CN105907349A - Nanometer zirconium oxide modified composite epoxy pouring sealant for LED display screen - Google Patents

Nanometer zirconium oxide modified composite epoxy pouring sealant for LED display screen Download PDF

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Publication number
CN105907349A
CN105907349A CN201610402064.3A CN201610402064A CN105907349A CN 105907349 A CN105907349 A CN 105907349A CN 201610402064 A CN201610402064 A CN 201610402064A CN 105907349 A CN105907349 A CN 105907349A
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China
Prior art keywords
zirconium oxide
led display
nano
led
composite epoxy
Prior art date
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.)
Pending
Application number
CN201610402064.3A
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Chinese (zh)
Inventor
肖宪书
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Bengbu Gaohua Resolution Technology Co Ltd
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Bengbu Gaohua Resolution Technology Co Ltd
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Priority to CN201610402064.3A priority Critical patent/CN105907349A/en
Publication of CN105907349A publication Critical patent/CN105907349A/en
Pending legal-status Critical Current

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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
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • 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
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2244—Oxides; Hydroxides of metals of zirconium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured 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)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Led Device Packages (AREA)

Abstract

The invention discloses a nanometer zirconium oxide modified composite epoxy pouring sealant for an LED display screen. According to the pouring sealant, nanometer zirconium oxide heat conductivity filler is subjected to surface coupling processing through a silane coupling agent, then the nanometer zirconium oxide heat conductivity filler and the silane coupling agent are subjected to mixing reaction, the obtained modified filler has performance of inorganic matter and organic matter and has good dispersity and combinability, the heat conductivity of the material is greatly improved after the modified filler is compounded with epoxy resin, the mechanical performance of epoxy resin adhesive is improved, an LED chip packaged by the pouring sealant is longer in service life and higher in light-emitting efficiency, and good application prospects are shown on the aspect of packaging of the LED display screen.

Description

A kind of LED display composite epoxy casting glue of nano oxidized modified zirconia
Technical field
The present invention relates to LED casting glue technical field, particularly relate to a kind of LED display answering with nano oxidized modified zirconia Close 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 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 nano zircite changes The composite epoxy casting glue of property.
The present invention is achieved by the following technical solutions:
A kind of LED display composite epoxy casting glue of nano oxidized modified zirconia, it is characterised in that this packaging plastic is by following heavy The raw material of amount part prepares: bisphenol A epoxide resin 40-60, silicon-based polyurethane performed polymer modified Nano zirconium oxide 20-40, diluent CYH-277 5-15, Lauryl Alcohol ester 1-2, curing agent 20-80, antioxidant 0.1-0.5, UV light stabilizing agent 0.01-0.05, purple Outer light absorber 0.01-0.05.
Described silicon-based polyurethane performed polymer modified Nano zirconium oxide is prepared by following raw material: PPG 10- 20, methyl diphenylene diisocyanate 5-10, diethanol amine be appropriate, nano zircite 40-50, silane coupler 2-3, 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) nano zircite is disperseed 1-1.5h with silane coupler mixed grinding, put into step (1) reaction subsequently In container, reduction system temperature, to 60-70 DEG C, adds dibutyl tin dilaurate, drips diethyl after mixed grinding reaction 2-3h Hydramine, continues cooling discharge after griding reaction 1-1.5h, obtains described silicon-based polyurethane performed polymer modified Nano zirconium oxide.
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 oxidation of silicon-based polyurethane performed polymer modified Nano Zirconium, Lauryl Alcohol ester, diluent, antioxidant, UV light stabilizing agent, UV absorbers mixing and stirring, add subsequently Curing agent, stirring while adding, after interpolation, mixed material is heated to 60-80 DEG C, and gained glue is noted after vacuum defoamation processes Enter in LED die to be packaged, take out pre-packaged LED after natural precuring 2-3h, be placed in vacuum drying chamber, be heated to 120-130 DEG C, after isothermal curing 3-4h, i.e. obtain the LED that embedding is good.
Nano zircite heat filling is first passed through silane coupler surface coupling processing by the present invention, then with polyurethane prepolymer Body hybrid reaction, the modified filler obtained has inorganic matter and organic performance concurrently, has good dispersiveness and associativity, with Drastically increase the heat conductivility of material after epoxy resin is compounding, improve the mechanical property of epoxide-resin glue, encapsulate with it LED chip longer for service life, light extraction efficiency is higher, demonstrates good application prospect in terms of LED display encapsulation.
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, silicon-based polyurethane pre-polymerization Modifies nano zircite 30, diluent CYH-277 10, Lauryl Alcohol ester 1.5, methyl hexahydrophthalic anhydride 50, antioxidant 0.2, purple Outer light stabilizer 0.02, UV absorbers 0.03.
Wherein silicon-based polyurethane performed polymer modified Nano zirconium oxide is prepared by following raw material: PPG 15, two Methylenebis phenyl isocyanate 8, diethanol amine are appropriate, nano zircite 45, silane coupler 2.5, 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 7.5h under the conditions of 80-90 DEG C.
(2) nano zircite is disperseed 1.2h with silane coupler mixed grinding, put into step (1) reaction subsequently and hold In device, reduction system temperature, to 60-70 DEG C, adds dibutyl tin dilaurate, drips diethanol after mixed grinding reaction 2.5h Amine, continues cooling discharge after griding reaction 1.5h, obtains described silicon-based polyurethane performed polymer modified Nano zirconium oxide.
The using method of this casting glue is: first by bisphenol A epoxide resin, the oxidation of silicon-based polyurethane performed polymer modified Nano Zirconium, Lauryl Alcohol ester, diluent, antioxidant, UV light stabilizing agent, UV absorbers mixing and stirring, add subsequently Curing agent, stirring while adding, after interpolation, mixed material is heated to 60-80 DEG C, and gained glue is noted after vacuum defoamation processes Enter in LED die to be packaged, take out pre-packaged LED after natural precuring 2.5h, be placed in vacuum drying chamber, be heated to 120 DEG C, after isothermal curing 3.5h, 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) 0.54
Elongation at break (%) 21.6
Hot strength (MPa) 12.3
Thermal coefficient of expansion 0.40
Water absorption rate 0.16

Claims (4)

1. the LED display composite epoxy casting glue of nano oxidized modified zirconia, it is characterised in that this packaging plastic is by following The raw material of weight portion prepares: bisphenol A epoxide resin 40-60, silicon-based polyurethane performed polymer modified Nano zirconium oxide 20-40, dilution Agent CYH-277 5-15, Lauryl Alcohol ester 1-2, curing agent 20-80, antioxidant 0.1-0.5, UV light stabilizing agent 0.01-0.05, UV absorbers 0.01-0.05.
A kind of LED display the most as claimed in claim 1 composite epoxy casting glue of nano oxidized modified zirconia, its feature exists In, described silicon-based polyurethane performed polymer modified Nano zirconium oxide is prepared by following raw material: PPG 10-20, two Methylenebis phenyl isocyanate 5-10, diethanol amine are appropriate, nano zircite 40-50, silane coupler 2-3, dibutyl tin Cinnamic acid 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) nano zircite is disperseed 1-1.5h with silane coupler mixed grinding, put into step (1) reaction vessel subsequently In, reduction system temperature, to 60-70 DEG C, adds dibutyl tin dilaurate, drips diethanol amine after mixed grinding reaction 2-3h, Continue cooling discharge after griding reaction 1-1.5h, obtain described silicon-based polyurethane performed polymer modified Nano zirconium oxide.
A kind of LED display the most as claimed in claim 1 composite epoxy casting glue of nano oxidized modified zirconia, its feature exists In, described curing agent is the one in methyl hexahydrophthalic anhydride, methyl tetrahydro phthalic anhydride.
A kind of LED display the most as claimed in claim 1 is with the user of the composite epoxy casting glue of nano oxidized modified zirconia Method is: first by bisphenol A epoxide resin, silicon-based polyurethane performed polymer modified Nano zirconium oxide, Lauryl Alcohol ester, diluent, antioxygen Agent, UV light stabilizing agent, UV absorbers mixing and stirring, add curing agent subsequently, stirring while adding, adds complete Rear mixed material is heated to 60-80 DEG C, and gained glue injects in LED die to be packaged after vacuum defoamation processes, naturally pre- Take out pre-packaged LED after solidification 2-3h, be placed in vacuum drying chamber, be heated to 120-130 DEG C, after isothermal curing 3-4h and get final product The LED that embedding is good.
CN201610402064.3A 2016-06-08 2016-06-08 Nanometer zirconium oxide modified composite epoxy pouring sealant for LED display screen Pending CN105907349A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107325768A (en) * 2017-05-19 2017-11-07 合肥市惠科精密模具有限公司 A kind of composite epoxy casting glue of LED display nano-silicon nitride toughening modifying

Citations (4)

* Cited by examiner, † Cited by third party
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 Epoxide resin pouring sealant with low density and high impact resistance and preparation method thereof
CN101847684A (en) * 2010-04-06 2010-09-29 南昌大学 Packaged circuit board with enhanced heat dissipation effect and manufacturing method thereof
CN102660212A (en) * 2012-06-08 2012-09-12 焦作市卓立烫印材料有限公司 Single-component epoxy heat-conducting adhesive
CN104178048A (en) * 2014-09-01 2014-12-03 络派模切（北京）有限公司 Ultrathin heat-conducting adhesive tape

Patent Citations (4)

* Cited by examiner, † Cited by third party
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 Epoxide resin pouring sealant with low density and high impact resistance and preparation method thereof
CN101847684A (en) * 2010-04-06 2010-09-29 南昌大学 Packaged circuit board with enhanced heat dissipation effect and manufacturing method thereof
CN102660212A (en) * 2012-06-08 2012-09-12 焦作市卓立烫印材料有限公司 Single-component epoxy heat-conducting adhesive
CN104178048A (en) * 2014-09-01 2014-12-03 络派模切（北京）有限公司 Ultrathin heat-conducting adhesive tape

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107325768A (en) * 2017-05-19 2017-11-07 合肥市惠科精密模具有限公司 A kind of composite epoxy casting glue of LED display nano-silicon nitride toughening modifying

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Application publication date: 20160831