CN107876795A - A kind of preparation method of monocrystalline copper powder - Google Patents
A kind of preparation method of monocrystalline copper powder Download PDFInfo
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- CN107876795A CN107876795A CN201711269097.6A CN201711269097A CN107876795A CN 107876795 A CN107876795 A CN 107876795A CN 201711269097 A CN201711269097 A CN 201711269097A CN 107876795 A CN107876795 A CN 107876795A
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- copper powder
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- copper
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 20
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 18
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229960004643 cupric oxide Drugs 0.000 claims abstract description 12
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- 229940116318 copper carbonate Drugs 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 6
- 238000005245 sintering Methods 0.000 claims abstract description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 230000001681 protective effect Effects 0.000 claims abstract description 5
- 238000010301 surface-oxidation reaction Methods 0.000 claims abstract description 5
- 239000002270 dispersing agent Substances 0.000 claims abstract description 4
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 3
- 239000006185 dispersion Substances 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000003963 antioxidant agent Substances 0.000 claims description 8
- 230000003078 antioxidant effect Effects 0.000 claims description 8
- 235000006708 antioxidants Nutrition 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- 229940043237 diethanolamine Drugs 0.000 claims description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 150000002334 glycols Chemical class 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical group [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 7
- 239000001301 oxygen Substances 0.000 abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 6
- 230000003026 anti-oxygenic effect Effects 0.000 abstract description 4
- 230000005611 electricity Effects 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 3
- 229910052802 copper Inorganic materials 0.000 description 9
- 239000010949 copper Substances 0.000 description 9
- 239000002002 slurry Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- RFVNOJDQRGSOEL-UHFFFAOYSA-N 2-hydroxyethyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCCO RFVNOJDQRGSOEL-UHFFFAOYSA-N 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229950007687 macrogol ester Drugs 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention provides a kind of preparation method of monocrystalline copper powder, it comprises the following steps：Copper sulfate solution and aqueous sodium carbonate are added drop-wise in reaction vessel simultaneously, reaction generation basic copper carbonate, washing reaction product, dry moisture content；Basic copper carbonate is placed on belt sintering stove and calcined, obtains cupric oxide fine grained；In closed reaction vessel, reaction dissolvent ethylene glycol, reducing agent, reaction promoter are added, adds cupric oxide fine grained, and protective gas is filled with reaction vessel, stirred simultaneously heating response, obtain monocrystalline superfine cupper powder.Monocrystalline superfine cupper powder, surface oxidation-resistant dispersant, solvent are well mixed and be added in roller dispersion machine, the processing of ball milling disperse modified, copper powder is then dried in vacuo, obtains monocrystalline single dispersing copper powder.Using technical scheme, obtained copper powder oxygen content is low, and antioxygenic property is good, conducts electricity very well, and single crystals single dispersing, particle diameter distribution is narrow, and tap density is high.
Description
Technical field
The invention belongs to technical field of metal material preparation, more particularly to a kind of preparation method of monocrystalline copper powder.
Background technology
With the fast development of electronic information field, high-performance and high accuracy electric slurry demand is growing, base metal electricity
Sub- slurry with the price lower than noble metal, excellent electric conductivity due to being widely used in electrocondution slurry, conducting resinl, battery panel
Cover the fields such as coating.Copper is a kind of raw material of the higher making electric slurry of cost performance, makes the copper powder of electric slurry at present
Common have that particle diameter distribution is thick, and antioxygenic property is poor, and oxygen content is high, electric conductivity difference etc..Especially for multi-layer ceramic capacitance
Device is higher with the requirement of copper electric slurry.
The content of the invention
For above technical problem, the invention discloses a kind of preparation method of monocrystalline copper powder, obtained copper powder oxygen content
It is low, conduct electricity very well, single crystals single dispersing, particle diameter distribution is small.
On the other hand, the technical solution adopted by the present invention is：
A kind of preparation method of monocrystalline copper powder, it comprises the following steps：
Step S1, copper sulfate solution and aqueous sodium carbonate are added drop-wise in reaction vessel simultaneously, reaction generation basic carbonate
Copper, washing reaction product, dry moisture content；Basic copper carbonate is placed on belt sintering stove and calcined, obtains cupric oxide fine grained；
Step S2, in high temperature high pressure enclosed reaction vessel, reaction dissolvent, reducing agent, reaction promoter are added, adds oxidation
Copper fine grained, and protective gas is filled with reaction vessel, simultaneously heating response is stirred, obtains monocrystalline superfine cupper powder.Further,
The reaction dissolvent is ethylene glycol；
This technical scheme is under high temperature protection atmosphere, and in neat solvent carrying out chemical reaction prepares superfine cupper powder.Due to
The polarity of water is larger, easily causes the reunion of powder granule, and containing substantial amounts of active hydrogen bond, the oxygen content of copper powder can be caused high.
The present invention is in neat solvent system, in high temperature protection atmosphere, adds reaction controlling agent control reaction rate, is advantageous to make
Standby monocrystalline powder.Reaction dissolvent ethylene glycol is apolar substance, and intermolecular force is average, it is possible to provide an anaerobic, each identical
The reaction environment of property, can reduce powder reuniting.
Step S3, it is added to the superfine cupper powder prepared, surface oxidation-resistant dispersant, solvent are well mixed roller and disperses
In machine, the processing of ball milling disperse modified, discharging vacuum drying copper powder, finally obtains monocrystalline single dispersing copper powder after the completion of disperseing.
This technical scheme is to carry out the anti-oxidant disperse modified of ball milling, superfine cupper powder surface energy to copper powder in tumbling ball mill
Height, it is oxidizable, easily reunite, the electric conductivity and performance of copper powder can be influenceed.The present invention by the anti-oxidant disperse modified of ball milling,
The antioxygenic property of copper powder can be lifted, while increases the dispersiveness of copper powder, reaches single dispersing effect.
As a further improvement on the present invention, in step S3, surface oxidation-resistant dispersant is polyethylene glycol or poly- second two
Alkoxide, solvent are absolute ethyl alcohol.
As a further improvement on the present invention, in step S3, anti-oxidant disperse modified processing time 1-3h.
As a further improvement on the present invention, the reducing agent is alkanol ammonia, triethanolamine, diethanol amine, an ethanol
One or two kinds of mixture in amine.
As a further improvement on the present invention, the reaction promoter is sodium hydroxide, potassium hydroxide, sodium borohydride, boron
One or two kinds of mixture in hydrofining.
As a further improvement on the present invention, the protective gas is nitrogen or argon gas.
As a further improvement on the present invention, in step S2, the temperature of the heating response is 120 DEG C ~ 195 DEG C.Reaction
For temperature at 120 DEG C ~ 195 DEG C, reaction speed is fast, can be rapidly the oxygen in cupric oxide be sloughed, reduces the oxygen content in copper, together
When also reduce influence of the copper due to intermolecular active force, cause the agglomeration of powder granule.
As a further improvement on the present invention, in step S1, calcination time is 1 ~ 3h.
Compared with prior art, beneficial effects of the present invention are：
Using technical scheme, the oxygen content of obtained copper powder is low, and antioxygenic property is good, conducts electricity very well, single crystals
Single dispersing, particle diameter distribution are up to 4.5g/cm in 0.1-5um, tap density3, suitable for multilayer ceramic capacitor copper electric slurry.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph that the monocrystalline superfine cupper powder that the embodiment of the present invention 1 is prepared amplifies 5000 times.
Fig. 2 is the scanning electron microscope (SEM) photograph that the monocrystalline superfine cupper powder that the embodiment of the present invention 1 is prepared amplifies 1000 times.
Embodiment
The preferably embodiment of the present invention is described in further detail below.
Embodiment 1
A kind of preparation method of the thin copper powder of monocrystalline, comprises the following steps：
（1）Presoma step of converting：First prepare 1m31mol/L copper-bath and 1.5mol/L sodium carbonate liquor, lead to
Piping is added drop-wise in reaction vessel simultaneously, reaction generation basic copper carbonate, washing reaction product, dries moisture content.By alkali formula carbon
Sour copper is placed on 300 DEG C of calcining 2h on belt sintering stove, obtains cupric oxide ultra-fine grain.
（2）Solvothermal step：In high temperature high pressure enclosed reaction vessel, ethylene glycol 400L, triethanolamine are added
20L, cupric oxide powder 200kg, sodium hydroxide 5kg, nitrogen environment in axe is kept, be heated to 160 DEG C, react 1h, through cooling, solid-liquid
Separation, absolute ethyl alcohol wash 3 times, are dried in vacuo and superfine cupper powder is made.
（3）The anti-oxidant disperse modified step of ball milling：In 100L tumbling ball mill, zirconium oxide rod 100kg is added, it is ultra-fine
Copper powder 20kg, absolute ethyl alcohol 40L, polyethylene glycol 40g, modification 2h, monocrystalline single dispersing copper powder after discharging vacuum drying.Obtain
Copper powder scanning electron microscope (SEM) photograph as depicted in figs. 1 and 2, from Fig. 1 and Fig. 2, obtained copper powder particle is uniform, scattered, group
It is poly- few.By detection, the particle diameter distribution of copper powder reaches 4.2g/cm in 0.1-5um, tap density3。
Embodiment 2
A kind of preparation method of the thin copper powder of monocrystalline, comprises the following steps：
（1）Presoma step of converting：First prepare 1m31mol/L copper-bath and 1.5mol/L sodium carbonate liquor, lead to
Piping is added drop-wise in reaction vessel simultaneously, reaction generation basic copper carbonate, washing reaction product, dries moisture content.By alkali formula carbon
Sour copper is placed on 300 DEG C of calcining 2h on belt sintering stove, obtains cupric oxide ultra-fine grain.
（2）Solvothermal step：In high temperature high pressure enclosed reaction vessel, ethylene glycol 400L, triethanolamine are added
20L, cupric oxide powder 200kg, sodium borohydride 2kg, negative pressure of vacuum environment in axe is kept, be heated to 170 DEG C, react 1h, through cooling down,
Separation of solid and liquid, absolute ethyl alcohol wash 3 times, are dried in vacuo and superfine cupper powder is made.
（3）The anti-oxidant disperse modified step of ball milling：In 100L tumbling ball mill, zirconium oxide rod 100kg is added, it is ultra-fine
Copper powder 20kg, absolute ethyl alcohol 40L, macrogol ester 20g, modification 1h, monocrystalline single dispersing copper powder after discharging vacuum drying.Through
Detection is crossed, the particle diameter distribution of obtained copper powder is up to 4.5g/cm in 0.1-3um, tap density3。
Comparative example 1
A kind of preparation method of the thin copper powder of monocrystalline, comprises the following steps：
（1）Presoma step of converting：First prepare 1m31mol/L copper-bath and 1.5mol/L sodium carbonate liquor, lead to
Piping is added drop-wise in reaction vessel simultaneously, reaction generation basic copper carbonate, washing reaction product, dries moisture content.By alkali formula carbon
Sour copper is placed on 300 DEG C of calcining 2h on belt sintering stove, obtains cupric oxide ultra-fine grain.
（2）Solvothermal step：In high temperature high pressure enclosed reaction vessel, 400L pure water, triethanolamine are added
20L, cupric oxide powder 200kg, sodium borohydride 2kg, negative pressure of vacuum environment in axe is kept, 100 DEG C is heated to, reacts no copper ion,
Through cooling, separation of solid and liquid, absolute ethyl alcohol washs 3 times, is dried in vacuo and copper powder is made.
（3）Anti-oxidant encapsulation steps：In stirring container, copper powder 20kg, absolute ethyl alcohol 40L, macrogol ester are added
20g, stirs 1h, and vacuum drying obtains anti-oxidant cladding copper powder.By detection, obtained copper powder size is distributed in 1-20um, shaken
Real density is less than 2.5 g/cm3。
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to is assert
The specific implementation of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of not departing from present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention's
Protection domain.
Claims (8)
- A kind of 1. preparation method of monocrystalline copper powder, it is characterised in that：It comprises the following steps：Step S1, copper sulfate solution and aqueous sodium carbonate are added drop-wise in reaction vessel simultaneously, reaction generation basic carbonate Copper, washing reaction product, dry moisture content；Basic copper carbonate is placed on belt sintering stove and calcined, obtains cupric oxide fine grained；Step S2, in closed reaction vessel, reaction dissolvent ethylene glycol, reducing agent, reaction promoter are added, adds cupric oxide Fine grained, and protective gas is filled with reaction vessel, simultaneously heating response is stirred, obtains monocrystalline superfine cupper powder；Step S3, the superfine cupper powder prepared, surface oxidation-resistant dispersant, solvent are well mixed and are added to roller dispersion machine In, the processing of ball milling disperse modified, discharging vacuum drying copper powder, finally obtains monocrystalline single dispersing copper powder after the completion of disperseing.
- 2. the preparation method of monocrystalline copper powder according to claim 1, its feature exist：The reducing agent is alkanol ammonia, three One or two kinds of mixture in monoethanolamine, diethanol amine, monoethanolamine.
- 3. the preparation method of monocrystalline copper powder according to claim 1, it is characterised in that：The reaction promoter is hydroxide One or two kinds of mixture in sodium, potassium hydroxide, sodium borohydride, potassium borohydride.
- 4. the preparation method of monocrystalline copper powder according to claim 1, it is characterised in that：The protective gas is nitrogen or argon Gas.
- 5. the preparation method of the monocrystalline copper powder according to claim 1 ~ 4 any one, it is characterised in that：In step S2, institute The temperature for stating heating response is 120 DEG C ~ 195 DEG C.
- 6. the preparation method of monocrystalline copper powder according to claim 5, it is characterised in that：In step S1, calcination time be 1 ~ 3h。
- 7. the preparation method of monocrystalline copper powder according to claim 1, it is characterised in that：In step S3, surface oxidation-resistant point Powder is polyethylene glycol or polyethylene glycol esters, and solvent is absolute ethyl alcohol.
- 8. the preparation method of monocrystalline copper powder according to claim 7, it is characterised in that：It is anti-oxidant to disperse to change in step S3 Property processing time 1-3h.
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| CN201711269097.6A CN107876795B (en) | 2017-12-05 | 2017-12-05 | Preparation method of single crystal copper powder |
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| CN201711269097.6A CN107876795B (en) | 2017-12-05 | 2017-12-05 | Preparation method of single crystal copper powder |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110116218A (en) * | 2019-05-29 | 2019-08-13 | 西安工程大学 | A kind of preparation method of the narrow copper powder of high-purity particle diameter distribution |
| CN110434346A (en) * | 2019-08-26 | 2019-11-12 | 华南理工大学 | A kind of method that high-energy ball milling method refines big partial size fine copper or copper alloy particle |
| CN110560702A (en) * | 2019-09-16 | 2019-12-13 | 上海交通大学 | method for preparing micron-sized single crystal copper powder at room temperature |
| CN110919022A (en) * | 2019-08-19 | 2020-03-27 | 张博成 | Preparation method of surface-modified nano-copper particles |
| CN110976901A (en) * | 2019-12-31 | 2020-04-10 | 湘潭大学 | Preparation method of nano copper powder |
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| CN114378300A (en) * | 2022-01-21 | 2022-04-22 | 重庆科技学院 | Method for preparing nano copper powder by using copper oxide as raw material |
| CN114378300B (en) * | 2022-01-21 | 2023-10-20 | 重庆科技学院 | Method for preparing nanometer copper powder by taking copper oxide as raw material |
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