JPS59170202A - Magnetic metallic powder and its production - Google Patents
Magnetic metallic powder and its productionInfo
- Publication number
- JPS59170202A JPS59170202A JP58042709A JP4270983A JPS59170202A JP S59170202 A JPS59170202 A JP S59170202A JP 58042709 A JP58042709 A JP 58042709A JP 4270983 A JP4270983 A JP 4270983A JP S59170202 A JPS59170202 A JP S59170202A
- Authority
- JP
- Japan
- Prior art keywords
- copper
- metallic powder
- magnetic metallic
- magnetic powder
- oxidation stability
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 title claims description 3
- 229910052802 copper Inorganic materials 0.000 claims abstract description 18
- 239000010949 copper Substances 0.000 claims abstract description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 12
- 150000001879 copper Chemical class 0.000 claims abstract description 7
- 239000000725 suspension Substances 0.000 claims abstract description 5
- 239000006247 magnetic powder Substances 0.000 claims description 29
- 229910052751 metal Inorganic materials 0.000 claims description 29
- 239000002184 metal Substances 0.000 claims description 29
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 abstract description 15
- 238000007254 oxidation reaction Methods 0.000 abstract description 15
- 229910052783 alkali metal Inorganic materials 0.000 abstract description 8
- 150000001340 alkali metals Chemical class 0.000 abstract description 8
- 230000005415 magnetization Effects 0.000 abstract description 7
- 230000007423 decrease Effects 0.000 abstract description 5
- 229910000365 copper sulfate Inorganic materials 0.000 abstract description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 abstract description 3
- -1 copper halide Chemical class 0.000 abstract description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 abstract description 2
- 239000012279 sodium borohydride Substances 0.000 abstract description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 22
- 229910052742 iron Inorganic materials 0.000 description 11
- 239000007864 aqueous solution Substances 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 description 3
- 239000001433 sodium tartrate Substances 0.000 description 3
- 229960002167 sodium tartrate Drugs 0.000 description 3
- 235000011004 sodium tartrates Nutrition 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000012448 Lithium borohydride Substances 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 229940116318 copper carbonate Drugs 0.000 description 1
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 1
- AVTYONGGKAJVTE-OLXYHTOASA-L potassium L-tartrate Chemical compound [K+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O AVTYONGGKAJVTE-OLXYHTOASA-L 0.000 description 1
- 239000001508 potassium citrate Substances 0.000 description 1
- 229960002635 potassium citrate Drugs 0.000 description 1
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 description 1
- 235000011082 potassium citrates Nutrition 0.000 description 1
- 239000001472 potassium tartrate Substances 0.000 description 1
- 229940111695 potassium tartrate Drugs 0.000 description 1
- 235000011005 potassium tartrates Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 229960001790 sodium citrate Drugs 0.000 description 1
- 235000011083 sodium citrates Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Abstract
Description
【発明の詳細な説明】
この発明は磁気記録媒体用として好適な金属磁性粉末お
よびその製造方法に関し、その目的とするところは酸化
安定性に優れる金属磁性粉末を提供することにある。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a metal magnetic powder suitable for use in magnetic recording media and a method for producing the same, and an object thereof is to provide a metal magnetic powder with excellent oxidation stability.
鉄、ニッケル、コバルト等の金属磁性粉末は従来の酸化
物系磁性粉末に比較して優れた磁気特性を有しているが
、反面粉末粒子表面が非常に活性なため空気中で非常に
酸化を受は易(、飽和磁化量が経時的に低下し、酸化安
定性に欠けるという難点がある。Metal magnetic powders such as iron, nickel, and cobalt have superior magnetic properties compared to conventional oxide-based magnetic powders, but on the other hand, the surface of the powder particles is very active, so they are highly susceptible to oxidation in the air. However, it has the disadvantage that the saturation magnetization decreases over time and lacks oxidation stability.
このような欠点を改善するため、従来から金属磁性粉末
の粒子表面に酸化物被膜を設けるなどして酸化安定性を
向上することが行われているが、未だ充分な酸化安定性
は得られていない。In order to improve these drawbacks, attempts have been made to improve oxidation stability by forming an oxide film on the particle surface of metal magnetic powder, but sufficient oxidation stability has not yet been achieved. do not have.
この発明者らはかかる現状に鑑み、種々検討を行った結
果、金属磁性粉末と銅塩とを含むアルカリ性懸濁液をア
ルカリ金属ボロハイドライドで還元すると金属磁性粉末
の粒子表面に酸化安定性に優れた銅被膜が形成されて、
酸化安定性に優れた金部磁性粉末が得られることを見い
だし、この発明をなすに至った。In view of the current situation, the inventors conducted various studies and found that when an alkaline suspension containing a metal magnetic powder and a copper salt is reduced with an alkali metal borohydride, the particle surface of the metal magnetic powder has excellent oxidation stability. A copper coating is formed,
It was discovered that Kanabe magnetic powder with excellent oxidation stability can be obtained, and the present invention was completed.
この発明において使用される銅塩としては、硫酸銅、ハ
ロゲン化銅、硝酸銅、炭酸銅などの各種水溶性の銅塩が
好適なものとして使用され、これらは間化剤とともにア
ルカリ水溶液に溶解して使用される。この種の銅塩は金
属磁性粉、末とともにそのアルカリ性懸濁液中でアルカ
リ金属ボロハイドライドによって還元されると、選択的
に金属磁性粉末の粒子表面に析出されて銅被膜が形成さ
れ、この銅被膜は非常に酸化安定性に優れるため金属磁
性粉末の酸化安定性が一段と向上される。このような銅
の使用量は、金属磁性粉末100重量部に対して1.0
〜20.0重量部の範囲内で使用するのが好ましく、少
なすぎると所期の効果が得られず、逆に多すぎると金属
磁性粉末の飽和磁化量がかえって低下する傾向があり磁
気記録媒体用として適さなくなる。As the copper salt used in this invention, various water-soluble copper salts such as copper sulfate, copper halide, copper nitrate, and copper carbonate are preferably used. used. When this type of copper salt is reduced with an alkali metal borohydride in an alkaline suspension together with the metal magnetic powder, it is selectively deposited on the surface of the metal magnetic powder particles to form a copper coating. Since the coating has excellent oxidation stability, the oxidation stability of the metal magnetic powder is further improved. The amount of copper used is 1.0 parts by weight per 100 parts by weight of metal magnetic powder.
It is preferable to use the amount within the range of ~20.0 parts by weight; if it is too small, the desired effect will not be obtained, and if it is too large, the saturation magnetization of the metal magnetic powder will tend to decrease. becomes unsuitable for use.
また、銅塩を溶解しかつ金属磁性粉末を分散させるアル
カリ水溶液としては、水酸化ナトリウム、水酸化カリウ
ム、アンモニア水、水酸化アンモニウム等の水溶液が好
適なものとして使用され、アルカリ濃度はPH12以上
にするのが好ましい。In addition, as the alkaline aqueous solution for dissolving the copper salt and dispersing the metal magnetic powder, aqueous solutions such as sodium hydroxide, potassium hydroxide, aqueous ammonia, and ammonium hydroxide are preferably used, and the alkaline concentration is PH12 or higher. It is preferable to do so.
金属磁性粉末としては、鉄、ニッケル、コバルト等の金
属粉末もしくはこれらの合金粉末、および鉄にAI、C
r、、Mn、S i、Znなどを含有させた鉄を主体と
する合金粉末等が好適なものとして使用され、また錯化
剤としては、酒石酸ナトリウム、クエン酸ナトリウム、
酒石酸カリウム、クエン酸カリウム等が好適なものとし
て使用される。Examples of metal magnetic powders include metal powders such as iron, nickel, and cobalt, or alloy powders of these metals, and iron containing AI, C, etc.
An alloy powder mainly composed of iron containing r, Mn, Si, Zn, etc. is preferably used, and as a complexing agent, sodium tartrate, sodium citrate,
Potassium tartrate, potassium citrate and the like are preferably used.
金属塩溶液から金属磁性粉を製造するには、アルカリ金
属ポロハイドライド、次亜リン酸塩などの還元剤を使用
して溶液中で還元すること社よって適当になし得、特に
アルカリ金属ボロノ\イドライドによる方法が推奨され
る。In order to produce metal magnetic powder from a metal salt solution, reduction in solution using a reducing agent such as alkali metal polyhydride or hypophosphite can be suitably carried out, especially alkali metal borohydride. This method is recommended.
アルカリ金属ボロハイドライドとしては、水素化ホウ素
ナトリウム、水素化夾4つ素カリウム、水素化ホウ素リ
チウムなどが好適に使用され、これらのアルカリ金属ボ
旧\イドライドを金属磁性粉末と銅塩とを含むアルカリ
性懸濁液に加えて還元する際のアルカリ金属ボロノ祠ド
ライドの濃度は0.1モル/!以下では充分な還元が行
えず、10モル/1以上になると還元反応が急激になり
すぎて金属磁性粉末の粒子表面に銅が形成されず、水溶
液中に単独に銅が析出するため0.1モル/l−10モ
ル/lの範囲内であることが好ましい。As the alkali metal borohydride, sodium borohydride, tetrapotassium borohydride, lithium borohydride, etc. are preferably used. The concentration of the alkali metal boronodryide when added to the suspension and reduced is 0.1 mol/! If it is less than 10 mol/1, the reduction reaction will be too rapid and copper will not be formed on the particle surface of the metal magnetic powder, but copper will precipitate alone in the aqueous solution. It is preferably within the range of mol/l to 10 mol/l.
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I
Logの金属鉄磁性粉末(粒径0.22μ、保磁力14
30エルステツド、飽和磁化量153emu/g)を2
50m1のアルカリ水溶液に懸濁させ、これに硫酸銅3
.9gと酒石酸ナトリウム3.6gを熔解させた水溶液
100mff1を添加し、攪拌しながら1モル/l濃度
の水酸化ホウ素ナトリウム水溶液100m1を流加して
還元を行い、金属鉄磁性粉末の粒子表面に銅を析出させ
た。次いで水洗後、アセトンで置換、洗浄した後、乾燥
して粒子表面に銅被膜を有する金属鉄磁性粉末を得た。Example I Log metal iron magnetic powder (particle size 0.22μ, coercive force 14
30 oersted, saturation magnetization 153 emu/g)
Suspend in 50 ml of alkaline aqueous solution, add 3 ml of copper sulfate to this
.. Adding 100 mff1 of an aqueous solution prepared by dissolving 9 g of sodium tartrate and 3.6 g of sodium tartrate, and adding 100 m1 of an aqueous solution of sodium borohydroxide with a concentration of 1 mol/l with stirring to perform reduction. was precipitated. Next, after washing with water, replacing with acetone, washing, and drying, a metal iron magnetic powder having a copper coating on the particle surface was obtained.
実施例1で得られた金属鉄磁性粉末および実施例1で使
用した銅被膜形成処理前の銅被膜を有しない金属鉄磁性
粉末(比較例)について、酸化安定性を試験した。酸化
安定性の試験は各金属鉄磁性粉末を、60℃、90%R
Hの条件下で24時間空気中に放置し、放置後の飽和磁
化量を測定して放置前の飽和磁化量からの低下率を調べ
た。Oxidation stability was tested for the metal iron magnetic powder obtained in Example 1 and the metal iron magnetic powder (comparative example) that did not have a copper coating before the copper coating formation treatment used in Example 1. In the oxidation stability test, each metal iron magnetic powder was tested at 60°C and 90% R.
The sample was left in the air for 24 hours under H conditions, and the saturation magnetization after being left was measured to examine the rate of decrease from the saturation magnetization before being left.
下表はその結果である。The table below shows the results.
上表から明らかなように、この発明で得られた粒子表面
に銅被膜を有する金属鉄磁性粉末(実施例1)は従来の
金属鉄磁性粉末(比較例)に比し、飽和磁化量σSの低
下率が小さく、このことからこの発明によって得られる
金属磁性粉末は酸化安定性に優れていることがわかる。As is clear from the above table, the metal iron magnetic powder (Example 1) having a copper coating on the particle surface obtained by the present invention has a saturation magnetization amount σS compared to the conventional metal iron magnetic powder (comparative example). The rate of decrease was small, which indicates that the metal magnetic powder obtained by the present invention has excellent oxidation stability.
Claims (1)
元剤で溶液中でX還元して金属磁性粉末の粒子表面に銅
被膜を形成することを特徴とする金属磁性粉末の製造方
法[Scope of Claims] I. Metal magnetic powder powder 2 having a copper coating on the surface of the powder particles. Metal magnetic powder obtained by reducing an alkaline suspension containing metal magnetic powder and copper salt with X in a solution using a reducing agent. A method for producing metal magnetic powder, characterized by forming a copper coating on the surface of the powder particles.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP58042709A JPS59170202A (en) | 1983-03-14 | 1983-03-14 | Magnetic metallic powder and its production |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP58042709A JPS59170202A (en) | 1983-03-14 | 1983-03-14 | Magnetic metallic powder and its production |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS59170202A true JPS59170202A (en) | 1984-09-26 |
Family
ID=12643594
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP58042709A Pending JPS59170202A (en) | 1983-03-14 | 1983-03-14 | Magnetic metallic powder and its production |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS59170202A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8911663B2 (en) | 2009-03-05 | 2014-12-16 | Quebec Metal Powders, Ltd. | Insulated iron-base powder for soft magnetic applications |
-
1983
- 1983-03-14 JP JP58042709A patent/JPS59170202A/en active Pending
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8911663B2 (en) | 2009-03-05 | 2014-12-16 | Quebec Metal Powders, Ltd. | Insulated iron-base powder for soft magnetic applications |
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