CN109763128A - A kind of method that alloy corrosion method prepares ultra-fine flakey copper powder - Google Patents
A kind of method that alloy corrosion method prepares ultra-fine flakey copper powder Download PDFInfo
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- CN109763128A CN109763128A CN201910224408.XA CN201910224408A CN109763128A CN 109763128 A CN109763128 A CN 109763128A CN 201910224408 A CN201910224408 A CN 201910224408A CN 109763128 A CN109763128 A CN 109763128A
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- copper powder
- ball
- fine
- ultra
- hydrochloric acid
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 238000000034 method Methods 0.000 title claims abstract description 33
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 30
- 239000000956 alloy Substances 0.000 title claims abstract description 30
- 230000007797 corrosion Effects 0.000 title claims abstract description 14
- 238000005260 corrosion Methods 0.000 title claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000010949 copper Substances 0.000 claims abstract description 40
- 229910052802 copper Inorganic materials 0.000 claims abstract description 39
- 238000000498 ball milling Methods 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000001301 oxygen Substances 0.000 claims abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 11
- 238000005520 cutting process Methods 0.000 claims description 9
- 239000011701 zinc Substances 0.000 claims description 9
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 8
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 5
- 229910001882 dioxygen Inorganic materials 0.000 claims description 5
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 8
- 239000002184 metal Substances 0.000 abstract description 7
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 239000008367 deionised water Substances 0.000 abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 abstract 1
- 239000002002 slurry Substances 0.000 description 9
- 238000000227 grinding Methods 0.000 description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 3
- 239000005751 Copper oxide Substances 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 3
- 229910000431 copper oxide Inorganic materials 0.000 description 3
- 229940105296 zinc peroxide Drugs 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910001369 Brass Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- TVZPLCNGKSPOJA-UHFFFAOYSA-N copper zinc Chemical compound [Cu].[Zn] TVZPLCNGKSPOJA-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention relates to a kind of methods that alloy corrosion method prepares ultra-fine flakey copper powder, belong to metal powder material field, preparation method is the following steps are included: be cut into area 0.8-1.5cm2 for ormolu piece, being immersed in mass percentage concentration is in 5%-10% hydrochloric acid solution, solution is heated to 35 DEG C -45 DEG C, and oxygen blast stirring is reacted 1-3 hours, it is washed with deionized water, dries, ball milling, obtaining ultra-fine flakey copper powder.Compared with preparing flake copper powder by fine copper ball milling, the ultra-fine flakey copper powder production cost of gained is low by the method for the invention, and raw material is easy to get, preparation flow is simple, and Ball-milling Time is short, and flake copper powder regular shape, radius-thickness ratio are big, even particle size distribution has high economic benefit.
Description
Technical field
The present invention relates to metal powder material field, specifically a kind of alloy corrosion method prepares the side of ultra-fine flakey copper powder
Method.
Background technique
Important component of the copper powder as conductive phase in electric slurry is widely used in the side such as electrocondution slurry, conducting resinl
Face.The pattern and partial size of copper powder have a very big impact the electric conductivity of slurry, the copper powder of people's preparation generally comprise it is spherical and
Two kinds of sheet.Wherein spherical copper powder is mainly point contact, and contact area is smaller, and flake copper powder is usually face contact, more furthermore
Large specific surface area, thus it is more preferable by the copper conductor slurry electric conductivity that flake copper powder is prepared.Currently, people pass through to fine copper
Carry out mechanical ball mill prepare flake copper powder, obtained flake copper powder shape size is different, and profile pattern is poor, electric conductivity compared with
It is weak.Therefore, the flake copper powder for preparing a kind of epigranular, regular shape has the electric conductivity for improving copper conductor slurry important
It influences.
Summary of the invention
For deficiency existing for present technology, the present invention provides the side that a kind of alloy corrosion method prepares ultra-fine flakey copper powder
Method, the flake copper powder regular shape prepared, radius-thickness ratio are big and even particle size distribution, this method effectively reduce the production of producer
Cost improves production efficiency.
Ormolu is the mixture of copper metal simple substance Cu, zinc metal simple-substance Zn composition.Since the hardness of alloy is greater than it
Metal in component, therefore, the hardness for the brass alloys being made of copper zinc are greater than the hardness of fine copper；Ormolu is immersed in salt
In acid solution, copper is not reacted with hydrochloric acid in alloy, and the zinc in alloy reacts the dissolution that is corroded with hydrochloric acid, and entire ormolu is just only
Remaining copper, sheet metal shows reticular structure after excessive erosion at this time, more crisp, then by after ball milling, can be by netted copper
It is standby to become flake copper powder.Compared with preparing flake copper powder by fine copper ball milling, the ultra-fine flakey copper of gained by the method for the invention
Powder production cost is low, and raw material is easy to get, and preparation flow is simple, and Ball-milling Time is short, and flake copper powder regular shape, radius-thickness ratio are big, granularity
It is evenly distributed, has high economic benefit.
Technical scheme is as follows:
Ormolu is cut into area 0.8-2cm by step (1)2The alloy sheet of left and right；
Step (2) prepares hydrochloric acid solution, and the alloy sheet of well cutting is put into hydrochloric acid solution；
Step (3) carries out hydrochloric acid solution with water-bath to be heated to certain temperature；
Oxygen is passed through in hydrochloric acid solution by plastic catheter, while being stirred by blender hydrochloric acid solution by step (4)
It mixes；
Step (5), reaction 1-3 hours, obtain netted copper sheet, dry after being washed with deionized；
Step (6), by after drying netted copper sheet and medium ball be added ball mill in, be added ball-milling medium, set ball milling turn
Speed and time, mixture is obtained after ball milling；
The mixture in ball grinder is sieved after step (7), grinding, obtained copper powder is washed with deionized 3-5 times, in vacuum
100 DEG C of dryings can be obtained ultra-fine flakey copper powder for 2 hours in drying box.
Preferably, mass percentage zinc is pressed in step (1) between 5%-55%.
Preferably, hydrochloric acid solution mass percentage concentration is 5%-10% in step (2).
Preferably, the hydrochloric acid in step (3) is heated to 35 DEG C -45 DEG C.
Preferably, the high purity oxygen gas that the oxygen being passed through in step (4) is 99.9% or more.Speed of agitator is 200 revs/min.
Preferably, it is washed copper sheet 3-4 times in step (5) by deionized water, then puts 100 DEG C of items in a vacuum drying oven
It is dried 10-15 minutes under part.
Preferably, the mass ratio of netted copper and medium ball is 1:60-80 in step (6).Medium ball is 25 millimeters of diameter phi
Stainless steel ball, hexadecanol is added by the 5%-20% of copper sheet weight and is used as ball-milling medium, when ball milling revolving speed be 1100-1200 turns/
Point, ball milling 3-5 hours.
Compared with prior art, beneficial effects of the present invention are as follows:
The present invention uses ormolu for raw material, when by cutting after sheet alloy be immersed in hydrochloric acid solution, copper in alloy
It is not reacted with hydrochloric acid, the zinc in alloy reacts the dissolution that is corroded with hydrochloric acid, and entire ormolu is just only left copper, at this time sheet metal
Reticular structure is showed after excessive erosion, it is more crisp, then by that netted copper can be prepared into flake copper powder after ball milling.It will
After corrosion reaction netted copper sheet be washed with deionized water, dry, ball milling, obtain ultra-fine flakey copper powder.This method raw material is easy to get,
Preparation flow is simple, at low cost；It is big that ultra-fine flakey copper powder regular shape, radius-thickness ratio is prepared, even particle size distribution.Technique
Simply, Ball-milling Time is short, and production cost is low, has high economic benefit.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
Other attached drawings are obtained according to these attached drawings.
Fig. 1 alloy corrosion method prepares the preparation technology flow chart of ultra-fine flakey copper powder；
The ultra-fine flakey copper powder SEM photograph of Fig. 2, the text below Fig. 2 do not know the content expression for not influencing the attached drawing.
Specific embodiment
Technical solution of the present invention is clearly and completely described with specific example below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained under that premise of not paying creative labor belongs to the model that the present invention protects
It encloses.
Embodiment 1
The ormolu that blocky or column Zn content is 50% is cut into 1cm using cutting element by step (1)2The alloy of left and right
Piece.
Step (2), the hydrochloric acid solution that configuration quality percentage concentration is 10%, are put into hydrochloric acid solution for the alloy sheet of well cutting
In.
Step (3) heats hydrochloric acid solution using water-bath, and being heated to temperature is 45 DEG C.
Step (4) is passed through the high purity oxygen gas that purity is 99.9% or more by plastic catheter into hydrochloric acid solution, leads to simultaneously
It crosses blender to be stirred hydrochloric acid solution, revolving speed is 200 revs/min.
Step (5), when reacted between take out copper sheet after 3 hours, using ionized water to netted copper sheet wash 3-4 times, true
In empty drying box 100 DEG C drying 12 minutes after it is spare.
Step (6), by after drying netted copper sheet and medium ball by weight 1:80 be added ball mill in, medium ball is
The stainless steel ball that 25 millimeters of diameter phi makees abrasive media by 20% addition hexadecanol of netted copper sheet weight, and revolving speed is when ball milling
1200 revs/min, ball milling 5 hours.
The copper powder mixture in ball grinder is sieved after step (7), grinding, obtained copper powder first passes around 10% concentration
Hydrochloric acid washs 3-5 times repeatedly, is then washed with deionized 3-5 times.100 DEG C of dryings can obtain for 2 hours in vacuum oven
To required ultra-fine flakey copper powder.
The flake copper powder obtained by the method, is uniformly dispersed, and partial size is about 1-2 μm, soilless sticking phenomenon.It is surveyed by XRD
Examination discovery, without the peak of zinc and copper oxide, it was demonstrated that made powder is pure copper powder.Its performance is measured after being prepared into slurry sintering, electricity
Resistance is 6-8m Ω, adhesive force 19-23N.The slurry of 2 μm of spherical copper powders preparation lower better than identical conditions.
Embodiment 2
The ormolu that blocky or column Zn content is 50% is cut into 1cm using cutting element by step (1)2The alloy of left and right
Piece.
Step (2), the hydrochloric acid solution that configuration quality percentage concentration is 10%, are put into hydrochloric acid solution for the alloy sheet of well cutting
In.
Step (3) heats hydrochloric acid solution using water-bath, and being heated to temperature is 45 DEG C.
Step (4) is passed through the high purity oxygen gas that purity is 99.9% or more by plastic catheter into hydrochloric acid solution, leads to simultaneously
It crosses blender to be stirred hydrochloric acid solution, revolving speed is 200 revs/min.
Step (5), when reacted between up to after 1 hour, take out netted copper sheet, copper sheet washed 3-4 times using deionized water,
In a vacuum drying oven 100 DEG C drying 15 minutes after it is spare.
Step (6), by after drying copper sheet and medium ball by weight 1:60 be added ball mill in, medium ball is diameter
The stainless steel ball that 25 millimeters of φ.Make abrasive media by 5% addition hexadecanol of copper sheet weight, revolving speed is 1100 revs/min when ball milling,
Ball milling 3 hours, obtain copper powder mixture.
The copper powder mixture in ball grinder is sieved after step (7), grinding, obtained copper powder first passes around 10% concentration
Hydrochloric acid washs 3-5 times repeatedly, is then washed with deionized 3-5 times, obtains within drying 2 hours for 100 DEG C in vacuum oven
Required ultra-fine flakey copper powder.
The flake copper powder obtained by the method, dispersion is more uniform, and partial size is about 1-2 μm, and there are fractions to reunite now
As.It is tested and is found by XRD, without the peak of zinc and copper oxide, it was demonstrated that made powder is pure copper powder.
Embodiment 3
The ormolu that blocky or column Zn content is 50% is cut into area 2cm using cutting element by step (1)2Left and right
Alloy sheet.
Step (2), the hydrochloric acid solution that configuration quality percentage concentration is 8%, are put into hydrochloric acid solution for the alloy sheet of well cutting
In.
Step (3) heats hydrochloric acid solution using water-bath, and heating temperature is 45 DEG C.
Step (4) is passed through the high purity oxygen gas that purity is 99.9% or more by plastic catheter into hydrochloric acid solution, leads to simultaneously
It crosses blender to be stirred hydrochloric acid solution, revolving speed is 200 revs/min.
Step (5), when reacted between up to after 3 hours.Take out copper sheet.Copper sheet is washed 3-4 times using deionized water.True
It is spare after being dried 11 minutes under the conditions of 100 DEG C in empty drying box.
Step (6), by after drying copper sheet and medium ball by weight 1,60 be added ball mills in, medium ball is diameter
The stainless steel ball that 25 millimeters of φ.Make abrasive media by 20% addition hexadecanol of copper sheet weight, revolving speed is 1200 revs/min when ball milling,
Ball milling 5 hours, obtain copper powder mixture.
The copper powder mixture in ball grinder is sieved after step (7), grinding, obtained copper powder first passes around 10% concentration
Hydrochloric acid washs 3-5 times repeatedly, is then washed with deionized 3-5 times.100 DEG C of dryings can obtain for 2 hours in vacuum oven
To required ultra-fine flakey copper powder.
The flake copper powder obtained by the method, is uniformly dispersed, and partial size is about 2-4 μm, soilless sticking phenomenon.It is surveyed by XRD
Examination discovery, without the peak of zinc and copper oxide, it was demonstrated that made powder is pure copper powder.Its performance is measured after being prepared into slurry sintering, electricity
Resistance is 10-15m Ω, adhesive force 14-17N.The slurry of 4 μm of spherical copper powders preparation lower better than identical conditions.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of method that alloy corrosion method prepares ultra-fine flakey copper powder, it is characterised in that the following steps are included:
Step (1), the alloy sheet that ormolu is cut into area 0.8-2cm2；
Step (2) prepares hydrochloric acid solution, and the alloy sheet of well cutting is put into hydrochloric acid solution；
Step (3) heats hydrochloric acid solution with water-bath；
Oxygen is passed through in hydrochloric acid solution by plastic catheter, while being stirred by blender to hydrochloric acid solution by step (4)
Reaction；
Step (5), reaction 1-3 hours, obtain netted copper sheet, dry after being washed with deionized；
Step (6), by after drying netted copper sheet and medium ball be put into ball mill, be added ball-milling medium, set ball milling turn
Speed and time, copper powder mixture is obtained by ball milling；
Step (7), by ball mill copper powder mixture sieving after, obtained copper powder is washed with deionized 3-5 times, in vacuum
Ultra-fine flakey copper powder is obtained within drying 2 hours for 100 DEG C in drying box.
2. the method that alloy corrosion method prepares ultra-fine flakey copper powder according to claim 1, it is characterised in that: step (1)
It is 5%-55% that mass percentage zinc is pressed in the ormolu.
3. alloy corrosion method prepares the preparation method of ultra-fine flakey copper powder according to claim 1, it is characterised in that: step
(2) the hydrochloric acid solution mass percentage concentration is 5%-10%.
4. the method that alloy corrosion method prepares ultra-fine flakey copper powder according to claim 1, it is characterised in that: step (3)
It is described to be heated to be that be heated to temperature be 35 DEG C -45 DEG C.
5. the method that alloy corrosion method prepares ultra-fine flakey copper powder according to claim 1, it is characterised in that: step (4)
In be passed through concentration be 99.9% or more high purity oxygen gas, with promote reaction progress, speed of agitator be 200 revs/min.
6. the method that alloy corrosion method prepares ultra-fine flakey copper powder according to claim 1, it is characterised in that: step (5)
Netted copper sheet is washed with deionized 3-4 times, then puts and dry 10-15 minutes under the conditions of 100 DEG C in a vacuum drying oven.
7. the method that alloy corrosion method prepares ultra-fine flakey copper powder according to claim 1, it is characterised in that: step (6)
In the mass ratio of netted copper sheet and medium ball be 1:60-80, medium ball is 25 millimeters of diameter phi of stainless steel ball, by copper sheet weight
5%-20% hexadecanol be added be used as ball-milling medium, revolving speed is 1100-1200 revs/min, ball milling 3-5 hours when ball milling.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910224408.XA CN109763128B (en) | 2019-03-23 | 2019-03-23 | Method for preparing superfine flaky copper powder by alloy corrosion method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910224408.XA CN109763128B (en) | 2019-03-23 | 2019-03-23 | Method for preparing superfine flaky copper powder by alloy corrosion method |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1513629A (en) * | 2003-08-18 | 2004-07-21 | 昆明理工大学 | Manufacturing method for scale shaped metal powder |
| JP2005530048A (en) * | 2002-06-19 | 2005-10-06 | ナノ パウダーズ インダストリーズ （イスラエル） リミテッド | Method for producing high-purity metal nanopowder and nanopowder produced by this method |
| CN103273056A (en) * | 2013-05-27 | 2013-09-04 | 中国科学院过程工程研究所 | Flake-shaped copper powder and preparing method thereof |
| CN107433328A (en) * | 2017-09-21 | 2017-12-05 | 上海交通大学 | A kind of flake copper for carrying nanometer copper crystal and preparation method thereof |
-
2019
- 2019-03-23 CN CN201910224408.XA patent/CN109763128B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005530048A (en) * | 2002-06-19 | 2005-10-06 | ナノ パウダーズ インダストリーズ （イスラエル） リミテッド | Method for producing high-purity metal nanopowder and nanopowder produced by this method |
| CN1513629A (en) * | 2003-08-18 | 2004-07-21 | 昆明理工大学 | Manufacturing method for scale shaped metal powder |
| CN103273056A (en) * | 2013-05-27 | 2013-09-04 | 中国科学院过程工程研究所 | Flake-shaped copper powder and preparing method thereof |
| CN107433328A (en) * | 2017-09-21 | 2017-12-05 | 上海交通大学 | A kind of flake copper for carrying nanometer copper crystal and preparation method thereof |
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