CN104497784B - Preparation method for hydrophobic nanometer modified resin composite paint used for LED base plate - Google Patents

Preparation method for hydrophobic nanometer modified resin composite paint used for LED base plate Download PDF

Info

Publication number
CN104497784B
CN104497784B CN201410690428.3A CN201410690428A CN104497784B CN 104497784 B CN104497784 B CN 104497784B CN 201410690428 A CN201410690428 A CN 201410690428A CN 104497784 B CN104497784 B CN 104497784B
Authority
CN
China
Prior art keywords
mass parts
colloidal sol
resin
led
nanometer
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.)
Expired - Fee Related
Application number
CN201410690428.3A
Other languages
Chinese (zh)
Other versions
CN104497784A (en
Inventor
杨辉
吴春春
张玲洁
阙永生
汪海风
钱骁
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zigong Innovation Center of Zhejiang University
Original Assignee
Zigong Innovation Center of Zhejiang University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Zigong Innovation Center of Zhejiang University filed Critical Zigong Innovation Center of Zhejiang University
Priority to CN201410690428.3A priority Critical patent/CN104497784B/en
Publication of CN104497784A publication Critical patent/CN104497784A/en
Application granted granted Critical
Publication of CN104497784B publication Critical patent/CN104497784B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/5406—Silicon-containing compounds containing elements other than oxygen or nitrogen
    • 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
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • 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
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention relates to preparation of paint, and aims at providing a preparation method for hydrophobic nanometer modified resin composite paint used for an LED base plate. The method comprises: firstly uniformly dispersing nanometer alpha-Al2O3 and butanol; then adding a silane coupling agent KH560 and ageing, so as to obtain a modified alpha-Al2O3 sol, and performing concentration distillation; uniformly mixing 1H,1H,2H,2H-perfluorooctyltriethoxysilane, n-butanol and formic acid, then adding deionized water, and ageing to obtain a silicon fluoride oligomer sol; and dispersing the former two products, an epoxy resin monomer, 2-butanone, xylene and 2,2,4-trimethyl-1,3-pentanediolmono(2-methylpropanoate), so as to obtain the paint. By introducing alpha-Al2O3 nano-particle into a conventional epoxy resin coating, the heat conductivity of resin is improved, also the excellent coating property and the workability of resin are maximumly kept, and the price is relatively appropriate. The hydrophobicity is substantially improved, and the short circuit problem caused by air moist is reduced. The prepared hydrophobic nanometer modified resin composite paint is suitable for production processing on a conventional production line, and is beneficial improvement on the basis of a conventional epoxy-resin-coated aluminium base plate.

Description

Preparation method for the dewatering nano modified resin composite coating of LED-baseplate
Technical field
The present invention relates to coating technology, especially for the preparation of the dewatering nano modified resin composite coating of LED-baseplate Method.
Background technology
LED-baseplate is to connect the bridge of LED and cooling mechanism, is that heat is delivered to the main thoroughfare in the external world from chip, because And to LED whether can trouble free service particularly significant, the circuit line due to LED directly connects up in substrate, thus the heat conduction to substrate Property and insulating properties require all very high.Simultaneously as LED circuit directly connects up on substrate, when surrounding air is moist, substrate is easy Absorption steam, causes the phenomenons such as circuit-line short circuit.Traditional LED-baseplate material is generally fine aluminium substrate surface and coats one layer of resin Insulating barrier is obtained, and in a typical LED structure, the heat that LED produces is transmitted to metal substrate by insulating barrier, then passes through Thermal interfacial material is transmitted to radiator, thus can be diffused into heats most produced by LED by way of convection current The in the air of surrounding.Resin insulating barrier has very high coating and adhesive force on aluminium sheet, but most aluminium base tree Fat insulating barrier has the heat conductivity of very little even without thermal conductivity, so allows for heat and can not be transmitted to fin from LED (metal substrate) is it is impossible to realize whole heat dissipation channel unimpeded.So, the heat history of LED will soon lead to LED failure.Therefore, The aluminium base with high thermal conductivity is most important for LED.α-Al2O3It is that a kind of thermal conductivity factor is high, the oxidation of good insulating Thing, is introduced in resin and can improve resin thermal conductivity well, the hydrophobic performance of silicon fluoride is very excellent simultaneously；The present invention selects Select in the nano aluminium oxide (α-Al with high-termal conductivity2O3)For filler, resin insulating barrier coating is modified, so that resin is applied Layer keeps on aluminium base that coating, adhesive force is excellent, insulating properties high on the premise of, reach high-termal conductivity, simultaneously silicon fluoride Long fluorocarbon chain adsorbs, by substantially reducing substrate, the short circuit phenomenon that steam causes in wet condition.
Content of the invention
It is an object of the invention to overcoming deficiency of the prior art, provide a kind of nano modification tree for LED-baseplate The preparation method of fat composite coating.
The invention provides a kind of preparation method of the nano modification resin compounded coating for LED-baseplate, including as follows Step：
(1) under the stir speed (S.S.) of 800～1000r/min, by the nanometer α-Al of 20～30 mass parts2O3With 55～70 matter It is uniformly dispersed in the butanol addition dispersion machine of amount part；Being subsequently adding hydrogen ion concentration in HCl regulation system is 10-3～10-4M, so Add the silane coupler KH560 of 10～15 mass parts afterwards, be aged 24 hours at 50 DEG C, obtain receiving through KH560 surface modification Rice α-Al2O3Colloidal sol；
(2) 20～30 mass parts tridecafluoro-n-octyltriethoxysilanes are added in 57～74 mass parts n-butanols, then Add 1～3 mass parts formic acid to mix, add 5～10 mass parts deionized waters, be aged 48 hours at 60 DEG C, obtain Silicon fluoride oligomer colloidal sol；
(3) L-H type Rotary Evaporators are utilized to modified α-Al2O3Colloidal sol concentrates distillation so that butanol evaporates, bath temperature 70 DEG C, rotary speed 60r/min, it is concentrated into α-Al2O3The mass concentration of colloidal sol is 50%～60%；
(4) by the concentration α-Al of 30～40 mass parts2O3Colloidal sol, 1～10 part of silicon fluoride oligomer colloidal sol, 30～60 mass The epoxy monomer of part, the 2,2,4- tri- of the MEK of 1～10 mass parts, the dimethylbenzene of 1～5 mass parts and 3～7 mass parts Methyl isophthalic acid, 3- pentanediol mono isobutyrate adds dispersion machine, disperses 1h, obtain under the rate of dispersion of 1500～2000r/min Dewatering nano α-Al2O3Modified epoxy resin LED-baseplate coating.
In the present invention, nanometer α-Al described in step (1)2O3Average grain diameter in 200～300nm, phase purity exists 99.9%.
In the present invention, step (3) epoxy resin monomer is glycidol type epoxy resin 6101 epoxy resin E-44.
Compared with existing technology of preparing, the invention has the characteristics that：
Traditional LED epoxy resin aluminium coating baseplate material has that filming performance is good, and adhesive force is excellent, cheap plus The advantages of work performance is good, but there is the critical defect of poor thermal conductivity, this has had a strong impact on the service life of LED component.LED at present Thermal conductivity preferably aluminium oxide ceramic substrate, silicon carbide substrate in stock, but pottery is substantially relatively costly, and all relatively Firmly, processing characteristics is poor, substandard products easily.Meanwhile, LED-baseplate is easily led because of absorption moisture content under the higher environment of humidity Cause the line short on its surface, this is also the major reason causing LED component quality problems.For the problems referred to above, this Invention introduces α-Al in conventional epoxies coating2O3Nano particle to improve the heat conductivility of resin, simultaneously farthest Remain excellent coating and the processability of resin, price also relative good.On this basis, introduce the long fluorine of silicon fluoride Carbochain makes resin hydrophobic performance significantly improve, and reduces the line short problem causing because there was dampness in the air.At present, in aluminium base The process route of upper coated with resins coating is very ripe, is well suited for production and processing on existing production line.It is to conventional epoxy tree Fat covers the useful improvement of aluminium base.
Specific embodiment
Below by example, the present invention is further described.
It is used for the preparation method of the nano modification resin compounded coating of LED-baseplate in the present invention, comprise the steps：
(1) under the stir speed (S.S.) of 800～1000r/min, by the nanometer α-Al of 20～30 mass parts2O3With 55～70 matter It is uniformly dispersed in the butanol addition dispersion machine of amount part；It is subsequently adding in HCl regulation system hydrogen ion concentration 10-3～10-4M, so Add the silane coupler KH560 of 10～15 mass parts afterwards, be aged 24 hours at 50 DEG C, obtain receiving through KH560 surface modification Rice α-Al2O3Colloidal sol.
(2) 20～30 mass parts tridecafluoro-n-octyltriethoxysilanes are added in 57～74 mass parts n-butanols, add 1 ～3 mass parts formic acid mix, and add 5～10 mass parts deionized waters, be aged 48 hours, obtain silicon fluoride low at 60 DEG C Polymers colloidal sol.
(3) L-H type Rotary Evaporators are utilized to modified α-Al2O3Colloidal sol concentrates distillation so that butanol evaporates, bath temperature 70 DEG C, rotary speed 60r/min, it is concentrated into α-Al2O3The mass concentration of colloidal sol is 50%～60%；
(4) by the concentration α-Al of 30～40 mass parts2O3Colloidal sol, 1～10 part of silicon fluoride oligomer colloidal sol, 30～60 mass The epoxy monomer of part, the 2,2,4- tri- of the MEK of 1～10 mass parts, the dimethylbenzene of 1～5 mass parts and 3～7 mass parts Methyl isophthalic acid, 3- pentanediol mono isobutyrate adds dispersion machine, disperses 1h, obtain under the rate of dispersion of 1500～2000r/min Dewatering nano α-Al2O3Modified epoxy resin LED-baseplate coating.
Test data in each embodiment see table (number of each component is mass fraction)：
In embodiments of the invention：
Nanometer α-Al2O3Average grain diameter in 200～300nm, phase purity 99.9%, is had by Hangzhou super prestige nano material Limit company produces.Nanometer α-Al2O3Grain graininess can neither be too little, nor too big, if grain graininess is too little (below 100nm) Resin is difficult disperse, if grain graininess is too big (more than several microns), easily produces the phenomenon of particle sedimentation, be unfavorable for leading The raising of hot property.
Butanol is to analyze pure butanol, and Hangzhou Chinese medicines group chemical reagent work produces.The reagent such as MEK, dimethylbenzene are analysis Pure, Hangzhou Chinese medicines group chemical reagent work.Tridecafluoro-n-octyltriethoxysilane, purity 99.7%, Hangzhou chemical research institute produces.Epoxy Resin monomer is glycidol type epoxy resin 6101 epoxy resin E-44, and the wooden Chemical Co., Ltd. in Jiangsu three produces.2,2,4- Trimethyl -1,3- pentanediol mono isobutyrate purity 99.8%, Dongguan Jiang Long Chemical Co., Ltd. produces.
Last in addition it is also necessary to it is noted that listed above be only the present invention be embodied as example.Obviously, the present invention is not It is limited to above example, can also have many deformation.Those of ordinary skill in the art can be straight from present disclosure Connect all deformation derived or associate, be all considered as protection scope of the present invention.

Claims (2)

1. a kind of preparation method of the dewatering nano modified resin composite coating for LED-baseplate is it is characterised in that include as follows Step：
(1) under the stir speed (S.S.) of 800～1000r/min, by the nanometer α-Al of 20～30 mass parts2O3With 55～70 mass parts Butanol add dispersion machine in be uniformly dispersed；Being subsequently adding hydrogen ion concentration in HCl regulation system is 10-3～10-4M, Ran Houjia Enter the silane coupler KH560 of 10～15 mass parts, be aged 24 hours at 50 DEG C, obtain nanometer α through KH560 surface modification- Al2O3Colloidal sol；Described nanometer α-Al2O3Average grain diameter in 200～300nm, phase purity is 99.9%；
(2) 20～30 mass parts tridecafluoro-n-octyltriethoxysilanes are added in 57～74 mass parts n-butanols, be subsequently adding 1 ～3 mass parts formic acid mix, and add 5～10 mass parts deionized waters, be aged 48 hours, obtain silicon fluoride at 60 DEG C Oligomer colloidal sol；
(3) L-H type Rotary Evaporators are utilized to modified α-Al2O3Colloidal sol concentrates distillation so that butanol evaporates, bath temperature 70 DEG C, rotary speed 60r/min, it is concentrated into α-Al2O3The mass concentration of colloidal sol is 50%～60%；
(4) by the concentration α-Al of 30～40 mass parts2O3Colloidal sol, 1～10 part of silicon fluoride oligomer colloidal sol, 30～60 mass parts Epoxy monomer, the 2,2,4- front three of the MEK of 1～10 mass parts, the dimethylbenzene of 1～5 mass parts and 3～7 mass parts Base -1,3- pentanediol mono isobutyrate adds dispersion machine, disperses 1h, dredged under the rate of dispersion of 1500～2000r/min Water nanometer α-Al2O3Modified epoxy resin LED-baseplate coating.
2. method according to claim 1 is it is characterised in that step (4) epoxy resin monomer is glycidol type ring Oxygen tree fat 6101.
CN201410690428.3A 2014-11-25 2014-11-25 Preparation method for hydrophobic nanometer modified resin composite paint used for LED base plate Expired - Fee Related CN104497784B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410690428.3A CN104497784B (en) 2014-11-25 2014-11-25 Preparation method for hydrophobic nanometer modified resin composite paint used for LED base plate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410690428.3A CN104497784B (en) 2014-11-25 2014-11-25 Preparation method for hydrophobic nanometer modified resin composite paint used for LED base plate

Publications (2)

Publication Number Publication Date
CN104497784A CN104497784A (en) 2015-04-08
CN104497784B true CN104497784B (en) 2017-02-22

Family

ID=52939245

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410690428.3A Expired - Fee Related CN104497784B (en) 2014-11-25 2014-11-25 Preparation method for hydrophobic nanometer modified resin composite paint used for LED base plate

Country Status (1)

Country Link
CN (1) CN104497784B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110669257B (en) * 2019-08-29 2021-04-30 平高集团有限公司 Coated modified alumina, preparation method thereof and epoxy composite insulating material

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101575478B (en) * 2008-05-05 2011-06-22 中国科学院宁波材料技术与工程研究所 Method for preparing epoxy resin super-hydrophobic coat
US8431220B2 (en) * 2009-06-05 2013-04-30 Xerox Corporation Hydrophobic coatings and their processes
CN101691909A (en) * 2009-07-10 2010-04-07 东莞市万丰纳米材料有限公司 LED packaging module and preparation method thereof
CN103409028B (en) * 2013-07-29 2017-11-17 复旦大学 A kind of photocatalytic type self-repairing super-hydrophobic coating and preparation method thereof

Also Published As

Publication number Publication date
CN104497784A (en) 2015-04-08

Similar Documents

Publication Publication Date Title
CN104592831B (en) Heat-conducting coating and preparation method of heat-conducting film
CN102770956B (en) Thermosetting resin composition, b-stage thermally conductive sheet, and power module
CN110643331B (en) Liquid metal heat-conducting paste and preparation method and application thereof
CN107974232B (en) LED chip insulating heat-conducting die bond adhesive and preparation method thereof
CN108102144A (en) A kind of graphene-based heat-conductive composite material and preparation method thereof
SE533966C2 (en) Insulating varnish that is resistant to partial discharge, insulated pipe and method of manufacturing the same
CN104178076A (en) Heat-conducting electric-insulating epoxy resin potting adhesive and preparation method thereof
CN104497477B (en) Heat conductive composite material and preparation method thereof
CN106189602A (en) A kind of modified white graphite alkene compound anti-oxidation coating and preparation thereof
KR101782231B1 (en) Coating composition for radiant heat having improved heat radiation property and surface hardness, preparation method thereof, and heat radiating coating comprising the same
CN103265702A (en) Preparation method of ultraviolet-resistant and high-temperature-resistant methyl silicone resin
CN105199619B (en) Aluminum-based copper-clad plate high-heat-conductivity glue membrane preparation method
CN104497784B (en) Preparation method for hydrophobic nanometer modified resin composite paint used for LED base plate
CN104194562A (en) Preparation method of normal-temperature-curing single-component nano composite water-based paint
CN104559807B (en) A kind of heat conduction bonding agent
CN106243867A (en) Heat dissipation coating and preparation method thereof
CN105086659A (en) Preparation method of high-thermal-conductivity nano carbon copper foil
CN106590548A (en) Low-density and high-strength heat-conducting silica gel gasket
JP4516779B2 (en) Metal oxide surface-treated particles, method for producing the same, and method for producing a resin composition
CN114410063A (en) Heat-conducting and insulating epoxy resin composite material and preparation method thereof
CN104497785B (en) Preparation method for nanometer modified resin composite paint used for LED base plate
CN107459775B (en) A kind of epoxy resins insulation heat-conductive composite material and preparation method thereof
CN113150728A (en) Heat-conducting pouring sealant and preparation method thereof
CN112694719A (en) Resin composition, preparation method thereof and metal substrate
CN105907273A (en) Method for preparing anti-static insulating paint

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20170222

Termination date: 20211125

CF01 Termination of patent right due to non-payment of annual fee