CN106281098A - A kind of preparation technology of the good conducting resinl of LED curable - Google Patents

A kind of preparation technology of the good conducting resinl of LED curable Download PDF

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Publication number
CN106281098A
CN106281098A CN201610654901.1A CN201610654901A CN106281098A CN 106281098 A CN106281098 A CN 106281098A CN 201610654901 A CN201610654901 A CN 201610654901A CN 106281098 A CN106281098 A CN 106281098A
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CN
China
Prior art keywords
conducting resinl
preparation
parts
led curable
powder
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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.)
Pending
Application number
CN201610654901.1A
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Chinese (zh)
Inventor
陈加根
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Wave Island Anhui Recreation Facility Co Ltd
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Wave Island Anhui Recreation Facility Co Ltd
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Priority to CN201610654901.1A priority Critical patent/CN106281098A/en
Publication of CN106281098A publication Critical patent/CN106281098A/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
    • C09J9/00Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02Electrically-conducting adhesives
    • 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
    • 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
    • C09J11/06Non-macromolecular additives organic
    • 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
    • C09J11/08Macromolecular additives
    • 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
    • C09J133/00Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/001Conductive additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • 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

Abstract

The present invention relates to the preparation technology of the good conducting resinl of a kind of LED curable, preparation process is as follows: the 1) preparation of alloyed powder, weighs nanometer silver powder, bismuth oxide, nano zine oxide, nikel powder, MTES, graphite;By each raw material by proportioning at 1500 DEG C~1650 DEG C, less than 10‑3The vacuum of torr is smelted into homogeneous alloy solution, and the gas low by activity prepares alloyed powder with the pressure peening of 20~30atm with moment atomization;2) preparation of conducting resinl, based on weight/mass percentage composition, by acrylic resin, phenolic resin, triphenyl phosphite, polymerization inhibitor, firming agent, stirs, is slowly added to alloyed powder, stir, froth in vacuum, prepares the good conducting resinl of described LED curable.Alloyed powder in conducting resinl formula of the present invention has preferable dispersion stabilization, and prepared conducting resinl resistivity is low, thermal conductivity is high, adhesive property is good, curing rate is fast, service life is long.

Description

A kind of preparation technology of the good conducting resinl of LED curable
Technical field
The invention belongs to technical field of electronic materials, be specifically related to the preparation technology of a kind of good conducting resinl of LED curable.
Background technology
LED conducting resinl, is the connection for LED chip and base material, it is possible to realize the function of heat conduction and conduction simultaneously.Lead Electric adhesive is also referred to as conducting resinl, is the solidification at a certain temperature being made up of matrix resin, firming agent and conductive filler or dry After dry can adhesive base plate material effectively, can have again the special adhesive of electric conductivity.Conducting resinl can be divided by matrix composition For structural type and the big class of filled-type two.Structural type refers to that the macromolecular material as conducting resinl matrix itself i.e. has electric conductivity Conducting resinl;Filled-type refer to usual adhesive as matrix, and rely on interpolation electroconductive stuffing make glue have electric action Conducting resinl.The preparation of conducting polymer composite at present also has bigger distance from reality application, and the most widely used being is filled out Fill type conducting resinl.As epoxy resin adhesive can solidify in room temperature to 150 DEG C, far below more than 200 DEG C of tin-lead welding Welding temperature, avoiding problems material deformation, the hot injury of electronic device and the formation of internal stress that welding high temperature may cause. Simultaneously as the developing rapidly of the densification of the miniaturization of electronic component, miniaturization and printed circuit board (PCB) and Highgrade integration, The minimum pitch of the 0.65mm of slicker solder welding can not meet far away the actual demand being conductively connected, and conducting resinl can make slurry Material, it is achieved the highest linear resolution.
The developing direction of LED industry is to develop towards the high-power direction of high brightness, super brightness, thus proposes conducting resinl Higher requirement, the great power LED thermal diffusivity to conducting resinl, traditional heat-conducting glue thermal conductivity is less than 10W/m K, and highlighted The cooling requirements of degree high-power LED chip is higher than 20W/m K;Develop suitable curing system, make the conducting resinl can be the longest Time stores, it is to avoid high cost of transportation and storage cost;The stability of contact resistance and the reliability of electric property.Cause How this, develop the LED conducting resinl that resistivity is low, thermal conductivity is high, curable is good, adhesive property is good the most urgent.
Summary of the invention
It is an object of the invention to provide the preparation technology of the good conducting resinl of a kind of LED curable, effectively solve high-power Thermal diffusivity problem after LED chip long-term work.
The technical scheme realizing the purpose of the present invention is: the preparation technology of the good conducting resinl of a kind of LED curable, preparation step Rapid as follows:
1) preparation of alloyed powder
Weigh nanometer silver powder 80~100 parts, bismuth oxide 8~15 parts, zinc oxide 20~30 parts, nikel powder 40~50 parts, MTES 10~15 parts, graphite 6~10 parts;By each raw material by proportioning at 1500 DEG C~1650 DEG C, less than 10- 3The vacuum of torr is smelted into homogeneous alloy solution, and the gas low by activity is atomized with moment with the pressure peening of 20~30atm And prepare alloyed powder;
2) preparation of conducting resinl
Based on weight/mass percentage composition, by acrylic resin 10%~15%, phenolic resin 2%~5%, triphenyl phosphite 4%~6%, polymerization inhibitor 0.3%~0.7%, firming agent 3%~8%, stir, be slowly added to step 1) obtained by conjunction Bronze 65%~75%, stirs, froth in vacuum, prepares the good conducting resinl of described LED curable.
Preferably, firming agent of the present invention is THPA, methyl tetrahydro phthalic anhydride, HHPA, methyl hexahydrobenzene One or more mixture in acid anhydride, methylnadic anhydride, dodecyl maleic anhydride.
Preferably, polymerization inhibitor of the present invention be hydroquinone, MEHQ, 2,6-di-t-butyl-4-methyl One or more mixture in phenol.
Preferably, step 1 of the present invention) gas that the activity that uses is low is selected from argon or nitrogen.
The technological merit of the present invention is: the alloyed powder in conducting resinl formula of the present invention has preferable dispersion stabilization, The conducting resinl resistivity prepared is low, thermal conductivity is high, adhesive property is good, curing rate is fast, service life is long.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.
A kind of preparation technology of the good conducting resinl of LED curable, preparation process is as follows:
Embodiment 1:
1) preparation of alloyed powder
Weigh nanometer silver powder 80 parts, bismuth oxide 8 parts, zinc oxide 20 parts, nikel powder 40 parts, MTES 10 Part, 6 parts of graphite;By each raw material by proportioning at 1500 DEG C~1650 DEG C, less than 10-3It is molten that the vacuum of torr is smelted into homogeneous alloy Liquid, the gas low by activity prepares alloyed powder with the pressure peening of 20~30atm with moment atomization;
2) preparation of conducting resinl
Based on weight/mass percentage composition, by acrylic resin 10%, phenolic resin 2%, triphenyl phosphite 4%, polymerization inhibitor 0.3%, firming agent 3%, stirs, and is slowly added to step 1) obtained by alloyed powder 65%, stir, froth in vacuum, Prepare the good conducting resinl of described LED curable.
Embodiment 2
1) preparation of alloyed powder
Weigh nanometer silver powder 100 parts, bismuth oxide 15 parts, zinc oxide 30 parts, nikel powder 50 parts, MTES 15 parts, 10 parts of graphite;By each raw material by proportioning at 1500 DEG C~1650 DEG C, less than 10-3The vacuum of torr is smelted into homogenizing and closes Gold solution, the gas low by activity prepares alloyed powder with the pressure peening of 20~30atm with moment atomization;
2) preparation of conducting resinl
Based on weight/mass percentage composition, by acrylic resin 15%, phenolic resin 5%, triphenyl phosphite 6%, polymerization inhibitor 0.7%, firming agent 8%, stirs, and is slowly added to step 1) obtained by alloyed powder 75%, stir, froth in vacuum, Prepare the good conducting resinl of described LED curable.
In above-described embodiment 1~2, selected firming agent is THPA, methyl tetrahydro phthalic anhydride, HHPA, methyl six One or more mixture in hydrogen phthalic anhydride, methylnadic anhydride, dodecyl maleic anhydride.Selected polymerization inhibitor is Hydroquinone, MEHQ, 2, one or more mixture in 6-di-tert-butyl-4-methy phenol.Selected activity Low gas is selected from argon or nitrogen.
Conducting resinl obtained by embodiment 1~2 is carried out the test of performance, specific insulation about 10-5~10-4Ω cm, Heat conductivity about 24.0W/m K, viscosity about 48200mPa.s.
Meanwhile, carrying out the test of viscosity after the conducting resinl room temperature obtained by embodiment 1~2 being placed 2 months, viscosity is about 48300mPa.s, it can be seen that prepared conducting resinl has good viscosity stability.
Above-mentioned each embodiment is further illustrating of making of the foregoing to the present invention, but should not be construed as the present invention The scope of above-mentioned theme is only limitted to above-described embodiment.It should be pointed out that, for those skilled in the art, not On the premise of departing from the technology of the present invention principle, it is also possible to make some improvements and modifications, these improvements and modifications also should be regarded as this The protection domain of invention.

Claims (4)

1. the preparation technology of the good conducting resinl of LED curable, it is characterised in that preparation process is as follows:
1) preparation of alloyed powder
Weigh nanometer silver powder 80~100 parts, bismuth oxide 8~15 parts, zinc oxide 20~30 parts, nikel powder 40~50 parts, methyl Triethoxysilane 10~15 parts, graphite 6~10 parts;By each raw material by proportioning at 1500 DEG C~1650 DEG C, less than 10-3Torr's Vacuum is smelted into homogeneous alloy solution, and the gas low by activity prepares with moment atomization with the pressure peening of 20~30atm Alloyed powder;
2) preparation of conducting resinl
Based on weight/mass percentage composition, by acrylic resin 10%~15%, phenolic resin 2%~5%, triphenyl phosphite 4% ~6%, polymerization inhibitor 0.3%~0.7%, firming agent 3%~8%, stir, be slowly added to step 1) obtained by alloyed powder 65%~75%, stir, froth in vacuum, prepare the good conducting resinl of described LED curable.
The preparation technology of one or more mixture good conducting resinl of LED curable the most according to claim 1, its feature Be: step 2) described in firming agent be that THPA, methyl tetrahydro phthalic anhydride, HHPA, methyl hexahydrophthalic anhydride, methyl are received One or more mixture in Dick anhydride, dodecyl maleic anhydride.
The preparation technology of one or more mixture good conducting resinl of LED curable the most according to claim 1, its feature Be: step 2) described in polymerization inhibitor be hydroquinone, MEHQ, 2, in 6-di-tert-butyl-4-methy phenol One or more mixture.
The preparation technology of one or more mixture good conducting resinl of LED curable the most according to claim 1, its feature It being: described step 1) gas that the activity that uses is low is selected from argon or nitrogen.
CN201610654901.1A 2016-08-11 2016-08-11 A kind of preparation technology of the good conducting resinl of LED curable Pending CN106281098A (en)

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Application Number Priority Date Filing Date Title
CN201610654901.1A CN106281098A (en) 2016-08-11 2016-08-11 A kind of preparation technology of the good conducting resinl of LED curable

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110964461A (en) * 2018-09-29 2020-04-07 北京梦之墨科技有限公司 Thermosetting anisotropic conductive adhesive and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102646458A (en) * 2011-02-16 2012-08-22 中国钢铁股份有限公司 Lead-free conducting resin and manufacture method thereof
CN103740309A (en) * 2013-12-10 2014-04-23 江苏瑞德新能源科技有限公司 Repairable conductive adhesive and preparation method thereof
CN105419672A (en) * 2015-12-24 2016-03-23 常熟昊虞电子信息科技有限公司 Preparation method of high-heat-dissipation electric-conductive glue used for high-power LED

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102646458A (en) * 2011-02-16 2012-08-22 中国钢铁股份有限公司 Lead-free conducting resin and manufacture method thereof
CN103740309A (en) * 2013-12-10 2014-04-23 江苏瑞德新能源科技有限公司 Repairable conductive adhesive and preparation method thereof
CN105419672A (en) * 2015-12-24 2016-03-23 常熟昊虞电子信息科技有限公司 Preparation method of high-heat-dissipation electric-conductive glue used for high-power LED

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110964461A (en) * 2018-09-29 2020-04-07 北京梦之墨科技有限公司 Thermosetting anisotropic conductive adhesive and preparation method thereof

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