CN108300408B - Organic silicon material for packaging LED with high luminous flux maintenance rate - Google Patents
Organic silicon material for packaging LED with high luminous flux maintenance rate Download PDFInfo
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- CN108300408B CN108300408B CN201711396294.4A CN201711396294A CN108300408B CN 108300408 B CN108300408 B CN 108300408B CN 201711396294 A CN201711396294 A CN 201711396294A CN 108300408 B CN108300408 B CN 108300408B
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- 230000004907 flux Effects 0.000 title claims abstract description 26
- 239000002210 silicon-based material Substances 0.000 title claims abstract description 20
- 238000012423 maintenance Methods 0.000 title claims abstract description 18
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 18
- -1 polymethylphenylsiloxane Polymers 0.000 claims abstract description 44
- 239000000203 mixture Substances 0.000 claims abstract description 41
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 39
- 239000010703 silicon Substances 0.000 claims abstract description 39
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 32
- 229920005989 resin Polymers 0.000 claims abstract description 27
- 239000011347 resin Substances 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 26
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000499 gel Substances 0.000 claims abstract description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 17
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 17
- 239000000741 silica gel Substances 0.000 claims abstract description 17
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 17
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 16
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 15
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 15
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229920001843 polymethylhydrosiloxane Polymers 0.000 claims abstract description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 8
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 7
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 7
- 229920001921 poly-methyl-phenyl-siloxane Polymers 0.000 claims abstract description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 66
- 238000006243 chemical reaction Methods 0.000 claims description 46
- 229920000734 polysilsesquioxane polymer Polymers 0.000 claims description 44
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 42
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 35
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 30
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims description 21
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 20
- 239000012044 organic layer Substances 0.000 claims description 18
- 238000004821 distillation Methods 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 0.000 claims description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical class [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 9
- DQEUYIQDSMINEY-UHFFFAOYSA-M magnesium;prop-1-ene;bromide Chemical compound [Mg+2].[Br-].[CH2-]C=C DQEUYIQDSMINEY-UHFFFAOYSA-M 0.000 claims description 9
- 230000007935 neutral effect Effects 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 8
- 238000010898 silica gel chromatography Methods 0.000 claims description 8
- HKILWKSIMZSWQX-UHFFFAOYSA-N tris(prop-2-enyl)silane Chemical compound C=CC[SiH](CC=C)CC=C HKILWKSIMZSWQX-UHFFFAOYSA-N 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000292 calcium oxide Substances 0.000 claims description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 5
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000178 monomer Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims description 4
- 239000005052 trichlorosilane Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
- WRECIMRULFAWHA-UHFFFAOYSA-N trimethyl borate Chemical compound COB(OC)OC WRECIMRULFAWHA-UHFFFAOYSA-N 0.000 claims description 3
- OBAJXDYVZBHCGT-UHFFFAOYSA-N tris(pentafluorophenyl)borane Chemical compound FC1=C(F)C(F)=C(F)C(F)=C1B(C=1C(=C(F)C(F)=C(F)C=1F)F)C1=C(F)C(F)=C(F)C(F)=C1F OBAJXDYVZBHCGT-UHFFFAOYSA-N 0.000 claims description 3
- 229920002050 silicone resin Polymers 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims 9
- 229920002379 silicone rubber Polymers 0.000 claims 2
- 239000004945 silicone rubber Substances 0.000 claims 2
- GQEZCXVZFLOKMC-UHFFFAOYSA-N n-alpha-hexadecene Natural products CCCCCCCCCCCCCCC=C GQEZCXVZFLOKMC-UHFFFAOYSA-N 0.000 claims 1
- 238000004383 yellowing Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000002834 transmittance Methods 0.000 description 9
- 239000005022 packaging material Substances 0.000 description 5
- 238000006459 hydrosilylation reaction Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 229920000587 hyperbranched polymer Polymers 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000008393 encapsulating agent Substances 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 229920003216 poly(methylphenylsiloxane) Polymers 0.000 description 1
- 229920013636 polyphenyl ether polymer Polymers 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052990 silicon hydride Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 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
- 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
- C09J11/04—Non-macromolecular additives inorganic
-
- 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
- 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
- C09J11/08—Macromolecular additives
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Silicon Polymers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses an organic silicon material for packaging an LED (light-emitting diode) with high luminous flux maintenance rate, which comprises an organic silicon gel A component, an organic silicon gel B component, nano magnesium oxide, fluorescent powder and an acrylic polymer; wherein the organic silica gel A component comprises the following components: 60-85 parts of polymethylphenylsiloxane with vinyl as a terminal group, 5-15 parts of polydimethylsiloxane with vinyl as a terminal group, 3-8 parts of active organic borosilicate tackifier, 10-25 parts of vinyl-terminated hyperbranched organic silicon resin and 0.05-0.5 part of platinum catalyst; the composition of the organic silica gel B is as follows: 35-45 parts of polymethylphenyl vinyl siloxane with vinyl as a terminal group, 45-55 parts of polymethylhydrosiloxane, 5-15 parts of MQ resin and 5-1723-8 parts of silane coupling agent; the organic silicon material comprises an organic silicon gel A component, an organic silicon gel B component, nano magnesium oxide, fluorescent powder and an acrylic polymer in a mass ratio of 100:100:2.5-18:3-8: 1-3. The invention has the following beneficial effects: (1) resisting cold and hot alternation of the environment; (2) no yellowing; (3) high luminous flux.
Description
Technical Field
The invention relates to an LED packaging material, in particular to an organic silicon material for packaging an LED with high luminous flux maintenance rate.
Background
The LED, namely the light emitting diode, is a high-efficiency solid light source, has the advantages of energy conservation and environmental protection, and has longer service life. Currently, LEDs are widely used in daily life and work of people, and the application principle is that a blue LED is used to irradiate a fluorescent substance to generate yellow light complementary to blue light, so as to obtain white light.
The star standard of energy requires that the light flux maintenance rate of an LED lamp with a lifetime of 25000 hours is 91.8% at 6000 hours, and has quite high standard requirements if the lamp type is a directional lamp and the highest test environment temperature reaches 55 +/-5 ℃.
For example, a packaging material for LED filament disclosed in chinese patent document, whose application publication No. CN 105542693A, includes red phosphor and a crosslinking agent mixed therewith; the cross-linking agent is prepared from the following raw materials in parts by weight: 72 parts of epoxy resin, 18-22 parts of polyphenyl ether powder, 4 parts of methyl phenyl silicone oil, 0.2-0.4 part of nano zinc sulfide, 6-8 parts of nano ceramic powder transparent liquid with the mass concentration of 30-40%, 4-5 parts of nano titanium dioxide, 0.1-0.2 part of benzoyl peroxide, 0.4-0.5 part of maleic anhydride, 0.1-0.2 part of silane coupling agent, 0.01-0.02 part of chloroform antioxidant and 20-25 parts of curing agent. The invention overcomes the technical defects of small emergence angle and low light emergence rate in the prior art, and provides the packaging material for improving the transmissivity and the luminous intensity. However, the LED lamp has many disadvantages, such as that the main material used in the formulation is epoxy resin, the texture is often brittle, the LED lamp may be cracked during the cold and hot alternation, and yellowing may occur during the use process, which is reflected in the luminous efficiency and luminous flux of the final LED lamp.
Disclosure of Invention
The invention provides an organic silicon material for LED packaging with high luminous flux maintenance rate, which can resist cold and hot alternation of environment, can not be yellowed and has high luminous flux, and aims to solve the problems that a packaging material in the prior art cannot resist cold and hot alternation, can possibly have yellowing possibility and has low luminous flux.
In order to achieve the purpose, the invention adopts the following technical scheme:
an organic silicon material for packaging an LED with high luminous flux maintenance rate comprises an organic silicon gel A component, an organic silicon gel B component, nano magnesium oxide, fluorescent powder and an acrylic polymer;
the organic silica gel A component comprises the following components: 60-85 parts of polymethylphenylsiloxane with vinyl as a terminal group, 5-15 parts of polydimethylsiloxane with vinyl as a terminal group, 3-8 parts of active organic borosilicate tackifier, 10-25 parts of vinyl-terminated hyperbranched organic silicon resin and 0.05-0.5 part of platinum catalyst;
the organosilicon B component comprises the following components: 35-45 parts of polymethylphenyl vinyl siloxane with vinyl as a terminal group, 45-55 parts of polymethylhydrosiloxane, 5-15 parts of MQ resin and A-172 parts of silane coupling agent;
the organic silicon material comprises an organic silicon component A, an organic silicon component B, nano magnesium oxide, fluorescent powder and an acrylic polymer in a mass part ratio of 100:100:2.5-18:3-8: 1-3.
The main material used in the invention is an organosilicon material, and the vinyl-containing component and the hydrosilation component in the organosilicon AB adhesive are subjected to hydrosilylation reaction under the action of a platinum catalyst, so that the organosilicon AB adhesive is cured into a whole, and the viscosity and the form of the whole resin can be effectively adjusted by adding the active organic borosilicate tackifier and the vinyl-terminated hyperbranched organosilicon resin, so that the organosilicon adhesive is suitable for the requirement of encapsulation, and meanwhile, the active groups are increased, so that more connection points are formed for curing, and the requirement of the encapsulating material on the mechanical property is met. The light flux of the packaging material can be effectively increased by adding the nano magnesium oxide component into the material. The addition of the acrylic polymer can reduce the light transmittance of the LED lamp beads by 5-10%, and the acrylic polymer gradually changes from milky color to colorless in the 6000-hour lighting process, so that the light extraction rate is gradually improved by 5-10%. The compensation maintains the stability of the luminous flux due to the decrease of the luminous flux during lighting.
Preferably, the preparation method of the active organic borosilicate adhesion promoter comprises the following steps: under the protection of nitrogen, 100 parts of polymethylhydrosiloxane, 100 parts of toluene and 0.02 part of tris (pentafluorophenyl) borane are uniformly stirred, then a solution of 15 parts of hydroxyethyl acrylate dissolved in 10 parts of toluene is dropwise added, the temperature is controlled to 30 ℃ after the dropwise addition is finished, the reaction is carried out for 30 minutes, then a solution of 4 parts of trimethyl borate dissolved in 10 parts of toluene is dropwise added, the temperature is raised to 50 ℃ and the reaction is continued for 2 hours, the temperature is lowered to room temperature, 2 parts of active carbon is added, the stirring adsorption is carried out for 0.5 hour, then the filtrate is filtered, and the toluene and low-boiling-point substances are evaporated under reduced pressure to obtain the active organic borosilicate tackifier.
The addition of the reactive organo-borosilicate tackifier enables the viscosity of the overall encapsulant to be adjusted so that it is suitable as an encapsulant. In addition, the acrylic acid structure is also contained, so that hydrosilylation reaction can be easily carried out with silicon hydride, reaction connection points are increased, and the mechanical strength of the acrylic acid structure is increased.
Preferably, the preparation method of the terminal vinyl hyperbranched silicone resin is as follows:
(a) preparation of monomers: under the protection of nitrogen and at the temperature of minus 20 ℃, adding 10 parts of trichlorosilane and 100 parts of dry ether in parts by mass into a reaction kettle, dropwise adding 200 parts of 1.0 mol/L allyl magnesium bromide ether solution 190-one while stirring, continuing to react for 30 minutes after dropwise adding, then heating to 20 ℃, continuing to react for 1.5 to 3 hours, stopping the reaction, adding 100ml of 1mol/L diluted hydrochloric acid into the mixture, stirring for 30 minutes, standing, separating liquid, taking an upper organic layer, washing the upper organic layer to be neutral by saturated sodium carbonate solution, and finally obtaining pure triallylsilane by carrying out reduced pressure distillation and silica gel column chromatography on the product;
(b) and (b) under the protection of nitrogen, adding 100 parts of triallyl silane obtained in the step (a), 150 parts of toluene and 0.1-0.5 part of Kaster catalyst containing 2% of platinum into a reaction kettle, uniformly stirring, raising the temperature to 90 ℃, reacting for 4-8 hours, carrying out reduced pressure distillation, and removing toluene and oligomer to obtain the vinyl-terminated hyperbranched organic silicon resin.
The hyperbranched polymer is a tree-shaped macromolecule with a highly branched three-dimensional structure, contains a large amount of terminal groups capable of being modified, and has the advantages of less intermolecular entanglement, good solubility, low viscosity, easy film formation, high reaction activity and the like. The vinyl-terminated hyperbranched organic silicon resin is used as one of hyperbranched polymers, not only has all properties of the hyperbranched polymers, but also has high reaction activity because the outer end of the structure contains a large amount of vinyl, and can well participate in hydrosilylation reaction.
Preferably, the organosilicon material also contains hexadecyl vinyl polysilsesquioxane.
Preferably, the preparation method of the hexadecyl vinyl polysilsesquioxane is as follows:
1) under the protection of nitrogen, dissolving 60 parts by weight of tetramethylammonium hydroxide and 10 parts by weight of calcium oxide in 80 parts by weight of methanol, adding the mixture into a reaction kettle, dropwise adding a solution of 20 parts by weight of vinyltrimethoxysilane in 60 parts by weight of methanol, stirring at normal temperature for reaction for 12-18 hours, raising the temperature to reflux, continuing the reaction for 24 hours, and carrying out reduced pressure distillation to obtain white powder, wherein the white powder is respectively washed by water and boiling n-hexane for 3 times to obtain octavinyl polysilsesquioxane;
2) taking 50 parts by mass of the octavinyl polysilsesquioxane, 100 parts by mass of tetrahydrofuran, 80-85 parts by mass of methyldimethoxysilane and 0.5 part by mass of Karster catalyst containing 2% of platinum in the step 1), stirring and reacting for 24 hours at a reflux temperature, adding 2 parts by mass of activated carbon after the reaction is finished, and stirring for 30 minutes. Filtering to obtain filtrate, and distilling under reduced pressure to remove tetrahydrofuran and unreacted methyldimethoxysilane to obtain polysilsesquioxane containing 16 methoxyl groups;
3) under the protection of nitrogen, 15 parts by weight of polysilsesquioxane containing 16 methoxyl groups in the step 2) is dissolved in 100 parts of tetrahydrofuran, 180ml of 1.0 mol/L allyl magnesium bromide ethyl ether solution is dropwise added into the tetrahydrofuran while stirring, the mixture reacts for 2 hours at 30 ℃, then the temperature is raised to 50 ℃, the reaction is stopped after the mixture continues to react for 30 minutes, 100ml of 1mol/L diluted hydrochloric acid is added into the mixture, the mixture is stirred for 30 minutes, the mixture is kept still and separated to obtain an upper organic layer, the upper organic layer is washed by saturated sodium carbonate solution until the mixture is neutral, and the product is subjected to reduced pressure distillation and silica gel column chromatography to obtain pure hexadecyl polysilsesquioxane.
Preferably, the organic silicon material contains 100:100:3 of the organic silicon gel component A, the organic silicon gel component B and the hexadecyl vinyl polysilsesquioxane.
The polysilsesquioxane is a unique cage-shaped structure organic silicon compound, and the structure of the polysilsesquioxane contains a rigid silica cage-shaped structure, so that the heat resistance and the mechanical property of molecules of the polysilsesquioxane are very excellent, the heat resistance and the mechanical property of the material can be effectively enhanced by adding the polysilsesquioxane into an encapsulating material, in addition, the refractive index of the material can be improved by adding the polysilsesquioxane into the encapsulating material, and the luminous efficiency of an LED lamp is facilitated.
Preferably, the organosilicon material is prepared from the components according to a formula, then is packaged by a dispenser, and then is baked and cured at 85-105 ℃.
Therefore, the invention has the following beneficial effects: (1) resisting cold and hot alternation of the environment; (2) no yellowing; (3) high luminous flux.
Detailed Description
The technical solution of the present invention is further described below by means of specific examples.
In the examples of the present invention, the raw materials used are those commonly used in the art, and the methods used in the examples are those conventional in the art, unless otherwise specified.
Example 1
An organic silicon material for packaging an LED with high luminous flux maintenance rate comprises an organic silicon gel A component, an organic silicon gel B component, nano magnesium oxide, fluorescent powder and an acrylic polymer;
the organic silica gel A component comprises the following components: 60 parts of polymethylphenylsiloxane with vinyl as a terminal group, 5 parts of polydimethylsiloxane with vinyl as a terminal group, 3 parts of active organic borosilicate tackifier, 10 parts of vinyl-terminated hyperbranched organic silicon resin and 0.05 part of platinum catalyst;
the organosilicon B component comprises the following components: 35 parts of polymethylphenyl vinyl siloxane with vinyl as a terminal group, 45 parts of polymethylhydrosiloxane, 5 parts of MQ resin and A-1723 parts of silane coupling agent;
in the organic silicon material, the mass part ratio of the organic silica gel A component to the organic silica gel B component to the nano magnesium oxide to the fluorescent powder to the acrylic polymer is 100:100:2.5:3: 1.
The organosilicon material is prepared from the components according to a formula, packaged by a dispenser, and then baked and cured at 85 ℃.
And then, carrying out a light transmittance test on the packaged LED lamp at 55 ℃, wherein the light transmittance is 95.6% and the refractive index is 1.52 after 6000 hours.
Example 2
An organic silicon material for packaging an LED with high luminous flux maintenance rate comprises an organic silicon gel component A, an organic silicon gel component B, hexadecyl vinyl polysilsesquioxane, nano magnesium oxide, fluorescent powder and an acrylic polymer;
the organic silica gel A component comprises the following components: 85 parts of polymethylphenylsiloxane with vinyl as a terminal group, 15 parts of polydimethylsiloxane with vinyl as a terminal group, 8 parts of active organic borosilicate tackifier, 25 parts of vinyl-terminated hyperbranched organic silicon resin and 0.5 part of platinum catalyst;
the organosilicon B component comprises the following components: 45 parts of polymethylphenyl vinyl siloxane with vinyl as a terminal group, 55 parts of polymethylhydrosiloxane, 15 parts of MQ resin and A-1728 parts of silane coupling agent;
in the organic silicon material, the mass part ratio of the organic silica gel A component, the organic silica gel B component, the hexadecyl vinyl polysilsesquioxane, the nano magnesium oxide, the fluorescent powder and the acrylic polymer is 100:100:3: 18: 8: 3.
The organosilicon material is prepared from the components according to a formula, packaged by a dispenser, and then baked and cured at 100 ℃.
And then, carrying out a light transmittance test on the packaged LED lamp at 55 ℃, wherein the light transmittance is 96.2% and the refractive index is 1.56 after 6000 hours.
Example 3
An organic silicon material for packaging an LED with high luminous flux maintenance rate comprises an organic silicon gel component A, an organic silicon gel component B, hexadecyl vinyl polysilsesquioxane, nano magnesium oxide, fluorescent powder and an acrylic polymer;
the organic silica gel A component comprises the following components: 75 parts of polymethylphenylsiloxane with vinyl as a terminal group, 8 parts of polydimethylsiloxane with vinyl as a terminal group, 5 parts of active organic borosilicate tackifier, 18 parts of vinyl-terminated hyperbranched organic silicon resin and 0.2 part of platinum catalyst;
the organosilicon B component comprises the following components: 40 parts of polymethylphenyl vinyl siloxane with vinyl as a terminal group, 50 parts of polymethylhydrosiloxane, 8 parts of MQ resin and A-1725 parts of silane coupling agent;
in the organic silicon material, the mass part ratio of the organic silica gel A component, the organic silica gel B component, the hexadecyl vinyl polysilsesquioxane, the nano magnesium oxide, the fluorescent powder and the acrylic polymer is 100:100:3:10:5: 2.
The organosilicon material is prepared from the components according to a formula, packaged by a dispenser, and then baked and cured at 105 ℃.
And then, carrying out a light transmittance test on the packaged LED lamp at 55 ℃, wherein the light transmittance is 95.9% and the refractive index is 1.55 after 6000 hours.
Example 4
An organic silicon material for packaging an LED with high luminous flux maintenance rate comprises an organic silicon gel component A, an organic silicon gel component B, hexadecyl vinyl polysilsesquioxane, nano magnesium oxide, fluorescent powder and an acrylic polymer;
the organic silica gel A component comprises the following components: 65 parts of polymethylphenylsiloxane with vinyl as a terminal group, 12 parts of polydimethylsiloxane with vinyl as a terminal group, 4 parts of active organic borosilicate tackifier, 20 parts of vinyl-terminated hyperbranched organosilicon resin and 0.4 part of platinum catalyst;
the organosilicon B component comprises the following components: 40 parts of polymethylphenyl vinyl siloxane with vinyl as a terminal group, 42 parts of polymethylhydrosiloxane, 13 parts of MQ resin and A-1727 parts of silane coupling agent;
in the organic silicon material, the mass part ratio of the organic silica gel A component, the organic silica gel B component, the hexadecyl vinyl polysilsesquioxane, the nano magnesium oxide, the fluorescent powder and the acrylic polymer is 100:100:3:12:7: 1.
The organosilicon material is prepared from the components according to a formula, packaged by a dispenser, and then baked and cured at 95 ℃.
And then, carrying out a light transmittance test on the packaged LED lamp at 55 ℃, wherein the light transmittance is 95.1% and the refractive index is 1.59 after 6000 hours.
Example 5
The preparation method of the active organic borosilicate tackifier comprises the following steps: under the protection of nitrogen, 100 parts of polymethylhydrosiloxane, 100 parts of toluene and 0.02 part of tris (pentafluorophenyl) borane are uniformly stirred, then a solution of 15 parts of hydroxyethyl acrylate dissolved in 10 parts of toluene is dropwise added, the temperature is controlled to 30 ℃ after the dropwise addition is finished, the reaction is carried out for 30 minutes, then a solution of 4 parts of trimethyl borate dissolved in 10 parts of toluene is dropwise added, the temperature is raised to 50 ℃ and the reaction is continued for 2 hours, the temperature is lowered to room temperature, 2 parts of active carbon is added, the stirring adsorption is carried out for 0.5 hour, then the filtrate is filtered, and the toluene and low-boiling-point substances are evaporated under reduced pressure to obtain the active organic borosilicate tackifier.
Example 6
The preparation method of the vinyl-terminated hyperbranched organic silicon resin comprises the following steps:
(a) preparation of monomers: under the protection of nitrogen and at the temperature of minus 20 ℃, adding 10 parts of trichlorosilane and 100 parts of dry diethyl ether in parts by mass into a reaction kettle, dropwise adding 190 parts of 1.0 mol/L allyl magnesium bromide diethyl ether solution while stirring, continuing to react for 30 minutes after dropwise adding, then heating to 20 ℃, continuing to react for 1.5 to 3 hours, stopping the reaction, adding 100ml of 1mol/L diluted hydrochloric acid into the mixture, stirring for 30 minutes, standing, separating liquid, taking an upper organic layer, washing the upper organic layer with saturated sodium carbonate solution to be neutral, and distilling the product under reduced pressure and passing through a silica gel column to obtain pure triallyl silane finally;
(b) and (b) under the protection of nitrogen, adding 100 parts of triallyl silane obtained in the step (a), 150 parts of toluene and 0.1 part of Kaster catalyst containing 2% of platinum into a reaction kettle, uniformly stirring, raising the temperature to 90 ℃, reacting for 4-8 hours, and carrying out reduced pressure distillation to remove toluene and oligomers to obtain the vinyl-terminated hyperbranched organic silicon resin.
The vinyl-terminated hyperbranched organic silicon resin is tested by GPC, toluene is taken as a mobile phase, polystyrene is taken as a standard sample, and the relative molecular weight of the vinyl-terminated hyperbranched organic silicon resin is 12863.
Example 7
The preparation method of the vinyl-terminated hyperbranched organic silicon resin comprises the following steps:
(a) preparation of monomers: under the protection of nitrogen and at the temperature of minus 20 ℃, adding 10 parts of trichlorosilane and 100 parts of dry ether in parts by mass into a reaction kettle, dropwise adding 200 parts of 1.0 mol/L allyl magnesium bromide ether solution 190-one while stirring, continuing to react for 30 minutes after dropwise adding, then heating to 20 ℃, continuing to react for 1.5 to 3 hours, stopping the reaction, adding 100ml of 1mol/L diluted hydrochloric acid into the mixture, stirring for 30 minutes, standing, separating liquid, taking an upper organic layer, washing the upper organic layer to be neutral by saturated sodium carbonate solution, and finally obtaining pure triallylsilane by carrying out reduced pressure distillation and silica gel column chromatography on the product;
(b) and (b) under the protection of nitrogen, adding 100 parts of triallyl silane obtained in the step (a), 150 parts of toluene and 0.1-0.5 part of Kaster catalyst containing 2% of platinum into a reaction kettle, uniformly stirring, raising the temperature to 90 ℃, reacting for 4-8 hours, carrying out reduced pressure distillation, and removing toluene and oligomer to obtain the vinyl-terminated hyperbranched organic silicon resin.
The vinyl-terminated hyperbranched organic silicon resin is subjected to GPC test, toluene is taken as a mobile phase, polystyrene is taken as a standard sample, and the relative molecular weight of the vinyl-terminated hyperbranched organic silicon resin is 14580.
Example 8
The preparation method of the hexadecyl vinyl polysilsesquioxane comprises the following steps:
1) under the protection of nitrogen, dissolving 60 parts by weight of tetramethylammonium hydroxide and 10 parts by weight of calcium oxide in 80 parts by weight of methanol, adding the mixture into a reaction kettle, dropwise adding a solution of 20 parts by weight of vinyltrimethoxysilane in 60 parts by weight of methanol, stirring at normal temperature for reaction for 12 hours, raising the temperature to reflux, continuing the reaction for 24 hours, and carrying out reduced pressure distillation to obtain white powder, wherein the white powder is respectively washed by water and boiling n-hexane for 3 times to obtain octavinyl polysilsesquioxane;
2) taking 50 parts of octavinyl polysilsesquioxane, 100 parts of tetrahydrofuran, 80 parts of methyldimethoxysilane and 0.5 part of Karster catalyst containing 2 percent of platinum in the step 1) according to weight percentage, stirring and reacting for 24 hours at a reflux temperature, adding 2 parts of activated carbon after the reaction is finished, and stirring for 30 minutes. Filtering to obtain filtrate, and distilling under reduced pressure to remove tetrahydrofuran and unreacted methyldimethoxysilane to obtain polysilsesquioxane containing 16 methoxyl groups;
3) under the protection of nitrogen, 15 parts by weight of polysilsesquioxane containing 16 methoxyl groups in the step 2) is dissolved in 100 parts of tetrahydrofuran, 180ml of 1.0 mol/L allyl magnesium bromide ethyl ether solution is dropwise added into the tetrahydrofuran while stirring, the mixture reacts for 2 hours at 30 ℃, then the temperature is raised to 50 ℃, the reaction is stopped after the mixture continues to react for 30 minutes, 100ml of 1mol/L diluted hydrochloric acid is added into the mixture, the mixture is stirred for 30 minutes, the mixture is kept still and separated to obtain an upper organic layer, the upper organic layer is washed by saturated sodium carbonate solution until the mixture is neutral, and the product is subjected to reduced pressure distillation and silica gel column chromatography to obtain pure hexadecyl polysilsesquioxane.
Example 9
The preparation method of the hexadecyl vinyl polysilsesquioxane comprises the following steps:
1) under the protection of nitrogen, dissolving 60 parts by weight of tetramethylammonium hydroxide and 10 parts by weight of calcium oxide in 80 parts by weight of methanol, adding the mixture into a reaction kettle, dropwise adding a solution of 20 parts by weight of vinyltrimethoxysilane in 60 parts by weight of methanol, stirring at normal temperature for reaction for 18 hours, raising the temperature to reflux, continuing the reaction for 24 hours, and carrying out reduced pressure distillation to obtain white powder, wherein the white powder is respectively washed by water and boiling n-hexane for 3 times to obtain octavinyl polysilsesquioxane;
2) taking 50 parts of octavinyl polysilsesquioxane, 100 parts of tetrahydrofuran, 85 parts of methyldimethoxysilane and 0.5 part of Karster catalyst containing 2 percent of platinum in the step 1) according to weight percentage, stirring and reacting for 24 hours at a reflux temperature, adding 2 parts of activated carbon after the reaction is finished, and stirring for 30 minutes. Filtering to obtain filtrate, and distilling under reduced pressure to remove tetrahydrofuran and unreacted methyldimethoxysilane to obtain polysilsesquioxane containing 16 methoxyl groups;
3) under the protection of nitrogen, 15 parts by weight of polysilsesquioxane containing 16 methoxyl groups in the step 2) is dissolved in 100 parts of tetrahydrofuran, 180ml of 1.0 mol/L allyl magnesium bromide ethyl ether solution is dropwise added into the tetrahydrofuran while stirring, the mixture reacts for 2 hours at 30 ℃, then the temperature is raised to 50 ℃, the reaction is stopped after the mixture continues to react for 30 minutes, 100ml of 1mol/L diluted hydrochloric acid is added into the mixture, the mixture is stirred for 30 minutes, the mixture is kept still and separated to obtain an upper organic layer, the upper organic layer is washed by saturated sodium carbonate solution until the mixture is neutral, and the product is subjected to reduced pressure distillation and silica gel column chromatography to obtain pure hexadecyl polysilsesquioxane.
Example 10
The preparation method of the hexadecyl vinyl polysilsesquioxane comprises the following steps:
1) under the protection of nitrogen, dissolving 60 parts by weight of tetramethylammonium hydroxide and 10 parts by weight of calcium oxide in 80 parts by weight of methanol, adding the mixture into a reaction kettle, dropwise adding a solution of 20 parts by weight of vinyltrimethoxysilane in 60 parts by weight of methanol, stirring at normal temperature for reaction for 15 hours, raising the temperature to reflux, continuing the reaction for 24 hours, and carrying out reduced pressure distillation to obtain white powder, wherein the white powder is respectively washed by water and boiling n-hexane for 3 times to obtain octavinyl polysilsesquioxane;
2) taking 50 parts of octavinyl polysilsesquioxane, 100 parts of tetrahydrofuran, 82 parts of methyldimethoxysilane and 0.5 part of Karster catalyst containing 2 percent of platinum in the step 1) according to weight percentage, stirring and reacting for 24 hours at a reflux temperature, adding 2 parts of activated carbon after the reaction is finished, and stirring for 30 minutes. Filtering to obtain filtrate, and distilling under reduced pressure to remove tetrahydrofuran and unreacted methyldimethoxysilane to obtain polysilsesquioxane containing 16 methoxyl groups;
3) under the protection of nitrogen, 15 parts by weight of polysilsesquioxane containing 16 methoxyl groups in the step 2) is dissolved in 100 parts of tetrahydrofuran, 180ml of 1.0 mol/L allyl magnesium bromide ethyl ether solution is dropwise added into the tetrahydrofuran while stirring, the mixture reacts for 2 hours at 30 ℃, then the temperature is raised to 50 ℃, the reaction is stopped after the mixture continues to react for 30 minutes, 100ml of 1mol/L diluted hydrochloric acid is added into the mixture, the mixture is stirred for 30 minutes, the mixture is kept still and separated to obtain an upper organic layer, the upper organic layer is washed by saturated sodium carbonate solution until the mixture is neutral, and the product is subjected to reduced pressure distillation and silica gel column chromatography to obtain pure hexadecyl polysilsesquioxane.
Claims (7)
1. An organic silicon material for packaging an LED with high luminous flux maintenance rate is characterized in that the organic silicon material comprises an organic silicon gel A component, an organic silicon gel B component, nano magnesium oxide, fluorescent powder and an acrylic polymer;
the organic silica gel A component comprises the following components: 60-85 parts of polymethylphenylsiloxane with vinyl as a terminal group, 5-15 parts of polydimethylsiloxane with vinyl as a terminal group, 3-8 parts of active organic borosilicate tackifier, 10-25 parts of vinyl-terminated hyperbranched organic silicon resin and 0.05-0.5 part of platinum catalyst;
the organosilicon B component comprises the following components: 35-45 parts of polymethylphenyl vinyl siloxane with vinyl as a terminal group, 45-55 parts of polymethylhydrosiloxane, 5-15 parts of MQ resin and 5-1723-8 parts of silane coupling agent;
the organic silicon material comprises an organic silicon component A, an organic silicon component B, nano magnesium oxide, fluorescent powder and an acrylic polymer in a mass part ratio of 100:100:2.5-18:3-8: 1-3.
2. The silicone material for packaging the LED with high luminous flux maintenance rate as claimed in claim 1, wherein the preparation method of the active organic borosilicate tackifier is as follows: under the protection of nitrogen, 100 parts of polymethylhydrosiloxane, 100 parts of toluene and 0.02 part of tris (pentafluorophenyl) borane are uniformly stirred, then a solution of 15 parts of hydroxyethyl acrylate dissolved in 10 parts of toluene is dropwise added, the temperature is controlled to 30 ℃ after the dropwise addition is finished, the reaction is carried out for 30 minutes, then a solution of 4 parts of trimethyl borate dissolved in 10 parts of toluene is dropwise added, the temperature is raised to 50 ℃ and the reaction is continued for 2 hours, the temperature is lowered to room temperature, 2 parts of active carbon is added, the stirring adsorption is carried out for 0.5 hour, then the filtrate is filtered, and the toluene and low-boiling-point substances are evaporated under reduced pressure to obtain the active organic borosilicate tackifier.
3. The silicone material for packaging the LED with high luminous flux maintenance rate as claimed in claim 1, wherein the preparation method of the vinyl-terminated hyperbranched silicone resin is as follows:
(a) preparation of monomers: under the protection of nitrogen and at the temperature of minus 20 ℃, adding 10 parts of trichlorosilane and 100 parts of dry ether in parts by mass into a reaction kettle, dropwise adding 200 parts of 1.0 mol/L allyl magnesium bromide ether solution 190-one while stirring, continuing to react for 30 minutes after dropwise adding, then heating to 20 ℃, continuing to react for 1.5 to 3 hours, stopping the reaction, adding 100ml of 1mol/L diluted hydrochloric acid into the mixture, stirring for 30 minutes, standing, separating liquid, taking an upper organic layer, washing the upper organic layer to be neutral by saturated sodium carbonate solution, and finally obtaining pure triallylsilane by carrying out reduced pressure distillation and silica gel column chromatography on the product;
(b) and (b) under the protection of nitrogen, adding 100 parts of triallyl silane obtained in the step (a), 150 parts of toluene and 0.1-0.5 part of Kaster catalyst containing 2% of platinum into a reaction kettle, uniformly stirring, raising the temperature to 90 ℃, reacting for 4-8 hours, carrying out reduced pressure distillation, and removing toluene and oligomer to obtain the vinyl-terminated hyperbranched organic silicon resin.
4. The silicone material for packaging an LED with high luminous flux maintenance rate as claimed in claim 1, wherein the silicone material further comprises hexadecafluoroethylsilsesquioxane.
5. The silicone material for packaging an LED with high luminous flux maintenance rate as claimed in claim 4, wherein the preparation method of the hexadecene vinyl polysilsesquioxane is as follows:
1) under the protection of nitrogen, dissolving 60 parts by weight of tetramethylammonium hydroxide and 10 parts by weight of calcium oxide in 80 parts by weight of methanol, adding the mixture into a reaction kettle, dropwise adding a solution of 20 parts by weight of vinyltrimethoxysilane in 60 parts by weight of methanol, stirring at normal temperature for reaction for 12-18 hours, raising the temperature to reflux, continuing the reaction for 24 hours, and carrying out reduced pressure distillation to obtain white powder, wherein the white powder is respectively washed by water and boiling n-hexane for 3 times to obtain octavinyl polysilsesquioxane;
2) taking 50 parts by mass of the octavinyl polysilsesquioxane, 100 parts by mass of tetrahydrofuran, 80-85 parts by mass of methyldimethoxysilane and 0.5 part by mass of Karster catalyst containing 2% of platinum in the step 1), stirring and reacting for 24 hours at a reflux temperature, adding 2 parts by mass of activated carbon after the reaction is finished, stirring for 30 minutes, filtering to obtain filtrate, and distilling under reduced pressure to remove the tetrahydrofuran and unreacted methyldimethoxysilane to obtain polysilsesquioxane containing 16 methoxyl groups;
3) under the protection of nitrogen, 15 parts by weight of polysilsesquioxane containing 16 methoxyl groups in the step 2) is dissolved in 100 parts of tetrahydrofuran, 180ml of 1.0 mol/L allyl magnesium bromide ethyl ether solution is dropwise added into the tetrahydrofuran while stirring, the mixture reacts for 2 hours at 30 ℃, then the temperature is raised to 50 ℃, the reaction is stopped after the mixture continues to react for 30 minutes, 100ml of 1mol/L diluted hydrochloric acid is added into the mixture, the mixture is stirred for 30 minutes, the mixture is kept still and separated to obtain an upper organic layer, the upper organic layer is washed by saturated sodium carbonate solution until the mixture is neutral, and the product is subjected to reduced pressure distillation and silica gel column chromatography to obtain pure hexadecyl polysilsesquioxane.
6. The silicone material for packaging an LED with high luminous flux maintenance rate as claimed in claim 4 or 5, wherein the silicone material comprises 100:100:3 of silicone rubber A component, silicone rubber B component and hexadecyl vinyl polysilsesquioxane.
7. The silicone material for packaging the LED with high luminous flux maintenance rate as claimed in claim 1, wherein the silicone material is prepared by preparing the components according to a formula, packaging the components by using a dispenser, and then baking and curing the components at 85-105 ℃.
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