CN107331437A - Graphene low-temperature solidified silver paste compound and preparation method thereof - Google Patents
Graphene low-temperature solidified silver paste compound and preparation method thereof Download PDFInfo
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- CN107331437A CN107331437A CN201710581726.2A CN201710581726A CN107331437A CN 107331437 A CN107331437 A CN 107331437A CN 201710581726 A CN201710581726 A CN 201710581726A CN 107331437 A CN107331437 A CN 107331437A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 70
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 40
- 239000004332 silver Substances 0.000 title claims abstract description 40
- 150000001875 compounds Chemical class 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000003822 epoxy resin Substances 0.000 claims abstract description 16
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000006259 organic additive Substances 0.000 claims abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 19
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 4
- 239000012286 potassium permanganate Substances 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- 239000013008 thixotropic agent Substances 0.000 claims description 4
- 239000012745 toughening agent Substances 0.000 claims description 4
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 3
- 235000010344 sodium nitrate Nutrition 0.000 claims description 3
- 239000004317 sodium nitrate Substances 0.000 claims description 3
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical compound CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 claims description 2
- 239000001856 Ethyl cellulose Substances 0.000 claims description 2
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical group CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000011353 cycloaliphatic epoxy resin Substances 0.000 claims description 2
- 229920001249 ethyl cellulose Polymers 0.000 claims description 2
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 2
- -1 phenol aldehyde Chemical class 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002562 thickening agent Substances 0.000 claims description 2
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- 239000003963 antioxidant agent Substances 0.000 claims 1
- 230000003078 antioxidant effect Effects 0.000 claims 1
- 239000002270 dispersing agent Substances 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 7
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 description 23
- 238000007711 solidification Methods 0.000 description 10
- 230000008023 solidification Effects 0.000 description 10
- 239000007788 liquid Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000002002 slurry Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 3
- 238000000703 high-speed centrifugation Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229930185605 Bisphenol Natural products 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 235000008504 concentrate Nutrition 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000010946 fine silver Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000006188 syrup Substances 0.000 description 1
- 235000020357 syrup Nutrition 0.000 description 1
Classifications
-
- 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
-
- 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
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Conductive Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a kind of graphene low-temperature solidified silver paste compound and preparation method thereof, the silver paste composition includes the following component of percentage：Epoxy resin：20~50%；Flake silver powder：40~60%；Modified graphene material：0.5~10%；Organic additive：0.5~10%.The preparation method is：Epoxy resin, flake silver powder, modified graphene material and organic additive are mixed, stirred.Low-temperature setting graphene silver paste prepared by this method, technique is simple to operation, with low cost, high financial profit, is adapted to large-scale industrial production.
Description
Technical field
The present invention relates to a kind of graphene low-temperature solidified silver paste compound and preparation method thereof, belong to coating technology neck
Domain.
Background technology
Silver paste is the Precious Metal of argentiferous, is one used earliest for dip-coating and silk screen process in electronics industry
Plant conductive material.It is broadly divided into following four kinds：Fine silver slurry, the silver-colored palladium slurry by base of silver, silver-colored platinum slurry and polymer syrup
Material.
In silicon solar cell manufacturing process, the improvement that conversion efficiency all concentrates on front side silver paste is improved.It is now major
The improved method of manufacturer is the depth-width ratio by improving sintering disposed slurry, uses reduction parallel resistance (Rs) and increase light-receiving area
To improve the conversion efficiency of battery.So it is dilute using the lower graphite of resistance ratio silver, lower parallel resistance (Rs) can be obtained.
And graphene has superior translucency, ratio is penetrated using what graphene substituted that most of lighttight silver powder can increase light,
So as to which more light can be injected in crystalline silicon, more photogenerated currents are produced, further the conversion of lifting solar cell
Efficiency.The problem of due to without considering shading, a great problem-depth-width ratio that present front side silver paste is faced also just completely can be with
Overcome.
Graphene is a kind of by two-dimensional material of the carbon atom by hexagonal array, table of the graphene oxide in graphene
Layer has carboxyl, and epoxy radicals, hydroxyl etc. contains base group modification.Due to graphene oxide, preparation technology is simpler, the cost of raw material
It is cheap, while graphene oxide is less susceptible to reunite compared with graphene in practical operation, therefore it can be widely applied to extensive
In industrial production.But deployment conditions of the graphene oxide in resin are bad, easily caused during mixing and mix uneven and promote
Make material of main part segment performance uneven, so as to cause material property unstable, therefore improve its deployment conditions work in the material
The problem of having to solve for the nowadays stage.
The content of the invention
For defect of the prior art, it is an object of the invention to provide a kind of graphene low-temperature solidified silver paste compound
And preparation method thereof.
The present invention is achieved by the following technical solutions：
In a first aspect, the invention provides a kind of graphene low-temperature solidified silver paste compound, it includes percentage by weight
The following component of number meter：
Epoxy resin content is crossed can influence slurry adhesion strength at least, and crossing at most influences electric conductivity；Modified graphene material
Content is very few not clear aobvious to silver paste electric conductivity enhancing performance, and the wasting of resources can at most be caused by crossing, and enhancing effect is reduced；It is organic
Additive level is very few, and reaction is incomplete, and the wasting of resources can at most be caused by crossing, and influence size performance；Flake silver powder content mistake
Electric conductivity can be influenceed less, excessively increase cost of sizing agent.
Preferably, the modified graphene material is redox graphene.
Preferably, the preparation method of the redox graphene comprises the following steps：
Graphene oxide is prepared using Hummers methods；
The graphene oxide is configured to suspension, sodium hydroxide is added, carried out under 50~80 DEG C of ultrasound condition
After reaction, centrifugation takes supernatant to carry out filtering washing, drying and obtains the redox graphene.
Preferably, the graphene oxide, sodium hydroxide, the weight ratio of sodium borohydride are 1：(2~3)：(2~
3)。
Preferably, the preparation method of the graphene oxide is specially：
Graphite powder and sodium nitrate are distributed in the concentrated sulfuric acid, potassium permanganate is added, is carried out at a temperature of no more than 40 DEG C
React 20~60min；35~50 DEG C are warming up to, 1~2h is reacted；80~100 DEG C are warming up to, deionized water and hydrogen peroxide is added,
Ultrasonically treated, addition watery hydrochloric acid is carried out after 10~30min of stirring, filtering is washed to sulfate radical-free ion presence, obtains yellowish-brown
Sediment, i.e. graphene oxide.
Preferably, the weight ratio of the graphite powder, sodium nitrate and potassium permanganate is (5~7):(2~4):(15~
20)。
Preferably, the mass fraction of the hydrogen peroxide is 30%.
Preferably, the epoxy resin be selected from cycloaliphatic epoxy resin, phenol aldehyde type epoxy resin, bisphenol A-type
At least one of epoxy resin.
Preferably, the organic additive is selected from thixotropic agent, thickener, toughener, surfactant and solvent
At least one of；The solvent is selected from least one of terpinol, ATBC, dibutyl phthalate；Institute
Thixotropic agent is stated for polyamide wax；The surfactant is polyethylene glycol；The toughener is ethyl cellulose.
Second aspect, the invention provides a kind of preparation side of graphene low-temperature solidified silver paste compound as the aforementioned
Method, it comprises the following steps：
Epoxy resin, flake silver powder, modified graphene material and organic additive are mixed, stirred.
Compared with prior art, the present invention has following beneficial effect：
Graphene silver paste is prepared the method comprises the steps of firstly, preparing redox graphene, and using redox graphene,
Solidify under silver paste cryogenic conditions prepared by this method, and add electric conductivity, the electric conductivity compared with silver paste under equal conditions
10~20% are improved, thus under equal electric conductivity, it is possible to decrease silver powder content, while reducing the material of solar energy silver paste
Cost, increase enterprise profit space.
Low-temperature setting graphene silver paste prepared by this method, technique is simple to operation, with low cost, high financial profit,
It is adapted to large-scale industrial production.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that to the ordinary skill of this area
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1
The present embodiment is related to a kind of preparation method of redox graphene, specifically includes following steps：
Step one, graphene oxide is prepared using Hummers methods
100mL 98% dense H is added into 500mL reaction bulbs2SO4, turn on agitator；Weigh respectively 3g graphite powders and
1.5g NaNO3Solid, add it in reaction bulb, stir 30min；Stirring adds KMnO after terminating410g, reaction temperature
Less than 20 DEG C, 20min is stirred；Water-bath is warming up to 35 DEG C, continues to stir 1.5h；Stirring terminates the temperature of water-bath being warming up to
90 DEG C, 200mL deionized waters are instilled in solution；Measure 50mL 30% H2O2, it is added in solution, solution is from dark brown discoloration
Into vivid yellow.Continue to stir 10min, solution is poured into beaker, ultrasonic 30min；Finally with the 5.5% of 1000mL it is dilute
Hydrochloric acid is filtered, and is then fully filtered untill sulfate radical-free ion in filtrate with deionized water again, now the close neutrality of solution,
Obtain tan precipitate thing；Dried in 60 DEG C of baking oven, obtain graphene oxide.
Step 2, prepares redox graphene
Above-mentioned graphene oxide is made into 1.5mg/mL suspensions, 200mL liquid is taken, 0.6g NaOH, 0.6g is added
NaBH4Ultrasonic reaction 15min, 50 DEG C of reaction temperature, reaction is cooled to room temperature after terminating, and high speed centrifugation takes supernatant liquid filtering water
Wash, drying obtains redox graphene.
Embodiment 2
The present embodiment is related to a kind of preparation method of redox graphene, specifically includes following steps：
Step one, graphene oxide is prepared using Hummers methods
100mL 98% dense H is added into 500mL reaction bulbs2SO4, turn on agitator；1g graphite powders and 1g are weighed respectively
NaNO3Solid, add it in reaction bulb, stir 30min；Stirring adds KMnO after terminating45g, reaction temperature is less than 20
DEG C, stir 20min；Water-bath is warming up to 35 DEG C, continues to stir 1h；Stirring terminates the temperature of water-bath being warming up to 90 DEG C, will
200mL deionized waters are instilled in solution；Measure 50mL 30% H2O2, it is added in solution, solution becomes vivid from brownish black
Yellow.Continue to stir 10min, solution is poured into beaker, ultrasonic 30min；Finally use 1000mL 5.5% watery hydrochloric acid mistake
Filter, is then fully filtered untill sulfate radical-free ion in filtrate with deionized water again, and now solution obtains Huang close to neutrality
Tan precipitate；Dried in 60 DEG C of baking oven, obtain graphene oxide.
Step 2, prepares redox graphene
Above-mentioned graphene oxide is made into 1.5mg/mL suspensions, 200mL liquid is taken, 0.4g NaOH, 0.4g is added
NaBH4Ultrasonic reaction 30min, 50 DEG C of reaction temperature, reaction is cooled to room temperature after terminating, and high speed centrifugation takes supernatant liquid filtering water
Wash, drying obtains redox graphene.
Embodiment 3
The present embodiment is related to a kind of preparation method of redox graphene, specifically includes following steps：
Step one, graphene oxide is prepared using Hummers methods
100mL 98% dense H is added into 500mL reaction bulbs2SO4, turn on agitator；3g graphite powders and 3g are weighed respectively
NaNO3Solid, add it in reaction bulb, stir 50min；Stirring adds KMnO after terminating415g, reaction temperature is less than
20 DEG C, stir 30min；Water-bath is warming up to 45 DEG C, continues to stir 1h；Stirring terminates the temperature of water-bath being warming up to 95 DEG C,
200mL deionized waters are instilled in solution；Measure 80mL 30% H2O2, it is added in solution, solution becomes fresh from brownish black
Bright yellow.Continue to stir 15min, solution is poured into beaker, ultrasonic 45min；Finally use 1000mL 5.5% watery hydrochloric acid
Filtering, is then fully filtered untill sulfate radical-free ion in filtrate with deionized water again, and now solution is obtained close to neutrality
Tan precipitate thing；Dried in 60 DEG C of baking oven, obtain graphene oxide.
Step 2, prepares redox graphene
Above-mentioned graphene oxide is made into 2.0mg/mL suspensions, 200mL liquid is taken, 1.0g NaOH, 1.0g is added
NaBH4Ultrasonic reaction 45min, 65 DEG C of reaction temperature, reaction is cooled to room temperature after terminating, and high speed centrifugation takes supernatant liquid filtering water
Wash, drying obtains redox graphene.
Embodiment 4
The present embodiment is related to a kind of preparation method of graphene low-temperature solidified silver paste compound, specifically includes following step
Suddenly：
Modified graphene material prepared by epoxy resin, flake silver powder, organic additive and embodiment 1 and respectively according to
20%th, after 60%, 10%, 10% percetage by weight is weighed, mixing.
Silver paste composition manufactured in the present embodiment is filmed：
Using semiautomatic precision printing machine, the mesh of half tone 280, film thickness is 30um, 120 DEG C of solidification 15min after printing, it
180 DEG C of solidification 30min, carry out resistance test afterwards afterwards, and resistivity is 0.9~2 Ω cm.
Embodiment 5
The present embodiment is related to a kind of preparation method of graphene low-temperature solidified silver paste compound, specifically includes following step
Suddenly：
Modified graphene material prepared by epoxy resin, flake silver powder, organic additive and embodiment 1 and respectively according to
50%th, after 40%, 9.5%, 0.5% percetage by weight is weighed, mixing.
Silver paste composition manufactured in the present embodiment is filmed：
Using semiautomatic precision printing machine, the mesh of half tone 280, film thickness is 30um, 120 DEG C of solidification 15min after printing, it
180 DEG C of solidification 30min, carry out resistance test afterwards afterwards, and resistivity is 5~8 Ω cm.
Embodiment 6
The present embodiment is related to a kind of preparation method of graphene low-temperature solidified silver paste compound, specifically includes following step
Suddenly：
Modified graphene material prepared by epoxy resin, flake silver powder, organic additive and embodiment 1 and respectively according to
50%th, after 40%, 0.5%, 9.5% percetage by weight is weighed, mixing.
Silver paste composition manufactured in the present embodiment is filmed：
Using semiautomatic precision printing machine, the mesh of half tone 280, film thickness is 30um, 120 DEG C of solidification 15min after printing, it
180 DEG C of solidification 30min, carry out resistance test afterwards afterwards, and resistivity is 4.5~7 Ω cm.
Embodiment 7
The present embodiment is related to a kind of preparation method of graphene low-temperature solidified silver paste compound, specifically includes following step
Suddenly：
Modified graphene material prepared by epoxy resin, flake silver powder, organic additive and embodiment 1 and respectively according to
35%th, after 50%, 5%, 10% percetage by weight is weighed, mixing.
Silver paste composition manufactured in the present embodiment is filmed：
Using semiautomatic precision printing machine, the mesh of half tone 280, film thickness is 30um, 120 DEG C of solidification 15min after printing, it
180 DEG C of solidification 30min, carry out resistance test afterwards afterwards, and resistivity is 2.1~3.8 Ω cm.
Embodiment 8
The present embodiment is related to a kind of preparation method of graphene low-temperature solidified silver paste compound, specifically includes following step
Suddenly：
Modified graphene material prepared by epoxy resin, flake silver powder, organic additive and embodiment 1 and respectively according to
40%th, after 45%, 10%, 5% percetage by weight is weighed, mixing.
Silver paste composition manufactured in the present embodiment is filmed：
Using semiautomatic precision printing machine, the mesh of half tone 280, film thickness is 30um, 120 DEG C of solidification 15min after printing, it
180 DEG C of solidification 30min, carry out resistance test afterwards afterwards, and resistivity is 2.5~4.0 Ω cm.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (10)
1. a kind of graphene low-temperature solidified silver paste compound, it is characterised in that the following component including percentage：
2. graphene low-temperature solidified silver paste compound as claimed in claim 1, it is characterised in that the modified graphene material
Expect for redox graphene.
3. graphene low-temperature solidified silver paste compound as claimed in claim 2, it is characterised in that the reduction-oxidation graphite
The preparation method of alkene comprises the following steps：
Graphene oxide is prepared using Hummers methods；
The graphene oxide is configured to suspension, sodium hydroxide, sodium borohydride are added, under 50~80 DEG C of ultrasound condition
After being reacted, centrifugation takes supernatant to carry out filtering washing, drying and obtains the redox graphene.
4. graphene low-temperature solidified silver paste compound as claimed in claim 3, it is characterised in that the graphene oxide,
Sodium hydroxide, the weight ratio of sodium borohydride are 1：(2~3)：(2~3).
5. graphene low-temperature solidified silver paste compound as claimed in claim 3, it is characterised in that the graphene oxide
Preparation method is specially：
Graphite powder and sodium nitrate are distributed in the concentrated sulfuric acid, potassium permanganate is added, is reacted at a temperature of no more than 40 DEG C
20~60min；35~50 DEG C are warming up to, 1~2h is reacted；80~100 DEG C are warming up to, deionized water and hydrogen peroxide, stirring is added
Ultrasonically treated, addition watery hydrochloric acid is carried out after 10~30min, filtering is washed to sulfate radical-free ion presence, obtains tan precipitate
Thing, i.e. graphene oxide.
6. graphene low-temperature solidified silver paste compound as claimed in claim 5, it is characterised in that the graphite powder, nitric acid
The weight ratio of sodium and potassium permanganate is (5~7):(2~4):(15~20).
7. graphene low-temperature solidified silver paste compound as claimed in claim 5, it is characterised in that the quality of the hydrogen peroxide
Fraction is 30%.
8. graphene low-temperature solidified silver paste compound as claimed in claim 1, it is characterised in that the choosing of the epoxy resin
From at least one of cycloaliphatic epoxy resin, phenol aldehyde type epoxy resin, bisphenol A type epoxy resin.
9. graphene low-temperature solidified silver paste compound as claimed in claim 1, it is characterised in that the organic additive choosing
From at least one of thixotropic agent, thickener, toughener, surfactant, antioxidant, dispersant and solvent；The solvent choosing
From at least one of terpinol, ATBC, dibutyl phthalate；The thixotropic agent is polyamide wax；It is described
Surfactant is polyethylene glycol；The toughener is ethyl cellulose.
10. a kind of preparation side of graphene low-temperature solidified silver paste compound as described in any one in claim 1~9
Method, it is characterised in that comprise the following steps：
Epoxy resin, flake silver powder, modified graphene material and organic additive are mixed, stirred.
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| CN108172322A (en) * | 2017-12-26 | 2018-06-15 | 深圳市百柔新材料技术有限公司 | Conductive consent slurry and its preparation method and application |
| CN111210923A (en) * | 2020-03-19 | 2020-05-29 | 德阳烯碳科技有限公司 | Conductive silver paste and preparation process thereof |
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Application publication date: 20171107 |