CN108994308B - A kind of preparation method of low-apparent-density atomization nickel powder - Google Patents

A kind of preparation method of low-apparent-density atomization nickel powder Download PDF

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Publication number
CN108994308B
CN108994308B CN201810887603.6A CN201810887603A CN108994308B CN 108994308 B CN108994308 B CN 108994308B CN 201810887603 A CN201810887603 A CN 201810887603A CN 108994308 B CN108994308 B CN 108994308B
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atomization
nickel powder
apparent
density
low
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CN108994308A (en
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宋谋通
何子川
龚继宝
王文鹏
陈国栋
冯泽树
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Jinchuan Group Nickel Cobalt Co ltd
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Jinchuan Group Co Ltd
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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
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • 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
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • B22F1/145Chemical treatment, e.g. passivation or decarburisation
    • 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
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0824Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
    • 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
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps

Abstract

The invention discloses a kind of preparation method of low-apparent-density atomization nickel powder, the atomization nickel powder of this method production, apparent density 2.0-2.2g/cm3, granularity D50 is at 8-10 microns, and nickel content is greater than 99.7%, and oxygen content is less than 0.3%.It is filled with domestic market water atomization nickel powder pine close generally in 3.5-4.0 g/cm3It compares, apparent density reduces 1.5-1.8 g/cm3, the present invention overcomes the nickel powder apparent density height of traditional atomization process production, the disadvantages of formability difference;Present invention process process is short, production cost is low, generates without pernicious gas;Product can be widely used for powder metallurgy mechanical parts, diamond tool, conducting resinl industry.

Description

A kind of preparation method of low-apparent-density atomization nickel powder
Technical field
The invention belongs to field of metallurgy, are related to nickel powder, in particular to a kind of preparation method of low-apparent-density atomization nickel powder.
Background technique
Although being atomized legal system powder has that process is short, production cost is low, the advantages such as environmentally friendly, the nickel powder particle that atomization is produced Pattern irregular shape, surface is smooth, and product apparent density is excessive, typically greater than 3.5g/cm3, powder forming is poor, with it is other After powder mixes powder, it is segregated transport, compacting, charging process are all different degrees of, influences using effect.
Summary of the invention
The purpose of the present invention is to problems of the prior art, a kind of low-apparent-density atomization nickel powder is provided Preparation method.
Technical solution of the present invention is as follows: a kind of preparation method of low-apparent-density atomization nickel powder, specific to wrap Include following steps:
Step a is melted sheet nickel using mid-frequency melting furnace, using charcoal deoxidation, when melt temperature is up to 1650 DEG C, Start to be atomized, atomization condition: atomizing medium is the oxalic acid solution of 8-10g/L, and 1650 DEG C of atomization temperature, protective gas argon gas leaks Eyelet diameter 4.0mm is atomized hydraulic pressure 80Mpa;
Nickel powder after step b atomization is separated by solid-liquid separation through filters pressing, and the nickel powder after being filtered dry is added in the container of stainless steel directly It is mixed evenly with mass percent for the industrial acetic acid of 36-38%, nickel powder and industrial acetic acid mass ratio are 20:1, and container adds Lid sealing 90-120 minutes, makes nickel powder surface roughening;
Step c opens container, will be mixed with wet-milling dry reduction in drying, reduction all-in-one oven of acetic acid, dryer section temperature 300 DEG C of degree, 300-450 DEG C of reduction section temperature, dry, recovery time 2.5-3.0 hour;
Step d. is broken to be broken up, sieves, and apparent density 2.0-2.2g/cm is both obtained3, at 8-10 microns, nickel contains granularity D50 Amount is greater than 99.7%, the atomization nickel powder of low-apparent-density of the oxygen content less than 0.3%.
Preferably, sheet nickel is melted using mid-frequency melting furnace in step a, using wood when temperature reaches 1580 DEG C Charcoal deoxidation.
Preferably, the oxalic acid solution of atomizing medium 8-10g/L is prepared using industrial pure water in step a.
Further, in step a, atomizing medium oxalic acid solution is recycled, and atomization ensures oxalic acid content in 8- every time Within the scope of 10g/L.
Further, in step c, reducing atmosphere is nitrogen, the hydrogen mixed gas after ammonolysis craft.
Preferably, in step c, 300 DEG C of dryer section temperature, 350 DEG C -400 DEG C of reduction section temperature.
Compared with the prior art, the advantages of the present invention are as follows:
Atomization process of the invention has argon gas protection, and atomizing medium is the oxalic acid solution of low concentration, it is ensured that atomization process Nickel surface No oxided film generate, for acetic acid be roughened powder surface create conditions and modified with organic acids be atomized nickel powder premise;Match The atomized water that oxalic acid processed uses prevents calcium ions and magnesium ions content height in water from causing calcium oxalate precipitation, influences into quality for industrial pure water Amount.For the present invention using acetic acid roughening Fine Nickel Powder surface, advantage is that the nickel powder after impregnating without washing, is directly entered dry go back Former all-in-one oven, non-wastewater discharge;The present invention enters high temperature reduction, and residue is decomposed into carbon dioxide and water vapour, to product and Environment is pollution-free.The fine low-apparent-density nickel powder for the water atomization technique production that the present invention uses, apparent density 2.0- 2.2g/cm3, granularity D50 is at 8-10 microns, and nickel content is greater than 99.7%, and oxygen content is less than 0.3%.Powder forming is good, the present invention Generally existing pine fills close 3.5-4.0 g/cm with existing market3Water atomization nickel powder compare, nickel powder of the invention and other powder Be not in segregation in transport, compacting, charging process after the mixed powder in end, overcome the nickel powder pine dress of traditional atomization process production Density is high, and formability is poor, mixes the problem of being easily segregated after powder with other powder.The atomization nickel produced using technique of the invention Powder reduces apparent density, and process flow is short, production cost is low, generates without pernicious gas, and product can be satisfied with powder metallurgy Component of machine, diamond tool, conducting resinl industry use, and that widens atomization nickel powder uses field.
Specific embodiment
A kind of production method of low-apparent-density atomization nickel powder, specifically includes the following steps:
Step a. is melted sheet nickel using mid-frequency melting furnace, using charcoal deoxidation when temperature reaches 1580 DEG C;
The preparation of step b. oxalic acid solution: dosage is that every cubic meter of water adds 8-10 kilograms of oxalic acid, is slowly uniformly added into band and stirs It mixes in tank, guarantees that oxalic acid sufficiently dissolves, above-mentioned prepared using industrial pure water ensures the oxalic acid content prepared in 8-10g/L range It is interior;
Step c. atomization: when nickel melt temperature starts to be atomized up to 1650 DEG C in furnace, atomization technique condition: atomizing medium is The solution of the 8-10g/L containing oxalic acid, 1650 DEG C of atomization temperature, protective gas argon gas leaks eyelet diameter 4.0mm, and (leakage eye is by high temperature nickel Liquid stream enters the diversion pipe of atomizer, and pore size influences powder size composition very big) atomization hydraulic pressure 80Mpa.
Step d. nickel powder roughing in surface: the nickel powder after atomization is separated by solid-liquid separation through filters pressing, and nickel powder is packed into stainless steel The industrial acetic acid for being directly 36% with mass content in cylinder mixes, and the mass ratio of nickel powder and industrial acetic acid is 20:1, is stirred Capping, Sealing period are not less than 1.5 hours after even, make nickel powder surface roughening;
Step e. opens cylinder, and the wet-milling that acetic acid is mixed in cylinder is taken out, and is added directly into the dry reduction all-in-one oven of steel band Reduction, is dried, restores, reduction technique condition are as follows:
Reducing atmosphere: for nitrogen, the hydrogen mixed gas after ammonolysis craft;
Dryer section temperature: 300 DEG C
Reduction section temperature: 300-450 DEG C
Dry, recovery time 2.5-3.0 hour
Step f. is broken to be broken up, crosses the screening of 300 meshes to get low-apparent-density atomization nickel powder of the invention is arrived.Broken, Screening process should try to control crushing temperature, prevent thermal oxide, cause oxygen content higher, once oxidation oxygen content is exceeded, need It to restore, but product apparent density be influenced little again.
Low-apparent-density obtained above is atomized nickel powder: apparent density 2.0-2.2g/cm3, granularity D50 at 8-10 microns, Nickel content is greater than 99.7%, the atomization nickel powder of low-apparent-density of the oxygen content less than 0.3%.
Embodiment 1
A kind of production method of low-apparent-density atomization nickel powder, specifically includes the following steps:
Intermediate frequency furnace fusing, heating, deoxidation is added in the blocky electrolytic nickel of step a) .100 kilogram;
The preparation of step b) oxalic acid solution: atomization oxalic acid solution medium, oxalic acid solution mass concentration 9.5g/L are prepared;
Step c) atomization: atomizing pressure 80MPa, leaks eyelet through 4.0mm by 1650 DEG C of atomization temperature;
Step d) nickel powder roughing in surface: the nickel powder after atomization is separated by solid-liquid separation through filters pressing, uses mass percent for 36% Industrial acetic acid, nickel powder and sour mass ratio 20:1, after being uniformly mixed, the sealed soak time 100 minutes;
Step e) is dry, reduction, is crushed, screening, 300 DEG C of drying temperature, 450 DEG C of reduction temperature, the dry recovery time 3.0 hour;300 meshes are crossed after broken, lower sieve is required product.
Technical target of the product is as shown in table 1,
1. low-apparent-density of table is atomized nickel powder the key technical indexes.
Embodiment 2
A kind of production method of low-apparent-density atomization nickel powder, specifically includes the following steps:
Intermediate frequency furnace fusing, heating, deoxidation is added in the blocky electrolytic nickel of step a) .100 kilogram;
The preparation of step b) oxalic acid solution: atomization oxalic acid solution medium, oxalic acid solution mass concentration 9.8g/L are prepared;
Step c) atomization: atomizing pressure 80MPa, leaks eyelet through 4.0mm by 1650 DEG C of atomization temperature;
Step d) nickel powder roughing in surface: the nickel powder after atomization is separated by solid-liquid separation through filters pressing, uses mass percent for 36% Industrial acetic acid, nickel powder and sour mass ratio 20:1, after being uniformly mixed, the sealed soak time 110 minutes;
Step e) is dry, reduction, is crushed, screening, 300 DEG C of drying temperature, 450 DEG C of reduction temperature, the dry recovery time 3.0 hour;300 meshes are crossed after broken, lower sieve is required product.
Technical target of the product is as shown in table 2,
2. low-apparent-density of table is atomized nickel powder the key technical indexes.
Embodiment 3
A kind of production method of low-apparent-density atomization nickel powder, specifically includes the following steps:
Intermediate frequency furnace fusing, heating, deoxidation is added in the blocky electrolytic nickel of step a) .100 kilogram;
The preparation of step b) oxalic acid solution: atomization oxalic acid solution medium, oxalic acid solution mass concentration 10g/L are prepared;
Step c) atomization: atomizing pressure 80MPa, leaks eyelet through 4.0mm by 1650 DEG C of atomization temperature;
Step d) nickel powder roughing in surface: the nickel powder after atomization is separated by solid-liquid separation through filters pressing, uses mass percent for 36% Industrial acetic acid, nickel powder and sour mass ratio 20:1, after being uniformly mixed, the sealed soak time 120 minutes;
Step e) is dry, reduction, is crushed, screening, 300 DEG C of drying temperature, 450 DEG C of reduction temperature, the dry, recovery time 3.0 hour;300 meshes are crossed after broken, lower sieve is required product.
Technical target of the product is as shown in table 3,
3. low-apparent-density of table is atomized nickel powder the key technical indexes.

Claims (5)

1. a kind of preparation method of low-apparent-density atomization nickel powder, it is characterised in that: specifically includes the following steps:
Step a is melted sheet nickel using mid-frequency melting furnace, using charcoal deoxidation, when melt temperature is up to 1650 DEG C, is started Atomization, atomization condition: atomizing medium is the oxalic acid solution of 8-10g/L, and 1650 DEG C of atomization temperature, protective gas argon gas leaks eyelet Diameter 4.0mm is atomized hydraulic pressure 80Mpa;The oxalic acid solution of atomizing medium 8-10g/L is prepared using industrial pure water;
Nickel powder after step b atomization is separated by solid-liquid separation through filters pressing, and nickel powder after being filtered dry is added in the container of stainless steel directly and matter The industrial acetic acid that amount percentage is 36-38% is mixed evenly, and nickel powder and industrial acetic acid mass ratio are 20:1, and container covers close Envelope 90-120 minutes, makes nickel powder surface roughening;
Step c opens container, will be mixed with wet-milling dry reduction in drying, reduction all-in-one oven of acetic acid, dryer section temperature 300 DEG C, 300-450 DEG C of reduction section temperature, dry, recovery time 2.5-3.0 hour;
Step d. is broken to be broken up, sieves, and apparent density 2.0-2.2g/cm is both obtained3, at 8-10 microns, nickel content is greater than granularity D50 99.7%, the atomization nickel powder of low-apparent-density of the oxygen content less than 0.3%.
2. a kind of preparation method of low-apparent-density atomization nickel powder according to claim 1, it is characterised in that: in step a, Sheet nickel is melted using mid-frequency melting furnace, using charcoal deoxidation when temperature reaches 1580 DEG C.
3. a kind of preparation method of low-apparent-density atomization nickel powder according to claim 1, it is characterised in that: in step a, Atomizing medium oxalic acid solution recycles, and atomization ensures oxalic acid content within the scope of 8-10g/L every time.
4. a kind of preparation method of low-apparent-density atomization nickel powder according to claim 1, it is characterised in that: in step c, Reducing atmosphere is nitrogen, the hydrogen mixed gas after ammonolysis craft.
5. a kind of preparation method of low-apparent-density atomization nickel powder according to claim 1, it is characterised in that: in step c, 300 DEG C of dryer section temperature, 350 DEG C -400 DEG C of reduction section temperature.
CN201810887603.6A 2018-08-06 2018-08-06 A kind of preparation method of low-apparent-density atomization nickel powder Active CN108994308B (en)

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JPS6389608A (en) * 1986-10-03 1988-04-20 Taiyo Yuden Co Ltd Production of rare earth magnet alloy powder
JP3414686B2 (en) * 2000-01-07 2003-06-09 大崎工業株式会社 Method for producing nickel powder having resistance to oxidation and sintering
CN1358592A (en) * 2000-12-09 2002-07-17 甘肃雷诺换热设备有限公司 Method for reducing metal powder bulk loading density
CN100484668C (en) * 2004-12-06 2009-05-06 荆门市格林美新材料有限公司 Production method and apparatus for super fine cobalt powder by circulating technology
CN1305617C (en) * 2005-02-06 2007-03-21 金川集团有限公司 Production method of dentritic morphology nickel powder
CN104227007B (en) * 2014-09-17 2016-02-24 北京科技大学 The method of aluminium powder and Al alloy powder is prepared in a kind of water atomization

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Effective date of registration: 20240219

Address after: 737100 No. 2 Lanzhou Road, Beijing Road Street, Jinchuan District, Jinchang City, Gansu Province

Patentee after: Jinchuan Group Nickel Cobalt Co.,Ltd.

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