JPH01281704A - Surface treatment of magnetic metal powder - Google Patents

Surface treatment of magnetic metal powder

Info

Publication number
JPH01281704A
JPH01281704A JP63110350A JP11035088A JPH01281704A JP H01281704 A JPH01281704 A JP H01281704A JP 63110350 A JP63110350 A JP 63110350A JP 11035088 A JP11035088 A JP 11035088A JP H01281704 A JPH01281704 A JP H01281704A
Authority
JP
Japan
Prior art keywords
magnetic metal
metal powder
benzoyl peroxide
surface treatment
iron
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
Application number
JP63110350A
Other languages
Japanese (ja)
Inventor
Kazufumi Hisaoka
久岡 一史
Tadayoshi Saruwatari
猿渡 忠良
Akira Ichiyanagi
彰 一柳
Masanori Konno
金野 聖憲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsui Mining and Smelting Co Ltd
Original Assignee
Mitsui Mining and Smelting Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Mitsui Mining and Smelting Co Ltd filed Critical Mitsui Mining and Smelting Co Ltd
Priority to JP63110350A priority Critical patent/JPH01281704A/en
Publication of JPH01281704A publication Critical patent/JPH01281704A/en
Pending legal-status Critical Current

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/06Magnets 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
    • H01F1/061Magnets 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

Landscapes

  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Magnetic Record Carriers (AREA)
  • Hard Magnetic Materials (AREA)
  • Paints Or Removers (AREA)
  • Powder Metallurgy (AREA)

Abstract

PURPOSE:To improve oxidation resistance and dispersion properties by performing surface treatment of a magnetic metal powder which consists of iron, or mainly consists of iron with hydrogen benzoyl. CONSTITUTION:A magnetic metal powder which consists of iron or mainly consists of iron is subject to surface treatment with benzoyl peroxide. Namely, the magnetic metal powder may be subject to surface treatment using benzoyl peroxide by normal method, but preferably the magnetic metal powder should be dipped into a treatment solution where benzoyl peroxide is dissolved or dispersed into an organic solvent. Also, benzoyl peroxide may be used alone or may be used along with a tertiary amine such as dimethylaniline to increase radical generation rate for further improved effect. It allows oxidation resistance and dispersion properties to be improved also for a magnetic metal powder with a high specific surface area.

Description

【発明の詳細な説明】 〈産業上の利用分野〉 本発明は、磁性金属粉末の耐酸化性及び分散性を向上さ
せるための磁性金属粉末の表面処理法に関する。
DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention relates to a method for surface treatment of magnetic metal powder to improve its oxidation resistance and dispersibility.

〈従来の技術〉 従来、オーディオテープ、ビデオテープなどの磁気テー
プ等の磁性粉末としては主に酸化鉄系磁性粉末が用いら
れていたが、近年、磁気テープの高性能化の要求に対応
するために鉄又は鉄を主体とする磁性金属粉末が用いら
れるようになってきた。しかし、この磁性金属粉末は、
従来の酸化鉄系磁性粉末と比較した場合優れた磁性特性
を有しているが、金属粉であるため化学的に不安定であ
るという欠点を有している。すなわち、磁性金属粉末は
空気中にて酸化され易いので場合によっては発火の危険
があるとともに、得られた磁気テープ等の磁気特性が経
時的に低下してしまうという問題がある。又、磁性金属
粉末は酸化鉄系磁性粉末と較べて凝集し易いので、例え
ば磁気テープ製造における塗料化の際に分散性が悪いと
いう問題がある。
<Conventional technology> In the past, iron oxide-based magnetic powders were mainly used as magnetic powders for magnetic tapes such as audio tapes and video tapes, but in recent years, iron oxide-based magnetic powders have been used to meet the demand for higher performance magnetic tapes. Iron or magnetic metal powders mainly composed of iron have come to be used. However, this magnetic metal powder
Although it has superior magnetic properties when compared to conventional iron oxide magnetic powder, it has the disadvantage of being chemically unstable because it is a metal powder. That is, since magnetic metal powder is easily oxidized in the air, there is a risk of ignition in some cases, and there is a problem that the magnetic properties of the obtained magnetic tape etc. deteriorate over time. Furthermore, since magnetic metal powders tend to aggregate more easily than iron oxide-based magnetic powders, there is a problem of poor dispersibility when, for example, they are made into paints for manufacturing magnetic tapes.

そこで、従来においては発火を防止し且つ安定化するた
めに磁性金、嘱粉末を気相あるいは液相にて徐々に酸化
して粒子表面に緻密な酸化皮膜を形成しており、さらに
耐酸化性を高めるとともに分散性を向上させるための表
面処理法が種々検討されている。例えば、特開昭49−
97738号公報には金属磁性粉末と高級脂肪酸粉末と
を有機溶剤中で撹拌混合することにより粒子表面に高級
脂肪酸基膜を形成する方法が開示されている。
Conventionally, in order to prevent and stabilize ignition, magnetic gold powder is gradually oxidized in the gas phase or liquid phase to form a dense oxide film on the particle surface, which further improves oxidation resistance. Various surface treatment methods have been studied to increase the dispersibility as well as to increase the dispersibility. For example, JP-A-49-
No. 97738 discloses a method of forming a higher fatty acid base film on the particle surface by stirring and mixing metal magnetic powder and higher fatty acid powder in an organic solvent.

一方、短波長記録による高記録密度化の流れの中で磁性
金属粉末の微細化が進められているが、磁性金属粉末に
おいては微細になればなるほど酸化され易くなるととも
に分散しにくくなるという問題がある。よって、微細化
された磁性金属粉末、例えば比表面積55m’ / g
以上の高比表面積を有する磁性金属粉末においては上述
したような表面処理では対処できないというのが現状で
ある。
On the other hand, with the trend toward higher recording densities through shorter wavelength recording, magnetic metal powders are being made finer, but the problem with magnetic metal powders is that the finer they become, the more easily they are oxidized and the more difficult they are to disperse. be. Therefore, a finely divided magnetic metal powder, for example, a specific surface area of 55 m'/g
The current situation is that magnetic metal powders having such a high specific surface area cannot be treated with the above-mentioned surface treatment.

本発明はこのような事情に鑑み、高比表面積の磁性金属
粉末に対しても耐酸化性及び分散性の双方を向上させる
ことができろ磁性金属粉末の表面処理法を提供すること
を目的とする。
In view of these circumstances, the present invention aims to provide a surface treatment method for magnetic metal powder that can improve both oxidation resistance and dispersibility even for magnetic metal powder with a high specific surface area. do.

く課題を解決するための手段〉 前記目的を達成する本発明の構成は鉄又は鉄を主体とす
る磁性金属粉末を過酸化ベンゾイルで表面処理すること
を特徴とする。
Means for Solving the Problems> The structure of the present invention that achieves the above object is characterized in that iron or magnetic metal powder mainly composed of iron is surface-treated with benzoyl peroxide.

本発明では、過酸化ベンゾイルを用いて常法により磁性
金属粉末の表面処理を行えばいいのであるが、好適には
過酸化ベンゾイルを有機溶媒に溶解又は分散した処理液
中に磁性金属粉末を浸漬することによって行うのがよい
In the present invention, the magnetic metal powder may be surface-treated by a conventional method using benzoyl peroxide, but it is preferable to immerse the magnetic metal powder in a treatment solution in which benzoyl peroxide is dissolved or dispersed in an organic solvent. It is better to do this by doing.

本発明で過酸化ベンゾイルは単独で用いてもよいが、ラ
ジカル生成速度を上げるため、ジメチルアニリン等の第
三級アミンを併用することにより、さらにその効果が顕
著に現れるようになる。
In the present invention, benzoyl peroxide may be used alone, but in order to increase the rate of radical generation, the effect becomes even more pronounced when a tertiary amine such as dimethylaniline is used in combination.

過酸化ベンゾイルは表面処理された磁性金属粉末!!量
に対して0.1〜7重量%、好ましくは3〜Sii量%
となる量を用いるのがよい。
Benzoyl peroxide is a surface-treated magnetic metal powder! ! 0.1 to 7% by weight, preferably 3 to Sii% by weight based on the amount
It is best to use an amount that satisfies the following.

これは0.1重量%未満では表面処理効果が不十分であ
り、7重量%を超えて用いても増量効果がみられないか
らである。
This is because if it is less than 0.1% by weight, the surface treatment effect is insufficient, and if it is used in excess of 7% by weight, no increase in weight is observed.

また、本発明方法が適用できる磁性金属粉末としては鉄
又は鉄を主体としてこれにNi。
The magnetic metal powder to which the method of the present invention can be applied is iron or iron as a main component, and Ni.

Co、Zn、Mn、Cr、Mg、P、AI、Si等を少
なくとも1種以上添加したものなどがあるが、この磁性
金属粉末は酸化皮膜形成前のものでもよいし、常法によ
り全体にあるいは部分的に酸化皮膜を形成したものでも
よい。
There are magnetic metal powders to which at least one of Co, Zn, Mn, Cr, Mg, P, AI, Si, etc. is added, but this magnetic metal powder may be before the formation of an oxide film, or it may be completely or It may also be one in which an oxide film is partially formed.

ここで、過酸化ベンゾイルを有機溶媒に溶解・分散した
処理液中に磁性金属粉末を浸漬することにより行う表面
処理法について説明する。
Here, a surface treatment method performed by immersing magnetic metal powder in a treatment liquid in which benzoyl peroxide is dissolved and dispersed in an organic solvent will be described.

過酸化ベンゾイルを溶解・分散するための有機溶媒とし
ては例えば、トルエン、メチルイソブチルケトン(MI
BK) 、エタノール等がある。これら溶媒を用いて処
理液を調製する場合には、過酸化ベンゾイルが表面処理
された磁性金属粉末重量に対して上述したように0.1
〜71i量%、好ましくは3〜5重量%となるようにす
る。この処理液による磁性金属粉末の処理60℃以上で
行うのがよい。この処理は0.5〜10時間、好ましく
は1〜5時間程度浸漬した後磁性金属粉末を取り出して
乾燥することにより行ってもよいし、磁性金属粉末を浸
漬している処理液から溶媒を蒸発・留去し、全て留去し
た後取り出すようにしてもよい。
Examples of organic solvents for dissolving and dispersing benzoyl peroxide include toluene, methyl isobutyl ketone (MI
BK), ethanol, etc. When preparing a treatment solution using these solvents, benzoyl peroxide is 0.1% of the weight of the surface-treated magnetic metal powder as described above.
~71i% by weight, preferably 3 to 5% by weight. The treatment of magnetic metal powder with this treatment liquid is preferably carried out at a temperature of 60° C. or higher. This treatment may be carried out by immersing the magnetic metal powder for 0.5 to 10 hours, preferably 1 to 5 hours, then taking it out and drying it, or by evaporating the solvent from the treatment liquid in which the magnetic metal powder is immersed. - You may distill it off and take it out after all of it has been distilled off.

さらに、この表面処理法を実施する場合には磁性金属粉
末として酸化膜形成前のものを用い、該磁性金属粉末が
浸漬された処理液に酸素含有ガスを導入することによゆ
、表面処理及び酸化皮膜形成を同時に行うようにするの
が好適である。
Furthermore, when carrying out this surface treatment method, the magnetic metal powder is used before oxide film formation, and the surface treatment and It is preferable to form the oxide film at the same time.

く実 施 例〉 以下に本発明の実施例を詳細に説明する。Example of implementation Examples of the present invention will be described in detail below.

(実施例1) ■ 表面処理 過酸化ベンゾイル60gをトルエン31!中に溶解して
処理液を調製し、この処理液に酸化皮膜形成後の磁性金
属粉末(長軸0.15μm1軸比7〜10、比表面積6
0rn’/ g) 1kgを浸漬し、−晩装置した。次
−にこの浸漬液を内容積201のステンレス製密閉容器
に全量を投入し、内部温度を60℃に保持しつつ5%酸
素含有ガスを201/分の流量で処理液中に導入するこ
とにより溶媒を完全に蒸発させて表面処理された磁性金
属粉末を取り出し、乾燥した。
(Example 1) ■ Surface treatment 60g of benzoyl peroxide to 31g of toluene! A treatment solution is prepared by dissolving the magnetic metal powder (major axis 0.15 μm, uniaxial ratio 7 to 10, specific surface area 6
0rn'/g) 1 kg was immersed and left overnight. Next, the entire amount of this immersion liquid was poured into a stainless steel airtight container with an internal volume of 201 cm, and while the internal temperature was maintained at 60°C, 5% oxygen-containing gas was introduced into the processing liquid at a flow rate of 201 m/min. The solvent was completely evaporated and the surface-treated magnetic metal powder was taken out and dried.

この表面処理磁性金属粉末の磁性特性、比表面積及び耐
酸化性を測定した。この結果を第1表に示す。なお、耐
酸化性は表面処理磁性金属粉末を60℃、90%RHの
空気中に暴露し、1週間経過後の飽和磁化を測定し、こ
の飽和磁化の暴露前の飽和磁化に対する劣化率(ΔσS
)で評価した。
The magnetic properties, specific surface area, and oxidation resistance of this surface-treated magnetic metal powder were measured. The results are shown in Table 1. The oxidation resistance is determined by exposing the surface-treated magnetic metal powder to air at 60°C and 90% RH, measuring the saturation magnetization after one week, and calculating the deterioration rate (ΔσS) of this saturation magnetization with respect to the saturation magnetization before exposure.
) was evaluated.

■ 磁気シートの作製 上記表面処理磁性金属粉末を用い、下記の組成でサンド
ミルにより分散塗料化した。
(2) Preparation of magnetic sheet The surface-treated magnetic metal powder described above was used to form a dispersion coating using a sand mill using the following composition.

塗料組成 (3f量部) 表面処理磁性金属粉末       100VAGH(
塩ビ・酢ビ共重合体)1) ポリウレタン樹脂           1ルシチン 
               2メチルエチルケトン
         80トルエン          
    80シクロへキサノン          4
0上述のようにして得た分散塗料をPETフィルム(厚
み10μm)上に塗布し、次いで、永久磁石3000G
により磁場配向させて乾燥し、磁性塗膜厚みが3μmの
磁気シートを得た。
Paint composition (3f parts) Surface treatment magnetic metal powder 100VAGH (
PVC/vinyl acetate copolymer) 1) Polyurethane resin 1 Lucitin
2 Methyl ethyl ketone 80 Toluene
80cyclohexanone 4
0 The dispersion paint obtained as described above was applied onto a PET film (thickness: 10 μm), and then a permanent magnet of 3000G was applied.
The magnetic sheet was oriented in a magnetic field and dried to obtain a magnetic sheet with a magnetic coating thickness of 3 μm.

得られた磁気シートの磁気特性を第2表に示す。The magnetic properties of the obtained magnetic sheet are shown in Table 2.

(実施例2) 過酸化ベンゾイル30g及びジメチルアニリン5gをト
ルエン31中に溶解して処理液を調製し、以下実施例1
と同様に操作した。
(Example 2) A treatment solution was prepared by dissolving 30 g of benzoyl peroxide and 5 g of dimethylaniline in 31 g of toluene, and the following Example 1
operated in the same way.

この結果を第1表及び第2表に示す。The results are shown in Tables 1 and 2.

(比較例1) 過酸化ベンゾイル及びジメチルアニリンを添加せず、ト
ルエンだけを用いて実施例1と同様の条件で操作した。
(Comparative Example 1) Operation was carried out under the same conditions as in Example 1 using only toluene without adding benzoyl peroxide and dimethylaniline.

この結果を第1表及び第2表に示す。The results are shown in Tables 1 and 2.

(比較例2) ステアリン酸40gをトルエン51中に溶解して処理液
とした他は、実施例1と同様に操作した。この結果を第
1表及び第2表に示す。
(Comparative Example 2) The same procedure as in Example 1 was carried out except that 40 g of stearic acid was dissolved in 51 parts of toluene to prepare a treatment liquid. The results are shown in Tables 1 and 2.

第1表 第2表 第1表より、実施例1,2による表面処理磁性金属粉末
は比較例1,2のものと比べて劣化率が著しく小さくな
っており、耐酸化性が向上しているのが認められた。ま
た磁気特性においても同等以上の値を示した。
Table 1 Table 2 Table 1 shows that the surface-treated magnetic metal powders according to Examples 1 and 2 have significantly lower deterioration rates and improved oxidation resistance than those of Comparative Examples 1 and 2. was recognized. The magnetic properties also showed equivalent or higher values.

また実施例1,2の表面処理磁性金属粉末を用いて作製
した磁気シートにおいては比較例1,2のものに比べて
特に角形比(Sq)が向上されているのが認められる。
Furthermore, it is observed that the magnetic sheets produced using the surface-treated magnetic metal powders of Examples 1 and 2 have particularly improved squareness ratios (Sq) compared to those of Comparative Examples 1 and 2.

すなわち、実施例1,2においては、空試験となる比較
例1に比べて0.05〜0.06、従来法による表面処
理を行った比較例2のものと比べて0.03〜0.04
角形比が改善されているが、これは塗料化の際の分散性
が大きく向上していることを示している。
That is, in Examples 1 and 2, 0.05 to 0.06 compared to Comparative Example 1, which is a blank test, and 0.03 to 0.0. 04
The squareness ratio has been improved, which indicates that the dispersibility during coating has been greatly improved.

〈発明の効果〉 以上、実施例とともに具体的に説明したように、本発明
方法によれば耐酸化性及び分散性が著しく向上した磁性
金属粉末を得ることができる。
<Effects of the Invention> As described above in detail with Examples, according to the method of the present invention, magnetic metal powder with significantly improved oxidation resistance and dispersibility can be obtained.

Claims (3)

【特許請求の範囲】[Claims] (1)鉄又は鉄を主体とする磁性金属粉末を過酸化ベン
ゾイルで表面処理することを特徴とする磁性金属粉末の
表面処理法。
(1) A method for surface treatment of magnetic metal powder, which comprises surface-treating iron or magnetic metal powder mainly composed of iron with benzoyl peroxide.
(2)過酸化ベンゾイルを有機溶媒に溶解又は分散した
処理液に磁性金属粉末を浸漬する特許請求の範囲第1項
記載の磁性金属粉末の表面処理法。
(2) The method for surface treatment of magnetic metal powder according to claim 1, wherein the magnetic metal powder is immersed in a treatment liquid in which benzoyl peroxide is dissolved or dispersed in an organic solvent.
(3)過酸化ベンゾイルを有機溶媒に溶解又は分散した
処理液に分解促進剤として第三級アミンを添加する特許
請求の範囲第2項記載の磁性金属粉末の表面処理法。
(3) A method for surface treatment of magnetic metal powder according to claim 2, wherein a tertiary amine is added as a decomposition accelerator to a treatment liquid in which benzoyl peroxide is dissolved or dispersed in an organic solvent.
JP63110350A 1988-05-09 1988-05-09 Surface treatment of magnetic metal powder Pending JPH01281704A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP63110350A JPH01281704A (en) 1988-05-09 1988-05-09 Surface treatment of magnetic metal powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP63110350A JPH01281704A (en) 1988-05-09 1988-05-09 Surface treatment of magnetic metal powder

Publications (1)

Publication Number Publication Date
JPH01281704A true JPH01281704A (en) 1989-11-13

Family

ID=14533537

Family Applications (1)

Application Number Title Priority Date Filing Date
JP63110350A Pending JPH01281704A (en) 1988-05-09 1988-05-09 Surface treatment of magnetic metal powder

Country Status (1)

Country Link
JP (1) JPH01281704A (en)

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