Insulating film for optoelectronic devices and manufacturing method therefor

Abstract

One aspect of the present invention relates to an insulating film for optoelectronic devices, the insulating film being manufactured from a curable composition comprising: a first polysiloxane comprising ArSiO3 / 2 units in an amount of 90 mol% or more; a second polysiloxane comprising R1SiO3 / 2 units in an amount of 70 to 30 mol% and SiO4 / 2 units in an amount of 30 to 70 mol%; and a crosslinking agent comprising an aminosilane, wherein the insulating film does not develop cracks even under high-temperature curing conditions and can exhibit excellent durability after curing.

Description

Insulating film for photovoltaic devices and method for manufacturing the same

[0001] The present disclosure relates to an insulating film for a photovoltaic device and a method for manufacturing the same.

[0002] Recently, as semiconductor circuits have become more miniaturized and highly integrated, the performance required for insulating films is also becoming more advanced. In particular, optoelectronic devices such as image sensors, photodiodes, OLEDs, and solar cells require insulating film materials with superior durability due to reasons such as combined stress from heat and light.

[0003] However, existing organic insulating films have limitations in ensuring reliability due to problems such as thermal deformation, cracking, degradation of electrical properties, and chemical damage during high-temperature heat treatment. Additionally, there have been frequent issues with film damage due to insufficient chemical resistance when exposed to etchants or stripper solutions used in semiconductor manufacturing processes. Due to these limitations, there is a growing need to develop new insulating film materials that can secure high surface hardness, crack resistance, and crack limit thickness even after high-temperature curing, while simultaneously maintaining excellent chemical resistance to etchants and stripper solutions.

[0004] One aspect of the present invention provides an insulating film with excellent durability and a method for manufacturing the same.

[0005] One aspect of the present invention is ArSiO 3 / 2 A first polysiloxane containing 90 mol% or more of the unit; R 1 SiO 3 / 2 Units 70 to 30 mol% and SiO 4 / 2 An insulating film for a photovoltaic device is provided, prepared from a curable composition comprising: a second polysiloxane comprising 30 to 70 mol% of a unit; and a crosslinking agent comprising an aminosilane (wherein Ar is a C6-C20 aryl, and R 1 is a C1-C7 alkyl.

[0006] The first polysiloxane and the second polysiloxane may be included in a weight ratio of 50:50 to 99:1.

[0007] The weight-average molecular weight of the first polysiloxane may be 500 to 100,000 g / mol.

[0008] The above first polysiloxane is the above ArSiO 3 / 2 It may be composed of units.

[0009] According to one embodiment, the insulating film for the photovoltaic device may have a crack limit thickness of 5 μm or more according to the following evaluation method.

[0010] [Crack limit thickness]

[0011] After applying the above-mentioned curable composition onto a substrate, the solvent is removed by heating at a temperature of 100°C for 2 minutes and curing at a temperature of 400°C for 30 minutes to form an insulating film while increasing the thickness from 1 μm to 10 μm in increments of 0.1 μm, and the thickness at the point where a crack occurs is called the crack limit thickness.

[0012] According to one embodiment, the insulating film for the photovoltaic device may not crack when immersed in a stripper solution at 60°C for 5 minutes and then subjected to heat treatment three times at 400°C for 30 minutes.

[0013] According to one embodiment, the insulating film for the photovoltaic device may not crack when immersed in an etchant at 60°C for 5 minutes and then subjected to heat treatment three times at 400°C for 30 minutes.

[0014] According to one embodiment, the insulating film for the photovoltaic device may have a surface hardness of 3H or higher according to ASTM-D3363.

[0015] Another aspect of the present invention provides a photoelectric device comprising an insulating film for the photoelectric device.

[0016] Another aspect of the present invention is ArSiO 3 / 2 A first polysiloxane containing 90 mol% or more of the unit; R 1 SiO 3 / 2Units 70 to 30 mol% and SiO 4 / 2 A curable composition is provided comprising a second polysiloxane containing 30 to 70 mol% of a unit; and a crosslinking agent containing an aminosilane.

[0017] According to one embodiment, the above-described curable composition may further include a curing agent.

[0018] According to one embodiment, the curable composition may further comprise a silicone-based surfactant.

[0019] An insulating film according to one embodiment of the present invention can achieve excellent durability through high-temperature curing, for example, curing at approximately 400°C. An insulating film cured in this way can secure excellent heat resistance as no cracks occur even under high-temperature conditions, and maintains stable durability even under repeated exposure to high temperatures. In addition, the insulating film is resistant to damage caused by chemicals such as etchants or stripper solutions, and thus has excellent chemical resistance. Therefore, the insulating film of the present invention can be very usefully applied as an insulating film material for various electronic devices, particularly optoelectronic devices, that require properties to withstand chemical stress while being repeatedly exposed to high-temperature environments.

[0020] Unless otherwise defined in this specification, all technical and scientific terms have the same meaning as generally understood by those skilled in the art to which the present invention pertains. The terms used in the description herein are merely for the purpose of effectively describing specific embodiments and are not intended to limit the present invention.

[0021] The singular form used in this specification is intended to include the plural form unless specifically indicated otherwise in the context.

[0022] Throughout this specification, the terms “comprising,” “having,” “containing,” or “having” any component mean that, unless specifically stated otherwise, other components are not excluded but may be included, and do not exclude elements, materials, or processes not additionally listed.

[0023] The numerical ranges used herein include lower and upper limits and all values ​​within the range, increments logically derived from the form and width of the defined range, all of which are limited, and all possible combinations of upper and lower limits of the numerical range defined in different forms. Unless otherwise specifically defined in this specification, values ​​outside the numerical range that may occur due to experimental error or rounding are also included in the defined numerical range.

[0024] Unless otherwise specifically defined in this specification, “about” may be considered to be a value within 30%, 25%, 20%, 15%, 10%, or 5% of the specified value.

[0025] RSiO in this specification 3 / 2 It refers to a T unit (ternary unit) in which one organic group (R) is bonded to silicon and the remaining three bonds are connected to other silicon through oxygen, R2SiO 2 / 2 It refers to a D unit (secondary unit) in which two organic groups (R) are bonded to silicon and two oxygen atoms are bonded to other silicon atoms, R3SiO 1 / 2 It means a monomeric unit in which three organic groups (R) are bonded to silicon and one oxygen is bonded to another silicon.

[0026] The present disclosure will be described in detail below. However, this is merely illustrative and the present disclosure is not limited to the specific embodiments described illustratively.

[0027] One embodiment of the present invention provides a heat-resistant insulating film for a photovoltaic device that does not crack even under high-temperature curing conditions and can achieve excellent durability after curing.

[0028] Specifically, an insulating film for a photovoltaic device according to one embodiment is ArSiO 3 / 2 A first polysiloxane containing 90 mol% or more of the unit; R 1 SiO 3 / 2 Units 70 to 30 mol% and SiO 4 / 2 It may be prepared from a curable composition comprising: a second polysiloxane containing 30 to 70 mol% of a unit; and a crosslinking agent comprising an aminosilane (wherein Ar is a C6-C20 aryl, and R 1 is a C1-C7 alkyl.

[0029] The first polysiloxane and the second polysiloxane may be included in a weight ratio of 50:50 to 99:1, specifically in a weight ratio of 60:40 to 99:1, or 70:30 to 99:1, or 80:20 to 95:5, and may provide an insulating film with even better crack resistance and chemical resistance.

[0030] The weight-average molecular weight of the first polysiloxane may be 500 g / mol to 100,000 g / mol, or 500 g / mol to 10,000 g / mol, or 1,000 g / mol to 5,000 g / mol, or 1,000 g / mol to 3,000 g / mol.

[0031] The above first polysiloxane is ArSiO 3 / 2 The unit may contain 90 mol% or more, or 95 mol% or more, or 97 mol% or more, or 98 mol% or more, or 99 mol% or more, and specifically, ArSiO 3 / 2 Composed of ArSiO units 3 / 2 It may contain 100% of the unit.

[0032] The above first polysiloxane is ArSiO 3 / 2In cases where additional units are included in addition to the unit, the first polysiloxane is SiO 4 / 2 , Ar2SiO 2 / 2 and Ar3SiO 1 / 2 It may further include one or more siloxane units selected from, and the first polysiloxane may be an aryl polysiloxane comprising only aryl substituents.

[0033] The above Ar may each independently be a C6-C20 aryl, and specifically, the above Ar may be the same and be a C6-C20 aryl or a C6-C12 aryl.

[0034] The above-mentioned first polysiloxane may be prepared by the hydrolysis and condensation reaction of a silane compound represented by the following chemical formula 11.

[0035] [Chemical Formula 11]

[0036] ArSi(OR a )3

[0037] (In the above chemical formula 11,

[0038] Ar is a C6-C20 aryl;

[0039] R a Each is independently a C1-C7 alkyl.

[0040] For example, the above Ar may be a C6-C12 aryl or phenyl.

[0041] For example, the above R a They are identical to each other and may be C1-C7 alkyl, C1-C4 alkyl, or C1-C3 alkyl.

[0042] For example, the silane compound represented by the above chemical formula 11 may be represented by the following chemical formula 12.

[0043] [Chemical Formula 12]

[0044]

[0045] The above second polysiloxane is the above R 1 SiO 3 / 2 Units and SiO 4 / 2It may contain units in a weight ratio of 30:70 to 70:30 or 40:60 to 60:40, and may be an alkyl polysiloxane having only alkyl groups.

[0046] The above second polysiloxane may be prepared by the hydrolysis and condensation reaction of a silane compound represented by the following chemical formulas 13 and 14.

[0047] [Chemical Formula 13]

[0048] R 1 Si(OR b )3

[0049] [Chemical Formula 14]

[0050] Si(OR c )4

[0051] (R in the above chemical formulas 13 and 14 1 , R b and R c Each is independently a C1-C7 alkyl.

[0052] For example, the above R 1 , R b and R c Each can independently be a C1-C4 alkyl or a C1-C3 alkyl.

[0053] The above hydrolysis and condensation reactions may be carried out in the presence of an acid catalyst or a base catalyst. The acid catalyst may be an inorganic acid selected from nitric acid (HNO3), hydrochloric acid (HCl), sulfuric acid (H2SO4), phosphoric acid (H3PO4), perchloric acid (HClO4), hydrobromide (HBr), etc.; or an organic acid selected from formic acid (HCOOH), acetic acid (CH3COOH), trifluoroacetic acid (CF3CO2H), etc., but is not limited thereto. The base catalyst may be selected from ammonia, triethylamine, monoethanolamine, diethanolamine, triethanolamine, sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide, etc., but is not limited thereto.

[0054] Preferably, the acid catalyst may be an inorganic acid selected from nitric acid (HNO3), hydrochloric acid (HCl), sulfuric acid (H2SO4), phosphoric acid (H3PO4), perchloric acid (HClO4), hydrobromide (HBr), etc., and the polysiloxane produced therefrom may have even better durability after curing.

[0055] The above acid catalyst may be used in an amount of 0.1 to 1 part by weight or 0.1 to 0.5 parts by weight per 100 parts by weight of the silane compound.

[0056] For example, the above reaction may be carried out in an organic solvent, and non-limiting examples of said organic solvents include glycol ether acetate-based solvents such as propylene glycol monomethyl ether acetate (PGMEA), propylene glycol monoethyl ether acetate (PGEEA), propylene glycol propyl ether acetate (PGPEA), ethylene glycol monomethyl ether acetate (EGMEA), and ethylene glycol monoethyl ether acetate (EGEEA); glycol ether-based solvents such as propylene glycol methyl ether (PGME), propylene glycol ethyl ether (PGEE), ethylene glycol methyl ether (EGME), and ethylene glycol ethyl ether (EGEE); It may be one or more selected from high-boiling point organic solvents such as γ-butyrolactone (GBL), N-methyl-2-pyrrolidone (NMP), dimethylacetamide (DMAc), and dimethyl sulfoxide (DMSO).

[0057] For example, the above reaction may be carried out for 30 minutes to 300 minutes, 30 minutes to 200 minutes, or 30 minutes to 100 minutes under temperature conditions of 50 to 150 ℃, or 70 to 150 ℃, or 70 to 90 ℃, or 90 to 150 ℃, or 90 to 120 ℃, and may be carried out in multiple stages under two or more of the above conditions, and may be changed depending on the amount of raw material used, etc.

[0058] The above aminosilane may be represented by the following chemical formula 15.

[0059] [Chemical Formula 15]

[0060] A n Si(OR d ) 4-n

[0061] The above A is a C1-C10 alkyl group having an amino group, and R d is independently hydrogen or a C1-C10 alkyl group, and n is an integer from 1 to 3.

[0062] For example, A is a C1-C7 alkyl group having an amino group, and R d is independently hydrogen or a C1-C7 alkyl group, and n is 1 or 2.

[0063] For example, A is a C1-C3 alkyl group having an amino group, and R d is independently hydrogen or a C1-C3 alkyl group, and n is 1 or 2.

[0064] For example, A is a C1-C3 alkyl group having an amino group, and R d is identical and is a C1-C3 alkyl group, and n is 1 or 2.

[0065] For example, the amino silane may be an aminoalkyltrialkoxysilane, specifically an amino(C1-C10)alkyltri(C1-C10)alkoxysilane, an amino(C1-C7)alkyltri(C1-C7)alkoxysilane, or an amino(C1-C3)alkyltri(C1-C3)alkoxysilane, and non-limiting examples may be (3-aminopropyl)triethoxysilane, (3-aminopropyl)trimethoxysilane, or a mixture thereof, but are not limited thereto.

[0066] According to one embodiment, the curable composition may include the polysiloxane and aminosilane in a weight ratio of 1:0.001 to 1:1, or 1:0.001 to 1:0.1, or 1:0.005 to 1:0.1, or 1:0.005 to 1:0.05, and may provide an insulating film with even better crack resistance and chemical resistance.

[0067] According to one embodiment, the insulating film for the optoelectronic device may have a crack limit thickness according to the following evaluation method of 5 μm or more, or 6 μm or more, or 7 μm or more, or 8 μm or more, or 10 μm or less, or 9 μm or less.

[0068] [Crack limit thickness]

[0069] After applying the above-mentioned curable composition onto a substrate, the solvent is removed by heating at a temperature of 100°C for 2 minutes and curing at a temperature of 400°C for 30 minutes to form an insulating film while increasing the thickness from 1 μm to 10 μm in increments of 0.1 μm, and the thickness at the point where a crack occurs is called the crack limit thickness.

[0070] In addition, the insulating film for the photovoltaic device according to one embodiment may have crack resistance such that no cracks occur when it is immersed in a stripper solution at 60°C for 5 minutes and then subjected to heat treatment three times at 400°C for 30 minutes.

[0071] In addition, the insulating film for the photovoltaic device according to one embodiment may have crack resistance such that no cracks occur when it is immersed in an etchant at 60°C for 5 minutes and then subjected to heat treatment three times at 400°C for 30 minutes.

[0072] In addition, the insulating film for the photovoltaic device according to one embodiment may have a surface hardness of 3H or higher, or 4H or higher, or 5H or higher, or 6H or higher according to ASTM-D3363.

[0073] Another aspect of the present invention provides a photoelectric device comprising an insulating film for the photoelectric device.

[0074] The above-mentioned photovoltaic device refers to a device that converts light (optical) energy into an electrical signal or electrical energy, or converts electrical energy into light energy, and may be selected from, for example, image sensors, photodiodes, OLEDs, solar cells, etc., but is not limited thereto.

[0075] Another aspect of the present invention is ArSiO 3 / 2 A first polysiloxane containing 90 mol% or more of the unit; R 1 SiO 3 / 2 Units 70 to 30 mol% and SiO 4 / 2 A curable composition is provided comprising a second polysiloxane containing 30 to 70 mol% of a unit; and a crosslinking agent containing an aminosilane.

[0076] The above-mentioned first polysiloxane, second polysiloxane, and aminosilane are identical to the definitions above, so a detailed description is omitted.

[0077] According to one embodiment, the curable composition may include an organic solvent, and the solid content may be 30 to 80 weight%, or 30 to 70 weight%, or 40 to 60 weight%.

[0078] The above organic solvent is not particularly limited, but may be an organic solvent selected from solvents capable of uniformly dissolving or dispersing each component of the composition. Specific examples include ethylene glycol monoalkyl ethers such as ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether, and ethylene glycol monobutyl ether; diethylene glycol dialkyl ethers such as diethylene glycol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol dipropyl ether, and diethylene glycol dibutyl ether; ethylene glycol alkyl ether acetates such as methyl cellosolve acetate and ethyl cellosolve acetate; and propylene glycol monoalkyl ethers such as propylene glycol monomethyl ether and propylene glycol monoethyl ether. These include propylene glycol alkyl ether acetates such as propylene glycol monomethyl ether acetate, propylene glycol monoethyl ether acetate, and propylene glycol monopropyl ether acetate; aromatic hydrocarbons such as benzene, toluene, and xylene; ketones such as methyl ethyl ketone, acetone, methyl amyl ketone, methyl isobutyl ketone, and cyclohexanone; and alcohols such as isopropanol and propanediol. These solvents may be used alone or in combination of two or more, and their content may vary depending on the coating method and the required thickness of the coating film.

[0079] The above curable composition may contain the polysiloxane in an amount of 50% or more by weight, or 60% or more by weight, or 70% or more by weight, or 80% or more by weight, or 90% or more by weight, or 98% or less by weight, or 96% or less, based on the total weight of the solid content.

[0080] According to one embodiment, the above-described curable composition may further include a curing agent.

[0081] The above curing agent may be any one or more combinations selected from the group consisting of 1,8-diazabicyclo[5.4.0]undecene (DBU), 1,4-diazabicyclo[2.2.2]octane (DABCO), and 1,5-diazabicyclo[4.3.0]nonene (DBN), but is not limited thereto. The above curing agent may be included in an amount of 1 to 30 parts by weight, or 1 to 20 parts by weight, or 1 to 10 parts by weight, per 100 parts by weight of the polysiloxane.

[0082] According to one embodiment, the curable composition may further include a silicone-based surfactant.

[0083] The above silicone-based surfactants are, for example, BYK-077, BYK-085, BYK-300, BYK-301, BYK-302, BYK-306, BYK-307, BYK-310, BYK-320, BYK-322, BYK-323, BYK-325, BYK-330, BYK-331, BYK-333, BYK-335, BYK-345, BYK-346, BYK-348, BYK-354, BYK-355, BYK-356, BYK-358, BYK-361, BYK-370, BYK-371, BYK375, BYK-380 of BYK Chemie. BYK-390, BYK-3550, etc. may be used, and specifically, it may be a polyether-modified polydimethylsiloxane-based surfactant, specifically BYK-333, but is not limited thereto. The silicone-based surfactant may be included in an amount of 0.1 to 10 parts by weight, or 0.1 to 5 parts by weight, or 0.1 to 3 parts by weight per 100 parts by weight of polysiloxane.

[0084] Another aspect of the present invention provides a method for manufacturing an insulating film for a photovoltaic device, comprising the step of heat-curing the curable composition at a temperature of 100°C or higher.

[0085] The above-mentioned heat curing may be at a temperature of 200°C or higher, or 300°C or higher, or 400°C or higher, or 600°C or lower, or 500°C or lower, and specifically may be performed under temperature conditions of 300°C to 500°C, or 350°C to 450°C, and the curable composition according to one embodiment can provide an insulating film with excellent durability without cracking even under the above-mentioned high-temperature curing conditions.

[0086] A method for manufacturing an insulating film for a photovoltaic device according to one embodiment may further include a drying step for removing a solvent before performing the heat curing, and the drying conditions may vary depending on the solvent used, but for example, may be performed at 50 to 200 ℃ or 100 to 150 ℃, but is not limited thereto.

[0087] The above-described embodiment will be explained in more detail below through examples. However, the following examples are for illustrative purposes only and do not limit the scope of the claims.

[0088] [Preparation Example 1] First polysiloxane (1)

[0089] 1,350 g of phenyltrimethoxysilane was added to a 2,000 ml three-necked flask, and 485 g of water and 2.1 g of nitric acid were mixed and quantitatively added over 30 minutes while stirring at room temperature. After the addition was completed, the solution was stirred for 30 minutes, then the internal temperature was raised to 80 ℃ and a condensation reaction was carried out for 60 minutes. Subsequently, the solution was heated and raised for 60 minutes to reach 95 ℃. During this process, 502 g of alcohol and water, which were by-products of the reaction, were released. After reaching 95 ℃, the condensation reaction was carried out for 2 hours and the reaction was terminated. After the final reaction was completed, the solution was diluted with propylene glycol methyl ether acetate (PGMEA) to achieve a solid content concentration of 30 wt%, thereby obtaining a polysiloxane with a weight-average molecular weight of 1,200 g / mol.

[0090] [Preparation Example 2] First polysiloxane (2)

[0091] Polysiloxane with a weight-average molecular weight of 1,160 g / mol was obtained by carrying out the same procedure as in Preparation Example 1 above, except that 1,243 g of phenyltrimethoxysilane and 132 g of diphenyldimethoxysilane were used instead of 1,350 g of phenyltrimethoxysilane.

[0092] [Preparation Example 3] Second polysiloxane

[0093] 551 g of methyltriethoxysilane, 648 g of tetraethoxysilane, and 150 g of PGMEA were added to a 2,000 ml three-necked flask. While stirring at room temperature, 465 g of water and 6.2 g of nitric acid were mixed and added over a period of 30 minutes. After the addition was completed, the temperature of the internal solution was raised to 80°C and a condensation reaction was performed for 60 minutes. Subsequently, the temperature of the solution was raised to 90°C over another 60 minutes. During this process, 345 g of alcohol and water, which were by-products of the reaction, were released. The condensation reaction was then performed for 2 hours at the raised temperature and the reaction was terminated. After the final reaction was completed, the mixture was diluted with PGMEA to achieve a solid content concentration of 30 wt%, thereby obtaining a polysiloxane with a weight-average molecular weight of 1,980 g / mol.

[0094] [Comparative Manufacturing Example 1]

[0095] 1,300 g of propylene glycol methyl ether acetate (PGMEA) was added to a 2,000 mL three-necked flask, and the temperature was raised to 95°C. Then, 235 g of methyl methacrylate, 102 g of 2-hydroxymethyl methacrylate, 161 g of styrene, 95 g of 3-methacryloxypropyltrimethoxysilane, and 11.2 g of t-butylperoxyoctoate (a thermal initiator) were mixed in a dropping funnel. The mixture was then quantitatively added while maintaining the temperature for 3 hours, and the reaction was carried out while maintaining the temperature for 6 hours until the reaction was complete. After the final reaction was terminated, an acrylate resin with a molecular weight of 15,000 g / mol and a solid content concentration of 30% was obtained.

[0096] [Comparative Manufacturing Example 2]

[0097] Polysiloxane with a weight-average molecular weight of 25,000 g / mol was obtained by carrying out the same procedure as in Preparation Example 1 above, except that 215 g of phenyltrimethoxysilane, 391 g of methyltriethoxysilane, and 230 g of tetraethoxysilane were used instead of 1,350 g of phenyltrimethoxysilane.

[0098] [Comparative Manufacturing Example 3]

[0099] Polysiloxane with a weight-average molecular weight of 1,150 g / mol was obtained by carrying out the same procedure as in Preparation Example 1 above, except that 1,183 g of phenyltrimethoxysilane and 111 g of methyltrimethoxysilane were used instead of 1,350 g of phenyltrimethoxysilane.

[0100] [Example 1]

[0101] 8.5 g of the first polysiloxane (1) of Preparation Example 1, 1.1 g of the second polysiloxane of Preparation Example 3, 0.042 g of a silicone-based surfactant (BYK, BYK 333), 0.084 g of 3-aminopropyltriethoxysilane, and 0.5 g of 1,8-diazabicyclo[5.4.0]undecene (DBU) were added to 10.1 g of propylene glycol-1-monomethyl ether-2-acetate and stirred to prepare a curable composition.

[0102] [Example 2]

[0103] The above Example 1 was carried out in the same manner except that the first polysiloxane (2) of Example 2 was used instead of the first polysiloxane (1) of Example 1.

[0104] [Comparative Example 1]

[0105] The above Example 1 was carried out in the same manner, except that 11.3 g of the acrylate resin of Comparative Example 1 was used instead of the first polysiloxane (1) of Preparation Example 1 and the second polysiloxane of Preparation Example 3.

[0106] [Comparative Example 2]

[0107] The above Example 1 was carried out in the same manner, except that 10.3 g of the polysiloxane of Comparative Example 2 was used instead of the first polysiloxane (1) of Preparation Example 1 and the second polysiloxane of Preparation Example 3.

[0108] [Comparative Example 3]

[0109] The above Example 1 was carried out in the same manner except that the polysiloxane of Comparative Example 3 was used instead of the first polysiloxane (1) of Manufacturing Example 1.

[0110] <Evaluation Example>

[0111] 1. Surface Hardness Evaluation

[0112] The curable compositions of the above examples and comparative examples were applied to a substrate that had undergone a predetermined pretreatment using a spin coating method to a thickness of 4 μm, then heated at 100 °C for 2 minutes to remove the solvent, and cured at 400 °C for 30 minutes to form an insulating film. The surface hardness of the insulating film was measured according to the method described in ASTM-D3363. Specifically, a Mitsubishi Pencil was brought into contact with the substrate using a Pencil Hardness Tester, and a 500 g weight was placed on top to increase the load. The surface of the substrate was then scratched at a speed of 50 mm / sec, and the surface was observed to measure the hardness. The measurement standard was evaluated based on the point where no wear, peeling, tearing, or scratching was observed on the surface at a level corresponding to pencil hardness.

[0113] 2. Crack Resistance Evaluation

[0114] The substrate with the insulating film formed in 1. above was immersed in a stripper (LGS-900) at 60°C for 5 minutes, and then subjected to heat treatment three times at 400°C for 30 minutes to check for the occurrence of cracks.

[0115] 3. Evaluation of Crack Limit Thickness

[0116] Insulating films were fabricated by increasing the thickness from 1 μm to 10 μm in increments of 0.1 μm using the same method as described in 1. above, and the film thickness at the point where cracks occur was defined as the crack limit thickness.

[0117] 4. Chemical Resistance Evaluation

[0118] The substrate with the insulating film formed in Section 1 above was immersed in etchant and stripper solutions under the following conditions to check the degree of damage to the insulating film. The immersion conditions were as follows: The substrate was immersed in BOE (buffered oxide etchant) etchant at room temperature for 3 hours to check the thickness and surface using a non-contact ellipsometer and an optical microscope, respectively. Afterward, the substrate was immersed in LGS-900 stripper at 60°C for 10 minutes to check the thickness and surface. The thickness before and after immersion in BOE and LGS-900 were calculated, and the rate of change was calculated. It was evaluated as ○ if surface damage was confirmed and Х if no damage was confirmed. In this case, the chemical resistance is superior as the thickness deviation and surface damage are reduced.

[0119] The results of the above evaluation are shown in Table 1 below.

[0120] Hardness Crack Resistance Crack Limit Thickness Chemical Resistance (Thickness Change / Damage) 1st 2nd 3rd BOELGS-900 Example 16 HXXX 6.4㎛ 99% / X 102% / X Example 25 HXXX 6.1㎛ 99% / X 99% / X Comparative Example 1 ------- Comparative Example 23 H crack crack crack 4.5㎛ 97% / X 114% / O Comparative Example 34 H crack crack crack 4.0㎛ 97% / X 110% / O

[0121] Referring to Table 1 above, it can be seen that the insulating film according to the present invention has excellent durability by possessing excellent surface hardness, crack resistance against thermal shock, crack limit thickness, and chemical resistance through high-temperature curing at 400°C.

[0122] On the other hand, in the case of Comparative Example 1, cracks occurred at a curing temperature of 400 ℃, so the insulating film was not properly formed and physical properties could not be measured. It was confirmed that the insulating films according to Comparative Examples 2 and 3 not only had lower surface hardness compared to the embodiment, but also had lower crack resistance against thermal shock, crack limit thickness, and chemical resistance.

[0123] In other words, the insulating film according to one embodiment can demonstrate excellence as an insulating film material used in environments with high temperature and chemical stress. The ability to minimize crack formation after high-temperature heat treatment ensures that the insulating film can perform its function without physical damage even during long-term use. Furthermore, it is possible to form a thicker film without cracking, thereby increasing the durability and reliability of the product, and its excellent chemical resistance enables stable performance in various chemical environments.

[0124] As described above, the present disclosure has been explained by specific details and limited embodiments, but this is provided only to aid in a more comprehensive understanding of the present disclosure. The present disclosure is not limited to the above embodiments, and various modifications and variations are possible from this description by those skilled in the art to which the present disclosure pertains.

[0125] Accordingly, the present disclosure is not limited to the embodiments described above, and all things equivalent to or having equivalent variations to the claims set forth below, as well as the claims set forth below, shall be considered to be within the scope of the present disclosure.

Claims

1. ArSiO 3 / 2 A first polysiloxane containing 90 mol% or more of the unit; R 1 SiO 3 / 2 Units 70 to 30 mol% and SiO 4 / 2 An insulating film for a photovoltaic device, prepared from a curable composition comprising: a second polysiloxane containing 30 to 70 mol%; and a crosslinking agent comprising an aminosilane. (The above Ar is a C6-C20 aryl, and R 1 is a C1-C7 alkyl.

2. In Paragraph 1, An insulating film for a photovoltaic device, wherein the first polysiloxane and the second polysiloxane are included in a weight ratio of 50:50 to 99:

1.

3. In Paragraph 1, An insulating film for a photovoltaic device, wherein the weight-average molecular weight of the first polysiloxane is 500 to 100,000 g / mol.

4. In Paragraph 1, The above first polysiloxane is the above ArSiO 3 / 2 An insulating film for a photovoltaic device, which is composed of units.

5. In Paragraph 1, The insulating film for the above-mentioned photovoltaic device is an insulating film for a photovoltaic device having a crack limit thickness of 5 μm or more according to the following evaluation method. [Crack limit thickness] After applying the above-mentioned curable composition onto a substrate, the solvent is removed by heating at a temperature of 100°C for 2 minutes and curing at a temperature of 400°C for 30 minutes to form an insulating film while increasing the thickness from 1 μm to 10 μm in increments of 0.1 μm, and the thickness at the point where a crack occurs is called the crack limit thickness.

6. In Paragraph 1, The insulating film for the above-mentioned photovoltaic device is an insulating film for a photovoltaic device that does not crack when immersed in a stripper solution at 60°C for 5 minutes and then subjected to heat treatment at 400°C for 30 minutes three times.

7. In Paragraph 1, The insulating film for the above-mentioned photovoltaic device is an insulating film that does not crack when immersed in an etchant at 60°C for 5 minutes and then subjected to heat treatment three times at 400°C for 30 minutes.

8. In Paragraph 1, The insulating film for the above-mentioned photovoltaic device is an insulating film for a photovoltaic device having a surface hardness of 3H or higher according to ASTM-D3363.

9. A photoelectric device comprising an insulating film for a photoelectric device selected from any one of claims 1 to 8. 10.ArSiO 3 / 2 A first polysiloxane containing 90 mol% or more of the unit; R 1 SiO 3 / 2 Units 70 to 30 mol% and SiO 4 / 2 A curable composition comprising: a second polysiloxane containing 30 to 70 mol% of units; and a crosslinking agent containing aminosilane.

11. In Paragraph 10, The above-mentioned curable composition is a curable composition that further comprises a curing agent.

12. In Paragraph 10, The above curable composition further comprises a silicone-based surfactant.

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