as the resin. This was applied to a polyethylene terephthalate film, oriented in a magnetic field, dried, and calendered to form a magnetic tape.
此の磁気テープの特性を表１に示す、叉、磁性鉄粉Ａ−
１を用いた樹脂吸着量を測定した結果も表１に示す、更
に磁気テープを６０″Ｃ５関係湿度９０χの高温高湿下
で劣化促進テストを行い、テスト前後のＢｒの差ΔＢｒ
をχで表示した結果も表１に示す。The characteristics of this magnetic tape are shown in Table 1.
Table 1 also shows the results of measuring the amount of resin adsorption using 60"C5. Further, a deterioration acceleration test was performed on the magnetic tape at a high temperature and high humidity of 90χ relative humidity for 60" C5, and the difference in Br before and after the test ΔBr
The results expressed in χ are also shown in Table 1.
以上の実施例１によれば磁性鉄粉に対する樹脂吸着量が
高（、磁気テープとした時の酸化安定性が良好である。According to Example 1, the amount of resin adsorbed to the magnetic iron powder is high (and the oxidation stability when used as a magnetic tape is good).
更に、安定化処理する前のＨｃと、安定化処理後のＨｅ
を比較してもＨｃの低下は生じていなかった、これは安
定化処理により焼結や酸化皮膜の不均一と言う損傷を受
けていないことが推定出来る。Furthermore, Hc before stabilization treatment and He after stabilization treatment
Even when compared with the above, no decrease in Hc occurred, which suggests that the stabilization treatment did not cause any damage such as sintering or non-uniformity of the oxide film.
実施例２
実施例１で得られた還元直後の磁性鉄粉Ｐ−１を用いて
安定化処理を行った、実施例１における水を含有するガ
スを通気する時の温度を２０°Ｃに変えた以外は実施例
１と同一の条件で安定化処理を行った、安定化された磁
性鉄粉は実施例１と同一方法で磁気テープ化と特性の測
定を行った。結果を表１に示す。Example 2 Stabilization treatment was performed using the magnetic iron powder P-1 immediately after reduction obtained in Example 1. The temperature when aerating the water-containing gas in Example 1 was changed to 20 ° C. The stabilized magnetic iron powder was subjected to stabilization treatment under the same conditions as in Example 1, except for the above, and the stabilized magnetic iron powder was made into a magnetic tape and its properties were measured in the same manner as in Example 1. The results are shown in Table 1.
実施例３
実施例１で得られた還元直後の磁性鉄粉Ｐ−１を用いて
安定化処理をおこなった、実施例１における水をメタノ
ールに変更した以外は実施例１と同一の条件で安定化処
理を行った、安定化された磁性鉄粉は、実施例１と同一
方法で磁気テープ化と特性の測定を行った。結果を表１
に示す。Example 3 Stabilization treatment was performed using magnetic iron powder P-1 immediately after reduction obtained in Example 1. Stable under the same conditions as Example 1 except that water in Example 1 was changed to methanol. The stabilized magnetic iron powder subjected to the chemical treatment was made into a magnetic tape and its properties were measured in the same manner as in Example 1. Table 1 shows the results.
Shown below.
比較例１
実施例１で得られた還元直後の磁性鉄粉Ｐ−１を用いて
、安定化処理を行った、実施例１における水を含有する
窒素ガスの通気は行わず、直ちに酸素を含有する窒素ガ
スを通気し、それ以外の条件は実施例１と同一に行い、
その磁気テープ化した時の特性を測定した、結果を表１
に示すが樹脂吸着量が低く、磁気テープとしたときの酸
化安定性が低い。叉、Ｈｃも低下しており、酸化処理過
程での損傷が明らかである。Comparative Example 1 Stabilization treatment was performed using the magnetic iron powder P-1 immediately after reduction obtained in Example 1. The nitrogen gas containing water was not vented as in Example 1, but the oxygen-containing powder was immediately added to the magnetic iron powder P-1. The other conditions were the same as in Example 1,
Table 1 shows the results of measuring the characteristics when made into magnetic tape.
However, the amount of resin adsorbed is low, and the oxidation stability when made into a magnetic tape is low. Moreover, Hc also decreased, and damage during the oxidation treatment process was evident.
第１表
〔発明の効果〕
本発明の方法により得られる鉄を主体とする磁性金属粉
は、金属粉の表面に対する樹脂の吸着性が極めて良くな
り、磁気テープにしたときの酸化安定性が格段に向上す
る。叉製造時酸化性ガスにより金属粉を酸化する工程に
於いて通常発生するＨｅの低下をおさえることが出来る
。Table 1 [Effects of the Invention] The magnetic metal powder mainly composed of iron obtained by the method of the present invention has extremely good adsorption of resin to the surface of the metal powder, and has excellent oxidation stability when made into a magnetic tape. improve. Furthermore, it is possible to suppress the decrease in He that normally occurs in the process of oxidizing metal powder with an oxidizing gas during production.
特許出願人 三井東圧化学株式会社Patent applicant: Mitsui Toatsu Chemical Co., Ltd.
Claims (1)
定化された磁気記録用金属粉を製造する方法に於いて、
予め、水及び／又はアルコールを含有させたガスを通気
し、水及び／又はアルコールを０．２〜５．０モル％吸
着させた後、酸化性ガスを通気して安定化させることを
特徴とする磁気記録用金属粉の安定化方法。In a method for producing metal powder for magnetic recording whose surface is stabilized by using an oxidizing gas in metal powder mainly composed of iron,
A gas containing water and/or alcohol is aerated in advance to adsorb 0.2 to 5.0 mol% of water and/or alcohol, and then an oxidizing gas is aerated to stabilize the material. A method for stabilizing metal powder for magnetic recording.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1016245A JPH02197504A (en) | 1989-01-27 | 1989-01-27 | Method for stabilizing metal powder for magnetic recording |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1016245A JPH02197504A (en) | 1989-01-27 | 1989-01-27 | Method for stabilizing metal powder for magnetic recording |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02197504A true JPH02197504A (en) | 1990-08-06 |
Family
ID=11911172
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1016245A Pending JPH02197504A (en) | 1989-01-27 | 1989-01-27 | Method for stabilizing metal powder for magnetic recording |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02197504A (en) |
-
1989
- 1989-01-27 JP JP1016245A patent/JPH02197504A/en active Pending
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