KR900000272B1 - Making process for magnetic metal powder - Google Patents

Making process for magnetic metal powder Download PDF

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KR900000272B1
KR900000272B1 KR1019860003057A KR860003067A KR900000272B1 KR 900000272 B1 KR900000272 B1 KR 900000272B1 KR 1019860003057 A KR1019860003057 A KR 1019860003057A KR 860003067 A KR860003067 A KR 860003067A KR 900000272 B1 KR900000272 B1 KR 900000272B1
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magnetic
atomic
powder
solution
aqueous solution
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KR1019860003057A
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KR870009797A (en
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이택동
나종갑
장평우
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한국과학 기술원
이정오
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof

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  • Manufacturing Of Magnetic Record Carriers (AREA)

Abstract

내용 없음.No content.

Description

자기기록용 금속자성분말을 제조하는 방법Method of manufacturing magnetic magnetic powder for magnetic recording

제1도는 Mn을 함유하는 α-FeOOH 분말을 전자현미경 사진(X20,000).1 is an electron micrograph (X20,000) of α-FeOOH powder containing Mn.

제2도는 자기기록용 금속자성분말의 내산화특성 그라프.2 is a graph of oxidation resistance of magnetic powder for magnetic recording.

본 발명은 자기기록매체로 사용되고 있는 금속자성분말을 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a magnetic metal powder used as a magnetic recording medium.

세계적으로 녹음기, VTR, 각종 소형 및 대형콤퓨터 등에 쓰이는 각종 자기기록재료의 수요는 매년 급격하게 늘어나고 있다. 현재까지 이러한 용도에 쓰이는 자기기록 재료는 γ-Fe2O3분말이나 Co피막처리 γ-Fe2O3분말을 각종 바인더와 섞어서 폴리에스터 필름이나 다른 기지에 도포하여 만든 도포형 소재가 주류를 이루고 있다. 그러나 최근 녹음기, VTR, 컴퓨터등이 소형화 경향으로 발전되어 가고 있기 때문에 여기에 쓰이는 자기기록 재료도 고밀도화와 고출력화가 요구되고 있다. 금속자성분말은 앞에서 언급한 산화물계 자성분말에 비하여 그 자기적인 특성 즉 보자력, 잔류자화 및 포화자화가 월등히 우수하여 고밀도, 고출력용 자기기록 재료로서 주목받아 왔다. 그러나 금속자성분말은 화학적으로 매우 불안정하기 때문에 쉽게 산화되어 그 자기적 특성이 나빠지는 결점이 있다. 이에 본 발명자들은 금속자성분말에 금속자성분말과는 성분이 다른 미량의 금속 또는 합금을 첨가시킴으로써 금속자성분말의 내산화성을 향상시킬 수 있음을 실험을 통하여 확인 하였다. 첨가한 금속 또는 합금의 성분으로는 Mn과 Mn에 소량의 Cu와 Zn의 1성분 또는 2성분이다. 첨가량은 Mn의 경우 금속자성분말에 대하여 0.01원자%에서 2원자%로 하였으며 Mn합금의 경우는 금속자성분말에 대하여 Mn이 0.01원자%에서 2원자%, Cu와 Zn이 각각 0.01원자%에서 1원자% 범위안에서 첨가하였다.Globally, the demand for magnetic recording materials used in recorders, VTRs, various small and large computers is increasing rapidly every year. Until now, the magnetic recording material used in these applications is mainly composed of a coating material made by mixing γ-Fe 2 O 3 powder or Co-coated γ-Fe 2 O 3 powder with various binders and applying it to a polyester film or another base. have. However, in recent years, recorders, VTRs, computers, and the like have been developed in miniaturization trends, and the magnetic recording materials used therein are also required to have high density and high output. The metal magnetic powder has attracted attention as a high density, high output magnetic recording material because of its excellent magnetic properties, coercive force, residual magnetization, and saturation magnetization, as compared to the oxide magnetic powder mentioned above. However, since the magnetic powder is chemically very unstable, it is easily oxidized and its magnetic properties deteriorate. Accordingly, the present inventors have confirmed through the experiment that the oxidation resistance of the metal magnetic powder can be improved by adding a trace amount of metal or an alloy different from the metal magnetic powder to the metal magnetic powder. The component of the added metal or alloy is one or two components of a small amount of Cu and Zn in Mn and Mn. The amount of Mn is 0.01 atomic% to 2 atomic% with respect to the metallic magnetic powder. For Mn alloys, Mn is 0.01 atomic% to 2 atomic percent with respect to the metallic magnetic powder, and Cu and Zn are 0.01 atomic% to 1 atomic percent, respectively. Added in% range.

이하 본 발명을 실시예로 들어 상세히 기재하면 다음과 같다.Hereinafter, the present invention will be described in detail with reference to Examples.

[실시예 1]Example 1

철 9mole를 함유한 황산제1철과 망간 0.05mole을 함유한 황산망간으로 만든 10ℓ의 수용액에 4.6N의 가성소다 수용액 9l를 첨가하여 19l의 수용액을 만들었다. 이 수용액을 30°~ 40℃로 가열하고 200l/min의 유속으로 공기를 취입하면서 산화시켜 장축 0.5㎛, 단축 0.09㎛의 침상형태를 갖는 α-FeOOH분말을 석출시켰다(제1도는 이 α-FeOOH분말의 형상을 보여주는 전자현미경 사진이다.) 이 α-FeOOH를 수세, 건조후 1l/min의 유속을 갖는 수소분위기의 전기로 내에서 700℃ 이하의 온도에서 2시간동안 환원시켜 망간을 함유한 금속분말을 얻었다. 이 자성분말의 내산화 특성은 이슬점이 40℃인 수증기를 포함한 40℃의 공기 분위기하에서 산화시켜 자성분말의 포화자화값의 저하율을 측정한 결과는 제2도에 도시하였다.To a 10 L aqueous solution made up of ferrous sulfate containing 9 mole of iron and manganese sulfate containing 0.05 mole of manganese, 9 l of an aqueous solution of 4.6 N of caustic soda was added to make 19 l of aqueous solution. The aqueous solution was heated to 30 ° C. to 40 ° C. and oxidized while blowing air at a flow rate of 200 l / min to precipitate α-FeOOH powder having a needle shape of 0.5 μm long axis and 0.09 μm short axis. Electron micrograph showing the shape of the powder.) The metal containing manganese was reduced by washing this α-FeOOH for 2 hours at a temperature of 700 ℃ or less in an electric furnace of a hydrogen atmosphere having a flow rate of 1 l / min after washing with water. A powder was obtained. The oxidation resistance of the magnetic powder was oxidized in an air atmosphere at 40 ° C including water vapor having a dew point of 40 ° C.

[실시예 2]Example 2

철 9mole을 함유한 황산제1철, 망간 0.05mole을 함유한 황산망간과 구리 0.05mole을 함유한 황산구리로 만든 10l의 수용액에 4.6N의 가성소다 수용액 9l를 첨가하여 19l의 수용액을 만들었다. 이하 실시예 1과 같은 방법으로 망간과 구리를 함유한 금속분말을 제조하였으며 내산화 특성을 측정한 결과는 제2도에 도시하였다.19 l of an aqueous solution of 4.6 N of caustic soda was added to a 10 l aqueous solution made of ferrous sulfate containing 9 mole of iron, manganese sulfate containing 0.05 mole of manganese, and copper sulfate containing 0.05 mole of copper. Hereinafter, a metal powder containing manganese and copper was prepared in the same manner as in Example 1, and the results of measuring oxidation resistance are shown in FIG. 2.

[실시예 3]Example 3

철 9mole을 함유한 황산제1철, 망간 0.05mole을 함유한 황산망간과 아연 0.005mole을 함유한 황산아연로 만든 10l의 수용액에 4.6N의 가성소다 수용액 9l을 첨가하여 19l의 수용액을 만들었다. 이하 실시예 1과 같은 방법으로 망간과 아연을 함유한 금속분말을 제조하였으며 내산화특성을 측정한 결과는 제2도에 도시하였다.9 l aqueous solution of 4.6 N of caustic soda was added to a 10 l aqueous solution made of ferrous sulfate containing 9 mole of iron, manganese sulfate containing 0.05 mole of manganese, and zinc sulfate containing 0.005 mole of zinc. Hereinafter, a metal powder containing manganese and zinc was prepared in the same manner as in Example 1, and the results of measuring oxidation resistance are shown in FIG. 2.

[비교예][Comparative Example]

철 9mole을 함유한 황산제1철로 만든 10l의 수용액에 4.6N의 가성소다 수용액 9l를 첨가하여 19l의 수용액을 만들었다. 이하 실시예 1과 같은 방법으로 금속분말을 제조하였으며 내산화특성을 측정한 결과는 제2도에 도시하였다.19 l of an aqueous solution of 4.6 N of caustic soda was added to 10 l of an aqueous solution of ferrous sulfate containing 9 mole of iron. Hereinafter, a metal powder was prepared in the same manner as in Example 1, and the results of measuring oxidation resistance are shown in FIG. 2.

이상에서 자기기록용 금속분말의 내산화특성이 비교예의 것보다 실시예의 내산화특성이 월등히 좋다는 것을 알 수 있다. 금속(합금)자성분말에 Mn이나 Cu나 Zn을 함유한 Mn합금을 첨가시킴으로써 금속자성분말의 내식특성을 월등히 향상시킬 수 있는 우수한 효과가 있음을 제2도에서 확인할 수 있다.As mentioned above, it can be seen that the oxidation resistance of the magnetic recording metal powder is much better than that of the comparative example. It can be seen from FIG. 2 that the addition of Mn, Cu or Zn-containing Mn alloy to the metal (alloy) magnetic powder has an excellent effect of significantly improving the corrosion resistance of the metal magnetic powder.

Claims (3)

Fe++를 함유하고 있는 황산철수용액에 0.01원자% 내지 2원자%의 Mn++을 함유하고 황산망간 수용액을 혼합한 혼합수용액에 4.6N의 가성소다 수용액을 첨가한 후 200ml/분의 유속의 공기로 공기 산화시키고, 탈수, 환원시켜서 된 자기기록용 금속자성분말을 제조하는 방법.200 ml / min flow rate after adding 4.6 N caustic soda solution to a mixed solution containing 0.01 to 2 atomic% Mn ++ in a solution of ferrous sulfate containing Fe ++ and a mixed solution of manganese sulfate A method for producing magnetic magnetic powder for magnetic recording obtained by air oxidation, dehydration and reduction with air. Fe++를 함유하고 있는 황산철수용액에 0.01원자% 내지 2원자%의 Mn++과 0.01원자% 내지 1원자 Cu++를 함유하고 있는 황산망간과 황산구리의 혼합수용액을 혼합한 혼합수용액에 4.6N의 가성소다 수용액을 첨가한 후 200ml/분의 유속의 공기로 공기 산화시키고, 탈수, 환원시켜서 된 자기기록용 금속자성분말을 제조하는 방법.4.6 in a mixed aqueous solution of a mixed solution of manganese sulfate and copper sulfate containing 0.01 to 2 atomic% Mn ++ and 0.01 to 1 atomic Cu ++ in an iron sulfate solution containing Fe ++ . A method of producing magnetic magnetic powder for magnetic recording obtained by adding N aqueous solution of caustic soda, followed by air oxidation with air at a flow rate of 200 ml / min, dehydration and reduction. Fe++를 함유하고 있는 황산철수용액에 0.01원자% 내지 2원자%의 Mn++과 0.01원자% 내지 1원자 Zn++를 함유하고 황산망간과 황산아연의 혼합수용액을 혼합한 혼합수용액에 4.6N의 가성소다 수용액을 첨가한 후 200ml/분의 유속의 공기로 공기 산화시키고, 탈수, 환원시켜서 된 자기기록용 금속자성분말을 제조하는 방법.4.6 to a mixed aqueous solution containing 0.01 to 2 atomic% Mn ++ and 0.01 to 1 atomic Zn ++ in a solution of iron sulfate containing Fe ++ and a mixed solution of manganese sulfate and zinc sulfate A method of producing magnetic magnetic powder for magnetic recording obtained by adding N aqueous solution of caustic soda, followed by air oxidation with air at a flow rate of 200 ml / min, dehydration and reduction.
KR1019860003057A 1986-04-21 1986-04-21 Making process for magnetic metal powder KR900000272B1 (en)

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