CN105368004A - High-performance liquid encapsulating composition and application - Google Patents
High-performance liquid encapsulating composition and application Download PDFInfo
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- CN105368004A CN105368004A CN201510951853.8A CN201510951853A CN105368004A CN 105368004 A CN105368004 A CN 105368004A CN 201510951853 A CN201510951853 A CN 201510951853A CN 105368004 A CN105368004 A CN 105368004A
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- Prior art keywords
- performance liquid
- embedding composition
- liquid embedding
- epoxy resin
- agent
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- 239000000203 mixture Substances 0.000 title claims abstract description 61
- 239000007788 liquid Substances 0.000 title claims abstract description 59
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 19
- 239000003822 epoxy resin Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 13
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 13
- 239000011353 cycloaliphatic epoxy resin Substances 0.000 claims description 16
- 150000008064 anhydrides Chemical class 0.000 claims description 15
- 239000003054 catalyst Substances 0.000 claims description 14
- 230000001070 adhesive effect Effects 0.000 claims description 13
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 13
- 239000013530 defoamer Substances 0.000 claims description 13
- 239000002002 slurry Substances 0.000 claims description 13
- 239000006096 absorbing agent Substances 0.000 claims description 12
- 239000000853 adhesive Substances 0.000 claims description 12
- 238000005728 strengthening Methods 0.000 claims description 12
- XCEUHXVTRJQJSR-UHFFFAOYSA-N bromo(phenyl)phosphane Chemical compound BrPC1=CC=CC=C1 XCEUHXVTRJQJSR-UHFFFAOYSA-N 0.000 claims description 8
- QUAMTGJKVDWJEQ-UHFFFAOYSA-N octabenzone Chemical compound OC1=CC(OCCCCCCCC)=CC=C1C(=O)C1=CC=CC=C1 QUAMTGJKVDWJEQ-UHFFFAOYSA-N 0.000 claims description 6
- -1 pentaerythritol ester Chemical class 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 3
- SMOKVADXFPKCFS-UHFFFAOYSA-M [Cl-].[PH4+].C(C1=CC=CC=C1)[P+](C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.[Cl-] Chemical compound [Cl-].[PH4+].C(C1=CC=CC=C1)[P+](C1=CC=CC=C1)(C1=CC=CC=C1)C1=CC=CC=C1.[Cl-] SMOKVADXFPKCFS-UHFFFAOYSA-M 0.000 claims description 3
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 3
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 claims description 3
- 229950002083 octabenzone Drugs 0.000 claims description 3
- MUTGBJKUEZFXGO-OLQVQODUSA-N (3as,7ar)-3a,4,5,6,7,7a-hexahydro-2-benzofuran-1,3-dione Chemical compound C1CCC[C@@H]2C(=O)OC(=O)[C@@H]21 MUTGBJKUEZFXGO-OLQVQODUSA-N 0.000 claims description 2
- ZXDDPOHVAMWLBH-UHFFFAOYSA-N 2,4-Dihydroxybenzophenone Chemical compound OC1=CC(O)=CC=C1C(=O)C1=CC=CC=C1 ZXDDPOHVAMWLBH-UHFFFAOYSA-N 0.000 claims description 2
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 claims description 2
- GHKOFFNLGXMVNJ-UHFFFAOYSA-N Didodecyl thiobispropanoate Chemical compound CCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCC GHKOFFNLGXMVNJ-UHFFFAOYSA-N 0.000 claims description 2
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 2
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 claims description 2
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims description 2
- IKWKJIWDLVYZIY-UHFFFAOYSA-M butyl(triphenyl)phosphanium;bromide Chemical compound [Br-].C=1C=CC=CC=1[P+](C=1C=CC=CC=1)(CCCC)C1=CC=CC=C1 IKWKJIWDLVYZIY-UHFFFAOYSA-M 0.000 claims description 2
- MFIUDWFSVDFDDY-UHFFFAOYSA-M butyl(triphenyl)phosphanium;chloride Chemical compound [Cl-].C=1C=CC=CC=1[P+](C=1C=CC=CC=1)(CCCC)C1=CC=CC=C1 MFIUDWFSVDFDDY-UHFFFAOYSA-M 0.000 claims description 2
- NJXBVBPTDHBAID-UHFFFAOYSA-M ethyl(triphenyl)phosphanium;chloride Chemical compound [Cl-].C=1C=CC=CC=1[P+](C=1C=CC=CC=1)(CC)C1=CC=CC=C1 NJXBVBPTDHBAID-UHFFFAOYSA-M 0.000 claims description 2
- QRPRIOOKPZSVFN-UHFFFAOYSA-M methyl(triphenyl)phosphanium;chloride Chemical compound [Cl-].C=1C=CC=CC=1[P+](C=1C=CC=CC=1)(C)C1=CC=CC=C1 QRPRIOOKPZSVFN-UHFFFAOYSA-M 0.000 claims description 2
- 150000002894 organic compounds Chemical class 0.000 claims description 2
- DXGLGDHPHMLXJC-UHFFFAOYSA-N oxybenzone Chemical compound OC1=CC(OC)=CC=C1C(=O)C1=CC=CC=C1 DXGLGDHPHMLXJC-UHFFFAOYSA-N 0.000 claims description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- WAGFXJQAIZNSEQ-UHFFFAOYSA-M tetraphenylphosphonium chloride Chemical compound [Cl-].C1=CC=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 WAGFXJQAIZNSEQ-UHFFFAOYSA-M 0.000 claims description 2
- AVCVDUDESCZFHJ-UHFFFAOYSA-N triphenylphosphane;hydrochloride Chemical compound [Cl-].C1=CC=CC=C1[PH+](C=1C=CC=CC=1)C1=CC=CC=C1 AVCVDUDESCZFHJ-UHFFFAOYSA-N 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 238000005538 encapsulation Methods 0.000 abstract description 11
- 230000009477 glass transition Effects 0.000 abstract description 2
- 230000002745 absorbent Effects 0.000 abstract 1
- 239000002250 absorbent Substances 0.000 abstract 1
- 150000008065 acid anhydrides Chemical class 0.000 abstract 1
- 239000002518 antifoaming agent Substances 0.000 abstract 1
- 235000006708 antioxidants Nutrition 0.000 abstract 1
- 239000012744 reinforcing agent Substances 0.000 abstract 1
- 239000004593 Epoxy Substances 0.000 description 10
- 238000007711 solidification Methods 0.000 description 9
- 230000008023 solidification Effects 0.000 description 9
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 5
- 238000001879 gelation Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 125000003700 epoxy group Chemical group 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 239000004844 aliphatic epoxy resin Substances 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000012764 mineral filler Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 102000011759 adducin Human genes 0.000 description 1
- 108010076723 adducin Proteins 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000007704 transition Effects 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
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
- C08G59/32—Epoxy compounds containing three or more epoxy groups
- C08G59/38—Epoxy compounds containing three or more epoxy groups together with di-epoxy compounds
-
- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/4215—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof cycloaliphatic
-
- 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
- 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
-
- 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)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a high-performance liquid encapsulating composition. The composition is prepared from, by weight, 100 parts of epoxy resin, 80-120 parts of an acid anhydride curing agent, 0.1-1.0 part of curing accelerator, 0.1-1.5 parts of an adhesion reinforcing agent, 0.1-1.5 parts of ultraviolet absorbent, 0.1-1.0 part of anti-oxidant, 0.01-0.1 part of transparent purple-blue color paste and 0.1-0.5 part of an antifoaming agent. The invention further discloses application of the high-performance liquid encapsulating composition for serving as a high-power LED encapsulating material, in particular to the application of serving as a COB encapsulating material. The encapsulating composition has the advantages of being high in heat resistance, high in hardness, high in refractive index and the like, the glass-transition temperature is 155-168 DEG C, the shore hardness is D/15: 80-89, the refractive index is larger than 1.53, and the composition is suitable for serving as the LED encapsulating material and particularly suitable for COB encapsulation.
Description
Technical field
The present invention relates to a kind of high-performance liquid embedding composition and application thereof, relate in particular to this application of high-performance liquid embedding composition in high power LED package field, particularly in the application of the integrated area source of superpower (COB) encapsulation field.
Background technology
Along with the fast development of high-power encapsulation and white light LEDs, study high performance LED Embedding Material and seem more and more urgent, especially high heat-resisting, the research and development of high rigidity, high refractive index LED Embedding Material are extremely urgent especially.
Compared with bisphenol A type resin, alicyclic structure saturated in cycloaliphatic epoxy resin structure can improve the resistance toheat of solidifying product, is applied to low power LED, but non-refractory, COB cooling requirements cannot be met.US6117953 discloses a kind of preparation method of semi-conductor liquid epoxy encapsulating compound, is filled with more silica glass, does not consider specific refractory power in this encapsulating compound, does not also mention the application in COB type LED field; CN1282105 discloses a kind of semiconductor-sealing-purpose liquid epoxies encapsulating compound, and this encapsulating compound contains a large amount of mineral fillers, and viscosity is comparatively large, does not consider specific refractory power; CN101831143 discloses a kind of LED high-performance liquid epoxy resin composition, this encapsulating compound viscosity is lower, easily cause fluorescent material rate of descent in COB encapsulation process too high, be not suitable for the encapsulation of COB, also not mentioned application in COB type LED.CN1125488 discloses liquid epoxy composite of a kind of semiconductor-sealing-purpose and uses thereof, this liquid epoxy composite is by liquid epoxies, anhydride curing agent, curing catalyst, silane coupling agent, be aided with a large amount of mineral filler compositions, the encapsulation of unicircuit and chip based semiconductor can only be used for.High amount of inorganic filler will inevitably affect the specific refractory power of LED, cannot be applied to LED.
Silicone resin has good heat conductivility, anti-moisture absorption property and high and low temperature resistance, but its adhesive property is more weak, and have certain toxicity, hardness is lower, and with high costs.CN104592931 discloses a kind of high power LED package glue composition, and this packaging plastic composition is that be aided with platinum catalyst and obtain, the hardness of solidifying product is obviously on the low side with polysiloxane and Methyl Hydrogen Polysiloxane Fluid for major ingredient.CN102676107 discloses a kind of organic-silicon-modified cycloaliphatic epoxy resin high-power LED encapsulation glue, the component A of this packaging plastic belongs to the structurally-modified epoxy resin of organosilicon chemistry, be aided with catalyzer by cycloaliphatic epoxy resin and silicone resin, at 120 DEG C, react decompression dehydration after 4 hours obtain, water byproduct in reaction process not easily removes, very easily solidifying product quality is had an impact, and this invention does not report specific refractory power.
Summary of the invention
The object of the invention is to overcome the deficiency that in prior art, LED Embedding Material resistance toheat is not good, hardness is low, specific refractory power is low, provides a kind of LED Embedding Material with high heat-resisting, high rigidity, high refractive index.
Another object of the present invention is the application providing this liquid Embedding Material in high temperature resistant LED field, especially in the application of COB encapsulation field.
The present invention's technical scheme used is:
A kind of high-performance liquid embedding composition, by weight, comprise 100 parts of epoxy resin, 80-120 part anhydride curing agent, 0.1-1.0 part curing catalyst, 0.1-1.5 part adhesive power strengthening agent, 0.1-1.5 part uv-absorbing agent, 0.1-1.0 part antioxidant, 0.01-0.1 part transparent violet blueness slurry, 0.1-0.5 part defoamer;
Wherein, described epoxy resin is at least one in structural formula I or the carboxylic-acid cycloaliphatic epoxy resin shown in formula II;
Structural formula I;
Structural formula II.
Preferably, described liquid embedding composition by weight, comprise 100 parts of epoxy resin, 90-100 part anhydride curing agent, 0.1-0.4 part curing catalyst, 0.5-1.0 part adhesive power strengthening agent, 0.4-1.0 part uv-absorbing agent, 0.1-0.5 part antioxidant, 0.01-0.05 part transparent violet blueness slurry, 0.1-0.2 part defoamer.
Preferred further, described high-performance liquid embedding composition by weight, comprise 100 parts of epoxy resin, 95-100 part anhydride curing agent, 0.3-0.4 part curing catalyst, 0.6-1.0 part adhesive power strengthening agent, 0.4-1.0 part uv-absorbing agent, 0.4-0.5 part antioxidant, 0.01 part of transparent violet blueness slurry, 0.2 part of defoamer.
Preferably, described epoxy resin is the mixture of the carboxylic-acid cycloaliphatic epoxy resin shown in structural formula I and the carboxylic-acid cycloaliphatic epoxy resin shown in structural formula II, and the weight ratio of the carboxylic-acid cycloaliphatic epoxy resin shown in structural formula I and the carboxylic-acid cycloaliphatic epoxy resin shown in structural formula II is 1:1 ~ 2.5.
Most preferred, described epoxy resin is the epoxy equivalent (weight) of the carboxylic-acid cycloaliphatic epoxy resin shown in structural formula I is 200-220, and the epoxy equivalent (weight) of the carboxylic-acid cycloaliphatic epoxy resin shown in structural formula II is 180-200.Epoxy equivalent (weight) refers to the epoxy resin grams containing monovalent epoxide group.
Preferably, described anhydride curing agent is at least one in methylhexahydrophthalic anhydride, hexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride.
Preferably, the equivalence ratio of the epoxide group in described anhydride curing agent in anhydride group and carboxylic-acid cycloaliphatic epoxy resin is 0.5-1.8:1.
Preferably, described curing catalyst is at least one in tetraphenyl phosphonium chloride, benzyltriphenyl phosphonium phosphonium chloride, methyl triphenyl phosphonium chloride, ethyl triphenyl phosphonium chloride, propyl group triphenyl phosphonium chloride, butyl triphenyl phosphonium chloride, 4-phenyl phosphonium bromide, benzyl three phenyl phosphonium bromide, first base three phenyl phosphonium bromide, second base three phenyl phosphonium bromide, propyl group three phenyl phosphonium bromide, butyl triphenyl phosphonium bromide.
Preferably, described adhesive power strengthening agent is softening temperature at the polyvinylacetal organic compound of 0-85 DEG C, at least one further preferably in polyvinyl formal, polyvinyl butyral acetal.
Preferably, described uv-absorbing agent is at least one in 2,4 dihydroxyl benzophenone, Octabenzone, ESCALOL 567.
Preferably, described antioxidant is at least one in four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 2,6 di tert butyl 4 methyl phenol, Tyox B.
Preferably, described transparent violet blueness slurry is the chlorination CuPc isobutanol solution of massfraction 0.1%.
Preferably, described defoamer is the dimethyl silicone oil isobutanol solution of massfraction 2%.
The preparation method of high-performance liquid embedding composition of the present invention, comprises the following steps: take each component according to formula; Epoxy resin, adhesive power strengthening agent, uv-absorbing agent, transparent violet blueness slurry and defoamer are stirred at 80-90 DEG C and obtain component A, anhydride curing agent, curing catalyst, antioxidant being stirred at 60-70 DEG C obtains B component; Component A and B component are stirred and obtains liquid embedding composition.
High-performance liquid embedding composition of the present invention is used as the application of high power LED package material, is especially used as the application of COB packaged material.
Superpower in high-capacity LED of the present invention refers to that power is greater than 0.35W.
Compared with prior art, advantage of the present invention:
The viscosity that employing rotational viscosimeter records before liquid embedding composition of the present invention solidification is (25 DEG C) 350-600cps, and when depositing for 25 DEG C, the time that viscosity raises 10% needs is greater than 8 hours.
Adopt 1g liquid embedding composition, the gelation time that gelation time tester is tested the liquid embedding composition before solidification prepared by the present invention is 9-12min.
Specific refractory power before adopting Abbe refractometer to record liquid embedding composition of the present invention solidification is greater than 1.53.
Liquid embedding composition the present invention prepared adopts 120 DEG C/1 hour, then 130 DEG C/1 hour curing molding, the performance of the liquid embedding composition after evaluate cure:
Adopt DSC under air atmosphere between 30-250 DEG C with the speed secondary temperature elevation of 10 DEG C/min, obtaining second-order transition temperature is 155-168 DEG C.
Surveying flexural strength according to GBT9341-2000 Plastics-Oetermination of flexural properties method is 130-146MPa.
Water-intake rate is tested: will
wafer sample in the boiling water of 100 DEG C, boil 8h, record soak before and after quality be respectively W1 and W2, then water-intake rate is according to formula (W2-W1)/W1 × 100%, and the result calculated is 0.4-0.6%.
Using sclerometer to measure penetration hardness (shore hardness) test method survey shore hardness according to GBT2411-2008 plastics and vulcanite is D/15:80-89.
Carry out encapsulation 5730LED lamp pearl with liquid embedding composition of the present invention, boil 1h, carry out red ink test in 100 DEG C of water-based red ink, it is qualified that test is.
Visible liquid embedding composition of the present invention has the feature of high heat-resisting, high rigidity, high refractive index, is suitable for being used as LED Embedding Material, is particularly suitable for COB encapsulation.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described in further detail.
A kind of high-performance liquid embedding composition, by weight, comprise 100 parts of epoxy resin, 80-120 part anhydride curing agent, 0.1-1.0 part curing catalyst, 0.1-1.5 part adhesive power strengthening agent, 0.1-1.5 part uv-absorbing agent, 0.1-1.0 part antioxidant, 0.01-0.1 part transparent violet blueness slurry, 0.1-0.5 part defoamer.
The preparation method of described high-performance liquid embedding composition, comprises the following steps: take each component according to formula; Epoxy resin, adhesive power strengthening agent, uv-absorbing agent, transparent violet blueness slurry and defoamer are stirred at 80-90 DEG C and obtain component A, anhydride curing agent, curing catalyst, antioxidant being stirred at 60-70 DEG C obtains B component; Component A and B component are stirred and obtains liquid embedding composition.
The formula of embodiment 1-6 liquid embedding composition is as shown in table 1.
The formula of table 1 embodiment 1-6 liquid embedding composition
Wherein, the carboxylic-acid cycloaliphatic epoxy resin shown in structural formula I adopts aliphatic epoxy resin EPOLEADGT401, basic index: epoxy equivalent (weight) is 220, and viscosity is 2300mPa.s/70 DEG C; Carboxylic-acid cycloaliphatic epoxy resin shown in structural formula II adopts aliphatic epoxy resin CELLOXIDE2081, and epoxy equivalent (weight) is 200, and viscosity is 340mPa.s/25 DEG C.
Transparent violet blueness slurry is the chlorination CuPc isobutanol solution of massfraction 0.1%.
Defoamer is the dimethyl silicone oil isobutanol solution of massfraction 2%.
The preparation method of embodiment 1 liquid embedding composition: in 1L four-hole boiling flask, add the carboxylic-acid cycloaliphatic epoxy resin shown in the carboxylic-acid cycloaliphatic epoxy resin shown in 40 weight part structural formula I and 60 weight part structural formulas II, 0.4 weight part Octabenzone, 0.01 weight part transparent violet blueness slurry, 1.0 weight account polyethylene butyrals, 0.2 weight part defoamer, stirs and obtains transparent component A at 80-90 DEG C; In 1L four-hole boiling flask, add 95 weight part methylhexahydrophthalic anhydrides, 0.4 weight part benzyltriphenyl phosphonium phosphonium chloride, 0.5 weight part 2,6 di tert butyl 4 methyl phenol, stirs and obtains transparent B component at 60-70 DEG C; Namely component A and B component at room temperature high-speed stirring obtain uniform liquid embedding composition for 15 minutes.
The preparation of embodiment 2-6 liquid embedding composition is with reference to embodiment 1.
Investigate the obtained liquid embedding composition of embodiment 1-6 and Solidified enzyme thereof.
Adopt the viscosity before the solidification of rotary viscosity design determining liquid embedding composition.
Adopt 1g liquid embedding composition, with the gelation time before the solidification of gelation time tester test liquid embedding composition.
Specific refractory power before adopting Abbe refractometer to measure the solidification of liquid embedding composition.
Liquid embedding composition is adopted 120 DEG C/1 hour, then 130 DEG C/1 hour curing molding, the performance of the liquid embedding composition after evaluate cure:
Adopt DSC under air atmosphere between 30-250 DEG C with the speed secondary temperature elevation of 10 DEG C/min, measure glass transition temperature Tg.
Flexural strength is surveyed according to GBT9341-2000 Plastics-Oetermination of flexural properties method.
Water-intake rate is tested: will
wafer sample in the boiling water of 100 DEG C, boil 8h, the quality before and after record soaks is respectively W1 and W2, calculates water-intake rate according to formula (W2-W1)/W1 × 100%.
Using sclerometer to measure penetration hardness (shore hardness) test method survey shore hardness according to GBT2411-2008 plastics and vulcanite is D/15s.
Carry out encapsulation 5730LED lamp pearl with obtained liquid embedding composition, in 100 DEG C of water-based red ink, boil 1h, carry out red ink test.
The liquid embedding composition that table 2 embodiment 1-6 is obtained and Solidified enzyme thereof
The liquid embedding composition that embodiment 1-6 obtains is when depositing for 25 DEG C, and the time that viscosity raises 10% needs is greater than 8 hours.
Gelation time before the liquid embedding composition solidification that embodiment 1-6 obtains is 9-12min.
Flexural strength after the liquid embedding composition solidification that embodiment 1-6 obtains is 130-146MPa.
Water-intake rate after the liquid embedding composition solidification that embodiment 1-6 obtains is 0.4-0.6%.
Claims (9)
1. a high-performance liquid embedding composition, by weight, comprise 100 parts of epoxy resin, 80-120 part anhydride curing agent, 0.1-1.0 part curing catalyst, 0.1-1.5 part adhesive power strengthening agent, 0.1-1.5 part uv-absorbing agent, 0.1-1.0 part antioxidant, 0.01-0.1 part transparent violet blueness slurry, 0.1-0.5 part defoamer;
Wherein, described epoxy resin is at least one in structural formula I or the carboxylic-acid cycloaliphatic epoxy resin shown in formula II;
2. a kind of high-performance liquid embedding composition as claimed in claim 1, it is characterized in that described liquid embedding composition by weight, comprise 100 parts of epoxy resin, 90-100 part anhydride curing agent, 0.1-0.4 part curing catalyst, 0.5-1.0 part adhesive power strengthening agent, 0.4-1.0 part uv-absorbing agent, 0.1-0.5 part antioxidant, 0.01-0.05 part transparent violet blueness slurry, 0.1-0.2 part defoamer.
3. a kind of high-performance liquid embedding composition as claimed in claim 2, it is characterized in that described high-performance liquid embedding composition by weight, comprise 100 parts of epoxy resin, 95-100 part anhydride curing agent, 0.3-0.4 part curing catalyst, 0.6-1.0 part adhesive power strengthening agent, 0.4-1.0 part uv-absorbing agent, 0.4-0.5 part antioxidant, 0.01 part of transparent violet blueness slurry, 0.2 part of defoamer.
4. a kind of high-performance liquid embedding composition as described in claim 1,2 or 3, is characterized in that described anhydride curing agent is at least one in methylhexahydrophthalic anhydride, hexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride;
Described curing catalyst is at least one in tetraphenyl phosphonium chloride, benzyltriphenyl phosphonium phosphonium chloride, methyl triphenyl phosphonium chloride, ethyl triphenyl phosphonium chloride, propyl group triphenyl phosphonium chloride, butyl triphenyl phosphonium chloride, 4-phenyl phosphonium bromide, benzyl three phenyl phosphonium bromide, first base three phenyl phosphonium bromide, second base three phenyl phosphonium bromide, propyl group three phenyl phosphonium bromide, butyl triphenyl phosphonium bromide.
5. a kind of high-performance liquid embedding composition as described in claim 1,2 or 3, is characterized in that described adhesive power strengthening agent is softening temperature at the polyvinylacetal organic compound of 0-85 DEG C; At least one preferably in polyvinyl formal, polyvinyl butyral acetal.
6. a kind of high-performance liquid embedding composition as described in claim 1,2 or 3, it is characterized in that described uv-absorbing agent is at least one in 2,4 dihydroxyl benzophenone, Octabenzone, ESCALOL 567; Described antioxidant is at least one in four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 2,6 di tert butyl 4 methyl phenol, Tyox B.
7. the preparation method of high-performance liquid embedding composition according to claim 1, comprises the following steps: take each component according to formula; Epoxy resin, adhesive power strengthening agent, uv-absorbing agent, transparent violet blueness slurry and defoamer are stirred at 80-90 DEG C and obtain component A, anhydride curing agent, curing catalyst, antioxidant being stirred at 60-70 DEG C obtains B component; Component A and B component are stirred and obtains liquid embedding composition.
8. high-performance liquid embedding composition according to claim 1 is used as the application of high power LED package material.
9. high-performance liquid embedding composition according to claim 1 is used as the application of the integrated area source packaged material of superpower.
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| CN112625633A (en) * | 2020-12-11 | 2021-04-09 | 固德电材系统（苏州）股份有限公司 | Weather-resistant epoxy resin adhesive for wind power blade and preparation method and application thereof |
| CN113462123A (en) * | 2021-06-10 | 2021-10-01 | 巴中市特兴智能科技有限公司 | Material composition for COB (chip on Board) packaged LED (light-emitting diode) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006152016A (en) * | 2004-11-25 | 2006-06-15 | Matsushita Electric Works Ltd | Epoxy resin composition, its manufacturing method, optical waveguide and electronic part |
| CN102775729A (en) * | 2011-05-13 | 2012-11-14 | 惠州市富济电子材料有限公司 | Conductive silver glue with raising yellowing resistance for blue LED and production technology thereof |
-
2015
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006152016A (en) * | 2004-11-25 | 2006-06-15 | Matsushita Electric Works Ltd | Epoxy resin composition, its manufacturing method, optical waveguide and electronic part |
| CN102775729A (en) * | 2011-05-13 | 2012-11-14 | 惠州市富济电子材料有限公司 | Conductive silver glue with raising yellowing resistance for blue LED and production technology thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112625633A (en) * | 2020-12-11 | 2021-04-09 | 固德电材系统（苏州）股份有限公司 | Weather-resistant epoxy resin adhesive for wind power blade and preparation method and application thereof |
| CN113462123A (en) * | 2021-06-10 | 2021-10-01 | 巴中市特兴智能科技有限公司 | Material composition for COB (chip on Board) packaged LED (light-emitting diode) |
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