CN110102757A - A kind of preparation method of the graphene coated copper conducting powder based on fabricated in situ - Google Patents
A kind of preparation method of the graphene coated copper conducting powder based on fabricated in situ Download PDFInfo
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- CN110102757A CN110102757A CN201910299339.9A CN201910299339A CN110102757A CN 110102757 A CN110102757 A CN 110102757A CN 201910299339 A CN201910299339 A CN 201910299339A CN 110102757 A CN110102757 A CN 110102757A
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
Abstract
The preparation method for the graphene coated copper conducting powder based on fabricated in situ that the present invention relates to a kind of.The present invention obtains graphene coated conductive copper powder first using high-molecular polyivnyl alcohol/polyethylene glycol as solid-state carbon source, by high concentration Polymer Solution impregnation technology combination chemical vapor deposition process.Temper carbon alkene in-stiu coating is carried out to above-mentioned graphene copper composite powders, obtains the graphene copper composite conductive powder that graphene coats at high proportion.Graphene has excellent chemical stability, electric conductivity and antiseptic property, the complete coated copper composite powders of graphene are prepared using in-situ chemical vapor deposition technique, composite granule has excellent electric conductivity and corrosion resisting property, to replace existing conductive silver powder and silver-plated copper powder, conductive coating cost is greatlyd save.
Description
Technical field
The preparation method for the graphene coated copper conducting powder based on fabricated in situ that the present invention relates to a kind of, belongs to conduction
The technical field of filler preparation.
Background technique
Conductive coating is one kind of functional coating, has the function of conducting electric current and excludes accumulative charge, is widely applied
In the antistatic of the products such as plastics, rubber, synthetic fibers and electromagnetic shielding.American scientist development in 1948 with silver and epoxy
Conducting resinl made of resin is earliest conductive coating generally acknowledged at present.Conductive filler can have decision for Electrical Conductivity of Conductive Coating
Property effect, silver is widely used in all kinds of conductive coatings due to having good conductive property and antioxygenic property.But due to
Metallic silver scarcity of resources, it is expensive, it is not able to satisfy the demand of development of modern industry.
Copper conductivity is good, and price is only the 1/20 of silver, is most hopeful to substitute silver as conductive filler.Copper powder is as conductive
The problem of copper powder maximum is that Copper Powder Surface is oxidizable, and oxide layer is non-conductive, its conductivity is caused to be remarkably decreased, so as to cause leading
Electrocoat failure.Commercial electroconductive copper powder is coated by Electroless Silver Plating in Copper Powder Surface mostly based on silver-plated copper powder at this stage
Silvering prevents oxidization of copper powder.The technique is also easy to produce chemical contamination, and the good silver-plated copper powder of electric conductivity its silver content exists
10% or more, price is still sufficiently expensive.
Graphene is the impermeable film of gas, can effectively completely cut off matrix and air, is ideal anti-corrosion film, and graphene
Chemical property is stablized, and electric conductivity is good.Mostly use graphene common with copper powder in current most of graphene denatured conductive slurries
Electrocondution slurry, conductive coating and electromagnetic screen coating are prepared as conductive filler, is mainly led by graphene and copper powder formation
Electric network come realize coating conduction, not can solve copper powder oxidizable the problem of causing conductivity to decline.If by copper powder table
The complete coated graphite alkene film in face improves copper conductive powder body corrosion resistance, can effectively replace existing conductive silver-coated copper powder, conduction
Silver powder, it is a large amount of to save silver-colored resource and production cost.
Carbon-coated copper composite conductive powder of patent of invention CN104036875.A- graphene-structured and preparation method thereof
It uses copper compound and low temperature liquid carbon source for raw material, obtains the carbon packet of graphene-structured by calcining in inert gas high temperature
The copper composite conductive powder covered, graphene coated copper powder pattern, particle size and distribution are not easy to control, influence conductive coating
Electric conductivity.Patent of invention CN201711125991.6- it is a kind of using CVD method directly in the side of Copper Powder Surface coated graphite alkene
A kind of graphene that is efficiently prepared in situ of method, CN201410066469.50- enhances the method for Cu-base composites, with carbon containing gas
Body is that carbon source in Copper Powder Surface grows graphene, and treatment process or the device is complicated, treatment temperature is high, and copper powder easy-sintering is one
It rises, subsequent composite molding processing difficulties.A kind of spherical copper powder surface in situ growth of patent of invention CN201610697806.X-
The preparation method of three-dimensional grapheme obtains ball using solid-state carbon source PMMA to be mixed with copper powder by ball-milling technology to ball-milling technology
The PMMA thickness for grinding Copper Powder Surface is larger, can not be translated into graphene, and ball milling completely during reduction treatment
Technique cannot make the complete coated high molecular carbon source of Copper Powder Surface, and gained graphene cannot coat copper powder completely.Patent of invention
A kind of side for preparing graphene/copper composite material in Copper Powder Surface supported solid carbon source with infusion process CN201510506051.6-
Method obtains graphene coated copper composite powders by the technique that solution impregnates using PMMA as solid-state carbon source.Its PMMA content is lower,
Only 20mg/ml, gained graphene cannot coat copper powder completely, and copper powder corrosion resistance can be effectively improved.
Summary of the invention
The purpose of the present invention is:.
The technical scheme is that in view of the above-mentioned problems, the present invention is using high-molecular polyivnyl alcohol/polyethylene glycol as solid-state
It is conductive to obtain high-content graphene coated by high concentration Polymer Solution impregnation technology combination chemical vapor deposition process for carbon source
Copper powder, graphene coated area ratio is high, has no that sintering is blocking between copper powder after high-temperature process.Further, pass through secondary original
Position synthesis technology realizes that graphene is coated in the superelevation ratio of Copper Powder Surface, significantly improves conductive copper powder corrosion resistance, and can
Graphene conductive network is formed inside conductive coating, improves its electric conductivity.
A kind of preparation method of graphene coated copper conducting powder based on fabricated in situ is provided, is included the following steps:
Step 1, using polyethylene glycol or polyvinyl alcohol as solid-state polymer carbon source, and solid-state polymer carbon source is dissolved in wine
Essence forms homogeneous mixture solotion；It is preferred that solution temperature is 20~80 DEG C；
Copper powder is sufficiently stirred step 2 in the homogeneous mixture solotion, after filtering by the copper powder in solution and be dry,
It can be coated with the macromolecule layer of polyethylene glycol or polyvinyl alcohol in Copper Powder Surface, the copper powder for being coated with macromolecule layer is obtained, will wrap
The copper powder for being covered with macromolecule layer is placed in heating and calcining in high-temperature heater, and heating and calcining temperature is 800~1050 DEG C, and the time is
0.5~2 hour, the protective gas of heating was the mixed gas of hydrogen and argon gas, the polyethylene glycol or polyvinyl alcohol of Copper Powder Surface
Graphene is converted into protective gas；
The copper powder for being coated with graphene is sufficiently stirred in the homogeneous mixture solotion step 3 again, will be in solution
After copper powder filtering and drying, it is placed in heating and calcining in high-temperature heater, heating and calcining temperature is 800~1050 DEG C, the time 0.5
~2 hours, the protective gas of heating was the mixed gas of hydrogen and argon gas, and the polyethylene glycol or polyvinyl alcohol of Copper Powder Surface are being protected
Graphene is converted into shield gas.
Further, in the homogeneous mixture solotion mass percent of polyethylene glycol or polyvinyl alcohol be 7.5%~
25%.
Further, step 3 is repeatedly carried out, Copper Powder Surface sufficiently wraps up graphene.
Further, solution temperature is 20~80 DEG C in step 1.
Further, heating and calcining temperature is 900~950 DEG C in step 2.
Further, the heating and calcining time is 1.5~2 hours in step 2.
Further, heating and calcining temperature is 900~950 DEG C in step 3.
Further, the heating and calcining time is 1.5~2 hours in step 3.
The invention has the advantages that 1. present invention pass through high concentration Polymer Solution impregnation technology combination chemical vapor deposition work
Skill obtains high-content graphene coated conductive copper powder, and copper powder is un-sintered blocking after high-temperature process, is conducive to the preparation of conductive coating.
2. realizing that graphene is coated in the high proportion of Copper Powder Surface by secondary fabricated in situ technique, significantly improving conduction
Copper powder corrosion resistance, and graphene conductive network can be formed inside conductive coating, improve its electric conductivity.
Detailed description of the invention
Fig. 1 is graphene coated copper powder scanned photograph in embodiment 1；
Fig. 2 is graphene coated copper powder scanned photograph in embodiment 2；
Fig. 3 is graphene coated copper powder Raman spectrogram in embodiment 2；
Fig. 4 a is graphene coated copper powder thermogravimetric test weight gain curve in embodiment 2；
Fig. 4 b is graphene coated copper powder thermogravimetric test rate of gain curve in embodiment 2.
Specific embodiment
The present invention is described in further details below.
Embodiment 1
A kind of preparation method of the graphene coated copper conducting powder based on fabricated in situ, includes the following steps:
Step 1, using polyethylene glycol as solid-state polymer carbon source, and by solid-state polymer carbon source be dissolved in alcohol formed quality
The polyethylene glycol alcoholic solution of score 30g/L；Solution temperature is 20~80 DEG C；
The 200 mesh electrolytic copper powders of 1Kg are sufficiently stirred step 2 in the homogeneous mixture solotion, by the copper powder in solution
After filtering and drying, it can be coated with the macromolecule layer of polyethylene glycol or polyvinyl alcohol in Copper Powder Surface, obtain being coated with macromolecule
The copper powder for being coated with macromolecule layer is placed in heating and calcining in high-temperature heater by the copper powder of layer, and heating and calcining temperature is 850 DEG C,
Time is 1 hour, and the protective gas of heating is the mixed gas of hydrogen and argon gas, and hydrogen: argon content ratio is 1:10, gas stream
Amount is 500sccm, and the polyethylene glycol of Copper Powder Surface is converted into graphene in protective gas；
The copper powder for being coated with graphene is sufficiently stirred in the homogeneous mixture solotion step 3 again, will be in solution
After copper powder filtering and drying, it is placed in heating and calcining in high-temperature heater, heating and calcining temperature is 850 DEG C, and the time is 1 hour, is added
The protective gas of heat is the mixed gas of hydrogen and argon gas, and the polyethylene glycol of Copper Powder Surface is converted into graphite in protective gas
Alkene.
Embodiment 2
A kind of preparation method of the graphene coated copper conducting powder based on fabricated in situ, includes the following steps:
Step 1, using polyethylene glycol as solid-state polymer carbon source, and by solid-state polymer carbon source be dissolved in alcohol formed quality
The polyethylene glycol alcoholic solution of score 80g/L；Solution temperature is 20~80 DEG C；
The 200 mesh electrolytic copper powders of 1Kg are sufficiently stirred step 2 in the homogeneous mixture solotion, by the copper powder in solution
After filtering and drying, it can be coated with the macromolecule layer of polyethylene glycol or polyvinyl alcohol in Copper Powder Surface, obtain being coated with macromolecule
The copper powder for being coated with macromolecule layer is placed in heating and calcining in high-temperature heater by the copper powder of layer, and heating and calcining temperature is 900 DEG C,
Time is 1 hour, and the protective gas of heating is the mixed gas of hydrogen and argon gas: argon content ratio is 1:10, and gas flow is
500sccm, the polyethylene glycol or polyvinyl alcohol of Copper Powder Surface are converted into graphene in protective gas；
The copper powder for being coated with graphene is sufficiently stirred in the homogeneous mixture solotion step 3 again, will be in solution
After copper powder filtering and drying, it is placed in heating and calcining in high-temperature heater, heating and calcining temperature is 900 DEG C, and the time is 1 hour, is added
The protective gas of heat is the mixed gas of hydrogen and argon gas, and the polyethylene glycol or polyvinyl alcohol of Copper Powder Surface are in protective gas transfer
Turn to graphene.
Thermogravimetric test test is carried out to it, measurement atmosphere is air, the results show that its 300 DEG C of condition in air atmosphere
Lower just to start to aoxidize, this shows that graphene coated copper powder has excellent corrosion resisting property.
Claims (8)
1. a kind of preparation method of the graphene coated copper conducting powder based on fabricated in situ, includes the following steps:
Step 1, using polyethylene glycol or polyvinyl alcohol as solid-state polymer carbon source, and solid-state polymer carbon source is dissolved in alcohol shape
At homogeneous mixture solotion；
Copper powder is sufficiently stirred step 2 in the homogeneous mixture solotion, after filtering by the copper powder in solution and is dry, in copper
Powder surface can be coated with the macromolecule layer of polyethylene glycol or polyvinyl alcohol, obtain the copper powder for being coated with macromolecule layer, will be coated with
The copper powder of macromolecule layer is placed in heating and calcining in high-temperature heater, and heating and calcining temperature is 800~1050 DEG C, and the time is 0.5~2
Hour, the protective gas of heating is the mixed gas of hydrogen and argon gas, and the polyethylene glycol or polyvinyl alcohol of Copper Powder Surface are being protected
Graphene is converted into gas；
The copper powder for being coated with graphene is sufficiently stirred in the homogeneous mixture solotion step 3 again, by the copper powder in solution
After filtering and drying, it is placed in heating and calcining in high-temperature heater, heating and calcining temperature is 800~1050 DEG C, and the time is 0.5~2
Hour, the protective gas of heating is the mixed gas of hydrogen and argon gas, and the polyethylene glycol or polyvinyl alcohol of Copper Powder Surface are being protected
Graphene is converted into gas.
2. a kind of preparation method of the graphene coated copper conducting powder based on fabricated in situ as described in claim 1, feature
Be: solution temperature is 20~80 DEG C in step 1.
3. a kind of preparation method of the graphene coated copper conducting powder based on fabricated in situ as described in claim 1, feature
Be: the mass percent of polyethylene glycol or polyvinyl alcohol is 7.5%~25% in the homogeneous mixture solotion.
4. a kind of preparation method of the graphene coated copper conducting powder based on fabricated in situ as described in claim 1, feature
It is: repeatedly carries out step 3, Copper Powder Surface sufficiently wraps up graphene.
5. a kind of preparation method of the graphene coated copper conducting powder based on fabricated in situ as described in claim 1, feature
Be: heating and calcining temperature is 900~950 DEG C in step 2.
6. a kind of preparation method of the graphene coated copper conducting powder based on fabricated in situ as described in claim 1, feature
Be: the heating and calcining time is 1.5~2 hours in step 2.
7. a kind of preparation method of the graphene coated copper conducting powder based on fabricated in situ as described in claim 1, feature
Be: heating and calcining temperature is 900~950 DEG C in step 3.
8. a kind of preparation method of the graphene coated copper conducting powder based on fabricated in situ as described in claim 1, feature
Be: the heating and calcining time is 1.5~2 hours in step 3.
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| CN113355787A (en) * | 2021-06-07 | 2021-09-07 | 宜禾股份有限公司 | Special-purpose tooling fabric with anti-static gathering function |
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