CN105950091A - Epoxy resin pouring sealant modified by composite silicon nitride thermal conductive filler and used for LED display screen - Google Patents
Epoxy resin pouring sealant modified by composite silicon nitride thermal conductive filler and used for LED display screen Download PDFInfo
- Publication number
- CN105950091A CN105950091A CN201610402038.0A CN201610402038A CN105950091A CN 105950091 A CN105950091 A CN 105950091A CN 201610402038 A CN201610402038 A CN 201610402038A CN 105950091 A CN105950091 A CN 105950091A
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- China
- Prior art keywords
- silicon nitride
- pouring sealant
- led display
- rare earth
- epoxy resin
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6681—Compounds 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
- C08G18/6688—Compounds 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
-
- 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
- C09J11/08—Macromolecular additives
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses epoxy resin pouring sealant modified by composite silicon nitride thermal conductive filler and used for an LED display screen. According to the epoxy resin pouring sealant, high-thermal-conductivity nanometer silicon carbide is subjected to surface coupling pretreatment with a rare earth oxide-titanium aluminum composite coupling agent, then a product is subjected to a mixed reaction with polyurethane prepolymer, and finally the composite thermal conductive filler with comprehensive performance of both organic matter and inorganic matter is obtained. The composite thermal conductive filler has good dispersity and combination performance, the compounding effect with epoxy resin is good, composite performance of the material is effectively improved, the prepared pouring sealant is good in packaging and protection effect, the service life of a chip is greatly prolonged, and good application prospect is displayed on the aspect of packaging of the large-power LED display screen.
Description
Technical field
The present invention relates to LED casting glue technical field, particularly relate to a kind of LED display composite silicon nitride heat filling
Modified epoxy pouring sealant.
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
Applied research in epoxy resin embedding glue " literary composition utilize heat conduction inorganic filler epoxy resin is modified process, in certain journey
Improving the heat 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 composite silicon nitride is led
The epoxy pouring sealant that heat is filler modified.
The present invention is achieved by the following technical solutions:
The epoxy pouring sealant that a kind of LED display composite silicon nitride heat filling is modified, it is characterised in that this packaging plastic by with
The raw material of lower weight portion prepares: bisphenol A epoxide resin 40-50, PEEK polymer 8-12, the modifies nitrogen of rare earth-polyurethane prepolymer
SiClx 30-50, acetylene carbon black 1-2, diluent CYH-277 5-15, firming agent 20-80, antioxidant 0.1-0.5, ultraviolet light stabilized
Agent 0.01-0.05, UV absorbers 0.01-0.05.
The described modifies silicon nitride of rare earth-polyurethane prepolymer is prepared by following raw material: polyether polyol 10-20,
Methyl diphenylene diisocyanate 5-10, diethanolamine are appropriate, 600-800 mesh silicon nitride 40-50, aluminate coupling agent 1-2, titanium
Acid esters 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 polyether polyol, 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
Uniformly post-heating is to 120-130 DEG C, hybrid reaction 4-5h, and products therefrom mixes dispersion and grinds 2-3h, subsequently by it with silicon nitride
Putting in step (1) reaction vessel, reduction system temperature, to 60-70 DEG C, adds dibutyl tin dilaurate, and mixed grinding reacts
Drip diethanolamine after 2-3h, continue cooling discharge after griding reaction 1-1.5h, obtain described rare earth-polyurethane prepolymer structural reform
Property silicon nitride.
Described firming 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, PEEK polymer, rare earth-polyurethane prepolymer structural reform
Property silicon nitride, acetylene carbon black, diluent, antioxidant, UV light stabilizing agent, UV absorbers mixing and stirring, the most again
Adding firming agent, stirring while adding, after interpolation, mixed material is heated to 60-80 DEG C, and gained glue processes through vacuum defoamation
In the LED die that rear injection is to be packaged, take out pre-packaged LED after natural precuring 4-5h, be placed in vacuum drying oven, heating
To 100-120 DEG C, after isothermal curing 4-5h, i.e. obtain the LED that embedding is good.
The present invention by silicon nitride filler through rare earth oxide-titanium aluminum composite coupler surface coupling pretreatment, then by its with
Base polyurethane prepolymer for use as hybrid reaction, finally gives the compounded mix having inorganic matter concurrently with Organic substance combination property, improves tradition
The defect that Nano filling is easily reunited, after it is compounding with resinite can the combination property that improve resin of uniform high-efficiency, preparation
Having high package strength and corrosion resistance after glue curing, its excellent heat-conducting effect ensure that the normal work of prolonged periods
Make, 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 45, PEEK polymer 10,
The modifies silicon nitride of rare earth-polyurethane prepolymer 40, acetylene carbon black 1.5, diluent CYH-277 10, methyl hexahydrophthalic anhydride 60, anti-
Oxygen agent 0.2, UV light stabilizing agent 0.02, UV absorbers 0.02.
Its modifies silicon nitride of middle rare earth-polyurethane prepolymer is prepared by following raw material: polyether polyol 15, diphenyl
Methane diisocyanate 8, diethanolamine are appropriate, 800 mesh silicon nitrides 45, aluminate coupling agent 1.5, titanate coupling agent 1.2, dilute
Soil oxide 0.5, dibutyl tin dilaurate 0.1.
Preparation method is:
(1) putting in reaction vessel by polyether polyol, heating removing moisture, is subsequently added diphenyl methane under nitrogen atmosphere
Diisocyanate, hybrid reaction 7h 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
Uniformly post-heating is to 120-130 DEG C, hybrid reaction 4.5h, and products therefrom mixes dispersion and grinds 2.5h, subsequently by it with silicon nitride
Putting in step (1) reaction vessel, reduction system temperature, to 60-70 DEG C, adds dibutyl tin dilaurate, and mixed grinding reacts
Drip diethanolamine after 2.5h, continue cooling discharge after griding reaction 1h, obtain the described modifies nitrogen of rare earth-polyurethane prepolymer
SiClx.
The using method of this casting glue is: first by bisphenol A epoxide resin, PEEK polymer, rare earth-polyurethane prepolymer structural reform
Property silicon nitride, acetylene carbon black, diluent, antioxidant, UV light stabilizing agent, UV absorbers mixing and stirring, the most again
Adding firming agent, stirring while adding, after interpolation, mixed material is heated to 70-80 DEG C, and gained glue processes through vacuum defoamation
In the LED die that rear injection is to be packaged, take out pre-packaged LED after natural precuring 4.5h, be placed in vacuum drying oven, heating
To 110-120 DEG C, after isothermal curing 4.5h, i.e. obtain 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) | 0.72 |
| Elongation at break (%) | 34.3 |
| Hot strength (MPa) | 11.5 |
| Thermal coefficient of expansion | 0.52 |
| Water absorption rate | 0.11 |
Claims (4)
1. a LED display modified epoxy pouring sealant of composite silicon nitride heat filling, it is characterised in that this packaging plastic by
The raw material of following weight portion prepares: bisphenol A epoxide resin 40-50, PEEK polymer 8-12, rare earth-polyurethane prepolymer are modifies
Silicon nitride 30-50, acetylene carbon black 1-2, diluent CYH-277 5-15, firming agent 20-80, antioxidant 0.1-0.5, ultraviolet light are steady
Determine agent 0.01-0.05, UV absorbers 0.01-0.05.
The epoxy pouring sealant that a kind of LED display composite silicon nitride heat filling the most as claimed in claim 1 is modified, it is special
Levying and be, the described modifies silicon nitride of rare earth-polyurethane prepolymer is prepared by following raw material: polyether polyol 10-20, two
Methylenebis phenyl isocyanate 5-10, diethanolamine are appropriate, 600-800 mesh silicon nitride 40-50, aluminate coupling agent 1-2, metatitanic acid
Ester 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 polyether polyol, 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
Post-heating is to 120-130 DEG C, and hybrid reaction 4-5h, products therefrom mixes dispersion and grinds 2-3h, put into subsequently with silicon nitride
In step (1) reaction vessel, reduction system temperature, to 60-70 DEG C, adds dibutyl tin dilaurate, mixed grinding reaction 2-3h
Rear dropping diethanolamine, continues cooling discharge after griding reaction 1-1.5h, obtains the described modifies nitrogen of rare earth-polyurethane prepolymer
SiClx.
The epoxy pouring sealant that a kind of LED display composite silicon nitride heat filling the most as claimed in claim 1 is modified, it is special
Levying and be, described firming agent is the one in methyl hexahydrophthalic anhydride, methyl tetrahydro phthalic anhydride.
Making of the epoxy pouring sealant that a kind of LED display composite silicon nitride heat filling the most as claimed in claim 1 is modified
By method it is: first by bisphenol A epoxide resin, PEEK polymer, the modifies silicon nitride of rare earth-polyurethane prepolymer, acetylene carbon black, dilute
Releasing agent, antioxidant, UV light stabilizing agent, UV absorbers mixing and stirring, add firming agent subsequently, limit edged stirs
Mixing, after interpolation, mixed material is heated to 60-80 DEG C, and gained glue injects LED mould to be packaged after vacuum defoamation processes
In tool, taking out pre-packaged LED, be placed in vacuum drying oven, be heated to 100-120 DEG C after natural precuring 4-5h, constant temperature is solid
I.e. obtain, after changing 4-5h, the LED that embedding is good.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610402038.0A CN105950091A (en) | 2016-06-08 | 2016-06-08 | Epoxy resin pouring sealant modified by composite silicon nitride thermal conductive filler and used for LED display screen |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610402038.0A CN105950091A (en) | 2016-06-08 | 2016-06-08 | Epoxy resin pouring sealant modified by composite silicon nitride thermal conductive filler and used for LED display screen |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105950091A true CN105950091A (en) | 2016-09-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610402038.0A Pending CN105950091A (en) | 2016-06-08 | 2016-06-08 | Epoxy resin pouring sealant modified by composite silicon nitride thermal conductive filler and used for LED display screen |
Country Status (1)
| Country | Link |
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| CN (1) | CN105950091A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107573679A (en) * | 2017-08-16 | 2018-01-12 | 芜湖晶鑫光电照明有限公司 | A kind of luminous substrate material of LED |
| CN111739990A (en) * | 2020-05-20 | 2020-10-02 | 天津中环电子照明科技有限公司 | Ultraviolet LED packaging method and ultraviolet LED packaging |
| CN115632002A (en) * | 2022-12-22 | 2023-01-20 | 天津德高化成新材料股份有限公司 | Packaging method of low-warpage mini LED display screen and display screen |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101580686A (en) * | 2009-05-07 | 2009-11-18 | 中国工程物理研究院化工材料研究所 | Low-density high-impact-resistance epoxy resin pouring sealant and preparation method thereof |
| CN104178076A (en) * | 2014-09-11 | 2014-12-03 | 黎明化工研究设计院有限责任公司 | Heat-conducting electric-insulating epoxy resin potting adhesive and preparation method thereof |
-
2016
- 2016-06-08 CN CN201610402038.0A patent/CN105950091A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101580686A (en) * | 2009-05-07 | 2009-11-18 | 中国工程物理研究院化工材料研究所 | Low-density high-impact-resistance epoxy resin pouring sealant and preparation method thereof |
| CN104178076A (en) * | 2014-09-11 | 2014-12-03 | 黎明化工研究设计院有限责任公司 | Heat-conducting electric-insulating epoxy resin potting adhesive and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107573679A (en) * | 2017-08-16 | 2018-01-12 | 芜湖晶鑫光电照明有限公司 | A kind of luminous substrate material of LED |
| CN111739990A (en) * | 2020-05-20 | 2020-10-02 | 天津中环电子照明科技有限公司 | Ultraviolet LED packaging method and ultraviolet LED packaging |
| CN115632002A (en) * | 2022-12-22 | 2023-01-20 | 天津德高化成新材料股份有限公司 | Packaging method of low-warpage mini LED display screen and display screen |
| CN115632002B (en) * | 2022-12-22 | 2023-04-21 | 天津德高化成新材料股份有限公司 | Packaging method of low-warpage mini LED display screen and display screen |
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Application publication date: 20160921 |