CN110804410A - High-temperature-resistant and high-humidity-resistant epoxy resin composition for packaging LED (light emitting diode) products - Google Patents
High-temperature-resistant and high-humidity-resistant epoxy resin composition for packaging LED (light emitting diode) products Download PDFInfo
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 54
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 54
- 239000000203 mixture Substances 0.000 title claims abstract description 33
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 150000008064 anhydrides Chemical class 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 125000002723 alicyclic group Chemical group 0.000 claims abstract description 6
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000654 additive Substances 0.000 claims abstract description 4
- 230000000996 additive effect Effects 0.000 claims abstract description 4
- 239000012745 toughening agent Substances 0.000 claims description 13
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 9
- 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 description 7
- 239000004593 Epoxy Substances 0.000 claims description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 6
- 229920000459 Nitrile rubber Polymers 0.000 claims description 6
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 6
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 6
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 claims description 6
- 229920000570 polyether Polymers 0.000 claims description 6
- 229920005862 polyol Polymers 0.000 claims description 6
- 150000003077 polyols Chemical class 0.000 claims description 6
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 4
- LTVUCOSIZFEASK-MPXCPUAZSA-N (3ar,4s,7r,7as)-3a-methyl-3a,4,7,7a-tetrahydro-4,7-methano-2-benzofuran-1,3-dione Chemical compound C([C@H]1C=C2)[C@H]2[C@H]2[C@]1(C)C(=O)OC2=O LTVUCOSIZFEASK-MPXCPUAZSA-N 0.000 claims description 3
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- 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
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- NZNMSOFKMUBTKW-UHFFFAOYSA-N cyclohexanecarboxylic acid Chemical compound OC(=O)C1CCCCC1 NZNMSOFKMUBTKW-UHFFFAOYSA-N 0.000 claims description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 229920002857 polybutadiene Polymers 0.000 claims description 2
- 239000004636 vulcanized rubber Substances 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- -1 3, 4-epoxy cyclohexyl Chemical group 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 239000000853 adhesive Substances 0.000 abstract description 5
- 239000012790 adhesive layer Substances 0.000 abstract description 5
- 239000005022 packaging material Substances 0.000 abstract description 3
- 239000004113 Sepiolite Substances 0.000 description 17
- 239000000835 fiber Substances 0.000 description 17
- 229910052624 sepiolite Inorganic materials 0.000 description 17
- 239000000047 product Substances 0.000 description 9
- 235000019355 sepiolite Nutrition 0.000 description 9
- 238000003756 stirring Methods 0.000 description 8
- 239000011324 bead Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- MPIAGWXWVAHQBB-UHFFFAOYSA-N [3-prop-2-enoyloxy-2-[[3-prop-2-enoyloxy-2,2-bis(prop-2-enoyloxymethyl)propoxy]methyl]-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(COC(=O)C=C)(COC(=O)C=C)COCC(COC(=O)C=C)(COC(=O)C=C)COC(=O)C=C MPIAGWXWVAHQBB-UHFFFAOYSA-N 0.000 description 3
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 description 2
- 150000008065 acid anhydrides Chemical class 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- KUBDPQJOLOUJRM-UHFFFAOYSA-N 2-(chloromethyl)oxirane;4-[2-(4-hydroxyphenyl)propan-2-yl]phenol Chemical compound ClCC1CO1.C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 KUBDPQJOLOUJRM-UHFFFAOYSA-N 0.000 description 1
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical group CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 1
- 229930185605 Bisphenol Natural products 0.000 description 1
- 206010040880 Skin irritation Diseases 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000000227 grinding Methods 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
- 230000005764 inhibitory process Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a high-temperature and high-humidity resistant epoxy resin composition for packaging an LED product, which relates to the technical field of LED packaging materials and comprises modified resin and a curing agent, wherein the modified resin comprises the following raw materials in parts by weight: 5-15 parts of alicyclic epoxy resin, 17-42 parts of phenolic F type epoxy resin, 40-50 parts of bisphenol S type epoxy resin, 8-10 parts of organic composite additive and 5-8 parts of superfine fumed silica; the curing agent comprises the following raw materials in parts by weight: 20-40 parts of trimellitic anhydride, 50-75 parts of liquid composite anhydride and 5-10 parts of composite accelerator. The epoxy resin composition has high adhesive force, forms an adhesive layer similar to a rivet structure on a metal contact surface, effectively combines a metal bracket and a chip together, and does not reduce the adhesive force of the rivet adhesive layer under the high-temperature and high-humidity environment.
Description
The technical field is as follows:
the invention relates to the technical field of LED packaging materials, in particular to a high-temperature and high-humidity resistant epoxy resin composition for packaging LED products.
Background art:
an LED lighting device is a lighting apparatus using an LED (light emitting diode) as a light source, and is widely used in outdoor fields such as outdoor advertisement display screens, landscape lighting, and special lighting as a novel green photo light source product.
The main devices of the LED lamp bead are as follows: bracket, chip, epoxy resin, curing agent and the like. The epoxy resin is used as a main packaging material to fixedly combine the bracket and the chip. The contact of chip and moisture can effectively be completely cut off at normal atmospheric temperature behind ordinary epoxy encapsulation shaping, but under the high temperature and high humidity condition, the adhesive property of ordinary epoxy with metal support, chip can descend, and tiny gap appears in the contact surface of epoxy and metal, and inside steam then permeated epoxy through these tiny gaps, corroded the chip, leads to the product bad.
The invention content is as follows:
the invention aims to provide an epoxy resin composition which is suitable for being used as an encapsulating material of an LED product, has strong adhesive force and excellent high-temperature and high-humidity resistance.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
the high-temperature and high-humidity resistant epoxy resin composition for packaging the LED product comprises modified resin and a curing agent, wherein the modified resin comprises the following raw materials in parts by weight: 5-15 parts of alicyclic epoxy resin, 17-42 parts of phenolic F type epoxy resin, 40-50 parts of bisphenol S type epoxy resin, 8-10 parts of organic composite additive and 5-8 parts of superfine fumed silica;
the curing agent comprises the following raw materials in parts by weight: 20-40 parts of trimellitic anhydride, 50-75 parts of liquid composite anhydride and 5-10 parts of composite accelerator.
The alicyclic epoxy resin is selected from 3, 4-epoxycyclohexylmethyl-3＇,4＇Epoxy cyclohexyl carboxylate, bisphenol A epoxy resin, hydrogenated bisphenol A or a mixture of several of them mixed in proportion.
The organic composite auxiliary agent is selected from one or a mixture of a plurality of polyether polyol, foam-breaking siloxane, cyclohexanone and xylene which are mixed according to a proportion. The organic composite auxiliary agent plays roles of defoaming and foam inhibition, and prevents a great amount of foam from affecting the curing effect of the epoxy resin.
The liquid composite anhydride is one or a mixture of several of methyl hexahydro anhydride, methyl nadic anhydride and methyl tetrahydrophthalic anhydride which are mixed according to a proportion. The liquid anhydride curing agent and the epoxy resin have curing reaction, and compared with amine curing agents, the liquid anhydride curing agent has the advantages of small volatility, small skin irritation, low toxicity, low viscosity after being mixed with the epoxy resin, and capability of being modified by adding various fillers, thereby reducing the cost.
The composite accelerator is one or a mixture of several of benzyl dimethylamine, DMP-30, imidazole and N-methyl pyrrolidone mixed according to a proportion. The benzyl dimethylamine, the DMP-30 and the imidazole belong to the accelerators of epoxy resin anhydride curing agents commonly used in the field, and can reduce the curing temperature of the anhydride curing agents and shorten the curing time so as to solve the problem that the anhydride curing agents can be cured only at a higher temperature when being cured slowly at room temperature; however, N-methyl pyrrolidone is not a substance known in the art as an accelerator for epoxy resin acid anhydride curing agents, and the curing temperature and curing time of the acid anhydride curing agent can be significantly reduced by using N-methyl pyrrolidone in the present invention.
The modified resin also comprises 5-10 parts of a toughening agent.
The toughening agent is at least one of self-vulcanized rubber, liquid nitrile rubber and liquid polybutadiene rubber. The flexibility of the epoxy resin is improved by adding the toughening agent, so that the mechanical property of the composite material is improved.
The toughening agent belongs to conventional choices in the field, and in order to further optimize the service performance of the toughening agent, the polydipentaerythritol hexaacrylate-sepiolite fiber melt is used as the toughening agent to replace the conventional toughening agent in the field, so that the mechanical property of the composite material can be obviously improved, and the high-temperature and high-humidity resistance of the composite material can be obviously improved.
The toughening agent is a poly dipentaerythritol hexaacrylate-sepiolite fiber melt, and the preparation method comprises the following steps: heating the poly dipentaerythritol hexaacrylate to a melting point at a heating rate of 5-10 ℃/min under low-speed stirring, preserving heat to form a melt, adding sepiolite fibers, stirring at a high speed, cooling to-10 ℃ at a cooling rate of 5-10 ℃/min, preserving heat, standing, and finally grinding into micro powder.
The mass ratio of the polydipentaerythritol hexaacrylate to the sepiolite fibers is 1-5: 1.
The molten polydipentaerythritol hexaacrylate permeates into the sepiolite fibers to form a firm polydipentaerythritol hexaacrylate-sepiolite fiber structure in a staggered mode, so that the mechanical property and the heat resistance of the composite material are improved, the improvement effect of the composite material is far better than that of a conventional mixture of the polydipentaerythritol hexaacrylate and the sepiolite fibers, and the polydipentaerythritol hexaacrylate does not belong to a substance which is known in the field and can be used as an epoxy resin toughening agent, so that the novel application of the novel substance of the polydipentaerythritol hexaacrylate-sepiolite fiber melt as the epoxy resin toughening agent is realized.
The invention has the beneficial effects that: the invention provides a novel epoxy resin composition which has high adhesive force, forms an adhesive layer similar to a rivet structure on a metal contact surface, effectively combines a metal bracket and a chip together, and does not reduce the adhesive force of the rivet adhesive layer under a high-temperature and high-humidity environment, so that the epoxy resin composition is suitable for serving as an encapsulating material of an LED product.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
The bisphenol A type epoxy resins in the following examples and comparative examples were obtained from DER331, a DER, a F-phenolic epoxy resin, a S-bisphenol epoxy resin, a 3005S, a polyether polyol, a MN-3050D soft foam polyether polyol, an ultrafine fumed silica, a K-D15 fumed silica, a polydipentaerythritol hexaacrylate, a sepiolite fiber, and a liquid nitrile rubber and plastic rubber from Henry, Inc., Kyoho, Inc., of Kyoho, of Yonghama, of Shandong, of Japan.
Example 1
(1) Preparation of modified resin: preheating 12kg of bisphenol A epoxy resin to 70 ℃ at the rotation speed of 500r/min, adding 30kg of phenolic F type epoxy resin and 42kg of bisphenol S type epoxy resin, heating to 70 ℃, adding 5kg of polyether polyol, 3kg of cyclohexanone and 7kg of superfine fumed silica, stirring and mixing for 30min, and maintaining the temperature at 70 ℃ to obtain the modified resin.
(2) Preparation of the curing agent: heating 63kg of methyl nadic anhydride to 120 ℃ at the rotating speed of 500r/min, adding 28kg of trimellitic anhydride, keeping the temperature, stirring for 30min, cooling to 70 ℃, adding 4kg of benzyl dimethylamine and 4kg of DMP-30, keeping the temperature, and stirring for 30min to obtain a curing agent;
(3) preparation and use of epoxy resin compositions: the modified resin and the curing agent are mixed according to the molar ratio of the epoxy group to the acid anhydride of 1:1 to obtain the epoxy resin composition which can be used for packaging LED products and cured for 5 hours at 130 ℃.
Example 2
The same as in example 1 except that benzyldimethylamine in example 1 was replaced with 2-methylimidazole.
As a result, it was found that the epoxy resin composition obtained was completely cured after curing at 130 ℃ for 4.5 hours.
Example 3
The same as in example 1 except that benzyldimethylamine in example 1 was replaced with N-methylpyrrolidone.
As a result, it was found that the epoxy resin composition obtained was completely cured after curing at 130 ℃ for 4 hours.
Example 4
The procedure of example 1 is replaced with "preheating 12kg of bisphenol a epoxy resin to 70 ℃, adding 30kg of novolac F-type epoxy resin and 42kg of bisphenol S-type epoxy resin at a rotation speed of 500r/min, heating to 70 ℃, adding 6kg of liquid nitrile rubber, 8kg of polyether polyol and 7kg of ultrafine fumed silica, stirring and mixing for 30min, and maintaining the temperature at 70 ℃ to obtain a modified resin", and the rest is the same as example 1.
Example 5
The liquid nitrile rubber of example 4 was replaced with an equal amount of the polydipentaerythritol hexaacrylate-sepiolite fiber melt and the remainder of example 4.
Preparation of polydipentaerythritol hexaacrylate-sepiolite fiber melt: heating 0.4kg of poly dipentaerythritol hexaacrylate to a melting point at a heating rate of 5 ℃/min at a rotating speed of 300r/min, then preserving heat and stirring for 0.5h to form a melt, adding 0.1kg of sepiolite fibers, stirring for 0.5h at a rotating speed of 800r/min, then cooling to-10 ℃ at a cooling rate of 5 ℃/min, preserving heat and standing for 3h, and finally preparing into 80-mesh micro powder by a pulverizer.
Comparative example
The same as in example 4 was repeated except that the molten polydipentaerythritol hexaacrylate-sepiolite fiber in example 4 was replaced with a mixture of equal amounts of polydipentaerythritol hexaacrylate and sepiolite fibers (0.4kg of polydipentaerythritol hexaacrylate and 0.1kg of sepiolite fibers).
Epoxy resin compositions were prepared by using the above examples and comparative examples, respectively, and were used for encapsulating LED lamp beads of the same lot and specification, the thickness of the adhesive layer after curing was 50 μm, and performance tests were performed, with the test results shown in table 1.
The Izod notched impact strength and heat distortion temperature were measured according to the standard SJ/T11125-1997.
And (3) red ink test: and putting the packaged lamp beads into boiling red ink, boiling for 4 hours in a boiling state, taking out and cleaning, and observing whether the lamp beads have the phenomena of glue cracking, degumming, lamp failure and permeation under a microscope.
High temperature and high humidity test: and (3) performing reflow soldering on the packaged lamp bead for 2 times, then placing the lamp bead for 500 hours at the temperature of 85 ℃ and the relative humidity of 85%, and observing whether the lamp bead has the phenomena of glue cracking, degumming, lamp death and poor electrical performance under a microscope.
TABLE 1
As can be seen from Table 1, the epoxy resin composition of the present invention shows the technical effects of good sealing performance, excellent mechanical properties, excellent heat resistance, and excellent high temperature and high humidity resistance when used for packaging LED products. The self-made poly dipentaerythritol hexaacrylate-sepiolite fiber melt is used as a toughening agent to replace liquid nitrile rubber, so that the mechanical property and the heat resistance can be obviously improved, but the conventional mixture of the poly dipentaerythritol hexaacrylate and the sepiolite fiber does not have the technical effect. And the technical effect of shortening the curing time can be achieved at the same curing temperature by using N-methyl pyrrolidone as an accelerator.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. A high-temperature and high-humidity resistant epoxy resin composition for packaging LED products is characterized in that: the curing agent is composed of modified resin and a curing agent, wherein the modified resin comprises the following raw materials in parts by weight: 5-15 parts of alicyclic epoxy resin, 17-42 parts of phenolic F type epoxy resin, 40-50 parts of bisphenol S type epoxy resin, 8-10 parts of organic composite additive and 5-8 parts of superfine fumed silica;
the curing agent comprises the following raw materials in parts by weight: 20-40 parts of trimellitic anhydride, 50-75 parts of liquid composite anhydride and 5-10 parts of composite accelerator.
2. The high temperature and high humidity resistant epoxy resin composition for encapsulating LED product according to claim 1, wherein: the alicyclic epoxy resin is selected from one or a mixture of 3, 4-epoxy cyclohexyl methyl-3 ', 4' -epoxy cyclohexyl carboxylate, bisphenol A type epoxy resin and hydrogenated bisphenol A which are mixed according to a proportion.
3. The high temperature and high humidity resistant epoxy resin composition for encapsulating LED product according to claim 1, wherein: the organic composite auxiliary agent is selected from one or a mixture of a plurality of polyether polyol, foam-breaking siloxane, cyclohexanone and xylene which are mixed according to a proportion.
4. The high temperature and high humidity resistant epoxy resin composition for encapsulating LED product according to claim 1, wherein: the liquid composite anhydride is one or a mixture of several of methyl hexahydro anhydride, methyl nadic anhydride and methyl tetrahydrophthalic anhydride which are mixed according to a proportion.
5. The high temperature and high humidity resistant epoxy resin composition for encapsulating LED product according to claim 1, wherein: the composite accelerator is one or a mixture of several of benzyl dimethylamine, DMP-30, imidazole and N-methyl pyrrolidone mixed according to a proportion.
6. A high-temperature and high-humidity resistant epoxy resin composition for packaging LED products is characterized in that: the curing agent is composed of modified resin and a curing agent, wherein the modified resin comprises the following raw materials in parts by weight: 5-15 parts of alicyclic epoxy resin, 17-42 parts of phenolic F type epoxy resin, 40-50 parts of bisphenol S type epoxy resin, 8-10 parts of organic composite additive, 5-8 parts of superfine fumed silica and 5-10 parts of toughening agent;
the curing agent comprises the following raw materials in parts by weight: 20-40 parts of trimellitic anhydride, 50-75 parts of liquid composite anhydride and 5-10 parts of composite accelerator.
7. The high temperature and high humidity resistant epoxy resin composition for encapsulating LED product according to claim 6, wherein: the toughening agent is at least one of self-vulcanized rubber, liquid nitrile rubber and liquid polybutadiene rubber.
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| CN102086365A (en) * | 2010-12-27 | 2011-06-08 | 东莞市腾威电子材料技术有限公司 | Adhesive, preparation method and application in integrated circuit board embedment thereof |
| CN105936815A (en) * | 2016-06-08 | 2016-09-14 | 天津德高化成光电科技有限责任公司 | Thixotropic epoxy resin, preparation method and application thereof in LED chip packaging |
| CN108948671A (en) * | 2018-06-25 | 2018-12-07 | 安徽众博新材料有限公司 | High-heat-resistance heating non-flowing epoxy resin encapsulating material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102086365A (en) * | 2010-12-27 | 2011-06-08 | 东莞市腾威电子材料技术有限公司 | Adhesive, preparation method and application in integrated circuit board embedment thereof |
| CN105936815A (en) * | 2016-06-08 | 2016-09-14 | 天津德高化成光电科技有限责任公司 | Thixotropic epoxy resin, preparation method and application thereof in LED chip packaging |
| CN108948671A (en) * | 2018-06-25 | 2018-12-07 | 安徽众博新材料有限公司 | High-heat-resistance heating non-flowing epoxy resin encapsulating material and preparation method thereof |
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Application publication date: 20200218 |