KR20000046248A - Alloy powder of copper-cobalt-iron and preparing method thereof - Google Patents

Alloy powder of copper-cobalt-iron and preparing method thereof Download PDF

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KR20000046248A
KR20000046248A KR1019980062925A KR19980062925A KR20000046248A KR 20000046248 A KR20000046248 A KR 20000046248A KR 1019980062925 A KR1019980062925 A KR 1019980062925A KR 19980062925 A KR19980062925 A KR 19980062925A KR 20000046248 A KR20000046248 A KR 20000046248A
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alloy powder
cobalt
iron
copper
powder
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KR1019980062925A
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KR100305329B1 (en
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정인범
홍경표
이병윤
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배창환
주식회사 창성
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0425—Copper-based alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/01—Reducing atmosphere

Abstract

PURPOSE: An alloy powder of copper-cobalt-iron and a preparing method thereof are provided to make simple preparing processes, to sinter at low temperature and to obtain uniform particle distribution and fine sintered form. CONSTITUTION: An alloy powder of copper-cobalt-iron is composed of less than 30wt% of cobalt, from 10wt% to 40wt% of iron, from 40wt% to 70wt% of copper and less than 3wt% of impurities. Cobalt chloride(CoCl2), copper nitric acid(Cu(No3)3) and iron chloride(FeCl3) are mixed in solution state. The mixed solution is reacted to oxalic acid solution to deposit into oxalate. The deposited oxalate is dehydrated, cleansed and dried at from 100°C to 120°C. The dried oxalate is reduced at from 500°C to 580°C in a reducing furnace and then milled.

Description

구리-코발트-철 합금 분말 및 그 제조방법Copper-cobalt-iron alloy powder and its manufacturing method

본 발명은 Cu-Co-Fe 합금 분말에 관한 것으로, 보다 상세하게는 제조 공정이 간단하고 소결시 균일한 입자 분포와 미세한 소결 조직을 나타내며, 낮은 온도에서도 소결가능한 Cu-Co-Fe 합금 분말 및 그 제조방법에 관한 것이다.The present invention relates to a Cu-Co-Fe alloy powder, and more particularly, to a Cu-Co-Fe alloy powder and its sinterable at low temperatures, the manufacturing process is simple and shows a uniform particle distribution and fine sintered structure during sintering It relates to a manufacturing method.

일반적으로, 석재의 절단 및 가공, 콘크리트와 아스팔트의 절단, 건축물 철거시 등에 사용되는 다이아몬드 공구는 다이아몬드 입자와 금속 합금 분말을 혼합하여 흑연 몰드에서 열과 압력을 동시에 가하는 핫 프레스(Hot Press) 공정에 의해 제작되며, 다이아몬드 공구에 사용되는 금속 분말은 Co, Fe, Ag, Zn, 청동(Bronze)등이 혼합사용된다.In general, diamond tools used for cutting and processing stone, cutting concrete and asphalt, and demolition of buildings are made by a hot press process in which graphite particles and metal alloy powder are mixed to simultaneously apply heat and pressure in a graphite mold. Co, Fe, Ag, Zn, Bronze, etc. are mixed and used as a metal powder used for diamond tools.

다이아몬드 공구에서 금속 분말은 다이아몬드 지립(砥粒)을 잡아주는 결합재로 금속분말 본드의 역할을 수행한다.In diamond tools, metal powder acts as a metal powder bond as a binder for diamond abrasive grains.

이러한 다이아몬드 공구용 금속분말은 다이아몬드 지립의 양호한 보지력(保持力), 강도와 연성의 적절한 결합, 다이아몬드 크기/농도와 작업 조건에 따른 마모율 제어, 높은 내식성 등의 기본 성질을 갖추는 것이 필요하다.Such metal powders for diamond tools need to have basic properties such as good holding strength of diamond abrasive grains, proper combination of strength and ductility, wear rate control according to diamond size / concentration and working conditions, and high corrosion resistance.

그러나, 다이아몬드 공구에 사용되는 금속분말로 Co, Fe, Cu, Sn, Ag, Ni, W, WC 등을 혼합사용하여 다이아몬드 공구를 제조하면, 공구의 기저 조직에 혼합 정도에 따라 편석이 존재하며, 혼합된 금속 분말의 크기가 Co: 1∼3㎛, Fe: 4∼7㎛, Ni: 4∼7㎛, 청동(Bronze): 20∼40㎛, Cu: 20∼40㎛으로 각각 상이하여 미세하고 균일한 소결 조직을 얻는 것이 곤란하다.However, when a diamond tool is manufactured by mixing Co, Fe, Cu, Sn, Ag, Ni, W, WC, etc. as a metal powder used in a diamond tool, segregation exists in the base structure of the tool depending on the degree of mixing. The sizes of the mixed metal powders are fine, Co: 1 to 3 µm, Fe: 4 to 7 µm, Ni: 4 to 7 µm, Bronze: 20 to 40 µm, Cu: 20 to 40 µm, respectively. It is difficult to obtain a uniform sintered structure.

또한, 혼합된 금속 분말을 사용하여 다이아몬드 공구를 제조하기 위해서는 금속 분말을 혼합하기 위한 별도의 공정이 필요하다.In addition, in order to manufacture diamond tools using the mixed metal powder, a separate process for mixing the metal powder is required.

더욱이, 다이아몬드 공구로서의 기본 성질을 확보하기 위해서는 혼합된 금속 분말을 800∼1000℃의 온도에서 소결하여야 하는데, 900℃ 이상의 온도에서는 다이아몬드의 탄화를 발생하는 문제가 있다.Furthermore, in order to secure basic properties as a diamond tool, the mixed metal powder should be sintered at a temperature of 800 to 1000 ° C., but there is a problem that carbonization of diamond occurs at a temperature of 900 ° C. or more.

그리고 금속분말중 사용량이 가장 많은 코발트(Co) 분말은 가격이 높고 수급이 불안정한 문제가 있었다.In addition, the cobalt (Co) powder, which is used the most among the metal powders, has high price and unstable supply and demand.

본 발명은 상기 설명한 종래 문제점을 해결하기 위하여 이루어진 것으로,가격이 저렴한 Cu, Fe 등의 금속 성분을 Co 와 함께 화학적으로 합금화하여 제조함으로써 다이아몬드 공구에 적용시 금속 조직 성질이 우수한 Cu-Co-Fe 합금 분말 및 그 제조방법을 제공함에 그 목적이 있다.The present invention has been made to solve the above-described problems, Cu-Co-Fe alloy having excellent metal structure properties when applied to diamond tools by producing a metal alloy, such as low-cost Cu, Fe chemically alloyed with Co It is an object to provide a powder and a method for producing the same.

도 1 은 본 발명의 Co-Cu-Fe 합금 분말의 제조공정을 나타내는 도면이다.BRIEF DESCRIPTION OF THE DRAWINGS It is a figure which shows the manufacturing process of the Co-Cu-Fe alloy powder of this invention.

상기 목적을 달성하기 위한 본 발명의 Cu-Co-Fe 합금 분말은, 중량%로, Co: 30% 이하, Fe: 10∼40%, Cu: 40∼70%, 및 3% 이하의 불순물 성분을 포함하여 이루어진다.Cu-Co-Fe alloy powder of the present invention for achieving the above object, by weight%, Co: 30% or less, Fe: 10-40%, Cu: 40-70%, and 3% or less of impurity components It is made to include.

또한, 본 발명의 Cu-Co-Fe 합금 분말 제조방법은, 염화코발트, 질산구리 및 염화철 용액을 제조하여 용액 상태로 혼합후, 옥살레이트(Dxalate)염으로 침전시키기 위하여 상기 혼합 용액을 수산용액에 투입하여 반응시킨후, 침전된 옥살레이트염을 탈수,세척후, 100∼120℃ 온도에서 건조시키며, 건조된 옥살레이트염을 환원로에서 500∼580℃ 온도에서 환원분위기에서 환원하고, 분쇄하여 제조하는 구성이다.In addition, in the method for preparing Cu-Co-Fe alloy powder of the present invention, a cobalt chloride, copper nitrate and iron chloride solution are prepared and mixed in a solution state, and then the mixed solution is added to an aqueous solution in order to precipitate with oxalate (Dxalate) salt. After the reaction, the precipitated oxalate salt is dehydrated and washed, dried at 100-120 ° C., and the dried oxalate salt is reduced in a reducing atmosphere at a temperature of 500-580 ° C. in a reduction furnace, and then pulverized. It is a constitution.

이하에서는 양호한 실시예와 관련하여 본 발명을 설명한다.The invention is described below in connection with the preferred embodiment.

본 발명의 일 태양으로서의 Co-Cu-Fe 합금 분말은, 중량%로, Co: 30% 이하, Fe: 10∼40%, Cu: 40∼70%, 및 3% 이하의 불순물 성분을 포함하여 이루어진다.Co-Cu-Fe alloy powder as one embodiment of the present invention, by weight%, Co: 30% or less, Fe: 10 to 40%, Cu: 40 to 70%, and 3% or less of impurity components .

본 발명에 의한 합금 분말은 가격이 저렴한 Cu 및 Fe 성분을 각각 40∼70 중량% 및 10∼40 중량% 함유하며, 가격이 높은 Co 성분을 30 중량% 이하 함유함을 특징으로 하는데, 이러한 성분 범위는 소재의 가격을 저하시키고, 다이아몬드 공구 등에 사용할 때 적절한 강도와 연성을 부여하고 높은 내식성을 부여하기 위하여 조성 범위가 선정된다.The alloy powder according to the present invention is characterized by containing 40 to 70% by weight and 10 to 40% by weight of inexpensive Cu and Fe components, respectively, and containing 30% by weight or less of the high cost Co component. The composition range is selected in order to lower the price of the material, to impart proper strength and ductility and to provide high corrosion resistance when used in diamond tools and the like.

또한, 상기와 같은 조성의 다이아몬드 공구용 Co-Cu-Fe합금 분말의 제조 방법은 다음과 같다.In addition, the manufacturing method of the Co-Cu-Fe alloy powder for diamond tools of the above composition is as follows.

도 1 도시와 같이, 우선 Co, Cu, Fe 금속을 산에 용해하여 염화코발트, 질산구리, 및 염화철의 용액을 각각 제조한다.As shown in FIG. 1, first, Co, Cu, Fe metals are dissolved in an acid to prepare a solution of cobalt chloride, copper nitrate, and iron chloride, respectively.

얻어진 각각의 용액을 여과하여 금속염 용액을 얻으며, 얻어진 금속염용액을 목표 중량비의 합금 분말을 얻도록 혼합한다.Each obtained solution is filtered to obtain a metal salt solution, and the obtained metal salt solution is mixed to obtain an alloy powder of a target weight ratio.

이어서, 수산용액에 투입하여 옥살레이트(Oxalate)염으로 침전시킨다.Subsequently, it is added to an aqueous solution and precipitated with an oxalate salt.

다음에 침전된 옥살레이트염을 탈수, 세척처리후 건조로에서 100∼120℃ 온도 범위에서 건조하는데, 120℃ 보다 높은 온도에서는 옥살레이트염의 변화가 발생하므로 상한 온도를 120℃로 한다.Next, the precipitated oxalate salt is dried at a temperature range of 100 to 120 ° C. in a drying furnace after dehydration and washing. However, at a temperature higher than 120 ° C., a change in the oxalate salt occurs, so the upper limit temperature is 120 ° C.

건조한 옥살레이트염을 이어서 롤 밀(Roll Mill)로 분쇄후에 환원로에서 500∼580℃ 온도 조건 및 수소와 질소의 혼합가스 분위기에서 환원시키는데, 500℃ 이상에서는 열분해가 완전히 발생하며 580℃ 이하에서는 소착이 심화되므로 온도 범위를 500∼580℃ 로 한정한다.The dry oxalate salt is then crushed into a roll mill and reduced in a reducing furnace at 500 to 580 ° C. temperature conditions and a mixed gas atmosphere of hydrogen and nitrogen. Pyrolysis occurs completely above 500 ° C. and sinters below 580 ° C. Since it deepens, the temperature range is limited to 500-580 degreeC.

이어서, 볼 밀(Ball Mill)로 분쇄하여 합금 분말을 제조한다.Subsequently, an alloy powder is prepared by grinding in a ball mill.

필요에 따라 제조된 분말을 검사한 후에 포장하여 합금 분말의 제조를 완료한다.If necessary, the prepared powder is inspected and then packaged to complete the preparation of the alloy powder.

이하에서는 실시예와 관련하여 본 발명을 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail with reference to Examples.

실시예Example

염화코발트(CoCl2) 용액 8.57ℓ(Co 1001g), 질산구리{Cu(NO3)3} 용액 12.9ℓ(Cu 1435g),염화철(FeCl3)용액 20.1ℓ(Fe 2555g)의 혼합금속염 용액을 반응조에서 24℃의 수산용액 170ℓ(수산 16,100g)에 균일 속도로 35 분간 투입하여 수산용액과 반응시켰다.Cobalt chloride (CoCl 2) solution 8.57ℓ (Co 1001g), copper nitrate {Cu (NO 3) 3} solution 12.9ℓ (Cu 1435g), a mixed metal salt solution of iron chloride (FeCl 3) solution 20.1ℓ (Fe 2555g) Reactor Was added to 170 L (16,100 g) of aquatic solution at 24 ° C. for 35 minutes at a uniform rate to react with the aquatic solution.

침전된 옥살레이트염을 탈수후 3회 세척을 실시하며, 이어서 건조 오븐에서 110℃에서 24hr 건조시킨후에 벨트 환원로에서 550℃, H215%-N285% 분위기에서 4hr 열분해하였다.The precipitated oxalate salt was washed three times after dehydration, and then dried for 24 hours at 110 ° C. in a drying oven, and then pyrolyzed at 550 ° C. and H 2 15% -N 2 85% in a belt reducing furnace for 4 hours.

열분해된 분말을 볼밀로 8hr 분쇄하여 Cu-Co-Fe 합금 분말을 제조하였다.The pyrolyzed powder was milled by a ball mill for 8hr to prepare a Cu-Co-Fe alloy powder.

성분 분석 결과, Cu: 54.6 중량%, Co: 23.7 중량%, Fe: 20.8 중량% 및 불순물 0.9 중량%의 Co-Cu-Fe 합금 분말을 얻었다.As a result of the component analysis, Co-Cu-Fe alloy powder having 54.6 wt% Cu, 23.7 wt% Co, 20.8 wt% Fe, and 0.9 wt% impurities was obtained.

분말 특성은 다음과 같았다.Powder properties were as follows.

분말 특성 - 겉보기 밀도 : 1.74g/㎤Powder Properties-Apparent Density: 1.74g / cm3

- 탭(Tap) 밀도: 3.23g/㎤Tap density: 3.23 g / cm 3

- 피셔 평균 입경(Fisher Sub-Sieve Size:FSSS): 2.4㎛Fischer Sub-Sieve Size (FSSS): 2.4㎛

핫 프레스(Hot Press) 소결 특성을 300㎏f 가압력으로 120 초간 소결한 후 측정한 바, 표 1 과 같다.The hot press sintering characteristics were measured after sintering at 300 kgf for 120 seconds and the results are as shown in Table 1.

No.No. 소결온도 (℃)Sintering Temperature (℃) 수축율(%)Shrinkage (%) 경 도Hardness 항절력(㎏f/㎟)Drag force (kgf / mm2) HRB HR B HRC HR C 1One 650650 95.795.7 101.5101.5 26.526.5 132132 22 700700 96.496.4 107.7107.7 29.629.6 136136 33 750750 96.596.5 106.3106.3 29.629.6 145145 44 800800 97.297.2 106.0106.0 28.228.2 148148

비교예Comparative example

표 2 에 나타낸 바와같은 Cu 분말, Fe 분말, EF Co 분말을 3차원 믹서(Mixer)를 사용하여 1시간 혼합하여 Co-Cu-Fe 혼합 분말을 제조하고, 소결 특성을 300㎏f 가압력으로 120 초간 소결한 후 측정하여 표 3 에 나타내었다.Cu powder, Fe powder, EF Co powder as shown in Table 2 was mixed for 1 hour using a three-dimensional mixer (Mixer) to prepare a Co-Cu-Fe mixed powder, and the sintering characteristics for 300 seconds at a pressure of 300 kgf After sintering, it was measured and shown in Table 3.

소결특성을 조사한 바, 비교예의 각각의 Co분말, Cu분말과 Fe 분말을 혼합하여 제조한 경우 소결 특성이 HRB의 경우 본 발명에 비해 휠씬 낮은 수치를 나타냈으며, HRc는 비교예의 경우는 측정할 수 없었다. 또한, 항절력의 평가에 의하면 일반적으로 본발명의 경우 보다 낮은 수치를 나타내었다.When the sintering characteristics were investigated, the Co powder, Cu powder, and Fe powder of the comparative example were prepared by mixing, and the sintering characteristics of HR B were much lower than those of the present invention, and HRc was measured in the comparative example. Could not. In addition, according to the evaluation of the pull force, the numerical value was lower than that of the present invention.

구 분division 조 성(중량%)Composition (% by weight) 사 용 분 말Powder FSSS(㎛)FSSS (μm) CuFeCoCuFeCo 54.821.224.054.821.224.0 전해동카보닐철EF CoElectrolytic Copper Carbonyl Iron EF Co 6.454.501.406.454.501.40

No.No. 소결온도 (℃)Sintering Temperature (℃) 수축율(%)Shrinkage (%) 경 도Hardness 항절력(㎏f/㎟)Drag force (kgf / mm2) HRB HR B HRcHRc 1One 650650 90.490.4 56.956.9 측정불가Not measurable 7171 22 700700 93.993.9 63.463.4 측정불가Not measurable 8484 33 750750 95.895.8 69.269.2 측정불가Not measurable 118118 44 800800 98.098.0 73.673.6 측정불가Not measurable 139139

본 발명에 따라 제조된 Cu-Co-Fe 합금 분말은 1∼3㎛ 크기의 미세한 분말로 제조되어 핫 프레스(Hot Press) 적용 소결시 균일한 입자 분포와 미세한 소결 조직을 나타내어 HRc ≥25, 소결밀도≥95%(진밀도 대비)의 기계적 특성을 얻었으며, Cu, Co, Fe 분말을 각각 혼합하여 제조함에 비해 공정이 휠씬 단순하고, Cu-Co-Fe 합금 분말의 소결 온도 구역이 600∼900℃로 낮은 온도에서도 소결가능하여 다이아몬드 공구 등 공구 소재로 유용하다.Cu-Co-Fe alloy powder prepared according to the present invention is made of a fine powder of 1 ~ 3㎛ size shows a uniform particle distribution and a fine sintered structure during hot press applied sintering HRc ≥ 25, sintered density Mechanical properties of ≥95% (compared to true density) are obtained, and the process is much simpler than that of mixing Cu, Co, and Fe powders respectively, and the sintering temperature range of Cu-Co-Fe alloy powder is 600 to 900 ° C. It is sinterable even at low temperatures, making it useful for tool materials such as diamond tools.

Claims (2)

염화코발트, 질산구리 및 염화철 용액을 제조하여 용액 상태로 혼합후, 옥살레이트(Dxalate)염으로 침전시키기 위하여 상기 혼합 용액을 수산용액에 투입하여 반응시킨후, 침전된 옥살레이트염을 탈수,세척후, 100∼120℃ 온도에서 건조시키며, 건조된 옥살레이트염을 환원로에서 500∼580℃ 온도에서 환원분위기에서 환원하고, 분쇄하여 제조한 것을 특징으로 하는 Cu-Co-Fe 합금 분말의 제조방법.Cobalt chloride, copper nitrate and iron chloride solutions are prepared and mixed in solution, and then the mixed solution is added to an aqueous solution to react with oxalate salt, followed by dehydration and washing of the precipitated oxalate salt. And drying at 100 to 120 ° C., reducing the dried oxalate salt in a reducing atmosphere at a temperature of 500 to 580 ° C. in a reduction furnace, and pulverizing to produce the Cu-Co-Fe alloy powder. 청구항 1항의 제조방법에 의하여 제조되며, 중량%로, Co:30% 이하, Cu:40∼70%, Fe:10∼40% 및 3% 이하의 불순물 성분으로 이루어진 것을 특징으로 하는 Cu-Co-Fe 합금 분말.It is prepared by the manufacturing method of claim 1, Cu-Co- characterized in that by weight, consisting of impurity components of 30% or less, Cu: 40 to 70%, Fe: 10 to 40% and 3% or less. Fe alloy powder.
KR1019980062925A 1998-12-31 1998-12-31 Cu-Co-Fe alloy powder and its manufacturing method KR100305329B1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100483169B1 (en) * 2002-05-24 2005-04-14 삼성코닝 주식회사 Method for the preparation of multielement-based metal oxide powders
CN109702217A (en) * 2019-03-04 2019-05-03 江苏萌达新材料科技有限公司 A kind of iron cobalt-copper alloy powder and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100483169B1 (en) * 2002-05-24 2005-04-14 삼성코닝 주식회사 Method for the preparation of multielement-based metal oxide powders
CN109702217A (en) * 2019-03-04 2019-05-03 江苏萌达新材料科技有限公司 A kind of iron cobalt-copper alloy powder and preparation method thereof

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