CN105860902A - Composite mesophase pitch-based carbon fiber filled and modified composite epoxy pouring sealant for LED display screen - Google Patents

Composite mesophase pitch-based carbon fiber filled and modified composite epoxy pouring sealant for LED display screen Download PDF

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Publication number
CN105860902A
CN105860902A CN201610402039.5A CN201610402039A CN105860902A CN 105860902 A CN105860902 A CN 105860902A CN 201610402039 A CN201610402039 A CN 201610402039A CN 105860902 A CN105860902 A CN 105860902A
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CN
China
Prior art keywords
based carbon
mesophase pitch
carbon fibers
composite
led display
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Pending
Application number
CN201610402039.5A
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Chinese (zh)
Inventor
夏云
夏建生
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BENGBU ZHENGYUAN ELECTRONIC TECHNOLOGY Co Ltd
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BENGBU ZHENGYUAN ELECTRONIC TECHNOLOGY Co Ltd
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Priority to CN201610402039.5A priority Critical patent/CN105860902A/en
Publication of CN105860902A publication Critical patent/CN105860902A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6666Compounds of group C08G18/48 or C08G18/52
    • C08G18/667Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/6681Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
    • C08G18/6688Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3271
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

Abstract

The invention discloses a composite mesophase pitch-based carbon fiber filled and modified composite epoxy pouring sealant for an LED display screen. The pouring sealant conducts surface coupling pretreatment on mesophase pitch-based carbon fibers which are good in mechanical enhancement effect and heat-conducting effect through a rare earth oxide-titanium aluminum composite coupling agent, the treated mesophase pitch-based carbon fibers and polyurethane prepolymer are subjected to hybrid reaction, and a composite filler with the comprehensive performance of inorganic matter and organic matter is obtained finally; the filler has good dispersity and associativity, the defect that a traditional nanofiller is prone to agglomeration is overcome, after the filler is composited with epoxy resin, the heat conductivity and mechanical property of the material are significantly improved, an LED chip packaged with the composite epoxy resin sealant is long in service life, and a good application prospect is shown in the aspect of high power LED display screen packaging.

Description

Filling-modified being combined of compound mesophase pitch-based carbon fibers of a kind of LED display Epoxy pouring sealant
Technical field
The present invention relates to LED casting glue technical field, particularly relate to the compound intermediate phase pitch-based carbon of a kind of LED display The composite epoxy casting glue that fiber is filling-modified.
Background technology
LED display is by assembling by light emitting diode, constitutes lattice module, thus realizes large-area display merit Can, it is widely used in daily life.LED display is progressively to more high brightness, more long-life, preferably luminescence at present Uniformity and the development of stability aspect, this requires integrated chip, high power undoubtedly, increasingly mature along with chip technology, The performance of chip can substantially meet use demand, and the requirement of encapsulation technology corresponding with this is more and more higher.It is known that encapsulation Effect directly influences serviceability and the life-span of LED chip, and the development in market proposes requirements at the higher level to encapsulation technology.
Casting glue be usually used in electronic component heat conduction, bonding, seal, embedding and coating protection etc., primarily serve protection against the tide, Dust-proof, anticorrosion, shockproof and improve effect such as stability of module.At present application more for epoxy resin casting glue, ring The oxygen class casting glue defect maximum when application is exactly that poor thermal conductivity, viscosity are big, reduces the service life of device.In order to be suitable for Market demand, necessary be modified traditional epoxy resin embedding adhesive processes, and encapsulates effect satisfactorily to obtaining Really." research of LED epoxy resin embedding adhesive " literary composition is using bisphenol A epoxide resin as material of main part, with polyurethane as increasing Tough dose, use low viscous mixing amine curing agent and epoxy active diluent, prepared that viscosity is little, light transmission good, power Learn the product of excellent performance, but this kind of modified epoxy class casting glue heat-conducting effect is poor, inadequate environmental protection;" ZnO is at Al2O3/ heat conduction ring Application study in epoxy resin embedding glue " literary composition utilize heat conduction inorganic filler epoxy resin is modified process, in certain journey Improving the thermal conductivity of epoxy resin on degree, but its mechanical property but has downward trend, viscosity becomes big.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that a kind of LED display drips by compound mesophase The composite epoxy casting glue that blue or green base carbon fibre is filling-modified.
The present invention is achieved by the following technical solutions:
The composite epoxy casting glue that a kind of LED display is filling-modified with being combined mesophase pitch-based carbon fibers, it is characterised in that This packaging plastic is prepared by the raw material of following weight portion: bisphenol A epoxide resin 40-60, the modifies mesophase of rare earth-polyurethane prepolymer Asphalt base carbon fiber 20-35, methyl-silicone oil 1-2, diluent CYH-277 5-15, polyurethanes 5-8, curing agent 20-80, Antioxidant 0.1-0.5, UV light stabilizing agent 0.01-0.05, UV absorbers 0.01-0.05.
The described modifies mesophase pitch-based carbon fibers of rare earth-polyurethane prepolymer is prepared by following raw material: polyethers Polyalcohol 10-20, methyl diphenylene diisocyanate 5-10, diethanol amine are appropriate, 800-1000 mesh intermediate phase pitch-based carbon is fine Dimension 40-50, aluminate coupling agent 1-2, titanate coupling agent 1-1.5, rare earth oxide 0.5-0.6, dibutyl tin dilaurate 0.1-0.2。
Preparation method is:
(1) putting in reaction vessel by PPG, heating removing moisture, is subsequently added diphenyl methane under nitrogen atmosphere Diisocyanate, hybrid reaction 6-8h under the conditions of 80-90 DEG C.
(2) aluminate coupling agent, titanate coupling agent, rare earth oxide are added in reaction vessel together, stirring mixing Being heated to 120-130 DEG C after Jun Yun, hybrid reaction 4-5h, products therefrom mixes dispersion and grinds 2-with mesophase pitch-based carbon fibers 3h, is put in step (1) reaction vessel subsequently, and reduction system temperature, to 60-70 DEG C, adds dibutyl tin dilaurate, Drip diethanol amine after mixed grinding reaction 2-3h, continue cooling discharge after griding reaction 1-1.5h, obtain described rare earth-poly- Urethane performed polymer modification mesophase pitch-based carbon fibers.
Described curing agent is the one in methyl hexahydrophthalic anhydride, methyl tetrahydro phthalic anhydride.
The using method of this casting glue is: first by bisphenol A epoxide resin, the drip of rare earth-polyurethane prepolymer modifies mesophase Blue or green base carbon fibre, methyl-silicone oil, polyurethanes, diluent, antioxidant, UV light stabilizing agent, UV absorbers mixing Stirring, add curing agent subsequently, stirring while adding, after interpolation, mixed material is heated to 60-80 DEG C, gained glue Inject in LED die to be packaged after vacuum defoamation processes, after natural precuring 4-5h, take out pre-packaged LED, be placed in true In empty drying box, it is heated to 90-105 DEG C, after isothermal curing 4-5h, i.e. obtains the LED that embedding is good.
Good mechanics is strengthened the mesophase pitch-based carbon fibers of effect and heat-conducting effect through rare earth oxide-titanium by the present invention Aluminium composite coupler surface coupling pretreatment, then by itself and base polyurethane prepolymer for use as hybrid reaction, finally give have concurrently inorganic matter with The compounded mix of organic matter combination property, it has good dispersiveness and associativity, and improve that conventional filler easily reunites lacks Fall into, thermal conductivity and the mechanical property with epoxy resin significantly improves material after compounding, encapsulate with this composite epoxy resin glue LED chip long for service life, in terms of high-power LED display screen encapsulation, demonstrate good application prospect.
Detailed description of the invention
The casting glue of this embodiment is prepared by the raw material of following weight portion: bisphenol A epoxide resin 50, rare earth-polyurethane are pre- Aggressiveness modification mesophase pitch-based carbon fibers 25, methyl-silicone oil 1.5, diluent CYH-277 10, polyurethanes 6, methyl HHPA 50, antioxidant 0.2, UV light stabilizing agent 0.02, UV absorbers 0.03.
Its modifies mesophase pitch-based carbon fibers of middle rare earth-polyurethane prepolymer is prepared by following raw material: polyethers is many Unit's alcohol 15, methyl diphenylene diisocyanate 8, diethanol amine are appropriate, 1000 mesh mesophase pitch-based carbon fibers 45, Aluminate are even Connection agent 1.5, titanate coupling agent 1.2, rare earth oxide 0.5, dibutyl tin dilaurate 0.1.
Preparation method is:
(1) putting in reaction vessel by PPG, heating removing moisture, is subsequently added diphenyl methane under nitrogen atmosphere Diisocyanate, hybrid reaction 6.5h under the conditions of 80-90 DEG C.
(2) aluminate coupling agent, titanate coupling agent, rare earth oxide are added in reaction vessel together, stirring mixing Being heated to 120-130 DEG C after Jun Yun, hybrid reaction 4.5h, products therefrom mixes dispersion and grinds with mesophase pitch-based carbon fibers 2.5h, is put in step (1) reaction vessel subsequently, and reduction system temperature, to 60-70 DEG C, adds dibutyl tin cinnamic acid Tin, drips diethanol amine after mixed grinding reaction 2.5h, continues cooling discharge after griding reaction 1.2h, obtain described rare earth- The modifies mesophase pitch-based carbon fibers of polyurethane prepolymer.
The using method of this casting glue is: first by bisphenol A epoxide resin, the drip of rare earth-polyurethane prepolymer modifies mesophase Blue or green base carbon fibre, methyl-silicone oil, polyurethanes, diluent, antioxidant, UV light stabilizing agent, UV absorbers mixing Stirring, add curing agent subsequently, stirring while adding, after interpolation, mixed material is heated to 70-80 DEG C, gained glue Inject in LED die to be packaged after vacuum defoamation processes, after natural precuring 4.5h, take out pre-packaged LED, be placed in true In empty drying box, it is heated to 90-100 DEG C, after isothermal curing 4.5h, i.e. obtains the LED that embedding is good.
The performance test results of this casting glue is as follows:
Detection project Testing result
Thermal conductivity (W.m-1.k-1) 0.87
Elongation at break (%) 62.5
Hot strength (MPa) 23.6
Thermal coefficient of expansion 0.26
Water absorption rate 0.10

Claims (4)

1. the composite epoxy casting glue that LED display is filling-modified with being combined mesophase pitch-based carbon fibers, its feature exists In, this packaging plastic is prepared by the raw material of following weight portion: during bisphenol A epoxide resin 40-60, rare earth-polyurethane prepolymer are modifies Between asphalt phase base carbon fibre 20-35, methyl-silicone oil 1-2, diluent CYH-277 5-15, polyurethanes 5-8, curing agent 20-80, antioxidant 0.1-0.5, UV light stabilizing agent 0.01-0.05, UV absorbers 0.01-0.05.
The complex loop that a kind of LED display the most as claimed in claim 1 is filling-modified with being combined mesophase pitch-based carbon fibers Oxygen casting glue, it is characterised in that the described modifies mesophase pitch-based carbon fibers of rare earth-polyurethane prepolymer is by following raw material system For obtaining: PPG 10-20, methyl diphenylene diisocyanate 5-10, diethanol amine are appropriate, 800-1000 mesh mesophase Asphalt base carbon fiber 40-50, aluminate coupling agent 1-2, titanate coupling agent 1-1.5, rare earth oxide 0.5-0.6, dibutyl Tin dilaurate tin 0.1-0.2;
Preparation method is:
(1) putting in reaction vessel by PPG, heating removing moisture, is subsequently added diphenyl methane under nitrogen atmosphere Diisocyanate, hybrid reaction 6-8h under the conditions of 80-90 DEG C;
(2) aluminate coupling agent, titanate coupling agent, rare earth oxide are added in reaction vessel together, be uniformly mixed After be heated to 120-130 DEG C, hybrid reaction 4-5h, products therefrom mix with mesophase pitch-based carbon fibers dispersion grind 2-3h, Being put in step (1) reaction vessel subsequently, reduction system temperature, to 60-70 DEG C, adds dibutyl tin dilaurate, mixing Drip diethanol amine after griding reaction 2-3h, continue cooling discharge after griding reaction 1-1.5h, obtain described rare earth-polyurethane Performed polymer modification mesophase pitch-based carbon fibers.
The complex loop that a kind of LED display the most as claimed in claim 1 is filling-modified with being combined mesophase pitch-based carbon fibers Oxygen casting glue, it is characterised in that described curing agent is the one in methyl hexahydrophthalic anhydride, methyl tetrahydro phthalic anhydride.
The complex loop that a kind of LED display the most as claimed in claim 1 is filling-modified with being combined mesophase pitch-based carbon fibers The using method of oxygen casting glue is: first by bisphenol A epoxide resin, rare earth-polyurethane prepolymer modifies intermediate phase pitch-based carbon fibre Dimension, methyl-silicone oil, polyurethanes, diluent, antioxidant, UV light stabilizing agent, UV absorbers mixing and stirring, Adding curing agent subsequently, stirring while adding, after interpolation, mixed material is heated to 60-80 DEG C, and gained glue takes off through vacuum Bubble injects in LED die to be packaged after processing, and takes out pre-packaged LED, be placed in vacuum drying chamber after natural precuring 4-5h In, it is heated to 90-105 DEG C, after isothermal curing 4-5h, i.e. obtains the LED that embedding is good.
CN201610402039.5A 2016-06-08 2016-06-08 Composite mesophase pitch-based carbon fiber filled and modified composite epoxy pouring sealant for LED display screen Pending CN105860902A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610402039.5A CN105860902A (en) 2016-06-08 2016-06-08 Composite mesophase pitch-based carbon fiber filled and modified composite epoxy pouring sealant for LED display screen

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Application Number Priority Date Filing Date Title
CN201610402039.5A CN105860902A (en) 2016-06-08 2016-06-08 Composite mesophase pitch-based carbon fiber filled and modified composite epoxy pouring sealant for LED display screen

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101495585A (en) * 2006-07-28 2009-07-29 帝人株式会社 Heat conductive adhesive

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101495585A (en) * 2006-07-28 2009-07-29 帝人株式会社 Heat conductive adhesive

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Application publication date: 20160817