CN106010427B - A kind of resistance to vulcanization LED packaging silicon rubber of high refractive index high tenacity - Google Patents
A kind of resistance to vulcanization LED packaging silicon rubber of high refractive index high tenacity Download PDFInfo
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- CN106010427B CN106010427B CN201610484779.8A CN201610484779A CN106010427B CN 106010427 B CN106010427 B CN 106010427B CN 201610484779 A CN201610484779 A CN 201610484779A CN 106010427 B CN106010427 B CN 106010427B
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- 238000004806 packaging method and process Methods 0.000 title claims abstract description 22
- 238000004073 vulcanization Methods 0.000 title claims abstract description 18
- 229920002379 silicone rubber Polymers 0.000 title abstract 2
- -1 methyl phenyl vinyl Chemical group 0.000 claims abstract description 62
- 229920002050 silicone resin Polymers 0.000 claims abstract description 37
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 18
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 16
- 239000000853 adhesive Substances 0.000 claims abstract description 15
- 230000001070 adhesive effect Effects 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 239000003112 inhibitor Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 30
- 239000001257 hydrogen Substances 0.000 claims description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000741 silica gel Substances 0.000 claims description 16
- 229910002027 silica gel Inorganic materials 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 15
- 229910052697 platinum Inorganic materials 0.000 claims description 13
- 239000005022 packaging material Substances 0.000 claims description 9
- 229920002554 vinyl polymer Polymers 0.000 claims description 9
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 8
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- VWRQCJRTHKUVNF-UHFFFAOYSA-N 1,1,3-triphenylprop-2-yn-1-ol Chemical compound C=1C=CC=CC=1C(C=1C=CC=CC=1)(O)C#CC1=CC=CC=C1 VWRQCJRTHKUVNF-UHFFFAOYSA-N 0.000 claims description 3
- 239000007822 coupling agent Substances 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 2
- 125000003700 epoxy group Chemical group 0.000 claims description 2
- 239000004971 Cross linker Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- 230000035939 shock Effects 0.000 abstract description 7
- 239000007767 bonding agent Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 9
- 238000005303 weighing Methods 0.000 description 8
- 238000004132 cross linking Methods 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- 239000003822 epoxy resin Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 229920000647 polyepoxide Polymers 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 230000035882 stress Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000005987 sulfurization reaction Methods 0.000 description 3
- 229920002725 thermoplastic elastomer Polymers 0.000 description 3
- 238000007551 Shore hardness test Methods 0.000 description 2
- 235000010290 biphenyl Nutrition 0.000 description 2
- 239000004305 biphenyl Substances 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 238000004383 yellowing Methods 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910052946 acanthite Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 1
- 229940056910 silver sulfide Drugs 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
- C08K5/5477—Silicon-containing compounds containing nitrogen containing nitrogen in a heterocyclic ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention relates to field of adhesive technology, more particularly to a kind of resistance to vulcanization LED packaging silicon rubber of high refractive index high tenacity, including the weight ratio of component A and component B, the component A and component B are 5:1；Wherein, the component A includes the raw material of following parts by weight: 80~90 parts of methyl phenyl vinyl polysiloxane, 10~20 parts of vinyl methyl phenyl polysiloxane, 1~5 part of bonding agent, 0.1~0.3 part of platinum group catalyst；The component B includes the raw material of following parts by weight: 10-20 parts of methyl phenyl vinyl polysiloxane, 70~80 parts of the hydrogeneous silicone resin of aminomethyl phenyl, and 1~10 part of hydrogeneous toughening crosslinking agent, 0.1~0.3 part of inhibitor.The present invention solidify after material internal stress reduce, improve the performance and high temperature resistance of the cold-resistant thermal shock of product.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to high-refractive-index high-toughness vulcanization-resistant LED packaging silica gel.
Background
As LEDs are applied more and more widely, the requirements for LED packaging materials are also higher and higher. The packaging materials used by the LED at present mainly comprise epoxy resin and organosilicon materials, the epoxy resin has large internal stress, too high light decay, yellowing resistance and poor aging resistance, and the organosilicon materials have small internal stress, yellowing resistance and low light decay and are obviously superior to the epoxy resin in comprehensive performance corresponding to the epoxy resin, so that the organosilicon materials can quickly replace the epoxy resin and are widely used in the field of LED packaging. Especially, the LED packaging silica gel with the refractive index higher than 1.50 has higher light extraction efficiency and is increasingly used.
With the development of industry, the sulfur content in the air is increased day by day, and if the packaging material is not properly selected, the sulfur in the air can penetrate through the packaging material or a bonding interface thereof to corrode a silver layer of a bracket to form black silver sulfide, so that the light attenuation is increased sharply. This therefore presents new challenges for the encapsulating material, which must be improved with respect to the resistance to vulcanization. Therefore, in the formula design, methods such as increasing the content of phenyl silicone resin and increasing the crosslinking density are mostly adopted to improve the sulfuration resistance, but the sulfuration resistance is improved, the internal stress of the packaging material is too high, so that the toughness of the material is reduced, and the phenomena of lamp death due to high and low temperature cold and hot shock, easy cracking of the packaging material after high and low temperature are caused after the packaging reaction and the like occur.
Disclosure of Invention
The invention aims to solve the technical problem of providing the LED packaging silica gel with high refractive index, high toughness, vulcanization resistance and excellent cold and heat shock resistance.
The technical scheme for solving the technical problems is as follows: the LED packaging silica gel with high refractive index comprises a component A and a component B, wherein the weight ratio of the component A to the component B is 5: 1;
wherein the component A comprises the following raw materials in parts by weight: 80-90 parts of methyl phenyl vinyl silicone resin, 10-20 parts of vinyl methyl phenyl polysiloxane, 1-5 parts of adhesive and 0.1-0.3 part of platinum catalyst.
The component B comprises the following raw materials, by weight, 10-20 parts of methyl phenyl vinyl silicone resin, 70-80 parts of methyl phenyl hydrogen-containing silicone resin, 1-10 parts of a hydrogen-containing toughening cross-linking agent and 0.1-0.3 part of an inhibitor.
The invention has the beneficial effects that: the LED packaging silica gel with high refractive index consists of A, B components, wherein the A component provides resin with improved strength, tough vinyl polysiloxane, a catalyst and an adhesive in the reaction, and the B component provides resin with improved strength, a hydrogen-containing toughening cross-linking agent and an inhibitor. According to the LED packaging silica gel with the high refractive index, the curing agent is methyl phenyl hydrogen-containing silicone resin except vinyl silicone resin, the content of the silicone resin is increased, and the vulcanization resistance is improved; in addition, in order to further increase the crosslinking density, a special hydrogen-containing toughening crosslinking agent is added, so that the crosslinking density is increased after curing, the vulcanization resistance is further improved, but the toughness is improved. The combination of the silicon resin and the hydrogen-containing toughening cross-linking agent reduces the internal stress of the cured material, and improves the cold and heat shock resistance and high temperature resistance of the product.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the molecular formula of the methyl phenyl vinyl silicone resin is (ViMe2SiO1/2) x (PhSiO3/2) y, wherein Me is methyl, Vi is vinyl, Ph is phenyl, x: y =1: 4-5.
The further scheme has the beneficial effects that the silicon resin used as the matrix resin contains vinyl, so that the strength and hardness of the product are improved, and the vulcanization resistance is improved.
Further, the molecular formula of the vinyl dimethyl diphenyl polysiloxane is as follows: (ViMe2SiO1/2) x (ViMePh2SiO1/2) y, wherein Me is methyl, Vi is vinyl, Ph is phenyl, x ranges from 10 to 50, and y ranges from 10 to 50.
The further scheme has the advantages that the addition of the vinyl dimethyl diphenyl polysiloxane reduces the viscosity of the system, provides vinyl capable of participating in reaction, reduces the stress of the system after curing, and improves the cold and heat shock resistance.
Furthermore, the adhesive contains a coupling agent of an epoxy group, and the structural formula of the coupling agent is as follows:
the addition of the adhesive improves the adhesion of the packaging material to plastic and metal substrates.
Further, the platinum catalyst is any one of platinum-methyl phenyl polysiloxane complex or platinum-olefin complex. Preferably a platinum-methyl phenyl polysiloxane complex, wherein the platinum content is 3000-10000 ppm.
Further, the curing agent is a hydrogen-containing silicone resin, wherein the molecular formula of the hydrogen-containing silicone resin is as follows: (HMe2SiO1/2)3(PhSiO3/2)4, wherein Me is methyl and Ph is phenyl.
The further scheme has the beneficial effects that the silicon resin serving as the hydrogen-containing curing agent not only provides active hydrogen to participate in crosslinking reaction, improves crosslinking density, has low viscosity, and plays roles of reducing viscosity and improving strength for the whole system.
Further, the hydrogen-containing toughening crosslinking agent is
Or
Wherein Ph is phenyl.
The addition of the hydrogen-containing toughening crosslinking agent increases the crosslinking density, improves the vulcanization resistance of the product, and increases the toughness of the system due to the existence of the flexible ring body in the crosslinking toughening agent.
Further, the inhibitor is any one of ethynyl cyclohexanol or 1,1, 3-triphenyl-2-propyn-1-ol. Preferably 1,1, 3-triphenyl-2-propyn-1-ol, the structural formula of which is as follows:
。
the preparation method of the LED packaging silica gel with the high refractive index comprises the steps of preparing a component A and preparing a component B; wherein,
the preparation steps of the component A are as follows: 80-90 parts of methyl phenyl vinyl silicone resin, 10-20 parts of vinyl methyl phenyl polysiloxane, 0.1-0.3 part of platinum catalyst and 1-5 parts of adhesive are sequentially added into a stirrer and uniformly mixed to obtain the component A;
the preparation steps of the component B are as follows: 10-20 parts of methyl phenyl vinyl silicone resin, 70-80 parts of methyl phenyl hydrogen-containing silicone resin, 1-10 parts of hydrogen-containing toughening cross-linking agent and 0.1-0.3 part of inhibitor are sequentially added into a stirrer and uniformly mixed to obtain the component B;
when the packaging material is used, the component A and the component B are uniformly mixed according to the weight ratio of 5:1, vacuum defoaming is carried out for 20-40 minutes, glue is dispensed or filled on a to-be-packaged component, the to-be-packaged component is heated at 80-120 ℃ for 0.5-1.5 hours, then heated at 140-200 ℃ for 3-5 hours, and curing is carried out.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
The LED packaging silica gel with high refractive index comprises a component A and a component B, wherein the weight ratio of the component A to the component B is 5: 1;
wherein the component A comprises the following raw materials in parts by weight: 80-90 parts of methyl phenyl vinyl silicone resin, 10-20 parts of vinyl methyl phenyl polysiloxane, 1-5 parts of adhesive and 0.1-0.3 part of platinum catalyst;
the component B comprises the following raw materials in parts by weight: 10-20 parts of methyl phenyl vinyl silicone resin, 70-80 parts of methyl phenyl hydrogen-containing silicone resin, 1-10 parts of hydrogen-containing toughening cross-linking agent and 0.1-0.3 part of inhibitor.
The invention is illustrated in detail below by means of a few specific preparation process examples. (the above parts by weight are expressed in grams in the specific examples)
Example 1
Preparation of component A: weighing 80 parts of methyl phenyl vinyl silicone resin, 14.9 parts of vinyl methyl phenyl polysiloxane, 0.1 part of platinum catalyst and 5 parts of adhesive, and sequentially adding the components into a stirrer to be uniformly mixed and stirred to obtain a component A;
preparation of the component B: weighing 19.7 parts of methyl phenyl vinyl silicone resin, 70 parts of methyl phenyl hydrogen-containing silicone resin, 10 parts of hydrogen-containing toughening cross-linking agent and 0.3 part of inhibitor. Sequentially adding the mixture into a stirrer, and uniformly mixing and stirring to obtain the component B;
when in use, the component A and the component B are uniformly mixed according to the weight ratio of 5:1, vacuum defoamed for 20 minutes, dispensed or filled on a to-be-packaged piece, heated at 80 ℃ for 1 hour, and then heated at 150 ℃ for 4 hours.
Example 2
Preparation of component A: weighing 88.7 parts of methyl phenyl vinyl silicone resin, 10 parts of vinyl methyl phenyl polysiloxane, 0.3 part of platinum catalyst and 1 part of adhesive, sequentially adding into a stirrer, and uniformly mixing and stirring to obtain a component A;
preparation of the component B: weighing 19.9 parts of methyl phenyl vinyl silicone resin, 80 parts of methyl phenyl hydrogen-containing silicone resin, 1 part of hydrogen-containing toughening cross-linking agent and 0.1 part of inhibitor. Sequentially adding the mixture into a stirrer, and uniformly mixing and stirring to obtain the component B;
when in use, the component A and the component B are uniformly mixed according to the weight ratio of 5:1, vacuum defoamed for 20 minutes, and then glue is dispensed or filled on a to-be-packaged piece, and then the to-be-packaged piece is heated at 100 ℃ for 1 hour and then heated at 160 ℃ for 4 hours.
Example 3
Preparation of component A: weighing 85 parts of methyl phenyl vinyl silicone resin, 12.3 parts of vinyl methyl phenyl polysiloxane, 0.2 part of platinum catalyst and 2.5 parts of adhesive, and sequentially adding into a stirrer to be uniformly mixed and stirred to obtain a component A;
preparation of the component B: weighing 19.3 parts of methyl phenyl vinyl silicone resin, 75 parts of methyl phenyl hydrogen-containing silicone resin, 5.5 parts of hydrogen-containing toughening crosslinking agent and 0.2 part of inhibitor. Sequentially adding the mixture into a stirrer, and uniformly mixing and stirring to obtain the component B;
when in use, the component A and the component B are uniformly mixed according to the weight ratio of 5:1, vacuum defoamed for 20 minutes, dispensed or filled on a to-be-packaged piece, heated at 120 ℃ for 1 hour, and then heated at 150 ℃ for 4 hours.
Comparative example 1
Preparation of component A: weighing 85 parts of methyl phenyl vinyl silicone resin, 12.3 parts of vinyl methyl phenyl polysiloxane, 0.2 part of platinum catalyst and 2.5 parts of adhesive, and sequentially adding into a stirrer to be uniformly mixed and stirred to obtain a component A;
preparation of the component B: weighing 15 parts of methyl phenyl vinyl silicone resin, 84.8 parts of methyl phenyl hydrogen-containing silicone resin and 0.2 part of inhibitor. Sequentially adding the mixture into a stirrer, and uniformly mixing and stirring to obtain the component B;
when in use, the component A and the component B are uniformly mixed according to the weight ratio of 5:1, vacuum defoamed for 20 minutes, dispensed or filled on a to-be-packaged piece, heated at 120 ℃ for 1 hour, and then heated at 150 ℃ for 4 hours.
A, B components of examples 1, 2 and 3 and comparative example 1 are weighed according to the weight ratio of 5:1, then are uniformly mixed, and are defoamed for 30 minutes, wherein the first is that: test pieces are manufactured according to the Shore hardness test method of GB2411-1980(1989) and GB/T528-2009 plastic and the tensile test method of vulcanized rubber, thermoplastic rubber and thermoplastic synthetic rubber; secondly, the following steps: and packaging the 2835 bracket, and keeping the color temperature range between 5500 and 6000K. Curing conditions are as follows: first at 120 ℃ for 1 hour and then at 150 ℃ for 4 hours. Testing one: testing the hardness of the test piece according to a Shore hardness test method of GB2411-1980 (1989); and (2) testing: testing the tensile strength and elongation at break of the samples according to the GB/T528-2009 vulcanizate, thermoplastic rubber and thermoplastic elastomer tensile test methods; and (3) testing: 2g of sulfur powder at the bottom of the sealed glass bottle, placing a 2835 bracket which is packaged and cured at the center of the bottle, testing the luminous flux before and after 8 hours at 80 ℃, and calculating the luminous flux retention rate; and (4) testing: and (3) placing the 2835 bracket after the packaging and curing is finished into a cold-hot impact box, wherein the temperature is-40-125 ℃, the temperature is 30min/30min, 1 cycle is carried out every hour, and the lamp death rate is tested after 200 cycles.
TABLE 1 Performance index Table
As can be seen from Table 1, in examples 1, 2 and 3, compared with comparative example 1, it can be seen that although the resin content is high, the hardness, tensile strength and vulcanization resistance are improved, the elongation at break is reduced, and the cold and hot shock resistance is reduced; the addition of the hydrogen-containing toughening cross-linking agent reduces the hardness and the tensile strength, but the sulfuration resistance is basically kept unchanged, the elongation at break is improved, and the cold and heat shock resistance is improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. The high-refractive-index high-toughness vulcanization-resistant LED packaging silica gel comprises a component A and a component B, wherein the weight ratio of the component A to the component B is 5: 1;
wherein the component A comprises the following raw materials in parts by weight: 80-90 parts of methyl phenyl vinyl silicone resin, 10-20 parts of vinyl methyl phenyl polysiloxane, 1-5 parts of adhesive and 0.1-0.3 part of platinum catalyst;
the component B comprises the following raw materials, by weight, 10-20 parts of methyl phenyl vinyl silicone resin, 70-80 parts of methyl phenyl hydrogen-containing silicone resin, 1-10 parts of a hydrogen-containing toughening cross-linking agent and 0.1-0.3 part of an inhibitor;
wherein the molecular formula of the methylphenyl hydrogen-containing silicone resin is as follows: (HMe2SiO1/2)3(PhSiO3/2)4, wherein Me is methyl and Ph is phenyl;
wherein the hydrogen-containing toughening crosslinking agent is a compound containing
One of the crosslinkers of structural formula wherein Ph is phenyl.
2. The high-refractive-index high-toughness vulcanization-resistant LED packaging silica gel according to claim 1, characterized in that: the molecular formula of the methyl phenyl vinyl silicone resin is (ViMe2SiO1/2) x (PhSiO3/2) y, wherein Me is methyl, Vi is vinyl, Ph is phenyl, x: y is 1: 4-5.
3. The high-refractive-index high-toughness vulcanization-resistant LED packaging silica gel according to claim 1, characterized in that: the structural formula of the coupling agent containing epoxy groups of the adhesive is as follows:
4. the high-refractive-index high-toughness vulcanization-resistant LED packaging silica gel according to claim 1, characterized in that: further, the platinum catalyst is any one of platinum-methyl phenyl polysiloxane complex or platinum-olefin complex, wherein the platinum content is 3000-10000 ppm.
5. The high-refractive-index high-toughness vulcanization-resistant LED packaging silica gel according to claim 1, characterized in that: the inhibitor is any one of ethynyl cyclohexanol or 1,1, 3-triphenyl-2-propyne-1-ol, and the structural formula is as follows:
6. the preparation method of the high-refractive-index high-toughness vulcanization-resistant LED packaging silica gel of claim 1 comprises the steps of preparing a component A and preparing a component B; wherein, the preparation steps of the component A are as follows: 80-90 parts of methyl phenyl vinyl silicone resin, 10-20 parts of vinyl methyl phenyl polysiloxane, 0.1-0.3 part of platinum catalyst and 1-5 parts of adhesive are sequentially added into a stirrer and uniformly mixed to obtain the component A; the preparation steps of the component B are as follows: 10-20 parts of methyl phenyl vinyl silicone resin, 70-80 parts of methyl phenyl hydrogen-containing silicone resin, 1-10 parts of hydrogen-containing toughening cross-linking agent and 0.1-0.3 part of inhibitor are sequentially added into a stirrer, and the components are uniformly mixed and stirred to obtain the component B.
7. The use method of the high-refractive-index high-toughness vulcanization-resistant LED packaging silica gel disclosed by claim 1 comprises the following steps: when the packaging material is used, the component A and the component B are uniformly mixed according to the weight ratio of 5:1, vacuum defoaming is carried out for 20-40 minutes, glue is dispensed or filled on a to-be-packaged component, the to-be-packaged component is heated at 80-120 ℃ for 0.5-1.5 hours, then heated at 140-200 ℃ for 3-5 hours, and curing is carried out.
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| CN106675506A (en) * | 2016-11-13 | 2017-05-17 | 复旦大学 | Organic silicon adhesive and preparation method thereof |
| CN106784270A (en) * | 2016-11-21 | 2017-05-31 | 深圳市佑明光电有限公司 | A kind of method of the resistance to vulcanization uv-resistance energy of the organosilicon material of raising LED encapsulation |
| CN109651425B (en) * | 2017-10-12 | 2021-02-26 | 弗洛里光电材料（苏州）有限公司 | Isocyanate compound containing multiple silicon-hydrogen bonds and application thereof |
| CN107880844A (en) * | 2017-12-04 | 2018-04-06 | 东莞市贝特利新材料有限公司 | A kind of photo-thermal dual curable type organosilicon liquid Optical adhesive composition |
| CN110055027B (en) * | 2019-04-30 | 2022-01-11 | 汕头市骏码凯撒有限公司 | Middle-folding refractive index LED packaging silicone rubber material and preparation method thereof |
| CN111647385A (en) * | 2020-07-03 | 2020-09-11 | 昆明耐维科技有限公司 | Coupling adhesive for ultrasonic real-time rail breakage monitoring system and preparation method and use method thereof |
| CN112341826A (en) * | 2020-11-26 | 2021-02-09 | 广东省科学院稀有金属研究所 | High-refractive-index optical-grade silica gel film and preparation method thereof |
| WO2022141146A1 (en) * | 2020-12-30 | 2022-07-07 | 3M Innovative Properties Company | Cured silicone adhesive composition |
| CN114276778A (en) * | 2021-12-30 | 2022-04-05 | 烟台德邦科技股份有限公司 | Organic silicon adhesive for packaging LED chip |
| CN115820114B (en) * | 2022-12-26 | 2023-07-14 | 慧智科技湖北有限公司 | High-temperature-resistant cold-hot-impact-resistant coating |
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| CN102965069B (en) * | 2012-11-16 | 2016-01-27 | 烟台德邦先进硅材料有限公司 | A kind of resistance to sulfuration LED silica gel |
| CN105246945A (en) * | 2013-05-31 | 2016-01-13 | 迈图高新材料日本合同公司 | Phenyl-containing functional polysiloxanes and polycarbonate-polysiloxane copolymers made therefrom |
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