JPH01100027A - Production of plate barium ferrite magnetic powder for magnetic recording - Google Patents
Production of plate barium ferrite magnetic powder for magnetic recordingInfo
- Publication number
- JPH01100027A JPH01100027A JP62256202A JP25620287A JPH01100027A JP H01100027 A JPH01100027 A JP H01100027A JP 62256202 A JP62256202 A JP 62256202A JP 25620287 A JP25620287 A JP 25620287A JP H01100027 A JPH01100027 A JP H01100027A
- Authority
- JP
- Japan
- Prior art keywords
- barium ferrite
- particles
- magnetic powder
- fine particles
- composition
- 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
- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000006247 magnetic powder Substances 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000000203 mixture Substances 0.000 claims abstract description 27
- 239000010419 fine particle Substances 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 23
- 230000004907 flux Effects 0.000 claims abstract description 11
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 4
- 229910052718 tin Inorganic materials 0.000 claims abstract description 3
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract description 10
- 238000009826 distribution Methods 0.000 abstract description 10
- 229910052725 zinc Inorganic materials 0.000 abstract description 9
- 229910052759 nickel Inorganic materials 0.000 abstract description 8
- 150000001412 amines Chemical class 0.000 abstract description 5
- 239000011780 sodium chloride Substances 0.000 abstract description 5
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052719 titanium Inorganic materials 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 239000011701 zinc Substances 0.000 description 14
- 239000002244 precipitate Substances 0.000 description 13
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 230000005415 magnetization Effects 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 6
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical group CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 3
- 229910001863 barium hydroxide Inorganic materials 0.000 description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 3
- 238000010335 hydrothermal treatment Methods 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 3
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 2
- 229910001626 barium chloride Inorganic materials 0.000 description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- -1 oxides Chemical class 0.000 description 2
- 150000003141 primary amines Chemical class 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 150000003512 tertiary amines Chemical class 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 229910001631 strontium chloride Inorganic materials 0.000 description 1
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Hard Magnetic Materials (AREA)
- Compounds Of Iron (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、六方晶マグネトブランバイト型バリウムフェ
ライト磁性粉の製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for producing hexagonal magnetoblanbite type barium ferrite magnetic powder.
さらに詳しくは、本発明は高密度記録用の磁気記録媒体
に用いるのに適した、比表面積が２０〜７０ ｒｄ／ｇ
、保磁力が２００〜１５０００ｅであり、飽和磁化が従
来のものと比較して飛曜的に向上しており、さらに保磁
力の温度変化が小さく、異方性磁界分布がシャープなマ
グネトブランバイト型バリウムフェライト磁性粉の製造
方法に関するものである。More specifically, the present invention is suitable for use in magnetic recording media for high-density recording, and has a specific surface area of 20 to 70 rd/g.
, a magnetoblanbite type with a coercive force of 200 to 15,000e, significantly improved saturation magnetization compared to conventional ones, small temperature change in coercive force, and sharp anisotropic magnetic field distribution. The present invention relates to a method for producing barium ferrite magnetic powder.
近年、磁気記録の高密度化の要求に伴い、バリウムフェ
ライト磁性粉を磁気記録媒体として用いる垂直磁気記録
方式の開発が進められている。In recent years, with the demand for higher density magnetic recording, development of perpendicular magnetic recording systems using barium ferrite magnetic powder as a magnetic recording medium has been progressing.
垂直磁気記録方式に用いられるバリウムフェライト磁性
粉としては、保磁力が適当な値（２００〜１５０００ｅ
）で、飽和磁化ができるだけ高く、保磁力の温度変化が
小さく、しかも異方性磁界分布がシャープなものが望ま
れている。The barium ferrite magnetic powder used in the perpendicular magnetic recording system has a coercive force of an appropriate value (200 to 15,000e).
), it is desired that the saturation magnetization is as high as possible, the temperature change in coercive force is small, and the anisotropic magnetic field distribution is sharp.
（従来の技術およびその問題点）
従来、バリウムフェライト磁性粉の製造方法としては、
例えば共沈法、ガラス結晶化法、水熱合成法等種々の方
法が知られており、ガラス結晶化法については、特公昭
６０−１５５７４号公報、水熱合成法については、例え
ば特開昭５９−１７５７０７号公報、特公昭６０−１２
９７３号公報、特公昭６０−１５５７６号公報、特開昭
６０−１３７００２号公報等で提案されている。(Conventional technology and its problems) Conventionally, as a method for producing barium ferrite magnetic powder,
For example, various methods such as coprecipitation method, glass crystallization method, and hydrothermal synthesis method are known. Publication No. 59-175707, Special Publication No. 1986-12
This method has been proposed in Japanese Patent Publication No. 973, Japanese Patent Publication No. 15576/1982, Japanese Patent Application Laid-open No. 137002/1982, and the like.
しかしながら、前記いずれの方法においても得られるバ
リウムフェライト磁性粉は、比表面積が４０ ｒｒｆ／
ｇ以上の微粒子になると５５ｅｓｕ／ｇ以下に低下して
しまい、また保磁力の温度変化が大きいという欠点があ
った。However, the barium ferrite magnetic powder obtained by any of the above methods has a specific surface area of 40 rrf/
When the particle size is larger than 1 g, the coercive force decreases to 55 esu/g or less, and there is a drawback that the coercive force changes greatly with temperature.
一方、特開昭６１−２３６１０４号公報、特開昭６２−
１６２３２号公報等には、Ｚｎを添加することにより飽
和磁化が向上することが開示されている。しかし、Ｚｎ
を添加して得られるバリウムフェライト磁性粉は異方性
磁界分布が広くなってしまうという問題があった。また
、Ｚｎを含有するバリウムフェライト磁性粉は一般に板
状比の高いものは得やすいが、板状比が７以下で、粒度
分布を揃えることが困難であった。また、板状比が高い
ものは、詰め率及び分散性（光沢度）の向上に過度の労
力が必要であった。On the other hand, JP-A-61-236104, JP-A-62-
Publication No. 16232 and the like disclose that saturation magnetization is improved by adding Zn. However, Zn
The barium ferrite magnetic powder obtained by adding the above has a problem in that the anisotropic magnetic field distribution becomes wide. Further, barium ferrite magnetic powder containing Zn is generally easy to obtain with a high plate-like ratio, but when the plate-like ratio is 7 or less, it is difficult to make the particle size distribution uniform. Moreover, those with a high plate-like ratio required excessive effort to improve the filling rate and dispersibility (gloss).
（発明の目的）
本発明の目的は、前記問題点を解決し、微粒子で板状比
が７以下で粒度分布が狭（、比表面積が２０〜７０ ｒ
ｒｆ／ｇ、保磁力が２００〜１５０００ｅであり、飽和
磁化が従来のものと比較して飛躍的に向上しており、さ
らに保磁力の温度変化が小さく、異方性磁界分布がシャ
ープであり、高密度記録用の磁気記録媒体に用いるのに
適したバリウムフェライト磁性粉の製造方法を提供する
ことにある。(Objective of the Invention) The object of the present invention is to solve the above-mentioned problems, and to obtain fine particles with a platelet ratio of 7 or less, a narrow particle size distribution (and a specific surface area of 20 to 70 r
rf/g, coercive force is 200-15000e, saturation magnetization is dramatically improved compared to conventional ones, furthermore, temperature change in coercive force is small, anisotropic magnetic field distribution is sharp, An object of the present invention is to provide a method for producing barium ferrite magnetic powder suitable for use in magnetic recording media for high-density recording.
（問題点を解決するための手段）
本発明は一般式
％式％）
（ただし、ＡはＴｉ、 Ｚｒ及びＳｎから選ばれた一種
以上の金属原子を示し、ｎ ＝ ０．９〜１．２．０．
５ ＜ ｘく２．０．５ ＜ ｙ ＜ ２、ｚ＋ｗ＜ｌ
、ｗ ＜ ０．５である。）で表される六方晶マグネト
ブランバイト型バリウムフェライト磁性粉を製造するに
際し、出発原料として、前記−最大の組成に比較してＮ
ｉ、Ｚｎ及びＣｏから選ばれる一種以上の２価元素の割
合が少ないか又は該２価元素を含有しない板状バリウム
フェライト微粒子を用い、
（１）該微粒子の組成を前記−最大の組成に合わす量の
２価元素を含む水溶液に該微粒子を懸濁させ、アミン類
を添加して該２価元素を粒子表面に付着させた後、濾別
、乾燥し、５００〜９５０℃で加熱するか、あるいは
（２）該微粒子の組成を前記−最大の組成に合わす量の
２価元素の化合物と該微粒子および融剤を十分混合し、
７００〜９５０℃で加熱した後、洗浄、濾別、乾燥する
ことにより、前記−最大の組成のバリウムフェライト磁
性粉を得ることを特徴とする磁気記録用板状バリウムフ
ェライト磁性粉の製造方法に関するものである。(Means for Solving the Problems) The present invention is based on the general formula % (where A represents one or more metal atoms selected from Ti, Zr, and Sn, and n = 0.9 to 1.2 .0.
5 < x × 2.0.5 < y < 2, z + w < l
, w < 0.5. ) When producing a hexagonal magnetobrambite barium ferrite magnetic powder represented by
Using plate-shaped barium ferrite fine particles that have a small proportion of one or more divalent elements selected from i, Zn, and Co or do not contain the divalent element, (1) Adjust the composition of the fine particles to the maximum composition mentioned above. The fine particles are suspended in an aqueous solution containing an amount of divalent elements, amines are added to attach the divalent elements to the particle surface, and then filtered, dried, and heated at 500 to 950 ° C. or (2) sufficiently mixing the fine particles and a flux with a compound of a divalent element in an amount that matches the composition of the fine particles to the maximum composition;
A method for producing plate-shaped barium ferrite magnetic powder for magnetic recording, characterized in that barium ferrite magnetic powder having the maximum composition is obtained by heating at 700 to 950°C, followed by washing, filtering, and drying. It is.
本発明において、前記−最大のＡはＴｉ５Ｚｒ及びＳｎ
から選ばれた一種以上の金属原子であり、ｎ＝０．９〜
１．２．０．５ ＜ ｘ ＜ ２．０．５ ＜ ｙ ＜
２．２＋ｗ＜ｌ、ｗ ＜ ０．５である＠ ＸＳ）’
、ＺおよびＷが前記範囲を外れると、板状比が高くなっ
たり、粒度分布が広くなる。さらに飽和磁化が高く、保
磁力の温度変化が小さ（、異方性磁界分布がシャープな
ものを得ることが困難となる。In the present invention, the maximum A is Ti5Zr and Sn
One or more metal atoms selected from n=0.9~
1.2.0.5 < x < 2.0.5 < y <
2.2+w<l, w<0.5@XS)'
, Z and W are out of the above ranges, the plate ratio becomes high or the particle size distribution becomes wide. Furthermore, the saturation magnetization is high, and the temperature change in coercive force is small (which makes it difficult to obtain a material with a sharp anisotropic magnetic field distribution).
本発明の出発原料である、前記−最大の組成に比較して
Ｎｌ５Ｚｎ及びＣｏから選ばれる一種以上の２価元素の
割合が少ないか又は該２価元素を含有しない板状バリウ
ムフェライト微粒子としては、特に制限はなく、水熱合
成法により水溶液中から生成したもの、およびこれを加
熱焼成したもの、あるいは共沈法、ガラス結晶化法によ
り得られたもののいずれをも用いることができる。含有
するＮｉ、Ｚｎ及びＣｏから選ばれる２価元素の量は合
計でバリウムフェライト１分子当たり、１．０原子以下
が好ましく、特にＺｎは０．４原子以下が望ましい。こ
れらの２価元素、特にＺｎが多く存在すると出発原料の
バリウムフェライト粒子が大きくなり、粒度分布も広（
なってしまうので好ましくない。The plate-shaped barium ferrite fine particles, which are the starting materials of the present invention, have a smaller proportion of one or more divalent elements selected from Nl5Zn and Co than the maximum composition or do not contain the divalent elements, as follows: There are no particular limitations, and any of those produced from an aqueous solution by a hydrothermal synthesis method, those obtained by heating and baking this, or those obtained by a coprecipitation method or a glass crystallization method can be used. The total amount of divalent elements selected from Ni, Zn, and Co contained is preferably 1.0 atoms or less per molecule of barium ferrite, and particularly preferably 0.4 atoms or less of Zn. When these divalent elements, especially Zn, are present in large amounts, the barium ferrite particles used as the starting material become large and the particle size distribution becomes wide (
This is not desirable because it becomes
本発明においては、出発原料である、前記−最大の組成
に比較してＮｉ、 Ｚｎ及びＣｏから選ばれる一種以上
の２価元素の割合が少ないか又は該２価元素を含有しな
い板状バリウムフェライト微粒子を用いて以下の（１）
及び（２）の方法により前記−最大のバリウムフェライ
ト磁性粉を製造する。In the present invention, the starting material is plate-shaped barium ferrite that has a smaller proportion of one or more divalent elements selected from Ni, Zn, and Co, or does not contain the divalent element, compared to the above-mentioned maximum composition. The following (1) using fine particles
and (2) to produce the largest barium ferrite magnetic powder.
（１）該微粒子の組成を前記−最大の組成に合わす量の
２価元素を含む水溶液に該微粒子を懸濁させ、アミン類
を添加して該２価元素を粒子表面に付着させた後、濾別
、乾燥し、５００〜９５０℃で加熱する。(1) After suspending the fine particles in an aqueous solution containing an amount of divalent elements that matches the composition of the fine particles to the above-mentioned maximum composition, and adding amines to attach the divalent elements to the particle surfaces, Separate by filtration, dry and heat at 500-950°C.
Ｎｉ、 Ｚｎ及びＣｏの化合物としては、それらの塩化
物、硝酸塩等が用いられる。As the compounds of Ni, Zn and Co, their chlorides, nitrates, etc. are used.
アミン類としては、メチルアミン、エチルアミン、ブチ
ルアミンなどの低級アルキル基を有する第一アミン、シ
クロヘキシルアミンなどの第一アミン、ジメチルアミン
、ジエチルアミンなどの低級アルキル基を有する第三ア
ミン、トリエチルアミンなどの低級アルキル基を有する
第三アミンを挙げることができる。これらのアミン類は
単独に使用してもよく、また水、アルコール類に溶解さ
せて使用してもよい。Examples of amines include primary amines having a lower alkyl group such as methylamine, ethylamine, and butylamine, primary amines such as cyclohexylamine, tertiary amines having a lower alkyl group such as dimethylamine and diethylamine, and lower alkyl groups such as triethylamine. Mention may be made of tertiary amines having groups. These amines may be used alone or dissolved in water or alcohol.
加熱温度は５００〜９５０℃、好ましくは７゜０〜９３
０°Ｃである。温度が低すぎるとＮｉ、 Ｚｎ及びＣｏ
の結晶格子への組み入れが十分に進まず、飽和磁化が低
くなる。また温度が高すぎると粒子が大きくなったり、
焼結が起こるので好ましくない。Heating temperature is 500~950℃, preferably 7℃~93℃
It is 0°C. If the temperature is too low, Ni, Zn and Co
Incorporation into the crystal lattice does not proceed sufficiently, resulting in low saturation magnetization. Also, if the temperature is too high, the particles will become larger,
This is not preferred because sintering occurs.
加熱時間は１０分〜３０時間程度が適当である。Appropriate heating time is about 10 minutes to 30 hours.
加熱雰囲気は特に制限されないが、一般に空気雰囲気が
便利である。また、加熱において、塩化ナトリウム、塩
化バリウムなどの融剤を加えてもよい。The heating atmosphere is not particularly limited, but an air atmosphere is generally convenient. Further, during heating, a fluxing agent such as sodium chloride or barium chloride may be added.
（２）該微粒子の組成を前記−最大の組成に合わす量の
２価元素の化合物と該微粒子および融剤を十分混合し、
７００〜９５０ ’Ｃで加熱した後、洗浄、濾別、乾燥
する。(2) sufficiently mixing the fine particles and a flux with a divalent element compound in an amount that matches the composition of the fine particles to the maximum composition;
After heating at 700-950'C, it is washed, filtered and dried.
Ｎｉ、 Ｚｎ及びＣｏの化合物としては、それらの塩化
物、酸化物、水酸化物、硝酸塩等が用いられる。As the compounds of Ni, Zn and Co, their chlorides, oxides, hydroxides, nitrates, etc. are used.
融剤としては、塩化ナトリウム、塩化バリウム、塩化カ
リウム、塩化ストロンチウム、フッ化ナトリウムなどが
用いられる。融剤の使用量はバリウムフェライト微粒子
に対して、１０〜１８０重量％、特に３０〜１２０重量
％が好ましい。融剤の量が少なすぎると粒子の焼結が起
こり、また多すぎても多くしたことによる利点はな（，
７経済的でない。バリウムフェライト微粒子、融剤およ
びＮｉ１Ｚｎ及びＣｏの化合物の混合方法は特に制限は
なく、水を加えて湿式混合した後、乾燥してもよ（、ま
た乾式混合してもよい。As the flux, sodium chloride, barium chloride, potassium chloride, strontium chloride, sodium fluoride, etc. are used. The amount of the flux used is preferably 10 to 180% by weight, particularly 30 to 120% by weight, based on the barium ferrite fine particles. If the amount of flux is too small, sintering of the particles will occur, and if it is too large, there will be no benefit from adding more.
7 It is not economical. There is no particular restriction on the method of mixing the barium ferrite fine particles, the flux, and the Ni1Zn and Co compounds, and the mixture may be wet-mixed by adding water and then dried (or may be dry-mixed).
加熱温度は７００〜９５０°Ｃ１好ましくは８００〜９
３０°Ｃである。温度が低すぎるとＮｉ、 Ｚｎ及びＣ
ｏの結晶格子への組み入れが十分に進まず、飽和磁化が
低くなる。また温度が高すぎると粒子が大きくなったり
、焼結が起こるので好ましくない。Heating temperature is 700-950°C, preferably 800-9
It is 30°C. If the temperature is too low, Ni, Zn and C
The incorporation of o into the crystal lattice does not progress sufficiently, resulting in low saturation magnetization. Furthermore, if the temperature is too high, the particles become large and sintering occurs, which is not preferable.
加熱時間は１０分〜３０時間程度が適当である。Appropriate heating time is about 10 minutes to 30 hours.
加熱雰囲気は特に制限されないが、一般に空気雰囲気が
便利である。洗浄は融剤、過剰のバリウムなどの不純物
を十分に除去できればどのような方法で行ってもよい、
洗浄液としては、水や硝酸、塩酸などの無機酸、酢酸、
プロピオン酸などの有機酸などを用いることができる。The heating atmosphere is not particularly limited, but an air atmosphere is generally convenient. Cleaning may be performed by any method that can sufficiently remove impurities such as flux and excess barium.
Cleaning liquids include water, inorganic acids such as nitric acid and hydrochloric acid, acetic acid,
Organic acids such as propionic acid can be used.
（実施例）
以下に実施例および比較例を示し、さらに詳しく本発明
について説明する。(Example) The present invention will be explained in more detail by showing Examples and Comparative Examples below.
実施例１
脱イオン水１３００ｄに、硝酸第二鉄［Ｆｅ（ＮＯｚ）
ｓ・９ＨｚＯ］１２２５．７ｇ、硝酸コバルト［Ｃ０（
ＮＯり ｚ”６８．０］５３．５ｇ、硝酸ニッケル［Ｎ
ｉ （ＮＯ＋） ｚ・６Ｈ２０コ８．９ｇ、硝酸亜鉛［
Ｚｎ（ＮＯ，）ｇ・６ＨｚＯ］９．２ｇおよび四塩化チ
タンＥＴｉＣ１ａ１１７．４ｇを溶解し、別に娩イオン
水１３００ｄに、水酸化バリウム［Ｂａ（ＯＨ） ｇ・
８１１ｚＯ］１４５．Ｏｇおよびカセイソ−ダ（ＮａＱ
Ｈ） １４８０ｇを溶解し、再溶液を混合して沈澱物を
生成させた。Example 1 Ferric nitrate [Fe(NOz)] was added to 1300 d of deionized water.
s・9HzO] 1225.7g, cobalt nitrate [C0(
NOri z"68.0] 53.5g, nickel nitrate [N
i (NO+) z・6H20 8.9g, zinc nitrate [
9.2 g of Zn(NO,)g・6HzO] and 117.4 g of titanium tetrachloride ETiC1a were dissolved, and separately, barium hydroxide [Ba(OH)
811zO]145. Og and caustic soda (NaQ
H) 1480 g was dissolved and remixed to form a precipitate.
得られた沈澱物を含むスラリをオートクレーブに入れ、
１４５°Ｃで８時間水熱処理を行った。次いで得られた
沈澱物を十分に水洗した後、濾過、乾燥し、これに融剤
としてＮａＣ１とＢａＣ１，・２Ｈ３０の重量比が１：
１の混合物を沈澱物に対して１００重景％加えて混合し
た。この混合物を空気雰囲気下で８６０°Ｃで２時間焼
成した。得られた焼成物を水で十分洗浄した後、濾過、
乾燥してバリウムフェライト微粒子を得た。The resulting slurry containing the precipitate was placed in an autoclave;
Hydrothermal treatment was performed at 145°C for 8 hours. Next, the obtained precipitate was thoroughly washed with water, filtered and dried, and a flux of NaCl and BaCl,.2H30 in a weight ratio of 1:1 was added to the precipitate.
1 was added to the precipitate in an amount of 100% by weight and mixed. This mixture was calcined at 860°C for 2 hours under an air atmosphere. After washing the obtained baked product thoroughly with water, filtration,
After drying, barium ferrite fine particles were obtained.
この微粒子を硝酸亜鉛４５．７ｇおよび硝酸ニッケル４
４．５ｇを脱イオン水２００１ｄｌに溶解した溶液に懸
濁させ、ジエチルアミン２０ｍを含む水溶液１００．ｄ
を加えた。得られたスラリを濾別、洗浄した後、乾燥し
、８５０’Ｃで熱処理して、バリウムフェライト磁性粉
を得た。The fine particles were mixed with 45.7 g of zinc nitrate and 4 g of nickel nitrate.
4.5 g of an aqueous solution containing 20 m of diethylamine are suspended in 2001 dl of deionized water. d
added. The resulting slurry was filtered, washed, dried, and heat treated at 850'C to obtain barium ferrite magnetic powder.
得られたバリウムフェライト磁性粉はＸ線粉末回折スペ
クトルおよび組成分析の結果、Ｂａ０４．０（Ｆｅｗ、
Ｊｉｏ、 ６Ｚｎａ、 ＆Ｃ０１１，１Ｔｉｏ、 ３
０１？、 ｚｓ）の均一な六方晶の結晶であった。As a result of X-ray powder diffraction spectrum and composition analysis, the obtained barium ferrite magnetic powder was Ba04.0 (Few,
Jio, 6Zna, &C011,1Tio, 3
01? , zs) was a uniform hexagonal crystal.
またこのバリウムフェライト磁性粉について、粒子形状
、磁気特性、塗膜の光沢度を測定した結果を第１表に示
す。Table 1 shows the results of measuring the particle shape, magnetic properties, and coating gloss of this barium ferrite magnetic powder.
実施例２〜３
実施例１において、Ｎｉ、 ＺｎおよびＣｏの添加を、
最初に硝酸コバル） ５３．５ｇ、次いで硝酸ニッケル
５３．４ｇおよび硝酸亜鉛６３．９ｇとかえた（実施例
２）、最初に硝酸ニッケル６２．３ｇ、次いで硝酸コバ
ルト５３．５ｇおよび硝酸亜鉛５４．８ｇとかえた（実
施例３）ほかは実施例１と同様にしてバリウムフェライ
ト磁性粉を得た。Examples 2 to 3 In Example 1, the addition of Ni, Zn and Co was
First 53.5 g of cobalt nitrate, then 53.4 g of nickel nitrate and 63.9 g of zinc nitrate (Example 2), first 62.3 g of nickel nitrate, then 53.5 g of cobalt nitrate and 54.8 g of zinc nitrate, etc. (Example 3) Barium ferrite magnetic powder was obtained in the same manner as in Example 1 except for the following.
このバリウムフェライト磁性粉について、粒子形状、磁
気特性、塗膜の光沢度を測定した結果を第１表に示す。Table 1 shows the results of measuring the particle shape, magnetic properties, and coating gloss of this barium ferrite magnetic powder.
実施例４
脱イオン水１３００ａｌ！に、硝酸第二鉄１２８７．６
ｇ、硝酸コバル） ４４．６ｇおよび四塩化チタン２３
．２ｇを溶解し、別に脱イオン水１３００ｄに、水酸化
バリウム１４５．０ｇおよびカセイソーダ１４８０ｇを
溶解し、再溶液を混合して沈澱物を生成させた。Example 4 Deionized water 1300al! , ferric nitrate 1287.6
g, cobal nitrate) 44.6 g and titanium tetrachloride 23
．． Separately, 145.0 g of barium hydroxide and 1480 g of caustic soda were dissolved in 1300 d of deionized water, and the solutions were mixed again to form a precipitate.
得られた沈澱物を含むスラリをオートクレーブに入れ、
２７０°Ｃで２時間水熱処理を行った。次いで得られた
沈澱物を十分に水洗した後、濾過、乾燥し、これに硝酸
ニッケル５３．４ｇと硝酸亜鉛５４．８ｇと融剤として
ＮａＣ１とＢａＣｊｚ’２ＨｔＯの重量比が１：１の混
合物を２００ｇ加えて混合した。この混合物を空気雰囲
気下で８８０℃で２時間焼成した。得られた焼成物を水
で十分洗浄した後、濾過、乾燥してバリウムフェライト
磁性粉を得た。The resulting slurry containing the precipitate was placed in an autoclave;
Hydrothermal treatment was performed at 270°C for 2 hours. Next, the obtained precipitate was thoroughly washed with water, filtered and dried, and a mixture of 53.4 g of nickel nitrate, 54.8 g of zinc nitrate, and a mixture of NaCl and BaCjz'2HtO in a weight ratio of 1:1 as a flux was added to the precipitate. 200g was added and mixed. This mixture was calcined at 880° C. for 2 hours under an air atmosphere. The obtained fired product was thoroughly washed with water, filtered and dried to obtain barium ferrite magnetic powder.
得られたバリウムフェライト磁性粉はＸ線粉末回折スペ
クトルおよび組成分析の結果、ＢａＯ’１．０（Ｆｅ＋
ｏ、 Ｊｉｏ、 ｈＺｎｏ、 ５ｃｏｏ、 ５Ｔｉｏ、
４ｏ１ ？＋ ４）の均一な六方晶の結晶であった。As a result of X-ray powder diffraction spectrum and composition analysis, the obtained barium ferrite magnetic powder was found to have BaO'1.0 (Fe+
o, Jio, hZno, 5coo, 5Tio,
4o1? +4) uniform hexagonal crystals.
またこのバリウムフェライト磁性粉について、粒子形状
、磁気特性、塗膜の光沢度を測定した結果を第１表に示
す。Table 1 shows the results of measuring the particle shape, magnetic properties, and coating gloss of this barium ferrite magnetic powder.
比較例１
脱イオン水１３００ｄに、硝酸第二鉄１２２５．７ｇ、
硝酸コバル） ５３．５ｇ、硝酸ニッケル５３．４ｇ、
硝酸亜鉛５４．８ｇおよび四塩化チタン１７．４ｇを溶
解し、別に脱イオン水１３００ｄに、水酸化バリウム１
４５．０ｇおよびカセイソーダ１４８０ｇを溶解し、再
溶液を混合して沈澱物を生成させた。Comparative Example 1 1225.7 g of ferric nitrate in 1300 d of deionized water,
Cobal nitrate) 53.5g, nickel nitrate 53.4g,
Dissolve 54.8 g of zinc nitrate and 17.4 g of titanium tetrachloride, and separately add 1 g of barium hydroxide in 1300 d of deionized water.
45.0 g and 1480 g of caustic soda were dissolved and the re-solutions were mixed to form a precipitate.
得られた沈澱物を含むスラリをオートクレーブに入れ１
．１４５℃で８時間水熱処理を行った。次いで得られた
沈澱物を十分に水洗した後、濾過、乾燥し、これに融剤
としてＮａＣ１とＢａＣｌ１．・２Ｈ３０の重量比が１
：１の混合物を沈澱物に対してｉｏｏ重量％加えて混合
した。この混合物を空気雰囲気下で８６０″Ｃで２時間
焼成した。得られた焼成物を水で十”分洗浄した後、濾
過、乾燥してバリウムフェライト磁性粉を得た。Put the slurry containing the obtained precipitate into an autoclave 1
．． Hydrothermal treatment was performed at 145°C for 8 hours. Next, the obtained precipitate was thoroughly washed with water, filtered and dried, and NaCl1 and BaCl1.・2H30 weight ratio is 1
A mixture of :1 was added in an amount of 100% by weight based on the precipitate and mixed. This mixture was fired in an air atmosphere at 860"C for 2 hours. The resulting fired product was washed with water for a sufficient amount of time, filtered and dried to obtain barium ferrite magnetic powder.
得られたバリウムフェライト磁性粉はＸ線粉末回折スペ
クトルおよび組成分析の結果、Ｂａ０４．０（Ｆｅｗ、
ｄＪｉ＠、 ｈＺｎｏ、 ６ＣＯ１１，ａＴｉａ、
３０１ ？、 ｚｓ）の均一な六方晶の結晶であった。As a result of X-ray powder diffraction spectrum and composition analysis, the obtained barium ferrite magnetic powder was Ba04.0 (Few,
dJi@, hZno, 6CO11, aTia,
301? , zs) was a uniform hexagonal crystal.
またこのバリウムフェライト磁性粉について、粒子形状
、磁気特性、塗膜の光沢度を測定した結′ｉ−
果を第１真に示す。In addition, the results of measuring the particle shape, magnetic properties, and coating gloss of this barium ferrite magnetic powder are shown in the first column.
第１表
比較例２
比較例１と同様な操作により、
Ｂａ（）１．０（Ｆｅｔｅ、 Ｊｉｏ、 ｚＺｎｏ、４
ＣＯ１１，１Ｔ１ｏ、 ４０１７．６）の組成のバリウ
ムフェライト磁性粉を得た。Table 1 Comparative Example 2 By the same operation as Comparative Example 1, Ba()1.0(Fete, Jio, zZno, 4
Barium ferrite magnetic powder having a composition of CO11,1T1o, 4017.6) was obtained.
このバリウムフェライト磁性粉について、粒子形状、磁
気特性、塗膜の光沢度を測定した結果を第１表に示す。Table 1 shows the results of measuring the particle shape, magnetic properties, and coating gloss of this barium ferrite magnetic powder.
特許出願人 宇部興産株式会社Patent applicant: Ube Industries Co., Ltd.
Claims (1)
ｎ＿ｙＣｏ＿ｚＡ＿ｗＯ＿１＿８＿−＿（＿ｘ＿＋＿ｙ
＿＋＿ｚ＿−＿ｗ＿）＿／＿２）（ただし、ＡはＴｉ、
Ｚｒ及びＳｎから選ばれた一種以上の金属原子を示し、
ｎ＝０．９〜１．２、０．５＜ｘ＜２、０．５＜ｙ＜２
、ｚ＋ｗ＜１、ｗ＜０．５である。）で表される六方晶
マグネトプランバイト型バリウムフェライト磁性粉を製
造するに際し、出発原料として、前記一般式の組成に比
較してＮｉ、Ｚｎ及びＣｏから選ばれる一種以上の２価
元素の割合が少ないか又は該２価元素を含有しない板状
バリウムフェライト微粒子を用い、 （１）該微粒子の組成を前記一般式の組成に合わす量の
２価元素を含む水溶液に該微粒子を懸濁させ、アミン類
を添加して該２価元素を粒子表面に付着させた後、濾別
、乾燥し、５００〜９５０℃で加熱するか、あるいは （２）該微粒子の組成を前記一般式の組成に合わす量の
２価元素の化合物と該微粒子および融剤を十分混合し、
７００〜９５０℃で加熱した後、洗浄、濾別、乾燥する
ことにより、前記一般式の組成のバリウムフェライト磁
性粉を得ることを特徴とする磁気記録用板状バリウムフ
ェライト磁性粉の製造方法。[Claims] General formula BaO・n(Fe_1_2_x_y_z_wNi_xZ
n_yCo_zA_wO_1_8_-_(_x_+_y
＿＋＿z＿−＿w＿）＿／＿２）(A is Ti,
Indicates one or more metal atoms selected from Zr and Sn,
n=0.9-1.2, 0.5<x<2, 0.5<y<2
, z+w<1, w<0.5. ) When producing the hexagonal magnetoplumbite type barium ferrite magnetic powder represented by Using plate-shaped barium ferrite fine particles containing little or no divalent element, (1) suspending the fine particles in an aqueous solution containing an amount of divalent elements that matches the composition of the fine particles to the composition of the general formula, and After the divalent element is attached to the surface of the particles by adding a compound of sufficiently mixing the divalent element compound, the fine particles and the flux,
A method for producing plate-shaped barium ferrite magnetic powder for magnetic recording, which comprises heating at 700 to 950°C, followed by washing, filtering, and drying to obtain barium ferrite magnetic powder having the composition of the general formula.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62256202A JPH0723223B2 (en) | 1987-10-13 | 1987-10-13 | Method for producing plate-shaped barium ferrite magnetic powder for magnetic recording |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62256202A JPH0723223B2 (en) | 1987-10-13 | 1987-10-13 | Method for producing plate-shaped barium ferrite magnetic powder for magnetic recording |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01100027A true JPH01100027A (en) | 1989-04-18 |
| JPH0723223B2 JPH0723223B2 (en) | 1995-03-15 |
Family
ID=17289334
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62256202A Expired - Lifetime JPH0723223B2 (en) | 1987-10-13 | 1987-10-13 | Method for producing plate-shaped barium ferrite magnetic powder for magnetic recording |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0723223B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03108303A (en) * | 1989-09-20 | 1991-05-08 | Toshiba Glass Co Ltd | Magnetic powder for high-density magnetic recording |
| JPH04214605A (en) * | 1990-10-11 | 1992-08-05 | Toshiba Corp | Magnetic powder for magnetic recording use |
-
1987
- 1987-10-13 JP JP62256202A patent/JPH0723223B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03108303A (en) * | 1989-09-20 | 1991-05-08 | Toshiba Glass Co Ltd | Magnetic powder for high-density magnetic recording |
| JPH04214605A (en) * | 1990-10-11 | 1992-08-05 | Toshiba Corp | Magnetic powder for magnetic recording use |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0723223B2 (en) | 1995-03-15 |
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