CN1613588A - Chemical Preparation for sheet superfine copper powder - Google Patents
Chemical Preparation for sheet superfine copper powder Download PDFInfo
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- CN1613588A CN1613588A CN 200310114035 CN200310114035A CN1613588A CN 1613588 A CN1613588 A CN 1613588A CN 200310114035 CN200310114035 CN 200310114035 CN 200310114035 A CN200310114035 A CN 200310114035A CN 1613588 A CN1613588 A CN 1613588A
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- Prior art keywords
- copper
- preparation
- substance
- copper ion
- copper powder
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Abstract
A chemical process for preparing the superfine flaky copper powder features the redox reaction between copper, complexing agent or chelating agent (NH3.H2O, complexon or its sodium salt and ethanediamine) and reducing agent (ascorbic acid).
Description
Technical field
The present invention relates to a kind of preparation method of copper powder conductive filler, or rather, the present invention relates to the preparation method of a kind of sheet, smooth surface ground superfine cupper powder.
Background technology
Superfine cupper powder is widely used in electricity field by people, as: electrically-conducting paint, conducting resinl, electrode material etc.Because the copper powder low price (only be silver-colored price 1/20), and (specific insulation is close with silver: Cu: ρ to have good electric conductivity
v1.72 * 10
-6Ω cm, Ag: ρ
v1.59 * 10
-6Ω cm), thereby more and more be subjected to people's attention, it has application fields.
Copper powder is as conductive filler, and its pattern and particle diameter have very big influence to the electric conductivity of conductive material.Generally speaking, the particle diameter of conductive filler is more little, and the electric conductivity of material is good more; Mainly be a contact between Ball-type packing, and the face between laminal filter contact helps the conduction of electric charge, and smooth surface can increase contact area, this all helps the raising of electric conductivity.Therefore, preparation sheet, smooth surface, conductive filler that granularity is little are the keys that improves conductive material electric conductivity.At present, the method for preparing superfine cupper powder is a lot, and as reducing process, electrolysis, atomization etc., but the copper powder of preparation all is spherical.Usually flake copper is to make by the mechanical ball milling copper powder, and this method cost is lower, and equipment is simple, but easily brings impurity in the mechanical milling process, the copper powder size distribution inequality, the surface irregularity that make, and performance is bad.
Summary of the invention
The objective of the invention is to overcome the weak point in the present technology, prepare a kind of sheet, ganoid superfine cupper powder.
The present invention is a kind of preparation method of copper powder conductive filler, its characteristics are: add Lip river mixture or chelating agent in copper-bath, stir, constant temperature adds certain density ascorbic acid solution in 60～95 ℃, make ascorbic acid reduction copper ion, stirring reaction 15 minutes～60 minutes is again through separating washing, vacuum drying makes sheet, ganoid copper powder.
Complexing agent of the present invention is NH
3H
2O, used NH
3H
2The amount of substance of O is 0.1～1.5 times of copper ion.
Chelating agent of the present invention is edta and its sodium salt and ethylenediamine, wherein edta and its sodium salt is meant in ethylenediamine tetra-acetic acid and single sodium salt, disodium salt and the trisodium salt any one, and its consumption is 0.02～0.25 times of copper ion amount of substance; The consumption of ethylenediamine is 0.1～2.5 times of copper ion amount of substance.Complexing agent here or chelating agent can form stable complex compound or chelate with copper ion, thereby control the speed of redox reaction effectively, are convenient to the preparation of sheet, ganoid copper powder.
The concentration of the used copper sulphate of the present invention is 0.05～3mol/L.
The concentration of the used ascorbic acid of the present invention is 0.05～2mol/L, and used amount of substance is 1.2 times of copper ion.
The present invention has a significant effect compared with the prior art, this method is simple, convenient, be easy to control, less energy consumption, the profile of the copper powder of preparation is sheet and smooth surface, its particle size distribution is 0.5um～20um, and can prepare the copper powder of different narrow size distribution by the consumption of regulating complexing agent or chelating agent.
The specific embodiment
Embodiment one
The 6.24g cupric sulfate pentahydrate is added in the 50ml distilled water, and stirring is dissolved it fully, drips the NH of 0.97ml 25% in solution
3H
2O stirs, and this mixed liquor is placed reactor, and constant temperature is in 90 ℃.In another container, the 5.28g ascorbic acid is dissolved in the 50ml distilled water, under stirring condition, ascorbic acid is added drop-wise in the reactor, stirring reaction 60 minutes.The standing separation copper powder with distilled water washing three times, is used 80 ℃ of oven dry of vacuum drying oven again.The profile of made copper powder is sheet and smooth surface, and its particle size distribution is 1um～8um.
Embodiment two
Remove complexing agent NH
3H
2O uses instead outside 0.93g chelating agent ethylenediamine tetra-acetic acid two receives, and all the other prescriptions, reaction condition and step are with embodiment one.The profile of made copper powder is sheet and smooth surface, and its particle size distribution is 2um～10um.
Embodiment three
Remove complexing agent NH
3H
2O uses instead outside the 0.85ml chelating agent ethylenediamine, and all the other prescriptions, reaction condition and step are with embodiment one.The profile of made copper powder is sheet and smooth surface, and its particle size distribution is 1um～6um.
Claims (5)
1. the chemical preparation process of a ultrafine flake copper powder, it is characterized in that: in copper-bath, add complexing agent or chelating agent, stir, constant temperature adds certain density ascorbic acid solution in 60～95 ℃, make ascorbic acid reduction copper ion, stirring reaction 15 minutes～60 minutes is again through separating washing, vacuum drying makes sheet, ganoid superfine cupper powder.
2. preparation method as claimed in claim 1 is characterized in that described complexing agent is NH
3H
2O, used NH
3H
2The amount of substance of O is 0.1～1.5 times of copper ion.
3. preparation method as claimed in claim 1, it is characterized in that used chelating agent is edta and its sodium salt and ethylenediamine, wherein edta and its sodium salt is meant in ethylenediamine tetra-acetic acid and single sodium salt, disodium salt and the trisodium salt any one, and its consumption is 0.02～0.25 times of copper ion amount of substance; The consumption of ethylenediamine is 0.1～2.5 times of copper ion amount of substance.
4. preparation method as claimed in claim 1, the concentration that it is characterized in that copper sulphate is 0.05～3mol/L.
5. preparation method as claimed in claim 1, the concentration that it is characterized in that used ascorbic acid is 0.05～2mol/L, used amount of substance is 1.2 times of copper ion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200310114035XA CN1315604C (en) | 2003-11-08 | 2003-11-08 | Chemical Preparation for sheet superfine copper powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200310114035XA CN1315604C (en) | 2003-11-08 | 2003-11-08 | Chemical Preparation for sheet superfine copper powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1613588A true CN1613588A (en) | 2005-05-11 |
| CN1315604C CN1315604C (en) | 2007-05-16 |
Family
ID=34760122
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200310114035XA Expired - Fee Related CN1315604C (en) | 2003-11-08 | 2003-11-08 | Chemical Preparation for sheet superfine copper powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1315604C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100488674C (en) * | 2005-12-16 | 2009-05-20 | 华南理工大学 | Sheet crystal cupper powder and liquid phase chemical preparation process thereof |
| CN102191494A (en) * | 2011-04-28 | 2011-09-21 | 中国科学院宁波材料技术与工程研究所 | Treatment solution for reducing oxidation films on surface of copper and copper alloys and treatment method thereof |
| CN101590530B (en) * | 2009-06-30 | 2012-10-03 | 广东风华高新科技股份有限公司 | Method for preparing high-inoxidability sphere-like copper powder |
| CN105290414A (en) * | 2014-06-11 | 2016-02-03 | 南京理工大学 | Method for synthesizing nano-copper particles |
| CN105817616A (en) * | 2016-05-30 | 2016-08-03 | 李�浩 | Copper nano-film loaded on substrate and preparation method and application thereof |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07107169B2 (en) * | 1987-01-27 | 1995-11-15 | 田中貴金属工業株式会社 | Method for producing fine copper particles |
| EP0363552B1 (en) * | 1988-07-27 | 1993-10-13 | Tanaka Kikinzoku Kogyo K.K. | Process for preparing metal particles |
| JPH05271721A (en) * | 1992-03-23 | 1993-10-19 | Tanaka Kikinzoku Kogyo Kk | Production of fine copper grain |
| CN1061579C (en) * | 1995-03-08 | 2001-02-07 | 上海市合成树脂研究所 | Process for preparing copper powder for electromagnetic shield conducting paint |
| JPH09165606A (en) * | 1995-12-15 | 1997-06-24 | Takeshi Hayakawa | Production of copper powder |
| CN1060982C (en) * | 1997-11-17 | 2001-01-24 | 北京有色金属研究总院 | Preparation of ultrafine metal powders |
-
2003
- 2003-11-08 CN CNB200310114035XA patent/CN1315604C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100488674C (en) * | 2005-12-16 | 2009-05-20 | 华南理工大学 | Sheet crystal cupper powder and liquid phase chemical preparation process thereof |
| CN101590530B (en) * | 2009-06-30 | 2012-10-03 | 广东风华高新科技股份有限公司 | Method for preparing high-inoxidability sphere-like copper powder |
| CN102191494A (en) * | 2011-04-28 | 2011-09-21 | 中国科学院宁波材料技术与工程研究所 | Treatment solution for reducing oxidation films on surface of copper and copper alloys and treatment method thereof |
| CN105290414A (en) * | 2014-06-11 | 2016-02-03 | 南京理工大学 | Method for synthesizing nano-copper particles |
| CN105817616A (en) * | 2016-05-30 | 2016-08-03 | 李�浩 | Copper nano-film loaded on substrate and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1315604C (en) | 2007-05-16 |
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