CN106187207A - A kind of great power LED cooling aluminum nitride ceramic substrate of best bright finish - Google Patents
A kind of great power LED cooling aluminum nitride ceramic substrate of best bright finish Download PDFInfo
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- CN106187207A CN106187207A CN201610574145.1A CN201610574145A CN106187207A CN 106187207 A CN106187207 A CN 106187207A CN 201610574145 A CN201610574145 A CN 201610574145A CN 106187207 A CN106187207 A CN 106187207A
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- aluminum nitride
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- 239000000919 ceramic Substances 0.000 title claims abstract description 31
- 239000000758 substrate Substances 0.000 title claims abstract description 24
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 21
- 238000001816 cooling Methods 0.000 title claims abstract description 13
- 229910017083 AlN Inorganic materials 0.000 claims abstract description 22
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 239000002608 ionic liquid Substances 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium oxide Inorganic materials O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims abstract description 8
- PVADDRMAFCOOPC-UHFFFAOYSA-N oxogermanium Chemical compound [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000005083 Zinc sulfide Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- 229910052984 zinc sulfide Inorganic materials 0.000 claims abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 5
- 239000001301 oxygen Substances 0.000 claims abstract description 5
- 238000000498 ball milling Methods 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 230000033228 biological regulation Effects 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 238000007766 curtain coating Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 5
- 239000007767 bonding agent Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 239000012298 atmosphere Substances 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000000280 densification Methods 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- 238000005266 casting Methods 0.000 abstract 1
- 239000004615 ingredient Substances 0.000 abstract 1
- 229940068984 polyvinyl alcohol Drugs 0.000 description 5
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 5
- 230000005855 radiation Effects 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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Abstract
nullThe invention discloses the great power LED cooling aluminum nitride ceramic substrate of a kind of best bright finish，This ceramic substrate uses ionic liquid and deionized water to mix as solvent medium，Instead of the toxic organic solvents in traditional casting molding processes，Improve dispersibility and the associativity of each raw material，In addition the present invention is using aluminum Ludox polyvinyl alcohol colloidal sol as bonding agent，This bonding agent adhesive effect is good，Good to the wellability of each raw material，Effective ingredient therein can also reduce the oxygen content of sintering atmosphere，Improve aluminium nitride lattice degree of purity，The nano titanium oxide added、Nano-zinc sulfide、The raw materials such as germanium oxide can not only reduce aluminium nitride sintering temperature，Further improve the crystal structure of aluminium nitride ceramics，Obtain ceramic body densification bright and clean，Tough drop resistant，Mechanical property is improved，Improve the defect of aluminum nitride ceramic substrate transport difficult，There is good economic benefit.
Description
Technical field
The present invention relates to aluminium nitride ceramics technical field, particularly relate to the great power LED cooling nitridation of a kind of best bright finish
Aluminum ceramic substrate.
Background technology
The heat that high-power LED chip produces can not scatter and disappear timely and effectively, will have a strong impact on the emission spectrum of LED, sends out
Light intensity, encapsulating material performance, the life-span etc. of chip, therefore, the heat dissipation problem of great power LED is always solid state lighting industry
One big technical bottleneck, in the LED that conventional package technique produces, substrate heat radiation becomes domestic because of its most effective heat radiation advantage
The object of outer primary study.At present research application more for aluminum base heat-radiating substrate, but, along with the lifting of LED radiating requirements,
The defect of aluminium base the most progressively shows, and its internal insulating barrier causes integral heat sink poor, easy junction temperature, thus reduces lamp
The service life of tool.Compared to aluminium base heat radiation external member, ceramic heat-dissipating substrate has high-insulativity, high-heating radiation, high heat conduction, electricity
The advantages such as magnetic compatibility is good become a kind of substitution material got most of the attention, and wherein aluminium nitride ceramics is that combination property is ideal
Encapsulating material, but, there is sintering temperature height, the defects such as heat conductivility is poor in aluminium nitride ceramics in actual applications, governs
The popularization and application of product.
《Y2O3With nano-aluminum nitride synergism on aluminium nitride ceramics sintering character and the impact of conduction of heat " literary composition describe with
Y2O3Under sintering temperature and low, the aluminium nitride pottery of high thermal conductivity it is made for as sintering aid and nano aluminum nitride synergism
Porcelain, though a certain degree of consistency that improve aluminium nitride ceramics of this method, its heat conductivity still has much room for improvement, and
The addition of nano-powder must be needed to improve aluminium nitride ceramics under higher sintering temperature by strict control
Performance.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that the great power LED cooling of a kind of best bright finish
Aluminum nitride ceramic substrate.
The present invention is achieved by the following technical solutions:
The great power LED cooling aluminum nitride ceramic substrate of a kind of best bright finish, this ceramic substrate is by the raw material system of following weight portion
Become: aluminium nitride 40-50, nano aluminum nitride 12-15, germanium oxide 0.4-0.6, nano titanium oxide 1-2, nano-zinc sulfide 0.5-
0.8, yittrium oxide 2-3, polyvinyl alcohol 1-2, ionic liquid 10-15, aluminum isopropylate. 0.1-0.2, tetraethyl orthosilicate 0.4-0.5, go
Ionized water 20-25, appropriate dilute nitric acid solution.
The oxygen content of described aluminium nitride be 0.5-1.5wt.%, D50 particle diameter be 0.5-2 μm.
Described yittrium oxide purity is more than 99.99%, and D50 particle diameter is 0.1-0.5 μm.
Described ionic liquid is water soluble ion liquid.
The preparation method of the great power LED cooling aluminum nitride ceramic substrate of described a kind of best bright finish is divided into following
Step:
(1) first being mixed by the deionized water of aluminum isopropylate. with 8-10 weight portion, be placed under 90 DEG C of water bath condition, magnetic agitation is mixed
Closing, till the pH value of liquid to be mixed no longer changes, be subsequently added dilute nitric acid solution, regulation system pH value is 4.0-5.0, subsequently water
Bath is warming up to 100 DEG C, and it is standby that continuation backflow 1-1.5h obtains stable Alumina gel.
(2) tetraethyl orthosilicate is mixed with the deionized water of surplus, ultrasonic reaction 20-in the water-bath of 50-60 DEG C
30min, drips dilute nitric acid solution subsequently, and regulation solution ph is 4.0-5.0, obtains Ludox standby after reaction 40-50min.
(3) Alumina gel prepared by step (1) is heated to 80-85 DEG C, is slowly added to Ludox prepared by step (2), limit
Edged stirs, and adds polyvinyl alcohol subsequently, standby after continuing stirring mixing 40-50min.
(4) by nano aluminum nitride, nano titanium oxide, nano-zinc sulfide and ionic liquid mixing and ball milling 20-30min, with
After it is mixed with aluminium nitride, germanium oxide, yittrium oxide, continue ball milling dispersion 3-4h, the thing it prepared with step (3) the most again
Material mixing, again ball milling dispersion 10-15h, ball milling terminates rear gained slurry vacuum defoamation, and control viscosity is 5500-
6500mPa.s, gained slurry carries out curtain coating process, controls thickness, obtains idiosome.
(5) prepared idiosome is warming up to 350-400 DEG C with the heating rate of 1-2 DEG C/min on load bearing board, insulation row
Glue 5-6h, subsequently vacuum heat-preserving sintering 4-5h under the conditions of 1650 DEG C-1750 DEG C, after discharging and get final product.
The invention has the advantages that, use ionic liquid and deionized water to mix as solvent medium, instead of traditional stream
Prolong the toxic organic solvents in moulding process, improve dispersibility and the associativity of each raw material, in addition the present invention with aluminum Ludox-
Polyvinyl alcohol colloidal sol is as bonding agent, and this bonding agent adhesive effect is good, and good to the wellability of each raw material, therein have
Effect composition can also reduce the oxygen content of sintering atmosphere, improves aluminium nitride lattice degree of purity, and the nano titanium oxide of addition, nanometer vulcanize
The raw material such as zinc, germanium oxide can not only reduce aluminium nitride sintering temperature, further improves the crystal structure of aluminium nitride ceramics, obtains pottery
Body densification is bright and clean, tough drop resistant, and mechanical property is improved, and improves the defect of aluminum nitride ceramic substrate transport difficult, has
Good economic benefit.
Detailed description of the invention
The great power LED cooling aluminum nitride ceramic substrate of a kind of best bright finish, this ceramic substrate is former by following weight portion
Material is made: aluminium nitride 40, nano aluminum nitride 12, germanium oxide 0.4, nano titanium oxide 1, nano-zinc sulfide 0.5, yittrium oxide 2, poly-
Vinyl alcohol 1, ionic liquid 10, aluminum isopropylate. 0.1, tetraethyl orthosilicate 0.4, deionized water 20, appropriate dilute nitric acid solution.
Wherein the oxygen content of aluminium nitride be 0.5wt.%, D50 particle diameter be 0.5 μm.
Wherein yittrium oxide purity is more than 99.99%, and D50 particle diameter is 0.1 μm.
Wherein ionic liquid is water soluble ion liquid.
This embodiment ceramic substrate is prepared by following step:
(1) first being mixed by the deionized water of aluminum isopropylate. and 8 weight portions, be placed under 90 DEG C of water bath condition, magnetic agitation mixes, and treats
Till the pH value of mixed liquor no longer changes, being subsequently added dilute nitric acid solution, regulation system pH value is 4.0, and warming-in-water is extremely subsequently
100 DEG C, it is standby that continuation backflow 1h obtains stable Alumina gel.
(2) tetraethyl orthosilicate is mixed with the deionized water of surplus, ultrasonic reaction 20min in the water-bath of 50 DEG C, subsequently
Dropping dilute nitric acid solution, regulation solution ph is 4.0, obtains Ludox standby after reaction 40min.
(3) Alumina gel prepared by step (1) is heated to 80 DEG C, is slowly added to Ludox prepared by step (2), limit edged
Stirring, adds polyvinyl alcohol subsequently, standby after continuing stirring mixing 40min.
(4) by nano aluminum nitride, nano titanium oxide, nano-zinc sulfide and ionic liquid mixing and ball milling 20min, subsequently will
It mixes with aluminium nitride, germanium oxide, yittrium oxide, continues ball milling dispersion 3h, is mixed by the material that itself and step (3) prepare
Closing, again ball milling dispersion 10h, ball milling terminates rear gained slurry vacuum defoamation, and control viscosity is 6000mPa.s, and gained slurry enters
Row curtain coating processes, and obtains the idiosome that thickness is 0.55mm.
(5) prepared idiosome is warming up to 350 DEG C with the heating rate of 1 DEG C/min on load bearing board, is incubated binder removal 5h, with
After under the conditions of 1700 DEG C vacuum heat-preserving sintering 4h, after discharging and get final product.
The property indices that this ceramic substrate obtains according to respective standard test is as follows:
Density: 3.20g.cm-3；Thermal conductivity: 175.5W/ (mk)；Surface roughness Rmax≤0.1μm；Bending strength: 389MPa；
Fracture toughness: 3.0 ± 0.05MPa.m1/2。
Claims (5)
1. the great power LED cooling aluminum nitride ceramic substrate of a best bright finish, it is characterised in that this ceramic substrate is by following heavy
The raw material of amount part is made: aluminium nitride 40-50, nano aluminum nitride 12-15, germanium oxide 0.4-0.6, nano titanium oxide 1-2, nanometer
Zinc sulfide 0.5-0.8, yittrium oxide 2-3, polyvinyl alcohol 1-2, ionic liquid 10-15, aluminum isopropylate. 0.1-0.2, tetraethyl orthosilicate
0.4-0.5, deionized water 20-25, appropriate dilute nitric acid solution.
The great power LED cooling aluminum nitride ceramic substrate of a kind of best bright finish the most as claimed in claim 1, it is characterised in that
The oxygen content of described aluminium nitride be 0.5-1.5wt.%, D50 particle diameter be 0.5-2 μm.
The great power LED cooling aluminum nitride ceramic substrate of a kind of best bright finish the most as claimed in claim 1, it is characterised in that
Described yittrium oxide purity is more than 99.99%, and D50 particle diameter is 0.1-0.5 μm.
The great power LED cooling aluminum nitride ceramic substrate of a kind of best bright finish the most as claimed in claim 1, it is characterised in that
Described ionic liquid is water soluble ion liquid.
The preparation method of the great power LED cooling aluminum nitride ceramic substrate of a kind of best bright finish the most as claimed in claim 1 is divided
For following step:
(1) first being mixed by the deionized water of aluminum isopropylate. with 8-10 weight portion, be placed under 90 DEG C of water bath condition, magnetic agitation is mixed
Closing, till the pH value of liquid to be mixed no longer changes, be subsequently added dilute nitric acid solution, regulation system pH value is 4.0-5.0, subsequently water
Bath is warming up to 100 DEG C, and it is standby that continuation backflow 1-1.5h obtains stable Alumina gel；
(2) tetraethyl orthosilicate is mixed with the deionized water of surplus, ultrasonic reaction 20-30min in the water-bath of 50-60 DEG C, with
Rear dropping dilute nitric acid solution, regulation solution ph is 4.0-5.0, obtains Ludox standby after reaction 40-50min；
(3) Alumina gel prepared by step (1) is heated to 80-85 DEG C, is slowly added to Ludox prepared by step (2), limit edged
Stirring, adds polyvinyl alcohol subsequently, standby after continuing stirring mixing 40-50min；
(4) by nano aluminum nitride, nano titanium oxide, nano-zinc sulfide and ionic liquid mixing and ball milling 20-30min, subsequently will
It mixes with aluminium nitride, germanium oxide, yittrium oxide, continues ball milling dispersion 3-4h, is mixed by the material that itself and step (3) prepare
Closing, again ball milling dispersion 10-15h, ball milling terminates rear gained slurry vacuum defoamation, and control viscosity is 5500-6500mPa.s, institute
Obtain slurry and carry out curtain coating process, control thickness, obtain idiosome；
(5) prepared idiosome is warming up to 350-400 DEG C with the heating rate of 1-2 DEG C/min on load bearing board, is incubated binder removal 5-
6h, subsequently vacuum heat-preserving sintering 4-5h under the conditions of 1650 DEG C-1750 DEG C, after discharging and get final product.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110350072A (en) * | 2019-06-25 | 2019-10-18 | 宁夏万泰照明科技股份有限公司 | A kind of preparation method of flip LED |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104387044A (en) * | 2014-10-29 | 2015-03-04 | 安徽省皖捷液压科技有限公司 | Germanium-oxide-containing ceramic and preparation method thereof |
| CN105384441A (en) * | 2015-10-27 | 2016-03-09 | 合肥龙多电子科技有限公司 | Nano-titania-toughened high-density aluminum nitride-silicon carbide composite circuit board substrate material and preparation method therefor |
-
2016
- 2016-07-20 CN CN201610574145.1A patent/CN106187207A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104387044A (en) * | 2014-10-29 | 2015-03-04 | 安徽省皖捷液压科技有限公司 | Germanium-oxide-containing ceramic and preparation method thereof |
| CN105384441A (en) * | 2015-10-27 | 2016-03-09 | 合肥龙多电子科技有限公司 | Nano-titania-toughened high-density aluminum nitride-silicon carbide composite circuit board substrate material and preparation method therefor |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110350072A (en) * | 2019-06-25 | 2019-10-18 | 宁夏万泰照明科技股份有限公司 | A kind of preparation method of flip LED |
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