WO2018218596A1 - 高硬度led封装材料及其制备方法 - Google Patents
高硬度led封装材料及其制备方法 Download PDFInfo
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- WO2018218596A1 WO2018218596A1 PCT/CN2017/086812 CN2017086812W WO2018218596A1 WO 2018218596 A1 WO2018218596 A1 WO 2018218596A1 CN 2017086812 W CN2017086812 W CN 2017086812W WO 2018218596 A1 WO2018218596 A1 WO 2018218596A1
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- 239000005022 packaging material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title description 10
- -1 methyl trifluoropropyl Chemical group 0.000 claims abstract description 33
- 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 20
- 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 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000003963 antioxidant agent Substances 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
- 239000004954 Polyphthalamide Substances 0.000 claims abstract description 11
- 239000011521 glass Substances 0.000 claims abstract description 11
- 229920006375 polyphtalamide Polymers 0.000 claims abstract description 11
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 10
- 239000011324 bead Substances 0.000 claims abstract description 10
- 235000011187 glycerol Nutrition 0.000 claims abstract description 10
- 229920002545 silicone oil Polymers 0.000 claims abstract description 10
- 229920006122 polyamide resin Polymers 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 229920003366 poly(p-phenylene terephthalamide) Polymers 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 66
- 238000003756 stirring Methods 0.000 claims description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- ZETYUTMSJWMKNQ-UHFFFAOYSA-N n,n',n'-trimethylhexane-1,6-diamine Chemical compound CNCCCCCCN(C)C ZETYUTMSJWMKNQ-UHFFFAOYSA-N 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-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
- 229920005989 resin Polymers 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 229910052895 riebeckite Inorganic materials 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 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
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 3
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 3
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical group 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 group CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims 2
- 150000004985 diamines Chemical class 0.000 claims 1
- 150000002118 epoxides Chemical class 0.000 claims 1
- 239000001294 propane Substances 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 description 27
- 150000001412 amines Chemical class 0.000 description 5
- 229920000470 poly(p-phenylene terephthalate) polymer Polymers 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000004382 potting Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- POULHZVOKOAJMA-UHFFFAOYSA-M dodecanoate Chemical compound CCCCCCCCCCCC([O-])=O POULHZVOKOAJMA-UHFFFAOYSA-M 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011325 microbead Substances 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
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
Definitions
- the invention relates to the technical field of LED luminaire materials, in particular to a high-hardness LED packaging material and a preparation method thereof.
- LED packaging has experienced the development stages of stent (LampLED), SMD (SMDLED), and power LED (PowerLED).
- LampLED stent
- SMDLED SMD
- PowerLED power LED
- a new technical idea must be adopted for the package design.
- the potting compound is required to have low hygroscopicity, low stress, and aging resistance.
- potting compounds include epoxy resin and silica gel.
- the hardness of the encapsulating material has a greater effect on the use of the LED.
- the lower hardness results in a decrease in the mechanical properties of the encapsulating material and lowers the product quality of the LED.
- Today's LED packaging materials generally have defects such as low hardness, poor light transmittance, and easy damage.
- the technical problem to be solved by the present invention is to provide a high-hardness LED packaging material and a preparation method thereof in view of the above-mentioned deficiencies in the prior art.
- a high-hardness LED packaging material comprising the following raw materials by weight:
- a high hardness LED packaging material comprising the following parts by weight:
- a high hardness LED packaging material comprising the following parts by weight:
- a high hardness LED packaging material comprising the following parts by weight:
- the filler is a mixture of diamond micropowder, nano silicon carbide powder, copper powder and asbestos powder.
- the curing agent is a mixture of one or more of diethylaminopropylamine, dipropylenetriamine, trimethylhexamethylenediamine, and trimethylhexamethylenediamine.
- the antioxidant is tris(2,4-di-tert-butylphenyl)phosphite, p-phenylenediamine and dihydroquinoline, 2,6-tributyl-4-methylphenol a mixture of one or more of the dodecanoate.
- the diluent is one of diglycidyl ether, propylene oxide butyl ether, propylene oxide phenyl ether, dipropylene oxide ethyl ether, tripropylene oxide propyl ether, and xylene. Or a mixture of multiples.
- a method for preparing a high hardness LED packaging material comprising the steps of:
- the mixture treated in the step 4) is added to a mold for curing, the curing temperature is 130 ° C - 155 ° C, and after curing, it is cooled to room temperature to prepare a high-hardness LED packaging material.
- the curing temperature in the step 5) is 145 °C.
- the invention has the beneficial effects that the high-hardness LED packaging material of the invention greatly improves the hardness, refractive index, bonding strength, light transmittance and heat resistance of the LED packaging material by optimizing the raw material formulation and the material preparation method, and making the system
- the LED package material has excellent comprehensive performance, which not only can effectively protect the LED, prolong the service life of the LED, but also effectively reduce the thermal resistance, improve the light extraction efficiency, improve the use effect of the LED, and has broad market prospects.
- a high hardness LED packaging material comprising the following parts by weight:
- the invention is applied to an LED package.
- the combination of bisphenol A epoxy resin and dicyclopentadiene phenol epoxy resin can improve the toughness of the material and overcome the defects of high brittleness of the bisphenol A epoxy resin when used alone.
- Polyamide resin can improve the brittleness of materials and improve the bonding ability of materials.
- Poly(p-phenylene terephthalamide) has superior mechanical properties including high strength, high stiffness, high fatigue resistance and high creep resistance.
- Polyphthalamide has high stability and heat resistance.
- the combination of phthaloyl p-phenylenediamine and polyphthalamide is added to the material, and the two synergistic effects can significantly improve the stiffness, hardness, toughness and toughness of the material, and can improve the obtained LED package. The comprehensive properties of the material.
- Methyltrifluoropropyl silicone oil and glycerin epoxy resin are compounded and added to synergistic effect with bisphenol A epoxy resin and dicyclopentadiene phenol epoxy resin, which can improve the weather resistance and high temperature resistance of the material. It can improve the refractive index and UV radiation resistance of materials and prolong the service life of materials.
- the nano-alumina powder has high hardness and high temperature resistance. The addition of nano-alumina powder can improve the hardness and toughness of the material, as well as the surface finish of the LED packaging material, and improve the overall performance of the material.
- the glass beads have high dispersion, high flow and high temperature resistance. The addition of glass beads can promote the uniform mixing of the components of the material, improve the high temperature resistance of the material, and improve the refractive index and surface smoothness of the obtained LED packaging materials. .
- the filler is a mixture of diamond micropowder, nano silicon carbide powder, copper powder and asbestos powder.
- Diamond micropowder can improve the toughness and rigidity of materials.
- Nano-SiC powder has large specific surface area, high surface activity, low bulk density, excellent mechanical, thermal, electrical and chemical properties.
- the addition of nano-silicon carbide powder increases the hardness of the material.
- thermal conductivity; the addition of copper powder can effectively enhance the thermal conductivity of the material; the addition of asbestos powder can improve the high temperature resistance of the material.
- the curing agent is a mixture of one or more of diethylaminopropylamine, dipropylenetriamine, trimethylhexamethylenediamine, and trimethylhexamethylenediamine.
- the antioxidants are tris(2,4-di-tert-butylphenyl)phosphite, p-phenylenediamine and dihydroquinoline, 2,6-tri-butyl-4-methylphenol, and dodecyl a mixture of one or more of the carbon alcohol esters.
- the diluent is one of diglycidyl ether, propylene oxide butyl ether, propylene oxide phenyl ether, dipropylene oxide ethyl ether, tripropylene oxide propyl ether, xylene or A variety of mixtures.
- the invention also provides a preparation method of a high-hardness LED packaging material, comprising the following steps:
- the mixture treated in the step 4) is added to a mold for curing, the curing temperature is 130 ° C - 155 ° C, and after curing, it is cooled to room temperature to prepare a high-hardness LED packaging material.
- a high hardness LED packaging material comprising the following 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 terephthalate) by weight parts.
- a high hardness LED packaging material comprising the following 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 terephthalate) by weight parts.
- a high hardness LED packaging material comprising the following 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 terephthalate) by weight parts.
- a high hardness LED packaging material comprising the following 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 terephthalate) by weight parts.
- a high hardness LED packaging material comprising the following 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 terephthalate) by weight parts.
- the high-hardness LED packaging materials prepared in Examples 1-5 were tested for performance.
- the test items included Shore hardness, refractive index, bond strength (MPa), light transmittance, and heat resistance of 200 ° C / 60 min.
- the test results are as follows: table:
- the high-hardness LED packaging material of the invention has high hardness, high refractive index, high bonding strength, excellent light transmittance and heat resistance, and has excellent comprehensive performance, and can effectively improve the use effect of the LED. And service life.
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- 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
本发明公开了一种高硬度LED封装材料，包括以下重量份的原料：双酚A型环氧树脂30-70重量份、双环戊二烯苯酚环氧树脂30-60重量份、甲基三氟丙基硅油10-40重量份、甘油环氧树脂10-30重量份、聚对苯二酰对苯二胺15-45重量份、聚邻苯二甲酰胺10-35重量份、聚酰胺树脂10-40重量份、纳米氧化铝粉末2-15重量份、玻璃微珠1-15重量份、填料4-40重量份、固化剂5-45重量份、抗氧剂5-40重量份、稀释剂15-45重量份。本发明的高硬度LED封装材料具有优异的综合性能，不仅能对LED形成有效的保护，延长LED的使用寿命；还能有效提高出光效率，改善LED的使用效果。
Description
本发明涉及LED灯具材料技术领域，尤其是一种高硬度LED封装材料及其制备方法。
LED封装方法、材料、结构和工艺的选择主要由芯片结构、光电/机械特性、具体应用和成本等因素决定。经过40多年的发展，LED封装先后经历了支架式(LampLED)、贴片式(SMDLED)、功率型LED(PowerLED)等发展阶段。随着芯片功率的增大，特别是固态照明技术发展的需求，对LED封装的光学、热学、电学和机械结构等提出了新的、更高的要求。为了有效地降低封装热阻，提高出光效率，必须采用全新的技术思路来进行封装设计。为提高LED封装的可靠性，要求灌封胶具有低吸湿性、低应力、耐老化等特性。目前常用的灌封胶包括环氧树脂和硅胶。封装材料的硬度对LED的使用有较大的作用，较低的硬度会导致封装材料的机械性能下降，降低了LED的产品品质。现在的LED封装材料普遍存在硬度低、透光性差、易损坏等缺陷。
发明内容
本发明所要解决的技术问题在于针对上述现有技术中的不足，提供一种高硬度LED封装材料及其制备方法。
为解决上述技术问题，本发明采用的技术方案是：一种高硬度LED封装材料，包括以下重量份的原料：
一种高硬度LED封装材料，包括以下重量份的原料：
一种高硬度LED封装材料，包括以下重量份的原料：
一种高硬度LED封装材料，包括以下重量份的原料：
优选的是，所述填料为金刚石微粉、纳米碳化硅粉、铜粉和石棉粉的混合物。
优选的是，所述固化剂为二乙氨基丙胺、二丙烯三胺、三甲基六亚甲基二胺、三甲基已二胺中的一种或多种的混合物。
优选的是，所述抗氧剂为三(2,4-二叔丁基本基)亚磷酸酯、对苯二胺和二氢喹啉、2，6-三级丁基-4-甲基苯酚、双十二碳醇酯中的一种或多种的混合物。
优选的是，所述稀释剂为二缩水甘油醚、环氧丙烷丁基醚、环氧丙烷苯基醚、二环氧丙烷乙基醚、三环氧丙烷丙基醚、二甲苯中的一种或多种的混合物。
一种高硬度LED封装材料的制备方法，包括以下步骤：
1)按重量份称取双酚A型环氧树脂30-70重量份、双环戊二烯苯酚环氧树脂30-60重量份、甲基三氟丙基硅油10-40重量份、甘油环氧树脂10-30重量份、聚对苯二酰对苯二胺15-45重量份、聚邻苯二甲酰胺10-35重量份、聚
酰胺树脂10-40重量份、稀释剂15-45重量份，加热并进行机械搅拌至混合均匀，得到混合物A；
2)将步骤1)得到的混合物A和按重量份称取的纳米氧化铝粉末2-15重量份、玻璃微珠1-15重量份、填料4-40重量份加入到高温反应釜中，加热并搅拌2-4小时，得到混合物B；
3)按重量份向步骤2)得到的混合物B中加入抗氧剂5-40重量份、固化剂5-45重量份，搅拌均匀；
4)将步骤3)得到的混合物置于真空脱泡机中进行脱泡，脱泡时间为1-4.5小时；
5)将步骤4)处理后的混合物加入到模具中进行固化，固化温度为130℃-155℃，固化后冷却至室温，制备得到高硬度LED封装材料。
优选的是，所述步骤5)中的固化温度为145℃。
本发明的有益效果：本发明的高硬度LED封装材料通过优化原材料配方和材料制备方法，大幅度提高了LED封装材料的硬度、折射率、粘结强度、透光率和耐热性能，使制得的LED封装材料具有优异的综合性能，不仅能对LED形成有效的保护，延长LED的使用寿命；还能有效降低热阻、提高出光效率，改善LED的使用效果，具有广阔的市场前景。
下面对本发明做进一步的详细说明，以令本领域技术人员参照说明书文字能够据以实施。
应当理解，本文所使用的诸如“具有”、“包含”以及“包括”术语并不配出一个或多个其它元件或其组合的存在或添加。
一种高硬度LED封装材料，包括以下重量份的原料：
本发明应用于LED封装。
其中，双酚A型环氧树脂和双环戊二烯苯酚环氧树脂复配使用，可改善材料的韧性，克服双酚A型环氧树脂单独使用时材料脆性高的缺陷。聚酰胺树脂可改善材料脆性，提高材料的粘接能力。聚对苯二酰对苯二胺具有优越的机械特性，包括高强度、高刚度、高耐疲劳性及高抗蠕变性，聚邻苯二甲酰胺具有高稳定性和耐热性，聚对苯二酰对苯二胺和聚邻苯二甲酰胺复配使用，添加到材料中，两种产生协同效应，能显著提高材料的刚度、硬度、韧性和耐韧性，能提高制得的LED封装材料的综合性能。甲基三氟丙基硅油和甘油环氧树脂复配混合添加，与双酚A型环氧树脂和双环戊二烯苯酚环氧树脂产生协同效应，既能提高材料的耐候、耐高温性能，又能提高材料的折射率和耐紫外辐射性能，延长材料的使用寿命。纳米氧化铝粉末具有高硬度、耐高温性能，纳米氧化铝粉末的添加能提高材料的硬度和韧性，以及制得的LED封装材料表面的光洁度，提高材料的综合性能。玻璃微珠具有高分散、高流动、耐高温性能，玻璃微珠的添加能促进材料各组分混合均匀，能提高材料的耐高温性能，提高制得的LED封装材料的折射率和表面光滑度。
其中，所述填料为金刚石微粉、纳米碳化硅粉、铜粉和石棉粉的混合物。金刚石微粉能提高材料的韧性和刚度；纳米碳化硅粉比表面积大、表面活性高、松装密度低、具有极好的力学、热学、电学和化学性能，纳米碳化硅粉的添加提高材料的硬度和导热性能；铜粉的添加能有效增强材料的导热性能；石棉粉的添加能提高材料的耐高温性能。
所述固化剂为二乙氨基丙胺、二丙烯三胺、三甲基六亚甲基二胺、三甲基已二胺中的一种或多种的混合物。所述抗氧剂为三(2,4-二叔丁基本基)亚磷酸酯、对苯二胺和二氢喹啉、2，6-三级丁基-4-甲基苯酚、双十二碳醇酯中的一种或多种的混合物。所述稀释剂为二缩水甘油醚、环氧丙烷丁基醚、环氧丙烷苯基醚、二环氧丙烷乙基醚、三环氧丙烷丙基醚、二甲苯中的一种或
多种的混合物。
本发明还提供一种高硬度LED封装材料的制备方法，包括以下步骤：
1)按重量份称取双酚A型环氧树脂30-70重量份、双环戊二烯苯酚环氧树脂30-60重量份、甲基三氟丙基硅油10-40重量份、甘油环氧树脂10-30重量份、聚对苯二酰对苯二胺15-45重量份、聚邻苯二甲酰胺10-35重量份、聚酰胺树脂10-40重量份、稀释剂15-45重量份，加热并进行机械搅拌至混合均匀，得到混合物A；
2)将步骤1)得到的混合物A和按重量份称取的纳米氧化铝粉末2-15重量份、玻璃微珠1-15重量份、填料4-40重量份加入到高温反应釜中，加热并搅拌2-4小时，得到混合物B；
3)按重量份向步骤2)得到的混合物B中加入抗氧剂5-40重量份、固化剂5-45重量份，搅拌均匀；
4)将步骤3)得到的混合物置于真空脱泡机中进行脱泡，脱泡时间为1-4.5小时；
5)将步骤4)处理后的混合物加入到模具中进行固化，固化温度为130℃-155℃，固化后冷却至室温，制备得到高硬度LED封装材料。
下面结合具体的实施例对本发明做进一步的详细说明。
实施例1：
一种高硬度LED封装材料，包括以下重量份的原料：
其制备方法为：1)按重量份称取双酚A型环氧树脂、双环戊二烯苯酚环氧树脂、甲基三氟丙基硅油、甘油环氧树脂、聚对苯二酰对苯二胺、聚邻苯二甲酰胺、聚酰胺树脂、稀释剂，加热并进行机械搅拌至混合均匀，得到混合物A；2)将步骤1)得到的混合物A和按重量份称取的纳米氧化铝粉末、玻璃微珠、填料加入到高温反应釜中，加热并搅拌3小时，得到混合物B；3)按重量份向步骤2)得到的混合物B中加入抗氧剂、固化剂，搅拌均匀；4)将步骤3)得到的混合物置于真空脱泡机中进行脱泡，脱泡时间为3小时；5)将步骤4)处理后的混合物加入到模具中进行固化，固化温度为145℃，固化后冷却至室温，制备得到高硬度LED封装材料。
实施例2：
一种高硬度LED封装材料，包括以下重量份的原料：
其制备方法为：1)按重量份称取双酚A型环氧树脂、双环戊二烯苯酚环氧树脂、甲基三氟丙基硅油、甘油环氧树脂、聚对苯二酰对苯二胺、聚邻苯二甲酰胺、聚酰胺树脂、稀释剂，加热并进行机械搅拌至混合均匀，得到混合物A；2)将步骤1)得到的混合物A和按重量份称取的纳米氧化铝粉末、玻璃微珠、填料加入到高温反应釜中，加热并搅拌3.5小时，得到混合物B；3)按重量份向步骤2)得到的混合物B中加入抗氧剂、固化剂，搅拌均匀；
4)将步骤3)得到的混合物置于真空脱泡机中进行脱泡，脱泡时间为3.5小时；5)将步骤4)处理后的混合物加入到模具中进行固化，固化温度为145℃，固化后冷却至室温，制备得到高硬度LED封装材料。
实施例3
一种高硬度LED封装材料，包括以下重量份的原料：
其制备方法为：1)按重量份称取双酚A型环氧树脂、双环戊二烯苯酚环氧树脂、甲基三氟丙基硅油、甘油环氧树脂、聚对苯二酰对苯二胺、聚邻苯二甲酰胺、聚酰胺树脂、稀释剂，加热并进行机械搅拌至混合均匀，得到混合物A；2)将步骤1)得到的混合物A和按重量份称取的纳米氧化铝粉末、玻璃微珠、填料加入到高温反应釜中，加热并搅拌3小时，得到混合物B；3)按重量份向步骤2)得到的混合物B中加入抗氧剂、固化剂，搅拌均匀；4)将步骤3)得到的混合物置于真空脱泡机中进行脱泡，脱泡时间为3小时；5)将步骤4)处理后的混合物加入到模具中进行固化，固化温度为140℃，固化后冷却至室温，制备得到高硬度LED封装材料。
实施例4
一种高硬度LED封装材料，包括以下重量份的原料：
其制备方法为：1)按重量份称取双酚A型环氧树脂、双环戊二烯苯酚环氧树脂、甲基三氟丙基硅油、甘油环氧树脂、聚对苯二酰对苯二胺、聚邻苯二甲酰胺、聚酰胺树脂、稀释剂，加热并进行机械搅拌至混合均匀，得到混合物A；2)将步骤1)得到的混合物A和按重量份称取的纳米氧化铝粉末、玻璃微珠、填料加入到高温反应釜中，加热并搅拌3小时，得到混合物B；3)按重量份向步骤2)得到的混合物B中加入抗氧剂、固化剂，搅拌均匀；4)将步骤3)得到的混合物置于真空脱泡机中进行脱泡，脱泡时间为3.5小时；5)将步骤4)处理后的混合物加入到模具中进行固化，固化温度为140℃，固化后冷却至室温，制备得到高硬度LED封装材料。
实施例5
一种高硬度LED封装材料，包括以下重量份的原料：
其制备方法为：1)按重量份称取双酚A型环氧树脂、双环戊二烯苯酚环氧树脂、甲基三氟丙基硅油、甘油环氧树脂、聚对苯二酰对苯二胺、聚邻苯二甲酰胺、聚酰胺树脂、稀释剂，加热并进行机械搅拌至混合均匀，得到混合物A；2)将步骤1)得到的混合物A和按重量份称取的纳米氧化铝粉末、玻璃微珠、填料加入到高温反应釜中，加热并搅拌3小时，得到混合物B；3)按重量份向步骤2)得到的混合物B中加入抗氧剂、固化剂，搅拌均匀；4)将步骤3)得到的混合物置于真空脱泡机中进行脱泡，脱泡时间为3小时；5)将步骤4)处理后的混合物加入到模具中进行固化，固化温度为140℃，固化后冷却至室温，制备得到高硬度LED封装材料。
对实施例1-5制得的高硬度LED封装材料进行性能检测，测试项目包括邵氏硬度、折射率、粘结强度(MPa)、透光率、耐热性200℃/60min，测试结果如下表：
表1
从测试结果可以看出，本发明的高硬度LED封装材料硬度高、折射率高、粘结强度大、透光率和耐热性均优异，具有优异的综合性能，能有效提高LED的使用效果和使用寿命。
尽管本发明的实施方案已公开如上，但其并不仅仅限于说明书和实施方式中所列运用。它完全可以被适用于各种适合本发明的领域。对于熟悉本领
域的人员而言，可容易地实现另外的修改。因此在不背离权利要求及等同范围所限定的一般概念下，本发明并不限于特定的细节。
Claims (10)
- 一种高硬度LED封装材料，其特征在于，包括以下重量份的原料：
- 根据权利要求1所述的高硬度LED封装材料，其特征在于，包括以下重量份的原料：
- 根据权利要求1所述的高硬度LED封装材料，其特征在于，包括以下重量份的原料：
- 根据权利要求1所述的高硬度LED封装材料，其特征在于，包括以下重量份的原料：
- 根据权利要求1-4中任意一项所述的高硬度LED封装材料，其特征在于，所述填料为金刚石微粉、纳米碳化硅粉、铜粉和石棉粉的混合物。
- 根据权利要求1-4中任意一项所述的高硬度LED封装材料，其特征在于，所述固化剂为二乙氨基丙胺、二丙烯三胺、三甲基六亚甲基二胺、三甲基已二胺中的一种或多种的混合物。
- 根据权利要求1-4中任意一项所述的高硬度LED封装材料，其特征在于， 所述抗氧剂为三(2,4-二叔丁基本基)亚磷酸酯、对苯二胺和二氢喹啉、2，6-三级丁基-4-甲基苯酚、双十二碳醇酯中的一种或多种的混合物。
- 根据权利要求1-4中任意一项所述的高硬度LED封装材料，其特征在于，所述稀释剂为二缩水甘油醚、环氧丙烷丁基醚、环氧丙烷苯基醚、二环氧丙烷乙基醚、三环氧丙烷丙基醚、二甲苯中的一种或多种的混合物。
- 一种如权利要求1所述的高硬度LED封装材料的制备方法，其特征在于，包括以下步骤：1)按重量份称取双酚A型环氧树脂30-70重量份、双环戊二烯苯酚环氧树脂30-60重量份、甲基三氟丙基硅油10-40重量份、甘油环氧树脂10-30重量份、聚对苯二酰对苯二胺15-45重量份、聚邻苯二甲酰胺10-35重量份、聚酰胺树脂10-40重量份、稀释剂15-45重量份，加热并进行机械搅拌至混合均匀，得到混合物A；2)将步骤1)得到的混合物A和按重量份称取的纳米氧化铝粉末2-15重量份、玻璃微珠1-15重量份、填料4-40重量份加入到高温反应釜中，加热并搅拌2-4小时，得到混合物B；3)按重量份向步骤2)得到的混合物B中加入抗氧剂5-40重量份、固化剂5-45重量份，搅拌均匀；4)将步骤3)得到的混合物置于真空脱泡机中进行脱泡，脱泡时间为1-4.5小时；5)将步骤4)处理后的混合物加入到模具中进行固化，固化温度为130℃-155℃，固化后冷却至室温，制备得到高硬度LED封装材料。
- 根据权利要求9所述的高硬度LED封装材料的制备方法，其特征在于，所述步骤5)中的固化温度为145℃。
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| CN104403277B (zh) * | 2014-12-25 | 2018-06-08 | 无锡嘉联电子材料有限公司 | 一种led封装用高性能环氧树脂组合物的制备方法 |
| CN104531027B (zh) * | 2015-01-21 | 2016-05-18 | 广州聚合新材料科技股份有限公司 | 环氧树脂类灌封材料及其制备方法和应用 |
| CN104962224A (zh) * | 2015-07-06 | 2015-10-07 | 深圳先进技术研究院 | 底部填充胶及其制备方法 |
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| US20050288396A1 (en) * | 2004-06-28 | 2005-12-29 | Nippon Steel Chemical Co., Ltd. | Epoxy resin compositions |
| CN101186803A (zh) * | 2007-12-12 | 2008-05-28 | 张向宇 | 一种环氧树脂基阻尼封装料 |
| CN104231994A (zh) * | 2013-06-19 | 2014-12-24 | 聚鼎科技股份有限公司 | 黏合材料 |
| CN104610707A (zh) * | 2015-01-19 | 2015-05-13 | 珠海全宝电子科技有限公司 | 一种用高性能rcc制造的大功率led用金属基覆铜板 |
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