CN107652886A - A kind of low LED organosilicon crystal-bonding adhesives of operating time long light decay - Google Patents
A kind of low LED organosilicon crystal-bonding adhesives of operating time long light decay Download PDFInfo
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- CN107652886A CN107652886A CN201710995178.8A CN201710995178A CN107652886A CN 107652886 A CN107652886 A CN 107652886A CN 201710995178 A CN201710995178 A CN 201710995178A CN 107652886 A CN107652886 A CN 107652886A
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- light decay
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Classifications
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- 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
- C09J11/06—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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
A kind of low LED organosilicon crystal-bonding adhesives of operating time long light decay, it is uniformly mixed according to following parts by weight addition raw material:75~85 parts of methyl vinyl silicone, 1~3 part of toughener, 10~15 parts of crosslinking agent, 1~3 part of bonding agent, 3~5 parts of light decay controlling agent, 0.2~2 part of inhibitor, 0.1~0.5 part of catalyst.The beneficial effects of the invention are as follows:Product viscosity is adjusted by silicones viscosity, does not adjust viscosity by adding thixotropic agent, and then improve the light emission rate of LED product;By adding light decay controlling agent, the light decay rate under LED product normal temperature and hot conditions is effectively reduced;By controlling the ratio of inhibitor and catalyst, extension operable time is reached.
Description
Technical field
Insulated organosilicon crystal-bonding adhesive the present invention relates to a kind of one pack system, more particularly to a kind of operable time is long, normal temperature/
High temperature lights the low LED crystal-bonding adhesives of rear light decay for a long time, belongs to middle and high end LED organosilicon adhesive fields.
Technical background
Die bond is also known as Die Bond or load.Die bond (is usually conducting resinl or insulation for LED i.e. by colloid
Glue) wafer bonding in the designated area of support, form heat passage or electric pathway, the work for the condition that provides connected for the routing of postorder
Sequence.
Although the usage amount of LED crystal-bonding adhesives is seldom, it is highly important to work, and LED encapsulation most base
The link of plinth.At present, the crystal-bonding adhesive used on LED is divided into two big systems:Epoxy crystal-bonding adhesive, organosilicon crystal-bonding adhesive;Epoxy die bond
Glue heat resistance is poor, easy xanthochromia, serious using light decay after a period of time, influences the light extraction efficiency of final products, reduces and uses
Life-span;Organosilicon crystal-bonding adhesive is mainly low folding, and its excellent temperature tolerance, electrical apparatus insulation, weatherability cause the property of LED product
Energy advantage is become apparent from, and the occupation rate of market of organosilicon crystal-bonding adhesive is stepped up.
At present, the operating time of organosilicon crystal-bonding adhesive both domestic and external is universal shorter, although in color inhibition and light decay performance than
Epoxy systems are excellent, but from the point of view of the demand in market, simply meet the minimum demand of client, client always searches for longer
Operating time, high light-emitting rate, the product of more low light attenuation.
The content of the invention
It is an object of the invention to further lift the properties of product of organosilicon crystal-bonding adhesive, meet the market demand, particularly
There is provided a kind of long light decay of operating time low LED organic silicon insulation crystal-bonding adhesives.The LED crystal-bonding adhesives have the longer operating time,
High light-emitting rate, low light attenuation (normal temperature/high temperature is lighted for a long time).
The premium properties reached for the realization present invention, technical scheme are as follows:
This LED crystal-bonding adhesives are that one-component is heating and curing Si―H addition reaction type organic silica gel, are added according to following parts by weight former
Material is uniformly mixed:
75~85 parts of methyl vinyl silicone
1~3 part of toughener
10~15 parts of crosslinking agent
1~3 part of bonding agent
3~5 parts of light decay controlling agent
0.2~2 part of inhibitor
0.1~0.5 part of catalyst
The beneficial effects of the invention are as follows:Product viscosity is adjusted by silicones viscosity, it is not viscous by adding thixotropic agent adjustment
Degree, and then improve the light emission rate of LED product;By adding light decay controlling agent, LED product normal temperature and high temperature bar are effectively reduced
Light decay rate under part;By controlling the ratio of inhibitor and catalyst, extension operable time is reached.
On the basis of above-mentioned technical proposal, the present invention can also do following improvement.
Further, the structural formula of the methyl vinyl silicone is:
(Me3SiO0.5)a(ViMe2SiO0.5)b(SiO2) (1)
Wherein, a=0.4~0.8, b=0.4~0.7, a+b=0.8~1.2;
It is using the beneficial effect of previous step:Methyl vinyl MQ resin is main body, effectively increases the entirety of crystal-bonding adhesive
Cross-link intensity, while product viscosity can be improved, it is not necessary to which thixotropic agent adjusts viscosity, reaches the problem of avoiding die drift.
Further, the toughener is methyl vinyl silicon oil, and vinyl is contained in end, side, and is at least to contain two
The organopolysiloxane of vinyl, its structure are:
Wherein, R1For-Vi;R2For-Vi or-Me, 8≤n1≤ 4,8≤n2≧4。
Further, the viscosity of above-mentioned toughener is 5000mPa.s~10000mPa.s, contents of ethylene is 0.1~
0.5wt%.
Using the beneficial effect of previous step:The toughness of crystal-bonding adhesive is improved, avoids the phenomenon to be ftractureed after glue curing.
Further, the crosslinking agent is methyl hydrogen polysiloxanes, and hydrogen content is 0.1~1.5wt%, viscosity is 10~
100mPa.s, the crosslinking agent contain hydrogen bond for end, side.Concrete structure formula such as (3)
Wherein, K1、K2For-H or-Me, and at least one is-H, 10≤n1≤ 0,15≤n2≧9。
Further, the bonding agent is one or two kinds of mixture in structural formula such as (4), (5), and mixed proportion is
Weight is than 1:1,
Wherein, n=6~8.
It is using the beneficial effect of previous step:Cementability of the crystal-bonding adhesive to various base materials is improved, ensure that consolidating for chip
It is fixed.
Further, the light decay controlling agent be structural formula such as (6),
Wherein, 10≤m≤3,3≤n≤1;
Using light decay controlling agent, the light decay after being lighted for a long time under LED product normal temperature and hot conditions is effectively reduced, is prolonged
The service life of product is grown.
Further, the inhibitor be 1- acetylene -1- cyclohexanol, the one of diethyl maleate or two kind be used in mixed way, it is excellent
Two kinds of compoundings are selected, compound proportion is weight than 1:1.
Beneficial effect using above-mentioned inhibitor is:Greatly extend product operable time at room temperature and production
The extended storage stability of product, has saved production cost.
Further, the catalyst should select platinum group catalyst, preferably platinum-vinyl siloxane complex, wherein platinum
Content is in 3000~7000ppm.
Embodiment
The principle in the present invention and feature are described below in conjunction with specific embodiment, example is intended merely to pair
Further explanation explanation of the present invention, not it is used for limiting the scope of the present invention.
Test process of the present invention:
1st, operating time method of testing;
Using automatic bonder at 35 DEG C, by the crystal-bonding adhesive dispensing in the present invention to 2835LED sky supports, record out
The time for now drawing glue whirl coating phenomenon is the operating time.
2nd, method for testing optical attenuation;
Support after above-mentioned dispensing is put in temperature programmed control baking oven and solidified, program curing:25min rises to 160 at room temperature
DEG C, 160 DEG C of insulation 2h, then take out cooling;
LED support after die bond is subjected to PLUS cleanings, bonding wire is carried out using bonding equipment after allowing;
LED support after bonding wire is being cleaned, then using moral nation9060 high folding casting glue encapsulation, according to 90
DEG C/1h+150 DEG C/4h solidifications;
Use the initial luminous flux of LED lamp bead made of the test of luminous flux tester;
Lighted using LED lamp bead fixture, test at normal temperature and 90 DEG C the light decay after 1000h is lighted respectively.
Embodiment 1
Weigh such as the methyl vinyl silicone 75g of structural formula (1), wherein a=0.5, b=0.5, a+b=1.0;Such as knot
Toughener (the n of structure formula (2)1=8, n2=6) 1g, viscosity 10000mPa.s, contents of ethylene 0.1wt%;Such as structural formula
(3) crosslinking agent (n1=10, n2=13) 11g, viscosity 100mPa.s, hydrogen content 0.1wt%;Such as the bonding of structural formula (4)
Agent 2g;Such as light decay controlling agent (m=3, n=3) 5g of structural formula (6);1- acetylene -1- cyclohexanol 2g;Platinum content is 3000ppm
Platinum-vinyl siloxane complex 0.5g, sequentially add and well mixed obtain organosilicon crystal-bonding adhesive.
Embodiment 2
Weigh such as the methyl vinyl silicone 80g of structural formula (1), wherein a=0.7, b=0.4, a+b=1.1;Such as knot
Toughener (the n of structure formula (2)1=6, n2=5) 2g, viscosity 7500mPa.s, contents of ethylene 0.3wt%;Such as structural formula (3)
Crosslinking agent (n1=5, n2=11) 13g, viscosity 50mPa.s, hydrogen content 1.0wt%;Such as the bonding agent (n of structural formula (5)
=7) 2g;Such as light decay controlling agent (m=6, n=2) 4g of structural formula (6);Diethyl maleate 1g;Platinum content is 7000ppm
Platinum-vinyl siloxane complex 0.2g, sequentially add and well mixed obtain organosilicon crystal-bonding adhesive.
Embodiment 3
Weigh such as the methyl vinyl silicone 85g of structural formula (1), wherein a=0.5, b=0.7, a+b=1.2;Such as knot
Toughener (the n of structure formula (2)1=6, n2=4) 3g, viscosity 5000mPa.s, contents of ethylene 0.5wt%;Such as structural formula (3)
Crosslinking agent (n1=1, n2=9) 15g, viscosity 15mPa.s, hydrogen content 1.5wt%;Such as the bonding agent of structural formula (4)
1.5g, such as structural formula (5) (n=6) bonding agent 1.5g;Such as light decay controlling agent (m=9, n=1) 3g of structural formula (6);1- second
Alkynes -1- cyclohexanol 1g, diethyl maleate 1g;Platinum content is 5000ppm platinum-vinyl siloxane complex 0.3g, is added successively
Enter to be well mixed and obtain organosilicon crystal-bonding adhesive.
Comparative example 1
Weigh such as the methyl vinyl silicone 75g of structural formula (1), wherein a=0.5, b=0.5, a+b=1.0;Such as knot
Toughener (the n of structure formula (2)1=8, n2=6) 1g, viscosity 10000mPa.s, contents of ethylene 0.1wt%;Such as structural formula
(3) crosslinking agent (n1=10, n2=13) 11g, viscosity 100mPa.s, hydrogen content 0.1wt%;Such as the bonding of structural formula (4)
Agent 2g;1- acetylene -1- cyclohexanol 2g;Platinum content is 3000ppm platinum-vinyl siloxane complex 0.5g, sequentially adds mixing
Uniformly obtain organosilicon crystal-bonding adhesive.
The component of comparative example 1 is compared with the component of embodiment 1, not using light decay controlling agent.
Comparative example 2
Weigh such as the methyl vinyl silicone 85g of structural formula (1), wherein a=0.5, b=0.7, a+b=1.2;Such as knot
Toughener (the n of structure formula (2)1=6, n2=4) 3g, viscosity 5000mPa.s, contents of ethylene 0.5wt%;Such as structural formula (3)
Crosslinking agent (n1=1, n2=9) 15g, viscosity 15mPa.s, hydrogen content 1.5wt%;Such as the bonding agent of structural formula (4)
1.5g, such as structural formula (5) (n=6) bonding agent 1.5g;Such as light decay controlling agent (m=9, n=1) 3g of structural formula (6);N, N,
N, N- tetramethylethylenediamine 2g;Platinum content is 5000ppm platinum-vinyl siloxane complex 0.3g, is sequentially added well mixed
Obtain organosilicon crystal-bonding adhesive.
For the component of comparative example 2 compared with the component of embodiment 3, the inhibitor of comparative example changes N, N, N, N- tetramethyl second into
Diamines.
Embodiment 1-3 and comparative example 1-2 performance parameter test result such as following table:
By embodiment 1,2,3 compared with comparative example 1, light decay controlling agent is added in formula, its light decay substantially reduces;Implement
Example 1,2,3 is inhibitor from 1- acetylene -1- cyclohexanol, diethyl maleate, hence it is evident that significantly extend compared with comparative example 2
Operating time.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention scope, it is every in the present invention
Spirit and principle within, any modification, equivalent substitution and improvements done etc. should be included in protection scope of the present invention
Within.
Claims (5)
1. the low LED organosilicon crystal-bonding adhesives of a kind of operating time long light decay, it is characterised in that include following raw material:
75~85 parts of methyl vinyl silicone
1~3 part of toughener
10~15 parts of crosslinking agent
1~3 part of bonding agent
3~5 parts of light decay controlling agent
0.2~2 part of inhibitor
0.1~0.5 part of catalyst
The structural formula of the methyl vinyl silicone is:(Me3SiO0.5)a(ViMe2SiO0.5)b(SiO2), wherein, a=0.4~
0.8, b=0.4~0.7, a+b=0.8~1.2;The light decay controlling agent be structural formula such as (6),
Wherein, 10≤m≤3,3≤n≤1.
2. crystal-bonding adhesive according to claim 1, it is characterised in that the toughener is methyl vinyl silicon oil, and viscosity is
5000mPa.s~10000mPa.s, contents of ethylene are 0.1~0.5wt%, and its structure is (2):
Wherein, R1For-Vi;R2For-Vi or-Me, 8≤n1≤ 4,8≤n2≧4。
3. crystal-bonding adhesive according to claim 1, it is characterised in that the crosslinking agent is methyl hydrogen polysiloxanes, hydrogeneous
Measure as 0.1~1.5wt%, viscosity is 10~100mPa.s, concrete structure formula such as (3)
Wherein, K1、K2For-H or-Me, and at least one is-H, 10≤n1≤ 0,15≤n2≧9。
4. crystal-bonding adhesive according to claim 1, it is characterised in that the bonding agent is one in structural formula such as (4), (5)
Kind or two kinds of mixture, mixed proportion are weight than 1:1,
Wherein, n=6~8.
5. crystal-bonding adhesive according to claim 1, it is characterised in that the inhibitor is 1- acetylene -1- cyclohexanol, maleic acid
The one of diethylester or two kind be used in mixed way, mixed proportion be weight than 1:1;Preferred platinum-the vinylsiloxane of catalyst is matched somebody with somebody
Compound, wherein platinum content is in 3000~7000ppm.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109294515A (en) * | 2018-09-29 | 2019-02-01 | 烟台德邦先进硅材料有限公司 | A kind of LED organosilicon crystal-bonding adhesive that excellent tenacity cementability is strong |
CN109536124A (en) * | 2018-12-07 | 2019-03-29 | 烟台德邦科技有限公司 | A kind of high adhesiveness LED crystal-bonding adhesive of zero fugitive constituent normal temperature storage |
CN111410932A (en) * | 2020-05-14 | 2020-07-14 | 南京科矽新材料科技有限公司 | High-flexibility and high-adhesion methyl organosilicon adhesive for L ED |
CN111471429A (en) * | 2020-05-14 | 2020-07-31 | 南京科矽新材料科技有限公司 | High-temperature-resistant yellowing organic silicon adhesive with strong adhesive property for L ED |
CN113337245A (en) * | 2021-07-26 | 2021-09-03 | 深圳市希顺有机硅科技有限公司 | Dealcoholized photovoltaic module sealant and preparation method thereof |
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CN104987853A (en) * | 2015-07-30 | 2015-10-21 | 烟台德邦先进硅材料有限公司 | Annular adhesive and synthesizing method thereof |
CN105505298A (en) * | 2015-12-11 | 2016-04-20 | 烟台德邦先进硅材料有限公司 | Organic silica gel with high self-adsorption property and preparation method thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN109294515A (en) * | 2018-09-29 | 2019-02-01 | 烟台德邦先进硅材料有限公司 | A kind of LED organosilicon crystal-bonding adhesive that excellent tenacity cementability is strong |
CN109536124A (en) * | 2018-12-07 | 2019-03-29 | 烟台德邦科技有限公司 | A kind of high adhesiveness LED crystal-bonding adhesive of zero fugitive constituent normal temperature storage |
CN111410932A (en) * | 2020-05-14 | 2020-07-14 | 南京科矽新材料科技有限公司 | High-flexibility and high-adhesion methyl organosilicon adhesive for L ED |
CN111471429A (en) * | 2020-05-14 | 2020-07-31 | 南京科矽新材料科技有限公司 | High-temperature-resistant yellowing organic silicon adhesive with strong adhesive property for L ED |
CN111410932B (en) * | 2020-05-14 | 2022-02-22 | 南京科矽新材料科技有限公司 | Methyl organosilicon adhesive with excellent flexibility and strong adhesion for LED |
CN113337245A (en) * | 2021-07-26 | 2021-09-03 | 深圳市希顺有机硅科技有限公司 | Dealcoholized photovoltaic module sealant and preparation method thereof |
CN113337245B (en) * | 2021-07-26 | 2022-03-25 | 深圳市希顺有机硅科技有限公司 | Dealcoholized photovoltaic module sealant and preparation method thereof |
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Effective date of registration: 20190215 Address after: 264006 Renewable Resource Processing Demonstration Zone No. 3-19 Kaifeng Road, Yantai Development Zone, Shandong Province Applicant after: Yantai Darbond Technology Co., Ltd. Address before: 264006 Kaifeng Road 3-3 Resource Regeneration and Processing Demonstration Zone, Yantai Development Zone, Shandong Province Applicant before: Yantai Debang Advanced Silicon Materials Co.,Ltd. |
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WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180202 |