CN107189447A - LED packaging silicon rubbers of wet-heat resisting and its preparation method and application - Google Patents
LED packaging silicon rubbers of wet-heat resisting and its preparation method and application Download PDFInfo
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- CN107189447A CN107189447A CN201710566871.3A CN201710566871A CN107189447A CN 107189447 A CN107189447 A CN 107189447A CN 201710566871 A CN201710566871 A CN 201710566871A CN 107189447 A CN107189447 A CN 107189447A
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- 238000004806 packaging method and process Methods 0.000 title claims abstract description 47
- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- -1 polysiloxane Polymers 0.000 claims abstract description 74
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 48
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000002994 raw material Substances 0.000 claims abstract description 33
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 5
- 229910020447 SiO2/2 Inorganic materials 0.000 claims description 39
- 229910020388 SiO1/2 Inorganic materials 0.000 claims description 21
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 7
- CFOAUMXQOCBWNJ-UHFFFAOYSA-N [B].[Si] Chemical compound [B].[Si] CFOAUMXQOCBWNJ-UHFFFAOYSA-N 0.000 claims description 7
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical compound [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 claims description 7
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 238000005187 foaming Methods 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- XCJXQCUJXDUNDN-UHFFFAOYSA-N chlordene Chemical compound C12C=CCC2C2(Cl)C(Cl)=C(Cl)C1(Cl)C2(Cl)Cl XCJXQCUJXDUNDN-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- YCIVSJFIXXVSRH-UHFFFAOYSA-N amino-methyl-phenylsilicon Chemical compound C[Si](N)C1=CC=CC=C1 YCIVSJFIXXVSRH-UHFFFAOYSA-N 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000010276 construction Methods 0.000 claims 1
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 claims 1
- MOSXLDGILGBOSZ-UHFFFAOYSA-N ethenyl-methyl-phenylsilicon Chemical compound C=C[Si](C)C1=CC=CC=C1 MOSXLDGILGBOSZ-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 25
- 239000003292 glue Substances 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 13
- 230000032683 aging Effects 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 4
- 238000005476 soldering Methods 0.000 abstract description 4
- 238000003860 storage Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 125000003944 tolyl group Chemical group 0.000 abstract 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 11
- 229920002545 silicone oil Polymers 0.000 description 7
- 239000000084 colloidal system Substances 0.000 description 5
- 238000001723 curing Methods 0.000 description 5
- 239000000741 silica gel Substances 0.000 description 5
- 229910002027 silica gel Inorganic materials 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- RCNRJBWHLARWRP-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane;platinum Chemical compound [Pt].C=C[Si](C)(C)O[Si](C)(C)C=C RCNRJBWHLARWRP-UHFFFAOYSA-N 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- ZMDQOPUHIXKWRO-UHFFFAOYSA-N CC1=CC=CC=C1.[Pt].C(=C)[Si](O[Si](C)(C)C=C)(C)C Chemical compound CC1=CC=CC=C1.[Pt].C(=C)[Si](O[Si](C)(C)C=C)(C)C ZMDQOPUHIXKWRO-UHFFFAOYSA-N 0.000 description 1
- 241000218202 Coptis Species 0.000 description 1
- 235000002991 Coptis groenlandica Nutrition 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000003483 aging Methods 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- MJULMZZKFYNTHK-UHFFFAOYSA-N ethenyl(phenyl)silicon Chemical compound C=C[Si]C1=CC=CC=C1 MJULMZZKFYNTHK-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 230000003335 steric effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- AACMXYCXYZGNBT-ZCFIWIBFSA-N trimethyl-[[(2R)-oxiran-2-yl]methoxy]silane Chemical group C([C@H]1CO1)O[Si](C)(C)C AACMXYCXYZGNBT-ZCFIWIBFSA-N 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
- 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
-
- 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)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Led Device Packages (AREA)
- Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to LED packaging silicon rubbers of a kind of wet-heat resisting and its preparation method and application, belong to material chemistry technical field.The LED packaging silicon rubbers of the wet-heat resisting are made up of component A and B component, wherein, part A includes：Methyl phenyl vinyl polysiloxane, platinum catalyst, add-on type tackifier；Part B includes：The hydrogeneous silicones of methyl phenyl vinyl polysiloxane, aminomethyl phenyl, reaction suppressor.The LED packaging silicon rubbers of the wet-heat resisting, by being cooperated from specific raw material, the LED packaging silicon rubbers of wet-heat resisting are obtained, improve the wet-hot aging performance of SMD devices, solve the moisture absorption during the storage of SMD devices, the problem of glue and degumming is easily split when in reflow soldering processing procedure, and then reduces risk, production efficiency is improved.
Description
Technical field
The present invention relates to material chemistry technical field, the LED packaging silicon rubbers of more particularly to a kind of wet-heat resisting and its preparation
Methods and applications.
Background technology
At present, commercialized LED illumination device is greatly the encapsulation shape using SMD (surface-adhered type) at present
Formula, and high folding LED silicones has the excellent transparency, heat resistance and anti-UV agings, therefore as the envelope of SMD devices mainly
Package material.
However, in actual application, SMD devices are after the completion of using high folding silicone encapsulation, because of sealing or envelope
The hygroscopicity and gas-premeable of package material, can absorb steam unavoidably during storage, and SMD devices need to be mounted on PCB
On circuit board, in reflow soldering processing procedure, colloid rupture and break-off easily occur for the SMD devices of the moisture absorption, so that envelope
Assembling structure is destroyed.
The content of the invention
Based on this, it is necessary in view of the above-mentioned problems, a kind of LED packaging silicon rubbers of wet-heat resisting are provided, using the wet-heat resisting
LED packaging silicon rubbers, improve the wet-hot aging performance of SMD devices, the moisture absorption during the storage of SMD devices are solved, in unleaded backflow
The problem of glue and degumming is easily split when being welded in journey, and then reduces risk, production efficiency is improved.
A kind of LED packaging silicon rubbers of wet-heat resisting, are made up of component A and B component,
The component A is prepared from by the raw material of following percentage by weight：
Methyl phenyl vinyl polysiloxane 40%-60%
Platinum catalyst 0.0002%-0.002%
Add-on type tackifier 0.1%-5%
The B component is mainly prepared from by the raw material of following percentage by weight：
Methyl phenyl vinyl polysiloxane 10%-40%
The hydrogeneous silicones 10%-45% of aminomethyl phenyl
Reaction suppressor 0.01%-0.2%
Component A and B component the raw material summation is 100%.
The LED packaging silicon rubbers of above-mentioned wet-heat resisting, select the methyl phenyl vinyl polysiloxane of specific structure, it is ensured that MDT
The intensity and pliability of type phenyl vinyl polysiloxane solidfied material simultaneously reduce the hygroscopicity of solidfied material；Also, select silicon boron type to increase
Stick, main function is to improve the cohesive force between colloid and base material, and above-mentioned silicon boron type tackifier are very big in the curing process
Raising and the bonding force of PPA and silver plated metals, such as the baking condition 170 of a standard especially after one section of high-temperature baking
DEG C/3hrs, the addition of silicon boron type tackifier improves the sealing between colloid and base material, reduces steam by colloid and base material
Between interface enter SMD devices possibility；And coordinate the hydrogeneous silicones of MDT type aminomethyl phenyls, it is ensured that the friendship of solidfied material
Join density, toughness can be lifted again, reduce the hygroscopicity of solidfied material.
In one of the embodiments, the component A is prepared from by the raw material of following percentage by weight：
Methyl phenyl vinyl polysiloxane 45%-55%
Platinum catalyst 0.0004%-0.001%
Add-on type tackifier 1%-3%
The B component is mainly prepared from by the raw material of following percentage by weight：
Methyl phenyl vinyl polysiloxane 15%-35%
The hydrogeneous silicones 25%-45% of aminomethyl phenyl
Reaction suppressor 0.05%-0.1%.
Addition of the above-mentioned methylphenyl vinyl polysiloxane in formula is preferably 45%-55%, methyl phenyl vinyl
Ratio-dependent of the addition of base silicones according to SiH/Vi, SiH/vi values are between 1-2.0, when the hydrogeneous silicones of aminomethyl phenyl
It when content is too low, cannot get a desired hardness, and when aminomethyl phenyl Silicon Containing Hydrogen resin content is too high, glue may be influenceed
The solidification of liquid.
When the addition of platinum catalyst is very few, hardening time extension, curing degree is incomplete, when addition is excessive,
Solidfied material may produce Yellowing, thus cause transparency to decline, by its addition control within the above range, with compared with
Good effect.
The addition of add-on type tackifier is preferably 1%-2%, and due adhesive effect is not had when addition is very few,
When addition is excessive, the transparency and the solidification of glue of colloid can be influenceed.
And to cause glue to have longer usage cycles and viscosity stability after mixing, selection adds reaction suppressor, and
Addition scope 0.01%~0.2%, when addition is very few, does not have good inhibition, when addition is excessive, glue
The hardening time extension of body, curing degree reduction cannot get desired hardness, addition is preferably 0.05%~0.1%.
In one of the embodiments, the methyl phenyl vinyl polysiloxane has following chemical formula：
(PhSiO3/2)a(Ph2SiO2/2)b(Me2SiO2/2)c(ViMe2SiO1/2)d
Wherein, a+b+c+d=1, and the ＜ d ＜ 0.3 of 0 ＜ a ＜, 0.6,0 ＜ b ＜, 0.4,0 ＜ C ＜ 0.4,0；
The hydrogeneous silicones of aminomethyl phenyl has following chemical formula：
(PhSiO3/2)a(Ph2SiO2/2)b(HMe2SiO1/2)c
Wherein, the ＜ C ＜ 0.4 of 0 ＜ a ＜ of a+b+c=1,0.5,0 ＜ b ＜ 0.4,0；
The add-on type tackifier are selected from silicon boron type add-on type tackifier, with following structure：
CH2OCHCH3H6(CH3O)2Si0(Ph2SiO2/2)a(MeSiO2/2)b(BO3/2)cOSi(OCH3)2CH2OCHCH3H6,
The ＜ c ＜ 0.1 of 0.7,0 ＜ b ＜ of wherein 0 ＜ a ＜ 0.3,0
When Boron contents are too high in silicon boron type tackifier, the problem of may result in deliquescence in atmosphere, therefore, control
(BO3The molar percentage of/2) c units in 0 ＜ c ＜ 0.1,
It is that phenyl, Me are that methyl, Vi are that vinyl, Si are that silicon, O are that oxygen, H are hydrogen, a, b, c, d representative structure unit by Ph
Molar average percentage in macromolecular.
In one of the embodiments, in the LED packaging silicon rubbers, SiH/Vi mol ratio is 1-2.It is preferred that 1.2-1.5.
When SiH/vi is when in this scope, curing reaction (remained in solidfied material can reactive group minimum) most completely is shown optimal
Performance, and the hygroscopicity reduction of solidfied material, moisture barrier characteristics are improved.
In one of the embodiments, in the hydrogeneous silicones of the aminomethyl phenyl, the ＜ b ＜ of 0.2 ＜ a ＜ 0.45,0.1
0.25,0.1 ＜ C ＜ 0.35, and (HMe2SiO1/2) group be end-capping group.The hydrogeneous silicones of aminomethyl phenyl is MDT type knots
Structure, strand is in " T " (PhSiO in branched shape, structure3/2) chain link plays strengthening action, " D " (Ph2SiO2/2)Chain link is then provided
" flexibility " segment, for phenyl, improves space steric effect, effectively increased wet to improve side in pliability, and D chain links
Gas barrier, the molar percentage of " T " chain link is between 0-50%, preferably 20%~45%, the molar percentage of " D " chain link
Between 0%~40%, preferably 10%-25%, M chain links are that, containing hydrogen functional group, its molar percentage is 0~40%, preferably
It is at least containing 2 M units in end-capping group, each strand for 10%~35%, especially M chain links.
In one of the embodiments, when the refractive index of the methyl phenyl vinyl polysiloxane is not less than 1.54,25 DEG C
Viscosity is 5000cps-100000cps；(being preferably 30000-60000cps), molecular weight is 200-1500, polydispersity index
(PDI) it is less than 1.3, and molecule molar content of the molecular weight less than 500 is less than 1%；
Viscosity is 200cps- when the refractive index of the hydrogeneous silicones of aminomethyl phenyl is not less than 1.54,25 DEG C
5000cps, (being preferably 1000-2000cps), molecular weight is 500-1000, and H mass fraction (is preferably for 0.1%-0.6%
0.2%-0.5%).When hydrogen content is very few, crosslink density is caused to decline, hygroscopicity increase, when hydrogen content is too high, crosslink density
Rise, but fragility increase simultaneously, pliability decline, by H content control in above range, with preferable effect.
In one of the embodiments, the platinum catalyst is selected from：The silicon of 1,3- divinyl -1,1,3,3- tetramethyls two
Oxygen alkane platinum (0), 1,3- divinyl -1,1,3,3- tetramethyl disiloxane platinum (0), chlordene closes at least one of platinum hydracid；
Preferably 1,3- divinyl -1,1,3,3- tetramethyl disiloxane platinum (0) toluene solutions, 1,3- divinyl -
1,1,3,3- tetramethyl disiloxane platinum (0) aqueous isopropanol, chlordene closes at least one of platinum hydracid aqueous isopropanol；
The reaction suppressor is selected from：At least one in ethynylcyclohexanol, many vinyl compounds, silane-modified alkynol
Kind.
In one of the embodiments, the platinum catalyst is 1,3- divinyl -1,1, the silica of 3,3- tetramethyl two
Alkane platinum (0).
The preparation method of the bright LED packaging silicon rubbers for also disclosing above-mentioned wet-heat resisting of this law, comprises the following steps：
Prepare component A：Each raw material of component A is well mixed, produced；
Prepare B component：Each raw material of B component is well mixed, produced.
The preparation method of the LED packaging silicon rubbers of above-mentioned wet-heat resisting, simple with technique, the characteristics of reliability is high can facilitate
It must be applied in industrial production.
In one of the embodiments, in the preparation component A step, each raw material is separately added into mixer, normal
Stirred under temperature, vacuumize removal foaming, produce；It is preferred that each raw material is separately added into planetary mixer, autorotation speed 35-
0.8-1.2h is stirred under 45r/min, normal temperature, stops stirring, vacuumizing and defoaming.
In the preparation B component step, each raw material is separately added into mixer, stirred at normal temperatures, is vacuumized
Foaming is removed, is produced.It is preferred that each raw material is separately added into planetary mixer, autorotation speed 35-45r/min, stirred under normal temperature
0.8-1.2h, stops stirring, vacuumizing and defoaming.
Above-mentioned normal temperature refers to 15-35 DEG C, preferably 25 DEG C.
The bright LED packaging silicon rubbers for also disclosing above-mentioned wet-heat resisting of this law are for encapsulating the application in LED.
Compared with prior art, the invention has the advantages that：
The LED packaging silicon rubbers of the wet-heat resisting of the present invention, SMD devices are improved by selecting specific raw material to cooperate
Wet-hot aging performance, solves the moisture absorption during the storage of SMD devices, asking for glue and degumming is easily split when in reflow soldering processing procedure
Topic, and then risk is reduced, improve production efficiency.
The preparation method of the LED packaging silicon rubbers of the wet-heat resisting of the present invention, simple with technique, the characteristics of reliability is high can
Facilitating to be applied in industrial production.
The LED packaging silicon rubbers of the wet-heat resisting encapsulate SMD devices in available for encapsulation LED especially with the LED packaging plastics
Part, greatly improves the wet-hot aging performance of SMD devices.
Brief description of the drawings
Fig. 1 be background technology in for LED chip and encapsulation glue coating relation schematic diagram；
Wherein：1. encapsulate glue；2. fluorescent material；3. gold thread；4. support；5. chip.
Embodiment
For the ease of understanding the present invention, the present invention is described more fully below with reference to relevant drawings.In accompanying drawing
Give presently preferred embodiments of the present invention.But, the present invention can be realized in many different forms, however it is not limited to this paper institutes
The embodiment of description.On the contrary, the purpose for providing these embodiments is to make the understanding to the disclosure more thorough
Comprehensively.
Unless otherwise defined, all of technologies and scientific terms used here by the article is with belonging to technical field of the invention
The implication that technical staff is generally understood that is identical.Term used in the description of the invention herein is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
The arbitrary and all combination of the Listed Items of pass.
Raw materials used in following examples is commercially available.
Embodiment 1
A kind of LED packaging silicon rubbers of wet-heat resisting, are made up of component A and B component,
The component A is prepared from the following materials：
Methyl phenyl vinyl polysiloxane ((PhSiO3/2)0.48(Ph2SiO2/2)0.16(Me2SiO2/2)0.09
(ViMe2SiO1/2) 0.27, viscosity is 30000cps, and refractive index is 1.543, molecular weight MW=951, PDI=1.253) 50g
Platinum catalyst (content is 5000ppm Pt-1,3,5,7 tetramethyls-divinyl silane toluene solution) 0.2g
Add-on type tackifier (boracic type tackifier,
CH2OCHCH3H6(CH3O)2Si0(Ph2SiO2/2)0.68(MeSiO2/2)0.25(BO3/2)0.07OSi(OCH3)2CH2OCHCH3H6)
1.0g
The B component is mainly prepared from the following materials：
Methyl phenyl vinyl polysiloxane ((PhSiO3/2)0.48(Ph2SiO2/2)0.16(Me2SiO2/2)0.09
(ViMe2SiO1/2) 0.27, viscosity is 30000cps, and refractive index is 1.543, molecular weight MW=951, PDI=1.253) 20g
Hydrogeneous the silicones ((PhSiO of aminomethyl phenyl3/2)0.51(Ph2SiO2/2)0.25(HMe2SiO1/2) 0.24, viscosity is
1000cps, refractive index 1.54, molecular weight mw=975, hydrogen content 0.3%) 30g
Reaction suppressor (1- ethynylcyclohexanols) 0.03g
The LED packaging silicon rubbers of the wet-heat resisting of the present embodiment, which are prepared by the following method, to be obtained：
First, component A is prepared.
Each raw material in component A is added separately in planetary mixer, 1.0h is mixed at normal temperatures, is vacuumized de-
Bubble, obtains component A.
2nd, B component is prepared.
Each raw material in B component is added separately in planetary mixer, 1.0h is mixed at normal temperatures, is vacuumized de-
Bubble, obtains B component.
Embodiment 2
A kind of LED packaging silicon rubbers of wet-heat resisting, are made up of component A and B component,
The component A is prepared from the following materials：
Methyl phenyl vinyl polysiloxane ((PhSiO3/2)0.5(Ph2SiO2/2)0.16(Me2SiO2/2)0.07
(ViMe2SiO1/2) 0.27, viscosity is 40000cps, and refractive index is 1.545, molecular weight MW=1025, PDI=1.237) 50g
Platinum catalyst (content is 5000ppm Pt-1,3,5,7 tetramethyls-divinyl silane toluene solution) 0.2g
Add-on type tackifier (boracic type tackifier,
CH2OCHCH3H6(CH3O)2Si0(Ph2SiO2/2)0.68(MeSiO2/2)0.25(BO3/2)0.07OSi(OCH3)2CH2OCHCH3H6)
1.0g
The B component is mainly prepared from the following materials：
Methyl phenyl vinyl polysiloxane ((PhSiO3/2)0.5(Ph2SiO2/2)0.16(Me2SiO2/2)0.07
(ViMe2SiO1/2) 0.27, viscosity is 40000cps, and refractive index is 1.545, molecular weight MW=1025, PDI=1.237) 15g
Hydrogeneous the silicones ((PhSiO of aminomethyl phenyl3/2)0.48(Ph2SiO2/2)0.27(HMe2SiO1/2) 0.25, viscosity is
2000cps, refractive index 1.54, molecular weight mw=700, hydrogen content 0.25%) 35g
Reaction suppressor (1- ethynylcyclohexanols) 0.03g
The LED packaging silicon rubbers of the wet-heat resisting of the present embodiment, which are prepared by the following method, to be obtained：
First, component A is prepared.
Each raw material in component A is added separately in planetary mixer, 1.0h is mixed at normal temperatures, is vacuumized de-
Bubble, obtains component A.
2nd, B component is prepared.
Each raw material in B component is added separately in planetary mixer, 1.0h is mixed at normal temperatures, is vacuumized de-
Bubble, obtains B component.
Embodiment 3
A kind of LED packaging silicon rubbers of wet-heat resisting, are made up of component A and B component,
The component A is prepared from the following materials：
Methyl phenyl vinyl polysiloxane ((PhSiO3/2)0.51(Ph2SiO2/2)0.15(Me2SiO2/2)0.07
(ViMe2SiO1/2) 0.27, viscosity is 45000cps, and refractive index is 1.543, molecular weight MW=1105, PDI=1.221) 50g
Platinum catalyst (content is 5000ppm Pt-1,3,5,7 tetramethyls-divinyl silane toluene solution)
0.2g
Add-on type tackifier (boracic type tackifier,
CH2OCHCH3H6(CH3O)2Si0(Ph2SiO2/2)0.68(MeSiO2/2)0.25(BO3/2)0.07OSi(OCH3)2CH2OCHCH3H6) 1.0g
The B component is mainly prepared from the following materials：
Methyl phenyl vinyl polysiloxane (((PhSiO3/2)0.51(Ph2SiO2/2)0.15(Me2SiO2/2)0.07
(ViMe2SiO1/2) 0.27, viscosity is 45000cps, and refractive index is 1.543, molecular weight MW=1105, PDI=1.221) 12g
Hydrogeneous the silicones ((PhSiO of aminomethyl phenyl3/2)0.48(Ph2SiO2/2)0.27(HMe2SiO1/2) 0.25 viscosity is
2000cps, refractive index 1.54, molecular weight mw=700, hydrogen content 0.25%) 38g
Reaction suppressor (1- ethynylcyclohexanols) 0.03g
The LED packaging silicon rubbers of the wet-heat resisting of the present embodiment, which are prepared by the following method, to be obtained：
First, component A is prepared.
Each raw material in component A is added separately in planetary mixer, 1.0h is mixed at normal temperatures, is vacuumized de-
Bubble, obtains component A.
2nd, B component is prepared.
Each raw material in B component is added separately in planetary mixer, 1.0h is mixed at normal temperatures, is vacuumized de-
Bubble, obtains B component.
Embodiment 4
A kind of LED packaging silicon rubbers of wet-heat resisting, are made up of component A and B component,
The component A is prepared from the following materials：
Methyl phenyl vinyl polysiloxane ((PhSiO3/2)0.52(Ph2SiO2/2)0.15(Me2SiO2/2)0.08
(ViMe2SiO1/2) 0.25, viscosity is 50000cps, and refractive index is 1.543, molecular weight MW=1208, PDI=1.228) 50g
Platinum catalyst (content is 5000ppm Pt-1,3,5,7 tetramethyls-divinyl silane toluene solution) 0.2g
Add-on type tackifier (boracic type tackifier,
CH2OCHCH3H6(CH3O)2Si0(Ph2SiO2/2)0.68(MeSiO2/2)0.25(BO3/2)0.07OSi(OCH3)2CH2OCHCH3H6)
1.0g
The B component is mainly prepared from the following materials：
Methyl phenyl vinyl polysiloxane ((PhSiO3/2)0.52(Ph2SiO2/2)0.15(Me2SiO2/2)0.08
(ViMe2SiO1/2) 0.25, viscosity is 50000cps, and refractive index is 1.543, molecular weight MW=1208, PDI=1.228) 8g
Hydrogeneous the silicones ((PhSiO of aminomethyl phenyl3/2)0.51(Ph2SiO2/2)0.25(HMe2SiO1/2) 0.24, viscosity is
2000cps, refractive index 1.54, molecular weight mw=700, hydrogen content 0.2%) 42g
Reaction suppressor (1- ethynylcyclohexanols) 0.03g
The LED packaging silicon rubbers of the wet-heat resisting of the present embodiment, which are prepared by the following method, to be obtained：
First, component A is prepared.
Each raw material in component A is added separately in planetary mixer, 1.0h is mixed at normal temperatures, is vacuumized de-
Bubble, obtains component A.
2nd, B component is prepared.
Each raw material in B component is added separately in planetary mixer, 1.0h is mixed at normal temperatures, is vacuumized de-
Bubble, obtains B component.
Embodiment 5
A kind of LED packaging silicon rubbers of wet-heat resisting, are made up of component A and B component,
The component A is prepared from the following materials：
Methyl phenyl vinyl polysiloxane ((PhSiO3/2)0.53(Ph2SiO2/2)0.17(Me2SiO2/2)0.04
(ViMe2SiO1/2) 0.26, viscosity is 50000cps, and refractive index is 1.543, molecular weight MW=1208, PDI=1.228) 50g
Platinum catalyst (content is 5000ppm Pt-1,3,5,7 tetramethyls-divinyl silane toluene solution) 0.2g
Add-on type tackifier (boracic type tackifier,
CH2OCHCH3H6(CH3O)2Si0(Ph2SiO2/2)0.68(MeSiO2/2)0.25(BO3/2)0.07OSi(OCH3)2CH2OCHCH3H6)
1.0g
The B component is mainly prepared from the following materials：
Methyl phenyl vinyl polysiloxane ((PhSiO3/2)0.52(Ph2SiO2/2)0.17(Me2SiO2/2)0.04
(ViMe2SiO1/2) 0.26, viscosity is 50000cps, and refractive index is 1.543, molecular weight MW=1208, PDI=1.228) 5g
Hydrogeneous the silicones ((PhSiO of aminomethyl phenyl3/2)0.51(Ph2SiO2/2)0.25(HMe2SiO1/2) 0.24, viscosity is
1500cps, refractive index 1.54, molecular weight mw=600, hydrogen content 0.25%) 45g
Reaction suppressor (1- ethynylcyclohexanols) 0.03g
The LED packaging silicon rubbers of the wet-heat resisting of the present embodiment, which are prepared by the following method, to be obtained：
First, component A is prepared.
Each raw material in component A is added separately in planetary mixer, 1.0h is mixed at normal temperatures, is vacuumized de-
Bubble, obtains component A.
2nd, B component is prepared.
Each raw material in B component is added separately in planetary mixer, 1.0h is mixed at normal temperatures, is vacuumized de-
Bubble, obtains B component.
Comparative example 1
A kind of LED packaging silicon rubbers of wet-heat resisting, substantially similar to the silica gel of embodiment 1, difference is：
Component A in this comparative example 1 is added with 6g methyl phenyl vinyl silicone oils.
Comparative example 2
A kind of LED packaging silicon rubbers of wet-heat resisting, substantially similar to the silica gel of embodiment 2, difference is：
Silicon boron type tackifier in this comparative example 2 replace with SHIN-ETSU HANTOTAI's chemistry KBM-403 tackifier, and the composition of the tackifier is
R- glycidoxy trimethyl silanes.
Comparative example 3
A kind of LED packaging silicon rubbers of wet-heat resisting, substantially similar to the silica gel of embodiment 3, difference is：
B component in this comparative example 3 is added with 5g containing hydrogen silicone oil, and the composition of the containing hydrogen silicone oil is tetramethyl diphenyl three
Siloxanes, structure such as following formula：
Comparative example 4
A kind of LED packaging silicon rubbers of wet-heat resisting, substantially similar to the silica gel of embodiment 4, difference is：
Component A in this comparative example 4 is added with 6g vinyl silicone oil, the structural formula such as following formula of the vinyl silicone oil：
Comparative example 5
A kind of LED packaging silicon rubbers of wet-heat resisting, substantially similar to the silica gel of embodiment 5, difference is：
The methyl and phenyl hydrogen-containing silicon oil of methyl phenyl vinyl silicone oil and 6g of the B component added with 6g in this comparative example 5,
The composition of the methyl phenyl vinyl silicone oil such as following formula：
The composition of the methyl and phenyl hydrogen-containing silicon oil such as following formula：
Experimental example
The LED packaging plastics that not be the same as Example and comparative example are prepared into wet-heat resisting carry out performance test.
Test side's method is as follows：
1st, A agent, B agent are well mixed with certain proportion, dispensing on SMD5050 pasters；
2nd, 80 DEG C/1hrs+170 DEG C/3hrs baking-curings；
3rd, the SMD5050 pasters being cured are put into constant temperature and humidity machine, humidity RH=85%, temperature Ta=85%；Point
24h, 48h, 72h are not placed；
4th, paster is taken out, is recovered 20 minutes in standard laboratory,
5th, reflow soldering processing procedure is carried out, 260 DEG C/30s, is crossed 3 times, record splits glue and degumming quantity；Split glue or degumming note
For failure.
Test result is as shown in the table.
Each LED packaging plastics formula of table 1. and the performance test results
As can be seen that the consumption of hydrogeneous silicones increases (Vi/SiH values are from small to large) in being formulated in from the above,
The hardness of cured glue body rises, and showing as the decline of MSL test failures percentage, (optimal result is embodiment 4vi/SiH=1/
1.5), but when adding phenyl-vinyl silicon oil in formula, the hardness of cured glue body declines, and shows as MSL test failures hundred
Rate is divided to rise.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope of this specification record is all considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and it describes more specific and detailed, but simultaneously
Can not therefore it be construed as limiting the scope of the patent.It should be pointed out that coming for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. the LED packaging silicon rubbers of a kind of wet-heat resisting, it is characterised in that be made up of component A and B component,
The component A is prepared from by the raw material of following percentage by weight：
Methyl phenyl vinyl polysiloxane 40%-60%
Platinum catalyst 0.0002%-0.002%
Add-on type tackifier 0.1%-5%
The B component is mainly prepared from by the raw material of following percentage by weight：
Methyl phenyl vinyl polysiloxane 10%-40%
The hydrogeneous silicones 10%-45% of aminomethyl phenyl
Reaction suppressor 0.01%-0.2%
Component A and B component the raw material summation is 100%.
2. the LED packaging silicon rubbers of wet-heat resisting according to claim 1, it is characterised in that the component A is by following weight hundred
The raw material of ratio is divided to be prepared from：
Methyl phenyl vinyl polysiloxane 45%-55%
Platinum catalyst 0.0004%-0.001%
Add-on type tackifier 1%-3%
The B component is mainly prepared from by the raw material of following percentage by weight：
Methyl phenyl vinyl polysiloxane 15%-35%
The hydrogeneous silicones 25%-45% of aminomethyl phenyl
Reaction suppressor 0.05%-0.1%.
3. the LED packaging silicon rubbers of wet-heat resisting according to claim 1 or 2, it is characterised in that the methyl phenyl vinyl
Silicones has following chemical formula：
(PhSiO3/2)a(Ph2SiO2/2)b(Me2SiO2/2)c(ViMe2SiO1/2)d
Wherein, a+b+c+d=1, and the ＜ d ＜ 0.3 of 0 ＜ a ＜, 0.6,0 ＜ b ＜, 0.4,0 ＜ C ＜ 0.4,0；
The hydrogeneous silicones of aminomethyl phenyl has following chemical formula：
(PhSiO3/2)a(Ph2SiO2/2)b(HMe2SiO1/2)c
Wherein, the ＜ C ＜ 0.4 of 0 ＜ a ＜ of a+b+c=1,0.5,0 ＜ b ＜ 0.4,0；
The add-on type tackifier are selected from silicon boron type add-on type tackifier, with following structure：
CH2OCHCH3H6(CH3O)2Si0(Ph2SiO2/2)a(MeSiO2/2)b(BO3/2)cOSi(OCH3)2CH2OCHCH3H6；Its
In, Ph is that phenyl, Me are that methyl, B are boron atom, and a, b, c represent the molar average percentage of each construction unit in the molecule respectively
Rate, wherein the ＜ c ＜ 0.1 of 0 ＜ a ＜, 0.7,0 ＜ b ＜ 0.3,0
Ph is that phenyl, Me are that methyl, Vi are that vinyl, Si are that silicon, O are that oxygen, H are hydrogen, and a, b, c, d representative structure unit are dividing greatly
Molar average percentage in son.
4. the LED packaging silicon rubbers of wet-heat resisting according to claim 3, it is characterised in that in the LED packaging silicon rubbers,
SiH/Vi mol ratio is 1-2.
5. the LED packaging silicon rubbers of wet-heat resisting according to claim 3, it is characterised in that the aminomethyl phenyl Silicon Containing Hydrogen tree
In fat, the ＜ C ＜ 0.35 of 0.2 ＜ a ＜, 0.45,0.1 ＜ b ＜ 0.25,0.1, and (HMe2SiO1/2) group be end-capping group.
6. the LED packaging silicon rubbers of wet-heat resisting according to claim 3, it is characterised in that the methyl phenyl vinyl silicon
Viscosity is 5000cps-100000cps when the refractive index of resin is not less than 1.54,25 DEG C；, molecular weight is 200-1500, polydispersion
Sex index is less than 1.3, and molecule molar content of the molecular weight less than 500 is less than 1%；
Viscosity is 200cps-5000cps when the refractive index of the hydrogeneous silicones of aminomethyl phenyl is not less than 1.54,25 DEG C, point
Son amount is 500-1000, and H mass fraction is 0.1%-0.6%.
7. the LED packaging silicon rubbers of wet-heat resisting according to claim 1 or 2, it is characterised in that the platinum catalyst choosing
From：1,3- divinyl -1,1,3,3- tetramethyl disiloxane platinum (0), 1,3- divinyl -1,1, the silica of 3,3- tetramethyl two
Alkane platinum (0), chlordene closes at least one of platinum hydracid
The reaction suppressor is selected from：At least one of ethynylcyclohexanol, many vinyl compounds, silane-modified alkynol.
8. the preparation method of the LED packaging silicon rubbers of the wet-heat resisting described in claim any one of 1-7, it is characterised in that including with
Lower step：
Prepare component A：Each raw material of component A is well mixed, produced；
Prepare B component：Each raw material of B component is well mixed, produced.
9. the preparation method of the LED packaging silicon rubbers of wet-heat resisting according to claim 8, it is characterised in that
In the preparation component A step, each raw material is separately added into mixer, stirred at normal temperatures, removal is vacuumized
Foaming, is produced；
In the preparation B component step, each raw material is separately added into mixer, stirred at normal temperatures, removal is vacuumized
Foaming, is produced.
10. the LED packaging silicon rubbers of the wet-heat resisting described in claim any one of 1-7 are for encapsulating the application in LED.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110922939A (en) * | 2019-12-16 | 2020-03-27 | 苏州瑞力博新材科技有限公司 | Organosilicon gel with conductivity |
| CN113025054A (en) * | 2019-12-25 | 2021-06-25 | 新特能源股份有限公司 | Silicon rubber composition, preparation method thereof and packaging adhesive |
| CN114316896A (en) * | 2022-01-17 | 2022-04-12 | 江苏斯迪克新材料科技股份有限公司 | Silicon gel, preparation method and protective film applying silicon gel |
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| US20140024796A1 (en) * | 2012-07-19 | 2014-01-23 | Shin-Etsu Chemical Co., Ltd. | Curable silicone resin composition |
| CN103834178A (en) * | 2014-02-28 | 2014-06-04 | 广东恒大新材料科技有限公司 | Organic silicon resin as well as preparation method and application thereof |
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| US20140024796A1 (en) * | 2012-07-19 | 2014-01-23 | Shin-Etsu Chemical Co., Ltd. | Curable silicone resin composition |
| CN103013431A (en) * | 2012-12-03 | 2013-04-03 | 烟台德邦先进硅材料有限公司 | High-refractivity LED (Light-Emitting Diode) package silica gel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110922939A (en) * | 2019-12-16 | 2020-03-27 | 苏州瑞力博新材科技有限公司 | Organosilicon gel with conductivity |
| CN110922939B (en) * | 2019-12-16 | 2021-10-22 | 苏州瑞力博新材科技有限公司 | Organosilicon gel with conductivity |
| CN113025054A (en) * | 2019-12-25 | 2021-06-25 | 新特能源股份有限公司 | Silicon rubber composition, preparation method thereof and packaging adhesive |
| CN114316896A (en) * | 2022-01-17 | 2022-04-12 | 江苏斯迪克新材料科技股份有限公司 | Silicon gel, preparation method and protective film applying silicon gel |
| CN114316896B (en) * | 2022-01-17 | 2023-08-25 | 江苏斯迪克新材料科技股份有限公司 | Silica gel, preparation method and protective film using silica gel |
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