CN107820507B - High-hardness LED packaging material and preparation method thereof - Google Patents
High-hardness LED packaging material and preparation method thereof Download PDFInfo
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- CN107820507B CN107820507B CN201780001771.4A CN201780001771A CN107820507B CN 107820507 B CN107820507 B CN 107820507B CN 201780001771 A CN201780001771 A CN 201780001771A CN 107820507 B CN107820507 B CN 107820507B
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- 239000005022 packaging material Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims description 13
- 239000003822 epoxy resin Substances 0.000 claims abstract description 28
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 28
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 16
- -1 methyl trifluoro propyl Chemical group 0.000 claims abstract description 13
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 12
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 239000003085 diluting agent Substances 0.000 claims abstract description 12
- 239000000945 filler Substances 0.000 claims abstract description 12
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 claims abstract description 11
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000011324 bead Substances 0.000 claims abstract description 11
- 239000011521 glass Substances 0.000 claims abstract description 11
- 235000011187 glycerol Nutrition 0.000 claims abstract description 10
- 229920006122 polyamide resin Polymers 0.000 claims abstract description 10
- 229920002545 silicone oil Polymers 0.000 claims abstract description 10
- 239000004954 Polyphthalamide Substances 0.000 claims abstract description 6
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims abstract description 6
- 229920006375 polyphtalamide Polymers 0.000 claims abstract description 6
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 58
- 238000003756 stirring Methods 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 16
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- ZETYUTMSJWMKNQ-UHFFFAOYSA-N n,n',n'-trimethylhexane-1,6-diamine Chemical compound CNCCCCCCN(C)C ZETYUTMSJWMKNQ-UHFFFAOYSA-N 0.000 claims description 6
- WRDNCFQZLUCIRH-UHFFFAOYSA-N 4-(7-azabicyclo[2.2.1]hepta-1,3,5-triene-7-carbonyl)benzamide Chemical compound C1=CC(C(=O)N)=CC=C1C(=O)N1C2=CC=C1C=C2 WRDNCFQZLUCIRH-UHFFFAOYSA-N 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000010425 asbestos Substances 0.000 claims description 4
- 229910003460 diamond Inorganic materials 0.000 claims description 4
- 239000010432 diamond Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 229910052895 riebeckite Inorganic materials 0.000 claims description 4
- IRFSXVIRXMYULF-UHFFFAOYSA-N 1,2-dihydroquinoline Chemical compound C1=CC=C2C=CCNC2=C1 IRFSXVIRXMYULF-UHFFFAOYSA-N 0.000 claims description 3
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 3
- IKEHOXWJQXIQAG-UHFFFAOYSA-N 2-tert-butyl-4-methylphenol Chemical compound CC1=CC=C(O)C(C(C)(C)C)=C1 IKEHOXWJQXIQAG-UHFFFAOYSA-N 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000007983 Tris buffer Substances 0.000 claims description 3
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 3
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 3
- POLCUAVZOMRGSN-UHFFFAOYSA-N dipropyl ether Chemical compound CCCOCCC POLCUAVZOMRGSN-UHFFFAOYSA-N 0.000 claims description 3
- GKQPCPXONLDCMU-CCEZHUSRSA-N lacidipine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C1=CC=CC=C1\C=C\C(=O)OC(C)(C)C GKQPCPXONLDCMU-CCEZHUSRSA-N 0.000 claims description 3
- QOHMWDJIBGVPIF-UHFFFAOYSA-N n',n'-diethylpropane-1,3-diamine Chemical compound CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 claims description 3
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- RNLMBKFMQZPRGW-UHFFFAOYSA-N 2,5,6-trioxatricyclo[2.1.1.01,4]hexane Chemical compound C1C23C(O1)(O2)O3 RNLMBKFMQZPRGW-UHFFFAOYSA-N 0.000 claims description 2
- 229960000735 docosanol Drugs 0.000 claims description 2
- NOPFSRXAKWQILS-UHFFFAOYSA-N docosanyl alcohol Natural products CCCCCCCCCCCCCCCCCCCCCCO NOPFSRXAKWQILS-UHFFFAOYSA-N 0.000 claims description 2
- 150000008301 phosphite esters Chemical class 0.000 claims description 2
- 239000001294 propane Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 description 21
- 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 12
- 238000002156 mixing Methods 0.000 description 6
- NAYYNDKKHOIIOD-UHFFFAOYSA-N phthalamide Chemical compound NC(=O)C1=CC=CC=C1C(N)=O NAYYNDKKHOIIOD-UHFFFAOYSA-N 0.000 description 5
- 229920003366 poly(p-phenylene terephthalamide) Polymers 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000004382 potting Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 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
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- 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
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Led Device Packages (AREA)
Abstract
The invention discloses a high-hardness LED packaging material which comprises the following raw materials in parts by weight: 30-70 parts of bisphenol A epoxy resin, 30-60 parts of dicyclopentadiene phenol epoxy resin, 10-40 parts of methyl trifluoro propyl silicone oil, 10-30 parts of glycerin epoxy resin, 15-45 parts of poly-terephthaloyl p-phenylenediamine, 10-35 parts of polyphthalamide, 10-40 parts of polyamide resin, 2-15 parts of nano alumina powder, 1-15 parts of glass beads, 4-40 parts of filler, 5-45 parts of curing agent, 5-40 parts of antioxidant and 15-45 parts of diluent. The high-hardness LED packaging material has excellent comprehensive performance, can effectively protect the LED and prolong the service life of the LED; and the light emitting efficiency can be effectively improved, and the using effect of the LED is improved.
Description
Technical Field
The invention relates to the technical field of LED lamp materials, in particular to a high-hardness LED packaging material and a preparation method thereof.
Background
The choice of LED packaging method, materials, structure and process is mainly determined by the chip structure, optoelectronic/mechanical properties, specific application and cost, etc. Through development for more than 40 years, the LED packaging successively goes through development stages such as a support type (LampLED), a surface mount type (SMDLED), a power type LED (PowerLED) and the like. With the increase of chip power, especially the development of solid-state lighting technology, new and higher requirements are put on the optical, thermal, electrical and mechanical structure of LED package. In order to effectively reduce the thermal resistance of the package and improve the light extraction efficiency, a brand new technical idea must be adopted for the package design. In order to improve the reliability of LED packaging, the potting adhesive is required to have low moisture absorption, low stress, aging resistance, and the like. Currently, common potting adhesives include epoxy resins and silica gels. The hardness of the packaging material has a great effect on the use of the LED, and the lower hardness can cause the mechanical property of the packaging material to be reduced, thereby reducing the product quality of the LED. The existing LED packaging material generally has the defects of low hardness, poor light transmission, easy damage and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-hardness LED packaging material and a preparation method thereof aiming at the defects in the prior art.
In order to solve the technical problems, the invention adopts the technical scheme that: a high-hardness LED packaging material comprises the following raw materials in parts by weight:
a high-hardness LED packaging material comprises the following raw materials in parts by weight:
a high-hardness LED packaging material comprises the following raw materials in parts by weight:
a high-hardness LED packaging material comprises the following raw materials in parts by weight:
preferably, the filler is a mixture of diamond micro powder, nano silicon carbide powder, copper powder and asbestos powder.
Preferably, the curing agent is one or more of diethylaminopropylamine, dipropylenetriamine, trimethylhexamethylenediamine and trimethylhexamethylenediamine.
Preferably, the antioxidant is one or more of a mixture of tris (2, 4-di-tert-butyl-based) phosphite, p-phenylenediamine and dihydroquinoline, 2, 6-tert-butyl-4-methylphenol and bisdodecyl alcohol ester.
Preferably, the diluent is one or more of diglycidyl ether, propylene oxide butyl ether, propylene oxide phenyl ether, propylene oxide ethyl ether, propylene oxide propyl ether and xylene.
A preparation method of a high-hardness LED packaging material comprises the following steps:
1) weighing 30-70 parts by weight of bisphenol A epoxy resin, 30-60 parts by weight of dicyclopentadiene phenol epoxy resin, 10-40 parts by weight of methyl trifluoropropyl silicone oil, 10-30 parts by weight of glycerin epoxy resin, 15-45 parts by weight of poly-p-phenylene terephthalamide, 10-35 parts by weight of polyphthalamide, 10-40 parts by weight of polyamide resin and 15-45 parts by weight of diluent, heating and mechanically stirring until the components are uniformly mixed to obtain a mixture A;
2) adding the mixture A obtained in the step 1) and 2-15 parts by weight of nano alumina powder, 1-15 parts by weight of glass beads and 4-40 parts by weight of filler which are weighed according to parts by weight into a high-temperature reaction kettle, heating and stirring for 2-4 hours to obtain a mixture B;
3) adding 5-40 parts by weight of antioxidant and 5-45 parts by weight of curing agent into the mixture B obtained in the step 2) according to the parts by weight, and uniformly stirring;
4) placing the mixture obtained in the step 3) in a vacuum defoaming machine for defoaming for 1-4.5 hours;
5) and (3) adding the mixture treated in the step (4) into a mold for curing, wherein the curing temperature is 130-155 ℃, and cooling to room temperature after curing to prepare the high-hardness LED packaging material.
Preferably, the curing temperature in said step 5) is 145 ℃.
The invention has the beneficial effects that: according to the high-hardness LED packaging material, by optimizing the raw material formula and the material preparation method, the hardness, the refractive index, the bonding strength, the light transmittance and the heat resistance of the LED packaging material are greatly improved, so that the prepared LED packaging material has excellent comprehensive performance, the LED can be effectively protected, and the service life of the LED is prolonged; the thermal resistance can be effectively reduced, the light-emitting efficiency is improved, the using effect of the LED is improved, and the LED light source has wide market prospect.
Detailed Description
The present invention is described in further detail below to enable those skilled in the art to practice the invention with reference to the description.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
A high-hardness LED packaging material comprises the following raw materials in parts by weight:
the invention is applied to LED packaging.
The bisphenol A epoxy resin and the dicyclopentadiene phenol epoxy resin are compounded for use, so that the toughness of the material can be improved, and the defect of high brittleness of the material when the bisphenol A epoxy resin is used alone is overcome. The polyamide resin can improve the brittleness of the material and improve the bonding capability of the material. The poly-p-phenylene terephthalamide has excellent mechanical properties including high strength, high rigidity, high fatigue resistance and high creep resistance, the polyphthalamide has high stability and heat resistance, and the poly-p-phenylene terephthalamide and the polyphthalamide are compounded and used, and are added into a material, so that the two synergistic effects are generated, the rigidity, the hardness, the toughness and the toughness resistance of the material can be obviously improved, and the comprehensive performance of the prepared LED packaging material can be improved. The methyl trifluoro propyl silicone oil and the glycerol epoxy resin are compounded, mixed and added to generate a synergistic effect with the bisphenol A type epoxy resin and the dicyclopentadiene phenol epoxy resin, so that the weather resistance and the high temperature resistance of the material can be improved, the refractive index and the ultraviolet radiation resistance of the material can be improved, and the service life of the material can be prolonged. The nano alumina powder has high hardness and high temperature resistance, and the addition of the nano alumina powder can improve the hardness and toughness of the material, the surface smoothness of the prepared LED packaging material and the comprehensive performance of the material. The glass beads have high dispersion, high flow and high temperature resistance, the addition of the glass beads can promote the uniform mixing of all components of the material, the high temperature resistance of the material can be improved, and the refractive index and the surface smoothness of the prepared LED packaging material are improved.
Wherein the filler is a mixture of diamond micropowder, nano silicon carbide powder, copper powder and asbestos powder. The diamond micro powder can improve the toughness and the rigidity of the material; the nano silicon carbide powder has the advantages of large specific surface area, high surface activity, low apparent density and excellent mechanical, thermal, electrical and chemical properties, and the addition of the nano silicon carbide powder improves the hardness and the heat conducting property of the material; the addition of the copper powder can effectively enhance the heat-conducting property of the material; the addition of the asbestos powder can improve the high-temperature resistance of the material.
The curing agent is one or a mixture of more of diethylaminopropylamine, dipropylenetriamine, trimethylhexamethylenediamine and trimethylhexamethylenediamine. The antioxidant is one or a mixture of more of tris (2, 4-di-tert-butyl basic) phosphite ester, p-phenylenediamine and dihydroquinoline, 2, 6-tert-butyl-4-methylphenol and docosanol ester. The diluent is one or a mixture of diglycidyl ether, epoxypropane butyl ether, epoxypropane phenyl ether, diepoxy propane ethyl ether, tri-epoxypropane propyl ether and xylene.
The invention also provides a preparation method of the high-hardness LED packaging material, which comprises the following steps:
1) weighing 30-70 parts by weight of bisphenol A epoxy resin, 30-60 parts by weight of dicyclopentadiene phenol epoxy resin, 10-40 parts by weight of methyl trifluoropropyl silicone oil, 10-30 parts by weight of glycerin epoxy resin, 15-45 parts by weight of poly-p-phenylene terephthalamide, 10-35 parts by weight of polyphthalamide, 10-40 parts by weight of polyamide resin and 15-45 parts by weight of diluent, heating and mechanically stirring until the components are uniformly mixed to obtain a mixture A;
2) adding the mixture A obtained in the step 1) and 2-15 parts by weight of nano alumina powder, 1-15 parts by weight of glass beads and 4-40 parts by weight of filler which are weighed according to parts by weight into a high-temperature reaction kettle, heating and stirring for 2-4 hours to obtain a mixture B;
3) adding 5-40 parts by weight of antioxidant and 5-45 parts by weight of curing agent into the mixture B obtained in the step 2) according to the parts by weight, and uniformly stirring;
4) placing the mixture obtained in the step 3) in a vacuum defoaming machine for defoaming for 1-4.5 hours;
5) and (3) adding the mixture treated in the step (4) into a mold for curing, wherein the curing temperature is 130-155 ℃, and cooling to room temperature after curing to prepare the high-hardness LED packaging material.
The present invention will be described in further detail with reference to specific examples.
Example 1:
a high-hardness LED packaging material comprises the following raw materials in parts by weight:
the preparation method comprises the following steps: 1) weighing bisphenol A type epoxy resin, dicyclopentadiene phenol epoxy resin, methyl trifluoropropyl silicone oil, glycerin epoxy resin, poly (p-phenylene terephthalamide), poly (phthalic diamide), polyamide resin and a diluent in parts by weight, heating, mechanically stirring and uniformly mixing to obtain a mixture A; 2) adding the mixture A obtained in the step 1), nano alumina powder, glass beads and a filler which are weighed according to parts by weight into a high-temperature reaction kettle, heating and stirring for 3 hours to obtain a mixture B; 3) adding an antioxidant and a curing agent into the mixture B obtained in the step 2) according to the parts by weight, and uniformly stirring; 4) placing the mixture obtained in the step 3) in a vacuum defoaming machine for defoaming for 3 hours; 5) and (3) adding the mixture treated in the step (4) into a mold for curing, wherein the curing temperature is 145 ℃, and cooling to room temperature after curing to prepare the high-hardness LED packaging material.
Example 2:
a high-hardness LED packaging material comprises the following raw materials in parts by weight:
the preparation method comprises the following steps: 1) weighing bisphenol A type epoxy resin, dicyclopentadiene phenol epoxy resin, methyl trifluoropropyl silicone oil, glycerin epoxy resin, poly (p-phenylene terephthalamide), poly (phthalic diamide), polyamide resin and a diluent in parts by weight, heating, mechanically stirring and uniformly mixing to obtain a mixture A; 2) adding the mixture A obtained in the step 1), nano alumina powder, glass beads and a filler which are weighed according to parts by weight into a high-temperature reaction kettle, heating and stirring for 3.5 hours to obtain a mixture B; 3) adding an antioxidant and a curing agent into the mixture B obtained in the step 2) according to the parts by weight, and uniformly stirring; 4) placing the mixture obtained in the step 3) in a vacuum defoaming machine for defoaming, wherein the defoaming time is 3.5 hours; 5) and (3) adding the mixture treated in the step (4) into a mold for curing, wherein the curing temperature is 145 ℃, and cooling to room temperature after curing to prepare the high-hardness LED packaging material.
Example 3
A high-hardness LED packaging material comprises the following raw materials in parts by weight:
the preparation method comprises the following steps: 1) weighing bisphenol A type epoxy resin, dicyclopentadiene phenol epoxy resin, methyl trifluoropropyl silicone oil, glycerin epoxy resin, poly (p-phenylene terephthalamide), poly (phthalic diamide), polyamide resin and a diluent in parts by weight, heating, mechanically stirring and uniformly mixing to obtain a mixture A; 2) adding the mixture A obtained in the step 1), nano alumina powder, glass beads and a filler which are weighed according to parts by weight into a high-temperature reaction kettle, heating and stirring for 3 hours to obtain a mixture B; 3) adding an antioxidant and a curing agent into the mixture B obtained in the step 2) according to the parts by weight, and uniformly stirring; 4) placing the mixture obtained in the step 3) in a vacuum defoaming machine for defoaming for 3 hours; 5) and (3) adding the mixture treated in the step (4) into a mold for curing, wherein the curing temperature is 140 ℃, and cooling to room temperature after curing to prepare the high-hardness LED packaging material.
Example 4
A high-hardness LED packaging material comprises the following raw materials in parts by weight:
the preparation method comprises the following steps: 1) weighing bisphenol A type epoxy resin, dicyclopentadiene phenol epoxy resin, methyl trifluoropropyl silicone oil, glycerin epoxy resin, poly (p-phenylene terephthalamide), poly (phthalic diamide), polyamide resin and a diluent in parts by weight, heating, mechanically stirring and uniformly mixing to obtain a mixture A; 2) adding the mixture A obtained in the step 1), nano alumina powder, glass beads and a filler which are weighed according to parts by weight into a high-temperature reaction kettle, heating and stirring for 3 hours to obtain a mixture B; 3) adding an antioxidant and a curing agent into the mixture B obtained in the step 2) according to the parts by weight, and uniformly stirring; 4) placing the mixture obtained in the step 3) in a vacuum defoaming machine for defoaming, wherein the defoaming time is 3.5 hours; 5) and (3) adding the mixture treated in the step (4) into a mold for curing, wherein the curing temperature is 140 ℃, and cooling to room temperature after curing to prepare the high-hardness LED packaging material.
Example 5
A high-hardness LED packaging material comprises the following raw materials in parts by weight:
the preparation method comprises the following steps: 1) weighing bisphenol A type epoxy resin, dicyclopentadiene phenol epoxy resin, methyl trifluoropropyl silicone oil, glycerin epoxy resin, poly (p-phenylene terephthalamide), poly (phthalic diamide), polyamide resin and a diluent in parts by weight, heating, mechanically stirring and uniformly mixing to obtain a mixture A; 2) adding the mixture A obtained in the step 1), nano alumina powder, glass beads and a filler which are weighed according to parts by weight into a high-temperature reaction kettle, heating and stirring for 3 hours to obtain a mixture B; 3) adding an antioxidant and a curing agent into the mixture B obtained in the step 2) according to the parts by weight, and uniformly stirring; 4) placing the mixture obtained in the step 3) in a vacuum defoaming machine for defoaming for 3 hours; 5) and (3) adding the mixture treated in the step (4) into a mold for curing, wherein the curing temperature is 140 ℃, and cooling to room temperature after curing to prepare the high-hardness LED packaging material.
The high-hardness LED encapsulating materials prepared in examples 1 to 5 were subjected to performance testing, wherein the test items include shore hardness, refractive index, adhesive strength (MPa), light transmittance, and heat resistance at 200 ℃/60min, and the test results are as follows:
TABLE 1
The test result shows that the high-hardness LED packaging material has the advantages of high hardness, high refractive index, high bonding strength, excellent light transmittance and heat resistance, excellent comprehensive performance, and capability of effectively improving the use effect and prolonging the service life of an LED.
While embodiments of the invention have been disclosed above, it is not intended to be limited to the uses set forth in the specification and examples. It can be applied to all kinds of fields suitable for the present invention. Additional modifications will readily occur to those skilled in the art. The invention is therefore not to be limited to the specific details described herein, without departing from the general concept as defined by the appended claims and their equivalents.
Claims (6)
1. The high-hardness LED packaging material is characterized by comprising the following raw materials in parts by weight:
the filler is a mixture of diamond micro powder, nano silicon carbide powder, copper powder and asbestos powder;
the curing agent is one or a mixture of more of diethylaminopropylamine, dipropylenetriamine, trimethylhexamethylenediamine and trimethylhexamethylenediamine;
the antioxidant is one or a mixture of more of tris (2, 4-di-tert-butyl basic) phosphite ester, p-phenylenediamine and dihydroquinoline, 2, 6-tert-butyl-4-methylphenol and docosanol ester;
the diluent is one or a mixture of diglycidyl ether, epoxypropane butyl ether, epoxypropane phenyl ether, diepoxy propane ethyl ether, tri-epoxypropane propyl ether and xylene.
2. The high-hardness LED packaging material as claimed in claim 1, comprising the following raw materials in parts by weight:
3. the high-hardness LED packaging material as claimed in claim 1, comprising the following raw materials in parts by weight:
4. the high-hardness LED packaging material as claimed in claim 1, comprising the following raw materials in parts by weight:
5. the preparation method of the high-hardness LED packaging material as claimed in claim 1, wherein the method comprises the following steps:
1) weighing 30-70 parts by weight of bisphenol A epoxy resin, 30-60 parts by weight of dicyclopentadiene phenol epoxy resin, 10-40 parts by weight of methyl trifluoropropyl silicone oil, 10-30 parts by weight of glycerin epoxy resin, 15-45 parts by weight of poly-p-phenylene terephthalamide, 10-35 parts by weight of polyphthalamide, 10-40 parts by weight of polyamide resin and 15-45 parts by weight of diluent, heating and mechanically stirring until the components are uniformly mixed to obtain a mixture A;
2) adding the mixture A obtained in the step 1) and 2-15 parts by weight of nano alumina powder, 1-15 parts by weight of glass beads and 4-40 parts by weight of filler which are weighed according to parts by weight into a high-temperature reaction kettle, heating and stirring for 2-4 hours to obtain a mixture B;
3) adding 5-40 parts by weight of antioxidant and 5-45 parts by weight of curing agent into the mixture B obtained in the step 2) according to the parts by weight, and uniformly stirring;
4) placing the mixture obtained in the step 3) in a vacuum defoaming machine for defoaming for 1-4.5 hours;
5) and (3) adding the mixture treated in the step (4) into a mold for curing, wherein the curing temperature is 130-155 ℃, and cooling to room temperature after curing to prepare the high-hardness LED packaging material.
6. The method for preparing the high-hardness LED packaging material according to claim 5, wherein the curing temperature in the step 5) is 145 ℃.
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| PCT/CN2017/086812 WO2018218596A1 (en) | 2017-06-01 | 2017-06-01 | Led packaging material having high hardness and preparation method therefor |
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| CN111019578B (en) * | 2019-12-26 | 2022-04-12 | 深圳德邦界面材料有限公司 | Epoxy resin heat-conducting adhesive sheet and preparation method thereof |
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| CN102437279A (en) * | 2010-09-29 | 2012-05-02 | 三星电机株式会社 | Radiating substrate and method for manufacturing the radiating substrate, and luminous element package with the radiating substrate |
| CN104531027A (en) * | 2015-01-21 | 2015-04-22 | 广州聚合电子材料有限公司 | Epoxy resin encapsulating material as well as preparation method and application thereof |
| CN104962224A (en) * | 2015-07-06 | 2015-10-07 | 深圳先进技术研究院 | Underfill adhesive and preparation method thereof |
| CN105086923A (en) * | 2014-05-08 | 2015-11-25 | 苏州达同新材料有限公司 | Organic silicon pouring sealant for LEDs and preparation method for organic silicon pouring sealant |
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| US6548189B1 (en) * | 2001-10-26 | 2003-04-15 | General Electric Company | Epoxy adhesive |
| JP4583821B2 (en) * | 2004-06-28 | 2010-11-17 | 新日鐵化学株式会社 | Liquid epoxy resin composition |
| US20090004484A1 (en) * | 2007-06-26 | 2009-01-01 | Doosan Corporation | Resine Composition For Printed Circuit Board And Composite Substrate And Copper Laminates Using The Same |
| CN100588696C (en) * | 2007-12-12 | 2010-02-10 | 张向宇 | Epoxy resin base damping packaging material |
| TWI468482B (en) * | 2013-06-19 | 2015-01-11 | Polytronics Technology Corp | Adhesive |
| CN104403277B (en) * | 2014-12-25 | 2018-06-08 | 无锡嘉联电子材料有限公司 | A kind of preparation method of LED encapsulation high-performance epoxy resin composition |
| CN104610707A (en) * | 2015-01-19 | 2015-05-13 | 珠海全宝电子科技有限公司 | Metal-base copper clad laminate manufactured through high-performance RCC (resin coated copper foil) and applied to high-power LED |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102437279A (en) * | 2010-09-29 | 2012-05-02 | 三星电机株式会社 | Radiating substrate and method for manufacturing the radiating substrate, and luminous element package with the radiating substrate |
| CN105086923A (en) * | 2014-05-08 | 2015-11-25 | 苏州达同新材料有限公司 | Organic silicon pouring sealant for LEDs and preparation method for organic silicon pouring sealant |
| CN104531027A (en) * | 2015-01-21 | 2015-04-22 | 广州聚合电子材料有限公司 | Epoxy resin encapsulating material as well as preparation method and application thereof |
| CN104962224A (en) * | 2015-07-06 | 2015-10-07 | 深圳先进技术研究院 | Underfill adhesive and preparation method thereof |
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