JPS63260103A - Magnetic powder for magnetic recording - Google Patents
Magnetic powder for magnetic recordingInfo
- Publication number
- JPS63260103A JPS63260103A JP62094801A JP9480187A JPS63260103A JP S63260103 A JPS63260103 A JP S63260103A JP 62094801 A JP62094801 A JP 62094801A JP 9480187 A JP9480187 A JP 9480187A JP S63260103 A JPS63260103 A JP S63260103A
- Authority
- JP
- Japan
- Prior art keywords
- magnetic powder
- magnetic
- value
- magnetic recording
- powder
- 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
- 239000006247 magnetic powder Substances 0.000 title claims abstract description 33
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 4
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 4
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 3
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 3
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 3
- 229910052684 Cerium Inorganic materials 0.000 claims abstract 2
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract 2
- 229910052804 chromium Inorganic materials 0.000 claims abstract 2
- 229910052745 lead Inorganic materials 0.000 claims abstract 2
- 239000002184 metal Substances 0.000 claims description 10
- 125000004429 atom Chemical group 0.000 claims description 5
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052788 barium Inorganic materials 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229910052712 strontium Inorganic materials 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 229910000859 α-Fe Inorganic materials 0.000 description 12
- 230000005415 magnetization Effects 0.000 description 10
- 239000007864 aqueous solution Substances 0.000 description 9
- 238000000975 co-precipitation Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 230000004907 flux Effects 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000000696 magnetic material Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 239000010419 fine particle Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- -1 organic acid salts Chemical class 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910001508 alkali metal halide Inorganic materials 0.000 description 1
- 150000008045 alkali metal halides Chemical class 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 229910001615 alkaline earth metal halide Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229940101545 mi-acid Drugs 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 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 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- PXLIDIMHPNPGMH-UHFFFAOYSA-N sodium chromate Chemical compound [Na+].[Na+].[O-][Cr]([O-])(=O)=O PXLIDIMHPNPGMH-UHFFFAOYSA-N 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000002195 soluble material 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
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は磁気記録用磁性粉に関し、更に詳しくは、高密
度磁気記録媒体用に適する微細な粒子からなる六方晶系
フェライト磁性粉に関するものである。Detailed Description of the Invention (Field of Industrial Application) The present invention relates to magnetic powder for magnetic recording, and more specifically to hexagonal ferrite magnetic powder consisting of fine particles suitable for high-density magnetic recording media. be.
（従来の技術）
近年、磁気記録に対する高密度化の要求に伴い磁気記録
媒体の厚味方向に磁界を記録する垂直磁気記録方式が注
目されている。このような垂直磁気記録方式において使
用される磁性材料は記録媒体表面に垂直な方向に磁化容
易軸を有することが必要である。(Prior Art) In recent years, with the demand for higher density magnetic recording, perpendicular magnetic recording methods that record magnetic fields in the thickness direction of a magnetic recording medium have been attracting attention. The magnetic material used in such perpendicular magnetic recording systems needs to have an axis of easy magnetization in a direction perpendicular to the surface of the recording medium.
六方晶系で一軸磁化異方性を有するフェライト、例えば
ＨａミツエライトＢａＦｅ、□Ｏ１，）は六角板状の結
晶であって、板面に垂直な方向に磁化容易軸を有してお
り、塗布膜タイプの垂直磁気記録用磁性材料として上記
の要件を満足するものである。該磁性材料としては適度
な保磁力（１１ｃ、通常２００〜２００００ｅ程度）と
できるだけ大きな飽和磁化（σ８、少くとも４０ｅ＋ｍ
ｕ／ｇ以上）を有している事、及び磁性粉の平均粒子径
は記録波長の関係から０．３μｍ以下であり、かつ超常
磁性の関係から０．０１μｍ以上の範囲であることが必
要である。Ferrite having a hexagonal crystal system and uniaxial magnetization anisotropy, such as Hamitzerite BaFe, □O1,) is a hexagonal plate-shaped crystal with an axis of easy magnetization perpendicular to the plate surface, and the coating film This material satisfies the above requirements as a type of magnetic material for perpendicular magnetic recording. The magnetic material should have a moderate coercive force (11c, usually about 200 to 20,000e) and a saturation magnetization as large as possible (σ8, at least 40e+m).
u/g or more), and the average particle diameter of the magnetic powder must be 0.3 μm or less in relation to the recording wavelength, and in the range of 0.01 μm or more in relation to superparamagnetism. be.
この範囲では平均粒子径はノイズの関係から小さい方が
好ましく、さらに０．１μｍ以下であることが好ましい
。In this range, the average particle diameter is preferably smaller in terms of noise, and more preferably 0.1 μm or less.
（発明が解決しようとする問題点）
ところで、Ｂａ−フェライトは保磁力が５００００ｅ以
上であり、このままでは磁気記録用磁性材料としては大
きすぎるので、Ｆｅの一部を他の各種金属で置換して、
保磁力を低下させる方法が提案されている（例えば特開
昭６１−４０８２３号公報など）。(Problems to be Solved by the Invention) By the way, Ba-ferrite has a coercive force of 50,000e or more, which is too large to be used as a magnetic material for magnetic recording as it is, so some of the Fe is replaced with various other metals. ,
A method of lowering the coercive force has been proposed (for example, Japanese Patent Application Laid-Open No. 61-40823).
しかしながら、公知のＦｅの一部を他の各種金属で置換
しただけの磁性粉は、平均粒径が０．ｌ１１ｍ以上と比
較的大きく垂直磁気記録用磁性粉としてはまだ不充分で
ある。また、バリウムフェライトの製造にはガラス結晶
化法、水熱合成法あるいは共沈法などが用いられている
が、共沈法は、保磁力制御やその他の目的で少量添加さ
れる各種金属との混合が非常に良いため均一なフェライ
トが得られること、共沈物が微結晶粉末であるので比較
的低温でフェライト化し得ることなど多くの長所を有し
ている。しかしながら、一般に、共沈法で得られる磁性
粉は、粒径は最小でも、０．１５μｍと大きく （特開
昭６１−１７４１１８号公報参照）、凝集した状態の粉
末が生成しやすく、粒径が０．５μｍ位のものが含まれ
ており形状の均一性も低く （特開昭５８−２２２３号
公報参照）、共沈法による磁気記録用に満足できる磁性
粉は未だ得られていない。However, known magnetic powders in which only a portion of Fe is replaced with various other metals have an average particle size of 0. It is relatively large, more than 11 m, and is still insufficient as a magnetic powder for perpendicular magnetic recording. In addition, glass crystallization, hydrothermal synthesis, coprecipitation, and other methods are used to manufacture barium ferrite, but the coprecipitation method uses various metals added in small amounts for coercive force control and other purposes. It has many advantages, such as being able to mix very well so that uniform ferrite can be obtained, and since the coprecipitate is a microcrystalline powder, it can be turned into ferrite at a relatively low temperature. However, magnetic powder obtained by the coprecipitation method generally has a large particle size of 0.15 μm at the minimum (see Japanese Patent Application Laid-Open No. 174118/1983), tends to produce agglomerated powder, and has a large particle size. It contains particles of about 0.5 μm, and the uniformity of the shape is low (see Japanese Patent Laid-Open No. 58-2223), and magnetic powder satisfactory for magnetic recording by the coprecipitation method has not yet been obtained.
本発明者等は、この様な背景に鑑み、従来にも増して平
均粒径の小さい垂直磁気記録用磁性粉を開発すべく鋭意
検討した結果、本発明において新たな磁性粉を開発する
に到った。In view of this background, the present inventors conducted intensive studies to develop a magnetic powder for perpendicular magnetic recording with a smaller average particle diameter than ever before, and as a result, they were able to develop a new magnetic powder in the present invention. It was.
（問題点を解決するための手段）
すなわち、本発明により、一般組成式
％式％［０
（ここでＭｌはＢａ、 Ｓｒ、 Ｃａ及びｐｂから選択
される少なくとも一種の金属元素を表わし、ＭＭはＣｒ
。(Means for solving the problem) That is, according to the present invention, the general composition formula % formula % [0 (where Ml represents at least one metal element selected from Ba, Sr, Ca and PB, and MM represents Cr
.
Ｍｏ、 Ｗ、 Ｃｅ、 Ｎａ、 Ｓｍ及びＰから選択さ
れる少なくとも一種の金属元素を表わし、ａ、ｂ、ｃ、
ｄ。Represents at least one metal element selected from Mo, W, Ce, Na, Sm and P, a, b, c,
d.
ｅ及びｆはそれぞれＦｅ、 Ｃｏ、 Ｓｔ、 ＭＩ、
Ｍ”及びＯの原子数であり、ａは８〜１２、ｂは０．０
１〜３．０、Ｃは０．０５〜２．０、ｄは０．５．〜３
．０及びｅは０．Ｏ１〜３．０の値をとり、ｆは他の元
素の原子価を満足する酸素の原子数を表わす。）で表わ
されることを特徴とする磁気記録用磁性粉が提供される
。e and f are respectively Fe, Co, St, MI,
M” and the number of atoms of O, a is 8 to 12, b is 0.0
1 to 3.0, C is 0.05 to 2.0, d is 0.5. ~3
．． 0 and e are 0. It takes a value of O1 to 3.0, and f represents the number of oxygen atoms satisfying the valences of other elements. ) A magnetic powder for magnetic recording is provided.
本発明においては、磁性粉の各成分元素の原子数ａ”−
ｅが上記の数値範囲内にあることが必要で、この範囲外
では平均粒子径が０．１μｍ以上と゛なるばかりでなく
磁気記録用磁性粉に適した保磁力や飽和磁化を持った磁
性粉は得られ難い。In the present invention, the number of atoms of each component element of the magnetic powder is a''-
It is necessary that e be within the above numerical range; outside this range, magnetic powder not only has an average particle diameter of 0.1 μm or more but also has coercive force and saturation magnetization suitable for magnetic recording magnetic powder. It's hard to get caught.
好ましい磁性粉の各成分割合は、ａは８〜１２、ｂは０
．０２〜２．４、Ｃは０．１〜１．０．ｂは０．８〜２
．０及びｅは０．０２〜２．４の値をとり、ｆは他の元
素の原子価を満足する酸素の原子数である。本発明の磁
性粉は、製造条件などによっては得られる磁性粉粒子の
結晶がかならずしも正常な六角板状を呈していない粒子
が混在している場合もあるが、該原子数が本発明の範囲
内であれば、本発明の目的を充分に達成することができ
る。The preferable ratio of each component of magnetic powder is a: 8 to 12, b: 0
．． 02-2.4, C is 0.1-1.0. b is 0.8-2
．． 0 and e take values of 0.02 to 2.4, and f is the number of oxygen atoms that satisfies the valences of other elements. The magnetic powder of the present invention may contain particles whose crystals do not necessarily have a normal hexagonal plate shape depending on the manufacturing conditions, but the number of atoms is within the range of the present invention. If so, the purpose of the present invention can be fully achieved.
本発明の磁性粉は平均粒径が０．１μｍ以下で、かつ磁
気記録用磁性粉として要求される所定の保磁力及び飽和
磁化を有している。The magnetic powder of the present invention has an average particle diameter of 0.1 μm or less, and has a predetermined coercive force and saturation magnetization required as a magnetic powder for magnetic recording.
本発明の磁性粉はガラス結晶化法、水熱合成法によって
も製造することができるが、共沈法もしくは共沈フラツ
クス性により製造すると粒径及び磁気特性が著しく改善
されるものとなる。以下に共沈法による本発明磁性粉の
製造について説明する。The magnetic powder of the present invention can also be produced by glass crystallization or hydrothermal synthesis, but when produced by coprecipitation or coprecipitation flux, the particle size and magnetic properties are significantly improved. The production of the magnetic powder of the present invention by the coprecipitation method will be explained below.
本発明の磁性粉を構成する各金属元素の原料化合物とし
ては酸化物、オキシ水酸化物、水酸化物、アンモニウム
塩、硝酸塩、硫酸塩、炭酸塩、有機酸塩、ハロゲン化物
、アルカリ金属塩等の塩類、遊離酸、酸無水物、縮合酸
等を挙げることができる。特に水溶性化合物が好ましい
。各金属元素の原料化合物は、各金属元素の原子数が前
記の６値となる様に水に混合溶解される。また、アルカ
リ水溶液に混合溶解した方が都合がよい場合には、後述
のアルカリ水溶液中に混合溶解される。The raw material compounds for each metal element constituting the magnetic powder of the present invention include oxides, oxyhydroxides, hydroxides, ammonium salts, nitrates, sulfates, carbonates, organic acid salts, halides, alkali metal salts, etc. Examples include salts, free acids, acid anhydrides, and condensed acids. Particularly preferred are water-soluble compounds. The raw material compounds of each metal element are mixed and dissolved in water so that the number of atoms of each metal element becomes the six values described above. Further, if it is convenient to mix and dissolve in an alkaline aqueous solution, it can be mixed and dissolved in an alkaline aqueous solution, which will be described later.
一方アルカリ水溶液に用いるアルカリ成分としては、水
溶性のものであれば特に限定されず、アルカリ金属の水
酸化物や炭酸塩、アンモニア、炭酸アンモニウム等が挙
げられる。例えばＮａ０１１゜ＮａｌＣｏ５． Ｎａｔ
ｌＣＯｔ、 ＫＯＨ，ＫｚＣＯｚ、 Ｎ１１４０１１．
（Ｎｌ１４）ｔｃＯ：＋等が用いられ、特に水酸化物と
炭酸塩の併用が賞月される。On the other hand, the alkaline component used in the alkaline aqueous solution is not particularly limited as long as it is water-soluble, and examples thereof include alkali metal hydroxides, carbonates, ammonia, ammonium carbonate, and the like. For example, Na011°NalCo5. Nat
lCOt, KOH, KzCOz, N114011.
(Nl14)tcO:+ etc. are used, and combinations of hydroxide and carbonate are particularly preferred.
しかして、上記金属イオン水溶液とアルカリ水溶液とを
混合し、ｐＨ５以上、好ましくはｐＨ８以上で共沈物を
生ぜしめる。得られた共沈物は、水洗した後決別する。Then, the metal ion aqueous solution and the alkaline aqueous solution are mixed to form a coprecipitate at a pH of 5 or higher, preferably at a pH of 8 or higher. The obtained coprecipitate is separated after washing with water.
この様にして得られたケーキ状ないしスラリー状の共沈
物は、共沈法による場合には、これを乾燥後、６００〜
１１００℃で１０分〜３０時間高温焼成して該当する六
方晶系フェライト［性粉を得る。また、共沈フラツクス
性による場合には、水洗された共沈物に水溶性フラック
ス（例えば塩化ナトリウムや塩化カリウム等のハロゲン
化アルカリ金属塩、塩化バリウムや塩化ストロンチウム
等のハロゲン化アルカリ土類金属塩、硫酸ナトリウム、
硫酸カリウム、硝酸ナトリウム、硝酸カリウム、及びこ
れ等の混合物等が通常使用される）を適当量加えて、あ
るいは、金属イオン水溶液とアルカリ水溶液との混合物
から得られる共沈物を水洗することなくそのまま水分を
蒸発させてこれを乾燥後、６００〜１１００℃で１０分
〜３０時間高温焼成した後、水溶性フラックスを水また
は酸水溶液で洗浄が別し、必要に応じ、更に水洗した後
、乾燥して該当する大方晶系フェライト磁性粉を得る。When using the coprecipitation method, the cake-like or slurry-like coprecipitate obtained in this way is dried and then
The corresponding hexagonal ferrite powder is obtained by high-temperature firing at 1100° C. for 10 minutes to 30 hours. In addition, in the case of coprecipitation flux, water-soluble flux (for example, alkali metal halides such as sodium chloride and potassium chloride, alkaline earth metal halides such as barium chloride and strontium chloride) is added to the washed coprecipitate. , sodium sulfate,
Potassium sulfate, sodium nitrate, potassium nitrate, and mixtures thereof are usually used), or a coprecipitate obtained from a mixture of a metal ion aqueous solution and an alkaline aqueous solution is directly hydrated without washing with water. After evaporating and drying this, it is fired at a high temperature of 600 to 1100°C for 10 minutes to 30 hours, and then the water-soluble flux is washed with water or an acid aqueous solution, and if necessary, after further washing with water, it is dried. A corresponding macrogonal ferrite magnetic powder is obtained.
（発明の効果）
本発明に係る磁性粉は六方晶Ｃ面に磁化容易軸を有する
板状粒子であり、平均粒径が０．１μｍ以下と小さいば
かりでなく、粒径もととのっており、しかも、磁気記録
用に要求される保磁力、飽和磁化を有するので、垂直磁
気記録用磁性材料として好適である。(Effect of the invention) The magnetic powder according to the present invention is a plate-shaped particle having an axis of easy magnetization in the hexagonal C plane, and not only has an average particle size of 0.1 μm or less, but also has a particle size that is the same as the original size. Since it has the coercive force and saturation magnetization required for magnetic recording, it is suitable as a magnetic material for perpendicular magnetic recording.
（実施例）
以下に実施例を挙げて、本発明をさらに具体的に説明す
る。なお実施例中の保磁力及び飽和磁化はＶＳＭ （振
動磁気測定装置）を用い、最大印加磁場１０ ｋＯｅ、
測定温度２８℃で測定した。平均粒子径は、透過型電子
顕微鏡で得られた写真から４００個の粒子の最大直径を
測定し算術平均により算出した。(Example) The present invention will be described in more detail with reference to Examples below. The coercive force and saturation magnetization in the examples were measured using a VSM (vibrating magnetometer), with a maximum applied magnetic field of 10 kOe,
The measurement was performed at a measurement temperature of 28°C. The average particle diameter was calculated by measuring the maximum diameter of 400 particles from a photograph taken with a transmission electron microscope and calculating the arithmetic average.
また、実施例中に示す磁性粉の組成式は、原料調製時の
各元素の原子比を用いている。磁性粉成分中の酸素の表
示については、簡略化のため省略した。Further, the compositional formula of the magnetic powder shown in the examples uses the atomic ratio of each element at the time of raw material preparation. The display of oxygen in the magnetic powder components has been omitted for the sake of brevity.
実施例１
ＢａＣＡ ！ ’ ２８ｚ０ ０．５５モル、ＣｏＣｌ
ｔ ・６Ｈｔ８０．４モル及びＦｅＣ１ｓ ・６Ｈｚ
０ ５．４モルを１０１の蒸留水にこの順に溶解し、こ
れをＡ液とした。Example 1 BaCA! '28z0 0.55 mol, CoCl
t ・6Ht80.4 mol and FeCls ・6Hz
5.4 mol of 0.0 was dissolved in 101 distilled water in this order, and this was used as liquid A.
Ｎａ０ｆｌ １７．５モル、ＮａｚＣＯｓ ４．７
２モル、ＮａｚＣｒＯ＝ １４１１ｚ０ ０．２モル及
びＮａ、ＳｉＯ，・９Ｈ２００，２モルを１５１の室温
の蒸留水に溶解し、これをＢ液とした。５０℃に熱した
Ａ液にＢ液を徐々に加えた後、５０℃で１６時間攪拌し
た。攪拌後のｐＨは１Ｏ０６であった。こうして得られ
た共沈物を濾別し充分水洗した後１５０℃で乾燥し、９
００℃で２時間電気炉で焼成した。こうして得られたＢ
ａ−フェライトはＢａｌ、 ＋Ｆｅｌ ｏ、 ５Ｃｏｏ
、 ａｃｒｅｌｓｉｏ、 ａで示される。Na0fl 17.5 mol, NazCOs 4.7
2 moles of NazCrO=1411z0 and 2 moles of Na, SiO, .9H200, were dissolved in 151 room temperature distilled water, and this was used as liquid B. After gradually adding Solution B to Solution A heated to 50°C, the mixture was stirred at 50°C for 16 hours. The pH after stirring was 1006. The coprecipitate thus obtained was separated by filtration, thoroughly washed with water, and then dried at 150°C.
It was fired in an electric furnace at 00°C for 2 hours. B thus obtained
a- Ferrite is Bal, +Fel o, 5Coo
, acrelsio, a.
この微粒子粉末は、平均粒径０．０７５μｍの板状であ
り、保磁力は６７５０ｅ、飽和磁化は５４．９ｅｍｕ／
ｇであった・
比較例１
クロム酸ナトリウムを除いた他は実施例１と全く同様の
方法でＢａ−フェライトを製造した。得られたＢａ−フ
ェライトはＢａｔ、 ｔＦｅ＋ １１． ＩＣ０６，ａ
ｓｉｏ、 ａで示される。この微粒子粉末は平均粒径０
．２３μｍの板状であり、Ｈｅは８６９０ｅ、Ｃ３は４
３．５ ｅｍｕ／ｇであった。This fine particle powder has a plate shape with an average particle size of 0.075 μm, a coercive force of 6750e, and a saturation magnetization of 54.9 emu/
Comparative Example 1 Ba-ferrite was produced in exactly the same manner as in Example 1 except that sodium chromate was removed. The obtained Ba-ferrite is Bat, tFe+ 11. IC06,a
sio, denoted by a. This fine particle powder has an average particle size of 0
．． It is a plate shape of 23 μm, He is 8690e, C3 is 4
It was 3.5 emu/g.
実施例２
［１ａＣ１’ ｔ ・２Ｈｚ８ ０．５５モル、ＣｏＣ
ｌ ｚ ’ ６Ｈｔ００．４５モル、Ｃｅ（ＮＯ＋）ｓ
’ ６Ｈｚ０ ０．０５モル及びＦ１３Ｃｊ！ ｓ
’ ６８ｚＯ５，５モルを１０７！の蒸留水にこの順に
溶解し、これをＡ液とした。ＮａＯＨ１７，５モル、Ｎ
ａｌＣｏ５ ４．７２モル及びＮａｚＳｉＯｚ ・９８
２００．２５モルを１５１の室温の蒸留水に溶解し、こ
れをＢ液とした。５０℃に熱したＡ液にＢ液を徐々に加
えた後、５０℃で１６時間攪拌した。攪拌後のｐＨは１
０．７であった。こうして得られた共沈物を決別し水洗
して得られたケーキ状の共沈物スラリ−にフラックスと
してＭａｃ１４００ｇを加え、充分に混合した後水分を
蒸発乾固せしめ、これを８４０℃で１．５時間電気炉で
焼成した。この焼成物を水を用いて可溶物がなくなるま
で洗浄した後、炉別、乾燥した。こうして得られたＢａ
−フェライートは、Ｂａ１１Ｆｅ＋ ｒ、 ｏＣｏ、）
、 ＊Ｃｅｏ、 ＋Ｓｉｏ、 ｓで示される。Example 2 [1aC1' t ・2Hz8 0.55 mol, CoC
l z' 6Ht00.45 mol, Ce(NO+)s
'6Hz0 0.05 mol and F13Cj! s
'68zO5.5 mole is 107! were dissolved in distilled water in this order, and this was used as Solution A. 17.5 mol of NaOH, N
alCo5 4.72 mol and NazSiOz 98
200.25 mol was dissolved in 151 room temperature distilled water, and this was used as liquid B. After gradually adding Solution B to Solution A heated to 50°C, the mixture was stirred at 50°C for 16 hours. pH after stirring is 1
It was 0.7. The coprecipitate thus obtained was separated and washed with water, and 1,400 g of Mac was added as a flux to the resulting cake-like coprecipitate slurry, and after thorough mixing, water was evaporated to dryness. It was fired in an electric furnace for 5 hours. The fired product was washed with water until all soluble materials were removed, then separated in a furnace and dried. Ba obtained in this way
- Ferrite is Ba11Fe+ r, oCo,)
, *Ceo, +Sio, s.
この微粒子粉末は、平均粒径０．０８１μｍの板状であ
り、Ｈｃは８１１０ｅ、σ、は５６．３ ｅｍｕ／ｇで
あった。This fine particle powder was plate-shaped with an average particle size of 0.081 μm, Hc was 8110e, and σ was 56.3 emu/g.
実施例３〜６
Ｍｌ成分、組成比、フラックスの種類及び量を変えた他
は実施例２と全く同様の方法で第１表に示すＢａ−フェ
ライトを製造した。Examples 3 to 6 Ba-ferrite shown in Table 1 was produced in exactly the same manner as in Example 2, except that the Ml component, composition ratio, and type and amount of flux were changed.
実施例１〜６の結果から、本発明に係る磁性粉は、０．
１μｍ以下の平均粒径を有する磁性粉が得られることが
わかる。From the results of Examples 1 to 6, the magnetic powder according to the present invention has a 0.
It can be seen that magnetic powder having an average particle size of 1 μm or less can be obtained.
実施例７〜２３
Ｍ１成分Ｍｘ成分及び組成比を変えた他は、実施例２と
全く同様の方法によって表−２に示す磁性粉を調製した
。なお、ＭＩ酸成分原料は塩化物を使用し、ＭＩ［成分
の原料は、Ｃｒはナトリウム塩、Ｍｏ、 Ｗ、及びＰは
アンモニウム塩を使用し、その他の成分は硝酸塩を使用
した＊ Ｃｒ９Ｍｏ、Ｗ、及びＰの原料化合物は、アル
カリ水溶液中に溶解した。Examples 7 to 23 Magnetic powders shown in Table 2 were prepared in exactly the same manner as in Example 2, except that the M1 component, Mx component, and composition ratio were changed. Note that chloride was used as the raw material for the MI acid component, and sodium salt was used for Cr, ammonium salt was used for Mo, W, and P, and nitrate was used for the other components. , and the raw material compounds of P were dissolved in an alkaline aqueous solution.
Claims (1)
＿ｆ（ここでＭ＾ＩはＢａ、Ｂｒ、Ｃａ及びＰｂから選
択される少なくとも一種の金属元素を表わし、Ｍ＾Ｉ＾
ＩはＣｒ、Ｍｏ、Ｗ、Ｃｅ、Ｎｄ、Ｓｍ及びＰから選択
される少なくとも一種の金属元素を表わし、ａ、ｂ、ｃ
、ｄ、ｅ及びｆはそれぞれＦｅ、Ｃｏ、Ｓｉ、Ｍ＾Ｉ、
Ｍ＾Ｉ＾Ｉ及びＯの原子数であり、ａは８〜１２、ｂは
０．０１〜３．０、ｃは０．０５〜２．０、、ｄは０．
５〜３．０及びｅは０．０１〜３．０の値をとり、ｆは
他の元素の原子価を満足する酸素の原子数である。） で表わされる磁気記録用磁性粉。[Claims] General composition formula Fe_aCo_bSi_cM^I_dM^I^I_eO
_f (here, M^I represents at least one metal element selected from Ba, Br, Ca, and Pb, and M^I^
I represents at least one metal element selected from Cr, Mo, W, Ce, Nd, Sm and P; a, b, c
, d, e and f are Fe, Co, Si, M^I, respectively.
The number of atoms of M^I^I and O, a is 8 to 12, b is 0.01 to 3.0, c is 0.05 to 2.0, and d is 0.
5 to 3.0 and e take values of 0.01 to 3.0, and f is the number of oxygen atoms satisfying the valences of other elements. ) Magnetic powder for magnetic recording.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62094801A JPS63260103A (en) | 1987-04-17 | 1987-04-17 | Magnetic powder for magnetic recording |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62094801A JPS63260103A (en) | 1987-04-17 | 1987-04-17 | Magnetic powder for magnetic recording |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63260103A true JPS63260103A (en) | 1988-10-27 |
Family
ID=14120162
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62094801A Pending JPS63260103A (en) | 1987-04-17 | 1987-04-17 | Magnetic powder for magnetic recording |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63260103A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0940823A1 (en) * | 1997-09-19 | 1999-09-08 | TDK Corporation | Oxide magnetic material, ferrite particles, bonded magnet, sintered magnet, method of manufacturing the same, and magnetic recording medium |
-
1987
- 1987-04-17 JP JP62094801A patent/JPS63260103A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0940823A1 (en) * | 1997-09-19 | 1999-09-08 | TDK Corporation | Oxide magnetic material, ferrite particles, bonded magnet, sintered magnet, method of manufacturing the same, and magnetic recording medium |
| EP0940823A4 (en) * | 1997-09-19 | 2001-05-23 | Tdk Corp | Oxide magnetic material, ferrite particles, bonded magnet, sintered magnet, method of manufacturing the same, and magnetic recording medium |
| US6402980B1 (en) | 1997-09-19 | 2002-06-11 | Tdk Corporation | Oxide magnetic material, ferrite particles, bonded magnet, sintered magnet, process for producing the same, and magnetic recording medium |
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