Organic silicon liquid glue for LED and preparation method thereof
By using a combined liquid glue of vinyl silicone resin and hydrogen-containing polysiloxane in the packaging materials of LED lamps, the problem of insufficient adhesiveness of the packaging materials in the prior art is solved, efficient chip-to-substrate bonding is achieved, and the service life and production yield of LED lamps are improved.
Patent Information
- Application Number
- CN202410031391.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-01-09
- Publication Date
- 2025-05-09
- Estimated Expiration
- 2044-01-09
AI Technical Summary
The existing packaging materials based on silicone resin have weak adhesion between the chip and substrate of LED lamps, which affects the service life of LED lamps and the yield of production lines.
A liquid glue for LEDs is prepared by specific mixing and reaction conditions to form a liquid glue with high adhesive strength, including 30-70 parts by mass of vinyl silicone resin and 30-70 parts by mass of hydrogen-containing polysiloxane.
The thrust of the silicone liquid glue can reach up to 600gf at 25℃ and above 560gf at 160℃, which significantly improves the bonding performance between the chip and the substrate, reduces the risk of chip falling off, and improves the yield of LED production.
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Figure CN117844445B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of organic silicon materials, and in particular relates to an organic silicon liquid adhesive for LED and a preparation method thereof. Background Art
[0002] LED lamps use solid semiconductor chips as light-emitting materials. Compared with traditional lamps, LED lamps are energy-saving, environmentally friendly, have excellent color rendering and response speed, and have been widely used. Bonding the chip to the optical substrate is one of the key links in the production of LED lamps. The commonly used resins for bonding adhesives are epoxy resins and silicone resins. Silicone resins are polymers composed of alternating silicon and oxygen atoms forming a skeleton, and silicon atoms are connected to different organic groups. They have the following advantages: (1) thermal oxidation stability, which is outstanding in low volatility when used in LED adhesives; (2) electrical insulation performance; (3) weather resistance, which can maintain performance stability for a long time. Based on this, silicone resins are usually used as packaging materials in the packaging process of LED lamps.
[0003] However, the current packaging materials based on silicone resin have poor adhesion. When used between chips and substrates, their weak adhesion directly affects the service life of LED lamps. Weak adhesion can easily cause the chip to fall off, affecting the production line yield. Therefore, it is necessary to propose a high-adhesion silicone liquid glue for LEDs and its preparation method. Summary of the invention
[0004] The present invention aims to solve at least one of the technical problems existing in the prior art, and provides a silicone liquid adhesive for LED and a preparation method thereof.
[0005] In one aspect of the present invention, there is provided a silicone liquid adhesive for LED, the components of which include:
[0006] 30-70 parts by mass of vinyl silicone resin;
[0007] 30-70 parts by mass of hydrogen-containing polysiloxane;
[0008] 0.01-10 parts by mass of a catalyst; wherein,
[0009] The vinyl silicone resin is at least one of a main-chain vinyl silicone resin and a branched-chain vinyl silicone resin;
[0010] The hydrogen-containing polysiloxane is a hydrogen-based silicone resin with a branched network structure.
[0011] Optionally, the components of the vinyl silicone resin include:
[0012] 30-200 parts by mass of tetrafunctional siloxane;
[0013] 40-200 parts by mass of trifunctional siloxane;
[0014] 20-200 parts by mass of difunctional siloxane;
[0015] 1-50 parts by mass of a vinyl end-capping agent.
[0016] Optionally, the tetrafunctional siloxane is selected from one or more of tetramethoxysilane, tetraethoxysilane and dimethoxydichlorosilane;
[0017] The trifunctional siloxane is selected from one or more of isopropyltriethoxysilane, methyltriethoxysilane, propyltriethoxysilane, phenyltriethoxysilane, ethyltrichlorosilane, phenyltrichlorosilane, phenylethoxydichlorosilane and methylethoxydifluorosilane;
[0018] The difunctional siloxane is selected from one or more of methylethyldimethoxysilane, methylethyldiethoxysilane, ethylphenyldimethoxysilane, methylvinylmethoxychlorosilane, dimethyldiethoxysilane, diphenyldimethoxysilane and methylvinyldichlorosilane;
[0019] The vinyl end-capping agent is selected from one or more of tetramethyldivinyldisiloxane, tetraethyldivinyldisiloxane, trichlorovinylsilane, ethyltrivinylsilane, dichlorodivinylsilane and hexavinyldisiloxane.
[0020] Optionally, the vinyl silicone resin is vinyl methyl silicone resin, vinyl phenyl silicone resin or vinyl propyl silicone resin.
[0021] Optionally, the components of the hydrogen-containing polysiloxane include:
[0022] 0-150 parts by mass of tetrafunctional siloxane;
[0023] 0-150 parts by mass of trifunctional siloxane;
[0024] 20-80 parts by mass of hydrogen-containing capping agent.
[0025] Optionally, the tetrafunctional siloxane is selected from one or more of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate and butyl orthosilicate;
[0026] The trifunctional siloxane is selected from one or more of ethyltrimethoxysilane, phenyltrichlorosilane, methyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane and ethyltrichlorosilane;
[0027] The hydrogen-containing end-capping agent is selected from one or more of tetraethyldihydrogendisiloxane, diphenyltetrahydrogendisiloxane and tetraphenyldihydrogendisiloxane.
[0028] Optionally, the LED silicone liquid glue further includes:
[0029] 0-10 parts by mass of a thixotropic agent;
[0030] 0-10 parts by mass of a tackifier;
[0031] 0-10 parts by mass of inhibitor.
[0032] Optionally, the thixotropic agent is one or more of hydrogenated castor oil, polyamide wax, fumed silica, polyurethane, polyvinyl alcohol and organic bentonite;
[0033] The tackifier is an organosilicon tackifier;
[0034] The catalyst is a platinum catalyst;
[0035] The inhibitor is an alkynol inhibitor.
[0036] Another aspect of the present invention provides a method for preparing the above-mentioned organic silicone liquid adhesive for LED, the method comprising:
[0037] Forming vinyl silicone resins;
[0038] forming a hydrogen-containing polysiloxane;
[0039] The vinyl silicone resin and the hydrogen-containing polysiloxane are mixed evenly at 120-150° C., a catalyst is added, and the mixture is mixed evenly to obtain a silicone liquid adhesive for LED.
[0040] Optionally, the forming of the vinyl silicone resin comprises:
[0041] 30-200 parts by mass of tetrafunctional siloxane, 40-200 parts by mass of trifunctional siloxane, 20-200 parts by mass of difunctional siloxane and 1-50 parts by mass of vinyl end-capping agent are mixed, stirred in an ice-water bath, and then an acidic solution is added. After that, after reacting in an ice-water bath for 2 to 3 hours, an alkaline solution is added to adjust the pH value. After that, the reaction is stirred at 120 to 140° C. for 3 to 5 hours to obtain the vinyl silicone resin.
[0042] Optionally, the forming of hydrogen-containing polysiloxane comprises:
[0043] 0-150 parts by mass of tetrafunctional siloxane, 0-150 parts by mass of trifunctional siloxane, and 20-80 parts by mass of hydrogen-containing end-capping agent are mixed and stirred, an acidic solution is added, and the mixture is reacted at 90-110° C. for 2-4 hours. Thereafter, an alkaline solution is added and the mixture is stirred and reacted at 70-90° C. for 0.2-1 hour to obtain hydrogen-containing polysiloxane.
[0044] The present invention proposes a silicone liquid glue for LED and a preparation method thereof, wherein the silicone liquid glue comprises: 30-70 parts by mass of vinyl silicone resin; 30-70 parts by mass of hydrogen-containing polysiloxane; 0.01-10 parts by mass of a catalyst; wherein the vinyl silicone resin is at least one of a main-chain vinyl silicone resin and a branched vinyl silicone resin; and the hydrogen-containing polysiloxane is a hydrogen-based silicone resin with a branched network structure. The silicone liquid glue for LED of the present invention has simple ingredients and good adhesion. The maximum thrust of the silicone liquid glue at 25°C can reach more than 600gf, and the maximum thrust at 160°C can reach more than 560gf, which effectively improves the bonding performance between the chip and the substrate, reduces the risk of chip falling off in subsequent stages, and improves the LED production yield. BRIEF DESCRIPTION OF THE DRAWINGS
[0045] Figure 1 The present invention is a flowchart of a method for preparing organic silicone liquid adhesive for LED according to an embodiment of the present invention. DETAILED DESCRIPTION
[0046] In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention is further described in detail below in conjunction with the accompanying drawings and specific implementation methods. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all of the embodiments. Based on the described embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work are within the scope of protection of the present invention.
[0047] In one aspect of the present invention, a silicone liquid glue for LED is provided, the ingredients of which include: 30-70 parts by mass of vinyl silicone resin; 30-70 parts by mass of hydrogen-containing polysiloxane; 0.01-10 parts by mass of a catalyst; wherein the vinyl silicone resin is at least one of a main chain vinyl silicone resin and a branched vinyl silicone resin; and the hydrogen-containing polysiloxane is a hydrogen-based silicone resin with a branched network structure.
[0048] In this embodiment, the structures of the vinyl silicone resin and the hydrogen-containing polysiloxane monomers are designed, that is, the vinyl silicone resin is a main chain vinyl silicone resin and a branched vinyl silicone resin terminated with a vinyl group, that is, the vinyl group can be located at the chain end, on the main chain, or on the branch chain; secondly, the hydrogen-containing polysiloxane is a hydrogen-based silicone resin with a branched network structure terminated with hydrogen, and more hydrogen-containing groups can be connected based on the branched network structure. In this way, the hydrogen-containing groups can be combined with vinyl groups distributed at multiple positions to effectively increase the crosslinking density. That is, based on the structural design of the above two components, it is possible to form a silicone liquid glue with high adhesion on the premise that the above two components are only mixed with a catalyst.
[0049] It should be noted that the vinyl silicone resin of the present embodiment is synthesized by hydrolysis and polycondensation of different numbers of methoxy / ethoxy siloxy monomers and vinyl end-capping agents. For example, tetrafunctional siloxane, trifunctional siloxane, difunctional siloxane and vinyl end-capping agents are synthesized by hydrolysis and polycondensation. The specific process is described below.
[0050] In some preferred embodiments, the components of the vinyl silicone resin include: 30-200 parts by mass of tetrafunctional siloxane; 40-200 parts by mass of trifunctional siloxane; 20-200 parts by mass of difunctional siloxane; and 1-50 parts by mass of a vinyl end-capping agent.
[0051] In other preferred embodiments, the tetrafunctional siloxane is selected from one or more of tetramethoxysilane, tetraethoxysilane and dimethoxydichlorosilane.
[0052] In other preferred embodiments, the trifunctional siloxane is selected from one or more of isopropyltriethoxysilane, methyltriethoxysilane, propyltriethoxysilane, phenyltriethoxysilane, ethyltrichlorosilane, phenyltrichlorosilane, phenylethoxydichlorosilane and methylethoxydifluorosilane.
[0053] In other preferred embodiments, the difunctional siloxane is selected from one or more of methylethyldimethoxysilane, methylethyldiethoxysilane, ethylphenyldimethoxysilane, methylvinylmethoxychlorosilane, dimethyldiethoxysilane, diphenyldimethoxysilane and methylvinyldichlorosilane.
[0054] In other preferred embodiments, the vinyl end-capping agent is selected from one or more of tetramethyldivinyldisiloxane, tetraethyldivinyldisiloxane, trichlorovinylsilane, ethyltrivinylsilane, dichlorodivinylsilane and hexavinyldisiloxane.
[0055] Based on the above preferred components, in the present embodiment, the vinyl silicone resin may preferably be vinyl methyl silicone resin, vinyl phenyl silicone resin or vinyl propyl silicone resin.
[0056] Furthermore, the hydrogen-containing polysiloxane of this embodiment is synthesized by hydrolysis and polycondensation of different numbers of methoxy / ethoxy siloxy monomers and hydrogen-containing end-capping agents. For example, tetrafunctional siloxane, trifunctional siloxane, and hydrogen-containing end-capping agents are synthesized by hydrolysis and polycondensation. The specific process is described below.
[0057] In some preferred embodiments, the components of the hydrogen-containing polysiloxane include: 0-150 parts by mass of tetrafunctional siloxane; 0-150 parts by mass of trifunctional siloxane; and 20-80 parts by mass of a hydrogen-containing capping agent.
[0058] In other preferred embodiments, the tetrafunctional siloxane is selected from one or more of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate and butyl orthosilicate.
[0059] In other preferred embodiments, the trifunctional siloxane is selected from one or more of ethyltrimethoxysilane, phenyltrichlorosilane, methyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane and ethyltrichlorosilane.
[0060] In other preferred embodiments, the hydrogen-containing end-capping agent is selected from one or more of tetraethyldihydrogendisiloxane, diphenyltetrahydrogendisiloxane and tetraphenyldihydrogendisiloxane.
[0061] Furthermore, the content of the catalyst may preferably be 0.01-2 parts by mass, and the catalyst may be a platinum-based catalyst, wherein the platinum catalyst is preferably one or more of a palladium-platinum alloy catalyst and / or a platinum black catalyst. Such catalysts have extremely high stability and performance, and can catalyze the curing of the silicone resin to form a liquid glue with high adhesion, while overcoming the yellowing of the colloid to keep the liquid glue transparent.
[0062] Furthermore, the organic silicone liquid glue for LED also includes 0-10 parts by mass of a thixotropic agent; 0-10 parts by mass of a thickener; and 0-10 parts by mass of an inhibitor. That is, by adding thixotropic agent, thickener and inhibitor components to the above components, the adhesion of the liquid glue is further improved.
[0063] In some preferred embodiments, the content of the thixotropic agent may be preferably 0.01-4 parts by mass, and the thixotropic agent may be one or more of hydrogenated castor oil, polyamide wax, fumed silica, polyurethane, polyvinyl alcohol and organic bentonite. The thixotropic agent can make the resin static or not subjected to shear force, have a higher consistency, increase the viscosity of the liquid glue system, and provide the glue with the ability to resist sag, so that it can stay on the vertical substrate surface. Under the action of external force, the temporary network structure is destroyed, the ability to resist flow is reduced, and the resin becomes a low-viscosity fluid substance, resulting in reduced viscosity and easy flow.
[0064] In other preferred embodiments, the content of the tackifier may be preferably 1-4.9 parts by mass, and the tackifier may be a silicone tackifier. The silicone tackifier may be preferably selected from one or more of aliphatic silicone tackifiers, alicyclic silicone tackifiers and / or aromatic silicone tackifiers, for example, vinyl tackifiers, which are beneficial to increase the viscosity of the resin, facilitate processing, and also improve the transparency of the colloid.
[0065] In other preferred embodiments, the content of the inhibitor may preferably be 0.02-4 parts by mass, and the inhibitor may be an alkynol inhibitor, which is preferably selected from one or more of 3-methyl-1-butyn-3-ol, 2-propyn-1-ol, 2-phenyl-1-butene-3-ol, 4-pentyn-1-ol, 2-methyl-3-butyn-2-ol and / or 3-methyl-2-pentene-4-ynol. The inhibitor is added to the liquid glue as an additive, which can react with the catalyst to form a complex and reduce the amount of catalyst used.
[0066] like Figure 1 As shown, another aspect of the present invention provides a method S100 for preparing the above-mentioned organic silicone liquid adhesive for LED, comprising the following steps S110 to S130:
[0067] S110, forming a vinyl silicone resin.
[0068] Specifically, 30-200 parts by mass of tetrafunctional siloxane, 40-200 parts by mass of trifunctional siloxane, 20-200 parts by mass of difunctional siloxane and 1-50 parts by mass of vinyl end-capping agent are mixed, and after stirring in an ice-water bath, an acidic solution (for example, a nitric acid solution) is added. After that, after reacting in an ice-water bath for 2 to 3 hours, an alkaline solution (for example, an aqueous sodium hydroxide solution) is added to adjust the pH value to 8-9. After that, the reaction is continued at 120 to 140° C. for 3 to 5 hours with stirring to obtain a vinyl silicone resin.
[0069] It should be noted that in step S110, the preferred components of the tetrafunctional siloxane, trifunctional siloxane, difunctional siloxane and vinyl end-capping agent can be referred to the above description and will not be described in detail here.
[0070] In this embodiment, different numbers of methoxy / ethoxysilaneoxy monomers and vinyl end-capping agents are used to synthesize vinyl silicone resins through hydrolysis and condensation, so that each silicone compound monomer is polymerized into a silicone polymer. In the silicone polymer, the vinyl group can be distributed on the chain end, the main chain and the side chain, so that the polymer has a higher degree of polymerization and molecular weight, thereby making the silicone liquid glue have better adhesion and application characteristics.
[0071] S120. Forming hydrogen-containing polysiloxane.
[0072] Specifically, 0-150 parts by mass of tetrafunctional siloxane, 0-150 parts by mass of trifunctional siloxane, and 20-80 parts by mass of a hydrogen-containing end-capping agent are mixed and stirred, an acidic solution (e.g., a nitric acid solution) is added, and the mixture is reacted at 90-110° C. for 2-4 hours, and then an alkaline solution is added and the mixture is stirred and reacted at 70-90° C. for 0.2-1 hour to obtain a hydrogen-containing polysiloxane.
[0073] It should be noted that the alkaline solution can be a strong alkaline solution or a weak alkaline solution. After the raw materials are mixed and stirred, a strong alkaline solution of sodium hydroxide is first added to adjust the pH value of the solution to 7-8, and then a weak alkaline solution of sodium bicarbonate is added for further reaction.
[0074] It should be further noted that, in step S120, the preferred components of the tetrafunctional siloxane, the trifunctional siloxane, and the hydrogen-containing end-capping agent can be referred to the above description, which will not be repeated here.
[0075] In this embodiment, different numbers of methoxy / ethoxy siloxy monomers are combined with hydrogen-containing end-capping agents through hydrolysis and condensation to form hydrogen-containing polysiloxane, so that each organosilicon compound monomer is polymerized into an organosilicon polymer with a higher degree of polymerization and molecular weight.
[0076] S130, 30-70 parts by mass of vinyl silicone resin and 30-70 parts by mass of hydrogenated polysiloxane are mixed uniformly at 120-150° C., cooled to room temperature for standby use, and then 0.01-10 parts by mass of catalysts are added in sequence and mixed uniformly to obtain silicone liquid glue for LED.
[0077] In some preferred embodiments, the catalyst is a platinum catalyst, and the platinum catalyst is preferably one or more selected from palladium-platinum alloy catalysts and / or platinum black catalysts. In addition, the content of the catalyst may be preferably 0.01-2 parts by mass.
[0078] Furthermore, in step S130, 30-70 parts by mass of vinyl silicone resin and 30-70 parts by mass of hydrogenated polysiloxane may be evenly mixed, and then 0-10 parts by mass of thixotropic agent, 0-10 parts by mass of tackifier, 0.01-10 parts by mass of catalyst and 0-10 parts by mass of inhibitor may be added in sequence, and then mixed again to obtain silicone liquid glue for LED.
[0079] In some preferred embodiments, the content of the thixotropic agent may also be preferably 0.01-4 parts by mass, and the thixotropic agent may preferably be one or more of hydrogenated castor oil, polyamide wax, fumed silica, polyurethane, polyvinyl alcohol and organic bentonite.
[0080] In other preferred embodiments, the content of the tackifier may also be preferably 1-4.9 parts by mass, and the tackifier may be preferably a silicone tackifier, and the silicone tackifier is preferably selected from one or more of aliphatic silicone tackifiers, alicyclic silicone tackifiers and / or aromatic silicone tackifiers.
[0081] In other preferred embodiments, the content of the inhibitor may also be preferably 0.02-4 parts by mass, and the inhibitor may preferably be an alkynol inhibitor, and the alkynol inhibitor is preferably selected from one or more of 3-methyl-1-butyn-3-ol, 2-propyn-1-ol, 2-phenyl-1-butene-3-ol, 4-pentyn-1-ol, 2-methyl-3-butyn-2-ol and / or 3-methyl-2-pentene-4-ynol.
[0082] In this embodiment, based on the above-mentioned preparation method, it is possible to prepare each polymer at a lower temperature and a shorter reaction time, thereby reducing the preparation process, shortening the monomer production time, and improving production efficiency. In addition, a silicone liquid glue with high adhesion is prepared in a simple manner, which effectively improves the adhesion between the chip and the substrate, reduces chip falling off in subsequent work stages, and improves the LED production yield.
[0083] Furthermore, the organic silicone liquid obtained in this embodiment can be used to bond the chip and substrate in the LED. When in use, the organic silicone liquid glue only needs to be applied on the bracket through a crystal bonding machine to bond the chip and the substrate, and then baked at 100°C for 2.5 hours, and then the wire bonding and other processes are performed. The organic silicone liquid glue has a maximum thrust of more than 600gf at 25°C and a maximum thrust of more than 560gf at 160°C. The organic silicone liquid glue greatly improves the bonding force between the chip and the substrate, the chip is not easy to fall off, and the service life of the LED lamp is effectively improved.
[0084] The following will further illustrate the preparation method of organic silicone liquid glue for LED with several specific examples:
[0085] Example 1
[0086] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0087] S1. Synthesis steps of vinyl silicone resin:
[0088] As shown in Table 1, each raw material (150 parts by mass of tetramethoxysilane, 45 parts by mass of isopropyltriethoxysilane, 20 parts by mass of methylethyldimethoxysilane, and 20 parts by mass of tetramethyldivinyldisiloxane) was weighed by weight, and each raw material was added to a reaction container in sequence. After stirring for 15 minutes under an ice-water bath, 3 parts by mass of nitric acid solution (1 part by mass of nitric acid corresponds to 17 parts by mass of aqueous solution) were added. After that, the reaction was continued under an ice-water bath for 2.5 hours with slow stirring throughout the process. After the reaction was completed, 5 parts by mass of sodium hydroxide aqueous solution was added to adjust the pH to 8-9, and the reaction was continued to be stirred at 130°C for 4 hours. After the reaction was completed, vinyl silicone resin H1-1 was obtained.
[0089] S2, hydrogen-containing polysiloxane synthesis steps:
[0090] As shown in Table 2, each raw material (140 parts by weight of methyl orthosilicate, 80 parts by weight of phenyltriethoxysilane, and 24 parts by weight of tetraethyldihydrodisiloxane) was weighed by weight, and each raw material was added to a reaction container in turn, stirred evenly, and then 3 parts by weight of nitric acid solution (1 part by weight of nitric acid corresponds to 17 parts by weight of aqueous solution) was added, heated to 100° C. and reacted for 3 hours, with slow stirring throughout the process. After the reaction, 1 wt % sodium hydroxide aqueous solution was added to adjust the pH to 7-8, and then 10 parts by weight of sodium bicarbonate aqueous solution was added, and stirred at 80° C. for 0.5 hours. After the reaction, the clear and transparent hydrogen polysiloxane H2-1 was obtained after washing with water until neutral.
[0091] S3, preparing the high-adhesion LED organic silicone liquid glue:
[0092] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-1 obtained in step S1 and the hydrogen-containing polysiloxane H2-1 obtained in step S2, and the two raw materials are mixed uniformly at room temperature. Then, polyvinyl alcohol thixotropic agent, tackifier, platinum catalyst and 3-methyl-1-butyn-3-ol inhibitor are added in sequence and mixed uniformly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0093] Further, the organic silicon liquid glue prepared in Example 1 was dotted on the bracket, and a 8*22mil 2 The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust was 412g at 25°C and 374g at 160°C.
[0094] Example 2
[0095] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0096] S1. Synthesis steps of vinyl silicone resin:
[0097] As shown in Table 1, each raw material (130 parts by mass of tetraethoxysilane, 60 parts by mass of methyltriethoxysilane, 25 parts by mass of methylethyldimethoxysilane, and 20 parts by mass of tetramethyldivinyldisiloxane) was weighed by weight, and each raw material was added to a reaction container in sequence. After stirring for 15 minutes under an ice-water bath, 3 parts by mass of nitric acid solution (1 part by mass of nitric acid corresponds to 17 parts by mass of aqueous solution) was added, and then the reaction was continued under an ice-water bath for 2.5 hours, with slow stirring throughout the process. After the reaction was completed, 5 parts by mass of sodium hydroxide aqueous solution was added to adjust the pH to 8-9, and the reaction was continued to be stirred at 130°C for 4 hours. After the reaction was completed, vinyl silicone resin H1-2 was obtained.
[0098] S2, the synthesis steps of hydrogen-containing polysiloxane are the same as those in Example 1:
[0099] S3, preparing the high-adhesion LED organic silicone liquid glue:
[0100] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-2 obtained in step S1 and the hydrogen-containing polysiloxane H2-1 obtained in step S2, and the two raw materials are mixed evenly at room temperature. Then, polyvinyl alcohol thixotropic agent, thickener, platinum catalyst and 3-methyl-1-butyn-4-ol inhibitor are added in sequence and mixed evenly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0101] Further, the organic silicon liquid glue prepared in Example 2 was dotted on the bracket, and a 8*22mil 2 The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust was 434g at 25°C and 403g at 160°C.
[0102] Example 3
[0103] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0104] S1. Synthesis steps of vinyl silicone resin:
[0105] As shown in Table 1, each raw material (145 parts by mass of dimethoxydichlorosilane, 60 parts by mass of propyltriethoxysilane, 40 parts by mass of diphenyldimethoxysilane, and 20 parts by mass of trichlorovinylsilane) was weighed by weight, and each raw material was added to a reaction container in sequence. After stirring for 15 minutes under an ice-water bath, 3 parts by mass of nitric acid solution (1 part by mass of nitric acid corresponds to 17 parts by mass of aqueous solution) was added, and then the reaction was continued under an ice-water bath for 2.5 hours, with slow stirring throughout the process. After the reaction was completed, 5 parts by mass of sodium hydroxide aqueous solution was added to adjust the pH to 8-9, and the reaction was continued to be stirred at 130°C for 4 hours. After the reaction was completed, vinyl silicone resin H1-3 was obtained.
[0106] S2. The steps for synthesizing hydrogen-containing polysiloxane are the same as those in Example 1.
[0107] S3, preparing the high-adhesion LED organic silicone liquid glue:
[0108] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-3 obtained in step S1 and the hydrogen-containing polysiloxane H2-1 obtained in step S2, and the two raw materials are mixed evenly at room temperature. Then, polyvinyl alcohol thixotropic agent, tackifier, platinum catalyst and 3-methyl-1-butyn-5-ol inhibitor are added in sequence and mixed evenly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0109] Further, the organic silicon liquid glue prepared in Example 3 was dotted on the bracket, and a 8*22mil 2 The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust was 456g at 25°C and 379g at 160°C.
[0110] Example 4
[0111] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0112] S1. Synthesis steps of vinyl silicone resin:
[0113] As shown in Table 1, each raw material (40 parts by mass of tetramethoxysilane, 135 parts by mass of phenyltriethoxysilane, 40 parts by mass of methylvinyldichlorosilane, and 20 parts by mass of trichlorovinylsilane) was weighed by weight, and each raw material was added to a reaction container in sequence. After stirring for 15 minutes under an ice-water bath, 3 parts by mass of nitric acid solution (1 part by mass of nitric acid corresponds to 17 parts by mass of aqueous solution) was added, and then the reaction was continued under an ice-water bath for 2.5 hours with slow stirring throughout the process. After the reaction was completed, 5 parts by mass of sodium hydroxide aqueous solution was added to adjust the pH to 8-9, and the reaction was continued at 130° C. with stirring for 4 hours. After the reaction was completed, vinyl silicone resin H1-4 was obtained.
[0114] S2. The steps for synthesizing hydrogen-containing polysiloxane are the same as those in Example 1.
[0115] S3, preparing the high-adhesion LED organic silicone liquid glue:
[0116] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-4 obtained in step S1 and the hydrogen-containing polysiloxane H2-1 obtained in step S2, and the two raw materials are mixed evenly at room temperature. Then, polyvinyl alcohol thixotropic agent, tackifier, platinum catalyst and 3-methyl-1-butyn-6-ol inhibitor are added in sequence and mixed evenly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0117] Further, the organic silicon liquid glue prepared in Example 4 was dotted on the bracket, and a 8*22mil 2 The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust was 575g at 25°C and 487g at 160°C.
[0118] Example 5
[0119] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0120] S1. The steps for synthesizing the vinyl silicone resin are the same as those in Example 1.
[0121] S2, hydrogen-containing polysiloxane synthesis steps:
[0122] As shown in Table 2, each raw material (150 parts by weight of methyl orthosilicate, 40 parts by weight of methyltriethoxysilane, and 24 parts by weight of tetraethyldihydrodisiloxane) was weighed by weight, and each raw material was added to a reaction container in turn, stirred evenly, and then 3 parts by weight of nitric acid solution (1 part by weight of nitric acid corresponds to 17 parts by weight of aqueous solution) was added, heated to 100°C for reaction for 3 hours, and stirred slowly throughout the process. After the reaction, sodium hydroxide aqueous solution was added to adjust the pH to 7-8, and then 10 parts by weight of sodium bicarbonate aqueous solution was added, and stirred at 80°C for 0.5 hours. After the reaction, the mixture was washed with water until neutral to obtain clear and transparent hydrogen polysiloxane H2-2.
[0123] S3. Preparation of high-adhesion silicone liquid glue for LED:
[0124] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-1 obtained in step S1 and the hydrogen-containing polysiloxane H2-2 obtained in step S2, and the two raw materials are mixed evenly at room temperature. Then, polyvinyl alcohol thixotropic agent, thickener, platinum catalyst and 3-methyl-1-butyn-7-ol inhibitor are added in sequence and mixed evenly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0125] Further, the organic silicon liquid glue prepared in Example 5 was dotted on the bracket, and a 8*22mil 2 The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust was 455g at 25°C and 401g at 160°C.
[0126] Example 6
[0127] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0128] S1. The steps for synthesizing the vinyl silicone resin are the same as those in Example 2.
[0129] S2. The steps for synthesizing hydrogen-containing polysiloxane are the same as those in Example 5.
[0130] S3. Preparation of high-adhesion silicone liquid glue for LED:
[0131] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-2 obtained in step S1 and the hydrogen-containing polysiloxane H2-2 obtained in step S2, and the two raw materials are mixed evenly at room temperature. Then, polyvinyl alcohol thixotropic agent, tackifier, platinum catalyst and 3-methyl-1-butyn-8-ol inhibitor are added in sequence and mixed evenly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0132] Further, the organic silicon liquid glue prepared in Example 6 was dotted on the bracket, and a 8*22mil 2 The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust was 345g at 25°C and 309g at 160°C.
[0133] Example 7
[0134] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0135] S1. The steps for synthesizing the vinyl silicone resin are the same as those in Example 3.
[0136] S2. The steps for synthesizing hydrogen-containing polysiloxane are the same as those in Example 5.
[0137] S3. Preparation of high-adhesion silicone liquid glue for LED:
[0138] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-3 obtained in step S1 and the hydrogen-containing polysiloxane H2-2 obtained in step S2, and the two raw materials are mixed evenly at room temperature. Then, polyvinyl alcohol thixotropic agent, tackifier, platinum catalyst and 3-methyl-1-butyn-9-ol inhibitor are added in sequence and mixed evenly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0139] Further, the organic silicon liquid glue prepared in Example 7 was dotted on the bracket, and a 8*22mil 2The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust was 567g at 25°C and 502g at 160°C.
[0140] Example 8
[0141] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0142] S1. The steps for synthesizing the vinyl silicone resin are the same as those in Example 4.
[0143] S2. The steps for synthesizing hydrogen-containing polysiloxane are the same as those in Example 5.
[0144] S3. Preparation of high-adhesion silicone liquid glue for LED:
[0145] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-4 obtained in step S1 and the hydrogen-containing polysiloxane H2-2 obtained in step S2, and the two raw materials are mixed evenly at room temperature. Then, polyvinyl alcohol thixotropic agent, tackifier, platinum catalyst and 3-methyl-1-butyn-10-ol inhibitor are added in sequence and mixed evenly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0146] Further, the organic silicon liquid glue prepared in Example 8 was dotted on the bracket, and a 8*22mil 2 The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust is 420g at 25°C and 381g at 160°C.
[0147] Example 9
[0148] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0149] S1. The steps for synthesizing the vinyl silicone resin are the same as those in Example 1.
[0150] S2, hydrogen-containing polysiloxane synthesis steps:
[0151] As shown in Table 2, each raw material (130 parts by weight of tetraethyl orthosilicate, 90 parts by weight of phenyltrichlorosilane, and 24 parts by weight of tetraphenyldihydrodisiloxane) was weighed by weight, and each raw material was added to a reaction container in turn, stirred evenly, and then 3 parts by weight of nitric acid solution (1 part by weight of nitric acid corresponds to 17 parts by weight of aqueous solution) was added, heated to 100°C for reaction for 3 hours, and stirred slowly throughout the process. After the reaction, sodium hydroxide aqueous solution was added to adjust the pH to 7-8, and then 5 parts by weight of sodium bicarbonate aqueous solution was added, and stirred at 80°C for 0.5 hours. After the reaction, the mixture was washed with water until neutral to obtain clear and transparent hydrogen polysiloxane H2-3.
[0152] S3. Preparation of high-adhesion silicone liquid glue for LED:
[0153] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-1 obtained in step S1 and the hydrogen-containing polysiloxane H2-3 obtained in step S2, and the two raw materials are mixed evenly at room temperature. Then, polyvinyl alcohol thixotropic agent, thickener, platinum catalyst and 3-methyl-1-butyn-11-ol inhibitor are added in sequence and mixed evenly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0154] Further, the organic silicon liquid glue prepared in Example 9 was dotted on the bracket, and a 8*22mil 2 The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust was 431g at 25°C and 413g at 160°C.
[0155] Example 10
[0156] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0157] S1. The steps for synthesizing the vinyl silicone resin are the same as those in Example 2.
[0158] S2. The steps for synthesizing hydrogen-containing polysiloxane are the same as those in Example 9.
[0159] S3. Preparation of high-adhesion silicone liquid glue for LED:
[0160] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-2 obtained in step S1 and the hydrogen-containing polysiloxane H2-3 obtained in step S2, and the two raw materials are mixed evenly at room temperature. Then, polyvinyl alcohol thixotropic agent, tackifier, platinum catalyst and 3-methyl-1-butyn-12-ol inhibitor are added in sequence and mixed evenly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0161] Further, the organic silicon liquid glue prepared in Example 10 was dotted on the bracket, and a 8*22mil 2 The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust was 555g at 25°C and 504g at 160°C.
[0162] Embodiment 11
[0163] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0164] S1. The steps for synthesizing the vinyl silicone resin are the same as those in Example 3.
[0165] S2. The steps for synthesizing hydrogen-containing polysiloxane are the same as those in Example 9.
[0166] S3. Preparation of high-adhesion silicone liquid glue for LED:
[0167] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-3 obtained in step S1 and the hydrogen-containing polysiloxane H2-3 obtained in step S2, and the two raw materials are mixed evenly at room temperature. Then, polyvinyl alcohol thixotropic agent, tackifier, platinum catalyst and 3-methyl-1-butyn-13-ol inhibitor are added in sequence and mixed evenly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0168] Further, the organic silicon liquid glue prepared in Example 11 was dotted on the bracket, and a 8*22mil 2 The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust was 598g at 25°C and 556g at 160°C.
[0169] Example 12
[0170] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0171] S1. The steps for synthesizing the vinyl silicone resin are the same as those in Example 4.
[0172] S2. The steps for synthesizing hydrogen-containing polysiloxane are the same as those in Example 9.
[0173] S3. Preparation of high-adhesion silicone liquid glue for LED:
[0174] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-4 obtained in step S1 and the hydrogen-containing polysiloxane H2-3 obtained in step S2, and the two raw materials are mixed evenly at room temperature. Then, polyvinyl alcohol thixotropic agent, tackifier, platinum catalyst and 3-methyl-1-butyn-14-ol inhibitor are added in sequence and mixed evenly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0175] Further, the organic silicon liquid glue prepared in Example 12 is dotted on the bracket, and a 8*22mil 2 The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust was 545g at 25°C and 491g at 160°C.
[0176] Embodiment 13
[0177] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0178] S1. The steps for synthesizing the vinyl silicone resin are the same as those in Example 1.
[0179] S2, hydrogen-containing polysiloxane synthesis steps:
[0180] As shown in Table 2, each raw material (70 parts by mass of propyl orthosilicate, 135 parts by mass of ethyltrimethoxysilane, and 24 parts by mass of diphenyltetrahydrodisiloxane) was weighed by weight, and each raw material was added to a reaction container in turn, stirred evenly, and then 3 parts by mass of nitric acid solution (1 part by mass of nitric acid corresponds to 17 parts by mass of aqueous solution) was added, heated to 100°C for reaction for 3 hours, and stirred slowly throughout the process. After the reaction, sodium hydroxide aqueous solution was added to adjust the pH to 7-8, and then 5 parts by mass of sodium bicarbonate aqueous solution was added, and stirred at 80°C for 0.5 hours. After the reaction, the clear and transparent hydrogen polysiloxane H2-4 was obtained after washing with water until neutral.
[0181] S3. Preparation of high-adhesion silicone liquid glue for LED:
[0182] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-1 obtained in step S1 and the hydrogen-containing polysiloxane H2-4 obtained in step S2, and the two raw materials are mixed evenly at room temperature. Then, polyvinyl alcohol thixotropic agent, tackifier, platinum catalyst and 3-methyl-1-butyn-15-ol inhibitor are added in sequence and mixed evenly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0183] Further, the organic silicon liquid glue prepared in Example 13 was dotted on the bracket, and a 8*22mil 2 The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust was 611g at 25°C and 569g at 160°C.
[0184] Embodiment 14
[0185] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0186] S1. The steps for synthesizing the vinyl silicone resin are the same as those in Example 2.
[0187] S2. The steps for synthesizing hydrogen-containing polysiloxane are the same as those in Example 13.
[0188] S3. Preparation of high-adhesion silicone liquid glue for LED:
[0189] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-2 obtained in step S1 and the hydrogen-containing polysiloxane H2-4 obtained in step S2, and the two raw materials are mixed evenly at room temperature. Then, polyvinyl alcohol thixotropic agent, tackifier, platinum catalyst and 3-methyl-1-butyn-16-ol inhibitor are added in sequence and mixed evenly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0190] Further, the organic silicon liquid glue prepared in Example 14 was dotted on the bracket, and a 8*22mil 2 The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust was 478g at 25°C and 425g at 160°C.
[0191] Embodiment 15
[0192] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0193] S1. The steps for synthesizing the vinyl silicone resin are the same as those in Example 3.
[0194] S2. The steps for synthesizing hydrogen-containing polysiloxane are the same as those in Example 13.
[0195] S3. Preparation of high-adhesion silicone liquid glue for LED:
[0196] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-3 obtained in step S1 and the hydrogen-containing polysiloxane H2-4 obtained in step S2, and the two raw materials are mixed evenly at room temperature. Then, polyvinyl alcohol thixotropic agent, tackifier, platinum catalyst and 3-methyl-1-butyn-17-ol inhibitor are added in sequence and mixed evenly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0197] Further, the organic silicon liquid glue prepared in Example 15 was dotted on the bracket, and a 8*22mil 2 The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust was 437g at 25°C and 380g at 160°C.
[0198] Example 16
[0199] The method for preparing organic silicone liquid glue for LED in this example includes the following steps:
[0200] S1. The steps for synthesizing the vinyl silicone resin are the same as those in Example 4.
[0201] S2. The steps for synthesizing hydrogen-containing polysiloxane are the same as those in Example 13.
[0202] S3. Preparation of high-adhesion silicone liquid glue for LED:
[0203] As shown in Table 3, the raw materials are weighed by weight, including the vinyl silicone resin H1-4 obtained in step S1 and the hydrogen-containing polysiloxane H2-4 obtained in step S2, and the two raw materials are mixed evenly at room temperature. Then, polyvinyl alcohol thixotropic agent, tackifier, platinum catalyst and 3-methyl-1-butyn-18-ol inhibitor are added in sequence and mixed evenly. After degassing, filtration and other treatments, a high-adhesion silicone liquid glue for LED is obtained.
[0204] Further, the organic silicon liquid glue prepared in Example 16 was dotted on the bracket, and a 8*22mil 2 The chip was fixed on the bracket to bond the chip and the substrate, and baked at 100°C for 2.5 hours. After the silicone liquid glue was cured, the inference value of the chip being pushed at 25°C and 160°C was tested. The test results are shown in Table 4 below. The thrust was 426g at 25°C and 393g at 160°C.
[0205] Table 1 Vinyl silicone resin synthesis raw materials and proportions
[0206]
[0207] Table 2 Raw materials and proportions for synthesis of hydrogen-containing siloxane
[0208]
[0209] Table 3 Raw materials for synthesis of organic silicone liquid adhesive
[0210]
[0211] Table 4 Chip thrust test results
[0212]
[0213]
[0214] In summary, the silicone liquid glue formed by mixing different vinyl silicone resins, hydrogen-containing polysiloxanes, tackifiers, thixotropic agents, catalysts and inhibitors has good adhesion. When it is used for LED packaging, for 8*22 size chips, the thrust can reach more than 600gf at 25°C, and the thrust can reach more than 560gf at 160°C. Most of the liquid glues have a thrust of more than 400gf at 25°C and 160°C, which shows that the liquid glue greatly improves the adhesion between the chip and the substrate, and can prevent the chip from falling off during long-term use.
[0215] It is to be understood that the above embodiments are merely exemplary embodiments used to illustrate the principles of the present invention, but the present invention is not limited thereto. For those of ordinary skill in the art, various modifications and improvements can be made without departing from the spirit and essence of the present invention, and these modifications and improvements are also considered to be within the scope of protection of the present invention.
Claims
1. A method for preparing organic silicone liquid glue for LED, characterized in that: The method comprises: Forming vinyl silicone resins, including: 30-200 parts by mass of tetrafunctional siloxane, 40-200 parts by mass of trifunctional siloxane, 20-200 parts by mass of difunctional siloxane and 1-50 parts by mass of vinyl end-capping agent are mixed, and an acidic solution is added after stirring in an ice-water bath, and then, after reacting in an ice-water bath for 2-3 hours, an alkaline solution is added to adjust the pH value, and then, the reaction is stirred at 120-140° C. for 3-5 hours to obtain a vinyl silicone resin; the vinyl silicone resin is at least one of a main-chain vinyl silicone resin and a branched-chain vinyl silicone resin; Forming a hydrogen-containing polysiloxane comprising: 0-150 parts by weight of tetrafunctional siloxane, 0-150 parts by weight of trifunctional siloxane, and 20-80 parts by weight of hydrogen-containing end-capping agent are mixed and stirred, an acidic solution is added, and the mixture is reacted at 90-110° C. for 2-4 hours, and then an alkaline solution is added and the mixture is stirred and reacted at 70-90° C. for 0.2-1 hour to obtain hydrogen-containing polysiloxane; the hydrogen-containing polysiloxane is a hydrogen-based silicone resin with a branched network structure; 30-70 parts by weight of vinyl silicone resin and 30-70 parts by weight of hydrogenated polysiloxane are mixed uniformly at 120-150° C., and after cooling to room temperature, 0.01-10 parts by weight of catalyst, thixotropic agent, tackifier and inhibitor are added and mixed uniformly to obtain silicone liquid glue for LED.
2. A silicone liquid adhesive for LED, characterized in that: The organic silicone liquid glue for LED is prepared by the method according to claim 1. The content of the thixotropic agent is 0-10 parts by mass; The content of the tackifier is 0-10 parts by mass; The content of the inhibitor is 0-10 parts by weight; The vinyl silicone resin is at least one of a main-chain vinyl silicone resin and a branched-chain vinyl silicone resin; The hydrogen-containing polysiloxane is a hydrogen-based silicone resin with a branched network structure.
3. The organic silicone liquid adhesive for LED according to claim 2, characterized in that: In the vinyl silicone resin, the tetrafunctional siloxane is selected from one or more of tetramethoxysilane, tetraethoxysilane and dimethoxydichlorosilane; The trifunctional siloxane is selected from one or more of isopropyltriethoxysilane, methyltriethoxysilane, propyltriethoxysilane, phenyltriethoxysilane, ethyltrichlorosilane, phenyltrichlorosilane, phenylethoxydichlorosilane and methylethoxydifluorosilane; The difunctional siloxane is selected from one or more of methylethyldimethoxysilane, methylethyldiethoxysilane, ethylphenyldimethoxysilane, methylvinylmethoxychlorosilane, dimethyldiethoxysilane, diphenyldimethoxysilane and methylvinyldichlorosilane; The vinyl end-capping agent is selected from one or more of tetramethyldivinyldisiloxane, tetraethyldivinyldisiloxane, trichlorovinylsilane, ethyltrivinylsilane, dichlorodivinylsilane and hexavinyldisiloxane.
4. The organic silicone liquid adhesive for LED according to claim 2, characterized in that: The vinyl silicone resin is vinyl methyl silicone resin, vinyl phenyl silicone resin or vinyl propyl silicone resin.
5. The organic silicone liquid adhesive for LED according to claim 2, characterized in that: In the hydrogen-containing polysiloxane, the tetrafunctional siloxane is selected from one or more of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate and butyl orthosilicate; The trifunctional siloxane is selected from one or more of ethyltrimethoxysilane, phenyltrichlorosilane, methyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane and ethyltrichlorosilane; The hydrogen-containing end-capping agent is selected from one or more of tetraethyldihydrogendisiloxane, diphenyltetrahydrogendisiloxane and tetraphenyldihydrogendisiloxane.
Citation Information
Patent Citations
Low-volatility adsorptive thermosetting organic silicon resin for LED (light-emitting diode)
CN116445126A