JPS62197323A - Production of magnetic powder - Google Patents

Production of magnetic powder

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Publication number
JPS62197323A
JPS62197323A JP61036888A JP3688886A JPS62197323A JP S62197323 A JPS62197323 A JP S62197323A JP 61036888 A JP61036888 A JP 61036888A JP 3688886 A JP3688886 A JP 3688886A JP S62197323 A JPS62197323 A JP S62197323A
Authority
JP
Japan
Prior art keywords
iron oxide
magnetic powder
powder
cobalt
oxide 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
Application number
JP61036888A
Other languages
Japanese (ja)
Inventor
Yoshiharu Katsuta
勝田 善春
Susumu Kitaoka
北岡 進
Haruo Ando
安藤 晴夫
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.)
Maxell Ltd
Original Assignee
Hitachi Maxell 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 Hitachi Maxell Ltd filed Critical Hitachi Maxell Ltd
Priority to JP61036888A priority Critical patent/JPS62197323A/en
Publication of JPS62197323A publication Critical patent/JPS62197323A/en
Pending legal-status Critical Current

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  • Compounds Of Iron (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

PURPOSE:To obtain magnetic powder capable of preparing a magnetic recording medium wherein erasing characteristics are fully enhanced by allowing iron oxide magnetic powder to react in an aq. soln. contg. cobalt salt, ferrous salt and alkali and crushing the reacted powder in a uniform particle size and thereafter heating it. CONSTITUTION:Iron oxide magnetic powder is allowed to reat in an aq. soln. contg. cobalt salt, ferrous salt and alkali, and the iron oxide layers contg. Co on the surface of the particles of iron oxide magnetic powder are formed. Then these are washed with water, filtered and dried and the obtained powder is crushed to uniformize the particle size and thereafter heat-treated. In such a way, when heat-treating the obtained powder after uniformizing the particle size, heat is uniformly conducted to all parts of powder and the iron oxide layers contg. Co uniformly are favorably formed. Therefore the iron oxide magnetic powder contg. Co which is extremely good in the distribution of coercive force and excellent in erasing characteristics is obtained.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 この発明は磁気記録媒体の記録素子として好適なコバル
ト含有酸化鉄磁性粉末の製造方法に関する。
DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing cobalt-containing iron oxide magnetic powder suitable as a recording element of a magnetic recording medium.

〔従来の技術〕[Conventional technology]

コバルトを含有する酸化鉄磁性粉末は、従来の磁気記録
媒体の記録素子として汎用されている酸化鉄磁性粉末に
比べ高保磁力を有するため、高性能磁気記録媒体の記録
素子として有用である。
Iron oxide magnetic powder containing cobalt has a higher coercive force than iron oxide magnetic powder commonly used as a recording element in conventional magnetic recording media, and is therefore useful as a recording element in high-performance magnetic recording media.

このようなコバルト含有酸化鉄磁性粉末の製造方法はこ
れまで種々提案されており、その代表的な方法の1つと
して、酸化鉄磁性粉末をコバルト塩および第一鉄塩を含
む水溶液中に分散させ、これにアルカリ水溶液を加えて
酸化鉄磁性粉末の粒子表面にコバルトを含む酸化鉄層を
形成させるものがある。(特開昭55−56019号)
〔発明が解決しようとする問題点〕 ところが、この従来の方法で得られるコバルト含有酸化
鉄磁性粉末は、転写特性に優れるものの消去特性が未だ
充分に良好でなく、特に、記録密度を向上させ、ノイズ
を低減するため、この種のコバルト含有酸化鉄磁性粉末
を微粒子化し、保磁力を向上させようとすると、消去特
性が劣化するという難点がある。
Various methods for producing such cobalt-containing iron oxide magnetic powder have been proposed, and one typical method involves dispersing iron oxide magnetic powder in an aqueous solution containing a cobalt salt and a ferrous salt. There is a method in which an aqueous alkaline solution is added to this to form an iron oxide layer containing cobalt on the surface of the iron oxide magnetic powder particles. (Unexamined Japanese Patent Publication No. 55-56019)
[Problems to be Solved by the Invention] However, although the cobalt-containing iron oxide magnetic powder obtained by this conventional method has excellent transfer characteristics, its erasing characteristics are still not sufficiently good. In order to reduce noise, if this type of cobalt-containing iron oxide magnetic powder is made into fine particles and an attempt is made to improve the coercive force, there is a problem in that the erasing characteristics deteriorate.

〔問題点を解決するための手段〕[Means for solving problems]

この発明は、かかる現状に鑑み鋭意研究を重ねた結果な
されたもので、酸化鉄磁性粉末を、コバルト塩および第
一鉄塩とアルカリとを含む水溶液中で反応させて酸化鉄
磁性粉末の粒子表面にコバルトを含む酸化鉄層を形成し
、次いで、これを水洗、濾過、乾燥した後、得られた粉
末を粉砕してその粒度を均一にし、しかる後、加熱処理
することによって、コバルト含有酸化鉄磁性粉末の消去
特性を改善し、このコバルト含有酸化鉄磁性粉末を使用
して得られる磁気記録媒体の消去特性を充分に向上させ
たものである。
This invention was made as a result of extensive research in view of the current situation, and was made by reacting iron oxide magnetic powder in an aqueous solution containing cobalt salts, ferrous salts, and alkali to improve the particle surface of the iron oxide magnetic powder. A cobalt-containing iron oxide layer is formed on the surface, which is then washed with water, filtered, and dried.The resulting powder is pulverized to make the particle size uniform, and then heat-treated to form a cobalt-containing iron oxide layer. The erasing properties of the magnetic powder are improved, and the erasing properties of the magnetic recording medium obtained using this cobalt-containing iron oxide magnetic powder are sufficiently improved.

この発明において、出発原料として用いる酸化鉄磁性粉
末は、たとえば、針状の7−Fe2O3粉末、Fe3O
4粉末およびr−Fe203を水素気流中で部分還元す
ることによって得られるγ−Fe2O3とFe3O4と
の中間の酸化状態の酸化鉄磁性粉末などが好適なものと
して使用される。
In this invention, the iron oxide magnetic powder used as a starting material is, for example, acicular 7-Fe2O3 powder, Fe3O
Iron oxide magnetic powder having an oxidation state intermediate between γ-Fe2O3 and Fe3O4, which is obtained by partially reducing r-Fe203 and r-Fe203 powder in a hydrogen stream, is preferably used.

これらの酸化鉄磁性粉末は、コバルト塩および第一鉄塩
とアルカリとを含む水溶液中で反応させて酸化鉄磁性粉
末の粒子表面にコバルトを含む酸化鉄層を形成し、次い
で、これを水洗、濾過、乾燥した後、得られた粉末を粉
砕してその粒度を均一にし、しかる後、加熱処理するの
が好ましく、このように粒度を均一にした後、加熱処理
すると熱が粉末全体に均一に伝わって、コバルトを均一
に含む酸化鉄層が良好に形成され、保磁力分布が非常に
良好で消去特性に優れたコバルト含有酸化鉄磁性粉末が
得られ、このコバルト含有酸化鉄磁性粉末を使用して得
られる磁気記録媒体の消去特性が充分に向上される。
These iron oxide magnetic powders are reacted in an aqueous solution containing a cobalt salt, a ferrous salt, and an alkali to form an iron oxide layer containing cobalt on the particle surface of the iron oxide magnetic powder, which is then washed with water, After filtration and drying, it is preferable to crush the resulting powder to make the particle size uniform, and then heat treat it. As a result, a cobalt-containing iron oxide magnetic powder with an excellent formation of an iron oxide layer containing cobalt uniformly, a very good coercive force distribution, and excellent erasing properties was obtained. The erasing characteristics of the magnetic recording medium obtained by this method are sufficiently improved.

このような粒子表面にコバルトを含む酸化鉄層を形成し
た酸化鉄磁性粉末の破砕は、乳鉢等を使用して行われ、
粒度は、次の加熱処理工程での熱の伝達が可及的に均一
に行われるように、10〜500メツシユの篩を通過で
きる程度に微細にし、かつ均一にするのが好ましい。
Such iron oxide magnetic powder, which has an iron oxide layer containing cobalt formed on the particle surface, is crushed using a mortar or the like.
The particle size is preferably fine enough to pass through a 10 to 500 mesh sieve and uniform so that heat transfer in the next heat treatment step is as uniform as possible.

また、コバルトを含む酸化鉄層を形成した酸化鉄磁性粉
末粒度を均一にした後の加熱処理は、180℃より高く
てはコバルトが固溶するため180℃以下の温度で行う
のが好ましい。なお、この加熱処理は非酸化性雰囲気中
で行うと、本発明の効果がいっそう顕著となる。
Further, the heat treatment after uniformizing the grain size of the iron oxide magnetic powder forming the cobalt-containing iron oxide layer is preferably carried out at a temperature of 180° C. or lower, since cobalt dissolves in solid solution at temperatures higher than 180° C. Note that the effect of the present invention becomes even more remarkable when this heat treatment is performed in a non-oxidizing atmosphere.

コバルト塩としては塩化コバルト、硫酸コバルトなどが
好適なものとして使用され、第一鉄塩としては塩化第一
鉄、硫酸第一鉄などが好ましく使用される。
Cobalt salts such as cobalt chloride and cobalt sulfate are preferably used, and ferrous salts such as ferrous chloride and ferrous sulfate are preferably used.

またアルカリとしては、通常、苛性ソーダが用いられ、
その好適な配合量は、コバルト塩と第一鉄塩との総量に
対して当量以上とするのが好ましい。
Caustic soda is usually used as the alkali.
The suitable amount of the cobalt salt and the ferrous salt is preferably equal to or more than the total amount of the cobalt salt and the ferrous salt.

〔作用〕[Effect]

以上のように、酸化鉄磁性粉末を、コバルト塩および第
一鉄塩とアルカリとを含む水溶液中で反応させて酸化鉄
磁性粉末の粒子表面にコバルトを含む酸化鉄層を形成し
、次いで、これを水洗、濾過、乾燥した後、得られた粉
末を粉砕してその粒度を均一にし、しかる後、加熱処理
すると、−粒子一粒子に熱が均一に作用するため、保磁
力分布が良好で消去特性に優れたコバルト含有酸化鉄磁
性粉末が得られ、この磁性粉末を使用して得られる磁気
記録媒体の消去特性が充分に向上される。
As described above, iron oxide magnetic powder is reacted in an aqueous solution containing a cobalt salt, a ferrous salt, and an alkali to form an iron oxide layer containing cobalt on the particle surface of the iron oxide magnetic powder. After washing with water, filtering, and drying, the obtained powder is crushed to make the particle size uniform, and then heat-treated.- Heat acts uniformly on each particle, so the coercive force distribution is good and erased. A cobalt-containing iron oxide magnetic powder with excellent properties is obtained, and the erasing properties of a magnetic recording medium obtained using this magnetic powder are sufficiently improved.

〔実施例〕〔Example〕

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 長軸径0,3μm、軸比8、BET法による比表面積3
2.Ord/g 、保磁力350エルステツド、飽和磁
化量75.1 emu 7gの針状r−Fe203粉末
100ffi量部を、水500重量部に分散させ、これ
に硫酸コバルト(Co SO4・7 H20)  14
重量部と硫酸第1鉄(F e SO4・7 H20)4
2重量部とを水200重量部に溶解した溶液を添加した
。次いで、水酸化ナトリウム100重量部を水300重
量部に溶解させた溶液を添加し、60℃の温度で3時間
攪拌して反応させた。次いで、これを水洗、濾過し、空
気中にて80℃の温度で10時間乾燥した。このように
して得られた磁性粉末の保磁力は670エルステツドで
飽和磁化量は??、8 emu 7gであった。次ぎに
、このようにして得られた磁性粉末を乳鉢で粉砕し、1
000μm目の篩(J I S 16メツシユ)にかけ
て、この篩を通過した試料を分級し、これを窒素ガス中
120℃の温度で2時間加熱処理し、室温まで徐冷して
コバルトを含む酸化鉄層を粒子表面に形成させた磁性粉
末を得た。このようにして得られたコバルト含有酸化鉄
磁性粉末は、保磁力が690エルステツドで飽和磁化量
は?7.8emu / gであった。またコバルト含有
量は2.6N量%であった。
Example 1 Major axis diameter 0.3 μm, axial ratio 8, specific surface area 3 by BET method
2. Ord/g, coercive force 350 oersted, saturation magnetization amount 75.1 emu 100 parts of acicular r-Fe203 powder of 7 g was dispersed in 500 parts by weight of water, and cobalt sulfate (Co SO4.7 H20) 14
Parts by weight and ferrous sulfate (F e SO4.7 H20) 4
A solution prepared by dissolving 2 parts by weight of 2 parts by weight in 200 parts by weight of water was added. Next, a solution prepared by dissolving 100 parts by weight of sodium hydroxide in 300 parts by weight of water was added, and the mixture was stirred at a temperature of 60° C. for 3 hours to react. Next, this was washed with water, filtered, and dried in air at a temperature of 80° C. for 10 hours. The magnetic powder thus obtained has a coercive force of 670 oersted and what is its saturation magnetization? ? , 8 emu 7g. Next, the magnetic powder obtained in this way was ground in a mortar, and 1
The sample that passed through this sieve was classified by passing it through a 000 μm sieve (JIS 16 mesh), heat treated in nitrogen gas at a temperature of 120°C for 2 hours, and slowly cooled to room temperature to extract iron oxide containing cobalt. Magnetic powder with a layer formed on the particle surface was obtained. The cobalt-containing iron oxide magnetic powder thus obtained has a coercive force of 690 Oersteds and a saturation magnetization amount? It was 7.8 emu/g. Further, the cobalt content was 2.6N%.

実施例2 実施例1において、乳鉢で粉砕後、105μm目(JI
S145メソシュ)の篩を通過し、44μm目(JIS
350メツシュ)を通過しないものに分級し、この試料
を使用した以外は実施例1と同様にしてコバルトを含む
酸化鉄層を粒子表面に形成させた磁性粉末を得た。この
ようにして得られたコバルト含有酸化鉄磁性粉末は、保
磁力が685エルステツドで飽和磁化量は7B、1em
u / gであった。またコバルト含有量は2.6重量
%であった。
Example 2 In Example 1, after grinding in a mortar, the 105 μm
S145 mesh) passed through a sieve of 44 μm (JIS
A magnetic powder having an iron oxide layer containing cobalt formed on the particle surface was obtained in the same manner as in Example 1 except that this sample was used. The cobalt-containing iron oxide magnetic powder thus obtained has a coercive force of 685 oersteds, a saturation magnetization of 7 B, and 1 em.
It was u/g. Further, the cobalt content was 2.6% by weight.

比較例1 実施例1において、乳鉢で粉砕後、分級操作を省いた以
外は実施例1と同様にしてコバルトを含む酸化鉄層を粒
子表面に形成させた磁性粉末を得た。このようにして得
られたコバルト含有酸化鉄磁性粉末には、5000μm
程度の粗粒が多く含まれていた。またこのようにして得
られたコバルト含有酸化鉄磁性粉末は、保磁力が692
エルステツドで飽和磁化量は78.2emu / gで
あった。またコバルト含有量は2.6重量%であった。
Comparative Example 1 Magnetic powder in which an iron oxide layer containing cobalt was formed on the particle surface was obtained in the same manner as in Example 1, except that the classification operation after pulverization in a mortar was omitted. The cobalt-containing iron oxide magnetic powder thus obtained has a diameter of 5000 μm.
It contained many coarse grains. The cobalt-containing iron oxide magnetic powder thus obtained has a coercive force of 692.
The saturation magnetization amount in Oersted was 78.2 emu/g. Further, the cobalt content was 2.6% by weight.

次に、上記実施例1.2および比較例1で得られたコバ
ルト含有酸化鉄磁性粉末を用いて、下記の配合組成によ
り磁性塗料を調製し、この塗料を12μm厚のポリエス
テルベースフィルム上に乾燥厚が5μmとなるように塗
布、乾燥して磁気テープをつくった。
Next, using the cobalt-containing iron oxide magnetic powder obtained in Example 1.2 and Comparative Example 1 above, a magnetic paint was prepared according to the formulation shown below, and this paint was dried on a 12 μm thick polyester base film. A magnetic tape was prepared by coating and drying to a thickness of 5 μm.

コバルト含有酸化鉄磁性粉末  100重量部VAGH
(tl、c、c社製、塩化ビ  13〃ニル−酢酸ビニ
ル−ビニルア ルコール共重合体) T5201(大日本インキ化学  10〃工業社製、ウ
レタンプレポリ マー) コロネートしく日本ポリウレ    2 〃タン工業社
製、三官能性細分 重量イソシアネート化合物) ラウリン酸            2 〃メチルイソ
ブチルケトン     75〃トルエン       
     75〃このようにして得られた各磁気テープ
について、保磁力および消去特性を調べた。消去特性は
、IKHzでの元信号レベルと、消去後信号レベルとの
差を測定して示した。なお、消去電流はハイポジション
カセットチーブの規定消去電流値を用いた。
Cobalt-containing iron oxide magnetic powder 100 parts by weight VAGH
(manufactured by TL, C, C, vinyl chloride-vinyl acetate-vinyl alcohol copolymer) T5201 (manufactured by Dainippon Ink Chemical Co., Ltd. 10, urethane prepolymer) Coronate Nippon Polyurethane 2, manufactured by Tan Kogyo Co., Ltd. , trifunctional subdivided weight isocyanate compound) Lauric acid 2 Methyl isobutyl ketone 75 Toluene
75. The coercive force and erasing characteristics of each of the magnetic tapes thus obtained were examined. The erasing characteristics were shown by measuring the difference between the original signal level at IKHz and the signal level after erasing. Note that the specified erase current value of the high position cassette chip was used as the erase current.

下表はその結果である。The table below shows the results.

C発明の効果〕 上表から明らかなように、この発明で得られたコバルト
含有酸化鉄磁性粉末を使用して得られた磁気テープ(実
施例1および2)は、従来の方法で得られたコバルト含
有酸化鉄磁性粉末を使用して得られた磁気テープ(比較
例1)に比し、消去特性がよく、このことから、この発
明の方法で得られるコバルト含有酸化鉄磁性粉末を使用
して得られる磁気記録媒体は消去特性に優れていること
がわかる。
C Effects of the Invention] As is clear from the above table, the magnetic tapes obtained using the cobalt-containing iron oxide magnetic powder obtained by the present invention (Examples 1 and 2) were as good as those obtained by the conventional method. Compared to the magnetic tape obtained using the cobalt-containing iron oxide magnetic powder (Comparative Example 1), the erasing properties are better, and from this, the cobalt-containing iron oxide magnetic powder obtained by the method of the present invention is used. It can be seen that the obtained magnetic recording medium has excellent erasing characteristics.

Claims (1)

【特許請求の範囲】[Claims] 1、酸化鉄磁性粉末を、コバルト塩および第一鉄塩とア
ルカリとを含む水溶液中で反応させて酸化鉄磁性粉末の
粒子表面にコバルトを含む酸化鉄層を形成し、次いで、
これを水洗、濾過、乾燥した後、得られた粉末を粉砕し
てその粒度を均一にし、しかる後、加熱処理することを
特徴とする磁性粉末の製造方法
1. The iron oxide magnetic powder is reacted in an aqueous solution containing a cobalt salt, a ferrous salt, and an alkali to form an iron oxide layer containing cobalt on the particle surface of the iron oxide magnetic powder, and then,
A method for producing magnetic powder, which comprises washing the powder with water, filtering it, drying it, pulverizing the obtained powder to make the particle size uniform, and then subjecting it to heat treatment.
JP61036888A 1986-02-20 1986-02-20 Production of magnetic powder Pending JPS62197323A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP61036888A JPS62197323A (en) 1986-02-20 1986-02-20 Production of magnetic powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP61036888A JPS62197323A (en) 1986-02-20 1986-02-20 Production of magnetic powder

Publications (1)

Publication Number Publication Date
JPS62197323A true JPS62197323A (en) 1987-09-01

Family

ID=12482315

Family Applications (1)

Application Number Title Priority Date Filing Date
JP61036888A Pending JPS62197323A (en) 1986-02-20 1986-02-20 Production of magnetic powder

Country Status (1)

Country Link
JP (1) JPS62197323A (en)

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