JPS5850005B2 - Jikikirokuyouji Seifun Matsuno Seizouhou - Google Patents
Jikikirokuyouji Seifun Matsuno SeizouhouInfo
- Publication number
- JPS5850005B2 JPS5850005B2 JP49095883A JP9588374A JPS5850005B2 JP S5850005 B2 JPS5850005 B2 JP S5850005B2 JP 49095883 A JP49095883 A JP 49095883A JP 9588374 A JP9588374 A JP 9588374A JP S5850005 B2 JPS5850005 B2 JP S5850005B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- iron oxide
- magnetic
- solution
- seizouhou
- 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.)
- Expired
Links
Landscapes
- Paints Or Removers (AREA)
- Magnetic Record Carriers (AREA)
- Hard Magnetic Materials (AREA)
- Compounds Of Iron (AREA)
Description
【発明の詳細な説明】 本発明は、磁気記録用磁性粉末の改良に関する。[Detailed description of the invention] The present invention relates to improvements in magnetic powder for magnetic recording.
近年、磁気記録の高性能化の要求にともない記録素子と
してコバルト原子を含む強磁性酸化鉄粉末を用いるもの
が開発されている。In recent years, with the demand for higher performance magnetic recording, recording elements using ferromagnetic iron oxide powder containing cobalt atoms have been developed.
この種の磁性粉末の製造法については、種々の提案がな
され、発明者らも、その一方法として針状のγ−Fe2
03粉末あるいは、Fe3O4粉末を核晶とし、この核
晶上にコバルト原子を含む強磁性酸化鉄被膜をエピタキ
シャルに成長させる方法を提案した。Various proposals have been made regarding the production method of this type of magnetic powder, and the inventors have also proposed a method for producing acicular γ-Fe2.
We proposed a method in which a ferromagnetic iron oxide film containing cobalt atoms is epitaxially grown on the core crystal using 03 powder or Fe3O4 powder.
この方法では、針状形の均一な粒径で、かつ安定した磁
気特性を有するコバルト原子を含む強磁性酸化鉄を容易
に製造することができるが核晶となる強磁性酸化鉄粉末
の性状によっては特性が十分に発揮されないことがある
。With this method, it is possible to easily produce ferromagnetic iron oxide containing cobalt atoms, which has a uniform needle-shaped particle size and stable magnetic properties. characteristics may not be fully demonstrated.
通常市販の強磁性Fe3O4やr−Fe203粉末はゲ
ーサイト粉末を加熱還元するかあるいは加熱還元後加熱
酸化して製造されるが、これらの方法で得られる強磁性
酸化鉄粉末は、良好な針状性と均一な粒度分布を有する
けれども、粒子内に比較的大きな多数の透孔が形成され
易い。Commercially available ferromagnetic Fe3O4 and r-Fe203 powders are usually produced by thermally reducing goethite powder or by thermally oxidizing it after thermal reduction, but the ferromagnetic iron oxide powder obtained by these methods has good acicular shape. Although the particles have a uniform particle size distribution, a large number of relatively large pores are likely to be formed within the particles.
したがって、このような多孔質の強磁性酸化鉄粉末を核
晶とし、この核晶上にコバルト原子を含む強磁性酸化鉄
被膜、特に薄い被膜を形成したとき、前記透孔が粒子内
に残在し易い。Therefore, when such porous ferromagnetic iron oxide powder is used as a nucleus crystal and a ferromagnetic iron oxide coating containing cobalt atoms, particularly a thin coating, is formed on the nucleus crystal, the pores remain in the particles. Easy to do.
この透孔を有する磁性粉末をバインダーとともに混練し
て磁性塗料を調製すると、粉末粒子の分散が困難であり
、実質的な充填度を高くできず所期の特性を得にくいこ
とがある。When a magnetic coating material is prepared by kneading this magnetic powder having perforated pores with a binder, it is difficult to disperse the powder particles, and a substantial degree of filling cannot be achieved, making it difficult to obtain desired characteristics.
本発明は、かかる観点からなされたもので、Fe3O4
、γ−Fe2O3などの強磁性酸化鉄粉末上に最初にエ
ピタキシャル成長し易いマグネタイト(Fe304)層
を形成して、透孔を充塞しあるいは表面を平滑化したの
ちこのマグネタイト層上にコバルト原子を含む強磁性酸
化鉄被膜をエピタキシャル成長させることによって磁性
粉末を得ようとするものである。The present invention was made from this viewpoint, and Fe3O4
A magnetite (Fe304) layer, which is easy to grow epitaxially, is first formed on a ferromagnetic iron oxide powder such as The purpose is to obtain magnetic powder by epitaxially growing a magnetic iron oxide film.
Fe3O4、γ−Fe2O3などの強磁性酸化鉄粉末上
にマグネタイト層を形成するには、前記酸化鉄粉末を塩
化第1鉄、硫酸第1鉄などの第1鉄塩溶液中に分散し、
これにアルカリ溶液を混合し、この混合溶液中で酸化反
応を行なわせることによって容易になし得る。To form a magnetite layer on a ferromagnetic iron oxide powder such as Fe3O4 or γ-Fe2O3, the iron oxide powder is dispersed in a ferrous salt solution such as ferrous chloride or ferrous sulfate;
This can be easily achieved by mixing an alkaline solution with this and allowing the oxidation reaction to occur in this mixed solution.
上記アルカリ溶液のアルカリ濃度は混合溶液で鉄水酸化
物の沈澱を起す程度であればよい。The alkaline concentration of the above-mentioned alkaline solution is sufficient as long as it causes precipitation of iron hydroxide in the mixed solution.
このようにして得られる磁性粉末粒子の表面性は、主と
して、前記酸化鉄粉末に対する第1鉄塩の添加量に左右
され、酸化鉄粉末100tに対し、第1鉄塩な0.05
モル以上添加することによって、好ましいマグネタイト
層が形成される。The surface properties of the magnetic powder particles obtained in this manner mainly depend on the amount of ferrous salt added to the iron oxide powder.
A preferable magnetite layer is formed by adding mol or more.
次に、このマグネタイト層上に、コバルト原子を含む強
磁性酸化鉄層をエピタキシャルに成長させるには、鉄塩
とコバルト塩を含む金属塩溶液と少くともコバルト水酸
化物が沈澱するアルカリ溶液の混合液中に、前記の核晶
粉末を分散し、この溶液中で空気などの酸化性ガスの吹
き込み、あるいはH2O2などの酸化剤の添加によって
、酸化反応を行なわしめることによってなし得る。Next, in order to epitaxially grow a ferromagnetic iron oxide layer containing cobalt atoms on this magnetite layer, a metal salt solution containing an iron salt and a cobalt salt is mixed with an alkaline solution in which at least cobalt hydroxide is precipitated. This can be achieved by dispersing the above-mentioned nuclear crystal powder in a liquid and carrying out an oxidation reaction by blowing an oxidizing gas such as air into the solution or adding an oxidizing agent such as H2O2.
この成長は、アルカリ溶液のアルカリ濃度および酸化温
度に影響され、アルカリ添加量が溶液中の金属イオン1
モルに対し、0.5モル当量比以上とするとき、ゲーサ
イトなどの新たな核晶の発生も抑制され、また酸化温度
が常温より高くなるにつれ、より促進される。This growth is influenced by the alkaline concentration of the alkaline solution and the oxidation temperature, and the amount of alkali added is
When the molar equivalent ratio is 0.5 or more, the generation of new nuclei such as goethite is also suppressed, and as the oxidation temperature becomes higher than room temperature, it is further promoted.
このようにして得られる磁性粉末の保磁力は主として磁
性粉末中のコバルト原子の含有量によって決定され、コ
バルト原子の含有量の増加とともに保磁力は増大する。The coercive force of the magnetic powder thus obtained is mainly determined by the content of cobalt atoms in the magnetic powder, and the coercive force increases as the content of cobalt atoms increases.
次に、本発明による実施例について説明する。Next, embodiments according to the present invention will be described.
実施例
硫酸第1鉄0.3モル11濃度の溶液31に対し、1.
8モル11濃度のNaOH溶液31を添加して鉄の水酸
化物を析出させる。Example For a solution 31 with a concentration of 0.3 mol 11 ferrous sulfate, 1.
An 8 molar 11 concentration NaOH solution 31 is added to precipitate iron hydroxide.
この溶液中に針状γ−Fe203粉末(長軸約0.3μ
、軸比約7、保磁力約300エルステツド、飽和磁束密
度約4350ガウス)を約2251を添加し、60℃3
時間攪拌しながら毎分31の空気を吹き込み酸化反応を
行なわせ、γ−Fe203粉末上にマグネタイト(Fe
304)結晶を析出させる。In this solution, acicular γ-Fe203 powder (long axis approximately 0.3μ
, axial ratio of about 7, coercive force of about 300 oersted, saturation magnetic flux density of about 4350 gauss) was added to about 2251, and heated at 60℃3.
The oxidation reaction was carried out by blowing air at a rate of 31/min while stirring for a period of time, and magnetite (Fe
304) Precipitate crystals.
このようにして得られた強磁性酸化鉄粉末は、保磁力約
350エルステツド、飽和磁束密度約4400ガウスを
有し、粒径がやや増大したものの形状はほとんど変らず
、表面滑性なものが得られる。The ferromagnetic iron oxide powder obtained in this way has a coercive force of about 350 oersted and a saturation magnetic flux density of about 4400 Gauss, and although the particle size has increased slightly, the shape has hardly changed and the surface is smooth. It will be done.
次に、この磁性粉末15ozを硫酸第1鉄0.02モル
、硫酸コバル)Q、01モルを水11に溶解した金属塩
溶液に対し、0.2モル11濃度のNaOH溶液11を
加えて鉄とコバルトの水酸化物を沈澱させた溶液中に添
加し、60℃で3時間攪拌しながら毎分31の空気を吹
き込み酸化反応を行なわせ、γ−Fe203粉末上に鉄
・コバルトの酸化物結晶を成長させる。Next, 15 oz of this magnetic powder was added to a metal salt solution in which 0.02 mol of ferrous sulfate and 1 mol of cobal sulfate (cobal sulfate) were dissolved in water 11, and a NaOH solution 11 with a concentration of 0.2 mol 11 was added to dissolve iron. and cobalt hydroxide were added to the precipitated solution, and an oxidation reaction was carried out by blowing air at a rate of 31/min while stirring at 60°C for 3 hours. grow.
反応後の磁性粉末は十分水洗して反応溶液を除去してか
ら乾燥する。After the reaction, the magnetic powder is thoroughly washed with water to remove the reaction solution, and then dried.
このようにして得られる磁性粉末はその保磁力が約40
0エルステツド飽和磁束密度4300ガウスである。The magnetic powder thus obtained has a coercive force of approximately 40
The saturation magnetic flux density is 4300 Gauss.
比較例
実施例においてマグネタイト層を形成することなく原料
の強磁性酸化鉄粉末粒子上に直接コバルト原子を含む強
磁性酸化鉄層を形成した。Comparative Example In the example, a ferromagnetic iron oxide layer containing cobalt atoms was directly formed on the ferromagnetic iron oxide powder particles of the raw material without forming a magnetite layer.
各実施例および比較例で得られた磁性粉末を使用し、磁
性塗料を調製して、この塗料を基体フィルム上に塗布し
て磁気テープを作り、その角型(Br/Bs)および感
度を測定した。Using the magnetic powder obtained in each example and comparative example, prepare a magnetic paint, apply this paint onto a base film to make a magnetic tape, and measure its square shape (Br/Bs) and sensitivity. did.
ちなみに、磁性塗料は下記の組成物を用いた。Incidentally, the following composition was used for the magnetic paint.
磁性粉末 75重量部塩ビー
酢ビ共重合体 25 〃DOP
5 〃トルエンーメチル
インブチルケ) 200 //ン混合溶剤
次表は、測定結果で、この結果から明らかなように、本
発明の方法で得られた磁性粉末は、従来のものに比べ、
角型および感度とも向上していることが分る。Magnetic powder 75 parts by weight Vinyl chloride vinyl acetate copolymer 25 〃DOP
5 〃Toluene-methylinbutylke) 200//n mixed solvent The following table shows the measurement results.As is clear from the results, the magnetic powder obtained by the method of the present invention has a
It can be seen that both the squareness and sensitivity are improved.
Claims (1)
このマグネタイト層上にコバルト原子を含む強磁性酸化
鉄層を析出させたことを特徴とする磁気記録用磁性粉末
。1 Precipitate a magnetite layer on ferromagnetic iron oxide powder,
A magnetic powder for magnetic recording, characterized in that a ferromagnetic iron oxide layer containing cobalt atoms is deposited on the magnetite layer.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP49095883A JPS5850005B2 (en) | 1974-08-20 | 1974-08-20 | Jikikirokuyouji Seifun Matsuno Seizouhou |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP49095883A JPS5850005B2 (en) | 1974-08-20 | 1974-08-20 | Jikikirokuyouji Seifun Matsuno Seizouhou |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS5123697A JPS5123697A (en) | 1976-02-25 |
JPS5850005B2 true JPS5850005B2 (en) | 1983-11-08 |
Family
ID=14149710
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP49095883A Expired JPS5850005B2 (en) | 1974-08-20 | 1974-08-20 | Jikikirokuyouji Seifun Matsuno Seizouhou |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS5850005B2 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0428808Y2 (en) * | 1985-06-01 | 1992-07-14 |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS59500739A (en) * | 1983-04-12 | 1984-04-26 | メモレックス・コーポレーション | ferromagnetic recording material |
DE3631194A1 (en) * | 1986-09-13 | 1988-03-24 | Bayer Ag | MAGNETIC IRON OXIDE PIGMENTS AND METHOD FOR THE PRODUCTION THEREOF |
DE3631193A1 (en) * | 1986-09-13 | 1988-03-24 | Bayer Ag | MAGNETIC IRON OXIDE PIGMENTS AND METHOD FOR THE PRODUCTION THEREOF |
EP0376033B1 (en) * | 1988-12-24 | 1993-01-20 | Bayer Ag | Process for preparing magnetic iron oxides, and pigments thus obtained |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS50154198A (en) * | 1974-05-06 | 1975-12-11 |
-
1974
- 1974-08-20 JP JP49095883A patent/JPS5850005B2/en not_active Expired
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS50154198A (en) * | 1974-05-06 | 1975-12-11 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0428808Y2 (en) * | 1985-06-01 | 1992-07-14 |
Also Published As
Publication number | Publication date |
---|---|
JPS5123697A (en) | 1976-02-25 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US3702270A (en) | Method of making a magnetic powder | |
US3720618A (en) | Method of producing a powder of cobalt-containing needle-like shaped gamma-ferric oxide particles as magnetic recording material | |
JPS5850005B2 (en) | Jikikirokuyouji Seifun Matsuno Seizouhou | |
US3252758A (en) | Gamma-ferric-oxide crystals and processes for their production | |
US4396596A (en) | Method of preparing gamma ferric hydroxyoxide powder | |
US4010310A (en) | Magnetic powder | |
JP2937211B2 (en) | Method for producing acicular magnetic iron oxide particles | |
JPH0633116A (en) | Ferromagnetic metallic powder for magnetic recording medium and production thereof | |
JP2970706B2 (en) | Method for producing acicular magnetic iron oxide particles | |
JPS6071509A (en) | Needlelike particle containing iron carbide | |
JPS5860624A (en) | Ferromagnetic powder and its preparation | |
JPS5813008B2 (en) | Manufacturing method of magnetic iron powder | |
JPS5941453A (en) | Needle crystal iron alloy magnetic particulate powder for magnetic recording and preparation thereof | |
JP2970705B2 (en) | Method for producing acicular magnetic iron oxide particles | |
JPS59169937A (en) | Production of magnetic powder | |
JPS58159311A (en) | Manufacture of metallic magnetic powder | |
JPS6051242B2 (en) | Method for producing magnetic iron oxide particles for magnetic recording materials | |
JPS6244842B2 (en) | ||
JPS609321B2 (en) | Magnetic recording medium and its manufacturing method | |
JPH03199301A (en) | Magnetic metallic powder and production thereof and magnetic recording medium | |
JPS607105A (en) | Manufacture of magnetic powder | |
JPH038083B2 (en) | ||
JPS60159102A (en) | Manufacture of ferromagnetic iron powder | |
JPH01301525A (en) | Production of alpha-iron hydroxide oxide | |
JPS596502A (en) | Manufacture of improved ferromagnetic iron powder |