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WO2014088180A1 - Composition adhésive pour module de cellule solaire, élément adhésif pour module de cellule solaire formé à partir de celle-ci et module de cellule solaire le comprenant - Google Patents

Composition adhésive pour module de cellule solaire, élément adhésif pour module de cellule solaire formé à partir de celle-ci et module de cellule solaire le comprenant Download PDF

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Publication number
WO2014088180A1
WO2014088180A1 PCT/KR2013/006465 KR2013006465W WO2014088180A1 WO 2014088180 A1 WO2014088180 A1 WO 2014088180A1 KR 2013006465 W KR2013006465 W KR 2013006465W WO 2014088180 A1 WO2014088180 A1 WO 2014088180A1
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WO
WIPO (PCT)
Prior art keywords
formula
solar cell
polysilsesquioxane
cell module
compound
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/KR2013/006465
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English (en)
Korean (ko)
Inventor
이윤만
손인영
김소현
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lotte Fine Chemical Co Ltd
Original Assignee
Samsung Fine Chemicals Co Ltd
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Filing date
Publication date
Application filed by Samsung Fine Chemicals Co Ltd filed Critical Samsung Fine Chemicals Co Ltd
Publication of WO2014088180A1 publication Critical patent/WO2014088180A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F19/00—Integrated devices, or assemblies of multiple devices, comprising at least one photovoltaic cell covered by group H10F10/00, e.g. photovoltaic modules
    • 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
    • C09J183/02—Polysilicates
    • 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
    • C09J183/14—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 in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F19/00—Integrated devices, or assemblies of multiple devices, comprising at least one photovoltaic cell covered by group H10F10/00, e.g. photovoltaic modules
    • H10F19/80—Encapsulations or containers for integrated devices, or assemblies of multiple devices, having photovoltaic cells
    • H10F19/804—Materials of encapsulations
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/12—Polysiloxanes containing silicon bound to hydrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy

Definitions

  • An adhesive composition for a solar cell module, an adhesive member for a solar cell module formed therefrom, and a solar cell module having the same are provided.
  • the solar cell module can produce a desired output by connecting several solar cells to each other, and is made of a structure that can protect the battery from long-term natural environments and external shocks.
  • a glass substrate with excellent light transmittance is used, and on the back, a back sheet made of a material having excellent moisture permeation prevention and electrical insulation properties is provided.
  • the solar cell module is manufactured by sealing and compressing a glass substrate, a back sheet, a solar cell, and a frame accommodating the solar cell using an adhesive member.
  • the adhesive member is generally formed by using a one-component adhesive composition containing a silsesquioxane oligomer, a filler, and the like in which a vinyl group, hydrogen and a hydroxyl group coexist in one molecule.
  • the above-described adhesive composition may not only be stored at a low temperature because the crosslinking reaction may occur during storage at room temperature, and the uniformity and adhesion of the cured coating film formed from the adhesive composition may not reach satisfactory levels.
  • Agent A containing a polysilsesquioxane compound having a C2-C10 alkenyl group and a C1-C10 alkyl group at the terminal and side chain according to one aspect of the present invention
  • an adhesive composition for a solar cell module comprising a B agent containing a polycelsesquioxane compound having hydrogen and a C1-C10 alkyl group at its terminal and side chains.
  • an adhesive member for a solar cell module including a curing reaction product of the adhesive composition for a solar cell module described above.
  • the adhesive composition for a solar cell module according to an embodiment of the present invention is excellent in storage stability, and by using this, an adhesive member for a solar cell module having improved adhesion and mechanical properties may be manufactured.
  • the adhesive composition for a solar cell module includes A containing a polysilsesquioxane compound having a C2-C10 alkenyl group and a C1-C10 alkyl group (hereinafter referred to as "polysilsesquioxane A”) at its terminal and side chains.
  • Agent, and a B agent containing a polycelsesquioxane compound having a hydrogen and a C1-C10 alkyl group hereinafter referred to as "polysilsesquioxane B" at the terminal and side chain.
  • the solar cell module adhesive composition is a two-component composition, unlike the conventional one-component adhesive composition is very excellent in storage stability and can be stored at room temperature.
  • the adhesive composition for the solar cell module does not use high specific gravity fillers such as silicon oxide (SiO 2 ) and calcium carbonate (CaCO 3 ), thereby improving workability by weight reduction. And using such an adhesive composition it can be produced an adhesive member for a solar cell module with improved mechanical properties and adhesion such as durability.
  • the agent A further includes at least one selected from an adhesion improving agent and a catalyst.
  • the agent B further includes one or more selected from antioxidants and reaction inhibitors.
  • the polysilsesquioxane compound A is a polysilsesquioxane compound having a C2-C10 alkenyl group, a C1-C10 alkyl group, and a hydroxyl group at the terminal and side chain (hereinafter, “the first sesquioxane compound ”) Is obtained by removing a hydroxyl group from the first polysilsesquioxane compound by reacting with a silicon compound represented by the following formula (4), a silicon compound represented by the following formula (5), and a silazane compound: .
  • R 3 is a C1-C10 alkyl group
  • Y 4 is a C1-C10 alkoxy group or a halogen element
  • n is an integer of 1 to 3
  • R ⁇ 4> is a C1-C10 alkyl group and Y ⁇ 5> is a C1-C10 alkoxy group or a halogen element.
  • the first polysilsesquioxane compound may be prepared by subjecting a silicon compound represented by the following Chemical Formula 1, a silicon compound represented by the following Chemical Formula 2, and a silicon compound represented by the following Chemical Formula 3 to a hydrolysis polycondensation reaction. have.
  • R 1 is a C2-C10 alkenyl group
  • Y 1 is a C1-C10 alkoxy group or a halogen element
  • n 1 to 3
  • R 2 is a C1-C10 alkyl group
  • Y 2 is a C1-C10 alkoxy group or a halogen element
  • n 1 to 3
  • Y 3 in Formula 3 is a C1-C10 alkoxy group or a halogen element.
  • polysilsesquioxane B is a polysilsesquioxane compound having a hydrogen, a C1-C10 alkyl group and a hydroxyl group at the terminal and side chain (hereinafter referred to as "second polysilsesquioxane compound")
  • second polysilsesquioxane compound a polysilsesquioxane compound having a hydrogen, a C1-C10 alkyl group and a hydroxyl group at the terminal and side chain
  • R 3 is a C1-C10 alkyl group
  • Y 4 is a C1-C10 alkoxy group or a halogen element
  • R ⁇ 4> is a C1-C10 alkyl group and Y ⁇ 5> is a C1-C10 alkoxy group or a halogen element.
  • the second polysilsesquioxane-based compound may be obtained by carrying out a reaction for hydrolytic condensation polymerization of a silicone compound represented by the following formula (2), a silicone compound represented by the following formula (3) and a silicone compound represented by the following formula (6): have.
  • R 2 in Formula 2 is a C2-C10 alkenyl group
  • Y 2 is a C1-C10 alkoxy group or a halogen element
  • n 1 to 3
  • Y 3 in Formula 3 is a C1-C10 alkoxy group or a halogen element
  • Y 6 in Formula 6 is a C1-C10 alkoxy group or a halogen element
  • n 1 to 3.
  • Silazane compounds used in the preparation of the first polysilsesquioxane compound include hexadimethylsilazane, hexadiethylsilazane, and hexadiphenylsilazane.
  • the number average molecular weight of the first polysilsesquioxane compound and the second polysilsesquioxane compound is 10,000 to 30,000.
  • the polysilsesquioxane compound A and the polysilsesquioxane compound B are hydroxy groups of the first polysilsesquioxane compound and the second polysilsesquioxane compound, a silicone compound and a silazane compound. It is a polymer modified and hydrophobized by using one selected from among the viscosity is 50,000 to 100,000 mPas, the number average molecular weight is 10,000 to 30,000.
  • the viscosity is evaluated according to the method of expressing the average value for the measured viscosity at 10 ⁇ 100RPM by rotating viscometer (Brook-Filed) at 25 °C, RH50% conditions.
  • the viscosity of the polysilsesquioxane-based compound A and the polysilsesquioxane-based compound B is in the above range, the flowability of the adhesive composition is appropriate, so that an operation of manufacturing the adhesive member can be easily performed.
  • the C2-C10 alkenyl group includes a vinyl group or an allyl group
  • the C1-C10 alkyl group includes a methyl, ethyl, n-propyl, n-pentyl, isopentyl or butyl group.
  • the C1-C10 alkoxy group includes a methoxy group, ethoxy group, propoxy group or pentyloxy, and the halogen element includes fluorine, chlorine, or iodine.
  • the first polysilsesquioxane-based compound includes a unit represented by the following formula (7) or represented by the following formula (7).
  • R 1 is a C2-C10 alkenyl group
  • R 2 is a C1-C10 alkyl group.
  • R 1 is a vinyl group
  • R 2 is a methyl group
  • the polysilsesquioxane compound A is represented by the following formula (8) or includes a unit represented by the following formula (8).
  • R 1 is a C2-C10 alkenyl group
  • R 2 is a C1-C10 alkyl group
  • R 3 is a C1-C10 alkyl group.
  • R 1 is a vinyl group
  • R 2 is a methyl group
  • R 3 is a methyl group.
  • the second polysilsesquioxane compound includes a unit represented by the following formula (9) or represented by the following formula (9).
  • R 2 in Formula 9 is a C1-C10 alkyl group.
  • the polysilsesquioxane B is represented by the following formula (10) or includes a unit represented by the formula (10).
  • R ⁇ 2> is a C1-C10 alkyl group and R ⁇ 3> is a C1-C10 alkyl group.
  • the polysilsesquioxane compound A includes a compound represented by the following formula (11) or (12).
  • x, y, z ' is independently a number greater than 0, for example, the number of 1 to 200,
  • x, y, z, w is independently a number greater than 0, for example 1 to 200.
  • the polymerization degree x, y, z of Formula 11 and the polymerization degree x, y, z, w of Formula 12 are selected such that the number average molecular weight of the compound represented by Formula 11 or Formula 12 is in the range of 10,000 to 30,000.
  • the polysilsesquioxane B includes a compound represented by the following Formula 13 or Formula 14.
  • x, y, z ' is independently a number greater than 0, for example, a number of 1 to 200,
  • x, y, z and w are each independently a number greater than 0, for example, 1 to 200.
  • X, y, z of Formula 13 and x, y, z, w of Formula 14 are selected such that the number average molecular weight of the compound represented by Formula 13 or Formula 14 is in the range of 10,000 to 30,000.
  • the polysilsesquioxane B made of B is used in an amount of 5 to 45 parts by weight based on 100 parts by weight of the polysilsesquioxane compound A made of the A.
  • the content of the polysilsesquioxane B is within the above range, it is possible to manufacture an adhesive member for a solar cell module having excellent durability.
  • the agent B further includes a polysilsesquioxane compound A.
  • a polysilsesquioxane compound A As such, when the polysilsesquioxane-based compound A is further added to the agent B, the viscosity of the agent A and the agent B is controlled to almost the same range, so that the agent A and the agent B are mixed evenly when sprayed from the nozzle of the filling cartridge, thereby making a perfect cured product. There is an advantage that can form.
  • the content of the polysilsesquioxane compound A of agent B is 30 to 80 parts by weight based on 100 parts by weight of the polysilsesquioxane compound A of agent A.
  • the agent A may include an adhesion improving agent and a catalyst.
  • the adhesion improving agent is a 3-aminopropyl triethoxysilane, 3-glycidoxypropyl trimethoxysilane, 3-methoglyoxypropyl trimethoxysilane as components added to improve the adhesion of the adhesive member formed from the adhesive composition. , N- ( ⁇ -aminoethyl) - ⁇ -aminopropyl trimethoxysilane, ⁇ -glycidoxypropyl triethoxy silane and ⁇ -glycidoxy trimethyldimethoxysilane.
  • the adhesion improving agent is 1 to 15 parts by weight based on 100 parts by weight of the polysilsesquioxane compound A in Agent A.
  • the content of the adhesion improving agent is in the above range, the adhesion of the adhesive member formed from the composition to the substrate is excellent.
  • the catalyst serves to promote the reaction between the polysilsesquioxane compound A and the polysilsesquioxane compound B.
  • the catalyst may also serve as a flame retardant.
  • a Speyer catalyst hereinafter, H 2 PtCl 6
  • the catalyst is used in 0.0001 to 0.5 moles based on 1 mole of the polysilsesquioxane compound A.
  • the content of the catalyst is in the above range, the reaction rate of the curing reaction of the polysilsesquioxane compound A and the polysilsesquioxane compound B is increased, thereby reducing the reaction time.
  • the B agent may include an antioxidant and a reaction inhibitor.
  • the antioxidant prevents the adhesive composition and the adhesive member formed from the adhesive composition from being oxidized by ultraviolet rays and heat, and prevents oxygen from being promoted by binding oxygen in the air to the ends of the broken molecules.
  • Such antioxidants include phenolic compounds, monophenolic compounds or bisphenolic compounds, and include, but are not limited to, isotridecyl-3- (3,5-di-t-butyl-4-hydroxyphenyl) propio Nate, benzene propanoic acid 3, 3-bis (1, 1- dimethylethyl) -4-hydroxy, C7-9- isoalkyl ester, etc. are mentioned.
  • the antioxidant is used in 0.0001 to 0.5 moles based on 1 mole of polysilsesquioxane compound B. When the content of the antioxidant is in the above range, yellowing of the solar cell adhesive member formed using the adhesive composition does not occur.
  • the reaction inhibitor inhibits the reaction of the components constituting the agent B before the agent A and the agent B are mixed.
  • the reaction refers to, for example, a hydrosilylation reaction.
  • the reaction inhibitor includes 1-ethynylcyclohexanol or 2-methyl-3-butyn-2-ol.
  • the reaction inhibitor is used in an amount of 0.0001 to 0.5 moles based on 1 mole of the polysilsesquioxane compound B.
  • a silane mixture is obtained by mixing the silicon compound represented by Chemical Formula 1, the silicon compound represented by Chemical Formula 2, and the silicon compound represented by Chemical Formula 3. The mixing is performed by stirring at room temperature for 0.5 to 1 hour.
  • the rotational speed per minute during the stirring is 300 to 500 rpm.
  • room temperature means 20 to 25 °C.
  • the silicone compound represented by Formula 2 is used in an amount of 10 to 100 parts by weight based on 100 parts by weight of the silicon compound represented by Formula 1, and the silicon compound represented by Formula 3 is 100 weight of the silicon compound represented by Formula 1 It is used in 10 to 120 parts by weight based on parts.
  • Acid and solvent are added and mixed to the silane mixture.
  • the acid includes sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid or acetic acid, and the acid is used in an amount of 0.01 to 2 moles based on 1 mole of the silicon compound represented by Formula 1.
  • the solvent includes water or an alcohol, and the amount of the solvent is 50 to 2000 parts by weight based on 100 parts by weight of the silicone compound represented by Formula 1.
  • the silicon compound represented by Formula 2 includes methyltrimethoxysilane (CH 3 Si (OCH 3 ) 3 ), or methyltriethoxysilane (CH 3 Si (OCH 2 CH 3 ) 3 ).
  • the silicon compound represented by Chemical Formula 3 includes tetraethylorthosilicate (Si (OCH 2 CH 3 ) 4 ), or tetramethylorthosilicate (Si (OCH 3 ) 4 ).
  • reaction mixture obtained according to the above process is heat-treated to perform hydrolysis and polycondensation reaction of the silicon compound.
  • the heat treatment temperature is 80 to 100 °C.
  • the heat treatment temperature is within the above range, the reactivity of the hydrolysis polycondensation reaction of the silicone compound is excellent.
  • the reaction mixture is cooled to 50 ° C. or lower, for example, 10 to 45 ° C., and a polysilsesquioxane compound having a C 2 -C 10 alkenyl group, C 1 -C 10 alkyl group and a hydroxyl group at the terminal and side chain ( 1 polysilsesquioxane compound) is prepared.
  • the first polysilsesquioxane compound and a solvent are mixed to obtain a mixture.
  • the solvent is tetrahydrofuran, pyridine, propylene glycol monomethylether acetate, or propylene glycol methyl ether, and the solvent is used at 30 to 2000 parts by weight based on 100 parts by weight of the first polysilsesquioxane compound.
  • the mixing may be performed by stirring at room temperature for 1 to 5 hours.
  • One selected from the silicone compound represented by Formula 4, the silicone compound represented by Formula 5, and silazane is used in an amount of 5 to 100 parts by weight based on 100 parts by weight of the first polysilsesquioxane compound.
  • the content of one selected from the silicon compound represented by Formula 4, the silicon compound represented by Formula 5, and silazane is within the above range, a polysilsesquioxane compound having controlled hydrophobicity may be obtained.
  • reaction mixture is heat-treated to perform a silanol capping reaction of the first polysilsesquioxane compound.
  • the heat treatment temperature is 80 to 100 °C.
  • the silanol capping reactivity of the first polysilsesquioxane compound is excellent.
  • the silicone compound represented by Chemical Formula 4 includes methyltrichlorosilane, dimethyldichlorosilane or trimethylchlorosilane.
  • the silicon compound represented by Chemical Formula 5 includes (CH 3 SiCl 2 ) 2 O.
  • the resultant of the silanol capping reaction is evaporated under reduced pressure to remove low boiling water, and then cooled to 50 ° C. or lower, for example, 10 to 45 ° C., to obtain polysilsesquioxane compound A.
  • polysilsesquioxane compound B is prepared according to the following procedure.
  • the silicon compound represented by Chemical Formula 2 the silicon compound represented by Chemical Formula 3, and the silicon compound represented by Chemical Formula 6 are stirred at room temperature for 0.5 to 1 hour to perform a mixing process.
  • the rotational speed per minute during the stirring is 300 to 500 rpm.
  • the type of the solvent is as described in the preparation of the first polysilsesquioxane compound.
  • the acid is used in an amount of 0.01 to 2 moles based on 1 mole of the silicon compound represented by Formula 2.
  • the solvent is used in an amount of 500 to 2000 parts by weight based on 100 parts by weight of the silicone compound represented by Formula 2.
  • the silicon compound represented by Chemical Formula 6 includes H-SiCH 3 (OCH 3 ) 2 or H-Si (OCH 3 ) 3 .
  • the silicone compound represented by Formula 3 is used in 10 to 150 parts by weight based on 100 parts by weight of the silicone compound represented by Formula 2, and the silicon compound represented by Formula 6 is 100 weight of the silicon compound represented by Formula 2 It is used in 10 to 150 parts by weight based on parts.
  • the heat treatment temperature is as described in the preparation of the first polysilsesquioxane compound.
  • the second polysilsesquioxane-based compound is dissolved in a solvent, and one or more selected from the silicon compound represented by the formula (4), the siloxane compound represented by the formula (5), and the silazane are added thereto, mixed, and heat-treated to obtain a second compound.
  • the silanol capping reaction which removes a hydroxyl group from a polysilsesquioxane type compound is performed.
  • the heat treatment temperature is the same as the manufacturing process of the polysilsesquioxane A.
  • the amount of one selected from the silicone compound represented by Formula 4, the siloxane compound represented by Formula 5, and silazane is 5 to 100 parts by weight based on 100 parts by weight of the second polysilsesquioxane compound.
  • the type of the solvent is the same as the preparation of the polysilsesquioxane compound A.
  • the content of the solvent is 30 to 2000 parts by weight based on 100 parts by weight of the second polysilsesquioxane compound.
  • the reaction product of the silanol capping reaction is evaporated under reduced pressure to remove low boiling water, and then cooled to 50 ° C. or lower, for example, 10 to 45 ° C. to obtain silsesquioxane compound B.
  • the mixing is according to the stirring process for 300 to 500 rpm, 0.5 to 3 hours at room temperature.
  • the mixing is carried out at the same temperature, stirring time and rotational speed conditions as in the case of preparation of agent A.
  • the polysilsesquioxane compound A can be further added to the agent B.
  • agent A and agent B are mixed to obtain an adhesive composition for a two-component solar cell module.
  • the weight ratio of the agent A and agent B is 1: 1 to 20: 1.
  • the weight of agent B to agent A is in the above range, the unreacted cured product of agent A and agent B is not formed and the hardness of the cured product is excellent.
  • Adhesive composition for a solar cell module is a weight ratio of agent A and agent B is 1: 1.
  • the viscosity of the agent A and the agent B is different, so that the mixing is easy, so that a complicated weighing process can be omitted during the operation and the curing time is short.
  • the adhesive composition for a solar cell module obtained according to the above production method has a viscosity of about 80,000 to 120,000 cPs (80,000 to 120,000 mPa.s).
  • the viscosity of the adhesive composition is lower than the above range, the discharge pressure is too low to contaminate the adhesive due to the adhesive outside the working area. If the viscosity is higher than the above range, the discharge pressure of the composition may be high, the adhesive force may be lowered, and the worker's fatigue may be increased. Workability may be degraded.
  • the adhesive composition can be packaged using a two-component cartridge.
  • the composition is an additional curing type adhesive composition, unlike conventional adhesive compositions, does not generate by-products such as water and hydrogen when cured, has high reliability and durability for mechanical properties, and does not have thickening and partial curing during storage, thereby improving storage stability at room temperature. Can be stored. In addition, since it does not contain a filler such as calcium carbonate, the fatigue of the worker is reduced and workability is improved by lightening.
  • an adhesive member including a cured product of the adhesive composition for a solar cell module and a solar cell module having the same.
  • the curing reaction of the composition includes a hydrogenation reaction in which hydrogen contained in the polysilsesquioxane compound B agent B is added to a double bond of the alkenyl group of the polysilsesquioxane compound A agent A.
  • the product obtained by the curing reaction of the composition is a hydrophobic polysilsesquioxane-based compound having random and ladder types, unlike when using an adhesive composition containing a conventional silsesquioxane oligomer.
  • the adhesive member includes a hydrophobic polysilsesquioxane-based compound, and the use of the adhesive member can prevent the frame corrosion in advance and prevent the solar cell from malfunctioning or reducing the life cycle of the solar cell due to the contamination. have.
  • Methyltrimethoxysilane (hereinafter referred to as MTMS) in an approximately 1 liter round bottom flask equipped with a condenser, stirrer, temperature control system (including circulator, heating mantle and thermocouple) ) 124 parts by weight, 162 parts by weight of vinyltrimethoxysilane (hereinafter referred to as VTMS), and 169 parts by weight of tetraethylorthosilicate (hereinafter referred to as TEOS) were added and stirred at room temperature at about 400 RPM for 30 minutes.
  • VTMS vinyltrimethoxysilane
  • TEOS tetraethylorthosilicate
  • the stirred solution was refluxed at about 90 ° C. for 3 hours and then distilled under reduced pressure to remove low boiling water.
  • the resultant from which the low-boiling water was removed was cooled to about 45 ° C. to prepare a first polysilsesquioxane compound represented by a colorless transparent formula (7) having a number average molecular weight (Mn) of about 20,000 including methyl and vinyl groups.
  • R 1 is a vinyl group
  • R 2 is a methyl group
  • THF tetrahydrofuran
  • MTCS methyltrichlorosilane
  • the reaction mixture was stirred for about 3 hours and then distilled under reduced pressure at 100 ° C. to remove low boiling water.
  • the reaction product from which low boiling water was removed was cooled to about 45 ° C., and the viscosity was about 80,000 mPa .
  • Polysilsesquioxane compound A represented by Chemical Formula 8 of s was prepared.
  • R ⁇ 1> is a vinyl group
  • R ⁇ 2> is a methyl group
  • R ⁇ 3> is a methyl group
  • Mn number average molecular weight
  • R 2 is a methyl group.
  • R 2 is a methyl group
  • R 3 is a methyl group
  • Vi PSQ a polysilsesquioxane compound represented by Formula 8 (hereinafter referred to as Vi PSQ) prepared according to Synthesis Example 2 in a vessel No. 1, 3-glycidoxypropyl trimethoxysilane (hereinafter referred to as GPTMS) 10 parts by weight, 1 part by weight of a Speyer catalyst (Speier catalyst) (H 2 PtCl 6 ) in order, and then stirred at about 400 rpm at room temperature for 30 minutes to prepare a agent A.
  • GPTMS 3-glycidoxypropyl trimethoxysilane
  • H PSQ polysilsesquioxane compound represented by Chemical Formula 10
  • isotridecyl-3- (3,5 10 parts by weight of di- t -butyl-4-hydroxyphenyl) propionate and 1 part by weight of 2-ethynylcyclohexanol (1-ETCH) were added in this order, followed by stirring at room temperature at about 400 rpm for 30 minutes.
  • H PSQ polysilsesquioxane compound represented by Chemical Formula 10
  • Agent A and agent B were mixed in a 1: 1 weight ratio to prepare an adhesive composition for a two-component solar cell module.
  • Example 1 As shown in Table 1, except that the content of the constituent components of the adhesive composition was changed, it was carried out in the same manner as in Example 1 to obtain an adhesive composition for a solar cell module.
  • Vi PSQ The content of the stage in the embodiment 2-4-vinyl content of the polysilsesquioxane (hereinafter referred to as Vi PSQ) in the A and B is 100 parts by weight of the vinyl polysilsesquioxane (hereinafter referred to as Vi PSQ) is carried out in 60 parts by weight of Example 2, 50 parts by weight of Example 3, and 40 parts by weight of Example 4.
  • Silsesquioxane oligomer (OSQ), ⁇ , ⁇ -vinyl terminated polydimethylsiloxane ( Vi PDMS), ⁇ , ⁇ -hydrogen terminated polydimethylsiloxane ( H PDMS), SiO 2 , CaCO 3 , triethylphosphate (TEP) , GPTMS and isotridecyl-3- (3,5-di-t-butyl-4-hydroxyphenyl) propionate and DBTDL were mixed in the composition of Table 1 to prepare a one-part adhesive composition.
  • OSQ Silsesquioxane oligomer
  • Vi PDMS Vi PDMS
  • H PDMS ⁇ -hydrogen terminated polydimethylsiloxane
  • SiO 2 SiO 2
  • CaCO 3 triethylphosphate
  • TEP triethylphosphate
  • GPTMS and isotridecyl-3- (3,5-di-t-butyl-4-hydroxy
  • Specimens were prepared according to the following method and the physical properties of each specimen were evaluated as follows.
  • each of the adhesive composition of Example 1-4 and the adhesive composition of Comparative Example 1-2 was each 2 ⁇ m in one portion (20 ⁇ 10 mm) of an aluminum (Al) specimen (size: 20 ⁇ 50 ⁇ 2 mm). After the coating with a thickness of another aluminum (Al) by attaching a specimen attached to stand at 100 °C, 1 hour to prepare an adhesive specimen (B).
  • Adhesion was measured according to the test method KSF1107A with UTM at 25 ° C. and RH 50% under the conditions of the adhesive specimen (B).
  • the specimen (C) was measured at 25 °C, RH 50% condition by contacting the surface with a finger and the time the adhesive does not appear.
  • the specimen D was measured at 25 ° C. and RH 50% at a Brook-Filed viscometer (10 rpm, Sp # 4 condition) to measure the intrinsic viscosity, and measured the change with time over time of the viscosity to double the initial viscosity. This time was determined as port life.
  • Specimen (A) was prepared to measure hardness, tensile strength, elongation, modulus, and the like, and specimen (A) was cut to 10 ⁇ 10 mm size, 5EA was made, and tweezers were placed in a chamber of an electronic hydrometer to measure specific gravity. Each 5EA was measured in turn and the average value was determined as the specific gravity.
  • Table 2 The physical property evaluation results are shown in Table 2 below.
  • the specimen using the adhesive composition of Example 1-4 is not only improved hardness, tensile strength, elongation, modulus characteristics, Scotch time compared to the specimen using the adhesive composition of Comparative Example 1-2 It was found that the pot life and adhesion properties were improved.
  • the test piece produced using the adhesive composition of Comparative Example 1-2 showed an increasing characteristic compared with the case of Example 1-4.
  • the viscosity is increased, the discharge pressure and specific gravity are increased when using the cartridge containing the adhesive composition, and as a result, the product becomes heavy and the worker's fatigue is increased and the working speed is slowed. Therefore, when using the adhesive composition of Example 1-4 it can be seen that the workability is improved by reducing the worker fatigue compared to the case of Comparative Example 1-2.
  • the adhesive composition for a solar cell module according to an embodiment of the present invention is excellent in storage stability, and by using this, an adhesive member for a solar cell module having improved adhesion and mechanical properties may be manufactured.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Silicon Polymers (AREA)

Abstract

La présente invention concerne une composition adhésive pour module de cellule solaire, un élément adhésif pour module de cellule solaire formé à partir de celle-ci et un module de cellule solaire le comprenant. La composition adhésive pour module de cellule solaire comprend : un agent A qui contient un composé à base de polysilsesquioxane ayant des groupes alcényle en C2 à C10 et des groupes alkyle en C1 à C10 à une extrémité et une chaîne latérale de ceux-ci ; et un agent B qui contient un composé à base de polysilsesquioxane ayant des hydrogènes et des groupes alkyle en C1 à C10 à une extrémité et une chaîne latérale de ceux-ci. La composition adhésive est très stable pendant son stockage et permet de produire un élément adhésif pour module de cellule solaire ayant une meilleure adhérence et de meilleures propriétés mécaniques.
PCT/KR2013/006465 2012-12-07 2013-07-19 Composition adhésive pour module de cellule solaire, élément adhésif pour module de cellule solaire formé à partir de celle-ci et module de cellule solaire le comprenant Ceased WO2014088180A1 (fr)

Applications Claiming Priority (2)

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KR1020120142314A KR20140075865A (ko) 2012-12-07 2012-12-07 태양전지 모듈용 접착 조성물, 이로부터 형성된 태양전지 모듈용 접착부재 및 이를 구비한 태양전지 모듈
KR10-2012-0142314 2012-12-07

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