CN106670489A - Preparing method for spherical high-purity nickel powder - Google Patents

Preparing method for spherical high-purity nickel powder Download PDF

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Publication number
CN106670489A
CN106670489A CN201611064754.9A CN201611064754A CN106670489A CN 106670489 A CN106670489 A CN 106670489A CN 201611064754 A CN201611064754 A CN 201611064754A CN 106670489 A CN106670489 A CN 106670489A
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CN
China
Prior art keywords
purity
nickel oxide
nikel powder
spherical high
nickel
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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
Application number
CN201611064754.9A
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Chinese (zh)
Inventor
许开华
郭苗苗
张云河
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Jingmen GEM New Material Co Ltd
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Jingmen GEM New Material Co Ltd
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Priority to CN201611064754.9A priority Critical patent/CN106670489A/en
Publication of CN106670489A publication Critical patent/CN106670489A/en
Pending legal-status Critical Current

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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
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • 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
    • B22F1/06Metallic powder characterised by the shape of the particles
    • B22F1/065Spherical particles

Abstract

The invention discloses a preparing method for spherical high-purity nickel powder. The preparing method specifically comprises the following steps that firstly, spherical nickelous hydroxide is roasted, and intermediate product nickel oxide is obtained; secondly, the nickel oxide in the first step is washed; thirdly, the nickel oxide washed in the second step is subjected to reducing; and fourthly, the nickel oxide subjected to reducing in the third step is crushed and screened, and the spherical high-purity nickel powder is obtained. According to the preparing method, the spherical nickelous hydroxide serves as a precursor, the content of sodium in the nickel powder is reduced through roasting, washing and reducing parameter setting, and the content of the sodium in the nickel powder is controlled to be below 50 ppm; meanwhile, the nickel powder is in a spherical shape and has good dispersity, AD, FSSS and other indexes are controllable; and in addition, the nickel powder meeting the requirement can be made by adjusting the technology according to different demands.

Description

A kind of preparation method of spherical high-purity nikel powder
Technical field
The invention belongs to metal-powder fabricating technology field, and in particular to a kind of preparation side of spherical high-purity nikel powder Method.
Background technology
Nikel powder is mainly used in coating and plastics make conducting pigment shielding electromagnetic interference and radio frequency interference, makees various high glaze dresses Decorations paint and plastics, replace aluminium powder to make anti-corrosive paint etc. in water-based system, and fine grained globular powdered nickel can be used for electrically conductive ink, purposes ratio It is wide.The mode of production of existing globular powdered nickel, sodium impurity by way of directly washing are difficult to remove, and cause nikel powder after reduction Sodium content it is higher.
The content of the invention
It is an object of the invention to provide a kind of preparation method of spherical high-purity nikel powder, using ball-shape nickel hydroxide as forerunner Body, reduces the content of sodium in nikel powder by the setting of parameter when roasting, washing and reduction.
The technical solution adopted in the present invention is, a kind of preparation method of spherical high-purity nikel powder:
Step 1, roasting ball-shape nickel hydroxide obtain intermediate product nickel oxide;
Step 2, washs to the nickel oxide of the step 1;
Step 3, reduces to the nickel oxide after the step 2 washing;
Step 4, carries out crushing to the nickel oxide after the step 3 reduction and sieves, obtain spherical high-purity nickel powder.
The characteristics of of the invention, also resides in,
In the step 1, the temperature of roasting is 400~600 DEG C.
In the step 1, the time of roasting is 3~5h.
The step 2 kind is washed to nickel oxide with pure water, and washing water temperature is 60~90 DEG C, and water consumption is nickel oxide weight 8~10 times of amount, stirring pulping and washing 3 times, filter after washing, and then dry at 100 DEG C again.
In the step 3, reduction temperature is 400~550 DEG C.
In the step 3, the recovery time is 3~6h.
In the step 3, boat charge is 5~8kg.
200 eye mesh screens are crossed after Mechanical Crushing is carried out in the step 4.
The invention has the beneficial effects as follows, a kind of preparation method of spherical high-purity nikel powder of the invention, by ball-shape nickel hydroxide As presoma, the content of sodium in nikel powder is reduced by the setting of parameter when roasting, washing and reduction, the sodium in nikel powder is made Content control in below 50ppm, and the pattern of nikel powder is for spherical, controllable with the index such as preferable dispersibility, AD, FSSS, Satisfactory nikel powder can be made according to different demands adjusting process in addition.
Description of the drawings
Fig. 1 provides the electron microscope of the nikel powder prepared in embodiment 1 for the present invention;
Fig. 2 provides the electron microscope of the nikel powder prepared in embodiment 2 for the present invention;
Fig. 3 provides the electron microscope of the nikel powder prepared in embodiment 3 for the present invention;
Fig. 4 provides the electron microscope of the nikel powder prepared in embodiment 4 for the present invention;
Fig. 5 provides the electron microscope of the nikel powder prepared in embodiment 5 for the present invention.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that specific embodiment described herein is not used to only to explain the present invention Limit the present invention.
The embodiment of the present invention provides a kind of preparation method of spherical high-purity nikel powder, specifically includes following steps:
Step 1, roasting ball-shape nickel hydroxide obtain intermediate product nickel oxide;
The temperature of roasting is 400~600 DEG C, and the time is 3~5h;
Step 2, washs to the nickel oxide of the step 1;
Nickel oxide is washed with pure water, washing water temperature is 60~90 DEG C, water consumption for nickel oxide weight 8~10 Times, stirring pulping and washing 3 times is filtered after washing, and is then dried at 100 DEG C again;
Step 3, reduces to the nickel oxide after the step 2 washing;
Reduction temperature is 400~550 DEG C, and the time is 3~6h, and boat charge is 5~8kg.
Step 4, carries out 200 eye mesh screens are crossed after Mechanical Crushing to the nickel oxide after the step 3 reduction, obtains spherical high-purity Nikel powder.
Compare compared with preparation method, the present invention mainly has following technical advantage:Using ball-shape nickel hydroxide as presoma, The setting of parameter by roasting, washing and when reducing reduces the content of sodium in nikel powder, controls the content of the sodium in nikel powder In below 50ppm, and the pattern of nikel powder is for spherical, controllable with the index such as preferable dispersibility, AD, FSSS, in addition can basis Different demands adjusting process makes satisfactory nikel powder.
Embodiment 1
Roasting is carried out to ball-shape nickel hydroxide first:The temperature of roasting is 450 DEG C, and the time is 4h, obtains intermediate product oxygen Change nickel;Secondly nickel oxide is washed:Washing water temperature is 60 DEG C, and 10 times for nickel oxide weight of water consumption, stirring pulp are washed Wash 3 times, filter after washing, then dry at 100 DEG C again;Then the nickel oxide after washing is reduced:Reduction temperature is 500 DEG C, boat charge is 8kg, and the time is 3h;Cross 200 eye mesh screens Mechanical Crushing is carried out finally after, the nikel powder amount containing sodium for obtaining is 45ppm, nikel powder AD are 2.85g/cm3, nikel powder FSSS is 3.84 μm (as shown in Figure 1).Under the conditions of same process, unwashed nickel Powder amount containing sodium is up to 203ppm.
Embodiment 2
Roasting is carried out to ball-shape nickel hydroxide first:The temperature of roasting is 550 DEG C, and the time is 4h, obtains intermediate product oxygen Change nickel;Secondly nickel oxide is washed:Washing water temperature is 90 DEG C, and 10 times for nickel oxide weight of water consumption, stirring pulp are washed Wash 3 times, filter after washing, then dry at 100 DEG C again;Then the nickel oxide after washing is reduced:Reduction temperature is 450 DEG C, boat charge is 8kg, and the time is 3h;Cross 200 eye mesh screens Mechanical Crushing is carried out finally after, the nikel powder amount containing sodium for obtaining is 48ppm, nikel powder AD are 2.38g/cm3, nikel powder FSSS is 3.8 μm (as shown in Figure 2).Under the conditions of same process, unwashed nickel Powder amount containing sodium is up to 213ppm.
Embodiment 3
Roasting is carried out to ball-shape nickel hydroxide first:The temperature of roasting is 400 DEG C, and the time is 3h, obtains intermediate product oxygen Change nickel;Secondly nickel oxide is washed:Washing water temperature is 70 DEG C, 8 times for nickel oxide weight of water consumption, stirs pulping and washing 3 times, filter after washing, then dry at 100 DEG C again;Then the nickel oxide after washing is reduced:Reduction temperature is 400 DEG C, boat charge is 5kg, and the time is 3h;Cross 200 eye mesh screens Mechanical Crushing is carried out finally after, the nikel powder amount containing sodium for obtaining is 50ppm, nikel powder AD are 2.55g/cm3, nikel powder FSSS is 3.62 μm (as shown in Figure 3).Under the conditions of same process, unwashed nickel Powder amount containing sodium is up to 197ppm.
Embodiment 4
Roasting is carried out to ball-shape nickel hydroxide first:The temperature of roasting is 600 DEG C, and the time is 5h, obtains intermediate product oxygen Change nickel;Secondly nickel oxide is washed:Washing water temperature is 80 DEG C, 9 times for nickel oxide weight of water consumption, stirs pulping and washing 3 times, filter after washing, then dry at 100 DEG C again;Then the nickel oxide after washing is reduced:Reduction temperature is 550 DEG C, boat charge is 7kg, and the time is 5h;Cross 200 eye mesh screens Mechanical Crushing is carried out finally after, the nikel powder amount containing sodium for obtaining is 44ppm, nikel powder AD are 3.08g/cm3, nikel powder FSSS is 4.97 μm (as shown in Figure 4).Under the conditions of same process, unwashed nickel Powder amount containing sodium is up to 209ppm.
Embodiment 5
Roasting is carried out to ball-shape nickel hydroxide first:The temperature of roasting is 450 DEG C, and the time is 4h, obtains intermediate product oxygen Change nickel;Secondly nickel oxide is washed:Washing water temperature is 85 DEG C, 8 times for nickel oxide weight of water consumption, stirs pulping and washing 3 times, filter after washing, then dry at 100 DEG C again;Then the nickel oxide after washing is reduced:Reduction temperature is 500 DEG C, boat charge is 6kg, and the time is 6h;Cross 200 eye mesh screens Mechanical Crushing is carried out finally after, the nikel powder amount containing sodium for obtaining is 41ppm, nikel powder AD are 3.51g/cm3, nikel powder FSSS is 4.54 μm (as shown in Figure 5).Under the conditions of same process, unwashed nickel Powder amount containing sodium is up to 195ppm.
The above, only presently preferred embodiments of the present invention is not intended to limit protection scope of the present invention.

Claims (8)

1. a kind of preparation method of spherical high-purity nikel powder, it is characterised in that specifically include following steps:
Step 1, roasting ball-shape nickel hydroxide obtain intermediate product nickel oxide;
Step 2, washs to the nickel oxide of the step 1;
Step 3, reduces to the nickel oxide after the step 2 washing;
Step 4, carries out crushing to the nickel oxide after the step 3 reduction and sieves, obtain spherical high-purity nickel powder.
2. the preparation method of a kind of spherical high-purity nikel powder according to claim 1, it is characterised in that in the step 1 The temperature of roasting is 400~600 DEG C.
3. the preparation method of a kind of spherical high-purity nikel powder according to claim 2, it is characterised in that in the step 1 The time of roasting is 3~5h.
4. a kind of preparation method of spherical high-purity nikel powder according to claim 3, it is characterised in that the step 2 kind Nickel oxide is washed with pure water, washing water temperature is 60~90 DEG C, 8~10 times for nickel oxide weight of water consumption, stirring slurry Change washing 3 times, filter after washing, then dry at 100 DEG C again.
5. the preparation method of a kind of spherical high-purity nikel powder according to claim 4, it is characterised in that in the step 3 Reduction temperature is 400~550 DEG C.
6. the preparation method of a kind of spherical high-purity nikel powder according to claim 5, it is characterised in that in the step 3 Recovery time is 3~6h.
7. the preparation method of a kind of spherical high-purity nikel powder according to claim 6, it is characterised in that in the step 3 Boat charge is 5~8kg.
8. the preparation method of a kind of spherical high-purity nikel powder according to claim 7, it is characterised in that in the step 4 200 eye mesh screens are crossed after carrying out Mechanical Crushing.
CN201611064754.9A 2016-11-28 2016-11-28 Preparing method for spherical high-purity nickel powder Pending CN106670489A (en)

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Application Number Priority Date Filing Date Title
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1344190A (en) * 1999-11-19 2002-04-10 堺化学工业株式会社 Method for producing fine powder of metallic nickel comprised of fine spherical particles
JP2005002395A (en) * 2003-06-11 2005-01-06 Sumitomo Metal Mining Co Ltd Porous spherical nickel powder, and its production method
JP2006016653A (en) * 2004-06-30 2006-01-19 Sumitomo Osaka Cement Co Ltd Method for producing nanoparticle of less noble metal
CN101077476A (en) * 2006-05-24 2007-11-28 比亚迪股份有限公司 Method for preparing globular shape powdered nickel precursor body and globular shape powdered nickel
JP2015040329A (en) * 2013-08-22 2015-03-02 住友金属鉱山株式会社 Nickel power and method for producing the same, and nickel paste using the same
CN104942301A (en) * 2015-06-19 2015-09-30 四川金广实业(集团)股份有限公司 Technology for producing nickel raw material for stainless steel by nickelous hydroxide
CN105382267A (en) * 2015-12-17 2016-03-09 宁波繁盛商业管理有限公司 Preparation method of hollow micron nickel spheres

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1344190A (en) * 1999-11-19 2002-04-10 堺化学工业株式会社 Method for producing fine powder of metallic nickel comprised of fine spherical particles
JP2005002395A (en) * 2003-06-11 2005-01-06 Sumitomo Metal Mining Co Ltd Porous spherical nickel powder, and its production method
JP4063151B2 (en) * 2003-06-11 2008-03-19 住友金属鉱山株式会社 Porous spherical nickel powder and method for producing the same
JP2006016653A (en) * 2004-06-30 2006-01-19 Sumitomo Osaka Cement Co Ltd Method for producing nanoparticle of less noble metal
CN101077476A (en) * 2006-05-24 2007-11-28 比亚迪股份有限公司 Method for preparing globular shape powdered nickel precursor body and globular shape powdered nickel
JP2015040329A (en) * 2013-08-22 2015-03-02 住友金属鉱山株式会社 Nickel power and method for producing the same, and nickel paste using the same
CN104942301A (en) * 2015-06-19 2015-09-30 四川金广实业(集团)股份有限公司 Technology for producing nickel raw material for stainless steel by nickelous hydroxide
CN105382267A (en) * 2015-12-17 2016-03-09 宁波繁盛商业管理有限公司 Preparation method of hollow micron nickel spheres

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