CN105382267A - Preparation method of hollow micron nickel spheres - Google Patents
Preparation method of hollow micron nickel spheres Download PDFInfo
- Publication number
- CN105382267A CN105382267A CN201510948596.2A CN201510948596A CN105382267A CN 105382267 A CN105382267 A CN 105382267A CN 201510948596 A CN201510948596 A CN 201510948596A CN 105382267 A CN105382267 A CN 105382267A
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- nickel
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- water
- properties
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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
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
- B22F1/0655—Hollow particles
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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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to a preparation method of hollow micron nickel spheres. The method comprises the following steps: fully dissolving nickel sulfate in water to obtain a water solution of nickel salt; adding hexamethylenetetramine based on a certain amount proportion to the water solution of nickel salt; stirring under room temperature to dissolve; feeding the obtained mixture into a high-pressure reaction kettle with a polytetrafluoroethylene liner; closing and heating until the temperature is 100 to 210 DEG C, and then maintaining the temperature for 2 to 8 hours; filtering the obtained product; repeatedly washing with water; then drying to obtain nickel hydroxide microspheres; directly feeding the nickel hydroxide microspheres into a furnace which is early heated to be 350 to 450 DEG C; reducing for more than 1 hour in a hydrogen atmosphere, so as to obtain the hollow micron nickel spheres. The method has the advantages of being simple in preparation process, low in raw material cost, short in production cycle, mild in conditions, high in product purity, and uniform in appearance.
Description
Technical field
The present invention relates to a kind of method preparing micron nickel, specifically a kind of preparation method of Properties of Hollow Nickel Sub-microsphere.
Background technology
The control preparation of micron and nano inorganic material pattern and size is subject to the extensive concern of scientific circles, and especially by the ordered nano material that self assembly is formed, its special performance receives much concern.
Nano-nickel powder is a kind of important metal dust, due to physics, the chemical property of its uniqueness, is widely used in many fields such as catalyst, magnetic material, electrocondution slurry, nano-coating material and hardmetall binders.Ultra-fine/nano-nickel powder is also the necessary raw material of the ultra-fine nickel alloy of preparation, it can be used as Addition ofelements can greatly put forward heavy alloyed intensity simultaneously, improves the combination property of alloy.Be made up of nickel nanocrystal, possess the extra-fine nickel powder of hollow-core construction, there is using value advantageously, comprise high catalytic activity, large specific area, the advantages such as low filling threshold value, therefore the exploitation of hollow-core construction micron nickel ball preparation method has major application value.
The method preparing nano-nickel powder comprises Physical and chemical method, and Physical is by pulverizing, micronized particles.Chemistry rule needs with nickel compound to be raw material, prepares nanometer powder by chemical reaction.Two kinds of methods respectively have pluses and minuses, and chemical method output is large, and technique is simple, are easy to lot-sizeization and produce.
Summary of the invention
The object of this invention is to provide a kind of compared with the method preparing Properties of Hollow Nickel Sub-microsphere under temperate condition fast.
Properties of Hollow Nickel Sub-microsphere preparation method of the present invention, comprises the following steps:
1) be fully dissolved in the water by ammonium nickel sulfate, the nickel ion concentration of preparation is the aqueous solution of 0.1 ~ 1mol/L;
2) joined by hexamethylenetetramine in the nickel salt solution that step 1) configures, the mol ratio of hexamethylenetetramine and nickel salt is 4:1 ~ 6:1, at room temperature stirring and dissolving evenly after, load autoclave, closed reactor, is heated 100 ~ 210 DEG C, insulation 2-8 hour;
3) by step 2) product of gained filters, repeatedly cleans with water, dry, can obtain nickel hydroxide microballoon.
4) by above-mentioned steps 3) nickel hydroxide micron ball directly puts in the stove being heated to 350 ~ 450 DEG C, and reduce more than 1 hour in hydrogen atmosphere, can Properties of Hollow Nickel Sub-microsphere be obtained.
Above-mentioned steps 2) in the mol ratio of preferably hexamethylenetetramine and nickel salt be 5:1.
Above-mentioned steps 4) described in the desired heating temperature of stove be 400 DEG C.
The present invention has the following advantages:
1) obtained product purity is high, and productive rate is high.
2) technique is simple, and production cost is low, with short production cycle, mild condition.
3) product pattern rule.
detailed description of the invention:
Embodiment 1:
Get ammonium nickel sulfate 0.02mol, then add 100mL distilled water, stir and make it fully dissolve, under room temperature, add 0.08mol hexamethylenetetramine, after stirring and dissolving is even, add reactor, react 4 hours at 150 DEG C after airtight.After reaction terminates, filtered by product, use water cyclic washing, after 120 DEG C of dryings, the nickel hydroxide microballoon obtained, reductase 12 hour in 400 degree of nitrogen and 10vol% hydrogen mixed gas atmosphere, obtains hollow ultra-fine nickel micron ball.
Embodiment 2:
Get ammonium nickel sulfate 0.03mol, then add 200mL distilled water, stir and make it fully dissolve, under room temperature, add 0.15mol hexamethylenetetramine, after stirring and dissolving is even, add reactor, react 2 hours at 180 DEG C after airtight.After reaction terminates, product is filtered, uses water cyclic washing, after 100 DEG C of dryings, nickel hydroxide microballoon will be obtained, wherein reduce 3 hours in the mixing of 350 degree of argon gas and 5vol% hydrogen, obtain the nickel micron ball of hollow form.
Embodiment 3:
Get ammonium nickel sulfate 0.02mol, then add 50mL distilled water, stir and make it fully dissolve, under room temperature, add 0.12mol hexamethylenetetramine, after stirring and dissolving is even, add reactor, react 8 hours at 200 DEG C after airtight.After reaction terminates, filtered by product, use water cyclic washing, 80 DEG C of dryings, subsequently prepared nickel hydroxide product, at 450 degree, the mixing of nitrogen and 10vol% hydrogen is wherein reduced 3 hours, namely obtains Hollow Nickel micron ball powder.
Claims (3)
1. a preparation method for Properties of Hollow Nickel Sub-microsphere, is characterized in that, comprises the following steps:
1) ammonium nickel sulfate is fully dissolved in the water, is mixed with the aqueous solution that nickel ion concentration is 0.1 ~ 1mol/L;
2) joined by hexamethylenetetramine in the nickel salt solution that step 1) configures, the mol ratio of hexamethylenetetramine and nickel salt is 4:1 ~ 6:1, at room temperature stirring and dissolving evenly after, load autoclave, closed reactor, is heated 100 ~ 210 DEG C, insulation 2-8 hour;
3) by step 2) product of gained filters, with water cleaning, dry, obtains nickel hydroxide micron ball;
4) by above-mentioned steps 3) nickel hydroxide micron ball directly puts in the stove being heated to 350 ~ 450 DEG C, reduces more than 1 hour in hydrogen atmosphere, obtains Properties of Hollow Nickel Sub-microsphere.
2., by the method preparing Properties of Hollow Nickel Sub-microsphere according to claim 1, it is characterized in that, step 2) described in hexamethylenetetramine and the mol ratio of nickel salt be 5:1.
3. by the method preparing Properties of Hollow Nickel Sub-microsphere according to claim 1, it is characterized in that, the heating-up temperature of the stove described in step 4) is 400 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510948596.2A CN105382267A (en) | 2015-12-17 | 2015-12-17 | Preparation method of hollow micron nickel spheres |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510948596.2A CN105382267A (en) | 2015-12-17 | 2015-12-17 | Preparation method of hollow micron nickel spheres |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105382267A true CN105382267A (en) | 2016-03-09 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510948596.2A Pending CN105382267A (en) | 2015-12-17 | 2015-12-17 | Preparation method of hollow micron nickel spheres |
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| CN (1) | CN105382267A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106670489A (en) * | 2016-11-28 | 2017-05-17 | 荆门市格林美新材料有限公司 | Preparing method for spherical high-purity nickel powder |
| CN112355318A (en) * | 2020-10-21 | 2021-02-12 | 荆楚理工学院 | Large-particle-size porous spherical nickel powder and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462171A (en) * | 2009-01-09 | 2009-06-24 | 南京大学 | Method for producing nano nickle sphere |
| CN101905904A (en) * | 2010-07-22 | 2010-12-08 | 北京航空航天大学 | Preparation method of nickel oxide microspheres consisting of lotus root-like nanosheets |
| CN101985366A (en) * | 2010-11-23 | 2011-03-16 | 金川集团有限公司 | Equipment and method for preparing carbonyl nickel spheres |
| CN103464781A (en) * | 2013-09-06 | 2013-12-25 | 浙江大学 | Method of producing nickel microspheres |
| CN103588253A (en) * | 2013-10-08 | 2014-02-19 | 浙江大学 | Method for preparing alpha-phase porous flaky nickel hydroxide microspheres |
| CN104148662A (en) * | 2014-07-15 | 2014-11-19 | 东华大学 | Hollow nanometer nickel sphere preparing method |
-
2015
- 2015-12-17 CN CN201510948596.2A patent/CN105382267A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462171A (en) * | 2009-01-09 | 2009-06-24 | 南京大学 | Method for producing nano nickle sphere |
| CN101905904A (en) * | 2010-07-22 | 2010-12-08 | 北京航空航天大学 | Preparation method of nickel oxide microspheres consisting of lotus root-like nanosheets |
| CN101985366A (en) * | 2010-11-23 | 2011-03-16 | 金川集团有限公司 | Equipment and method for preparing carbonyl nickel spheres |
| CN103464781A (en) * | 2013-09-06 | 2013-12-25 | 浙江大学 | Method of producing nickel microspheres |
| CN103588253A (en) * | 2013-10-08 | 2014-02-19 | 浙江大学 | Method for preparing alpha-phase porous flaky nickel hydroxide microspheres |
| CN104148662A (en) * | 2014-07-15 | 2014-11-19 | 东华大学 | Hollow nanometer nickel sphere preparing method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106670489A (en) * | 2016-11-28 | 2017-05-17 | 荆门市格林美新材料有限公司 | Preparing method for spherical high-purity nickel powder |
| CN112355318A (en) * | 2020-10-21 | 2021-02-12 | 荆楚理工学院 | Large-particle-size porous spherical nickel powder and preparation method thereof |
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Application publication date: 20160309 |