CN101524763A - Method for preparing submicron spherical copper powder - Google Patents
Method for preparing submicron spherical copper powder Download PDFInfo
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- CN101524763A CN101524763A CN200910082504A CN200910082504A CN101524763A CN 101524763 A CN101524763 A CN 101524763A CN 200910082504 A CN200910082504 A CN 200910082504A CN 200910082504 A CN200910082504 A CN 200910082504A CN 101524763 A CN101524763 A CN 101524763A
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Abstract
The invention discloses a method for preparing submicron spherical copper powder, relating to a method which obtains submicron spherical copper powder by two-step deoxidization in the same system. The method is characterized in that in the preparing process, glucose solution, sodium hydroxide solution and dispersant solution are mixed to obtain base solution; the base solution is bathed in water to the constant temperature of 60 DEG C; cupric salt solution is then added to transform the solution to obtain cuprous oxide; and hydrazine hydrate solution is finally added to deoxygenize the cuprous oxide; and the solution is aged, filtered and dried to obtain submicron spherical copper powder with high purity and excellent dispersibility. The method of the invention can obtain spherical copper powder of 0.4-0.8mum. Technical process of the method is simple and the method is applicable to industrial mass production.
Description
Technical field
A kind of method for preparing submicron spherical copper powder relates to and a kind ofly obtains the submicron spherical copper powder method with two step reduction in same system.
Background technology
The specific surface that ultrafine dust is big, high surface energy make it have many peculiar physicochemical properties, show extremely important using value in fields such as metallurgy, chemical industry, light industry, electronics, national defence, nuclear technology and Aero-Space.
Submicron spherical copper powder is meant particle size at the copper powder more than the 0.1 μ m, below the 1 μ m, the nearly ball-type of profile.Because of its low price and have good electric conductivity, be widely used in electricity field, as: electrically-conducting paint, conducting resinl, electrode material etc.Traditional electrolytic copper powder is not suitable for making superfine cupper powder because particle is bigger, and atomization is difficult to promote because anti-oxidant problem is difficult to solve.The method of submicron spherical copper powder preparation at present has ball-milling method, gas phase steam method, plasma method, gamma-radiation irradiation-hydrothermal crystallization combination method, metallic vapour cohesion-original position cold-press moulding method, freeze-drying and liquid phase reduction, former kinds belong to physical method, the shortcoming that have cost height, complex process, yields poorly.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provides that a kind of equipment is simple, technological process short, investment is little, output is big, cost is low, prepares the purity height, good dispersion, easily realizes that the employing liquid phase chemical reduction legal system of suitability for industrialized production is equipped with the method for submicron spherical copper powder.
The objective of the invention is to be achieved through the following technical solutions.
A kind of method for preparing submicron spherical copper powder, it is characterized in that its preparation process is that glucose solution, sodium hydroxide solution, dispersant solution are mixed the back as end liquid, with end liquid constant temperature water bath to 60 ℃, add copper salt solution then and change into cuprous oxide, add the hydrazine hydrate solution reduction at last, through the submicron spherical copper powder of ageing, filtration, dry preparation purity height, good dispersion.
A kind of method for preparing submicron spherical copper powder of the present invention, the concentration that it is characterized in that described glucose solution is 350g/L, its addition is 5～6 times of copper mass in the copper salt solution.
A kind of method for preparing submicron spherical copper powder of the present invention, the concentration that it is characterized in that described sodium hydroxide solution is 100g/L, its consumption reaches 12～13 for the pH value of control end liquid.
A kind of method for preparing submicron spherical copper powder of the present invention is characterized in that dispersant in the described dispersant solution is one or more in PVP, PVA, the gelatin, its addition be in the copper salt solution copper mass 1%～2%.
A kind of method for preparing submicron spherical copper powder of the present invention is characterized in that described copper salt solution is a kind of solution or the mixed solution in copper sulphate, copper nitrate or its hydrate, and the Cu ion concentration in its copper salt solution is 50～60g/L.
A kind of method for preparing submicron spherical copper powder of the present invention is characterized in that described hydrazine hydrate solution concentration is 40%, and its addition is 5～6 times of copper mass in the copper salt solution.
A kind of method for preparing submicron spherical copper powder of the present invention is characterized in that described employing hydrazine hydrate solution reduction process is controlled at 12～13 with the pH value of reaction system, and temperature is controlled at 60 ℃.
A kind of method for preparing submicron spherical copper powder of the present invention, the digestion time that it is characterized in that described ageing process is 30～60min.
Method of the present invention adopts in liquid-phase system, is raw material, is that prereduction agent, hydrazine hydrate are that reducing agent is reduced into copper powder with the Cu ion with glucose with the divalence soluble copper salt.Relevant chemical equation is:
Cu(NO
3)
2+2NaOH＝＝Cu(OH)
2↓+2NaNO
3
2Cu(OH)
2+C
6H
12O
6＝＝Cu
2O+C
6H
12O
7+2H
2O
2Cu
2O+N
2H
4·H
2O＝＝4Cu+N
2↑+3H
2O
Adopting the copper powder of method preparation of the present invention is aubergine, and outward appearance is subsphaeroidal, and particle diameter is 0.4～0.8 μ m, narrow diameter distribution.The submicron spherical copper powder of preparation is mainly used in electricity field, and ball milling and coating through the later stage have shown excellent conducting performance and antioxygenic property.
Agents useful for same of the present invention extensively is easy to get, and process is simple, makes that the spherical copper powder in submicro cost of preparation is lower, has stronger economic benefit.
Description of drawings
The stereoscan photograph of the copper powder that Fig. 1 makes for embodiment 1, multiplication factor are 4000 times.
The stereoscan photograph of the copper powder that Fig. 2 makes for embodiment 2, multiplication factor are 4000 times.
The stereoscan photograph of the copper powder that Fig. 3 makes for embodiment 3, multiplication factor are 4000 times.
The specific embodiment
A kind of method for preparing submicron spherical copper powder, it is characterized in that its preparation process is that glucose solution, sodium hydroxide solution, dispersant solution are mixed the back as end liquid, with end liquid constant temperature water bath to 60 ℃, add copper salt solution then and change into cuprous oxide, add the hydrazine hydrate solution reduction at last, through the submicron spherical copper powder of ageing, filtration, dry preparation purity height, good dispersion.Concrete steps comprise:
(1) with the water-soluble copper salt solution that is mixed with of mantoquita, mantoquita is a kind of or mixture of copper sulphate, copper nitrate or its water and thing, and the Cu ion concentration in its copper salt solution is 50g/L～60g/L.
(2) be that 5～6 times glucose of copper mass is mixed with the glucose solution that concentration is 350g/L in the copper salt solution with quality.
(3) with quality be in the copper salt solution 1%～2% dispersant of copper mass to be mixed with concentration be 1% solution, dispersant is one or more in PVP, PVA, the gelatin.
(4) NaOH is mixed with the solution that concentration is 100g/L.
(5) glucose solution, dispersant solution and the sodium hydroxide solution for preparing mixed as end liquid, end liquid pH value is 12～13, constant temperature water bath to 60 ℃.
(6) copper salt solution for preparing is added end liquid, mantoquita is changed into cuprous oxide.
(7) be that 5～6 times of copper mass, concentration are that 40% hydrazine hydrate solution adds end liquid in the copper salt solution with quality, the control reaction temperature is 60 ℃, and the pH value of controlling reaction system simultaneously is 12～13, and cuprous oxide is changed into copper powder.
(8) carry out ageing, digestion time 30～60min after the hydrazine hydrate adding finishes.
Embodiment 1
Compound concentration is the sodium hydroxide solution 500mL of glucose solution 450mL, the 100g/L of 350g/L, 1% gelatin solution 50mL respectively, above-mentioned solution is mixed the back as end liquid constant temperature to 60 ℃, with copper content is the copper nitrate solution 500mL adding end liquid of 60g/L, then 40% hydrazine hydrate solution 180mL is added reaction system, the temperature of this process control system is 60 ℃, the pH value is 13, and hydrazine hydrate adds back ageing 30min.
Embodiment 2
Compound concentration is the sodium hydroxide solution 450mL of glucose solution 400mL, the 100g/L of 350g/L, 1% PVP solution 50mL respectively, above-mentioned solution is mixed the back as end liquid constant temperature to 60 ℃, with copper content is the copper nitrate solution 500mL adding end liquid of 55g/L, then 40% hydrazine hydrate solution 160mL is added reaction system, the temperature of this process control system is 60 ℃, the pH value is 13, and hydrazine hydrate adds back ageing 60min.
Embodiment 3
Compound concentration is the sodium hydroxide solution 430mL of glucose solution 380mL, the 100g/L of 350g/L, 2% PVA solution 30mL respectively, above-mentioned solution is mixed the back as end liquid constant temperature to 60 ℃, with copper content is the copper nitrate solution 500mL adding end liquid of 50g/L, then 40% hydrazine hydrate solution 140mL is added reaction system, the temperature of this process control system is 60 ℃, the pH value is 13, and hydrazine hydrate adds back ageing 60min.
Claims (8)
1. method for preparing submicron spherical copper powder, it is characterized in that its preparation process is that glucose solution, sodium hydroxide solution, dispersant solution are mixed the back as end liquid, with end liquid constant temperature water bath to 60 ℃, add copper salt solution then and change into cuprous oxide, add the hydrazine hydrate solution reduction at last, through the submicron spherical copper powder of ageing, filtration, dry preparation purity height, good dispersion.
2. a kind of method for preparing submicron spherical copper powder according to claim 1, the concentration that it is characterized in that described glucose solution is 350g/L, its addition is 5～6 times of copper mass in the copper salt solution.
3. a kind of method for preparing submicron spherical copper powder according to claim 1, the concentration that it is characterized in that described sodium hydroxide solution is 100g/L, its addition reaches 12～13 for the pH value of control end liquid.
4. a kind of method for preparing submicron spherical copper powder according to claim 1 is characterized in that dispersant in the described dispersant solution is one or more in PVP, PVA, the gelatin, its addition be in the copper salt solution copper mass 1%～2%.
5. a kind of method for preparing submicron spherical copper powder according to claim 1, it is characterized in that described copper salt solution is a kind of solution or the mixed solution in copper sulphate, copper nitrate or its hydrate, the Cu ion concentration in its copper salt solution is 50～60g/L.
6. a kind of method for preparing submicron spherical copper powder according to claim 1 is characterized in that described hydrazine hydrate solution concentration is 40%, and its addition is 5～6 times of copper mass in the copper salt solution.
7. a kind of method for preparing submicron spherical copper powder according to claim 1 is characterized in that described employing hydrazine hydrate solution reduction process is controlled at 12～13 with the pH value of reaction system, and temperature is controlled at 60 ℃.
8. a kind of method for preparing submicron spherical copper powder according to claim 1, the digestion time that it is characterized in that described ageing process is 30～60min.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101886016A (en) * | 2010-07-13 | 2010-11-17 | 吉维群 | Submicron copper-based running-in restorative and application thereof |
| CN102344709A (en) * | 2010-08-05 | 2012-02-08 | 广东科学技术职业学院 | Preparation method of aqueous electromagnetic shielding coating containing copper |
| CN102691060A (en) * | 2012-06-14 | 2012-09-26 | 昆明理工大学 | Coloring process for spot copper |
| CN102941351A (en) * | 2012-11-27 | 2013-02-27 | 中国船舶重工集团公司第七一二研究所 | Preparation method of superfine copper powder |
| CN103212719A (en) * | 2013-03-22 | 2013-07-24 | 李丙服 | Production method of high-performance submicron copper powder |
| CN104625085A (en) * | 2015-01-23 | 2015-05-20 | 中国矿业大学 | Method for simply and stably preparing micro-nano hollow copper |
| CN105026079A (en) * | 2012-12-25 | 2015-11-04 | 户田工业株式会社 | Method for producing copper powder, copper powder, and copper paste |
| CN106513696A (en) * | 2015-09-09 | 2017-03-22 | 广州千顺工业材料有限公司 | Micro-nano copper powder and preparation method thereof |
| CN109622986A (en) * | 2018-12-26 | 2019-04-16 | 天津理工大学 | A kind of preparation method of copper-based modification infusorial earth |
| CN110640162A (en) * | 2019-10-08 | 2020-01-03 | 三峡大学 | Method for preparing, pretreating and dispersing superfine copper powder |
| CN111957986A (en) * | 2020-08-20 | 2020-11-20 | 湖南泽宇新材料有限公司 | Spherical nano copper powder and preparation method and application thereof |
| CN113523269A (en) * | 2021-06-08 | 2021-10-22 | 五邑大学 | Copper powder and preparation method and application thereof |
-
2009
- 2009-04-23 CN CN200910082504A patent/CN101524763A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101886016A (en) * | 2010-07-13 | 2010-11-17 | 吉维群 | Submicron copper-based running-in restorative and application thereof |
| CN102344709A (en) * | 2010-08-05 | 2012-02-08 | 广东科学技术职业学院 | Preparation method of aqueous electromagnetic shielding coating containing copper |
| CN102344709B (en) * | 2010-08-05 | 2014-06-25 | 广东科学技术职业学院 | Preparation method of aqueous electromagnetic shielding coating containing copper |
| CN102691060A (en) * | 2012-06-14 | 2012-09-26 | 昆明理工大学 | Coloring process for spot copper |
| CN102691060B (en) * | 2012-06-14 | 2014-12-31 | 昆明理工大学 | Coloring process for spot copper |
| CN102941351B (en) * | 2012-11-27 | 2015-08-26 | 中国船舶重工集团公司第七一二研究所 | A kind of preparation method of superfine cupper powder |
| CN102941351A (en) * | 2012-11-27 | 2013-02-27 | 中国船舶重工集团公司第七一二研究所 | Preparation method of superfine copper powder |
| CN105026079A (en) * | 2012-12-25 | 2015-11-04 | 户田工业株式会社 | Method for producing copper powder, copper powder, and copper paste |
| CN103212719A (en) * | 2013-03-22 | 2013-07-24 | 李丙服 | Production method of high-performance submicron copper powder |
| CN104625085A (en) * | 2015-01-23 | 2015-05-20 | 中国矿业大学 | Method for simply and stably preparing micro-nano hollow copper |
| CN106513696A (en) * | 2015-09-09 | 2017-03-22 | 广州千顺工业材料有限公司 | Micro-nano copper powder and preparation method thereof |
| CN106513696B (en) * | 2015-09-09 | 2019-08-02 | 广州千顺工业材料有限公司 | Micro-nano copper powder and preparation method thereof |
| CN109622986A (en) * | 2018-12-26 | 2019-04-16 | 天津理工大学 | A kind of preparation method of copper-based modification infusorial earth |
| CN110640162A (en) * | 2019-10-08 | 2020-01-03 | 三峡大学 | Method for preparing, pretreating and dispersing superfine copper powder |
| CN111957986A (en) * | 2020-08-20 | 2020-11-20 | 湖南泽宇新材料有限公司 | Spherical nano copper powder and preparation method and application thereof |
| CN111957986B (en) * | 2020-08-20 | 2023-04-18 | 湖南泽宇新材料有限公司 | Spherical nano copper powder and preparation method and application thereof |
| CN113523269A (en) * | 2021-06-08 | 2021-10-22 | 五邑大学 | Copper powder and preparation method and application thereof |
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