CN105860906B - A kind of conducting resinl for LED chip bonding - Google Patents

A kind of conducting resinl for LED chip bonding Download PDF

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CN105860906B
CN105860906B CN201610447519.3A CN201610447519A CN105860906B CN 105860906 B CN105860906 B CN 105860906B CN 201610447519 A CN201610447519 A CN 201610447519A CN 105860906 B CN105860906 B CN 105860906B
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parts
acid
epoxy resin
conducting resinl
led chip
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CN105860906A (en
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李康
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Shanghai far sand Electronic Technology Co., Ltd.
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Shanghai Far Sand Electronic Technology Co Ltd
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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
    • 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
    • C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02—Electrically-conducting adhesives
    • 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
    • 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

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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)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The present invention relates to a kind of conducting resinls for LED chip bonding, belong to LED encapsulation technologies field.It include following component by weight：30~40 parts of modified epoxy, 40~50 parts of bisphenol f type epoxy resin, 15~20 parts of modified polypropene acid resin, 12~15 parts of epoxy resin diluent, 300~600 parts of silver powder, 3~4 parts of curing agent, 2~5 parts of curing accelerator, 30~40 parts of organic solvent, 1~3 part of ultra-violet absorber, 3~5 parts of dispersant.The conducting resinl that the present invention is prepared, have the advantages that adhesive strength is high, conduct electricity very well, heat-transfer effect it is good.

Description

A kind of conducting resinl for LED chip bonding
Technical field
The present invention relates to a kind of conducting resinls for LED chip bonding, belong to LED encapsulation technologies field.
Background technology
High-power LED encapsulation directly influences performance and the service life of LED due to structure and complex process, always It is research hotspot in recent years, especially large power white light LED encapsulation is even more the hot spot in research hotspot.The function of LED encapsulation Include mainly：1. mechanical protection, to improve reliability；2. reinforcing heat dissipation, to reduce junction temperature of chip, LED performances are improved；3. optics Control improves light extraction efficiency, optimizes beam distribution；4. power supply management, including ac/dc transformation and power supply control etc..
LED encapsulation method, material, structure and technique selection mainly by chip structure, photoelectricity/mechanical property, specifically answer It is determined with factors such as costs.By development in more than 40 years, LED encapsulation successively experienced stent-type (Lamp LED), patch type The developing stage such as (SMD LED), power-type LED (Power LED).With the increase of chip power, especially solid-state lighting skill The demand of art development proposes new, higher requirement to optics, calorifics, the electrical and mechanical structure etc. of LED encapsulation.In order to It is effectively reduced packaging thermal resistance, improves light extraction efficiency, it is necessary to which design is packaged using completely new technical thought.
Conducting resinl is that LED produces a kind of glue indispensable in encapsulation, and the requirement to conductive silver paste is conductive, heat conduction The performance number of wanting, shear strength is big, and cohesive force is eager to excel.
CN102634313A discloses a kind of epoxy conducting suitable for LED chip bonding, by by organic carrier 8- 18%, epoxide diluent 2-5% is added, and is stirred evenly, vacuumizing and defoaming 15-20 minutes, and it is latent then to press content addition respectively Property curing agent 0.6-1.8%, curing accelerator 0.4-1.2%, epoxy resin toughener 1-3%, additive 1-3% are in reaction kettle In after mixing, vacuumize 30-60min, vacuum degree is -0.1MPa；Silver powder 65- is finally added in three-dimensional stirred tank 85%, it is put into three-roller after stirring and grinds 1-3 times, is made.It is high that CN105419672A is related to a kind of high-capacity LED The preparation method of thermal diffusivity conducting resinl, belongs to technical field of electronic materials.Preparation process is as follows：1）The preparation of nano silver aluminium powder, Weigh nano-silver powder, aluminium nitride, nano zine oxide, aluminium powder, methyltriethoxysilane, butanone；Each raw material is uniformly mixed, is ground It is dried after mill is uniform, is then transferred to calcining kiln roasting and nano silver aluminium powder is made；2）The preparation of conducting resinl, by quality hundred Divide content meter to stir evenly epoxy resin, succinic anhydride, dimethyl silicone polymer, antifoaming agent, curing agent, is slowly added to receive The silver-colored aluminium powder of rice, stirs evenly, froth in vacuum, high-capacity LED high-cooling property conducting resinl is made.
But above-mentioned conducting resinl has that heat conductivility is bad, adhesive strength is not high.
Invention content
The purpose of the present invention is：LED chip is solved during encapsulation adhesion, thermal conductivity and conduction existing for adhesive The all bad problem of glue, is mainly realized by being modified to epoxide-resin glue.
Technical solution is：
A kind of conducting resinl for LED chip bonding includes following component by weight：Modified epoxy 30 ~40 parts, 40~50 parts of bisphenol f type epoxy resin, 15~20 parts of modified polypropene acid resin, epoxy resin diluent 12~15 Part, 300~600 parts of silver powder, 3~4 parts of curing agent, 2~5 parts of curing accelerator, 30~40 parts of organic solvent, ultra-violet absorber 1~3 part, 3~5 parts of dispersant.
As dispersant, nonionic surface active agent such as polyoxyethylene isodecyl ether, polyoxyethylene laural can be used Base ether, polyoxyethylene β naphthyl ethers, polyoxyethylene styrylphenyl ether and polyoxyethylene diphenylethyllene phenyl ether, Yi Jiyin Ionic surfactant such as polyoxyethylene lauryl ether sulfate, polyoxyethylene β naphthalenes ether sulfate, polyoxyethylene benzene second Alkenyl phenyl ether phosphate, polyoxyethylene diphenylethyllene phenyl carboxylic acid salt, lauryl ether phosphate, octyl ether carboxylate, two Styrylphenyl ether sulfate, styrylphenyl ether phosphate and β naphthalene ether carboxylates.
Ultra-violet absorber, it is preferably excellent to the absorbability of wavelength 370nm ultraviolet lights below, to wavelength 400nm with On visible light the few substance of absorption, as concrete example, for example, compound in triazine class, oxygroup benzophenone (oxybenzophnone) class compound, benzotriazole compound, salicylic acid ester type compound, benzophenone compound, Cyanoacrylate compound, nickel network salt compounds etc., however it is not limited to these compounds.
The organic solvent used, general more common person are ethylene glycol monomethyl ether, ethylene glycol ethyl ether, diethylene glycol methyl ether, diethylene glycol (DEG) Ether, diethylene glycol (DEG) positive propyl ether, diethylene glycol n-butyl ether, triethylene glycol methyl ether, triethylene glycol ether, propylene glycol monomethyl ether, propylene-glycol ethyl ether, one Contracting dipropylene glycol methyl ether, dipropylene glycol ether, dipropylene glycol positive propyl ether, dipropylene glycol n-butyl ether, two contractings three Propylene glycol monomethyl ether (tripropyleneglycolmonomethylether), tripropylene glycol ether (tripropyleneglycolmonoethylether) its (poly-) alkylene glycol mono alkane ethers such as；Ethylene glycol monomethyl ether acetic acid Ester, ethylene glycol ether acetate, propylene glycol methyl ether acetate, propylene-glycol ethyl ether acetate etc. (poly-) alkylene glycol mono alkane ether vinegar Esters of gallic acid；Other ethers such as diethylene glycol dimethyl ether, diethylene glycol (DEG) ethyl methyl ether, diethyl carbitol, tetrahydrofuran；Methyl ethyl ketone, hexamethylene The ketones such as ketone, 2-HEPTANONE, 3- heptanone；The lactic acid alkyl ester class such as 2 hydroxy propanoic acid methyl esters, 2 hydroxy propanoic acid ethyl ester；2- hydroxyl -2- first Base methyl propionate, 2- hydroxy-2-methyls ethyl propionate, 3- methoxy methyl propionates, 3- methoxypropionates, 3- ethoxy-cs Sour methyl esters, 3- ethoxyl ethyl propionates, ethoxy ethyl acetate, hydroxyl ethyl acetate, 2- hydroxy-3-methyls methyl butyrate, 3- Methyl -3- methoxybutyls acetic acid esters, 3- methyl -3- methoxybutyls propionic ester, ethyl acetate, n-butyl acetate, acetic acid are just Propyl ester, isopropyl acetate, n-butyl acetate, isobutyl acetate, n-amyl acetate, isoamyl acetate, n-butyl propionate, butyric acid second Ester, propyl butyrate, isopropyl isobutyrate, butyric acid N-butyl, methyl pyruvate, ethyl pyruvate, pyruvic acid n-propyl, acetyl second Other esters such as sour methyl esters, ethyl acetoacetate, 2- oxygroup ethyl butyrates；The aromatic hydrocarbons class such as toluene, dimethylbenzene； Carboxylic acyloxies amine such as N-Methyl pyrrolidone, n,N-Dimethylformamide, n,N-dimethylacetamide etc..The equal solvent can be single It solely uses, can also mix two or more use.
Further include having epoxy resin diluent in the composition, glycidol ethers can be selected from, as normal-butyl shrink is sweet Oily ether, octyl glycidyl ether, C12~C14 alkyl glycidyl ethers, methyl propenoic acid glycidyl ether, benzoic acid shrink sweet Oily ether, diglycidyl ether, glycol glycidyl ethers, l, 4- butanediol glycidol ethers, hexylene glycol glycidol ether, new penta Glycol glycidol ether, resorcinol glycidol ether, glycerin triglycidyl ether, trihydroxymethylpropanyltri diglycidyl ether One or more of mixture.
Further include having curing agent in composition, dosage preferred scope is 4~9 parts, generally as epoxy curing agent And known curing agent can use.Preferred curing agent is phenol system curing agent.There is phenoloid in phenol system curing agent, Phenoloid also includes phenolic resin in addition to the phenolic compounds as single compound.As the specific of phenol system curing agent Example, can enumerate：Bisphenol-A, Bisphenol F, 4,4 '-dihydroxydiphenyl methane, 4,4 '-dihydroxy diphenyl ethers, bis- (the 4- hydroxyls of Isosorbide-5-Nitrae- Phenoxy group) benzene, bis- (4- hydroxyphenoxies) benzene of 1,3-, 4,4 '-dihydroxy diphenyl sulfides, 4,4 '-dihydroxydiphenyl ketone, 4, 4 '-dihydroxy-diphenyl sulfones, 4,4 '-dihydroxybiphenyls, 2,2 '-dihydroxybiphenyls, 10- (2,5- dihydroxy phenyl) -10H-9- Oxa- -10- phospho hetero phenanthrene -10- oxides, phenol novolacs, bisphenol A novolac, o-cresol novolak, metacresol phenolic aldehyde Varnish, paracresol novolaks, xylenol novolaks, poly(4-hydroxystyrene), hydroquinone, resorcinol, catechol, Tert-butyl catechol, tert-butyl hydroquinone, pyrogallol, tert-butyl o benzenetriol, allylation pyrogallol, polyene third Base pyrogallol, 1,2,4- benzene triols, 2,3,4- trihydroxybenzophenones, 1,2- dihydroxy naphthlenes, 1,3- dihydroxy naphthlenes, Isosorbide-5-Nitrae- Dihydroxy naphthlene, 1,5- dihydroxy naphthlenes, 1,6- dihydroxy naphthlenes, 1,7- dihydroxy naphthlenes, 1,8- dihydroxy naphthlenes, 2,3- dihydroxy naphthlenes, 2, 4- dihydroxy naphthlenes, 2,5- dihydroxy naphthlenes, 2,6- dihydroxy naphthlenes, 2,7- dihydroxy naphthlenes, 2,8- dihydroxy naphthlenes, above-mentioned dihydroxy naphthlene Allyl compound or polyallyl compound, allylation bisphenol-A, allylation Bisphenol F, allylation phenol novolacs, alkene Propylated pyrogallol etc..
Further include having curing accelerator in composition, is organic ureas accelerating agent, such as fenuron；Or imidazoles, imidazole derivatives Object, such as 2- ethyls 4-methylimidazole (2E4MI).
The preparation method of the modified epoxy, includes the following steps：
S11, by weight, by 10~15 parts of tung oil, 40~55 parts of fatty alcohol, acid or basic catalyst 0.05~ 0.08 part of generation alcoholysis reaction, obtains the first reactant；
Then S12 is added 40~60 parts of organic acid anhydride, 5~10 parts of polyphosphoric acid, 0.1~0.2 part of polymerization inhibitor, is reacted, Obtain the second reactant；
Second reactant, 5~10 parts of Isosorbide-5-Nitrae butanediol, 3~5 parts of trimethylolpropane are added to E51 epoxy resin S13 It in 100~150 parts, is reacted, obtains modified epoxy.
In the S11 steps, fatty alcohol is selected from isomerous tridecanol, ten alcohol of isomery, seven alcohol of isomery, polyethylene glycol or poly- third One or more of mixture in glycol.
In the S12 steps, organic acid anhydride is a kind of or several in maleic anhydride, acetic anhydride, phthalic anhydride The mixture of kind.
In the S11 steps, basic catalyst is sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium ethoxide, potassium ethoxide, first Sodium alkoxide, potassium methoxide or calcium oxalate.
In the S11 steps, acidic catalyst is sulfuric acid, hydrochloric acid, nitric acid or sulfonic acid.
In the S11 steps, reaction temperature is 180~220 DEG C, 1~10h of reaction time.
In the S12 steps, reaction temperature is 50~200 DEG C, 1~10h of reaction time.
In the S13 steps, reaction temperature is 110~120 DEG C, 1~3 hour reaction time.
The preparation method of the modified polypropene acid resin, includes the following steps：
S21, by weight, by 20~25 parts of ethyl methacrylate, 15~20 parts of methyl acrylate and acrylic acid 15 ~20 parts are uniformly mixed, as monomer mixture；4~6 parts of cationic monomer, N, N- dihexyls is added in monomer mixture again 5~10 parts of 5~10 parts of methylamine and trim,ethylchlorosilane are uniformly mixed；
S22 adds 140~170 parts of assistant for emulsifying agent, 70~80 parts of water, and after mixing, initiator 10 is added dropwise in heating ~15 parts, after being added dropwise, insulation reaction cools the temperature to room temperature after reaction, be added ammonium hydroxide adjust pH value to 7.5~ 9.5；Filtering and discharging, decompression steam solvent and obtain resin.
In the S21 steps, the cationic monomer is MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, metering system Sour dimethylamino ethyl ester or dimethyl diallyl ammonium chloride.
In the S22 steps, initiator is ammonium persulfate, potassium peroxydisulfate or azo diisobutyl amidine hydrochloride；Reaction 2~4 hours time, 60~80 DEG C of reaction temperature.
The preparation method of conducting resinl, includes the following steps：After mixing by each component, using grinding.
Advantageous effect
The conducting resinl that the present invention is prepared, have the advantages that adhesive strength is high, conduct electricity very well, heat-transfer effect it is good.
Specific implementation mode
Embodiment 1
For the conducting resinl of LED chip bonding, it is made of following component by weight：30 parts of modified epoxy, 40 parts of bisphenol f type epoxy resin, 15 parts of modified polypropene acid resin, epoxy resin diluent (methyl propenoic acid glycidyl ether) 12 parts, 300 parts of silver powder, 3 parts of curing agent (tert-butyl hydroquinone), 2 parts of imidazoles system curing accelerator, organic solvent isopropyl acetate 30 parts of ester, 1 part of triazine-based ultraviolet absorbent, 3 parts of dispersant (sodium laureth sulfate)；Preparation method is will be each A component after mixing, using grinding.
The preparation method of the modified epoxy, includes the following steps：
S11, by weight, by 0.05 part of 10 parts of tung oil, 40 parts of isomerous tridecanol, potassium hydroxide catalyst generation alcoholysis Reaction, reaction temperature is 180 DEG C, and reaction time 1h obtains the first reactant；
Then S12 is added 40 parts of acetic anhydride, 5 parts of polyphosphoric acid, 0.1 part of polymerization inhibitor, is reacted, reaction temperature is 50 DEG C, Reaction time 1h obtains the second reactant；
Second reactant, 5 parts of Isosorbide-5-Nitrae butanediol, 3 parts of trimethylolpropane are added to 100 parts of E51 epoxy resin S13 In, it is reacted, reaction temperature is 110 DEG C, in 1 hour reaction time, obtains modified epoxy.
The preparation method of the modified polypropene acid resin, includes the following steps：
S21, it is by weight, 20 parts of ethyl methacrylate, 15 parts of methyl acrylate and 15 parts of mixing of acrylic acid are equal It is even, as monomer mixture；4 parts of dimethylaminoethyl methacrylate, N, N- dihexyls is added in monomer mixture again 5 parts of 5 parts of methylamine and trim,ethylchlorosilane are uniformly mixed；
S22 adds 140 parts of assistant for emulsifying agent, 70 parts of water, and after mixing, initiator ammonium persulfate 10 is added dropwise in heating Part, after being added dropwise, insulation reaction, in 2 hours reaction time, 60 DEG C of reaction temperature after reaction, cools the temperature to room temperature, Ammonium hydroxide is added and adjusts pH value to 7.5, filtering and discharging, decompression steams solvent and obtains resin.
Embodiment 2
For the conducting resinl of LED chip bonding, it is made of following component by weight：40 parts of modified epoxy, 50 parts of bisphenol f type epoxy resin, 20 parts of modified polypropene acid resin, epoxy resin diluent (methyl propenoic acid glycidyl ether) 15 parts, 600 parts of silver powder, 4 parts of curing agent (tert-butyl hydroquinone), 5 parts of imidazoles system curing accelerator, organic solvent acetic acid it is different 40 parts of propyl ester, 3 parts of triazine-based ultraviolet absorbent, 5 parts of dispersant (sodium laureth sulfate)；Preparation method is After mixing by each component, using grinding.
The preparation method of the modified epoxy, includes the following steps：
S11, by weight, by 0.08 part of 15 parts of tung oil, 55 parts of isomerous tridecanol, potassium hydroxide catalyst generation alcoholysis Reaction, reaction temperature is 220 DEG C, and reaction time 10h obtains the first reactant；
Then S12 is added 60 parts of acetic anhydride, 10 parts of polyphosphoric acid, 0.2 part of polymerization inhibitor, is reacted, reaction temperature is 200 DEG C, reaction time 10h obtains the second reactant；
Second reactant, 10 parts of Isosorbide-5-Nitrae butanediol, 5 parts of trimethylolpropane are added to 150 parts of E51 epoxy resin S13 In, it is reacted, reaction temperature is 120 DEG C, in 3 hours reaction time, obtains modified epoxy.
The preparation method of the modified polypropene acid resin, includes the following steps：
S21, it is by weight, 25 parts of ethyl methacrylate, 20 parts of methyl acrylate and 20 parts of mixing of acrylic acid are equal It is even, as monomer mixture；6 parts of dimethylaminoethyl methacrylate, N, N- dihexyls is added in monomer mixture again 10 parts of 10 parts of methylamine and trim,ethylchlorosilane are uniformly mixed；
S22 adds 170 parts of assistant for emulsifying agent, 80 parts of water, and after mixing, initiator ammonium persulfate 15 is added dropwise in heating Part, after being added dropwise, insulation reaction, in 4 hours reaction time, 80 DEG C of reaction temperature after reaction, cools the temperature to room temperature, Ammonium hydroxide is added and adjusts pH value to 9.5, filtering and discharging, decompression steams solvent and obtains resin.
Embodiment 3
For the conducting resinl of LED chip bonding, it is made of following component by weight：35 parts of modified epoxy, 45 parts of bisphenol f type epoxy resin, 18 parts of modified polypropene acid resin, epoxy resin diluent (methyl propenoic acid glycidyl ether) 13 parts, 500 parts of silver powder, 3 parts of curing agent (tert-butyl hydroquinone), 3 parts of imidazoles system curing accelerator, organic solvent isopropyl acetate 35 parts of ester, 2 parts of triazine-based ultraviolet absorbent, 4 parts of dispersant (sodium laureth sulfate)；Preparation method is will be each A component after mixing, using grinding.
The preparation method of the modified epoxy, includes the following steps：
S11, by weight, by 0.07 part of 12 parts of tung oil, 50 parts of isomerous tridecanol, potassium hydroxide catalyst generation alcoholysis Reaction, reaction temperature is 200 DEG C, and reaction time 5h obtains the first reactant；
Then S12 is added 50 parts of acetic anhydride, 7 parts of polyphosphoric acid, 0.1 part of polymerization inhibitor, is reacted, reaction temperature is 150 DEG C, reaction time 7h obtains the second reactant；
Second reactant, 7 parts of Isosorbide-5-Nitrae butanediol, 4 parts of trimethylolpropane are added to 140 parts of E51 epoxy resin S13 In, it is reacted, reaction temperature is 115 DEG C, in 2 hours reaction time, obtains modified epoxy.
The preparation method of the modified polypropene acid resin, includes the following steps：
S21, it is by weight, 22 parts of ethyl methacrylate, 16 parts of methyl acrylate and 17 parts of mixing of acrylic acid are equal It is even, as monomer mixture；5 parts of dimethylaminoethyl methacrylate, N, N- dihexyls is added in monomer mixture again 6 parts of 6 parts of methylamine and trim,ethylchlorosilane are uniformly mixed；
S22 adds 160 parts of assistant for emulsifying agent, 75 parts of water, and after mixing, initiator ammonium persulfate 12 is added dropwise in heating Part, after being added dropwise, insulation reaction, in 3 hours reaction time, 65 DEG C of reaction temperature after reaction, cools the temperature to room temperature, Ammonium hydroxide is added and adjusts pH value to 8.0, filtering and discharging, decompression steams solvent and obtains resin.
Reference examples 1
With embodiment 3 difference lies in：Epoxy resin without modification.
For the conducting resinl of LED chip bonding, it is made of following component by weight：It is 35 parts of E51 epoxy resin, double 45 parts of phenol F types epoxy resin, 18 parts of modified polypropene acid resin, epoxy resin diluent (methyl propenoic acid glycidyl ether) 13 Part, 500 parts of silver powder, 3 parts of curing agent (tert-butyl hydroquinone), 3 parts of imidazoles system curing accelerator, organic solvent isopropyl acetate 35 parts, 2 parts of triazine-based ultraviolet absorbent, 4 parts of dispersant (sodium laureth sulfate)；Preparation method is will be each Component after mixing, using grinding.
The preparation method of the modified polypropene acid resin, includes the following steps：
S21, it is by weight, 22 parts of ethyl methacrylate, 16 parts of methyl acrylate and 17 parts of mixing of acrylic acid are equal It is even, as monomer mixture；5 parts of dimethylaminoethyl methacrylate, N, N- dihexyls is added in monomer mixture again 6 parts of 6 parts of methylamine and trim,ethylchlorosilane are uniformly mixed；
S22 adds 160 parts of assistant for emulsifying agent, 75 parts of water, and after mixing, initiator ammonium persulfate 12 is added dropwise in heating Part, after being added dropwise, insulation reaction, in 3 hours reaction time, 65 DEG C of reaction temperature after reaction, cools the temperature to room temperature, Ammonium hydroxide is added and adjusts pH value to 8.0, filtering and discharging, decompression steams solvent and obtains resin.
Reference examples 2
With embodiment 3 difference lies in：Polyphosphoric acid is not added in the modification procedure of epoxy resin.
For the conducting resinl of LED chip bonding, it is made of following component by weight：35 parts of modified epoxy, 45 parts of bisphenol f type epoxy resin, 18 parts of modified polypropene acid resin, epoxy resin diluent (methyl propenoic acid glycidyl ether) 13 parts, 500 parts of silver powder, 3 parts of curing agent (tert-butyl hydroquinone), 3 parts of imidazoles system curing accelerator, organic solvent isopropyl acetate 35 parts of ester, 2 parts of triazine-based ultraviolet absorbent, 4 parts of dispersant (sodium laureth sulfate)；Preparation method is will be each A component after mixing, using grinding.
The preparation method of the modified epoxy, includes the following steps：
S11, by weight, by 0.07 part of 12 parts of tung oil, 50 parts of isomerous tridecanol, potassium hydroxide catalyst generation alcoholysis Reaction, reaction temperature is 200 DEG C, and reaction time 5h obtains the first reactant；
Then S12 is added 50 parts of acetic anhydride, 0.1 part of polymerization inhibitor, is reacted, reaction temperature is 150 DEG C, the reaction time 7h obtains the second reactant；
Second reactant, 7 parts of Isosorbide-5-Nitrae butanediol, 4 parts of trimethylolpropane are added to 140 parts of E51 epoxy resin S13 In, it is reacted, reaction temperature is 115 DEG C, in 2 hours reaction time, obtains modified epoxy.
The preparation method of the modified polypropene acid resin, includes the following steps：
S21, it is by weight, 22 parts of ethyl methacrylate, 16 parts of methyl acrylate and 17 parts of mixing of acrylic acid are equal It is even, as monomer mixture；5 parts of dimethylaminoethyl methacrylate, N, N- dihexyls is added in monomer mixture again 6 parts of 6 parts of methylamine and trim,ethylchlorosilane are uniformly mixed；
S22 adds 160 parts of assistant for emulsifying agent, 75 parts of water, and after mixing, initiator ammonium persulfate 12 is added dropwise in heating Part, after being added dropwise, insulation reaction, in 3 hours reaction time, 65 DEG C of reaction temperature after reaction, cools the temperature to room temperature, Ammonium hydroxide is added and adjusts pH value to 8.0, filtering and discharging, decompression steams solvent and obtains resin.
For the above-mentioned epoxide resin conductive adhesive being prepared after being heating and curing, performance parameter is as follows：
Conductivity Ω cm Thermal conductivity W/mK Shear strength mPa
Embodiment 1 6.1×10-4 3.2 7.6
Embodiment 2 6.2×10-4 3.2 7.6
Embodiment 3 7.1×10-4 3.6 8.3
Reference examples 1 8.7×10-5 2.2 7.4
Reference examples 2 4.2×10-5 2.6 7.6
As can be seen from the table, the conducting resinl that the present invention is prepared not only maintains preferable electric conductivity, simultaneously also With preferable thermal conductivity and shear strength.Embodiment 3 is compared with reference examples 1 as can be seen that by changing to E51 epoxy resin Property, the heat conductivility of the conducting resinl can be effectively improved by introducing phosphate grafted moiety；Embodiment 3 can with the comparison of reference examples 1 To find out, by introducing polyphosphoric acid during epoxy resin modification, the adhesive strength of conducting resinl can effectively improve.

Claims (5)

1. a kind of conducting resinl for LED chip bonding, which is characterized in that include following component by weight：It is modified 30~40 parts of epoxy resin, 40~50 parts of bisphenol f type epoxy resin, 15~20 parts of modified polypropene acid resin, epoxy resin are dilute Release 12~15 parts of agent, 300~600 parts of silver powder, 3~4 parts of curing agent, 2~5 parts of curing accelerator, 30~40 parts of organic solvent, purple 1~3 part of ultraviolet absorbers, 3~5 parts of dispersant；The preparation method of the modified epoxy, includes the following steps：S11, By weight, by 10~15 parts of tung oil, 40~55 parts of fatty alcohol, acid or 0.05~0.08 part of generation alcoholysis of basic catalyst Reaction, obtains the first reactant；Then 40~60 parts of organic acid anhydride, 5~10 parts of polyphosphoric acid, polymerization inhibitor 0.1~0.2 is added in S12 Part, it is reacted, obtains the second reactant；S13, by the second reactant, 5~10 parts of Isosorbide-5-Nitrae butanediol, trimethylolpropane 3~5 Part is added into 100~150 parts of E51 epoxy resin, is reacted, obtains modified epoxy；In the S11 steps, fat Alcohol mixture one or more of in isomerous tridecanol, ten alcohol of isomery, seven alcohol of isomery, polyethylene glycol or polypropylene glycol； In the S12 steps, one or several kinds of mixing of the organic acid anhydride in maleic anhydride, acetic anhydride, phthalic anhydride Object；In the described S11 steps, basic catalyst be sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium ethoxide, potassium ethoxide, sodium methoxide, Potassium methoxide or calcium oxalate；In the S11 steps, acidic catalyst is sulfuric acid, hydrochloric acid, nitric acid or sulfonic acid.
2. the conducting resinl according to claim 1 for LED chip bonding, which is characterized in that the dispersant is preferred It is sodium laureth sulfate.
3. the conducting resinl according to claim 1 for LED chip bonding, which is characterized in that the curing agent is uncle Butylhydroquinone.
4. the conducting resinl according to claim 1 for LED chip bonding, which is characterized in that the epoxy resin is dilute It is methyl propenoic acid glycidyl ether to release agent.
5. the conducting resinl according to claim 1 for LED chip bonding, which is characterized in that the organic solvent is Isopropyl acetate.
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CN107353853A (en) * 2017-08-24 2017-11-17 蒋磊 A kind of graphite conductive adhesive and its preparation technology
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CN116130143A (en) * 2022-12-30 2023-05-16 上海席亚高分子材料有限公司 High-temperature-resistant elastic conductive silver paste and preparation method thereof

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CN103242775A (en) * 2013-05-16 2013-08-14 长春永固科技有限公司 Acrylic ester modified epoxy resin conductive chip adhesive
CN103627357A (en) * 2013-11-18 2014-03-12 长春永固科技有限公司 Large-power conductive chip adhesive
CN104629642A (en) * 2015-02-12 2015-05-20 矽照光电（厦门）有限公司 Preparation method of epoxy resin conductive adhesive for bonding LED chip

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CN103242775A (en) * 2013-05-16 2013-08-14 长春永固科技有限公司 Acrylic ester modified epoxy resin conductive chip adhesive
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