CN104900793A - Preparation and application of insulating core shell composite structure high in heat conduction and high in reflectivity - Google Patents
Preparation and application of insulating core shell composite structure high in heat conduction and high in reflectivity Download PDFInfo
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- CN104900793A CN104900793A CN201510293744.1A CN201510293744A CN104900793A CN 104900793 A CN104900793 A CN 104900793A CN 201510293744 A CN201510293744 A CN 201510293744A CN 104900793 A CN104900793 A CN 104900793A
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- heat conduction
- high reflectance
- shell structure
- core
- high heat
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- 239000011258 core-shell material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002310 reflectometry Methods 0.000 title claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000741 silica gel Substances 0.000 claims abstract description 12
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 23
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- 238000009413 insulation Methods 0.000 claims description 20
- 150000001875 compounds Chemical class 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 17
- 238000005516 engineering process Methods 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 229910052782 aluminium Inorganic materials 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000004411 aluminium Substances 0.000 claims description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 8
- 229910003460 diamond Inorganic materials 0.000 claims description 8
- 239000010432 diamond Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 7
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 239000011824 nuclear material Substances 0.000 claims description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 5
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 5
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 5
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 5
- 229940043237 diethanolamine Drugs 0.000 claims description 5
- 238000010345 tape casting Methods 0.000 claims description 5
- 239000004246 zinc acetate Substances 0.000 claims description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- 238000007650 screen-printing Methods 0.000 claims description 4
- 238000003854 Surface Print Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 15
- 238000004806 packaging method and process Methods 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 2
- 230000017525 heat dissipation Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 23
- 239000010408 film Substances 0.000 description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 239000006185 dispersion Substances 0.000 description 9
- 230000007613 environmental effect Effects 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 238000000280 densification Methods 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- 238000000875 high-speed ball milling Methods 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910001593 boehmite Inorganic materials 0.000 description 2
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 1
- 229910001573 adamantine Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000027950 fever generation Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000013464 silicone adhesive Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/64—Heat extraction or cooling elements
- H01L33/641—Heat extraction or cooling elements characterized by the materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/483—Containers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/58—Optical field-shaping elements
- H01L33/60—Reflective elements
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/005—Processes relating to semiconductor body packages relating to encapsulations
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/0058—Processes relating to semiconductor body packages relating to optical field-shaping elements
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/0075—Processes relating to semiconductor body packages relating to heat extraction or cooling elements
Landscapes
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Led Device Packages (AREA)
Abstract
The invention relates to the preparation field of insulating core shell composite structures, and concretely relates to preparation and applications of insulating core shell composite structures high in heat conduction and high in reflectivity. Compared with insulating core shell composite structures produced by the prior art, nano to micron insulating core shell composite structures prepared are high in heat conduction and high in reflectivity, and exhibit excellent insulating properties. Meanwhile, the insulating core shell composite structures can disperse steady in silica gel. An adopted synthesis process is environment-friendly, simple, and low in cost. Furthermore, a one-step packaging method is provided to enable LED chip packaging to be realized while highly reflective film layers can be printed. Module packaging steps are simplified, and the heat dissipation efficiency of devices is improved.
Description
Technical field
The present invention relates to the preparation field of insulation core-shell structure, is a kind of preparations and applicatio of insulation core-shell structure of high heat conduction high reflectance concretely.
Background technology
Light-emitting diode is a kind of semiconductor lighting with energy-conservation, environmental protection, the advantage such as the life-span is long, volume is little, high brightness, is regarded as replacing incandescent lamp and fluorescent lamp and becomes the mainstream technology of general illumination.
At present, based on single-chip package pattern because its luminous flux is limited, for actual illumination application, need the integrated making of plurality of LEDs.But direct insertion LED integrated after have dazzle that people is done not feel like oneself, therefore generally adopt multi-chip serial or parallel connection adhere to or be welded on aluminium base, be made into luminous uniform area source.Meanwhile, along with chip power increases, required operating current is increasing.Device local pyrexia causes chip temperature to raise, and especially adopt blue chip to excite yellow fluorescent powder to produce the technology of white light, working temperature rising can make chip wavelength shift, cannot effective excitated fluorescent powder, the luminous efficiency of reduction module.
For LED technique, there is the material of more than at least four layers, insulating barrier, conductive copper rete, reflective film layer and silicone adhesive layer etc. between usual aluminium base to chip, thus entire thermal resistance amount is comparatively large, and actual heat transfer efficiency is low.Wherein, the traditional handicraft of reflective film layer is at substrate surface adhesion metal thin layer by sputtering or the method such as evaporation or plating, as Chinese patent CN100403503C, the high-reflectivity metal thin layers such as tin, nickel or aluminium are plated at circuit board surface, but there is complicated process of preparation, the defects such as energy consumption is large, seriously polluted.In heat conductive silica gel, adulterate the nanometer of high reflectance to micron-sized powder, and on aluminium base, adhere to by silk screen printing or knife coating the technology that high reverse--bias thin layer is comparatively main flow at present, the advantages such as this technique has with low cost, environmental protection, simple to operate.But, there is at visible ray 400-700nm the Al of high reflectance
2o
3, TiO
2, the oxide such as ZnO because of its conductive coefficient on the low side, affect overall device radiating efficiency, reduce chip light emitting efficiency, make light source less reliable, reduction of service life.
There is provided a kind of with low cost, insulation core-shell structure with high heat conduction and high reflectance and preparation method thereof to be very important for this reason.
Summary of the invention
The difficult problem that the present invention breaches prior art devises a kind of with low cost, insulation core-shell structure with high heat conduction and high reflectance.
The present invention devises a kind of insulation core-shell structure of high heat conduction high reflectance in order to achieve the above object, and its preparation technology is as follows:
Step 1, carries out physical grinding and forms nuclear material powder by the one in SiC, AlN, BN and diamond;
Step 2, puts into 95% ethanolic solution by nuclear material powder and carries out ultrasonic cleaning purifying, forms core powder;
Step 3, it is in the precursor solution of 10-50% that core powder is dispersed in concentration range according to weight proportion 15-35%, ultrasonic disperse 1 hour, then precipitation reagent is added according to the ratio of 1:10 and 2:5, catalyst stirs 3-5 hour, then dry at being placed in drying box 60-100 DEG C, form composite material;
Step 4, calcines 5-6 hour, forms compound calcined materials at 500-900 DEG C by composite material;
Step 5, is placed on ultrasonic disperse 30-60 minute in mixed solution by compound calcined materials, drip 2-5ml tetraethoxysilane and 1-8ml ammoniacal liquor, magnetic agitation 6-10 hour, obtains high reflectance insulated compound core-shell material.
Described presoma is the one in aluminum nitrate, aluminium chloride, butyl titanate, zinc acetate, zinc nitrate.
Described precipitation reagent is the one in NaOH, ammoniacal liquor, diethanol amine, hydrochloric acid.
In the present invention, catalyst is the one in acetic acid, nitric acid, hydrochloric acid.
Described mixed solution is the deionized water of 1:5 and mixing of ethanol by volume ratio.
The conductive coefficient of described high reflectance insulated compound core-shell material is 0.5-3.0W/ (mk), and the scope internal reflection rate being 400-700nm at visible ray light wave is 93%-98%, and voltage endurance is 2000V.
A kind of application of insulation core-shell structure of high heat conduction high reflectance is as follows:
Step 1, carries out physical grinding by the high reflectance insulated compound core-shell material of preparation and ethylene glycol and silica gel by the mass ratio of 1:6-10:1-18, obtains composite mortar;
Step 2, slurry is pressed figure by silk screen printing or knife coating on aluminium base surface print, chip is directly sticked on slurry according to circuit configuration, at 1 atmospheric pressure or heated under vacuum to 100-200 DEG C, forms the high heat conduction high reflectivity film layer that thickness is 10-50 μm.
Described physical grinding is mechanical ball milling, and be 8-15:16-30 mixing in mass ratio by composite mortar and agate ball, then under the rotating speed of 300-500 revolutions per second, carry out ball milling, Ball-milling Time is 1-4 hour.
Compared with the existing technology, obtained nanometer has high heat conduction, high reflectance and excellent insulating properties to micron order insulation core-shell structure in the present invention, energy stable dispersion in silica gel simultaneously, the synthesis technique environmental protection of employing, simple, low cost; And propose a step package method namely print high reverse--bias thin layer while packaging LED chips, simplify module package step, improve the radiating efficiency of device.
Embodiment
The present invention devises a kind of with low cost, insulation core-shell structure with high heat conduction and high reflectance in order to achieve the above object, and its preparation technology is as follows:
Step 1, carries out physical grinding and forms nuclear material powder by the one in SiC, AlN, BN and diamond;
Step 2, puts into 95% ethanolic solution by nuclear material powder and carries out ultrasonic cleaning purifying, forms core powder;
Step 3, it is in the precursor solution of 10-50% that core powder is dispersed in concentration range according to weight proportion 15-35%, ultrasonic disperse 1 hour, then precipitation reagent is added according to the ratio of 1:10 and 2:5, catalyst stirs 3-5 hour, then dry at being placed in drying box 60-100 DEG C, form composite material;
Step 4, calcines 5-6 hour, forms compound calcined materials at 500-900 DEG C by composite material;
Step 5, is placed on ultrasonic disperse 30-60 minute in mixed solution by compound calcined materials, drip 2-5ml tetraethoxysilane and 1-8ml ammoniacal liquor, magnetic agitation 6-10 hour, obtains high reflectance insulated compound core-shell material.
Described presoma is the one in aluminum nitrate, aluminium chloride, butyl titanate, zinc acetate, zinc nitrate.
Described precipitation reagent is the one in NaOH, ammoniacal liquor, diethanol amine, hydrochloric acid.
In the present invention, catalyst is the one in acetic acid, nitric acid, hydrochloric acid.
Described mixed solution is the deionized water of 1:5 and mixing of ethanol by volume ratio.
The conductive coefficient of described high reflectance insulated compound core-shell material is 0.5-3.0W/ (mk), and the scope internal reflection rate being 400-700nm at visible ray light wave is 93%-98%, and voltage endurance is 2000V.
A kind of application of insulation core-shell structure of high heat conduction high reflectance is as follows:
Step 1, carries out physical grinding by the high reflectance insulated compound core-shell material of preparation and ethylene glycol and silica gel by the mass ratio of 1:6-10:1-18, obtains composite mortar;
Step 2, slurry is pressed figure by silk screen printing or knife coating on aluminium base surface print, chip is directly sticked on slurry according to circuit configuration, at 1 atmospheric pressure or heated under vacuum to 100-200 DEG C, forms the high heat conduction high reflectivity film layer that thickness is 10-50 μm.
Described physical grinding is mechanical ball milling, and be 8-15:16-30 mixing in mass ratio by composite mortar and agate ball, then under the rotating speed of 300-500 revolutions per second, carry out ball milling, Ball-milling Time is 1-4 hour.
Compared with the existing technology, obtained nanometer has high heat conduction, high reflectance and excellent insulating properties to micron order insulation core-shell structure in the present invention, energy stable dispersion in silica gel simultaneously, the synthesis technique environmental protection of employing, simple, low cost; And propose a step package method namely print high reverse--bias thin layer while packaging LED chips, simplify module package step, improve the radiating efficiency of device.
In concrete enforcement:
Embodiment 1
Take the AlN powder of 10 g6-8um, adopt satellite form ball mill, carry out the dispersion of high speed ball milling, the AlN powder dispersion crossed by ball milling carries out ultrasonic cleaning in ethanolic solution, and the time is 5-10 hour.Taking 13ml butyl titanate is dissolved into as presoma in 27ml ethanolic solution, and pretreated AlN powder joins in above-mentioned solution by magnetic agitation 30 minutes, ultrasonic disperse 1 hour; Get a certain amount of deionized water again and 5ml acetic acid is dissolved in ethanolic solution, make solution be acid, magnetic agitation, after 20 minutes, is added dropwise in above-mentioned butyl titanate solution while stirring, stirs 4-5 hour, forms the TiO including AlN
2colloidal sol, question response is complete, dries, the composite material of oven dry is calcined 5-6 hour at 500-900 DEG C at putting into baking oven 60-100 DEG C.By volume for 1:5 prepares the mixed liquor of deionized water and ethanol, be dispersed in above-mentioned solution, ultrasonic disperse 30-60 minute by the composite material after calcining, drip 0.07-0.1ml tetraethoxysilane, ammoniacal liquor does precipitation reagent, magnetic agitation 6-10 hour, obtains AlNTiO
2siO
2multilayer edge core-shell structure, wherein AlN content is 76-89%, TiO
2layer thickness is 100-300 nm, SiO
2thin film layer thickness is 5-10 nm.Then, the multilayer edge core-shell structure material of preparation and ethylene glycol and silica gel are carried out mechanical ball milling by 1:6-10:1-15 mass ratio, the obtained reflective glue of high heat conduction, high reverse--bias film is prepared on aluminium base surface by knife coating, chip is directly sticked on slurry according to circuit configuration, at 1 atmospheric pressure or heated under vacuum to 100-200 DEG C, form the high heat conduction of densification and the high reflectivity film of 30-50 um thickness.Conductive coefficient is 0.85-2.3 W/ (mk), is 95%-98% at the reflectivity of visible ray 400-700 nm.
Embodiment 2
Take the diamond dust of 10 g 500nm-4um, adopt satellite form ball mill, carry out the dispersion of high speed ball milling, the diamond dust crossed by ball milling is dispersed in ethanolic solution and carries out ultrasonic cleaning, and the time is 5-10 hour.Taking 15g aluminum nitrate (nine water) is dissolved into as presoma in the 45ml aqueous solution, and magnetic agitation 30 minutes, joins pretreated diamond dust in above-mentioned solution, ultrasonic disperse 1 hour; Get 4-12 ml concentrated ammonia liquor again, be added dropwise in above-mentioned aluminum nitrate solution while stirring, add 0.4-1.2ml red fuming nitric acid (RFNA) simultaneously, promote reaction, stir 3-5 hour, formed and include adamantine boehmite sol, question response is complete, dry at putting into baking oven 85-100 DEG C, the compound of oven dry is calcined 5-6 hour at 500-900 DEG C.SiO is prepared by step in example 1
2thin layer, obtains diamond Al
2o
3siO
2multilayer edge core-shell structure, wherein diamond content is 62-83%, Al
2o
3layer thickness is 30-100 nm, SiO
2thin film layer thickness is 5-10 nm.Then, the multilayer edge core-shell structure material of preparation and ethylene glycol and silica gel are carried out mechanical ball milling by 1:6-10:3-18 mass ratio, the obtained reflective glue of high heat conduction, high reverse--bias film is prepared on aluminium base surface by silk screen print method, chip is directly sticked on slurry according to circuit configuration, at 1 atmospheric pressure or heated under vacuum to 100-200 DEG C, form the high heat conduction of densification and the high reflectivity film of 10-40 um thickness.Conductive coefficient is 1.3-3.0 W/ (mk), is 94%-97% at the reflectivity of visible ray 400-700nm.
Embodiment 3
Take the BN powder of 10 g500nm-1um, adopt satellite form ball mill, carry out the dispersion of high speed ball milling, the BN powder dispersion crossed by ball milling carries out ultrasonic cleaning in ethanolic solution, and the time is 5-10 hour.Taking 17-22 g zinc acetate (two water) is dissolved into as presoma in ethanolic solution, and magnetic agitation 30 minutes, joins in above-mentioned solution by pretreated BN powder, ultrasonic disperse 1 hour; The diethanol amine getting 4-5 ml is again dissolved in ethanolic solution, be added dropwise in above-mentioned zinc acetate solution while stirring, add deionized water and slow down reaction rate, stir 4-5 hour, form the ZnO colloidal sol including BN, question response is complete, dries, the compound of oven dry is calcined 5-6 hour at 500-900 DEG C at putting into baking oven 60-100 DEG C.SiO is prepared by step in example 1
2thin layer, obtains BNZnOSiO
2multilayer edge core-shell structure, wherein BN content is 52-58%, and ZnO layer thickness is 20-50 nm, SiO
2thin film layer thickness is 5-10 nm.Then, the multilayer edge core-shell structure material of preparation and ethylene glycol and silica gel are carried out mechanical ball milling by 1:6-10:5-18 mass ratio, the obtained reflective glue of high heat conduction, high reverse--bias film is prepared on aluminium base surface by silk screen print method, chip is directly sticked on slurry according to circuit configuration, at 1 atmospheric pressure or heated under vacuum to 100-200 DEG C, form the high heat conduction of densification and the high reflectivity film of 10-40 um thickness.Conductive coefficient is 0.5-1.14 W/ (mk), is 93%-96% at the reflectivity of visible ray 400-700nm.
Embodiment 4
Take the SiC powder of 10 g 1-5um, adopt satellite form ball mill, carry out the dispersion of high speed ball milling, the SiC powder crossed by ball milling is dispersed in ethanolic solution carries out ultrasonic cleaning, and the time is 5-10 hour.Taking 2.5-6 g aluminium chloride is dissolved into as presoma in the aqueous solution, and pretreated SiC powder joins in above-mentioned solution by magnetic agitation 30 minutes, ultrasonic disperse 1 hour; Get the ammoniacal liquor of 2.2-2.7ml again, be added dropwise in above-mentioned liquor alumini chloridi while stirring, add 0.16-0.2ml hydrochloric acid simultaneously, promote reaction, stir 3-5 hour, form the boehmite sol including SiC, question response is complete, dry at putting into baking oven 85-100 DEG C, the compound of oven dry is calcined 5-6 hour at 500-900 DEG C.SiO is prepared by step in example 1
2thin layer, obtains SiC Al
2o
3siO
2multilayer edge core-shell structure, wherein SiC content is 78-82%, Al
2o
3layer thickness is 30-100 nm, SiO
2thin film layer thickness is 5-10 nm.Then, the multilayer edge core-shell structure material of preparation and ethylene glycol and silica gel are carried out mechanical ball milling by 1:6-10:5-18 mass ratio, the obtained reflective glue of high heat conduction, high reverse--bias film is prepared on aluminium base surface by silk screen print method, chip is directly sticked on slurry according to circuit configuration, at 1 atmospheric pressure or heated under vacuum to 100-200 DEG C, form the high heat conduction of densification and the high reflectivity film of 20-40 um thickness.Conductive coefficient is 0.7-1.9 W/ (mk), is 94%-97% at the reflectivity of visible ray 400-700nm.
Compared with the existing technology, obtained nanometer has high heat conduction, high reflectance and excellent insulating properties to micron order insulation core-shell structure in the present invention, energy stable dispersion in silica gel simultaneously, the synthesis technique environmental protection of employing, simple, low cost; And propose a step package method namely print high reverse--bias thin layer while packaging LED chips, simplify module package step, improve the radiating efficiency of device.
Claims (8)
1. the preparation technology of the insulation core-shell structure of one kind high heat conduction high reflectance is as follows:
Step 1, carries out physical grinding and forms nuclear material powder by the one in SiC, AlN, BN and diamond;
Step 2, puts into 95% ethanolic solution by nuclear material powder and carries out ultrasonic cleaning purifying, forms core powder;
Step 3, it is in the precursor solution of 10-50% that core powder is dispersed in concentration range according to weight proportion 15-35%, ultrasonic disperse 1 hour, then precipitation reagent is added according to the ratio of 1:10 and 2:5, catalyst, stir 3-5 hour, dry at being then placed in drying box 60-100 DEG C, form composite material;
Step 4, calcines 5-6 hour, forms compound calcined materials at 500-900 DEG C by composite material;
Step 5, is placed on ultrasonic disperse 30-60 minute in mixed solution by compound calcined materials, drip 2-5ml tetraethoxysilane and 1-8ml ammoniacal liquor, magnetic agitation 6-10 hour, obtains high reflectance insulated compound core-shell material.
2. the preparation technology of the insulation core-shell structure of a kind of high heat conduction high reflectance according to claim 1, is characterized in that: described presoma is the one in aluminum nitrate, aluminium chloride, butyl titanate, zinc acetate, zinc nitrate.
3. the preparation technology of the insulation core-shell structure of a kind of high heat conduction high reflectance according to claim 1, is characterized in that: described precipitation reagent is the one in NaOH, ammoniacal liquor, diethanol amine, hydrochloric acid.
4. the preparation technology of the insulation core-shell structure of a kind of high heat conduction high reflectance according to claim 1, is characterized in that: described catalyst is the one in NaOH, ammoniacal liquor, diethanol amine, hydrochloric acid.
5. the preparation technology of the insulation core-shell structure of a kind of high heat conduction high reflectance according to claim 1, is characterized in that: described mixed solution is the deionized water of 1:5 and mixing of ethanol by volume ratio.
6. the preparation technology of the insulation core-shell structure of a kind of high heat conduction high reflectance according to claim 1, it is characterized in that: the conductive coefficient of described high reflectance insulated compound core-shell material is 0.5-3.0W/ (mk), the scope internal reflection rate being 400-700nm at visible ray light wave is 93%-98%, and voltage endurance is 2000V.
7. the application of the insulation core-shell structure of one kind high heat conduction high reflectance is as follows:
Step 1, carries out physical grinding by the high reflectance insulated compound core-shell material of preparation and ethylene glycol and silica gel by the mass ratio of 1:6-10:1-18, obtains composite mortar;
Step 2, slurry is pressed figure by silk screen printing or knife coating on aluminium base surface print, chip is directly sticked on slurry according to circuit configuration, at 1 atmospheric pressure or heated under vacuum to 100-200 DEG C, forms the high heat conduction high reflectivity film layer that thickness is 10-50 μm.
8. the preparations and applicatio of the insulation core-shell structure of a kind of high heat conduction high reflectance according to claim 7, it is characterized in that: described physical grinding is mechanical ball milling, be 8-15:16-30 mixing in mass ratio by composite mortar and agate ball, then under the rotating speed of 300-500 revolutions per second, carry out ball milling, Ball-milling Time is 1-4 hour.
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