CN109903887A - Anti-oxidant copper-based electrocondution slurry of one kind and preparation method thereof - Google Patents
Anti-oxidant copper-based electrocondution slurry of one kind and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of anti-oxidant copper-based electrocondution slurries and preparation method thereof, comprising the following steps: (1) ethanol solution of copper powder aniline is carried out the copper powder that processing prepares Polyaniline-modified；(2) hydrochloric acid solution of ammonium persulfate is added in solution made from step (1) under conditions of ice bath, the sediment in reaction system is retained by filtering after being stirred to react, is resuspended after being washed with ethanol solution, mixture A is made；(3) surface is made in step (2) and modifies one layer of silver layer；(4) organic bond is prepared；(5) by compound copper powder made from step (3), organic bond it is processed after anti-oxidant copper-based electrocondution slurry is made.Electrocondution slurry adhesive ability produced by the present invention is strong, resistivity is low, while having good antioxygenic property.Therefore, the electrode in solar battery is applied as electrocondution slurry, there is important practical value.
Description
Technical field
The present invention relates to a kind of electrocondution slurries, and in particular to anti-oxidant copper-based electrocondution slurry of one kind and preparation method thereof.
Background technique
The conductive filler being now widely used in electrocondution slurry can be divided into silver-based, palladium-silver, auri, platinum base, copper-based, nickel
Base and other metal packings, the electric conductivity and inoxidizability of conductive filler directly affect the superiority and inferiority of electrocondution slurry performance.With it
He compares conductive filler, and copper is represented as base metal, cheap, and electric conductivity is only second to silver, and electricity will not occur for copper
Sub- transport phenomena, therefore, it is very big that copper-based slurry is that the optimal alternative materials of silver-based paste but micron-stage sheet-like copper powder have
Specific surface area, surface can greatly and therefore high surface activity is easily oxidized in air, generates the oxide of copper, and electrocondution slurry
During the sintering process, the copper powder that the oxidation of copper powder can be accelerated to be oxidized surface is as conductive filler it is possible that many is asked
Topic, it is small, cause electric slurry resistivity rapidly to increase, breaking phenomena occur, influence using, it is too big then to occur local electrical resistance greatly,
Amount of heat is generated, accident is caused.
Summary of the invention
Above of the existing technology in order to solve the problems, such as, the purpose of the present invention is to provide a kind of anti-oxidant copper-based conductions
Slurry and preparation method thereof.
To achieve the goals above, the present invention the following technical schemes are provided:
A kind of preparation method of anti-oxidant copper-based electrocondution slurry, comprising the following steps:
(1) 50-80 parts of copper powder are added in the aqueous solution of the 30-60 parts of dispersing agents containing 10-20wt%, in the condition of stirring
The lower hydrochloric acid solution that 8-15 parts of 0.5-1M are added, is then added the ethanol solution of 5-10 parts of 1-5mg/mL aniline, stirs at room temperature
Mix mixing 20-40min；Add 2-4 parts of chloroform stirring 5-10min；
(2) it is obtained that the hydrochloric acid solution of the 4-8 parts of ammonium persulfates containing 1-5wt% is added to step (1) under conditions of ice bath
In solution, 2-5h is reacted while stirring；The sediment in reaction system is retained by filtering, and molten with ethyl alcohol
Liquid washs 3-5 times, finally washed once again with aqueous solution, and sediment is resuspended in 30-60 parts of steps (1) containing 10-20wt%
In the aqueous solution of dispersing agent, mixture A is made；
(3) by AgNO3It is added in the mixture A in step (2), so that AgNO3Final concentration of 1-5M, then stirring
2-5 parts of reducing agents are added under conditions of mixing, reaction 1-2h is stirred at room temperature, supernatant are removed by centrifugation, and washed with ethanol solution
It 3-5 times, finally washed once again with aqueous solution, precipitating particle be collected after centrifugation, is placed in baking oven and dries, compound antioxygen is made
Change copper powder, it is spare after being ground；
(4) E-5115-30 parts of epoxy resin, 12-20 parts of polyvinyl acetal adhesive, 8-16 parts of rosin resin, 3- are shunk
4-8 parts of glyceryl etheroxypropyltrimethoxysilane, 3-6 parts of 2,5- ditert-butylhydro quinone be added to 30-50 parts of tetrahydro furans
Mutter in solution, 80-100 DEG C at a temperature of be stirred 30-50min, be then eventually adding 1-3 parts of levelling agent and wetting agent 2-
5 parts, 60-80 DEG C is cooled the temperature to, continues to be stirred 1-2h to get organic bond；
(5) compound copper powder made from step (3), organic bond are added in de-airing mixer and stir 1-2h, formed equal
Even mixture, then through three-high mill grinding distribution, it is ground into homogeneous slurry, scraper plate fineness≤5 μm are controlled, then through 500 mesh silks
Net filtration obtains anti-oxidant copper-based electrocondution slurry.
Further, in the preparation method of the anti-oxidant copper-based electrocondution slurry of one kind of the present invention, in the step (1)
Dispersing agent be polyvinylpyrrolidone, lauryl sodium sulfate or polyethylene glycol one or more combinations.
Further, in the preparation method of the anti-oxidant copper-based electrocondution slurry of one kind of the present invention, the levelling agent is
Esters of acrylic acid levelling agent or organosilicon levelling agent.
Further, in the preparation method of the anti-oxidant copper-based electrocondution slurry of one kind of the present invention, the wetting agent is
Dinethylformamide or polysorbas20.
Preferably, each in the step (4) in the preparation method of the anti-oxidant copper-based electrocondution slurry of one kind of the present invention
The parts by weight of raw material are as follows: E-5122 parts of epoxy resin, 16 parts of polyvinyl acetal adhesive, 12 parts of rosin resin, 3- glycidol ether
6 parts of oxygroup propyl trimethoxy silicane, 4.5 parts of 2,5- ditert-butylhydro quinone, 40 parts of tetrahydrofuran solution, 2 parts of levelling agent,
3.5 parts of wetting agent.
Anti-oxidant copper-based electrocondution slurry made from preparation method of the present invention.
The utility model has the advantages that the present invention exists first the present invention provides a kind of anti-oxidant copper-based electrocondution slurry and preparation method thereof
Copper Powder Surface modifies polyaniline, then wraps up silver layer again, greatly improves the antioxygenic property of electrocondution slurry.It is produced by the present invention
Electrocondution slurry adhesive ability is strong, resistivity is low, has good electric conductivity, while the conduction placed and be placed at room temperature for through 230 DEG C
The change in resistance of slurry is little, to illustrate that copper-based electrocondution slurry produced by the present invention has good antioxygenic property.Cause
This, applies the electrode in solar battery as electrocondution slurry, has important practical value.
Specific embodiment
The invention will now be further described with reference to specific embodiments, but examples are merely exemplary, not to this hair
Bright range constitutes any restrictions.It will be understood by those skilled in the art that without departing from the spirit and scope of the invention
Can with the details and forms of the technical scheme of the invention are modified or replaced, but these modification and replacement each fall within it is of the invention
In protection scope.
Embodiment 1
A kind of preparation method of anti-oxidant copper-based electrocondution slurry, comprising the following steps:
(1) 65 parts of copper powder are added in the aqueous solution of 45 parts of dispersing agents containing 15wt%, 12 is added under stirring conditions
The hydrochloric acid solution of part 0.5M, is then added the ethanol solution of 8 parts of 3mg/mL aniline, and mixing 30min is stirred at room temperature；It adds
3 parts of chloroforms stir 8min；
(2) solution made from step (1) is added in the hydrochloric acid solution of 6 parts of ammonium persulfates containing 3wt% under conditions of ice bath
In, 3.5h is reacted while stirring；The sediment in reaction system is retained by filtering, and is washed with ethanol solution
It washs 4 times, finally washed once again with aqueous solution, sediment is resuspended in the water-soluble of the dispersing agent containing 15wt% in 45 parts of steps (1)
In liquid, mixture A is made；
(3) by AgNO3It is added in the mixture A in step (2), so that AgNO3Final concentration of 3M, then stirring
Under conditions of 3.5 parts of reducing agents are added, reaction 1.5h is stirred at room temperature, supernatant is removed by centrifugation, and washs 3-5 with ethanol solution
It is secondary, it finally washed once again with aqueous solution, precipitating particle be collected after centrifugation, is placed in baking oven and dries, compound anti-oxidation is made
Copper powder, it is spare after being ground；
(4) by E-5122 parts of epoxy resin, 16 parts of polyvinyl acetal adhesive, 12 parts of rosin resin, 3- glycidyl ether oxygen
6 parts of base propyl trimethoxy silicane, 4.5 parts of 2,5- ditert-butylhydro quinone be added in 40 parts of tetrahydrofuran solutions, 90
It is stirred 40min at a temperature of DEG C, is then eventually adding 2 parts and 3.5 parts of wetting agent of levelling agent, cools the temperature to 70 DEG C, after
It is continuous to be stirred 1.5h to get organic bond；
(5) compound copper powder made from step (3), organic bond are added in de-airing mixer and stir 1.5h, formed equal
Even mixture, then through three-high mill grinding distribution, it is ground into homogeneous slurry, scraper plate fineness≤5 μm are controlled, then through 500 mesh silks
Net filtration obtains anti-oxidant copper-based electrocondution slurry.
Dispersing agent in the step (1) is polyvinylpyrrolidone.
The levelling agent is esters of acrylic acid levelling agent.
The wetting agent is dinethylformamide.
Embodiment 2
A kind of preparation method of anti-oxidant copper-based electrocondution slurry, comprising the following steps:
(1) 50 parts of copper powder are added in the aqueous solution of 30 parts of dispersing agents containing 10wt%, 8 parts is added under stirring conditions
The ethanol solution of 5 parts of 1mg/mL aniline is then added in the hydrochloric acid solution of 0.5M, and mixing 20min is stirred at room temperature；Add 2
Part chloroform stirs 5min；
(2) solution made from step (1) is added in the hydrochloric acid solution of 4 parts of ammonium persulfates containing 1wt% under conditions of ice bath
In, 2h is reacted while stirring；The sediment in reaction system is retained by filtering, and is washed with ethanol solution
It 3-5 times, finally washed once again with aqueous solution, sediment be resuspended in the water-soluble of the dispersing agent containing 10wt% in 30 parts of steps (1)
In liquid, mixture A is made；
(3) by AgNO3It is added in the mixture A in step (2), so that AgNO3Final concentration of 1M, then stirring
Under conditions of 2 parts of reducing agents are added, reaction 1h is stirred at room temperature, supernatant is removed by centrifugation, and is washed 3-5 times with ethanol solution,
It finally washed once again with aqueous solution, precipitating particle be collected after centrifugation, is placed in baking oven and dries, compound anti-oxidation copper is made
Powder, it is spare after being ground；
(4) by E-5115 parts of epoxy resin, 12 parts of polyvinyl acetal adhesive, 8 parts of rosin resin, 3- glycidol ether oxygroup
4 parts of propyl trimethoxy silicane, 3 parts of 2,5- ditert-butylhydro quinone be added in 30 parts of tetrahydrofuran solutions, at 80 DEG C
At a temperature of be stirred 30min, be then eventually adding 1 part of levelling agent and 2 parts of wetting agent, cool the temperature to 60 DEG C, continue to stir
1h is mixed to get organic bond；
(5) compound copper powder made from step (3), organic bond are added in de-airing mixer and stir 1h, formed uniform
Mixture, then through three-high mill grinding distribution, it is ground into homogeneous slurry, scraper plate fineness≤5 μm are controlled, then through 500 mesh silk screens
Anti-oxidant copper-based electrocondution slurry is obtained by filtration.
Dispersing agent in the step (1) is lauryl sodium sulfate.
The levelling agent is organosilicon levelling agent.
The wetting agent is polysorbas20.
Embodiment 3
A kind of preparation method of anti-oxidant copper-based electrocondution slurry, comprising the following steps:
(1) 60 parts of copper powder are added in the aqueous solution of 40 parts of dispersing agents containing 12wt%, 10 is added under stirring conditions
The hydrochloric acid solution of part 0.6M, is then added the ethanol solution of 6 parts of 2mg/mL aniline, and mixing 25min is stirred at room temperature；It adds
2.5 parts of chloroforms stir 6min；
(2) solution made from step (1) is added in the hydrochloric acid solution of 5 parts of ammonium persulfates containing 2wt% under conditions of ice bath
In, 3h is reacted while stirring；The sediment in reaction system is retained by filtering, and is washed with ethanol solution
It 3-5 times, finally washed once again with aqueous solution, sediment be resuspended in the water-soluble of the dispersing agent containing 12wt% in 40 parts of steps (1)
In liquid, mixture A is made；
(3) by AgNO3It is added in the mixture A in step (2), so that AgNO3Final concentration of 2M, then stirring
Under conditions of 3 parts of reducing agents are added, reaction 1.2h is stirred at room temperature, supernatant is removed by centrifugation, and washs 3-5 with ethanol solution
It is secondary, it finally washed once again with aqueous solution, precipitating particle be collected after centrifugation, is placed in baking oven and dries, compound anti-oxidation is made
Copper powder, it is spare after being ground；
(4) by E-5120 parts of epoxy resin, 15 parts of polyvinyl acetal adhesive, 10 parts of rosin resin, 3- glycidyl ether oxygen
5 parts of base propyl trimethoxy silicane, 4 parts of 2,5- ditert-butylhydro quinone be added in 35 parts of tetrahydrofuran solutions, at 85 DEG C
At a temperature of be stirred 35min, be then eventually adding 1.5 parts of levelling agent and 3 parts of wetting agent, cool the temperature to 65 DEG C, continue
1.2h is stirred to get organic bond；
(5) compound copper powder made from step (3), organic bond are added in de-airing mixer and stir 1.2h, formed equal
Even mixture, then through three-high mill grinding distribution, it is ground into homogeneous slurry, scraper plate fineness≤5 μm are controlled, then through 500 mesh silks
Net filtration obtains anti-oxidant copper-based electrocondution slurry.
Dispersing agent in the step (1) is Macrogol 600.
The levelling agent is esters of acrylic acid levelling agent.
The wetting agent is dinethylformamide.
Embodiment 4
A kind of preparation method of anti-oxidant copper-based electrocondution slurry, comprising the following steps:
(1) 80 parts of copper powder are added in the aqueous solution of 60 parts of dispersing agents containing 20wt%, 15 is added under stirring conditions
The hydrochloric acid solution of part 1M, is then added the ethanol solution of 10 parts of 5mg/mL aniline, and mixing 40min is stirred at room temperature；Add 4
Part chloroform stirs 10min；
(2) solution made from step (1) is added in the hydrochloric acid solution of 8 parts of ammonium persulfates containing 5wt% under conditions of ice bath
In, 5h is reacted while stirring；The sediment in reaction system is retained by filtering, and is washed with ethanol solution
It 3-5 times, finally washed once again with aqueous solution, sediment be resuspended in the water-soluble of the dispersing agent containing 20wt% in 60 parts of steps (1)
In liquid, mixture A is made；
(3) by AgNO3It is added in the mixture A in step (2), so that AgNO3Final concentration of 5M, then stirring
Under conditions of 5 parts of reducing agents are added, reaction 2h is stirred at room temperature, supernatant is removed by centrifugation, and is washed 3-5 times with ethanol solution,
It finally washed once again with aqueous solution, precipitating particle be collected after centrifugation, is placed in baking oven and dries, compound anti-oxidation copper is made
Powder, it is spare after being ground；
(4) by E-5130 parts of epoxy resin, 20 parts of polyvinyl acetal adhesive, 16 parts of rosin resin, 3- glycidyl ether oxygen
8 parts of base propyl trimethoxy silicane, 6 parts of 2,5- ditert-butylhydro quinone be added in 50 parts of tetrahydrofuran solutions, at 100 DEG C
At a temperature of be stirred 50min, be then eventually adding 3 parts of levelling agent and 5 parts of wetting agent, cool the temperature to 80 DEG C, continue to stir
Mixing 2h is mixed to get organic bond；
(5) compound copper powder made from step (3), organic bond are added in de-airing mixer and stir 2h, formed uniform
Mixture, then through three-high mill grinding distribution, it is ground into homogeneous slurry, scraper plate fineness≤5 μm are controlled, then through 500 mesh silk screens
Anti-oxidant copper-based electrocondution slurry is obtained by filtration.
Dispersing agent in the step (1) is the polyvinylpyrrolidone and lauryl sodium sulfate that mass ratio is 1:1.
The levelling agent is organosilicon levelling agent.
The wetting agent is polysorbas20.
Comparative example 1
Comparative example 1 the difference from embodiment 1 is that, the copper powder in comparative example 1 does not pass through the processing of step (1).
Comparative example 2
Comparative example 2 the difference from embodiment 1 is that, the copper powder in comparative example 2 does not pass through the processing of step (3).
The electrocondution slurry of embodiment 1-4 and comparative example 1-2 is subjected to following performance test, test result is as shown in table 1.
Thermal oxidation test: obtained electrocondution slurry is placed at a temperature of 230 DEG C and places 48h, surveys the change of its resistivity
Change；
Antioxygenic property test: electrocondution slurry obtained is placed in and is placed 30 days at room temperature, the variation of its resistivity is surveyed.
It being obtained from table 1, electrocondution slurry adhesive ability produced by the present invention is strong, resistivity is low, there is good electric conductivity,
The change in resistance for the electrocondution slurry placed and be placed at room temperature for through 230 DEG C simultaneously is little, to illustrate produced by the present invention copper-based
Electrocondution slurry has good antioxygenic property.
Table 1
Claims (6)
1. a kind of preparation method of anti-oxidant copper-based electrocondution slurry, which comprises the following steps:
(1) 50-80 parts of copper powder are added in the aqueous solution of the 30-60 parts of dispersing agents containing 10-20wt%, under stirring conditions plus
Enter the hydrochloric acid solution of 8-15 parts of 0.5-1M, the ethanol solution of 5-10 parts of 1-5mg/mL aniline is then added, is stirred at room temperature mixed
Close 20-40min；Add 2-4 parts of chloroform stirring 5-10min；
(2) solution made from step (1) is added in the hydrochloric acid solution of the 4-8 parts of ammonium persulfates containing 1-5wt% under conditions of ice bath
In, 2-5h is reacted while stirring；The sediment in reaction system is retained by filtering, and is washed with ethanol solution
It washs 3-5 times, finally washed once again with aqueous solution, sediment is resuspended in 30-60 parts of steps (1) and is dispersed containing 10-20wt%
In the aqueous solution of agent, mixture A is made；
(3) by AgNO3It is added in the mixture A in step (2), so that AgNO3Final concentration of 1-5M, then in stirring
Under the conditions of 2-5 part reducing agents are added, reaction 1-2h is stirred at room temperature, by centrifugation removal supernatant, and washs 3-5 with ethanol solution
It is secondary, it finally washed once again with aqueous solution, precipitating particle be collected after centrifugation, is placed in baking oven and dries, compound anti-oxidation is made
Copper powder, it is spare after being ground；
(4) by E-5115-30 parts of epoxy resin, 12-20 parts of polyvinyl acetal adhesive, 8-16 parts of rosin resin, 3- glycidol
4-8 parts of ether oxygen base propyl trimethoxy silicane, 3-6 parts of 2,5- ditert-butylhydro quinone to be added to 30-50 parts of tetrahydrofurans molten
In liquid, 80-100 DEG C at a temperature of be stirred 30-50min, be then eventually adding 1-3 parts of levelling agent and wetting agent 2-5 parts,
60-80 DEG C is cooled the temperature to, continues to be stirred 1-2h to get organic bond；
(5) compound copper powder made from step (3), organic bond are added in de-airing mixer and stir 1-2h, formed uniformly mixed
Object is closed, then through three-high mill grinding distribution, is ground into homogeneous slurry, controls scraper plate fineness≤5 μm, then through 500 mesh silk screen mistakes
Filter obtains anti-oxidant copper-based electrocondution slurry.
2. the preparation method of the anti-oxidant copper-based electrocondution slurry of one kind according to claim 1, which is characterized in that the step
(1) dispersing agent in is one or more combinations of polyvinylpyrrolidone, lauryl sodium sulfate or polyethylene glycol.
3. the preparation method of the anti-oxidant copper-based electrocondution slurry of one kind according to claim 1, which is characterized in that the levelling
Agent is esters of acrylic acid levelling agent or organosilicon levelling agent.
4. the preparation method of the anti-oxidant copper-based electrocondution slurry of one kind according to claim 1, which is characterized in that the wetting
Agent is dinethylformamide or polysorbas20.
5. the preparation method of the anti-oxidant copper-based electrocondution slurry of one kind according to claim 1, which is characterized in that the step
(4) parts by weight of each raw material in are as follows: E-5122 parts of epoxy resin, 16 parts of polyvinyl acetal adhesive, 12 parts of rosin resin, 3- shrink
6 parts of glyceryl etheroxypropyltrimethoxysilane, 4.5 parts of 2,5- ditert-butylhydro quinone, 40 parts of tetrahydrofuran solution, levelling
2 parts of agent, 3.5 parts of wetting agent.
6. anti-oxidant copper-based electrocondution slurry made from the described in any item preparation methods of claim 1-5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111799012A (en) * | 2020-06-23 | 2020-10-20 | 厦门大学 | Antioxidant copper material and preparation method thereof |
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Application publication date: 20190618 |