CN106433551A - Thermal shock resistant high-refraction LED packaging glue composition and preparation method thereof - Google Patents

Thermal shock resistant high-refraction LED packaging glue composition and preparation method thereof Download PDF

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Publication number
CN106433551A
CN106433551A CN201610851840.8A CN201610851840A CN106433551A CN 106433551 A CN106433551 A CN 106433551A CN 201610851840 A CN201610851840 A CN 201610851840A CN 106433551 A CN106433551 A CN 106433551A
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parts
component
thermal shock
methyl phenyl
glue composition
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Inventor
吴向荣
张利利
薛俊发
程宪涛
王佐
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ZHAOQING HOMEEN ORGANIC SILICON CO Ltd
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ZHAOQING HOMEEN ORGANIC SILICON CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives 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
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor 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
    • H01L33/48Semiconductor 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
    • H01L33/52Encapsulations
    • H01L33/56Materials, e.g. epoxy or silicone resin
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer 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)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a thermal shock resistant high-refraction LED packaging glue composition and a preparation method thereof; the LED packaging glue composition is prepared from component A and component B at a weight ratio of 1:1; the component A is prepared from, by weight, 25-35 parts of methyl phenyl vinyl silicone resin, 10-20 parts of methyl phenyl vinyl silicone oil, 0.1-0.3 part of a catalyst, and 0.01-0.03 part of a heat resistant; the component B is prepared from, by weight, 5-15 parts of methyl phenyl vinyl silicone resin, 30-45 parts of methyl phenyl hydrogen-containing silicone resin, 0.02-0.1 part of an inhibitor, and 0.5-3 parts of an adhesion promoter. The invention belongs to the technical field of LED packaging and provides the LED packaging glue composition, having the excellent properties, such as adhesion, thermal shock resistance, permeability, refractivity and hardness, and capable of meeting the requirements of high-power LED packaging.

Description

High refraction LED encapsulation glue composition of cold-resistant thermal shock and preparation method thereof
Technical field
The invention belongs to the high refraction LED packaging plastic combination in LED encapsulation technology field, more particularly to a kind of cold-resistant thermal shock Thing and preparation method thereof.
Background technology
LED is because having life-span length, energy-saving and environmental protection, it has also become the key project of global energy-saving and emission-reduction, highly energy-consuming Electric filament lamp will be gradually backed out the arena of history.
At present, LED encapsulation material is mainly organosilicon material, and which has excellent thermostability, internal stress is little, do not turn yellow Advantage.With the development of LED encapsulation technology, the requirement more and more higher to LED encapsulation material, the developing direction of LED encapsulation technology Mainly include:North efficiency occurred frequently, high reliability, high heat-sinking capability and slimming.With high-power LED illuminating light source development and Application, the requirement of high caloric value to aspects such as the intensity of package material profit, cold-resistant thermal shock, substrate bondings is gradually stepped up.
Cold-resistant thermal shock is the important indicator of the high refraction LED packaging plastic performance of assessment, the high refraction LED for putting goods on the market at present The universal deviation of the cold-resistant thermal shock resistance properties of packaging plastic.Improve cold-resistant thermal shock method include to improve colloid to LED support base material and The bonding force of reflective metal layer, and improve the heat resistance of colloid itself.
Chinese patent application CN104592932 discloses a kind of high power LED package glue composition, comprising component A have Phenyl vinyl polysiloxane, MDQ resin, platinum catalyst are made, comprising B component hydrogeneous by high phenyl hydrogen-containing silicon oil or high phenyl Silicones, viscosifier are made.Although LED encapsulation glue composition is with good refractive index and hardness, its saturating north property and resistance to Thermal shock effect is still not ideal enough.
Chinese patent application CN103725249 discloses a kind of high index of refraction LED packaging silicon rubber, including the first component and Two components, the first component is made up of methyl phenyl vinyl polysiloxane, methyl phenyl vinyl silicone oil, platinum group catalyst, and second Component is made up of POSS modified silicon oil, methyl phenyl vinyl polysiloxane, methyl phenyl vinyl silicone oil and inhibitor.In encapsulation Add a kind of addition of POSS modified silicon oil, POSS modified silicon oil both to effectively increase crosslink density in glue, improve to base again Material bonding and thermostability, but the POSS modified silicon oil compatibility is poor, and reactivity is relatively low, seeks the saturating north for causing LED packaging plastic Rate is low.
Therefore it provides a kind of while the high refraction LED packaging plastic with good bonding performance and cold-resistant thermal shock resistance properties has Significant.
Content of the invention
For solving problems of the prior art, inventor is sieved to the component of LED packaging plastic by lot of experiments Select and compounding, and corresponding adhesive property and cold-resistant thermal shock resistance properties etc. is investigated, it has been unexpectedly found that:By in component A A small amount of iron content silazane coordination compound being added as heat-resistant agent, a small amount of Borosiloxane oligomer is added in B component as viscous Accelerator is connect, obtained LED encapsulation glue composition has excellent adhesive property, cold-resistant thermal shock resistance properties, light transmittance, refractive index With performances such as hardness, the requirement of high power LED package can be met.Based on above-mentioned discovery, so as to complete the present invention.
The purpose of the present invention will be further described in detail below reflect and description.
The present invention provides a kind of high refraction LED encapsulation glue composition of cold-resistant thermal shock, by component A and B component with 1: 1 Weight is than composition;Component A includes following component and its parts by weight:25~35 parts of methyl phenyl vinyl polysiloxane, methylbenzene 10~20 parts of base vinyl silicone oil, 0.1~0.3 part of catalyst, 0.01~0.03 part of heat-resistant agent;B component include following component and Its parts by weight:30~45 parts of the hydrogeneous rock resin of 5~15 parts of methyl phenyl vinyl rock resin, aminomethyl phenyl, inhibitor 0.02 ~0.1 part, 0.5~3 part of adhesion promoters.
Heat-resistant agent is used as by the iron content silazane coordination compound for adding a small amount of in component A, in B component, adds a small amount of boron Silica a heatable brick bed oligomer significantly improves high refraction LED packaging plastic combination as adhesion promoters by the synergism of each component The cementability of thing, cold-resistant thermal shock, the performance such as high temperature resistant, can meet the requirement of high power LED package.
Preferably, the component A includes following component and its parts by weight:Methyl phenyl vinyl polysiloxane 28~32 Part, 14~18 parts of methyl phenyl vinyl silicone oil, 0.1~0.3 part of catalyst, 0.01~0.03 part of heat-resistant agent;B component include as Lower component and its parts by weight:32~40 parts of the hydrogeneous silicones of 8~12 parts of methyl phenyl vinyl polysiloxane, aminomethyl phenyl, suppression 0.02~0.08 part of preparation, 1~2 part of adhesion promoters.
It is highly preferred that the component A includes following component and its parts by weight:30 parts of methyl phenyl vinyl polysiloxane, 15 parts of methyl phenyl vinyl silicone oil, 0.2 part of catalyst, 0.02 part of heat-resistant agent;B component includes following component and its weight portion Number:35 parts of the hydrogeneous silicones of 10 parts of methyl phenyl vinyl polysiloxane, aminomethyl phenyl, 0.05 part of inhibitor, adhesion promoters 1 Part.
Preferably, the heat-resistant agent is that iron content silazane coordination compound, its structural formula is: The iron content silazane coordination compound is obtained with two silicon nitrogen a heatable brick bed of ring, iron chloride and tertiary butyl lithium as Material synthesis, with methyl phenyl vinyl Base silicone oil has the good compatibility.
Iron content rock azane coordination compound is added to be used as heat-resistant agent, iron content rock nitrogen by encapsulating in glue composition in high refraction LED Alkane coordination compound has gone up the organo-functional group of long-chain due to grafting, has the preferable compatibility with organosilicon systems, in pyroprocess The middle free radical that can be quenched produced by polysiloxanes oxidation, suppresses the oxidation of side chain, significantly improves high refraction LED packaging plastic Cold-hot impact effect.By many experiments, inventor has found that a small amount of iron content silazane coordination compound is remarkably improved high refraction The cold-hot impact effect of LED packaging plastic, when the addition of iron content silazane coordination compound is more than 0.03 part, with 0.02 part of interpolation When compare cold-hot impact effect improve limited, but light transmittance occur decline;When the addition of iron content silazane coordination compound is more than When 0.2 part, the catalytic degradation due to excessive metal is acted on, and the cold-hot impact effect of high refraction LED packaging plastic can be caused to be deteriorated.
Preferably, the adhesion promoters are that Borosiloxane oligomer, its structural formula is:
The Borosiloxane oligomer is obtained with phenyltrimethoxysila,e, boric acid, phenol, hydrochloric acid as Material synthesis.The boron Silica a heatable brick bed oligomer has the excellent compatibility, and its non-hydrolytic group has good affinity with polymer, PPA;Hydrolyzable Group can be reacted with material with LED support reflection gold, solve a difficult problem for system cementability.Meanwhile, low by the Borosiloxane Polymers is used cooperatively with iron content silicon nitrogen a heatable brick bed coordination compound, is further increased the resistance to elevated temperatures of colloid and is resisted cold-resistant thermal impact Energy.
Add borosilicate oxygen a heatable brick bed oligomer to be used as adhesion promoters by encapsulating in glue composition in high refraction LED, solve The problem of LED packaging plastic and substrate bonding, and water white transparency.
Preferably, the molecular formula of the methyl phenyl vinyl polysiloxane is (ViMeSiO1/2)a(ViPhSiO3/2)b, viscosity For 500~20000cps, contents of ethylene 5%~8%, wherein, it is vinyl that Me is methyl, Vi, Ph be phenyl, a be 10~ 30, b is 10~30.More preferably:It is 12~25 that a is 15~25, b..
Preferably, the molecular formula of the methyl phenyl vinyl silicone oil is (ViMe2PhSiO1/2)c(MePhSiO)d, viscosity For 1000~30000cps, it is 10~50 for 5~12, b that contents of ethylene is 1%~5%, wherein a.It is highly preferred that b be 20~ 45.
Preferably, the molecular formula of the hydrogeneous silicones of the aminomethyl phenyl is Me3SiO(PhHSiO)n(Me2SiO)mSiMe3, glue Spend for 40~2000cps, hydrogen content is that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10~30 that 0.1%~0.5%, wherein it is 10.It is highly preferred that n be 8~ 10, m is 15~20.
Preferably, the catalyst is platinum group catalyst, selected from 1,3- dimethyl -1,3- diphenyl -1,3- divinyl Silica a heatable brick bed platinum complex, the platinum catalyst of tetrahydrofuran coordination, the platinum catalyst of methyl vinyl silicone coordination and adjacent benzene two One or more in the platinum catalyst of formic acid diethylester coordination;
The inhibitor be methylpentynol, N, N, N, N- tetramethylethylenediamine, diallyl maleate and 1,3,5,7- tetravinyl -1, one or more in 3,5,7- tetramethyl cyclotetrasiloxane silica a heatable brick bed.
Correspondingly, present invention also offers the high refraction LED of cold-resistant thermal shock encapsulates the preparation method of glue composition, including Following steps:
S1 prepares component A:Methyl phenyl vinyl rock resin and methyl phenyl vinyl silicone oil are weighed in reaction vessel, Stir, heat-resistant agent and catalyst is added, is stirred, then vacuumizing and defoaming, obtain final product component A;
S2 prepares B component:The hydrogeneous rock resin of aminomethyl phenyl, methyl phenyl vinyl resin are weighed in another reaction vessel In, stir, adhesion promoters and inhibitor is added, is stirred, then vacuumizing and defoaming, obtain final product B component;
Component A and B component are mixed by S3, vacuum defoamation, obtain the high refraction LED encapsulation glue composition of cold-resistant thermal shock.
During use, by the high refraction LED encapsulation glue composition dispensing of cold-resistant thermal shock or encapsulating in components and parts to be packaged On, first 80 DEG C of heating 1h, transfer to 150 DEG C of heating 3h.
Compared with prior art, the invention has the beneficial effects as follows:The present invention is by adding a small amount of iron content silicon in component A Nitrogen a heatable brick bed coordination compound adds a small amount of Borosiloxane oligomer as adhesion promoters, by each group as heat-resistant agent in B component The synergism for dividing, the LED encapsulation glue composition for obtaining has excellent adhesive property, cold-resistant thermal shock resistance properties, heat-resisting quantity Can, the saturating performance such as north rate, refractive index and hardness, the requirement of high power LED package can be met, specifically included:1. prepared by the present invention High refraction LED encapsulation glue composition solidification after, the high-temperature baking of 300 DEG C/24h can be born, non yellowing is not cracked;2. solidify Afterwards, after the sulphur ageing experiment of 80 DEG C/24h, light decay < 3%;3., after solidifying, standing the impact experiment (- 40 of 600 bouts DEG C/0.5h~100 DEG C/0.5h) after will not peel off from base material, invariant color, do sem observation using aobvious, becoming does not occur in gold thread Shape, lights rear light decay < 3%;4. after solidifying, 24h being heated in 260 DEG C of heating platforms, puts in 0 DEG C of frozen water rapidly and soak 10min, can also light after taking-up;5., after solidifying, 2h is boiled in red ink solution, not ink feed, not unsticking.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail.
In the embodiment of the present invention, methyl phenyl vinyl polysiloxane, methyl phenyl vinyl silicone oil and aminomethyl phenyl are hydrogeneous In rock resin corresponding a be 8, b be 25, c be 9, d be 20, m be 18, n be 9.
The high refraction LED encapsulation glue composition of embodiment one
High refraction LED encapsulation glue composition, is made up of with 1: 1 weight ratio component A and B component;Component A is included as the following group Divide and its parts by weight:30 parts of methyl phenyl vinyl polysiloxane, 15 parts of methyl phenyl vinyl silicone oil, 1,3- dimethyl -1, 3- diphenyl -1,0.2 part of 3- divinyl silica a heatable brick bed platinum complex, 0.02 part of iron content rock azane coordination compound;B component includes as follows Component and its parts by weight:35 parts of the hydrogeneous rock resin of 10 parts of methyl phenyl vinyl rock resin, aminomethyl phenyl, 3- methyl-1-pentene 0.05 part of alkynes -3- alcohol, 1 part of Borosiloxane oligomer.
Preparation method comprises the steps:Prepare component A:Weigh methyl phenyl vinyl polysiloxane and methyl phenyl vinyl Base silicone oil is stirred in reaction vessel, is added heat-resistant agent and catalyst, is stirred, then vacuumizing and defoaming, obtain final product A Component;Prepare B component:The hydrogeneous rock resin of aminomethyl phenyl, methyl phenyl vinyl resin are weighed in another reaction vessel, stirring Uniformly, adhesion promoters and inhibitor is added, stirs, then vacuumizing and defoaming, obtain final product B component;By component A and B component Mix, vacuum defoamation, obtain the high refraction LED encapsulation glue composition of cold-resistant thermal shock.
The high refraction LED encapsulation glue composition of embodiment two
High refraction LED encapsulation glue composition, is made up of with 1: 1 weight ratio component A and B component;Component A is included as the following group Divide and its parts by weight:32 parts of methyl phenyl vinyl polysiloxane, 18 parts of methyl phenyl vinyl silicone oil, 1,3- dimethyl -1, 3- diphenyl -1,0.3 part of 3- divinylsiloxanes platinum complex, 0.02 part of iron content silazane coordination compound;B component includes as follows Component and its parts by weight:40 parts of the hydrogeneous silicones of 12 parts of methyl phenyl vinyl polysiloxane, aminomethyl phenyl, 3- methyl-1-pentene 0.08 part of alkynes -3- alcohol, 1.5 parts of Borosiloxane oligomer.
Preparation method is with embodiment one.
Embodiment three-hypers refraction LED encapsulation glue composition
High refraction LED encapsulation glue composition, is made up of with 1: 1 weight ratio component A and B component;Component A is included as the following group Divide and its parts by weight:28 parts of methyl phenyl vinyl polysiloxane, 14 parts of methyl phenyl vinyl silicone oil, 1,3- dimethyl -1, 3- diphenyl -1,0.2 part of 3- divinylsiloxanes platinum complex, 0.01 part of iron content rock azane coordination compound;B component includes as follows Component and its parts by weight:32 parts of the hydrogeneous silicones of 8 parts of methyl phenyl vinyl polysiloxane, aminomethyl phenyl, 3- methyl-1-pentene 0.03 part of alkynes -3- alcohol, 1 part of Borosiloxane oligomer.
Preparation method is with embodiment one.
One LED of comparative example encapsulates glue composition
High refraction LED encapsulation glue composition, is made up of with 1: 1 weight ratio component A and B component;Component A is included as the following group Divide and its parts by weight:30 parts of methyl phenyl vinyl polysiloxane, 15 parts of methyl phenyl vinyl silicone oil, 1,3- dimethyl -1, 3- diphenyl -1,0.2 part of 3- divinylsiloxanes platinum complex, 0.02 part of copper oxide;B component includes following component and its weight Amount number:35 parts of the hydrogeneous rock resin of 10 parts of methyl phenyl vinyl rock resin, aminomethyl phenyl, methylpentynol 0.05 Part, 1 part of Borosiloxane oligomer.
Preparation method is with embodiment one.
Comparative example one is with the difference of embodiment one:In component A, iron content silazane coordination compound is changed into copper oxide.
Two LED of comparative example encapsulates glue composition
High refraction LED encapsulation glue composition, is made up of with 1: 1 weight ratio component A and B component;Component A is included as the following group Divide and its parts by weight:30 parts of methyl phenyl vinyl polysiloxane, 15 parts of methyl phenyl vinyl silicone oil, 1,3- dimethyl -1, 3- diphenyl -1,0.2 part of 3- divinylsiloxanes platinum complex, 0.02 part of iron content silazane coordination compound;B component includes as follows Component and its parts by weight:35 parts of the hydrogeneous rock resin of 10 parts of methyl phenyl vinyl rock resin, aminomethyl phenyl, 3- methyl-1-pentene 0.05 part of alkynes -3- alcohol, γ -1 part of glycidyl ether oxygen propyl trimethoxy silicon a heatable brick bed.
Preparation method is with embodiment one.
Comparative example two is with the difference of embodiment one:In B component, boron rock oxygen alkane oligomer is changed into γ-glycidyl ether Oxygen propyl trimethoxy silicon a heatable brick bed.
Three LED of comparative example encapsulates glue composition
Will the encapsulation of LED as obtained in embodiment in CN103725249 three glue composition as a comparison case three.
Test example:The test effect of LED encapsulation glue composition
The LED packaging plastic group for respectively embodiment one, embodiment three, comparative example one, comparative example two and comparative example three being obtained Compound dispensing or encapsulating are on components and parts to be packaged, and first 80 DEG C of heating 1h, transfer to 150 DEG C of heating 3h.Carry out northern rate, The dead lamp rate of refractive index, thermal shock, the test of the aspect such as high temperature resistant, as a result as shown in table 1.
The thoroughly detection of the index such as north rate, refractive index, using relevant criterion method or industry conventional process, such as:Light transmittance Determine with reference to the method in GB/T 2410-2008;The method for determining in reference GB/T6488-2008 of refractive index.
The test result of 1 difference LED of table encapsulation glue composition
As known from Table 1, the embodiment of the present invention one and LED encapsulation glue composition obtained in embodiment three have excellent bonding The performance such as performance, cold-resistant thermal shock resistance properties, light transmittance, refractive index and hardness, can meet the requirement of high power LED package, cold The dead lamp rate of thermal shock, the aspect such as high temperature resistant are better than comparative example one to comparative example three.Wherein, the resultant effect of embodiment one is optimal, Therefore, embodiment one is highly preferred embodiment of the present invention.
Above content is further description made for the present invention with reference to specific preferred implementation, it is impossible to assert Being embodied as of the present invention is confined to these explanations.For general technical staff of the technical field of the invention, On the premise of present inventive concept, some simple deduction or replace can also be made, portion should be considered as belonging to the present invention's Protection domain.

Claims (10)

1. the high refraction LED of cold-resistant thermal shock encapsulates glue composition, it is characterised in that:By component A and B component with 1: 1 weight Than composition;Component A includes following component and its parts by weight:25~35 parts of methyl phenyl vinyl polysiloxane, aminomethyl phenyl second 10~20 parts of thiazolinyl silicone oil, 0.1~0.3 part of catalyst, 0.01~0.03 part of heat-resistant agent;B component includes following component and its weight Amount number:30~45 parts of the hydrogeneous silicones of 5~15 parts of methyl phenyl vinyl polysiloxane, aminomethyl phenyl, inhibitor 0.02~0.1 Part, 0.5~3 part of adhesion promoters.
2. the high refraction LED of cold-resistant thermal shock according to claim 1 encapsulates glue composition, it is characterised in that:The A group Dividing includes following component and its parts by weight:28~32 parts of methyl phenyl vinyl polysiloxane, methyl phenyl vinyl silicone oil 14 ~18 parts, 0.1~0.3 part of catalyst, 0.01~0.03 part of heat-resistant agent;B component includes following component and its parts by weight:Methyl 32~40 parts of the hydrogeneous silicones of 8~12 parts of phenyl vinyl polysiloxane, aminomethyl phenyl, 0.02~0.08 part of inhibitor, bonding promote Enter 1~2 part of agent.
3. the high refraction LED of cold-resistant thermal shock according to claim 2 encapsulates glue composition, it is characterised in that:The A group Dividing includes following component and its parts by weight:30 parts of methyl phenyl vinyl polysiloxane, 15 parts of methyl phenyl vinyl silicone oil, urge 0.2 part of agent, 0.02 part of heat-resistant agent;B component includes following component and its parts by weight:Methyl phenyl vinyl polysiloxane 10 Part, 35 parts of the hydrogeneous silicones of aminomethyl phenyl, 0.05 part of inhibitor, 1 part of adhesion promoters.
4. the high refraction LED of cold-resistant thermal shock according to any one of claim 1 to 3 encapsulates glue composition, and its feature exists In:The heat-resistant agent is iron content silazane coordination compound, and its structural formula is:
5. the high refraction LED of cold-resistant thermal shock according to any one of claim 1 to 3 encapsulates glue composition, it is characterised in that: The adhesion promoters are Borosiloxane oligomer, and its structural formula is:
6. the high refraction LED of cold-resistant thermal shock according to any one of claim 1 to 3 encapsulates glue composition, its feature It is:The molecular formula of the methyl phenyl vinyl polysiloxane is (ViMeSiO1/2)a(ViPhSiO3/2)b, viscosity be 500~ 20000cps, contents of ethylene 5%~8%, wherein, it is vinyl that Me is methyl, Vi, and it is 10 for 10~30, b that Ph is phenyl, a ~30.
7. the high refraction LED of cold-resistant thermal shock according to any one of claim 1 to 3 encapsulates glue composition, its feature It is:The methyl phenyl vinyl silicone oil molecular formula is (ViMe2PhSiO1/2)c(MePhSiO)d, viscosity be 1000~ 30000cps, it is 10~50 for 5~12, d that contents of ethylene is 1%~5%, wherein c.
8. the high refraction LED of cold-resistant thermal shock according to any one of claim 1 to 3 encapsulates glue composition, its feature It is:The molecular formula of the hydrogeneous silicones of the aminomethyl phenyl is Me3SiO(PhHSiO)n(Me2SiO)mSiMe3, viscosity be 40~ 2000cps, hydrogen content is that 0.1%~0.5%, wherein it is 10~30 that n is 5~12, m.
9. the high refraction LED of cold-resistant thermal shock according to any one of claim 1 to 3 encapsulates glue composition, its feature It is:The catalyst is platinum group catalyst, and selected from 1,3- dimethyl -1,3- diphenyl -1,3- divinylsiloxanes platinum is joined Compound, the platinum catalyst of tetrahydrofuran coordination, the platinum catalyst of methyl vinyl silicone coordination and diethyl phthalate One or more in the platinum catalyst of coordination;
The inhibitor is methylpentynol, N, N, N, N- tetramethylethylenediamine, diallyl maleate and 1,3, 5,7- tetravinyl -1, one or more in 3,5,7- tetramethyl cyclotetrasiloxane silica a heatable brick bed.
10. the high refraction LED of cold-resistant thermal shock according to any one of claim 1 to 9 encapsulates the preparation of glue composition Method, it is characterised in that:Comprise the steps:
S1 prepares component A:Methyl phenyl vinyl polysiloxane and methyl phenyl vinyl silicone oil are weighed in reaction vessel, stirring Uniformly, heat-resistant agent and catalyst is added, stirs, then vacuumizing and defoaming, obtain final product component A;
S2 prepares B component:The hydrogeneous silicones of aminomethyl phenyl, methyl phenyl vinyl resin are weighed in another reaction vessel, stir Mix uniformly, adhesion promoters and inhibitor is added, is stirred, then vacuumizing and defoaming, obtain final product B component;
Component A and B component are mixed by S3, vacuum defoamation, obtain the high refraction LED encapsulation glue composition of cold-resistant thermal shock.
CN201610851840.8A 2016-09-25 2016-09-25 Thermal shock resistant high-refraction LED packaging glue composition and preparation method thereof Pending CN106433551A (en)

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CN112322251A (en) * 2020-10-27 2021-02-05 复旦大学 Thermosetting yellowing-resistant full-lamination special material and preparation method and application thereof
CN112322251B (en) * 2020-10-27 2021-12-07 复旦大学 Thermosetting yellowing-resistant full-lamination special material and preparation method and application thereof
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