CN113930216A - Preparation method of low-silver-filling-amount conductive adhesive - Google Patents
Preparation method of low-silver-filling-amount conductive adhesive Download PDFInfo
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- CN113930216A CN113930216A CN202111263112.2A CN202111263112A CN113930216A CN 113930216 A CN113930216 A CN 113930216A CN 202111263112 A CN202111263112 A CN 202111263112A CN 113930216 A CN113930216 A CN 113930216A
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- 239000000853 adhesive Substances 0.000 title claims abstract description 40
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 77
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000011049 filling Methods 0.000 claims abstract description 9
- 229920005989 resin Polymers 0.000 claims abstract description 8
- 239000011347 resin Substances 0.000 claims abstract description 8
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 230000004048 modification Effects 0.000 claims abstract description 6
- 238000012986 modification Methods 0.000 claims abstract description 6
- 239000003607 modifier Substances 0.000 claims abstract description 6
- 239000000654 additive Substances 0.000 claims abstract description 5
- 230000000996 additive effect Effects 0.000 claims abstract description 5
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 5
- 239000010703 silicon Substances 0.000 claims abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000011231 conductive filler Substances 0.000 claims abstract description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 25
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 21
- 239000003054 catalyst Substances 0.000 claims description 14
- 229910001312 Amalgam (dentistry) Inorganic materials 0.000 claims description 13
- 239000004944 Liquid Silicone Rubber Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 229920002379 silicone rubber Polymers 0.000 claims description 13
- 239000003085 diluting agent Substances 0.000 claims description 12
- 239000003112 inhibitor Substances 0.000 claims description 12
- 229910052697 platinum Inorganic materials 0.000 claims description 12
- 229920002050 silicone resin Polymers 0.000 claims description 11
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- -1 methyl vinyl Chemical group 0.000 claims description 9
- 239000003921 oil Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000007547 defect Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000010907 mechanical stirring Methods 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000001132 ultrasonic dispersion Methods 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 3
- 238000010248 power generation Methods 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000000713 high-energy ball milling Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000007259 addition reaction Methods 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a preparation method of a low-silver-filling-amount conductive adhesive, which comprises the following steps: 1) carrying out heat treatment on the conductive filler flake silver powder; 2) adding the silver powder subjected to the heat treatment in the step 1) into a surface modifier solution, performing surface modification treatment, dispersing, performing ultrasonic treatment, performing suction filtration, washing and drying to obtain surface modified silver powder; 3) and (2) taking organic silicon resin as base resin, adding an additive, mixing and dispersing uniformly, adding the surface modified silver powder obtained in the step 2), and mixing uniformly to obtain the conductive adhesive with the silver powder filling amount of 55-65%. The conductive adhesive prepared by the invention not only meets the conductive performance and mechanical property required by the laminated assembly, but also reduces the consumption of silver powder, effectively reduces the cost and is beneficial to popularization and application of the laminated assembly.
Description
Technical Field
The invention relates to the field of electronic materials, in particular to a preparation method of a conductive adhesive with low silver filling amount.
Background
With the continuous development of human society, people have more and more demands on energy. Solar energy is used as a green pollution-free renewable energy source, the storage capacity is huge, the acquisition is convenient, people pay attention in recent years, and photovoltaic power generation is one of the most direct modes for human to utilize solar energy.
The power generation amount of a single battery is very small, so that battery pieces are required to be connected in parallel or in series to form an assembly, and enough current can be obtained for people to utilize. The traditional assembly is to connect the battery plates by using tin-lead welding strips and transmit current. However, the solder strip also has many limitations, such as the limitation of silicon wafer thickness, the reduction of power generation caused by battery plate shielding, the occurrence of metal corrosion, etc.
In the tile-stacking technology, the conductive adhesive is used for replacing a welding strip, so that the shielding of the welding strip is avoided, the internal resistance is effectively reduced, and the power of the assembly is promoted; the photovoltaic module is mainly outdoors, and silver is generally used as a filler of the conductive adhesive in consideration of the possibility of oxidation and corrosion, but the cost of silver powder is high.
Disclosure of Invention
The invention provides a preparation method of a low-silver-filling-amount conductive adhesive, which comprises the following steps:
1) carrying out heat treatment on the conductive filler flake silver powder;
2) adding the silver powder subjected to the heat treatment in the step 1) into a surface modifier solution, performing surface modification treatment, dispersing, performing ultrasonic treatment, performing suction filtration, washing and drying to obtain surface modified silver powder;
3) and (2) taking organic silicon resin as base resin, adding an additive, mixing and dispersing uniformly, adding the surface modified silver powder obtained in the step 2), and mixing uniformly to obtain the conductive adhesive with the silver powder filling amount of 55-65%.
Preferably, in step 1), the heat treatment is: and (3) placing the flake silver powder in a vacuum drying oven, preserving heat for 6-8 h at 150-170 ℃, and naturally cooling in the drying oven after heat preservation is finished.
Preferably, in step 2), the surface modifier solution comprises: 85-95 parts by mass of an ethanol solution, 1-9 parts by mass of gamma-methacryloxypropyltrimethoxysilane and 1-6 parts by mass of dilute nitric acid.
Preferably, in the step 2), the concentration of the ethanol solution is 85-95%.
Preferably, in step 2), toluene is used for washing.
Preferably, in step 3), the silicone resin is selected from methyl vinyl liquid silicone rubber and hydrogen-containing liquid silicone resin.
Preferably, in step 3), the additive is selected from one or more of an inhibitor, a diluent and a catalyst.
Preferably, in the step 3), the ethynyl cyclohexanol is used as an inhibitor, the dearomatized solvent oil is used as a diluent, and the platinum catalyst is used as a catalyst.
Preferably, in the step 1), the amount of the flake silver powder is 55 to 65 parts by mass.
Preferably, in the step 3), the amount of the methyl vinyl liquid silicone rubber is 15-25 parts by mass, the amount of the hydrogen-containing liquid silicone resin is 10-20 parts by mass, the amount of the ethynylcyclohexanol serving as an inhibitor is 0.1-0.3 part by mass, the amount of the dearomatization solvent oil serving as a diluent is 5-7 parts by mass, and the amount of the platinum catalyst is 0.2-0.5 part by mass.
The invention has the advantages and beneficial effects that: the preparation method of the conductive adhesive with low silver filling amount is provided, and the flaky silver powder is subjected to heat treatment, so that the lattice defects generated in the preparation process of the flaky silver powder by high-energy ball milling are reduced and eliminated, the microstructure of the silver powder is improved, and the silver powder forms a better lap joint passage in the conductive adhesive; after the heat treatment is finished, the surface of the silver powder is modified, so that the dispersibility of the silver powder and the intermiscibility of an inorganic-organic interface are improved, and the bonding performance of the conductive adhesive is improved; on the premise of low silver filling amount, the conductive adhesive is ensured to have excellent conductivity and reliable bonding force.
In general, spherical silver powder is industrially prepared by a chemical reduction method, and flake silver powder is obtained by a mechanical ball milling method, and the flake silver powder prepared by severe plastic deformation generated by impact, grinding pressure and the like of a high-energy grinding ball on the spherical silver powder is often accompanied by the change of the microstructure and the structure of the material, such as the generation of defects of lattice distortion, dislocation, twin crystal, holes and the like. The defects have strong scattering effect on moving electrons, so that the intrinsic resistance of the silver powder is increased, and the conductivity of the conductive film layer prepared by the silver powder is directly influenced.
According to the invention, the heat treatment is carried out on the flake silver powder, so that the silver powder can be recrystallized, and the size and the crystallinity of crystal grains are increased; moreover, the residual stress and strain generated by strong plastic deformation in the ball milling process are eliminated in the heat treatment process, and the lattice distortion is reduced; the crystal defects such as dislocation, twin crystal and the like generated by ball milling can be reduced, and the distortion of the flake silver powder is released, so that the flake silver powder is in a more stable structural form and energy state, the conductivity of the flake silver powder is effectively improved, and the silver powder filling amount of the conductive adhesive can be reduced.
In addition, after the filling amount of the silver powder is reduced, in order to prevent the mechanical property of the conductive adhesive from being reduced, the surface of the silver powder subjected to heat treatment is modified, the dispersibility and the intermiscibility of an inorganic-organic interface of the silver powder are improved, and the bonding property of the conductive adhesive is improved; on the premise of low silver filling amount, the conductive adhesive is ensured to have excellent conductivity and reliable bonding force.
The ethanol solution used in the step 2) can disperse the silver powder and dissolve the coupling agent, so that the silver powder is more fully contacted with the modifier; the gamma-methacryloxypropyltrimethoxysilane is used as a coupling agent, is combined on the surface of the silver powder in a chemical bonding mode after being hydrolyzed to form an organic coating layer, so that the dispersibility of the silver powder in resin is improved, and the intermiscibility of inorganic and organic interfaces is promoted, thereby improving the bonding property of the conductive adhesive; the dilute nitric acid can adjust the pH of the system to a certain value, so that the coupling agent is hydrolyzed.
The residual organic matter which is not grafted and is left in the surface modification solution can be removed by adopting toluene for washing in the step 2).
The methyl vinyl liquid silicone rubber used in the step 3) can be used as a basic polymer of addition type liquid silicone rubber; the hydrogen-containing liquid silicone resin can be used as a cross-linking agent of the addition type liquid silicone rubber; the inhibitor ethynylcyclohexanol is adopted, and the inhibitor ethynylcyclohexanol can form a coordination bond with a platinum atom in a platinum catalyst under a low-temperature condition, so that addition reaction of zero-valent platinum on silicon vinyl (Si-Vi) and a hydrosilation group (Si-H) is prevented, and the sizing material can be placed for a long time at room temperature; the diluent dearomatization solvent oil can be used as a diluent to reduce the viscosity of the system, so that the silver powder can be well dispersed in the matrix resin, and simultaneously good conductive contact is formed among the silver powder, the adhesive layer and the bonded object; the platinum catalyst is adopted, and the curing reaction of the addition type liquid silicone rubber is completed under the catalytic action of a complex of platinum, so that the addition type liquid silicone rubber can be quickly cured by heating.
The conductive adhesive prepared by the invention not only meets the conductive performance and mechanical property required by the laminated assembly, but also reduces the consumption of silver powder, effectively reduces the cost and is beneficial to popularization and application of the laminated assembly.
Detailed Description
The following further describes embodiments of the present invention with reference to examples. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
The invention provides a preparation method of a low-silver-filling-amount conductive adhesive, which comprises the following steps:
1) putting 55-65 parts by mass of flaky silver powder into a vacuum drying oven, preserving heat for 6-8 hours at 150-170 ℃, and naturally cooling in the drying oven after heat preservation;
2) adding the silver powder subjected to the heat treatment in the step 1) into 100-120 parts by mass of an ethanol solution, wherein the concentration of the ethanol solution is 85% -95%, the ethanol solution also contains 1-9 parts by mass of gamma-methacryloxypropyltrimethoxysilane, then dropwise adding 1-6 parts by mass of dilute nitric acid, keeping the temperature at 30-50 ℃, performing ultrasonic dispersion, and performing mechanical stirring, after 0.3-0.5 h, performing suction filtration on a reactant, then washing with toluene, performing vacuum drying for 12-24 h, and obtaining the surface modified silver powder at the temperature of 50-70 ℃;
3) uniformly mixing and uniformly mixing 15-25 parts by mass of methyl vinyl liquid silicone rubber, 10-20 parts by mass of hydrogen-containing liquid silicone resin, 0.1-0.3 part by mass of inhibitor ethynylcyclohexanol, 5-7 parts by mass of diluent dearomatization solvent oil and 0.2-0.5 part by mass of platinum catalyst at normal temperature, adding the surface modified silver powder obtained in the step 2), fully stirring and uniformly mixing, and performing vacuum defoaming to prepare the conductive adhesive with the silver powder filling amount of 55-65%.
According to the invention, through carrying out heat treatment on the flake silver powder, the reduction and elimination of lattice defects generated in the preparation process of the flake silver powder by high-energy ball milling are realized, the microstructure of the silver powder is improved, and the silver powder forms a better lap joint passage in the conductive adhesive; after the heat treatment is finished, the surface of the silver powder is modified, so that the dispersibility of the silver powder and the intermiscibility of an inorganic-organic interface are improved, and the bonding performance of the conductive adhesive is improved; on the premise of low silver filling amount, the conductive adhesive is ensured to have excellent conductivity and reliable bonding force.
The specific embodiment of the invention is as follows:
example 1
1) Putting 60 parts by mass of flake silver powder into a vacuum drying oven, preserving heat for 6 hours at 170 ℃, and naturally cooling in the drying oven after heat preservation is finished;
2) adding the silver powder subjected to the heat treatment in the step 1) into 110 parts by mass of ethanol solution, wherein the concentration of the ethanol solution is 92%, the ethanol solution also contains 5 parts by mass of gamma-methacryloxypropyltrimethoxysilane, then dropwise adding 3 parts by mass of dilute nitric acid, keeping the temperature at 40 ℃, performing ultrasonic dispersion, performing mechanical stirring, after 0.5h, performing suction filtration on a reactant, then washing with toluene, performing vacuum drying for 24h at the temperature of 60 ℃, and obtaining the surface modified silver powder;
3) uniformly mixing and uniformly mixing 22 parts by mass of methyl vinyl liquid silicone rubber, 11 parts by mass of hydrogen-containing liquid silicone resin, 0.2 part by mass of inhibitor ethynylcyclohexanol, 6.5 parts by mass of diluent dearomatization solvent oil and 0.3 part by mass of platinum catalyst at normal temperature, adding the surface modified silver powder obtained in the step 2), fully stirring and uniformly mixing, and performing vacuum defoaming to obtain the conductive adhesive with the silver powder filling amount of 60%.
The conductive adhesive prepared in example 1 has the following properties: curing at 170 deg.C for 10min, and volume resistivity of 8 × 10-4Omega cm, shear strength 4.4 MPa.
Example 2
1) Putting 65 parts by mass of flake silver powder into a vacuum drying oven, preserving heat for 8 hours at 150 ℃, and naturally cooling in the drying oven after heat preservation is finished;
2) adding the silver powder subjected to the heat treatment in the step 1) into 120 parts by mass of ethanol solution, wherein the concentration of the ethanol solution is 91%, the ethanol solution also contains 7 parts by mass of gamma-methacryloxypropyltrimethoxysilane, then dropwise adding 2 parts by mass of dilute nitric acid, keeping the temperature at 50 ℃, performing ultrasonic dispersion, performing mechanical stirring, after 0.3h, performing suction filtration on a reactant, then washing with toluene, performing vacuum drying for 15h at the temperature of 70 ℃, and obtaining surface modified silver powder;
3) uniformly mixing and uniformly mixing 20 parts by mass of methyl vinyl liquid silicone rubber, 9.7 parts by mass of hydrogen-containing liquid silicone resin, 0.1 part by mass of inhibitor ethynylcyclohexanol, 5 parts by mass of diluent dearomatization solvent oil and 0.2 part by mass of platinum catalyst at normal temperature, adding the surface modified silver powder obtained in the step 2), fully stirring and uniformly mixing, and performing vacuum defoaming to obtain the conductive adhesive with the silver powder filling amount of 65%.
The conductive adhesive prepared in example 2 has the following properties: curing at 170 deg.C for 10min, and volume resistivity of 6.8 × 10-4Omega cm, shear strength of 7.5 MPa.
Example 3
1) Putting 55 parts by mass of flake silver powder into a vacuum drying oven, preserving heat for 6 hours at 160 ℃, and naturally cooling in the drying oven after heat preservation is finished;
2) adding the silver powder subjected to the heat treatment in the step 1) into 100 parts by mass of ethanol solution, wherein the concentration of the ethanol solution is 95%, the ethanol solution also contains 3 parts by mass of gamma-methacryloxypropyltrimethoxysilane, then dropwise adding 2 parts by mass of dilute nitric acid, keeping the temperature at 50 ℃, performing ultrasonic dispersion, performing mechanical stirring, after 0.2h, performing suction filtration on a reactant, then washing with toluene, performing vacuum drying for 20h at the temperature of 60 ℃, and obtaining the surface modified silver powder;
3) uniformly mixing 25 parts by mass of methyl vinyl liquid silicone rubber, 12.5 parts by mass of hydrogen-containing liquid silicone resin, 0.1 part by mass of inhibitor ethynylcyclohexanol, 7 parts by mass of diluent dearomatization solvent oil and 0.4 part by mass of platinum catalyst at normal temperature, adding the surface modified silver powder obtained in the step 2), fully stirring and uniformly mixing, and performing vacuum defoaming to obtain the conductive adhesive with the silver powder filling amount of 55%.
The conductive adhesive prepared in example 3 has the following properties: curing at 170 deg.C for 10min, and volume resistivity of 1.2 × 10-3Omega cm, shear strength of 2.8 MPa.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The preparation method of the conductive adhesive with low silver filling amount is characterized by comprising the following steps:
1) carrying out heat treatment on the conductive filler flake silver powder;
2) adding the silver powder subjected to the heat treatment in the step 1) into a surface modifier solution, performing surface modification treatment, dispersing, performing ultrasonic treatment, performing suction filtration, washing and drying to obtain surface modified silver powder;
3) and (2) taking organic silicon resin as base resin, adding an additive, mixing and dispersing uniformly, adding the surface modified silver powder obtained in the step 2), and mixing uniformly to obtain the conductive adhesive with the silver powder filling amount of 55-65%.
2. The method for preparing the conductive adhesive with low silver filling amount according to claim 1, wherein in the step 1), the heat treatment is as follows: and (3) placing the flake silver powder in a vacuum drying oven, preserving heat for 6-8 h at 150-170 ℃, and naturally cooling in the drying oven after heat preservation is finished.
3. The method of claim 1, wherein in step 2), the surface modifier solution comprises: 85-95 parts by mass of an ethanol solution, 1-9 parts by mass of gamma-methacryloxypropyltrimethoxysilane and 1-6 parts by mass of dilute nitric acid.
4. The method for preparing the conductive adhesive with low silver filling amount according to claim 3, wherein the concentration of the ethanol solution in the step 2) is 85-95%.
5. The method for preparing the low silver loading conductive paste according to claim 3, wherein in the step 2), toluene washing is used.
6. The method for preparing the conductive adhesive with low silver filling amount according to claim 1, wherein in the step 3), the silicone resin is selected from methyl vinyl liquid silicone rubber and hydrogen-containing liquid silicone resin.
7. The method for preparing the conductive adhesive with low silver filling amount according to claim 6, wherein in the step 3), the additive is one or more selected from an inhibitor, a diluent and a catalyst.
8. The method for preparing the conductive adhesive with low silver filling amount according to claim 7, wherein in the step 3), the ethynyl cyclohexanol is used as an inhibitor, the dearomatized solvent oil is used as a diluent, and the platinum catalyst is used as a catalyst.
9. The method for preparing the conductive adhesive with low silver filling amount according to claim 8, wherein the flake silver powder is used in an amount of 55 to 65 parts by mass in the step 1).
10. The method for preparing the conductive adhesive with low silver filling amount according to claim 9, wherein in the step 3), the amount of the methyl vinyl liquid silicone rubber is 15-25 parts by mass, the amount of the hydrogen-containing liquid silicone resin is 10-20 parts by mass, the amount of the inhibitor ethynylcyclohexanol is 0.1-0.3 part by mass, the amount of the diluent dearomatization solvent oil is 5-7 parts by mass, and the amount of the platinum catalyst is 0.2-0.5 part by mass.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111961436A (en) * | 2020-08-11 | 2020-11-20 | 上海锐朗光电材料有限公司 | Photovoltaic laminated tile assembly organic silicon conductive adhesive and preparation method thereof |
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2021
- 2021-10-28 CN CN202111263112.2A patent/CN113930216A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111961436A (en) * | 2020-08-11 | 2020-11-20 | 上海锐朗光电材料有限公司 | Photovoltaic laminated tile assembly organic silicon conductive adhesive and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 王国建 编著: "《功能高分子材料》", 30 June 2014, 同济大学出版社 * |
| 车龙 等: "《热处理对片状银粉微观结构的影响》", 《贵金属》 * |
| 黄志彬: "《导热透明有机硅灌封胶的制备与性能研究》", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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Application publication date: 20220114 |