CN1019459B - Fabrication method of superifine colummar metallic powder - Google Patents
Fabrication method of superifine colummar metallic powderInfo
- Publication number
- CN1019459B CN1019459B CN 88105875 CN88105875A CN1019459B CN 1019459 B CN1019459 B CN 1019459B CN 88105875 CN88105875 CN 88105875 CN 88105875 A CN88105875 A CN 88105875A CN 1019459 B CN1019459 B CN 1019459B
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- Prior art keywords
- solution
- direct current
- copper
- solidified
- ultra
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Abstract
The present invention relates to a method for preparing ultrafine columnar metal powder. Fine metal particles are added to a salt solution of metal, and the solution is solidified. Direct current is switched on, the metal particles grow to be columnar fine particles, then, solidified electrolytes are liquified, and the columnar metal particles are separated. The present invention is easy to obtain the ultrafine columnar powder with large length and diameters, has the advantages of simple process, no material loss, etc., and only needs common devices.
Description
The invention belongs to the method for preparing submicron metal, particularly prepare the method for ultra-fine column copper powder.
Submicron metal with special shape has peculiar function and purposes.Superifine colummar metallic powder particularly, it is up-and-coming photoelectric conversion material and important optical material, also is a kind of novel pigment, can also be as the special toughener of high molecule plastic.Therefore, the preparation of submicron metal has caused the preparation method of people's attention, particularly superifine colummar metallic powder, and people are in research mutually unexpectedly.American A.Marks has reported several methods that prepare superifine colummar metallic powder in the U.S. Pat 3813265 that obtained in 1974, wherein best is the method for growing metal whisker on tinsel, its basic technology is: two tinsels are placed in the rare gas element that contains this metallic vapor abreast, two metal sheets is at a distance of several millimeters, and keep certain temperature head, the dividing potential drop of the temperature of pilot-gas, air pressure and metallic vapor just vertically grows metal whisker on a colder tinsel rightly.This metal whisker is the bigger superifine colummar metallic powder of length-to-diameter.But this method will keep having between the minimum two metal sheets of spacing the temperature difference of appropriate (several degrees centigrade) in implementation process, need accurate heating and measuring and controlling temp system; In addition, it is also difficult to modulate gas total pressure and metallic vapor dividing potential drop simultaneously; And, for common metal, be with rare gas element as the diluent gas of metallic vapor, oxygen and nitrogen should strictly be removed, thereby the growth room should be evacuated earlier, and and atmospheric isolation; Also, can not recycle, have only small amount of steam to be grown to whisker, so the waste of material is bigger because a large amount of metallic vapor can be deposited in the growth room.
The objective of the invention is to propose a kind of novel method for preparing ultra-fine column copper powder with the electrolysis solidified electrolyte.This method prepares the bigger ultra-fine column copper powder of length-to-diameter easily, and technology is simple, does not need vacuum condition and precise control system, and does not have the waste of material.
Main points of the present invention are to be diameter 1000-2000
Small copper particle add in a kind of salts solution of copper, this salts solution is that mantoquita concentration is the aqueous solution of 5-10%, this solution is contained in nonconducting container, and stirring makes copper particle be suspended in the solution equably, and with solution curing, be solidified electrolyte to call this solidified salts solution in the following text, add copper electrode at the two ends of solidified electrolyte, pass to galvanic current, current density is 250-300 μ A/cm
2, be tens to tens hours conduction time, treat that copper particle grows up to ultra-fine column particulate gradually after, with solidified electrolyte liquefaction, the ultra-fine column copper separation of particles in the solution is come out again with whizzer, just obtain ultra-fine column copper powder.
Principle of the present invention is to add top electrode at the two ends of solidified electrolyte, passes to galvanic current, so the copper positive ion in the solidified electrolyte will move along direction of an electric field, when it contacts with copper particle, obtains electronics and is reduced to copper atom, and be deposited on the copper particle.Like this, the copper particle that adds in advance in the salts solution plays a part growth cores, and because salts solution is cured, and these copper particle can not be done random motion or rotation, the orientation of each copper particle is changeless to electric field.Therefore, its direction of growth also remains unchanged, and it will constantly obtain copper atom and grow along the reverse direction of electric field, become ultra-fine column particulate gradually.
Accompanying drawing 1 is the synoptic diagram of electrolysis solidified electrolyte.
Accompanying drawing 2 is the stereoscan photographs that utilize the ultra-fine column copper powder that the present invention prepares, (amplifying 10,000 times).
The invention will be further described below in conjunction with drawings and Examples.
The salts solution of the copper that the present invention is used can be the organic solution or the aqueous solution, by stirring, vibration or ultrasonication copper particle is suspended in the solution equably.The solidified mode can be to dissolve in organic polymer to make it to become full-bodied colloid in solution, also can solution is freezing and solidify.As shown in Figure 1, solidified electrolyte A contains in container B, adds top electrode C at the two ends of solidified electrolyte A, and electrode C available metal or graphite are made.Two electrode C link with the positive-negative output end of direct supply D respectively, and the electric current that applies can be direct current or pulsating direct current, also can be that direct current adds pulsating direct current, can also be to replace reverse direct current with some cycles to add pulsating direct current.By concentration, temperature, current density and the conduction time of control salts solution, just can control the length of ultra-fine column copper particulate, obtain required length-to-diameter.
Embodiment 1: with diameter is 1000
About copper particle to add weight concentration be 10% CuSO
4In the aqueous solution, solution is contained in the synthetic glass container, stirs, and is refrigerated to icing.Make electrode with copper coin, electric current is a direct current, and current density is 300 μ A/cm
2, switch on after tens hours the CuSO that freezes
4The aqueous solution thaws, and separates obtaining the superfine copper powder again with whizzer, its stereoscan photograph as shown in Figure 2, the diameter of particulate is 1000 in the powder
About, length-to-diameter is 3 to 8.
Embodiment 2: with diameter is 1000 to 2000
Copper particle to add weight concentration be 5% CuCl
2In the aqueous solution, the temperature of solution is a room temperature, and solution is contained in Glass Containers, and dissolve polyvinyl alcohol also stirs and becomes full-bodied colloid in solution, makes electrode with copper coin, adds a pulsating direct current between two electrodes, and current density is 250 μ A/cm
2, switch on after tens hours, grow length-to-diameter greater than 5 column copper particulate, separate with whizzer then and obtain ultra-fine column copper powder.
The present invention adopts the electrolysis solidified electrolyte to prepare ultra-fine column copper powder, because copper particle is oriented growth in solidified electrolyte, this is the column particulate with regard to the copper powder that has guaranteed preparation; And the factor that influences particulate length is concentration, temperature, current density and the conduction time of salts solution, and these need general device with regard to may command, and processing ease, so compared with the prior art, technology of the present invention is simple.In addition, the growth of column particulate can also realize in concentration, temperature and the current density range of broad.The present invention is when the electrolysis solidified electrolyte, and the copper that electrolysis goes out is partly long, and another part is then collected by negative potential, and can regain utilization on column copper particulate, therefore, and can waste material.
Claims (3)
1, the method for the ultra-fine column copper powder of preparation is characterized in that with diameter be 1000-2000
Copper particle add in a kind of aqueous solution of mantoquita, mantoquita concentration is 5-10%, this salts solution is contained in nonconducting container, and stir, copper particle evenly is suspended in the solution, solution is solidified, two ends at solidified electrolyte add copper electrode, are 250-300 μ A/cm by current density
2Galvanic current, be tens to tens hours conduction time, treat that copper particle grows into ultra-fine column particulate after, with solidified electrolyte liquefaction, the ultra-fine column copper separation of particles in the solution is come out with whizzer.
2, according to the method for claim 1, it is characterized in that solution is solidified, the solidified mode can be that solution is freezing, also can be to dissolve in organic polymer (as polyvinyl alcohol) in solution.
3, according to the method for claim 1 or 2, it is characterized in that galvanic current can be direct current or pulsating direct current, also can be that direct current adds pulsating direct current, can also be to replace reverse direct current with some cycles to add pulsating direct current.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88105875 CN1019459B (en) | 1988-03-09 | 1988-03-09 | Fabrication method of superifine colummar metallic powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88105875 CN1019459B (en) | 1988-03-09 | 1988-03-09 | Fabrication method of superifine colummar metallic powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1035629A CN1035629A (en) | 1989-09-20 |
| CN1019459B true CN1019459B (en) | 1992-12-16 |
Family
ID=4833997
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88105875 Expired CN1019459B (en) | 1988-03-09 | 1988-03-09 | Fabrication method of superifine colummar metallic powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1019459B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW561085B (en) * | 2001-10-29 | 2003-11-11 | Phild Co Ltd | Method and device for producing metal powder |
| CN1844473B (en) * | 2005-04-06 | 2010-09-01 | 四川大学 | Electrolytic emulsifying method for grain size controllable copper, silver and etc. ultrafine metal powder |
| CN111761069B (en) * | 2020-09-01 | 2020-12-01 | 西安赛隆金属材料有限责任公司 | Powder making equipment and method |
-
1988
- 1988-03-09 CN CN 88105875 patent/CN1019459B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN1035629A (en) | 1989-09-20 |
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