CN116731653A - Epoxy packaging material for small-space display screen and preparation method and application thereof - Google Patents

Epoxy packaging material for small-space display screen and preparation method and application thereof Download PDF

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Publication number
CN116731653A
CN116731653A CN202310989864.XA CN202310989864A CN116731653A CN 116731653 A CN116731653 A CN 116731653A CN 202310989864 A CN202310989864 A CN 202310989864A CN 116731653 A CN116731653 A CN 116731653A
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epoxy resin
epoxy
parts
bisphenol
bond
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CN116731653B (en
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单秋菊
谭晓华
孙绪筠
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Tianjin Degao Huacheng Optoelectronics Technology Co ltd
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Tianjin Degao Huacheng Optoelectronics 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
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/14—Polycondensates modified by chemical after-treatment
    • C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
    • C08G59/1438—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/14—Polycondensates modified by chemical after-treatment
    • C08G59/1494—Polycondensates modified by chemical after-treatment followed by a further chemical treatment thereof
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Emergency Medicine (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • Epoxy Resins (AREA)

Abstract

The application relates to the technical field of packaging materials, and particularly provides a small-space display screen epoxy packaging material, and a preparation method and application thereof. According to the application, different epoxy resins are compounded and used, the epoxy resins are modified, and the synergistic performance of the components is utilized, so that the epoxy packaging material has lower warpage and shrinkage, and also has excellent flowability, ink consistency, packaging reliability, high and low temperature impact resistance, reflow soldering resistance and other performances during packaging use, and can meet the packaging requirements of a thinner BT resin substrate.

Description

Epoxy packaging material for small-space display screen and preparation method and application thereof
Technical Field
The application relates to the technical field of packaging materials, in particular to a small-space display screen epoxy packaging material and a preparation method and application thereof.
Background
The small-spacing LED display screen refers to an indoor LED display screen with the LED point spacing of P2.5 or below. The small-spacing LED display screen adopts a pixel-level point control technology to realize the state control of the brightness, color reducibility and uniformity of the pixel units of the display screen. Along with the improvement of the manufacturing technology of the LED display screen, the resolution of the traditional LED display screen is greatly improved, graphic images and videos with higher definition can be displayed, more paths of videos and image pictures can be displayed, and particularly, the application in the aspect of image splicing can be realized, so that seamless and arbitrary large-area splicing can be realized.
The LED packaging material mainly comprises epoxy resin, organic silicon and the like, and the organic silicon material has better high and low temperature resistance, oxidation resistance and weather resistance, but has the defects of low hardness, easy moisture absorption, insufficient compactness, lower bonding strength and the like, so that the application of the LED packaging material is limited; epoxy resin has excellent formability, heat resistance, mechanical properties and adhesiveness, but has large shrinkage and is easy to warp, and particularly when the epoxy resin is used as a packaging material on a BT resin substrate, the packaging material is used as a packaging material on a thin substrate because the thermal expansion coefficient of the epoxy resin and the packaging material is about 158ppm different, and the packaging material is often warped when being solidified and cooled, so that a device cannot be cut or the cutting yield is reduced, and the packaging requirement of a small-space display screen and the use of the device on the thin substrate are difficult to meet.
Chinese patent publication No. CN102558769B, 11/25, discloses an epoxy resin composition for encapsulating semiconductor devices and semiconductor devices encapsulated by the epoxy resin composition, wherein the epoxy resin used is an arene-formaldehyde resin modified novolac epoxy resin, and although the composition prepared therefrom has good flowability, it is difficult to meet the encapsulation requirement of BT resin substrates, and there is a potential risk of warpage. The Chinese patent publication No. CN103468095B is specially beneficial to the 8 th and 10 th of 2016 and discloses a silane coupling agent modified epoxy resin and a preparation method thereof.
Disclosure of Invention
In order to solve the technical problems, the application firstly provides the epoxy packaging material for the small-space display screen, and the packaging material has the characteristics of small shrinkage, low warpage, high packaging reliability, high and low temperature impact resistance, reflow soldering resistance and the like by utilizing the synergistic effect of the components.
Further, the epoxy packaging material comprises the following components in parts by weight: 100 parts of modified epoxy resin, 0.001-1 part of pigment, 20-850 parts of inorganic filler, 0.01-4 parts of adhesion promoter, 1-3 parts of antioxidant and 0.1-2 parts of auxiliary agent.
Further, the preparation raw materials of the modified epoxy resin comprise: 100 parts of epoxy resin, 20-160 parts of curing agent, 3-50 parts of chain extender and 0.05-3 parts of cross-linking agent.
The components of the small-spacing display screen epoxy packaging material are different from the metering standard of the weight parts of the preparation raw materials of the modified epoxy resin.
Further, the epoxy resin is selected from one or a combination of several of alicyclic epoxy resin, bisphenol A/bisphenol F/bisphenol S type linear phenolic epoxy resin, biphenyl type epoxy resin, naphthalene ring epoxy resin, hydrogenated bisphenol A/bisphenol F/bisphenol S type linear phenolic epoxy resin, multifunctional group epoxy resin, aliphatic glycidyl ether type epoxy resin, polyphenol type glycidyl ether type epoxy resin, glycidyl ester type epoxy resin, triglycidyl isocyanurate, diglycidyl isocyanurate.
Further, the epoxy resin comprises at least one of alicyclic epoxy resin, biphenyl type epoxy resin, naphthalene ring epoxy resin, polyphenol type glycidyl ether epoxy resin, triglycidyl isocyanurate and diglycidyl isocyanurate, and the dosage of the epoxy resin is 30-90wt.% of the total amount of the epoxy resin; preferably 40-85wt.%; further preferably 50-80wt.%.
Preferably, the epoxy resin comprises an alicyclic epoxy resin selected from at least one or a combination of several of bis (7-oxabicyclo [4.1.0] 3-heptylmethyl) adipate, bis ((3, 4-epoxycyclohexyl) methyl) adipate, poly [ (2-oxiranyl) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether.
Further, the epoxy resin further comprises at least one of bisphenol A/bisphenol F/bisphenol S type linear epoxy resin, bisphenol A/bisphenol F/bisphenol S type linear phenolic epoxy resin, hydrogenated bisphenol A/bisphenol F/bisphenol S type linear epoxy resin and aliphatic glycidyl ether type epoxy resin.
Preferably, the epoxy resin further comprises at least one of bisphenol a/bisphenol F/bisphenol S type linear epoxy resins.
Further, the curing agent is selected from any one of phenolic resin, anhydride and aromatic amine.
Preferably, the curing agent is an anhydride, and may be at least one selected from the group consisting of phthalic anhydride, trimellitic anhydride, pyromellitic dianhydride, hydrogenated pyromellitic dianhydride, maleic anhydride, tetrahydrophthalic anhydride, methylphthalic anhydride, methyltetrahydrophthalic anhydride, hexahydrophthalic anhydride, methylhexahydrophthalic anhydride, tung oil anhydride, dodecenylsuccinic anhydride, nadic anhydride, methylnadic anhydride, glutaric anhydride, hydrogenated methylnadic anhydride, methylcyclohexene tetracarboxylic dianhydride, polyazelaic anhydride, polysebacic anhydride, and 1,4,5, 6-tetrabromophthalic anhydride.
In a preferred embodiment, the curing agent is any one of phthalic anhydride, tetrahydrophthalic anhydride, methyltetrahydrophthalic anhydride, maleic anhydride, and methylphthalic anhydride.
Further, the chain extender is a diol or polyol, preferably a C2-C6 diol or polyol.
Further, the C2-C8 dihydric or polyhydric alcohol includes, but is not limited to, at least one of ethylene glycol, propylene glycol, 1, 3-propanediol, 1, 4-butanediol, 1, 3-butanediol, 1, 2-butanediol, 1, 5-pentanediol, 1, 6-hexanediol, neopentyl glycol, diethylene glycol, triethylene glycol, dipropylene glycol, 3-methyl-1, 5-pentanediol, 1, 3-or 1, 4-cyclohexanedimethanol and mixtures thereof, 1, 4-cyclohexanediol, 1, 4-dihydroxy-2-butene, 2, 6-dimethyl-1-octene-3, 8-diol, trimethylolpropane.
In a preferred embodiment, the C2-C8 dihydric or polyhydric alcohol is any one of propylene glycol, 1, 3-propylene glycol, 1, 4-butanediol, 1, 3-butanediol, 1, 2-butanediol.
Further, the cross-linking agent is a C9-C20 ester ring compound containing Si-O bond and/or a C4-C15 chain compound containing Si-O bond.
Preferably, the crosslinking agent is a combination of a C9-C20 ester ring compound containing Si-O bonds and a C4-C15 chain compound containing Si-O bonds.
The compound containing Si-O bond can branch Si-O bond into molecular chain of ring-opened epoxy resin, and because of structural characteristic of Si-O bond, its grafting on epoxy resin molecular chain can effectively raise crosslinking degree of system, raise structural strength of epoxy resin and inhibit its shrink deformation capability, but the application unexpectedly discovers that: when a combination of a C9-C20 ester ring compound having Si-O bond and a C4-C15 chain compound having Si-O bond is used, the mass ratio thereof is further defined as (0.5-5): 1, the epoxy encapsulating material prepared also has more excellent PCT reliability and impact resistance, presumably because: the C9-C20 ester ring compound containing Si-O bond can further improve the mechanical property of the epoxy resin and the crosslinking degree of the system due to the existence of the ester ring, but when the content of the ester ring compound is too high, the cohesion of the system is too strong to buffer the internal stress; the fluidity of the C4-C15 chain compound containing Si-O bonds is good, but when the compound is excessive, the compactness of the epoxy resin system is poor, and the epoxy resin system is more easily influenced by temperature and water vapor; the proportion of the two is regulated and controlled, and the mechanical strength, flexibility and compatibility of the epoxy packaging material are improved by utilizing the synergistic effect of the epoxy packaging material and other components in the system.
Further, the C9-C20 ester ring compound containing Si-O bond includes but is not limited to one of 1- [2- (trimethoxysilyl) ethyl ] -3, 4-epoxycyclohexane, 2,4,6, 8-tetramethyl-2- [3- (oxiranylmethoxy) propyl ] cyclotetrasiloxane.
Further, the Si-O bond-containing C4-C15 chain compound is at least one selected from the group consisting of 3- (trimethoxysilyl) -1-propanethiol, 3-triethoxysilyl-1-propanamine, 3- (trimethoxysilyl) propyl-2-methyl-2-acrylate, N- (. Beta. -aminoethyl-. Gamma. -aminopropyl) trimethoxysilane.
Further, the preparation method of the modified epoxy resin comprises the following steps: stirring epoxy resin at 130-180 ℃; then adjusting the temperature to 40-125 ℃, adding the curing agent, the chain extender and the crosslinking agent, and stirring for 5-40 min.
Further, the pigment is selected from one or a combination of several of carbon black, iron oxide black, zinc powder, lakes, azo, heterocyclic and phthalocyanine.
Further, the inorganic filler has a general formula of M (1-x-y-z-u)+v A x B y C z D u E v O 0.5(1+x+2y+3z+3u) Wherein M is selected from Na or K; a is selected from any one of Mg, ca, sr, zn; b is selected from any one of B, al and Ga; c is selected from any one of Si, ge and Sn; d is selected from Zr or Ti; e is selected from F or Cl; specifying x<0.3；0.1<y<0.3；0.4<z<0.7；u<0.3；v<0.1, and x+y+z+u-v>0.1。
Further, the inorganic filler has a particle diameter D50 of 1-10 μm; the refractive index is 1.4 to 1.6, more preferably 1.46 to 1.56.
Preferably, the inorganic filler is an inorganic oxide microbead disclosed in chinese patent CN110283561B, which was issued by the present inventors 2021, 9, 10.
Further, the adhesion promoter is selected from one or more of silanes, pyrimidines and triazines; silanes are preferred.
Preferably, the adhesion promoter is selected from one or more of aminoethylaminopropyl trimethoxysilane, aminopropyl triethoxysilane, gamma-glycidoxypropyl trimethoxysilane, gamma-methacryloxypropyl methyl dimethoxy silane, gamma-methacryloxypropyl methyl diethoxysilane, gamma- (2, 3-glycidoxypropyl) propyl triethoxysilane, gamma- (glycidoxypropyl) propyl methyl dimethoxy silane, beta- (epoxycyclohexyl) ethyl trimethoxysilane, mercaptopropyl triethoxysilane, tetraepoxycyclohexylethyl tetramethyl cyclosiloxane, trioxycyclohexylethyl tetramethyl cyclosiloxane, dicyclohexylethyl tetramethyl cyclosiloxane, tetramethyl cyclohexylethyl cyclosiloxane, tetramethyl tetraethyl methoxypropyl cyclosiloxane, tetramethyl ethylene oxide methoxypropyl cyclosiloxane, vinyl tri (beta-methylethylvinyl) silane.
In a preferred embodiment, the amino ethyl amino propyl trimethoxysilane, gamma-glycidyl ether oxypropyl trimethoxysilane, gamma-methacryloxypropyl trimethoxysilane, mercaptopropyl triethoxysilane, vinyl tris (beta-methylethylvinyl) silane, amino propyl triethoxysilane.
Further, the antioxidant is selected from any one or a combination of a plurality of hindered phenol antioxidants, phosphite antioxidants and thioester antioxidants.
The hindered phenol antioxidant is preferably selected from any one or a combination of a plurality of BHT, 1010, 1076, 1098, 1024 and 245.
The phosphite antioxidant is selected from 168 and/or 626.
The thio ester antioxidant is selected from DLTP and/or DSTP.
In one embodiment, the antioxidant is a combination of hindered phenolic antioxidants and phosphite antioxidants, in a mass ratio of 1: (0.1-3).
In a preferred embodiment, the antioxidants are 168 and 1010 in a mass ratio of 1: (0.2-2).
In another preferred embodiment, the antioxidant is 245.
Further, the auxiliary agent is at least one selected from amide, organic phosphine, organic phosphate, organic phosphonium halide, amine substance and nitrogen-containing heterocyclic compound.
Further, the auxiliary agent is at least one selected from caprolactam, triphenylphosphine, methyl trioctyl phosphonium dimethyl phosphate, tetrabutyl phosphonium acetate, methyl tributyl phosphonium dimethyl phosphate, benzyl triphenyl phosphonium chloride, tetrabutyl phosphonium chloride, N-dimethylaminobenzene, N-dimethylcyclohexylamine, N-dimethylbenzylamine, ethylamine, methylamine, isopropylamine, N-propylamine triethylamine, diethylenetriamine, triethanolamine, 2-methylimidazole, 2-ethylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, benzimidazole and dimethylimidazole urea.
Preferably, the auxiliary agent is any one of 2-methylimidazole, 2-ethylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, benzimidazole, ethylamine, methylamine, isopropylamine and diethylenetriamine.
The application further provides a preparation method of the small-space display screen epoxy packaging material, which comprises the following steps: mixing inorganic filler, pigment, adhesion promoter, antioxidant and modified epoxy resin, stirring at 60-140deg.C for 5-60min, adding adjuvant, stirring for 1-15min, discharging, cooling, pulverizing, and making cake.
Furthermore, the application also provides application of the small-space display screen epoxy packaging material in BT resin substrate packaging.
Further, the thickness of the encapsulation layer of the epoxy encapsulation material is smaller than 0.6mm.
Further, the BT resin substrate thickness is 0.28mm or less.
Advantageous effects
According to the application, different epoxy resins are used in a compounding way, and anhydride, a C9-C20 ester ring compound containing Si-O bonds and a C4-C15 chain compound containing Si-O bonds are used for modifying the epoxy resins, so that the synergistic effect of the modified epoxy resins, inorganic fillers and other components is utilized to regulate the crosslinking degree and structural strength of an epoxy resin system, the basic thermal expansion coefficient difference between the modified epoxy resins and BT resins is reduced, and the warping and shrinkage rate of the prepared packaging material after packaging the BT resin substrate is reduced; the warping degree is further reduced through component optimization and the synergistic effect of the components, and meanwhile, the packaging material has excellent ink consistency, packaging reliability, high and low temperature impact resistance, reflow soldering resistance and other performances.
Drawings
Fig. 1 is a sample of the epoxy encapsulating material of example 1 after encapsulation for handling properties.
Fig. 2 is a sample to be tested for warpage performance of the epoxy encapsulation material of example 1.
Detailed Description
Examples
Example 1
The embodiment provides a small-space display screen epoxy packaging material; the epoxy packaging material comprises the following components in parts by weight: 100 parts of modified epoxy resin, 0.3 part of carbon black and inorganic oxidized microbeads (the component is Na 0.1 O 0.05 ·Si 0.5 O 1.0 ·B 0.1 O 0.15 ·Zr 0.3 O 0.6 ) 550 parts of aminoethylaminopropyl trimethoxysilane, 2 parts of an antioxidant and 1 part of an auxiliary agent; the antioxidant is a combination of IRGAFOS 168 and Irganox 1010, and the mass ratio is 1:1, a step of; the auxiliary agent is 2-ethyl-4-methylimidazole.
The preparation method of the modified epoxy resin comprises the following steps: 71.5 parts of bis (7-oxabicyclo [4.1.0] 3-heptylmethyl) adipate and 28.5 parts of bisphenol A type linear epoxy resin are taken and stirred for 1h at 130 ℃; then the temperature is regulated to 60 ℃, 100 parts of phthalic anhydride, 43 parts of 1, 4-butanediol, 0.35 part of 1- [2- (trimethoxysilyl) ethyl ] -3, 4-epoxycyclohexane and 0.35 part of 3- (trimethoxysilyl) -1-propanethiol are added and stirred for 10min to be uniformly mixed.
The preparation method of the epoxy packaging material comprises the following steps: mixing modified epoxy resin, carbon black, fused silica, aminoethylaminopropyl trimethoxysilane, an antioxidant and modified epoxy resin, stirring at 120 ℃ for 40min, adding an auxiliary agent, stirring for 15min, discharging, cooling, crushing and beating.
Example 2
The embodiment provides a small-space display screen epoxy packaging material; the epoxy packaging material comprises the following components in parts by weight: 100 parts of modified epoxy resin, 0.2 part of carbon black and inorganic oxidized microbeads (the component is Na 0.1 O 0.05 ·Si 0.5 O 1.0 ·B 0.1 O 0.15 ·Zr 0.3 O 0.6 ) 400 parts of gamma-glycidyl ether oxypropyl trimethoxy silane 2 parts, an antioxidant 1 part and an auxiliary agent 2 parts; the antioxidant is Irganox 245; the auxiliary agent is diethylenetriamine.
The preparation method of the modified epoxy resin comprises the following steps: 50 parts of bis (7-oxabicyclo [4.1.0] 3-heptylmethyl) adipate and 50 parts of bisphenol A linear epoxy resin are taken and stirred for 1h at 150 ℃; then the temperature is regulated to 125 ℃, 70 parts of phthalic anhydride, 45 parts of 1, 4-butanediol, 0.67 part of 1- [2- (trimethoxysilyl) ethyl ] -3, 4-epoxycyclohexane and 1.33 parts of 3- (trimethoxysilyl) -1-propanethiol are added and stirred for 40min to be uniformly mixed.
The preparation method of the epoxy packaging material comprises the following steps: mixing modified epoxy resin, carbon black, fused silica, aminoethylaminopropyl trimethoxysilane, an antioxidant and modified epoxy resin, stirring at 140 ℃ for 20min, adding an auxiliary agent, stirring for 10min, discharging, cooling, crushing and beating.
Example 3
The embodiment provides a small-space display screen epoxy packaging material; the epoxy packaging material comprises the following components in parts by weight: 100 parts of modified epoxy resin, 0.6 part of carbon black and inorganic oxidized microbeads (the component is Na 0.1 O 0.05 ·Si 0.5 O 1.0 ·B 0.1 O 0.15 ·Zr 0.3 O 0.6 ) 850 parts of aminoethylaminopropyl trimethoxysilane, 4 parts of an antioxidant, 3 parts of an auxiliary agent and 2 parts of an auxiliary agent; the antioxidant is a combination of IRGAFOS 168 and Irganox 1010, and the mass ratio is 1:2; the auxiliary agent is 2-ethyl-4-methylimidazole.
The preparation method of the modified epoxy resin comprises the following steps: 80 parts of bis (7-oxabicyclo [4.1.0] 3-heptylmethyl) adipate and 20 parts of bisphenol A linear epoxy resin are taken according to parts by weight and stirred for 1h at 160 ℃; then, the temperature is regulated to 70 ℃, 50 parts of phthalic anhydride, 45 parts of 1, 4-butanediol, 1.6 parts of 1- [2- (trimethoxysilyl) ethyl ] -3, 4-epoxycyclohexane and 0.4 part of 3- (trimethoxysilyl) -1-propanethiol are added and stirred for 10min to be uniformly mixed.
The preparation method of the epoxy packaging material comprises the following steps: mixing modified epoxy resin, carbon black, fused silica, aminoethylaminopropyl trimethoxysilane, an antioxidant and modified epoxy resin, stirring at 80 ℃ for 20min, adding an auxiliary agent, stirring for 10min, discharging, cooling, crushing and beating.
Comparative example 1
Substantially identical to example 1, except that: the epoxy resin is bisphenol A type linear epoxy resin.
Comparative example 2
Substantially identical to example 1, except that: the raw material of the modified epoxy resin is not added with a chain extender 1, 4-butanediol.
Comparative example 3
Substantially identical to example 1, except that: the raw material of the modified epoxy resin comprises 55 parts of 1, 4-butanediol.
Comparative example 4
Substantially identical to example 1, except that: the auxiliary agent is 0.05 part.
Comparative example 5
Substantially identical to example 1, except that: the auxiliary agent is 3 parts.
Comparative example 6
Substantially identical to example 1, except that: in the preparation method of the modified epoxy resin, 1.72 parts of 1- [2- (trimethoxysilyl) ethyl ] -3, 4-epoxycyclohexane and 0.28 part of 3- (trimethoxysilyl) -1-propanethiol are adopted.
The bisphenol a linear epoxy resin was purchased from mitsubishi chemical, model JER1004; the carbon black is cabot CSX 935; the preparation method of the inorganic oxidized microbeads is shown in China patent with publication number of CN110283561B and publication date of 2021, 9 and 10 days.
The performance test method comprises the following steps:
1. the operation performance is as follows: the epoxy packaging material in the embodiment is preheated and extruded into a die cavity, the light-emitting diode chip is embedded in the die cavity, the die is cured for 300 seconds at 150 ℃, the die is cured for 4 hours at 150 ℃, the packaging condition of the material on the chip is observed, and whether the problems of poor filling, glue overflow, bubbles or punching and the like occur or not is judged, so that the operability is judged. The results were as follows: sequential evaluation of excellent > better > poor; wherein the excellent judgment criteria are: good filling, no bad problems such as glue overflow, bubbles or punching line, etc.; the better judgment standard is as follows: the filling is good, and the bad problems of obvious glue overflow, bubbles or line flushing and the like are avoided; the criterion of the difference is: the problems of obvious glue overflow, bubbles or line flushing and the like occur;
2. PCT performance evaluation: the PCT reliability performance of the packaging material was evaluated by the failure condition of the lamp beads by lighting the lamp beads after testing for 168 hours under PCT conditions (121 ℃ c. x 2atom x 100% rh), and the results were as follows: sequential evaluation of excellent > better > difference, wherein the excellent evaluation criteria are: the failure rate is 0; the better evaluation criteria are: failure rate is less than or equal to 1 percent; the evaluation criteria for the differences were: failure rate is more than 1%;
3. warp performance evaluation: packaging the epoxy packaging material on a BT resin substrate with the thickness of 0.28mm, curing for 4 hours at 150 ℃, and testing the warpage height of the substrate; the warp height is lower than 2mm, and the evaluation result is qualified; the warp height is higher than 2mm, and the evaluation result is unqualified; and observing whether the curing is complete or not, and evaluating the heat curing performance;
4. adhesion properties: carrying out a red ink experiment on a sample of the packaged LED chip after detecting the operation performance, boiling for 2 hours, and evaluating the adhesion performance of the sample; if there is a red ink leak, the determination is failed.
Performance test results:
the test results are shown in Table 1.
TABLE 1

Claims (10)

1. The epoxy packaging material for the small-space display screen is characterized by comprising the following components in parts by weight: 100 parts of modified epoxy resin, 0.001-1 part of pigment, 20-850 parts of inorganic filler, 0.01-4 parts of adhesion promoter, 1-3 parts of antioxidant and 0.1-2 parts of auxiliary agent;
the preparation raw materials of the modified epoxy resin comprise: 100 parts of epoxy resin, 20-160 parts of curing agent, 3-50 parts of chain extender and 0.05-3 parts of cross-linking agent;
the cross-linking agent is a C9-C20 ester ring compound containing Si-O bond and/or a C4-C15 chain compound containing Si-O bond.
2. The epoxy encapsulating material of claim 1 wherein the epoxy resin comprises at least one of an alicyclic epoxy resin, a biphenyl epoxy resin, a naphthalene epoxy resin, a polyphenol type glycidyl ether epoxy resin, triglycidyl isocyanurate, and diglycidyl isocyanurate.
3. The epoxy encapsulating material of claim 2 wherein the epoxy resin further comprises at least one of bisphenol a/bisphenol F/bisphenol S type linear epoxy resin, bisphenol a/bisphenol F/bisphenol S type linear phenolic epoxy resin, hydrogenated bisphenol a/bisphenol F/bisphenol S type linear epoxy resin, aliphatic glycidyl ether type epoxy resin.
4. The epoxy encapsulating material of claim 1 wherein the chain extender is a glycol or polyol.
5. The epoxy encapsulation material of claim 1, wherein the Si-O bond containing C9-C20 ester ring compound comprises one of 1- [2- (trimethoxysilyl) ethyl ] -3, 4-epoxycyclohexane, 2,4,6, 8-tetramethyl-2- [3- (oxiranylmethoxy) propyl ] cyclotetrasiloxane; the C4-C15 chain compound containing Si-O bond is at least one selected from 3- (trimethoxysilyl) -1-propanethiol, 3-triethoxysilyl-1-propylamine, 3- (trimethoxysilyl) propyl-2-methyl-2-acrylic ester and N- (beta-aminoethyl-gamma-aminopropyl) trimethoxysilane.
6. The epoxy encapsulating material according to claim 1, wherein the mass ratio of the Si-O bond-containing C9-C20 ester ring compound and the Si-O bond-containing C4-C15 chain compound is (0.5-5): 1.
7. the epoxy encapsulation material of claim 1, wherein the inorganic filler has a refractive index of 1.4 to 1.6.
8. The method of producing an epoxy encapsulating material according to any one of claims 1 to 7, characterized in that the method of producing is: mixing inorganic filler, pigment, adhesion promoter, antioxidant and modified epoxy resin, stirring at 60-140deg.C for 5-60min, adding adjuvant, stirring for 1-15min, discharging, cooling, pulverizing, and making cake.
9. Use of an epoxy encapsulation material according to any one of claims 1-8 in BT resin substrate encapsulation.
10. The use of an epoxy encapsulation material according to claim 9 for BT resin substrate encapsulation, wherein the BT resin substrate thickness is 0.28mm or less.
CN202310989864.XA 2023-08-08 2023-08-08 Epoxy packaging material for small-space display screen and preparation method and application thereof Active CN116731653B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002194119A (en) * 2000-12-22 2002-07-10 Mitsubishi Gas Chem Co Inc Prepreg and metal foil clad laminated plate
CN102558769A (en) * 2010-12-31 2012-07-11 第一毛织株式会社 Epoxy resin composition for encapsulating semiconductor device and semiconductor device encapsulated with an encapsulant prepared from the composition
CN103468095A (en) * 2013-07-23 2013-12-25 江苏博特新材料有限公司 Silane coupling agent-modified epoxy resin, and preparation method and application thereof
CN111154432A (en) * 2020-01-16 2020-05-15 北京龙苑伟业新材料有限公司 High-temperature-resistant storage sealant for bonding aluminum plate for automobile and preparation method thereof
CN112852371A (en) * 2021-01-14 2021-05-28 天津德高化成新材料股份有限公司 Small-spacing epoxy plastic packaging material applied to outdoor display screen and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002194119A (en) * 2000-12-22 2002-07-10 Mitsubishi Gas Chem Co Inc Prepreg and metal foil clad laminated plate
CN102558769A (en) * 2010-12-31 2012-07-11 第一毛织株式会社 Epoxy resin composition for encapsulating semiconductor device and semiconductor device encapsulated with an encapsulant prepared from the composition
CN103468095A (en) * 2013-07-23 2013-12-25 江苏博特新材料有限公司 Silane coupling agent-modified epoxy resin, and preparation method and application thereof
CN111154432A (en) * 2020-01-16 2020-05-15 北京龙苑伟业新材料有限公司 High-temperature-resistant storage sealant for bonding aluminum plate for automobile and preparation method thereof
CN112852371A (en) * 2021-01-14 2021-05-28 天津德高化成新材料股份有限公司 Small-spacing epoxy plastic packaging material applied to outdoor display screen and preparation method thereof

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