CN108907183A - A kind of metal-powder of double-coating and its preparation method and application - Google Patents
A kind of metal-powder of double-coating and its preparation method and application Download PDFInfo
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- CN108907183A CN108907183A CN201810892563.4A CN201810892563A CN108907183A CN 108907183 A CN108907183 A CN 108907183A CN 201810892563 A CN201810892563 A CN 201810892563A CN 108907183 A CN108907183 A CN 108907183A
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
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- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45555—Atomic layer deposition [ALD] applied in non-semiconductor technology
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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Abstract
The invention belongs to technical field of composite materials, and in particular to a kind of metal-powder of double-coating, the surface of metal-powder are coated with inorganic coating layer, and the surface of inorganic coating layer is coated with conductive carbon layer.The present invention also provides the preparation method of above-mentioned metal-powder, 1）Metal-powder is put into porous container, reaction chamber is vacuumized and replaces nitrogen；2）Metal-powder is dispersed；3）Inorganic coating layer is formed on the surface of metal-powder using ALD；4）Organic clad is formed in inorganic coating layer surface using MLD；5）After carbonizing in a vacuum, organic coating layer carbonizes to form conductive carbon layer, then is heat-treated, and the metal-powder of double-coating is obtained.The present invention also provides a kind of application of the metal-powder of above-mentioned double-coating, the metal-powder of double-coating is used as the conductive component of electrocondution slurry.The present invention can be not only oxidized, but also do not influence the electric conductivity of electrocondution slurry by forming inorganic-organic double-coating on metal-powder surface to avoid metal-powder.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of metal-powder of double-coating and preparation method thereof
And application.
Background technique
Electrocondution slurry is mainly for the manufacture of thick film integrated circuit, sensing element, capacitor, battery, wiring plate, electromagnetic shielding
Equal fields, are the critical materials of encapsulation, electrode and interconnection.Conductive component in electrocondution slurry generally by graphite composite powder, gold, silver,
The powder composition of copper, palladium, platinum, ruthenium.On electric conductivity, the electric conductivity of metal-powder is preferable；And in stability, noble metal
It is more stable but expensive；Although silver-colored price is relatively cheap, silver ion, which is easy migration, causes conductivity to decline；Commonly
The electric conductivity such as metal-powder such as copper, iron, aluminium are preferable, but are oxidized easily, and influence the electric conductivity of electrocondution slurry.
Therefore, it is necessary to a kind of metal-powder of new double-coating be designed, to overcome the above problem.
Summary of the invention
In order to overcome the shortcomings of the prior art described above, the object of the present invention is to provide a kind of metal powders of double-coating
Body and its preparation method and application, neither influences the electric conductivity of electrocondution slurry, and can be oxidized to avoid metal-powder.
To achieve the above object, the technical scheme is that a kind of metal-powder of double-coating, the metal-powder
Surface be coated with inorganic coating layer, the surface of the inorganic coating layer is coated with conductive carbon layer.
Further, the metal powder is at least one of silver, copper, iron and aluminium；The inorganic coating layer is metal
Oxide, metal fluoride, metal sulfide, any one in TiN, W, Ni.Wherein, metal oxide, metal fluoride,
Metal in metal sulfide is any one in Al, Ti, Mg, Zr, Cr, Si, Zn, La, B, Hf, Nb.When inorganic coating layer
When for metal oxide, metal fluoride or metal sulfide, inorganic coating layer with a thickness of 1~4nm；When inorganic coating layer is
When TiN, W or Ni, inorganic coating layer with a thickness of 1~50nm.
The present invention also provides the preparation methods of the metal-powder of above-mentioned double-coating, include the following steps：
1）Metal-powder is put into porous container, porous container is placed in reaction chamber, is vacuumized to reaction chamber and is replaced nitrogen；
2）Metal-powder is dispersed by the method for fluidisation or rotating porous container；
3）Inorganic coating layer is formed on the surface of metal-powder using atomic layer deposition method；
4）Inorganic coating layer surface using molecular-layer deposition method in metal-powder forms organic clad；
5）After carbonizing in a vacuum, organic coating layer carbonizes to form conductive carbon layer, then is heat-treated, and the gold of double-coating is obtained
Belong to powder.
Further, when inorganic coating layer is metal oxide, metal fluoride or metal sulfide, inorganic coating layer
With a thickness of 1~4nm；When inorganic coating layer be TiN, W or Ni when, inorganic coating layer with a thickness of 1~50nm.
Further, the conductive carbon layer with a thickness of 1~50nm.
Further, step 3）In atomic layer deposition method specific step is as follows：
a）The type of the oxide cladding layers deposited as needed selects the presoma of reaction, and deposition process parameters are arranged：Deposition
Temperature is 25~150 DEG C, and deposition pressure is 0.01~500torr；
b）Precursor vapor is introduced into reaction chamber under argon gas carrying, the retention time is 10~120 seconds；
c）Reaction chamber is purged with argon gas, oxygen source steam is introduced into reaction chamber under argon gas carrying, the retention time is 10~120
Second；
d）Reaction chamber is purged with argon gas；
e）Repetitive process b）~d）, until depositing to required inorganic coating thickness degree；
Wherein, step b）Middle presoma is at least one of metal halide, metal organic complex；Step c）Middle oxygen source is
Water, hydrogen peroxide, oxygen, ozone, any one in elemental oxygen.
Further, step 4）In molecular-layer deposition method specific step is as follows：
a）The type for depositing organic clad as needed selects the first presoma of reaction, and deposition process parameters are arranged：Deposition
25~400 DEG C of temperature, deposition pressure is 0.01~500torr；
b）The first precursor vapor is introduced into reaction chamber in the case where nitrogen or argon gas carry, the first precursor vapor is adsorbed on just
On the material powder of pole, the retention time is 10~120 seconds；
c）Reaction chamber is purged with nitrogen or argon gas, the second presoma is introduced into reaction chamber in the case where nitrogen or argon gas carry, the
Two presomas and first forerunner's precursor reactant obtain organic coating layer, and the reaction time is 10~120 seconds；
d）Reaction chamber is purged with nitrogen or argon gas；
e）Repetitive process b）~d）, until depositing to required organic coating thickness degree；
Step b）In the first presoma be paraphenylene diisocyanate, pyromellitic acid anhydride, paraphenylene diisocyanate, trimethyl aluminium
In any one, step c）In the second presoma be 1,6- hexamethylene diamine, ethylenediamine, 1,10- diamino decane, 1,4- dihydroxy
Base -2- butine, ethylene glycol, any one in glycerine.
Further, step 5）The treatment temperature of middle charing is 350 ~ 450 DEG C, and the processing time is 2 ~ 4h；The place of heat treatment
Managing temperature is 800 ~ 900 DEG C, and the processing time is 1 ~ 3h.
The present invention also provides a kind of application of the metal-powder of above-mentioned double-coating, the metal-powder of the double-coating is used
Make the conductive component of electrocondution slurry.
Further, the mass percent of each component is in the electrocondution slurry：The metal-powder 75 ~ 90% of double-coating,
Organic carrier 1 ~ 10%, glass powder 2 ~ 10%, viscosity modifier 1 ~ 5%.
Wherein the organic carrier includes resin, solvent and auxiliary agent, and the mass percent of each component is in organic carrier：
Resin accounts for 10 ~ 30%, and solvent accounts for 65 ~ 80%, and auxiliary agent accounts for 1 ~ 10%；
The resin is oxygen resin, phenolic resin, any one in unsaturated polyester resin；
The solvent is that ethylene glycol, diethylene glycol (DEG), triethylene glycol, glycerol, terpineol, ethyl carbitol, carbitol acetate, butyl are molten
At least one of fine agent；
The auxiliary agent is at least one of curing agent, antioxidant, coupling agent, corrosion inhibitor；
Antioxidant is tert-butyl hydroquinone, thio-2 acid, any one in lipoic acid；
Corrosion inhibitor is phosphine carboxylic acid, coloured glaze base benzothiazole, any one in benzotriazole；
The curing agent is polyamide-based curing agent, in fatty amines curing agent, alicyclic ring amine curing agent, aromatic amine curing agent
At least one；
The coupling agent is using any one in phosphate coupling agent, silane coupling agent, aluminate coupling agent；
The viscosity modifier is methylcellulose, ethyl cellulose, hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl first
At least one of base cellulose and carboxymethyl cellulose；
The component of the glass powder and the mass fraction of each component are：SiO215 ~ 40%, ZnO10 ~ 25%, B2O35 ~ 20%,
Bi2O315 ~ 30%, TiO21 ~ 3%, Al2O35 ~ 10%, Sb2O31 ~ 2%, K2O1 ~ 1.5%, CeO21 ~ 2%, MgO1 ~ 3%, MnO21 ~ 5%,
P2O51~5%。
Compared with prior art, the invention has the advantages that：
（1）The present invention, both can be to avoid metal-powder by oxygen by forming inorganic-organic double-coating on metal-powder surface
Change, and does not influence the electric conductivity of electrocondution slurry；
（2）The present invention first uses ALD（Atomic layer deposition method）It is coated on metal-powder surface and forms inorganic coating layer, then use
MLD（Molecular-layer deposition method）When cladding forms organic clad, ALD cladding can provide uniform reaction for the formation of organic matter
Interface, and control at 1-4 nanometers hereinafter, conduct electronics can with transition, it will not influence conductivity；When ALD clad is
When conductivity ceramics or the metal layer of resistance to oxidation corrosion, cladding thickness can be thicker to guarantee the even compact coated, tool
There is better protective effect；And organic coating layer forms conductive carbon layer on metal-powder surface by charing and heat treatment, it can be with
Promote the electric conductivity of metal-powder；High temperature carbonization process also makes inorganic matter clad become to cause from loose undefined structure simultaneously
Close crystal form clad further promotes barrier water oxygen ability；
（3）In the present invention when by ALD in metal surface coated metal oxide, metal fluoride or metal sulfide,
Cladding can be accurately controlled thickness by frequency of depositing with a thickness of 1~4nm, avoid too thin cladding being caused not have not exclusively
The effect for protecting metal-powder not oxidized, it is too thick that nonconducting inorganic layer is caused to be hindered electron transition, it influences to starch
The electric conductivity of material；And when the metal in metal surface cladding resistance to oxidation（W or Ni）Or conductivity ceramics（TiN）When, thickness can
For 1~50nm because TiN, W or Ni be it is conductive, thicker degree can increase the ability for resisting water oxygen erosion.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel all other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment one
The present embodiment provides a kind of silver powder of double-coating, the surface of silver powder is coated with TiO2Clad, TiO2The table of clad
Bread is covered with conductive carbon layer.
Wherein TiO2Clad with a thickness of 1~4nm, conductive carbon layer with a thickness of 1~50nm.
The present embodiment also provides the preparation method of the silver powder of above-mentioned double-coating, includes the following steps：
1）Silver powder is put into the porous container with micropore size, porous container is placed in reaction chamber, is taken out to reaction chamber
Vacuum, displacement nitrogen at least three times, by between particle or in hole oxygen and water remove, avoid residue and precursor gas
Reaction；Reaction chamber is warming up to 25 DEG C, and reaction chamber maintains the pressure of 100torr；
2）Rotating porous container, so that silver powder is fully dispersed in porous container cavity；
3）By the presoma TiCl of atomic layer deposition4Steam pulse under argon gas carrying enters reaction chamber, is adsorbed on silver powder,
And kept for 60 seconds, then argon gas purges and takes away remaining TiCl4Steam, argon gas purge time are 60s, same H2O steam is in argon
Pulse enters reaction chamber and is kept for 50 seconds under the carrying of gas, and with the TiCl that has been adsorbed on silver powder4Reaction generates TiO2, the time
For 50s, subsequent excessive H2O steam and by-product are purged by argon gas takes reaction chamber out of, and purge time 30s is thus completed
One ALD deposition cycle；It repeats above-mentioned ALD deposition and completes circulation 10 times, i.e., formed on silver powder surface uniform and fine and close
TiO2Clad；
4）By the first presoma pyromellitic acid anhydride of molecular-layer deposition, pulse enters reaction chamber under argon gas carrying, adsorbs
In existing TiO2It on the silver powder of clad, and is kept for 60 seconds, remaining pyromellitic acid anhydride is then purged and taken away with argon gas,
Argon gas purge time is 60s, and the pulse under the carrying of argon gas of same second presoma ethylenediamine enters reaction chamber and kept for 60 seconds,
And reacted with the pyromellitic acid anhydride being adsorbed on silver powder, generate polyimides, time 60s, subsequent excessive second two
Amine and by-product are purged by argon gas takes reaction chamber out of, and purge time 30s, this completes a MLD deposition cycles；It repeats
Above-mentioned MLD deposition completes circulation 100 times, i.e., in the TiO of silver powder2Cover surface forms organic clad；
5）Charing process 2h at 400 DEG C in a vacuum, organic coating layer carbonizes to form conductive carbon layer, then is heat-treated at 900 DEG C
1h obtains TiO2Clad-conductive carbon layer cladding silver powder.
The present embodiment also provides above-mentioned TiO2The application of clad-conductive carbon layer cladding silver powder, the double-coating
Metal-powder is used as the conductive component of electrocondution slurry.
Further, the mass percent of each component is in the electrocondution slurry：The silver powder 75% of double-coating, has airborne
Body 10%, glass powder 10%, viscosity modifier 5%.
Wherein, organic carrier includes resin, solvent and auxiliary agent, and auxiliary agent is antioxidant, and oxygen resin accounts in organic carrier
10%, terpineol accounts for 80%, and thio-2 acid accounts for 10%；
Viscosity modifier is methylcellulose；The component of glass powder and the mass fraction of each component are：SiO240%,
ZnO10%, B2O320%, Bi2O315%, TiO21%, Al2O35%, Sb2O31%, K2O1%, CeO21%, MgO1%, MnO24%, P2O51%。
Embodiment two
The present embodiment provides a kind of copper powder of double-coating, the surface of copper powder is coated with AlF3Clad, AlF3The table of clad
Bread is covered with conductive carbon layer.
Wherein AlF3Clad with a thickness of 1~4nm, conductive carbon layer with a thickness of 1~50nm.
The present embodiment also provides the preparation method of the copper powder of above-mentioned double-coating, includes the following steps：
1）Copper powder is put into the porous container with micropore size, porous container is placed in reaction chamber, is taken out to reaction chamber
Vacuum, displacement nitrogen at least three times, by between particle or in hole oxygen and water remove, avoid residue and precursor gas
Reaction；Reaction chamber is warming up to 350 DEG C, and reaction chamber maintains the pressure of 10torr；
2）Using argon gas streaming mode, so that copper powder is fully dispersed in porous container cavity；
3）By the precursor A l (CH of atomic layer deposition3)3Steam pulse under argon gas carrying enters reaction chamber, is adsorbed on copper powder
On, and kept for 50 seconds, then argon gas purges and takes away remaining Al (CH3)3Steam, argon gas purge time are 50s, and same HF steams
Vapour pulse under the carrying of argon gas enters reaction chamber and is kept for 50 seconds, and with the Al (CH that has been adsorbed on copper powder3)3Reaction generates
AlF3, time 50s, then excessive HF steam and by-product are purged by argon gas takes reaction chamber out of, purge time 50s, this
Sample just completes an ALD deposition cycle；Repeat above-mentioned ALD deposition and complete circulation 20 times, i.e., Copper Powder Surface formed uniformly and
Fine and close AlF3Clad；
4）By the first presoma Adipoyl Chloride of molecular-layer deposition, pulse enters reaction chamber under argon gas carrying, is adsorbed on existing
AlF3It on the copper powder of clad, and is kept for 60 seconds, remaining Adipoyl Chloride, argon gas purge time is then purged and taken away with argon gas
For 60s, same second presoma 1,6- hexamethylene diamine pulse under the carrying of argon gas enters reaction chamber and is kept for 60 seconds, and with inhaled
The Adipoyl Chloride reaction being attached on copper powder, generate polyamide, time 60s, subsequent excessive 1,6- hexamethylene diamine and by-product by
Argon gas purging takes reaction chamber out of, and purge time 30s, this completes a MLD deposition cycles；Repeat above-mentioned MLD deposition
Complete circulation 300 times, i.e., in the AlF of copper powder3Cover surface forms organic clad；
5）Charing process 4h at 350 DEG C in a vacuum, organic coating layer carbonizes to form conductive carbon layer, then is heat-treated at 800 DEG C
3h obtains AlF3Clad-conductive carbon layer cladding copper powder.
The present embodiment also provides above-mentioned AlF3The application of clad-conductive carbon layer cladding copper powder, the double-coating
Metal-powder is used as the conductive component of electrocondution slurry.
Further, the mass percent of each component is in the electrocondution slurry：The metal-powder 90% of double-coating, has
Airborne body 7%, glass powder 2%, viscosity modifier 1%.
Wherein, organic carrier includes resin, solvent and auxiliary agent, and auxiliary agent includes antioxidant and corrosion inhibitor, organic carrier
Middle oxygen resin accounts for 30%, and terpineol accounts for 65%, and tert-butyl hydroquinone accounts for 2%, and coloured glaze base benzothiazole accounts for 3%；
Viscosity modifier is the mixture of ethyl cellulose and hydroxyethyl cellulose；The component of glass powder and the matter of each component
Measuring score is：SiO230%, ZnO20%, B2O310%, Bi2O320%, TiO23%, Al2O36%, Sb2O32%, K2O1.5%, CeO21.5%,
MgO3%, MnO21%, P2O52%。
Embodiment three
The present embodiment provides a kind of aluminium powder of double-coating, the surface of aluminium powder is coated with TiN clad, the surface of TiN clad
It is coated with conductive carbon layer.
Wherein TiN clad with a thickness of 1~50nm, conductive carbon layer with a thickness of 1~50nm.
The present embodiment also provides the preparation method of the aluminium powder of above-mentioned double-coating, includes the following steps：
1）Aluminium powder is put into the porous container with micropore size, porous container is placed in reaction chamber, is taken out to reaction chamber
Vacuum, displacement nitrogen at least three times, by between particle or in hole oxygen and water remove, avoid residue and precursor gas
Reaction；Reaction chamber is warming up to 150 DEG C, and reaction chamber maintains the pressure of 10torr；
2）Using argon gas streaming mode, so that aluminium powder is fully dispersed in porous container cavity；
3）By the presoma TiCl of atomic layer deposition4Steam pulse under argon gas carrying enters reaction chamber, is adsorbed on aluminium powder,
And kept for 50 seconds, then argon gas purges and takes away remaining TiCl4Steam, argon gas purge time are 50s, same NH3Steam is in argon
Pulse enters reaction chamber and is kept for 50 seconds under the carrying of gas, and with the TiCl that has been adsorbed on aluminium powder4Reaction generates TiN, time
For 50s, subsequent excessive NH3Steam and by-product are purged by argon gas takes reaction chamber out of, and purge time 50s is thus completed
One ALD deposition cycle；It repeats above-mentioned ALD deposition and completes circulation 50 times, i.e., form uniform and fine and close TiN on aluminium powder surface
Clad；
4）By the first presoma pyromellitic acid anhydride of molecular-layer deposition, pulse enters reaction chamber under argon gas carrying, adsorbs
It on the aluminium powder of existing TiN clad, and is kept for 60 seconds, remaining pyromellitic acid anhydride is then purged and taken away with argon gas,
Argon gas purge time is 60s, and same second presoma 1, the pulse under the carrying of argon gas of 10- diamino decane enters reaction chamber simultaneously
It is kept for 60 seconds, and is reacted with the pyromellitic acid anhydride being adsorbed on aluminium powder, generation polyimide-amide, time 60s,
Subsequent excessive 1,10- diamino decane and by-product take reaction chamber out of by argon gas purging, purge time 30s, thus complete
At a MLD deposition cycle；It repeats above-mentioned MLD deposition and completes circulation 300 times, i.e., formed in the TiN cover surface of aluminium powder
Organic coating layer；
5）Charing process 4h at 450 DEG C in a vacuum, organic coating layer carbonizes to form conductive carbon layer, then is heat-treated at 850 DEG C
3h obtains TiN clad-conductive carbon layer cladding aluminium powder.
The present embodiment also provides the application of above-mentioned TiN clad-conductive carbon layer cladding aluminium powder, the gold of the double-coating
Belong to the conductive component that powder is used as electrocondution slurry.
Further, the mass percent of each component is in the electrocondution slurry：The metal-powder 80% of double-coating, has
Airborne body 10%, glass powder 7%, viscosity modifier 3%.
Wherein, organic carrier includes resin, solvent and auxiliary agent, and auxiliary agent includes antioxidant, corrosion inhibitor and curing agent, is had
Oxygen resin accounts for 20% in airborne body, and terpineol accounts for 70%, and thio-2 acid accounts for 2%, and benzotriazole accounts for 4%, fatty amines curing agent 4%；
Viscosity modifier is the mixture of ethyl cellulose and hydroxyethyl cellulose；The component of glass powder and the matter of each component
Measuring score is：SiO215%, ZnO25%, B2O35%, Bi2O330%, TiO23%, Al2O310%, Sb2O32%, K2O1%, CeO22%,
MgO3%, MnO23%, P2O51%。
Example IV
The present embodiment provides a kind of silver powder of double-coating, the surface of silver powder is coated with W clad, the surface cladding of W clad
There is conductive carbon layer.
Wherein W clad with a thickness of 1~50nm, conductive carbon layer with a thickness of 1~50nm.
The present embodiment also provides the preparation method of the silver powder of above-mentioned double-coating, includes the following steps：
1）Silver powder is put into the porous container with micropore size, porous container is placed in reaction chamber, is taken out to reaction chamber
Vacuum, displacement nitrogen at least three times, by between particle or in hole oxygen and water remove, avoid residue and precursor gas
Reaction；Reaction chamber is warming up to 400 DEG C, and reaction chamber maintains the pressure of 200orr；
2）By the way of rotating porous container, so that silver powder is fully dispersed in porous container cavity；
3）By the presoma WF of atomic layer deposition6Steam pulse under argon gas carrying enters reaction chamber, is adsorbed on silver powder, and
It is kept for 50 seconds, then argon gas purges and takes away remaining WF6Steam, argon gas purge time are 50s, same B2H6Steam is in argon gas
Carrying under pulse enter reaction chamber and kept for 50 seconds, and with the WF that has been adsorbed on silver powder6Reaction generates W, time 50s,
Subsequent excessive B2H6Steam and by-product are purged by argon gas takes reaction chamber out of, and purge time 50s, this completes one
ALD deposition cycle；It repeats above-mentioned ALD deposition and completes circulation 80 times, i.e., form uniform and fine and close W clad on silver powder surface；
4）By the first presoma paraphenylene diisocyanate of molecular-layer deposition, pulse enters reaction chamber under argon gas carrying, adsorbs
It on the silver powder of existing W clad, and is kept for 60 seconds, is then purged with argon gas and take away remaining paraphenylene diisocyanate, argon
Air-blowing flyback time is 60s, and same second presoma Isosorbide-5-Nitrae-dihydroxy -2- butine pulse under the carrying of argon gas enters reaction chamber simultaneously
It is kept for 60 seconds, and is reacted with the paraphenylene diisocyanate being adsorbed on silver powder, generate polyurethane, time 60s, subsequent mistake
The Isosorbide-5-Nitrae of amount-dihydroxy -2- butine and by-product are purged by argon gas takes reaction chamber out of, purge time 30s, this completes
One MLD deposition cycle；It repeats above-mentioned MLD deposition and completes circulation 200 times, i.e., form organic packet in the W cover surface of silver powder
Coating；
5）Charing process 3h at 400 DEG C in a vacuum, organic coating layer carbonizes to form conductive carbon layer, then is heat-treated at 850 DEG C
2h obtains W clad-conductive carbon layer cladding silver powder.
The present embodiment also provides the application of above-mentioned W clad-conductive carbon layer cladding silver powder, the metal of the double-coating
Powder is used as the conductive component of electrocondution slurry.
Further, the mass percent of each component is in the electrocondution slurry：The metal-powder 85% of double-coating, has
Airborne body 1%, glass powder 10%, viscosity modifier 4%.
Wherein, organic carrier includes resin, solvent and auxiliary agent, and auxiliary agent includes antioxidant, coupling agent and curing agent, is had
Oxygen resin accounts for 15% in airborne body, and terpineol accounts for 75%, and thio-2 acid accounts for 1%, and silane coupling agent accounts for 2%, aromatic amine curing agent
3%, alicyclic ring amine curing agent 4%；
Viscosity modifier is the mixture of ethyl cellulose and hydroxyethyl cellulose；The component of glass powder and the matter of each component
Measuring score is：SiO225%, ZnO19%, B2O310%, Bi2O320%, TiO22%, Al2O38%, Sb2O32%, K2O1%, CeO22%,
MgO1%, MnO25%, P2O55%。
Due to the double-coating prepared in embodiment one, embodiment two, embodiment three, example IV metal-powder most
Outer layer is all conductive carbon layer, is all black, can not find out its oxidation resistant ability, therefore, to embodiment one, embodiment two,
Room temperature is respectively placed in using the metal-powder after ALD coated inorganic nitride layer in embodiment three, example IV（20 DEG C, humidity 50%）
Under, observe its metamorphosis；In addition four comparative examples are done respectively, and wherein comparative example one is uncoated silver powder, and comparative example two is
Uncoated copper powder, comparative example three is uncoated aluminium powder, by the metal-powder in comparative example one, comparative example two, comparative example three
Identical room temperature is placed in after first being cleaned with hydrochloric acid again（20 DEG C, humidity 50%）Under, observe its metamorphosis；Four embodiments and
The variation of the metal-powder of three comparative examples is as shown in table 1 below.
From table 1 it follows that silver powder surface is in brilliant white after over cleaning, Copper Powder Surface is in bright rufous, aluminium powder
Surface is silvery white in color, and over time, surface starts rapid oxidation, and color is gradually dimmed, its shape after 8 hours
State is not changing substantially, and silver powder surface is in black, and Copper Powder Surface is in burgundy, and aluminium powder surface is in canescence；And embodiment
One, embodiment two, embodiment three, in example IV using the metal-powder after ALD coated inorganic nitride layer, by 24 hours skies
Gas exposure, significant change does not occur for pattern, and after 7 days, still there is no significant changes for surface color, after 30 days,
Embodiment one, embodiment two, embodiment three, example IV sample be respectively in black, burgundy, yellowish-brown, black, to the 60th
Its end, the color of sample are very close with the 30th day；It can be seen that the metal-powder of coated inorganic object its there is oxidative phenomena more
Add slowly, clad can be played the role of good oxygen obstruction and water vapor rejection by inorganic matter, and effective protection metal-powder is not
It is oxidized.
The color of 1 metal-powder of table with exposure duration variation
It chooses in embodiment two and prepares AlF3Clad-conductive carbon layer cladding copper powder and the uncoated copper in comparative example two
The resistivity of the sample of powder at normal temperature surveys its resistivity, at specific heat after being then heat-treated 1 hour at 200 DEG C respectively
The change in resistance of front and back is managed, as shown in table 2, it can be seen that the copper powder sample of comparative example two is after Overheating Treatment, resistivity
Thousand times are increased relative to the resistivity value under room temperature；And the copper powder of the double-coating in embodiment two is after Overheating Treatment,
Resistivity only increases by 3 times relative to the resistivity value under room temperature；It can be seen that using the copper of double-coating provided by the invention
Conductive component of the powder as electrocondution slurry, electric conductivity are more preferable.
The resistivity value of 2 metal-powder of table（Ω·m）
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of metal-powder of double-coating, it is characterised in that：The surface of the metal-powder is coated with inorganic coating layer, institute
The surface for stating inorganic coating layer is coated with conductive carbon layer.
2. a kind of metal-powder of double-coating as described in claim 1, it is characterised in that：The metal powder be silver, copper,
At least one of iron and aluminium；The inorganic coating layer is metal oxide, metal fluoride, metal sulfide, TiN, W, Ni
In any one.
3. a kind of preparation method of the metal-powder of the double-coating as described in claim 1-2 any one, which is characterized in that
Include the following steps：
1）Metal-powder is put into porous container, porous container is placed in reaction chamber, is vacuumized to reaction chamber and is replaced nitrogen；
2）Metal-powder is dispersed by the method for fluidisation or rotating porous container；
3）Inorganic coating layer is formed on the surface of metal-powder using atomic layer deposition method；
4）Inorganic coating layer surface using molecular-layer deposition method in metal-powder forms organic clad；
5）After carbonizing in a vacuum, organic coating layer carbonizes to form conductive carbon layer, then is heat-treated, and the gold of double-coating is obtained
Belong to powder.
4. the preparation method of the metal-powder of double-coating as claimed in claim 3, it is characterised in that：When inorganic coating layer is
When metal oxide, metal fluoride or metal sulfide, inorganic coating layer with a thickness of 1~4nm；When inorganic coating layer is
When TiN, W or Ni, inorganic coating layer with a thickness of 1~50nm.
5. the preparation method of the metal-powder of double-coating as claimed in claim 3, it is characterised in that：The conductive carbon layer
With a thickness of 1~50nm.
6. the preparation method of the metal-powder of double-coating as claimed in claim 3, it is characterised in that：Step 3）In atom
Specific step is as follows for layer sedimentation：
a）The type of the oxide cladding layers deposited as needed selects the presoma of reaction, and deposition process parameters are arranged：Deposition
Temperature is 25~400 DEG C, and deposition pressure is 0.01~500torr；
b）Precursor vapor is introduced into reaction chamber under argon gas carrying, the retention time is 10~120 seconds；
c）Reaction chamber is purged with argon gas, oxygen source steam is introduced into reaction chamber under argon gas carrying, the retention time is 10~120
Second；
d）Reaction chamber is purged with argon gas；
e）Repetitive process b）~d）, until depositing to required inorganic coating thickness degree；
Wherein, step b）Middle presoma is at least one of metal halide, metal organic complex；Step c）Middle oxygen source is
Water, hydrogen peroxide, oxygen, ozone, any one in elemental oxygen.
7. the preparation method of the metal-powder of double-coating as claimed in claim 3, it is characterised in that：Step 4）In molecule
Specific step is as follows for layer sedimentation：
a）The type for depositing organic clad as needed selects the first presoma of reaction, and deposition process parameters are arranged：Deposition
25~400 DEG C of temperature, deposition pressure is 0.01~500torr；
b）The first precursor vapor is introduced into reaction chamber in the case where nitrogen or argon gas carry, the first precursor vapor is adsorbed on just
On the material powder of pole, the retention time is 10~120 seconds；
c）Reaction chamber is purged with nitrogen or argon gas, the second presoma is introduced into reaction chamber in the case where nitrogen or argon gas carry, the
Two presomas and first forerunner's precursor reactant obtain organic coating layer, and the reaction time is 10~120 seconds；
d）Reaction chamber is purged with nitrogen or argon gas；
e）Repetitive process b）~d）, until depositing to required organic coating thickness degree；
Step b）In the first presoma be paraphenylene diisocyanate, pyromellitic acid anhydride, paraphenylene diisocyanate, trimethyl aluminium
In any one, step c）In the second presoma be 1,6- hexamethylene diamine, ethylenediamine, 1,10- diamino decane, 1,4- dihydroxy
Base -2- butine, ethylene glycol, any one in glycerine.
8. the preparation method of the metal-powder of double-coating as claimed in claim 3, it is characterised in that：Step 5）Middle charing
Treatment temperature is 350 ~ 450 DEG C, and the processing time is 2 ~ 4h；The treatment temperature of heat treatment be 800 ~ 900 DEG C, processing the time be 1 ~
3h。
9. a kind of application of the metal-powder of the double-coating as described in claim 1-2 any one, it is characterised in that：It is described
The metal-powder of double-coating is used as the conductive component of electrocondution slurry.
10. the application of the metal-powder of double-coating as claimed in claim 9, it is characterised in that：It is each in the electrocondution slurry
The mass percent of component is：The metal-powder 75 ~ 90% of double-coating, organic carrier 1 ~ 10%, glass powder 2 ~ 10%, viscosity
Regulator 1 ~ 5%.
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