CN106751893A - A kind of refractive power LED encapsulation add-on type liquid silicon rubbers high and preparation method thereof - Google Patents
A kind of refractive power LED encapsulation add-on type liquid silicon rubbers high and preparation method thereof Download PDFInfo
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- CN106751893A CN106751893A CN201611097117.1A CN201611097117A CN106751893A CN 106751893 A CN106751893 A CN 106751893A CN 201611097117 A CN201611097117 A CN 201611097117A CN 106751893 A CN106751893 A CN 106751893A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- 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
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- 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
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- 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
Abstract
The invention discloses a kind of refractive power LED encapsulation add-on type liquid silicon rubbers high and preparation method thereof, it is 1 by component A and B component that described liquid silastic is in mass ratio:1~10:1 composition；Wherein, component A is made up of according to a certain ratio base rubber, phenyl hydrogen containing siloxane and alkynol class inhibitor；B component is made up of according to a certain ratio the platinum complex compound that base rubber, phenyl are coordinated, base rubber is made up of according to a certain ratio a kind of methyl base organopolysiloxane of ethenyl blocking with methyl vinyl phenyl silicones, liquid silastic of the invention has excellent mobility, and solidfied material has excellent electrical insulating property, waterproof seal, resisting etiolation, anti-aging and cold-and-heat resistent alternation performance；Solidfied material is in water white transparency colloid, there is fabulous adhesion and sealing to PPA and metal, through strict test, is not cracked, non-sclerous, light transmittance is high, refractive index is high, heat endurance good.The need for fully meeting LED pasters (SMD) encapsulation and integrated optical source (COB) encapsulation field.
Description
Technical field
It is to be related to a kind of refractive power LED encapsulation high to use specifically the present invention relates to a kind of liquid silastic and preparation method thereof
Liquid silastic and preparation method thereof, belongs to silastic material technical field.
Background technology
LED (Light Emitting Diode), light emitting diode is a kind of semiconductor devices of solid-state, and it can be straight
Connect and electricity is converted into light.The electric energy of light emitting diode (LED) consumption of super brightness is only the 1/10 of conventional light source, with not making
The advantages of with the mercury of severe contamination environment, small volume, long lifespan, the lighting sources such as incandescent lamp are replaced substantially, as the 4th
For lighting source.
LED encapsulation materials can be divided mainly into epoxy resin, makrolon, polymethyl methacrylate, ultra-clear glasses and
The transparent material high such as organosilicon material.Wherein makrolon, polymethyl methacrylate, ultra-clear glasses etc. only can be used as LED
Outer shell lens；Epoxy resin, modified epoxy resin, organosilicon material etc. are mainly as LED chip encapsulating material, it is also possible to make
It is outer shell lens.Because organosilicon material has the advantages that other materials are difficult to substitute, such as heatproof, resistance to discoloration, current property high
Energy organosilicon material has become the primary study direction of high-end LED encapsulation material.LED chip is encapsulated to organosilicon encapsulating material
Major requirement have：With high transmission rate, heat endurance is good, stress is small, to substrate bonding good (cohesional failure) etc., the present invention
In set and to product index of refraction reach more than 1.54, have appropriate mobility before curing, shape, release property is good, solidification
High transparency, high rigidity, high intensity afterwards, the features such as can keep high transparency under hot and humid environment, have pole to PPA and metal
Good adhesion and sealing, through strict test, are not cracked, non-sclerous, light transmittance is high, refractive index is high, heat endurance good, in future
To have a wide range of applications in high-power LED encapsulation.
The content of the invention
For achieving the above object, the technical solution adopted by the present invention is as follows：
A kind of refractive power LED encapsulation high add-on type liquid silicon rubber (refractive power LED packaging plastics referred to as high) and preparation method thereof.
It is 1 by component A and B component that described liquid silastic is in mass ratio:1~10:1 composition；Wherein, component A be by base rubber,
Phenyl hydrogen containing siloxane and alkynol class inhibitor are constituted according to a certain ratio；B component is that the platinum being coordinated by base rubber, phenyl is complexed
Thing is constituted according to a certain ratio, and the base rubber is by the aminomethyl phenyl organopolysiloxane and methyl ethylene of a kind of ethenyl blocking
Phenyl polysiloxane is constituted according to a certain ratio.The preparation of described liquid silastic include the preparation of silicone oil, phenyl polysiloxane prepare,
Four steps such as prepared by base rubber, component A/B component preparation.
A, prepare silicone oil
Methyl vinyl phenyl polysiloxanes is by tetramethyl divinyl disiloxane, octaphenylcyclotetrasiloxane and eight first
Basic ring tetrasiloxane under silanol potassium catalytic action copolymerization and obtain, viscosity be 500~10000cp, contents of ethylene be 0.3
~1.5wt.%, phenyl content are 15~25wt.%
B, prepare phenyl polysiloxane
Methyl vinyl phenyl silicones is by phenyl trichlorosilane, vinyl trichlorosilane, tetraethyl orthosilicate, pregnancy
The hydrolysis of base disiloxane is obtained, and contents of ethylene is 0.8~2.5wt.%, and phenyl content is 10~45%.
Phenyl hydrogen containing siloxane is by octaphenylcyclotetrasiloxane, tetramethyl-ring tetrasiloxane, the silica of prestox ring four
Alkane and HMDO copolymerization, hydrogen content are 0.5~1.0wt.%, and phenyl content is for 5~15wt.% degree of polymerization
20~50.
C, preparation base rubber
(1) the methyl vinyl phenyl silicones of the dimethylbenzene of 100-200KG and 100-200KG, is added into closed stirring
In kettle；The methyl vinyl phenyl polysiloxanes of 100KG is subsequently adding, is stirred 1-2 hours at a temperature of 40 DEG C；
(2) stirred 2-4 hours at a temperature of, being warming up to 40 DEG C；
(3) the methyl vinyl phenyl polysiloxanes of 100KG, is subsequently adding, is stirred 1-2 hours at a temperature of 40 DEG C；
(4) and then it is warmed up to 140 DEG C, is vacuumized under 200 handkerchief vacuum conditions 2~4 hours, obtains final product described base rubber；
D, A/B component prepare component A
It is prepared by component A
Base rubber 100KG is taken, phenyl 1~10KG of hydrogen containing siloxane, 0.02~0.1KG of composite inhibitor is added, viscosified
Agent 0.5-3KG, is well mixed in A agent special-purpose stirring machines, obtains final product described component A；
The compositing formula of B component is as follows：
Take base rubber 100KG, the mass parts of platinum complex compound 0.1~0.5 of phenyl coordination；Mix in B agent special-purpose stirring machines
Uniformly, described B component is obtained final product；
Obtained component A and B component are pressed into certain mass than separately packaging, described refractive power LED packaging plastic glue high is obtained final product
Water.
Product canonical parameter index is as follows：
Compared with prior art, the beneficial effects of the invention are as follows：Set in the present invention and to product index of refraction reach 1.54
More than, there is appropriate mobility before curing, shape, release property is good, high transparency, high rigidity, high intensity after solidification, in height
The features such as high transparency being kept under warm high humidity environment.There is fabulous adhesion and sealing to PPA and metal, through strict test,
It is not cracked, non-sclerous, light transmittance is high, refractive index is high, heat endurance good, widely should will has in following high-power LED encapsulation
With value.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1：Prepare high refractive index LED paster (SMD) packaging silicon rubber
A, preparation base rubber
It is 0.8wt.% by the dimethylbenzene of 50KG and 100KG contents of ethylene, phenyl content is the ethylene methacrylic of 32wt%
Base phenyl polysiloxane is added in 500 liters of closed stirred tanks, is stirred 2 hours at room temperature, silicones is fully dissolved with dimethylbenzene；So
It is 1000cp, the methyl ethylene benzene that contents of ethylene is 0.65wt.%, phenyl content is 25wt.% to add 100KG viscosity afterwards
Based polysiloxane, stirs 1 hour at a temperature of 40；Then 140 DEG C being warmed up to again, being vacuumized and is deviate from dimethylbenzene, base rubber is obtained.
B, preparation component A
Base rubber 200kg is taken, the platinum catalyst of 0.6kg phenyl coordination is added, is well mixed, obtain final product described component A；
C, preparation B component
Base rubber 200kg is taken, 4.5kg hydrogen contents is added for 1.0wt.%, phenyl content is the hydrogeneous poly- silica of 15wt.%
Alkane, the hydrogeneous tackifier of 4KG and 0.08kg composite inhibitors, are well mixed, and obtain final product described B component；
D, by obtained component A and B component 1：1 is well mixed, and 150 × 150 are fabricated under the conditions of 150 DEG C/120min
The test piece of × 2mm, carries out physical property measurement, and test result is shown in Table 1.
The physical property measurement result of the liquid silastic obtained by table 1
After obtained glue is packaged solid people to LED pasters, do not ftracture to PPA substrate bondings firmly, non yellowing.
Embodiment 2：Prepare high refractive index LED (COB) integrated optical source packaging silicon rubber
A, preparation base rubber
It is 0.8wt.% by the dimethylbenzene of 50KG and 100KG contents of ethylene, phenyl content is the ethylene methacrylic of 45wt%
Base phenyl polysiloxane is added in 500 liters of closed stirred tanks, is stirred 2 hours at room temperature, silicones is fully dissolved with dimethylbenzene；So
It is 500cp, the methyl vinyl phenyl that contents of ethylene is 1.2wt.%, phenyl content is 25wt.% to add 100KG viscosity afterwards
Polysiloxanes, stirs 1 hour at a temperature of 40；Then 140 DEG C being warmed up to again, being vacuumized and is deviate from dimethylbenzene, base rubber is obtained.
B, preparation component A
Base rubber 200kg is taken, the platinum catalyst of 0.5kg phenyl coordination is added, is well mixed, obtain final product described component A；
C, preparation B component
Base rubber 200kg is taken, 4.5kg hydrogen contents is added for 1.0wt.%, phenyl content is the hydrogeneous poly- silica of 15wt.%
Alkane, the hydrogeneous tackifier of 4KG and 0.08kg composite inhibitors, are well mixed, and obtain final product described B component；
D, by obtained component A and B component 1：1 is well mixed, and 150 × 150 are fabricated under the conditions of 150 DEG C/120min
The test piece of × 2mm, carries out physical property measurement, and test result is shown in Table 2.
The physical property measurement result of the liquid silastic obtained by table 2
After obtained glue is packaged solid people to LED integrated optical sources, do not ftracture to PPA substrate bondings firmly, it is not yellow
Become.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding can carry out various changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.
Claims (8)
1. a kind of refractive power LED packaging plastics high, it is characterised in that：In mass ratio it is 1 by component A and B component:1~10:1 composition；
Wherein, the compositing formula of component A includes the mass parts of base rubber 100, the mass parts of phenyl hydrogen containing siloxane 1~10, alkynol class
The mass parts of inhibitor 0.02~0.1, tackifier 0.5-3 mass parts, the compositing formula of B component includes the mass parts of base rubber 100, phenyl
The mass parts of platinum complex compound 0.1~0.5 of coordination；
The compositing formula of the base rubber includes the mass parts of methyl vinyl phenyl polysiloxanes 100, methyl vinyl phenyl silicon tree
Fat 100-200 mass parts, dimethylbenzene 100-200 mass parts；
Described methyl vinyl phenyl polysiloxanes is for 500~10000cp, contents of ethylene are in 25 DEG C of viscosity of measure
0.3~1.5wt.%, phenyl content are the organopolysiloxane of the ethenyl blocking of 15~25wt.%；Described ethylene methacrylic
Base phenyl silicon tree is white powder, and contents of ethylene is 0.8~2.5wt.%, and phenyl content is 10~45wt.%；Described
Tackifier are hydrogeneous tackifier.
2. refractive power LED packaging plastics high according to claim 1, it is characterised in that：Described platinum complex compound is by chlorine platinum
Acid is coordinated synthesis with vinyl benzene base silane, and platinum content therein is 1000~3000ppm.
3. refractive power LED packaging plastics high according to claim 1, it is characterised in that：Described phenyl hydrogen containing siloxane is
By octaphenylcyclotetrasiloxane, tetramethyl-ring tetrasiloxane, octamethylcy-clotetrasiloxane and HMDO copolymerization,
Hydrogen content is 0.5~1.0wt.%, and phenyl content is that 5~15wt.% degree of polymerization is 20~50.
4. refractive power LED packaging plastics high according to claim 1, it is characterised in that：Described alkynol class inhibitor is by second
Alkenyl cyclotetrasiloxane and 2- methyl -3- butyne-2-alcohols are 1 in mass ratio:1 mixes.
5. refractive power LED packaging plastics high according to claim 1, it is characterised in that：The poly- silicon of described methyl vinyl phenyl
Oxygen alkane is to be catalyzed to make in silanol potassium by tetramethyl divinyl disiloxane, octaphenylcyclotetrasiloxane and octamethylcy-clotetrasiloxane
Obtained with lower copolymerization.Viscosity be 500~10000cp, contents of ethylene be 0.3~1.5wt.%, phenyl content be 0.2~
2.5wt.%.
6. refractive power LED packaging plastics high according to claim 1, it is characterised in that：Described methyl vinyl phenyl silicon tree
Fat is that, by phenyl trichlorosilane, vinyl trichlorosilane, tetraethyl orthosilicate, HMDO hydrolysis are obtained.Vinyl
Content is 0.8~2.5wt.%, and phenyl content is 1.0~2.5wt.%.
7. refractive power LED packaging plastics high according to claim 6, it is characterised in that：Described hydrogeneous tackifier are tetramethyl
Two hydrogen-based -1- glycidyl ethers -4- ethyls-trimethoxy silane basic ring tetrasiloxane, it is by tetramethyl-ring tetrasiloxane
It is obtained with acrylic glycidol ether, vinyltrimethoxy silane addition reaction.
8. a kind of refractive power LED packaging plastic preparation methods high prepared described in claim 1, it is characterised in that comprise the following steps：
A, preparation base rubber
(1), by the methyl vinyl phenyl silicones closed stirred tank of addition of the dimethylbenzene of 100-200KG and 100-200KG；
The methyl vinyl phenyl polysiloxanes of 100KG is subsequently adding, is stirred 1-2 hours at a temperature of 40 DEG C；.
(2) stirred 2-4 hours at a temperature of, being warming up to 40 DEG C；
(3) the methyl vinyl phenyl polysiloxanes of 100KG, is subsequently adding, is stirred 1-2 hours at a temperature of 40 DEG C；
(4) and then it is warmed up to 140 DEG C, is vacuumized under 200 handkerchief vacuum conditions 2~4 hours, obtains final product described base rubber；
B, preparation component A
Base rubber 100KG is taken, phenyl 1~10KG of hydrogen containing siloxane, 0.02~0.1KG of composite inhibitor, tackifier is added
0.5-3KG, is well mixed in A agent special-purpose stirring machines, obtains final product described component A；
The compositing formula of B component is as follows：
Take base rubber 100KG, the mass parts of platinum complex compound 0.1~0.5 of phenyl coordination；It is well mixed in B agent special-purpose stirring machines,
Obtain final product described B component；
C, obtained component A and B component are pressed certain mass than separately packaging, obtain final product described refractive power LED packaging plastic glue high.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286900A (en) * | 2017-06-19 | 2017-10-24 | 合肥市惠科精密模具有限公司 | A kind of high index of refraction modified silica-gel encapsulated for Micro LED displays |
| CN108559398A (en) * | 2018-01-10 | 2018-09-21 | 广东天跃新材料股份有限公司 | A kind of environmental-friendly silicon rubber leather and its coating process |
| CN109266013A (en) * | 2018-09-07 | 2019-01-25 | 苏州歌诗夫新材料有限公司 | Height refraction, color inhibition add-on type silica gel material and preparation method thereof |
| CN109817789A (en) * | 2018-12-25 | 2019-05-28 | 广州硅能照明有限公司 | A kind of COB encapsulation and preparation method thereof |
| CN110272627A (en) * | 2019-07-24 | 2019-09-24 | 杭州之江新材料有限公司 | A kind of silicon gel of high refractive index and preparation method thereof |
| CN115433541A (en) * | 2022-09-30 | 2022-12-06 | 郑州中原思蓝德高科股份有限公司 | Conductive adhesive and preparation method thereof |
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| CN103122149A (en) * | 2013-03-18 | 2013-05-29 | 株洲时代新材料科技股份有限公司 | Silicon rubber with high refractive index and high transparency for optical encapsulation and preparation method thereof |
| CN103589387A (en) * | 2013-11-20 | 2014-02-19 | 广州集泰化工有限公司 | High-strength bonding room temperature curing organosilicone potting adhesive for LED (light-emitting diode) and preparation method of adhesive |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107286900A (en) * | 2017-06-19 | 2017-10-24 | 合肥市惠科精密模具有限公司 | A kind of high index of refraction modified silica-gel encapsulated for Micro LED displays |
| CN108559398A (en) * | 2018-01-10 | 2018-09-21 | 广东天跃新材料股份有限公司 | A kind of environmental-friendly silicon rubber leather and its coating process |
| CN109266013A (en) * | 2018-09-07 | 2019-01-25 | 苏州歌诗夫新材料有限公司 | Height refraction, color inhibition add-on type silica gel material and preparation method thereof |
| CN109817789A (en) * | 2018-12-25 | 2019-05-28 | 广州硅能照明有限公司 | A kind of COB encapsulation and preparation method thereof |
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| CN110272627A (en) * | 2019-07-24 | 2019-09-24 | 杭州之江新材料有限公司 | A kind of silicon gel of high refractive index and preparation method thereof |
| CN115433541A (en) * | 2022-09-30 | 2022-12-06 | 郑州中原思蓝德高科股份有限公司 | Conductive adhesive and preparation method thereof |
| CN115433541B (en) * | 2022-09-30 | 2023-11-07 | 郑州中原思蓝德高科股份有限公司 | Conductive adhesive and preparation method thereof |
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