CN104227012A - Preparation method for ultra-fine copper powder - Google Patents
Preparation method for ultra-fine copper powder Download PDFInfo
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- CN104227012A CN104227012A CN201310253888.5A CN201310253888A CN104227012A CN 104227012 A CN104227012 A CN 104227012A CN 201310253888 A CN201310253888 A CN 201310253888A CN 104227012 A CN104227012 A CN 104227012A
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Abstract
The invention discloses a preparation method for ultra-fine copper powder. The preparation method comprises the following steps of (1) cleaning copper powder by using hydrazine hydrate as reducing agents to obtain saturated red copper powder A1; (2) cleaning the copper powder A1 by using formaldehyde as reducing agents to obtain atropurpureus copper powder A2; (3) pre-reducing the copper powder A2 by using glucose and performing secondary reduction cleaning on the copper powder A2 by using hydrazine hydrate to obtain red copper powder A3; (4) pre-reducing the copper powder A3 by using the glucose and performing secondary reduction cleaning on the copper powder A3 by using the formaldehyde to obtain red copper powder A4; and (5) pre-reducing the copper powder A4 by using the glucose and cleaning the copper powder A4 by using an ascorbic acid and PVP (polyvinyl pyrrolidone) through a two-step reduction method so as to obtain rose red copper powder A5. By the preparation method, the rose red copper powder with excellent performance is obtained through a liquid phase reduction method, and is spherical or is similarly spherical; mass distribution of the rose red copper powder is uniform; the grain size of the rose red copper powder is 1 micrometer to 3 micrometers; clustering is avoided; the dispersibility is high; and technological requirements on preparation of copper paste are met.
Description
Technical field
The present invention is specially a kind of preparation method of superfine cupper powder.
Background technology
Along with the fast development of microelectric technique, the demand of complete electronic set in miniaturized, portable, multi-functional, digitlization and high reliability, high-performance, has promoted electronic component further day by day to future development that is microminiaturized, integrated and high frequency.At present, the most power circuit of world market uses DBC heat radiation, the thick conductor layer that DBC technology can provide power circuit to need, it is the Copper Foil ceramic substrate two sides Direct Bonding 200 ~ 500 μm, and etch figure, relatively be applicable on high temperature and big current, but DBC method can not meet requirement little, thin, light needed for surface mounting technique.Thick-film metalliz method, be exactly by serigraphy sealing-in metal level, conductor and resistance etc. on ceramic substrate, soldering metal level, circuit and lead contact etc. are formed through sintering, the replacement of serigraphy copper slurry is adopted to cover copper, the ceramic radiating fin that size is little, thickness is thin, density is high can be prepared, improve the requirement of the density of surface mounting technique wiring.Copper slurry is rolled into by copper metal powder end, glass powder and organic carrier the paste mixed through three-high mill.But preparing copper, to starch the copper metal powder end used be a kind of superfine cupper powder, so the preparation method inventing a kind of superfine cupper powder is very in need.
Summary of the invention
Technical problem solved by the invention is the preparation method providing a kind of superfine cupper powder, to solve the problem proposed in above-mentioned background technology.
In order to achieve the above object, the present invention realizes by the following technical solutions:
A preparation method for superfine cupper powder, comprises the following steps:
(1) be that reducing agent cleans copper powder with hydrazine hydrate: the preparation copper-bath of 1mol/L and the sodium hydroxide solution of 2.5mol/L, be mixed in the beaker of 3L by the solution prepared, beaker be placed in electric-heated thermostatic water bath and at the uniform velocity stir and slowly heat up; When temperature rises to 50 DEG C, slowly add hydrazine hydrate in batches, when 60 DEG C, constant temperature is after 30 minutes, leave standstill one day, pour out supernatant, then by powder cleaning repeatedly, finally use alcohol washes, suction filtration, after powder is soaked 25-35 minute in protection solution, suction filtration, dry, obtain the red copper powder A1 of comparatively dark colour;
(2) take formaldehyde as reducing agent cleaning copper powder A1: the preparation copper-bath of 1mol/L and the sodium hydroxide solution of 2.5mol/L, be mixed in the beaker of 3L by the solution prepared, beaker be placed in electric-heated thermostatic water bath and at the uniform velocity stir; After 25 minutes, leave standstill one day, pour out supernatant, then by powder cleaning repeatedly; Finally use alcohol washes, suction filtration, after powder is soaked 25-35 minute in protection solution, suction filtration, dries, obtains atropurpureus copper powder A2;
(3) with glucose prereduction, hydrazine hydrate secondary reduction cleaning copper powder A2:
1. prepare the glucose solution of 3mol/L, the copper-bath prepared and sodium hydroxide solution are put into the beaker of 3L, and beaker is put into water-bath at the uniform velocity stir; Add the glucose of half when 50 DEG C in reaction vessel, when 60 DEG C, remaining glucose is all added in reaction system, after 30 minutes, leave standstill one day, pour out supernatant, repeatedly clean several times, until upper strata is clear liquid;
2. prepare a certain amount of hydrazine hydrate and dispersant, beaker is placed in water-bath, add a small amount of dispersant, at the uniform velocity stir and slowly heating, when temperature rises to 55 DEG C, hydrazine hydrate is slowly added in reaction system, after 60 DEG C, be incubated 20 minutes, leave standstill, pour out supernatant, repeatedly clean several times; Finally use alcohol washes, suction filtration, powder is soaked 25-35 minute, suction filtration in protection solution, dries, obtain red copper powder A3;
(4) with glucose prereduction, formaldehyde secondary reduction cleaning copper powder A3:
1. prepare the glucose solution of 3mol/L, the copper-bath prepared and sodium hydroxide solution are put into the beaker of 3L, and beaker is put into water-bath at the uniform velocity stir; Add the glucose of half when 50 DEG C in reaction vessel, when 60 DEG C, remaining glucose is all added in reaction system, after 30 minutes, leave standstill one day, pour out supernatant, repeatedly clean several times, until upper strata is clear liquid;
2. prepare a certain amount of formaldehyde and dispersant, beaker is placed in water-bath, add a small amount of dispersant, at the uniform velocity stir, formaldehyde is slowly added in reaction system, after 25 minutes, leave standstill, pour out supernatant; Repeatedly clean several times; Finally use alcohol washes, suction filtration, powder is soaked 25-35 minute, suction filtration in protection solution, dries, obtain red copper powder A4;
(5) with glucose prereduction, ascorbic acid and PVP two step reduction method cleaning copper powder A4:
The copper-bath prepared and sodium hydroxide solution are put into the beaker of 3L, and beaker is put into water-bath at the uniform velocity stir.Its preparation process is as follows:
1. 800g copper sulfate crystal 2L pure water is dissolved and make solution, add 14g glucose and 0.4gPVP;
2. 5g ascorbic acid is dissolved in 15ml deionized water;
3. 40g NaOH is dissolved in 800ml deionized water;
Heat above-mentioned 3 kinds of solution to 70 DEG C, will 3. under agitation add 1., 2. reaction 15-25 minute, then will add again, stirs, and reaction 20-30 minute, washes 3 ~ 4 times with water the copper powder generated, obtain rose copper powder A5.
To 3. add 1., the color that solution produces precipitation is changed to:
Navy blue → light blue → yellow → kermesinus
After 2. adding, the color that solution produces precipitation is changed to again:
Kermesinus → black → atropurpureus
Through detecting, obtaining rose copper powder A5 particle diameter at 1 ~ 1.8 μm, meeting the physical index of superfine cupper powder.
Further, the copper sulfate crystal described in step (5) is specially CuSO
45H
2o.
Beneficial effect:
Present invention process preparation method obtains piece red copper powder of function admirable by liquid phase reduction, and shape is spherical or class is spherical, and Mass Distribution is even, and particle diameter is at 1 ~ 3 μm, and soilless sticking and good dispersion, meet the technological requirement that copper slurry makes.
Accompanying drawing explanation
Fig. 1 is preparation technology's flow chart of a kind of superfine cupper powder of the present invention;
Fig. 2 is the process chart cleaning copper powder in present invention process step (5) with glucose prereduction, ascorbic acid and PVP two step reduction method.
Detailed description of the invention
Reaching object to make technological means of the present invention, creation characteristic, workflow, using method and effect is easy to understand, illustrating the specific embodiment of the invention below in conjunction with accompanying drawing, setting forth the present invention further.
A preparation method for superfine cupper powder, comprises the following steps:
(1) be that reducing agent cleans copper powder with hydrazine hydrate: the preparation copper-bath of 1mol/L and the sodium hydroxide solution of 2.5mol/L, be mixed in the beaker of 3L by the solution prepared, beaker be placed in electric-heated thermostatic water bath and at the uniform velocity stir and slowly heat up; When temperature rises to 50 DEG C, slowly add hydrazine hydrate in batches, when 60 DEG C, constant temperature is after 30 minutes, leave standstill one day, pour out supernatant, then by powder cleaning repeatedly, finally use alcohol washes, suction filtration, after powder is soaked 25-35 minute in protection solution, suction filtration, dry, obtain the red copper powder A1 of comparatively dark colour;
(2) take formaldehyde as reducing agent cleaning copper powder A1: the preparation copper-bath of 1mol/L and the sodium hydroxide solution of 2.5mol/L, be mixed in the beaker of 3L by the solution prepared, beaker be placed in electric-heated thermostatic water bath and at the uniform velocity stir; After 25 minutes, leave standstill one day, pour out supernatant, then by powder cleaning repeatedly; Finally use alcohol washes, suction filtration, after powder is soaked 25-35 minute in protection solution, suction filtration, dries, obtains atropurpureus copper powder A2;
(3) with glucose prereduction, hydrazine hydrate secondary reduction cleaning copper powder A2:
1. prepare the glucose solution of 3mol/L, the copper-bath prepared and sodium hydroxide solution are put into the beaker of 3L, and beaker is put into water-bath at the uniform velocity stir; Add the glucose of half when 50 DEG C in reaction vessel, when 60 DEG C, remaining glucose is all added in reaction system, after 30 minutes, leave standstill one day, pour out supernatant, repeatedly clean several times, until upper strata is clear liquid;
2. prepare a certain amount of hydrazine hydrate and dispersant, beaker is placed in water-bath, add a small amount of dispersant, at the uniform velocity stir and slowly heating, when temperature rises to 55 DEG C, hydrazine hydrate is slowly added in reaction system, after 60 DEG C, be incubated 20 minutes, leave standstill, pour out supernatant, repeatedly clean several times; Finally use alcohol washes, suction filtration, powder is soaked 25-35 minute, suction filtration in protection solution, dries, obtain red copper powder A3;
(4) with glucose prereduction, formaldehyde secondary reduction cleaning copper powder A3:
1. prepare the glucose solution of 3mol/L, the copper-bath prepared and sodium hydroxide solution are put into the beaker of 3L, and beaker is put into water-bath at the uniform velocity stir; Add the glucose of half when 50 DEG C in reaction vessel, when 60 DEG C, remaining glucose is all added in reaction system, after 30 minutes, leave standstill one day, pour out supernatant, repeatedly clean several times, until upper strata is clear liquid;
2. prepare a certain amount of formaldehyde and dispersant, beaker is placed in water-bath, add a small amount of dispersant, at the uniform velocity stir, formaldehyde is slowly added in reaction system, after 25 minutes, leave standstill, pour out supernatant; Repeatedly clean several times; Finally use alcohol washes, suction filtration, powder is soaked 25-35 minute, suction filtration in protection solution, dries, obtain red copper powder A4;
(5) with glucose prereduction, ascorbic acid and PVP two step reduction method cleaning copper powder A4:
The copper-bath prepared and sodium hydroxide solution are put into the beaker of 3L, and beaker is put into water-bath at the uniform velocity stir.Its preparation process is as follows:
4. 800g copper sulfate crystal 2L pure water is dissolved and make solution, add 14g glucose and 0.4gPVP;
5. 5g ascorbic acid is dissolved in 15ml deionized water;
6. 40g NaOH is dissolved in 800ml deionized water;
Heat above-mentioned 3 kinds of solution to 70 DEG C, will 3. under agitation add 1., 2. reaction 15-25 minute, then will add again, stirs, and reaction 20-30 minute, washes 3 ~ 4 times with water the copper powder generated, obtain rose copper powder A5.
To 3. add 1., the color that solution produces precipitation is changed to:
Navy blue → light blue → yellow → kermesinus
After 2. adding, the color that solution produces precipitation is changed to again:
Kermesinus → black → atropurpureus
Through detecting, obtaining rose copper powder A5 particle diameter at 1 ~ 1.8 μm, meeting the physical index of superfine cupper powder.
Further, the copper sulfate crystal described in step (5) is specially CuSO
45H
2o.
More than show and describe general principle of the present invention and principal character and advantage of the present invention; the technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications; these changes and improvements all fall in the claimed scope of the invention, and application claims protection domain is defined by appending claims and equivalent thereof.
Claims (2)
1. a preparation method for superfine cupper powder, is characterized in that, comprises the following steps:
(1) be that reducing agent cleans copper powder with hydrazine hydrate, obtain the red copper powder A1 of comparatively dark colour;
(2) take formaldehyde as reducing agent cleaning copper powder A1, obtain atropurpureus copper powder A2;
(3) with glucose prereduction, hydrazine hydrate secondary reduction cleaning copper powder A2, red copper powder A3 is obtained;
(4) with glucose prereduction, formaldehyde secondary reduction cleaning copper powder A3, red copper powder A4 is obtained;
(5) with glucose prereduction, ascorbic acid and PVP two step reduction method cleaning copper powder A4, obtain rose copper powder A5, through detecting, particle diameter is at 1 ~ 1.8 μm, and this production technology prepares the physical index that superfine cupper powder meets the use of copper slurry.
2. the preparation method of a kind of superfine cupper powder according to claim 1, it is characterized in that, the copper sulfate crystal described in step (5) is specially CuSO
45H
2o.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106363165A (en) * | 2016-09-05 | 2017-02-01 | 国核电力规划设计研究院 | Flaky copper particles, preparation method thereof, catalyst and electrode |
| CN107030293A (en) * | 2016-11-28 | 2017-08-11 | 荆门市格林美新材料有限公司 | A kind of preparation method of utilization secondary reduction high-purity nickel powder |
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| JPH02294414A (en) * | 1989-05-10 | 1990-12-05 | Seidou Kagaku Kogyo Kk | Production of fine copper powder |
| CN101195170A (en) * | 2006-12-06 | 2008-06-11 | 比亚迪股份有限公司 | Method for preparing superfine copper powder |
| CN101279377A (en) * | 2008-05-15 | 2008-10-08 | 金川集团有限公司 | Method for preparing spherical superfine copper powder |
| CN101474678A (en) * | 2008-11-28 | 2009-07-08 | 中国兵器工业第五二研究所 | Method for preparing antioxidated superfine copper powder |
| CN101890505A (en) * | 2010-07-21 | 2010-11-24 | 株洲冶炼集团股份有限公司 | Superfine cupper powder and preparation method thereof |
| CN102601383A (en) * | 2012-03-30 | 2012-07-25 | 电子科技大学 | Method for preparing ultrafine copper powder at room temperature |
| CN102764898A (en) * | 2012-08-09 | 2012-11-07 | 深圳市圣龙特电子有限公司 | method for preparing ultrafine copper powder for electronic paste |
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2013
- 2013-06-14 CN CN201310253888.5A patent/CN104227012A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02294414A (en) * | 1989-05-10 | 1990-12-05 | Seidou Kagaku Kogyo Kk | Production of fine copper powder |
| CN101195170A (en) * | 2006-12-06 | 2008-06-11 | 比亚迪股份有限公司 | Method for preparing superfine copper powder |
| CN101279377A (en) * | 2008-05-15 | 2008-10-08 | 金川集团有限公司 | Method for preparing spherical superfine copper powder |
| CN101474678A (en) * | 2008-11-28 | 2009-07-08 | 中国兵器工业第五二研究所 | Method for preparing antioxidated superfine copper powder |
| CN101890505A (en) * | 2010-07-21 | 2010-11-24 | 株洲冶炼集团股份有限公司 | Superfine cupper powder and preparation method thereof |
| CN102601383A (en) * | 2012-03-30 | 2012-07-25 | 电子科技大学 | Method for preparing ultrafine copper powder at room temperature |
| CN102764898A (en) * | 2012-08-09 | 2012-11-07 | 深圳市圣龙特电子有限公司 | method for preparing ultrafine copper powder for electronic paste |
Non-Patent Citations (1)
| Title |
|---|
| 胡磊 等: "致密银包铜粉基体-铜粉的制备及其性能研究", 《热加工工艺》, vol. 41, no. 11, 30 November 2012 (2012-11-30), pages 11 - 14 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106363165A (en) * | 2016-09-05 | 2017-02-01 | 国核电力规划设计研究院 | Flaky copper particles, preparation method thereof, catalyst and electrode |
| CN107030293A (en) * | 2016-11-28 | 2017-08-11 | 荆门市格林美新材料有限公司 | A kind of preparation method of utilization secondary reduction high-purity nickel powder |
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Application publication date: 20141224 |