CN102965069A - Vulcanization-proof LED (light-emitting diode) packaging silica gel - Google Patents
Vulcanization-proof LED (light-emitting diode) packaging silica gel Download PDFInfo
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- CN102965069A CN102965069A CN2012104659146A CN201210465914A CN102965069A CN 102965069 A CN102965069 A CN 102965069A CN 2012104659146 A CN2012104659146 A CN 2012104659146A CN 201210465914 A CN201210465914 A CN 201210465914A CN 102965069 A CN102965069 A CN 102965069A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 28
- 239000000741 silica gel Substances 0.000 title claims abstract description 28
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 28
- -1 methyl phenyl vinyl Chemical group 0.000 claims abstract description 43
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 26
- 239000011347 resin Substances 0.000 claims abstract description 25
- 229920005989 resin Polymers 0.000 claims abstract description 25
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 19
- 229920002545 silicone oil Polymers 0.000 claims abstract description 18
- 239000000853 adhesive Substances 0.000 claims abstract description 16
- 230000001070 adhesive effect Effects 0.000 claims abstract description 16
- 238000004073 vulcanization Methods 0.000 claims abstract description 15
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 239000003112 inhibitor Substances 0.000 claims abstract description 13
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 125000000524 functional group Chemical group 0.000 claims abstract description 4
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 6
- 239000011593 sulfur Substances 0.000 claims description 6
- 229910004674 SiO0.5 Inorganic materials 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 229920001843 polymethylhydrosiloxane Polymers 0.000 claims description 3
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O[Si](C)(C=C)O1 VMAWODUEPLAHOE-UHFFFAOYSA-N 0.000 claims description 2
- 239000004593 Epoxy Substances 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 2
- 239000012964 benzotriazole Substances 0.000 claims description 2
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- 229920002379 silicone rubber Polymers 0.000 claims 2
- 239000004945 silicone rubber Substances 0.000 claims 2
- 229920001296 polysiloxane Polymers 0.000 claims 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract description 8
- 238000004132 cross linking Methods 0.000 abstract description 7
- 239000011521 glass Substances 0.000 abstract description 4
- 238000002834 transmittance Methods 0.000 abstract description 4
- 239000012790 adhesive layer Substances 0.000 abstract description 3
- 229910052709 silver Inorganic materials 0.000 abstract description 3
- 239000004332 silver Substances 0.000 abstract description 3
- DLNKOYKMWOXYQA-APPZFPTMSA-N phenylpropanolamine Chemical compound C[C@@H](N)[C@H](O)C1=CC=CC=C1 DLNKOYKMWOXYQA-APPZFPTMSA-N 0.000 abstract 2
- 239000007767 bonding agent Substances 0.000 abstract 1
- DLNKOYKMWOXYQA-UHFFFAOYSA-N dl-pseudophenylpropanolamine Natural products CC(N)C(O)C1=CC=CC=C1 DLNKOYKMWOXYQA-UHFFFAOYSA-N 0.000 abstract 1
- 229960000395 phenylpropanolamine Drugs 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 13
- 238000003756 stirring Methods 0.000 description 11
- 238000005303 weighing Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 5
- 239000003822 epoxy resin Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229920000647 polyepoxide Polymers 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000005022 packaging material Substances 0.000 description 4
- 239000002210 silicon-based material Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 229910052946 acanthite Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate 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
- 238000005987 sulfurization reaction Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to an LED (light-emitting diode) packaging silica gel, and in particular relates to a vulcanization-proof LED packaging silica gel, belonging to the technical field of adhesives. The vulcanization-proof 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 1: 1; the component A comprises raw materials based on parts by weight: 50-60 parts of methyl phenyl vinyl silicone oil, 30-60 parts of methyl vinyl MQ resin, 0.1-0.3 part of platinum catalyst and 3-5 parts of bonding agent; and the component B comprises raw materials based on parts by weight: 40-50 parts of methyl phenyl vinyl silicone oil, 30-50 parts of methyl vinyl MQ resin, 5-15 parts of cross-linking agent and 0.1-0.3 part of inhibitor. The vulcanization-proof LED packaging silica gel has excellent adhesive force for silver, phenyl-propanolamine (PPA), glass and the like, and has the light transmittance of more than 98%; and phenyl-containing functional groups and branched chain type vinyl are introduced into the LED packaging silica gel, and the dosage of the vinyl MQ resin is increased, so that the crosslinking density and the curing handness are improved, and therefore, the vulcanization resistance of a packaging adhesive layer can be improved.
Description
Technical Field
The invention relates to an LED packaging silica gel, in particular to a vulcanization-resistant LED packaging silica gel, belonging to the technical field of adhesives.
Background
The currently used packaging materials of the LED comprise epoxy resin, polymethyl methacrylate, glass, organic silicon and other high-transparency materials, wherein the epoxy resin and the organic silicon material are used as main packaging materials, the epoxy resin has overlarge internal stress, is yellowed, has poor high and low temperature resistance and poor aging resistance, while the current organic silicon material has small internal stress, good high and low temperature resistance, is not yellowed and has higher light transmittance than the epoxy resin, so the epoxy resin is rapidly replaced and is widely used in the field of LED packaging, but the organic silicon material, particularly the low-refractive-index organic silicon material, has low cross-linking density due to the use of long-chain terminal vinyl polydimethylsiloxane, has long molecular chain length and low vinyl content, leads to good air permeability of an adhesive layer, can partially penetrate through the silicon packaging material under the action of sulfur-containing gas, reacts with a silver layer at a silicon interface to generate silver sulfide, and leads to blackening of, the light attenuation increases rapidly.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an LED packaging silica gel, in particular to an LED packaging silica gel with sulfuration resistance.
The technical scheme for solving the technical problems is as follows: the 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 1: 1; wherein,
the component A comprises the following raw materials in parts by weight: 50-60 parts of methyl phenyl vinyl silicone oil, 30-60 parts of methyl vinyl MQ resin, 0.1-0.3 part of platinum catalyst and 3-5 parts of adhesive;
the component B comprises the following raw materials in parts by weight: 40-50 parts of methyl phenyl vinyl silicone oil, 30-50 parts of methyl vinyl MQ resin, 5-15 parts of a cross-linking agent and 0.1-0.3 part of an inhibitor.
The invention has the beneficial effects that: the LED packaging silica gel is composed of A, B components, wherein A component provides phenyl, polyfunctional vinyl and adhesive in reaction, B component provides phenyl, polyfunctional vinyl and cross-linking agent, the LED packaging silica gel has excellent adhesive force to silver, PPA, glass and the like, the light transmittance exceeds 98%, and the vulcanization resistance of the packaging adhesive layer is improved because phenyl-containing functional groups, branched vinyl and the use amount of vinyl MQ resin are introduced, the cross-linking density and the curing hardness are improved.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the viscosity of the methyl phenyl vinyl silicone oil is 1000-20000 centipoises, and the structural formula is as follows:
wherein Me is methyl, Vi is vinyl, n1=20～50，n2=25～55，n3＝10～30
The beneficial effect of adopting the further scheme is that: compared with vinyl-terminated polydisiloxane, the vinyl-terminated polydisiloxane as matrix resin contains partial phenyl, does not influence the compatibility with other low-refractive-index raw materials, reduces the air permeability of the silica gel material after introducing phenyl for curing, improves the crosslinking density because the terminal group and the side group both contain vinyl, and can adjust different viscosities.
Further, the structural formula of the methyl vinyl MQ resin is as follows: (Me)3SiO0.5)a(ViMe2SiO0.5)b(SiO2) Wherein Me is methyl, Vi is vinyl, and a = 06-0.8 and b = 0.1-0.2.
The beneficial effect of adopting the further scheme is that: the addition of the methyl vinyl MQ resin improves the crosslinking density and strength of the whole silica gel and reduces the air permeability of the silica gel.
Furthermore, the molar mass of the vinyl in the methyl vinyl MQ resin accounts for 3-5%.
Further, the adhesive contains epoxy functional groups, and the structural formula of the adhesive is as follows:
structural formula I;
or,
structural formula II
Further, the cross-linking agent is polymethylhydrosiloxane.
Further, the platinum catalyst is any one of alcohol solution of chloroplatinic acid, platinum-vinyl siloxane complex and platinum-olefin complex.
Further, the platinum-based catalyst is preferably a platinum-vinyl siloxane complex, and the mass content of platinum is 3000-7000 ppm.
Further, the inhibitor is any one of ethynylcyclohexanol, tetramethyltetravinylcyclotetrasiloxane or benzotriazole.
Further, the inhibitor is selected from ethynyl cyclohexanol.
The preparation method of the vulcanization-resistant LED packaging silica gel comprises the steps of preparing the component A and preparing the component B; wherein the preparation steps of the component A are as follows: sequentially adding 50-60 parts by weight of methyl phenyl vinyl silicone oil, 30-60 parts by weight of methyl vinyl MQ resin, 0.1-0.3 part by weight of catalyst and 3-5 parts by weight of adhesive into a stirrer, and uniformly mixing and stirring to obtain a component A;
the preparation steps of the component B are as follows: 40-50 parts of methyl phenyl vinyl silicone oil, 30-50 parts of methyl vinyl MQ resin, 5-15 parts of a cross-linking agent and 0.1-0.3 part of an inhibitor are sequentially added into a stirrer, and the mixture is uniformly mixed and stirred 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 1:1, 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 80-100 ℃ for 0.5-1.5 hours, then heated at 100-200 ℃ for 1.5-4 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.
Example 1
Preparation of component A: weighing 50g of methyl phenyl vinyl silicone oil, 44.9g of methyl vinyl MQ resin, 5g of adhesive (namely the structural formula I), and 0.1g of catalyst platinum-vinyl siloxane complex, wherein the mass content of platinum is 7000ppm, sequentially adding the materials into a stirrer, and uniformly mixing and stirring to obtain the component A;
preparation of the component B: weighing 50g of methyl phenyl vinyl silicone oil, 34.8g of methyl vinyl MQ resin, 15g of cross-linking agent polymethyl hydrogen siloxane and 0.2g of inhibitor ethynyl cyclohexanol, sequentially adding 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 1:1, 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 90 ℃ for 1 hour and then heated at 150 ℃ for 3 hours.
Example 2
Preparation of component A: weighing 60g of methyl phenyl vinyl silicone oil, 36.7g of methyl vinyl MQ resin, 3g of adhesive (namely the structural formula II), and 0.3g of catalyst platinum-vinyl siloxane complex, wherein the mass content of platinum is 7000ppm, sequentially adding the materials into a stirrer, and uniformly mixing and stirring to obtain the component A;
preparation of the component B: weighing 40g of methyl phenyl vinyl silicone oil, 50g of methyl vinyl MQ resin, 9.8g of cross-linking agent polymethyl hydrogen siloxane and 0.2g of inhibitor ethynyl cyclohexanol, sequentially adding 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 1:1, vacuum defoamed for 20 minutes, dispensed or filled on a to-be-packaged piece, heated at 90 ℃ for 1 hour, and then heated at 150 ℃ for 3 hours.
Example 3
Preparation of component A: weighing 53.9g of methyl phenyl vinyl silicone oil, 42g of methyl vinyl MQ resin, 4g of adhesive (structural formula I) and 0.1g of catalyst platinum-vinyl siloxane complex, wherein the mass content of platinum is 5000ppm, sequentially adding the materials into a stirrer, and uniformly mixing and stirring to obtain a component A;
preparation of the component B: weighing 45g of methyl phenyl vinyl silicone oil, 41g of methyl vinyl MQ resin, 13.8g of cross-linking agent polymethyl hydrogen siloxane and 0.2g of inhibitor ethynyl cyclohexanol, sequentially adding the components 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 1:1, vacuum defoamed for 20 minutes, dispensed or filled on a to-be-packaged piece, heated at 90 ℃ for 1 hour, and then heated at 150 ℃ for 3 hours.
Comparative example 1
Preparation of component A: weighing 50g of vinyl-terminated polydisiloxane, 44.9g of methyl vinyl MQ resin, 5g of adhesive (structural formula I), 0.1g of catalyst platinum-vinyl siloxane complex and 7000ppm of platinum mass content, sequentially adding into a stirrer, and uniformly mixing and stirring to obtain the component A;
preparation of the component B: weighing 50g of vinyl-terminated polydisiloxane, 34.8g of methyl vinyl MQ resin, 15g of cross-linking agent polymethyl hydrogen siloxane and 0.2g of inhibitor ethynyl cyclohexanol, sequentially adding 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 1:1, vacuum defoamed for 20 minutes, dispensed or filled on a to-be-packaged piece, heated at 90 ℃ for 1 hour, and then heated at 150 ℃ for 3 hours.
Comparative example 2
Preparation of component A: weighing 98.8g of vinyl-terminated polydisiloxane, 2g of adhesive (structural formula II), 0.2g of catalyst platinum-vinyl siloxane complex and 5000ppm of platinum by mass, sequentially adding into a stirrer, and uniformly mixing and stirring to obtain the component A;
preparation of the component B: weighing 89.8g of vinyl polydisiloxane, 10g of cross-linking agent polymethylhydrosiloxane and 0.2g of inhibitor ethynylcyclohexanol, 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 1:1, vacuum defoamed for 20 minutes, dispensed or filled on a to-be-packaged piece, heated at 90 ℃ for 1 hour, and then heated at 150 ℃ for 3 hours.
A, B components of examples 1, 2 and 3 and comparative examples 1 and 2 are weighed according to the weight ratio of 1:1, then uniformly mixed, and defoamed for 30 minutes, wherein firstly, the mixture is dispensed on a processed 3528LED bracket; secondly, respectively manufacturing sheets according to the GB/T528-2009 requirements, and leveling the mixture in a mold. Curing conditions are as follows: first heated at 90 ℃ for 1 hour and then at 150 ℃ for 3 hours. Testing one: carrying out light transmittance test on the cured sample; and (2) testing: carrying out a vulcanization light decay experiment on a sample of the LED chip (3528) after curing and packaging the silica gel, placing the sample in a 100ml sealed glass bottle, placing 0.2g of powdered sulfur in the bottle, placing the bottle for 24 hours under a sealed condition at 60 ℃, and testing light decay by using an LED light decay tester; and (3) testing: manufacturing a dumbbell-shaped silica gel sample according to the GB/T528-2009 requirement, and testing the tensile strength by using a tensile machine; and (4) testing: and testing the hardness of the cured silica gel by using a Shore A durometer according to GB/T2411-2008.
TABLE 1 Performance index Table
As can be seen from Table 1, when example 1 is compared with comparative example 1, it can be seen that the cross-linking density of the phenyl-containing branched vinyl silicone oil is increased after curing compared with vinyl terminated polydisiloxane, so that the hardness and strength are obviously increased; the examples 1, 2 and 3 are added with the phenyl branched vinyl silicone oil and the methyl vinyl MQ resin, compared with the comparative examples 1 and 2, the crosslinking density is increased, the hardness and the strength are high, the light decay is obviously reduced after a vulcanization test, and the requirements of customers on vulcanization are met
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 (10)
1. The vulcanization-resistant LED packaging silica gel is characterized by comprising a component A and a component B, wherein the weight ratio of the component A to the component B is 1: 1; wherein,
the component A comprises the following raw materials in parts by weight: 50-60 parts of methyl phenyl vinyl silicone oil, 30-60 parts of methyl vinyl MQ resin, 0.1-0.3 part of platinum catalyst and 3-5 parts of adhesive;
the component B comprises the following raw materials in parts by weight: 40-50 parts of methyl phenyl vinyl silicone oil, 30-50 parts of methyl vinyl MQ resin, 5-15 parts of a cross-linking agent and 0.1-0.3 part of an inhibitor.
2. The vulcanization-resistant LED packaging silica gel according to claim 1, wherein the methyl phenyl vinyl silicone oil has a viscosity of 1000 to 20000 centipoise, and has a structural formula:
wherein Me is methyl, Vi is vinyl, n1=20～50，n2=25～55，n3＝10～30。
3. The sulfur-resistant LED encapsulating silica gel of claim 1, wherein the methyl vinyl MQ resin has the structural formula: (Me)3SiO0.5)a(ViMe2SiO0.5)b(SiO2) Wherein Me is methyl, Vi is vinyl, and a = 06-0.8 and b = 0.1-0.2.
4. The vulcanization-resistant LED packaging silicone rubber according to claim 1 or 3, wherein the methyl vinyl MQ resin has a vinyl content of 3-5% by mass.
5. The sulfur-resistant LED packaging silicone according to claim 1, wherein the adhesive contains epoxy functional groups and has the formula:
or
6. The vulcanization-resistant LED packaging silicone rubber according to claim 1, wherein the crosslinking agent is polymethylhydrosiloxane.
7. The vulcanization-resistant LED packaging silica gel of claim 1, wherein the platinum-based catalyst is any one of an alcohol solution of chloroplatinic acid, a platinum-vinylsiloxane complex, and a platinum-olefin complex.
8. The vulcanization-resistant LED packaging silica gel according to claim 1 or 7, wherein the platinum-based catalyst is preferably a platinum-vinylsiloxane complex, and the mass content of platinum is 3000 to 7000 ppm.
9. The sulfur-resistant LED packaging silica gel of claim 1, wherein the inhibitor is any one of ethynylcyclohexanol, tetramethyltetravinylcyclotetrasiloxane, or benzotriazole.
10. The vulcanization-resistant LED packaging silica gel of claim 1 or 9, wherein the inhibitor is ethynylcyclohexanol.
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