CN110229648B - Single-component organic silicon conductive adhesive and preparation method and application thereof - Google Patents
Single-component organic silicon conductive adhesive and preparation method and application thereof Download PDFInfo
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- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- 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
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/204—Applications use in electrical or conductive gadgets use in solar cells
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Adhesives Or Adhesive Processes (AREA)
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Abstract
The invention provides a single-component organic silicon conductive adhesive and a preparation method and application thereof. The single-component organic silicon conductive adhesive comprises the following raw materials: 50-85 parts of conductive powder, 10-40 parts of matrix resin, 0.8-5 parts of hydrogen-containing silicone oil, 0.5-3 parts of tackifier, 0.5-3 parts of accelerator, 0.4-2 parts of reinforcing agent and 0.1-0.8 part of polystyrene-coated platinum catalyst, wherein the total amount of the raw materials of the single-component organic silicon conductive adhesive is 100 parts by weight. The invention also provides a preparation method of the conductive adhesive, and the conductive adhesive is used for preparing a solar cell module. The single-component organic silicon conductive adhesive has long storage time, does not need to be added with an inhibitor, does not react at room temperature, and can react quickly at high temperature.
Description
Technical Field
The invention relates to a conductive adhesive, in particular to a single-component organic silicon conductive adhesive, and belongs to the technical field of solar cells.
Background
At present, most of matrixes of common commercial conductive adhesives are composed of epoxy resin, acrylate and organic silicon matrixes. When the epoxy resin or the acrylate is packaged or assembled at 260 ℃ or higher, reliability problems such as decomposition of the body and delamination from the substrate occur. Silicones have excellent weatherability (high temperature, low temperature, high humidity, ultraviolet, etc.) and can be used at high temperatures and in most harsh environments. The solar cell stack tile assembly is used in outdoor environment for more than 25 years, and high-reliability conductive adhesive is needed for interconnection among the cells.
The curing mode of the organic silicon matrix conductive adhesive is mainly condensation type moisture curing and addition type heating curing, compared with condensation type moisture curing organic silicon, the curing speed of the addition type heating curing is high, and the production efficiency can be greatly improved.
Addition-type organosilicon is cross-linked by hydrosilylation using silicon-hydrogen bonds and carbon-carbon unsaturated bonds (usually vinyl) under the catalysis of a noble metal catalyst (usually a platinum complex). Addition silicones are difficult to make as a single component (hydrosilation, vinyl, and catalyst react even at room temperature). The two-component process brings inconvenience to the construction: accurate measurement by an operator is required; mixing equipment and debubbling equipment are required (especially for high viscosity systems); if the mixed materials cannot be used in time, the materials can be solidified to cause waste and the equipment is difficult to clean.
In the prior art, a large amount of stabilizing agent (such as alkynol) is required to be added into the single-component addition type organic silicon conductive adhesive. The stabilizer can volatilize in the curing process, so that the volume shrinkage rate of the product is increased, and the flatness of the surface of the product is influenced; in general, alkynols have a certain toxicity, which limits their use in some fields. Moreover, most of the existing organosilicon conductive adhesives need to be stored at low temperature, have large demand on energy, bring inconvenience to transportation and storage, and simultaneously have short stable storage time.
Chinese patent application CN108239520 discloses a single-component addition type organosilicon conductive adhesive and a preparation method thereof. According to the single-component addition type organic silicon conductive adhesive, the cyanuric acid ester group capable of stabilizing the catalyst is introduced into a base material of the conductive adhesive through molecular design, so that the single-component addition type organic silicon conductive adhesive which is stable in storage at room temperature is obtained. The single-component addition type organic silicon conductive adhesive can be stably stored without adding a large amount of stabilizer such as alkynol, and has good storage stability at room temperature, high curing speed and good conductivity.
However, the conductive adhesive needs to reduce the activity of the catalyst, avoid catalyst poisoning and reduce the addition of an inhibitor by selecting the vinyl modified silicone resin and utilizing the complexation of the melamine in the vinyl modified silicone resin on Pt. Although the method can inhibit the reaction at low temperature to a certain extent, the inhibition functional monomer is connected to the main resin through modification and chemical action, and the inhibition functional monomer also has influence on the catalytic activity at high temperature.
Chinese patent application CN109401724 discloses a single-component conductive silica gel for solar packaging and a preparation method thereof. The coating comprises the following components in parts by weight: 55-80 parts of modified silver powder; 10-20 parts of addition type liquid silicone oil; 0.02-1 part of coupling agent; 2-10 parts of a reinforcing agent; 0.5-4 parts of a crosslinking agent; 2-5 parts of special active diluent; 0.0002 to 0.02 portion of platinum catalyst; 5-20 parts of a solvent. The conductive silica gel can be rapidly cured at a medium and low temperature, has low viscosity, can meet the process requirement of rapid curing of a lamination assembly line, has low cost due to low silver addition amount, can be applied to a solar laminated tile assembly on a large scale, and has the advantages of no toxicity, environmental protection, rapid heat dissipation, high conductivity and good aging resistance, so that the requirements of ultrahigh power, low hot spot effect and outdoor 25-year use of the laminated tile assembly can be met.
However, the conductive adhesive contains a solvent, does not contain an inhibitor, has short storage time and is not environment-friendly.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a single-component silicone conductive adhesive which can be stored stably and has low cost.
In order to achieve the technical purpose, the invention provides a single-component organic silicon conductive adhesive, which comprises the following raw materials: 50-85 parts of conductive powder, 10-40 parts of matrix resin, 0.8-5 parts of hydrogen-containing silicone oil, 0.5-3 parts of tackifier, 0.5-3 parts of accelerator, 0.4-2 parts of reinforcing agent and 0.1-0.8 part of polystyrene-coated platinum catalyst, wherein the total amount of the raw materials of the single-component organic silicon conductive adhesive is 100 parts by weight.
In one embodiment of the present invention, the polystyrene-coated platinum catalyst is prepared by the following steps:
mixing chloroplatinic acid, silane monomer and isopropanol, heating to 50-60 ℃, and reacting for 0.5-3 hours;
slowly adding sodium bicarbonate, stirring and reacting for 1-3 hours at the temperature of 70-80 ℃, and filtering to remove precipitates;
adding the filtrate into the polystyrene dispersion liquid under the stirring condition, filtering and cleaning to obtain a polystyrene-coated platinum catalyst;
wherein the mass ratio of chloroplatinic acid to silane monomer to isopropanol to sodium bicarbonate to polystyrene dispersion is 0.1-10: 1-50: 10-300: 1-3: 50-500.
The polystyrene-coated platinum catalyst obtained by the preparation method of the polystyrene-coated platinum catalyst has a micro-capsule structure. The micro-capsule catalyst and other components of the conductive adhesive have synergistic effect, so that the single-component organic silicon conductive adhesive has the advantages of stable performance at normal temperature and quick curing at high temperature. Moreover, the single-component organic silicon conductive adhesive adopts the capsule type platinum catalyst and the conductive powder with low apparent density, so that the single-component organic silicon conductive adhesive has stable performance, is stored at normal temperature and has lower cost.
The concentration of the polystyrene-coated platinum catalyst can be adjusted by adding a corresponding polystyrene dispersion liquid according to the target.
In one embodiment of the present invention, the stirring speed when preparing the polystyrene-coated platinum catalyst is 800rpm to 1500 rpm.
In one embodiment of the invention, the silane monomer comprises tetramethyldivinyldisiloxane, vinyltrimethoxysilane or vinyltriethoxysilane.
The single-component organic silicon conductive adhesive contains conductive powder.
In one embodiment of the present invention, the conductive powder includes one or a combination of two or more of silver powder, copper powder, gold powder, aluminum powder, nickel powder, and silver-coated copper powder.
In one embodiment of the present invention, the conductive powder used has a particle size of 50 μm or less (preferably 0.1 to 50 μm).
In one embodiment of the present invention, the conductive powder used has a bulk density of 0.9g/mm3-5g/mm3。
The single-component organic silicon conductive adhesive contains matrix resin, and the matrix resin plays a role in bonding and carrying.
In one embodiment of the present invention, the base resin is obtained by mixing methyl vinyl MQ resin and/or phenyl vinyl MQ resin with vinyl silicone oil in a mass ratio of 1: 1. Namely, the matrix resin is obtained by mixing methyl vinyl MQ resin and vinyl silicone oil in a mass ratio of 1: 1; or obtained by mixing phenyl vinyl MQ resin and vinyl silicone oil in a mass ratio of 1: 1; or methyl vinyl MQ resin, phenyl vinyl MQ resin and vinyl silicone oil in a mass ratio of 1: 1.
In one embodiment of the present invention, the viscosity of the matrix resin is 500Pa · S to 5000Pa · S. The base resin with the viscosity is convenient to operate and screen printing.
The single-component organic silicon conductive adhesive contains hydrogen-containing silicone oil which is used as a cross-linking agent in a system.
In a specific embodiment of the invention, the hydrogen-containing silicone oil is hydrogen-terminated silicone oil and side hydrogen silicone oil in a molar ratio of 1:1-1: 5.
The single-component organic silicon conductive adhesive contains the tackifier, has no special requirement on the selection of the tackifier, and can be prepared by adopting the conventional reagent in the field.
The single-component organic silicon conductive adhesive contains an accelerant, wherein the accelerant is an adhesion promoter.
In one embodiment of the present invention, the accelerator used may be one or a combination of two or more of vinyltriethoxysilane, vinyltrimethoxysilane, vinyl-3- (2-methoxyethoxy) silane, gamma-methacryloxypropyltrimethoxysilane, epoxy silane oligomer, and beta- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane.
The single-component organic silicon conductive adhesive contains a reinforcing agent. The reinforcing agent can improve the strength after curing and increase the bonding force of the conductive adhesive.
In one embodiment of the present invention, the strengthening agent used may be fumed silica.
The invention also provides a preparation method of the single-component organic silicon conductive adhesive, which comprises the following steps:
mixing the matrix resin, the hydrogen-containing silicone oil, the tackifier and the accelerant, stirring for 5min-60min, adding the reinforcing agent, and stirring for 5min-60min to obtain a mixture;
and adding conductive powder into the mixture, stirring for 10min-120min, adding a polystyrene-coated platinum catalyst, and stirring for 1min-60min to obtain the single-component organic silicon conductive adhesive.
The invention provides a solar cell module, wherein the single-component organic silicon conductive adhesive is adopted as a conductive adhesive when the solar cell module is prepared. The solar module herein includes, but is not limited to, a solar shingle module.
The curing time of the single-component organic silicon conductive adhesive at 140-180 ℃ is 0.1-30 min.
The single-component organic silicon conductive adhesive has long storage time, does not need to be added with an inhibitor (the yellowing phenomenon caused by the addition of the inhibitor is avoided), does not react at room temperature, and quickly reacts at high temperature.
The single-component organic silicon conductive adhesive disclosed by the invention is solvent-free, environment-friendly and high in reliability.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Examples
The polystyrene-coated platinum catalyst is prepared by the following steps:
mixing 1g of chloroplatinic acid, 5g of ligand silane monomer (tetramethyl divinyl disiloxane) and 40g of isopropanol, heating to 55 ℃, and reacting for 3 hours;
slowly adding 1.5g sodium bicarbonate (after 5 min), stirring at 75 deg.C for 2 hr, and filtering to remove precipitate;
the filtrate was added to 200g of a resin (polystyrene) solution (toluene) at 800-.
The catalysts in the subsequent examples were prepared in this way.
The single-component organic silicon conductive adhesive is prepared by the following steps:
weighing the base resin (the mass ratio of the methyl ethyl MQ resin to the vinyl silicone oil is 1:1 in examples 1-3, and the viscosity is 2500 Pa.S; the mass ratio of the phenyl vinyl MQ resin to the vinyl silicone oil is 1:1 in examples 4-6, and the viscosity is 2000 Pa.s), the hydrogen-containing silicone oil (the molar ratio of the hydrogen-terminated silicone oil to the side hydrogen silicone oil is 1: 2), the tackifier and the adhesion promoter (gamma-methacryloxypropyl trimethoxy silane) in sequence according to the content of the table 1, stirring for 15min, continuously adding the reinforcing agent (fumed silica), and stirring for 15min to obtain a mixture;
and adding conductive powder into the mixture, stirring for 50min, adding a catalyst, stirring for 30min, and removing bubbles in vacuum to obtain the final conductive adhesive.
Testing the curing speed at 150 ℃; the tensile force of the adhesive tape is tested at normal temperature (no industry standard number, all the internal standards of enterprises, the length of a bonding area is 1mm, and the width is 400 mu m), and the result is shown in table 1.
The preparation process of the laminated cell component comprises the following steps:
and printing the finished battery piece printed with the front electrode and the back electrode on a designated position by using a screen printing method, slicing, stacking, curing (testing tensile force by using the cured stacked piece), and packaging the spliced pieces to obtain the laminated assembly.
TABLE 1
The comparison is shown in Table 2.
TABLE 2
The above examples illustrate that the one-component silicone conductive adhesive of the present invention has a long storage time, does not require the addition of an inhibitor (which prevents yellowing due to the addition of an inhibitor), does not react at room temperature, and reacts rapidly at high temperatures.
Claims (12)
1. The single-component organic silicon conductive adhesive is characterized by comprising the following raw materials: 50-85 parts of conductive powder, 10-40 parts of matrix resin, 0.8-5 parts of hydrogen-containing silicone oil, 0.5-3 parts of tackifier, 0.5-3 parts of accelerator, 0.4-2 parts of reinforcing agent and 0.1-0.8 part of polystyrene-coated platinum catalyst, wherein the total amount of the raw materials of the single-component organic silicon conductive adhesive is 100 parts by weight;
the polystyrene-coated platinum catalyst is prepared by the following steps:
mixing chloroplatinic acid, silane monomer and isopropanol, heating to 50-60 ℃, and reacting for 0.5-3 hours;
adding sodium bicarbonate, stirring and reacting for 1-3 hours at the temperature of 70-80 ℃, and filtering to remove precipitates;
adding the filtrate into the polystyrene dispersion liquid under the stirring condition, filtering and cleaning to obtain a polystyrene-coated platinum catalyst, wherein the polystyrene-coated platinum catalyst has a micro-capsule structure;
wherein the mass ratio of chloroplatinic acid to silane monomer to isopropanol to sodium bicarbonate to polystyrene dispersion is 0.1-10: 1-50: 10-300: 1-3: 50-500;
wherein the loose packed density of the conductive powder is 0.9g/mm3-5g/mm3。
2. The one-component silicone conductive adhesive according to claim 1, wherein the stirring speed is 800rpm to 1500 rpm.
3. The one-component silicone conductive paste according to claim 1, wherein the silane monomer comprises tetramethyldivinyldisiloxane, vinyltrimethoxysilane, or vinyltriethoxysilane.
4. The single-component silicone conductive adhesive according to claim 1, wherein the conductive powder comprises one or a combination of two or more of silver powder, copper powder, gold powder, aluminum powder, nickel powder, and silver-coated copper powder.
5. The single-component silicone conductive adhesive according to claim 1, wherein the particle size of the conductive powder is not more than 50 μm.
6. The one-component silicone conductive paste according to claim 1, wherein the base resin is obtained by mixing a methyl vinyl MQ resin and/or a phenyl vinyl MQ resin with a vinyl silicone oil at a mass ratio of 1: 1.
7. The one-component silicone conductive adhesive according to claim 1, wherein the viscosity of the matrix resin is 500 Pa-S to 5000 Pa-S.
8. The single-component silicone conductive adhesive according to claim 1, wherein the hydrogen-containing silicone oil is hydrogen-terminated silicone oil and side hydrogen silicone oil in a molar ratio of 1:1-1: 5.
9. The single-component silicone conductive adhesive according to claim 1, wherein the accelerator is one or a combination of two or more of vinyltriethoxysilane, vinyltrimethoxysilane, vinyl-3- (2-methoxyethoxy) silane, γ -methacryloxypropyltrimethoxysilane, epoxy silane oligomer, and β - (3, 4-epoxycyclohexyl) ethyltrimethoxysilane.
10. The one-component silicone conductive paste according to claim 1, wherein the reinforcing agent is fumed silica.
11. The method for preparing the one-component silicone conductive adhesive according to any one of claims 1 to 10, comprising the steps of:
mixing the matrix resin, the hydrogen-containing silicone oil, the tackifier and the accelerant, stirring for 5min-60min, adding the reinforcing agent, and stirring for 5min-60min to obtain a mixture;
and adding conductive powder into the mixture, stirring for 10min-120min, adding a polystyrene-coated platinum catalyst, and stirring for 1min-60min to obtain the single-component organic silicon conductive adhesive.
12. A solar cell module, wherein the single-component silicone conductive paste according to any one of claims 1 to 10 is used as a conductive paste when the solar cell module is manufactured.
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CN111394012B (en) * | 2020-04-15 | 2021-07-09 | 苏州世诺新材料科技有限公司 | Self-repairing organic silicon conductive adhesive |
CN112961646A (en) * | 2021-03-03 | 2021-06-15 | 上海斟众新材料科技股份有限公司 | Fast-curing anti-overflow conductive adhesive and preparation method thereof |
CN115433541B (en) * | 2022-09-30 | 2023-11-07 | 郑州中原思蓝德高科股份有限公司 | Conductive adhesive and preparation method thereof |
CN116496752B (en) * | 2023-04-11 | 2023-10-03 | 上海德朗聚新材料有限公司 | High-toughness organosilicon shingle conductive adhesive and preparation method thereof |
CN116618642B (en) * | 2023-07-13 | 2023-10-10 | 长沙立优金属材料有限公司 | Nickel powder with large particles and low apparent density and preparation method and application thereof |
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