CN107876795B - Preparation method of single crystal copper powder - Google Patents
Preparation method of single crystal copper powder Download PDFInfo
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- CN107876795B CN107876795B CN201711269097.6A CN201711269097A CN107876795B CN 107876795 B CN107876795 B CN 107876795B CN 201711269097 A CN201711269097 A CN 201711269097A CN 107876795 B CN107876795 B CN 107876795B
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000013078 crystal Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 18
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229940116318 copper carbonate 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 12
- 239000005751 Copper oxide Substances 0.000 claims abstract description 10
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 7
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 6
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 6
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000010419 fine particle 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
- 239000007810 chemical reaction solvent Substances 0.000 claims abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 5
- 239000002270 dispersing agent Substances 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000011049 filling Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000006185 dispersion Substances 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 230000004048 modification Effects 0.000 claims description 9
- 238000012986 modification Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- 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
- 230000003064 anti-oxidating effect Effects 0.000 claims description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 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
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 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
- 150000002334 glycols Chemical class 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 7
- 239000001301 oxygen Substances 0.000 abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 abstract description 7
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000005054 agglomeration Methods 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
- 239000002243 precursor Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000011882 ultra-fine particle Substances 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 2
- 239000010953 base metal Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003985 ceramic capacitor Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 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
- 239000008213 purified water Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
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- 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
Abstract
The invention provides a preparation method of single crystal copper powder, which comprises the following steps: adding copper sulfate aqueous solution and sodium carbonate aqueous solution into a reaction container at the same time, reacting to generate basic copper carbonate, washing a reaction product, and drying water; placing basic copper carbonate on a belt type sintering furnace for calcining to obtain copper oxide fine particles; and adding a reaction solvent ethylene glycol, a reducing agent and a reaction promoter into a closed reaction container, adding copper oxide fine particles, filling protective gas into the reaction container, stirring and heating for reaction to obtain the single-crystal superfine copper powder. And uniformly mixing the single-crystal superfine copper powder, the surface antioxidant dispersant and the solvent, adding the mixture into a roller dispersing machine, carrying out ball milling, dispersing and modifying treatment, and then drying the copper powder in vacuum to obtain the single-crystal monodisperse copper powder. By adopting the technical scheme of the invention, the obtained copper powder has low oxygen content, good oxidation resistance, good conductivity, monodisperse single crystal, narrow particle size distribution and high tap density.
Description
Technical Field
The invention belongs to the technical field of metal material preparation, and particularly relates to a preparation method of single crystal copper powder.
Background
With the rapid development of the electronic information field, the demand of high-performance and high-precision electronic paste is increasing day by day, and the base metal electronic paste is widely applied to the fields of conductive paste, conductive adhesive, battery shielding coating and the like due to the lower price and excellent conductive performance of the base metal electronic paste compared with noble metal. Copper is a raw material for manufacturing electronic paste with high cost performance, and the copper powder for manufacturing the electronic paste generally has the defects of coarse particle size distribution, poor oxidation resistance, high oxygen content, poor conductivity and the like. In particular, the requirement for the copper electronic paste for the multilayer ceramic capacitor is higher.
Disclosure of Invention
Aiming at the technical problems, the invention discloses a preparation method of single crystal copper powder, and the obtained copper powder has low oxygen content, good conductivity, monodisperse single crystal and small particle size distribution.
In contrast, the technical scheme adopted by the invention is as follows:
a preparation method of single-crystal copper powder comprises the following steps:
step S1, adding the copper sulfate aqueous solution and the sodium carbonate aqueous solution into a reaction container at the same time, reacting to generate basic copper carbonate, washing the reaction product, and drying the water; placing basic copper carbonate on a belt type sintering furnace for calcining to obtain copper oxide fine particles;
and step S2, adding a reaction solvent, a reducing agent and a reaction promoter into the high-temperature high-pressure closed reaction container, adding copper oxide fine particles, filling protective gas into the reaction container, stirring and heating for reaction to obtain the single-crystal superfine copper powder. Further, the reaction solvent is ethylene glycol;
the technical scheme is that the superfine copper powder is prepared by chemical reaction in a pure solvent under the environment of high-temperature protective atmosphere. The high polarity of water easily causes the agglomeration of powder particles, and contains a large amount of active hydrogen bonds, which causes the high oxygen content of the copper powder. The invention adds a reaction control agent to control the reaction rate in a pure solvent system and in a high-temperature protective atmosphere environment, and is beneficial to preparing single crystal powder. The reaction solvent ethylene glycol is a non-polar substance, the intermolecular force is average, an oxygen-free and isotropic reaction environment can be provided, and the powder agglomeration can be reduced.
And step S3, uniformly mixing the prepared superfine copper powder, the surface antioxidant dispersant and the solvent, adding the mixture into a roller dispersion machine, carrying out ball milling dispersion modification treatment, discharging after dispersion, and carrying out vacuum drying on the copper powder to obtain the single-crystal monodisperse copper powder.
The technical scheme is that the copper powder is subjected to ball milling anti-oxidation dispersion modification in a roller ball mill, so that the superfine copper powder has high surface energy, is easy to oxidize and agglomerate, and can influence the conductivity and the use performance of the copper powder. The invention can improve the oxidation resistance of the copper powder by ball milling, anti-oxidation dispersion modification, and simultaneously increase the dispersibility of the copper powder to achieve the monodispersion effect.
In step S3, the surface antioxidant dispersant is polyethylene glycol or polyethylene glycol esters, and the solvent is absolute ethanol.
As a further improvement of the invention, in step S3, the time of the antioxidant dispersion modification treatment is 1-3 h.
As a further improvement of the invention, the reducing agent is one or a mixture of two of alkanol ammonia, triethanolamine, diethanolamine and monoethanolamine.
As a further improvement of the invention, the reaction promoter is one or a mixture of two of sodium hydroxide, potassium hydroxide, sodium borohydride and potassium borohydride.
As a further improvement of the invention, the protective gas is nitrogen or argon.
As a further improvement of the invention, in step S2, the temperature of the heating reaction is 120-195 ℃. The reaction temperature is 120-195 ℃, the reaction speed is high, oxygen in the copper oxide can be rapidly removed, the oxygen content in the copper is reduced, and the agglomeration phenomenon of powder particles caused by the influence of intermolecular acting force of the copper is also reduced.
As a further improvement of the invention, in step S1, the calcination time is 1-3 h.
Compared with the prior art, the invention has the beneficial effects that:
by adopting the technical scheme of the invention, the obtained copper powder has low oxygen content, good oxidation resistance, good conductivity, monodispersion of single crystal, particle size distribution of 0.1-5um and tap density of up to 4.5g/cm3It is suitable for multilayer ceramic capacitor copper electronic paste.
Drawings
FIG. 1 is a scanning electron microscope image of single-crystal ultra-fine copper powder prepared in example 1 of the present invention, magnified 5000 times.
FIG. 2 is a scanning electron microscope image of the single-crystal ultra-fine copper powder prepared in example 1 of the present invention magnified 1000 times.
Detailed Description
Preferred embodiments of the present invention are described in further detail below.
Example 1
A preparation method of single-crystal fine copper powder comprises the following steps:
(1) a precursor conversion step: first prepare 1m3The 1mol/L copper sulfate solution and the 1.5mol/L sodium carbonate solution are simultaneously dripped into a reaction vessel through a pipeline to react to generate basic copper carbonate, a reaction product is washed, and water is dried. And (3) calcining the basic copper carbonate on a belt type sintering furnace at 300 ℃ for 2h to obtain copper oxide ultrafine particles.
(2) A solvent thermal reduction step: adding 400L of ethylene glycol, 20L of triethanolamine, 200kg of copper oxide powder and 5kg of sodium hydroxide into a high-temperature high-pressure closed reaction container, keeping the nitrogen environment in the container, heating to 160 ℃, reacting for 1h, cooling, performing solid-liquid separation, washing for 3 times by using absolute ethyl alcohol, and performing vacuum drying to obtain the superfine copper powder.
(3) Ball milling, anti-oxidation, dispersion and modification: 100kg of zirconia bar, 20kg of superfine copper powder and 40L of absolute ethyl alcohol are added into a 100L roller ball mill,40g of polyethylene glycol, modifying for 2 hours, discharging, and drying in vacuum to obtain the single crystal monodisperse copper powder. The scanning electron micrographs of the obtained copper powder are shown in FIG. 1 and FIG. 2, and it can be seen from FIG. 1 and FIG. 2 that the obtained copper powder has uniform particles, good dispersibility and less aggregation. Through detection, the particle size distribution of the copper powder is 0.1-5um, and the tap density reaches 4.2g/cm3。
Example 2
A preparation method of single-crystal fine copper powder comprises the following steps:
(1) a precursor conversion step: first prepare 1m3The 1mol/L copper sulfate solution and the 1.5mol/L sodium carbonate solution are simultaneously dripped into a reaction vessel through a pipeline to react to generate basic copper carbonate, a reaction product is washed, and water is dried. And (3) calcining the basic copper carbonate on a belt type sintering furnace at 300 ℃ for 2h to obtain copper oxide ultrafine particles.
(2) A solvent thermal reduction step: adding 400L of ethylene glycol, 20L of triethanolamine, 200kg of copper oxide powder and 2kg of sodium borohydride into a high-temperature high-pressure closed reaction container, maintaining a vacuum negative pressure environment in the container, heating to 170 ℃, reacting for 1h, cooling, performing solid-liquid separation, washing for 3 times with absolute ethyl alcohol, and performing vacuum drying to obtain the superfine copper powder.
(3) Ball milling, anti-oxidation, dispersion and modification: 100kg of zirconia rod, 20kg of superfine copper powder, 40L of absolute ethyl alcohol and 20g of polyethylene glycol ester are added into a 100L roller ball mill, modification treatment is carried out for 1h, and the single crystal monodisperse copper powder is discharged and dried in vacuum. The detection shows that the particle size distribution of the obtained copper powder is 0.1-3um, and the tap density is as high as 4.5g/cm3。
Comparative example 1
A preparation method of single-crystal fine copper powder comprises the following steps:
(1) a precursor conversion step: first prepare 1m3The 1mol/L copper sulfate solution and the 1.5mol/L sodium carbonate solution are simultaneously dripped into a reaction vessel through a pipeline to react to generate basic copper carbonate, a reaction product is washed, and water is dried. And (3) calcining the basic copper carbonate on a belt type sintering furnace at 300 ℃ for 2h to obtain copper oxide ultrafine particles.
(2) A solvent thermal reduction step: adding 400L of purified water, 20L of triethanolamine, 200kg of copper oxide powder and 2kg of sodium borohydride into a high-temperature high-pressure closed reaction container, maintaining a vacuum negative pressure environment in the container, heating to 100 ℃, reacting without copper ions, cooling, performing solid-liquid separation, washing with absolute ethyl alcohol for 3 times, and performing vacuum drying to obtain the copper powder.
(3) An anti-oxidation coating step: and adding 20kg of copper powder, 40L of absolute ethyl alcohol and 20g of polyethylene glycol ester into a stirring container, stirring for 1h, and drying in vacuum to obtain the antioxidant coated copper powder. The detection shows that the obtained copper powder has the particle size distribution of 1-20 um and the tap density lower than 2.5 g/cm3。
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (7)
1. A preparation method of single crystal copper powder is characterized by comprising the following steps: which comprises the following steps:
step S1, adding the copper sulfate aqueous solution and the sodium carbonate aqueous solution into a reaction container at the same time, reacting to generate basic copper carbonate, washing the reaction product, and drying the water; placing basic copper carbonate on a belt type sintering furnace for calcining to obtain copper oxide fine particles;
step S2, adding reaction solvent ethylene glycol, reducing agent and reaction accelerator into a closed reaction container, then adding copper oxide fine particles, filling protective gas into the reaction container, stirring and heating for reaction to obtain single crystal superfine copper powder;
step S3, uniformly mixing the prepared superfine copper powder, the surface antioxidant dispersant and the solvent, adding the mixture into a roller dispersion machine, carrying out ball milling dispersion modification treatment, discharging after dispersion, and carrying out vacuum drying on the copper powder to obtain single crystal monodisperse copper powder;
in step S2, the temperature of the heating reaction is 120-195 ℃.
2. The method for producing single-crystal copper powder according to claim 1, wherein: the reducing agent is one or a mixture of two of alkanol ammonia, triethanolamine, diethanolamine and ethanolamine.
3. The method for producing single-crystal copper powder according to claim 1, wherein: the reaction promoter is one or a mixture of two of sodium hydroxide, potassium hydroxide, sodium borohydride and potassium borohydride.
4. The method for producing single-crystal copper powder according to claim 1, wherein: the protective gas is nitrogen or argon.
5. The method for producing single-crystal copper powder according to claim 4, wherein: in step S1, the calcination time is 1-3 h.
6. The method for producing single-crystal copper powder according to claim 1, wherein: in step S3, the surface antioxidant dispersant is polyethylene glycol or polyethylene glycol esters, and the solvent is absolute ethanol.
7. The method for producing single-crystal copper powder according to claim 6, wherein: in step S3, the anti-oxidation dispersion modification treatment time is 1-3 h.
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| CN110116218B (en) * | 2019-05-29 | 2022-06-17 | 西安工程大学 | Preparation method of high-purity narrow-particle-size-distribution copper powder |
| CN110919022A (en) * | 2019-08-19 | 2020-03-27 | 张博成 | Preparation method of surface-modified nano-copper particles |
| CN110434346B (en) * | 2019-08-26 | 2021-10-26 | 华南理工大学 | Method for refining large-particle-size pure copper or copper alloy particles by high-energy ball milling method |
| 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 |
| CN110976901A (en) * | 2019-12-31 | 2020-04-10 | 湘潭大学 | Preparation method of nano copper powder |
| 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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| CN101274370A (en) * | 2007-03-26 | 2008-10-01 | 中南大学 | Method for preparing monodisperse high-crystallinity copper powder |
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