CN102368518B - A kind of simple nanoscale PSS substrate fabrication method - Google Patents
A kind of simple nanoscale PSS substrate fabrication method Download PDFInfo
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- CN102368518B CN102368518B CN201110330647.7A CN201110330647A CN102368518B CN 102368518 B CN102368518 B CN 102368518B CN 201110330647 A CN201110330647 A CN 201110330647A CN 102368518 B CN102368518 B CN 102368518B
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- 239000000758 substrate Substances 0.000 title claims abstract description 41
- 229920001467 poly(styrenesulfonates) Polymers 0.000 title claims abstract description 20
- 201000009594 systemic scleroderma Diseases 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 58
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 23
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 23
- 229910052904 quartz Inorganic materials 0.000 claims abstract description 23
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 23
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 23
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 18
- 239000010980 sapphire Substances 0.000 claims abstract description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000137 annealing Methods 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 7
- 239000001117 sulphuric acid Substances 0.000 claims abstract description 7
- 235000011149 sulphuric acid Nutrition 0.000 claims abstract description 7
- 230000000694 effects Effects 0.000 claims abstract description 6
- 238000005260 corrosion Methods 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 238000001312 dry etching Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 9
- 239000008187 granular material Substances 0.000 claims description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N HF Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000005530 etching Methods 0.000 claims description 4
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 7
- 239000002253 acid Substances 0.000 abstract 1
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 5
- 238000000605 extraction Methods 0.000 description 4
- 229920000069 poly(p-phenylene sulfide) Polymers 0.000 description 4
- 229910002601 GaN Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 241001025261 Neoraja caerulea Species 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000875 corresponding Effects 0.000 description 1
- 238000000609 electron-beam lithography Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 235000005035 ginseng Nutrition 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000001127 nanoimprint lithography Methods 0.000 description 1
- TWXTWZIUMCFMSG-UHFFFAOYSA-N nitride(3-) Chemical compound [N-3] TWXTWZIUMCFMSG-UHFFFAOYSA-N 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
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- 229910010271 silicon carbide Inorganic materials 0.000 description 1
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Abstract
The open a kind of simple nanoscale PSS substrate fabrication method of the present invention, one layer of SiO of deposition on a sapphire substrate2Film, at SiO2Film one layer of ITO or ZnO of deposition, by high annealing, makes ITO or ZnO film produce agglomeration, and annealing temperature height changes SiO2On film, ITO or the size of ZnO particle and distributed degrees, fall the SiO not blocked by ITO or ZnO particle with dry etching2Film, so uniform ITO or ZnO nano grain pattern transfer to SiO2Film layer, is then placed in sulphuric acid and corrosion or the dry etching in phosphoric acid mixed solution of high temperature, again by the SiO of even level2Grain pattern is transferred in Sapphire Substrate, finally removes SiO with HF acid2Mask, thus form nanoscale PSS substrate.This invention can improve the outer quantum effect of LED chip, and processing technology is simple, low cost, production high efficiency.
Description
Technical field
The present invention relates to a kind of LED substrate manufacture method, especially a kind of simple nanoscale PSS substrate fabrication method.
Background technology
Light emitting diode (LED) is the advantages such as a kind of electro-optic conversion, energy-efficient, environmental protection, life-span length, refers in traffic
Show, indoor and outdoor total colouring, the aspect such as LCD TV backlight source have a wide range of applications, and especially can realize partly leading with LED
Body solid-state illumination, it is expected to become a new generation's light source and enters huge numbers of families, causes the mankind to illuminate the revolution in history, wherein sapphire
Applying yellow fluorescent powder on the blue-light LED chip of substrate growth epitaxy of gallium nitride, blue light excitated fluorescent powder sends gold-tinted, blue light with
Gold-tinted is mixed to get white light, thus obtains white light with blue-ray LED.Gallium nitride substrate material is common two kinds, i.e. sapphire and carbon
SiClx, carborundum machining property is poor, and the problem in terms of expensive and patent makes it apply to be limited, the most currently
Substrate for GaN epitaxial growth is mainly sapphire, and epitaxial layer of gallium nitride and sapphire lattice mismatch are quite big,
Residualinternal stress is relatively big, so growing gallium nitride easily causes substantial amounts of defect on sapphire, and these defects are substantially reduced
Luminescent device luminous efficiency；There is the difference of bigger refractive index between GaN and air, light shooting angle is less simultaneously, the biggest portion
Dividing is totally reflected back to inside LED chip, reduces the extraction efficiency of light, increases heat radiation difficulty, affects the reliable of LED component
Property.Employing nanoscale PPS substrate technology can be substantially reduced the density of the dislocation of nitride material, produces when relaxing epitaxial growth
Residualinternal stress, improves internal quantum efficiency, and light extraction efficiency is substantially improved.
Realize nanoscale PPS substrate technology at present mainly to use: electron beam lithography, nano imprint lithography, poly-
Compound photoetching technique；Above technology processed complex, cost are high.
Summary of the invention
It is an object of the invention to provide a kind of nanoscale PPS substrate manufacture method, its processing procedure is simple, quick, low cost,
Photon extraction efficiency is high, improving product yield.
The technical scheme is that a kind of simple nanoscale PSS substrate fabrication method, preparation process is as follows:
A, Sapphire Substrate (see Fig. 1-A) one layer of SiO of upper deposition2Film；Deposit by PECVD device in step Sapphire Substrate
One layer of SiO2Film, thickness 2000～5000 angstroms, see Fig. 1-B.
B, at SiO2Deposit one layer of ITO or ZnO, thickness 1000～3000 angstroms on film, see Fig. 1-C.
C, the substrate of step b one layer of ITO or ZnO of deposition is put in the annealing furnace of 300～600 DEG C, carry out annealing 0.5～
2 hours, SiO2Generate uniform ITO or ZnO crystal grain on film surface, see Fig. 1-D.
D, after c step annealing effect, re-use RIE equipment, etch away the SiO failing to be blocked by ITO or ZnO particle2Film,
Uniform nanometer shape ITO or ZnO particle figure is made to transfer to SiO2Film layer, forms the SiO of nanometer shape2Granule.The ginseng of RIE etching
Number is: CF4: 30～60sccm；Reaction pressure: 20～100mTorr；Power: 300～500W, etch period: 10～30 minutes.
See Fig. 1-E.
E, the sulphuric acid placing into 230～350 DEG C of temperature after Step d and H in phosphoric acid mixed solution2SO4:H3PO4=3:1
Corrode about 10～30 minutes, erode not by SiO2The Sapphire Substrate that granule blocks, is shown in Fig. 1-F.
F, after step e with HF acid corrosion 10～30 minutes, remove SiO2Mask, formed nanoscale PSS substrate, see Fig. 1-
G。
It is an advantage of the current invention that: its processing procedure requires relatively low relative to conventional PSS technology, its technology, and etching speed is fast；
Exempting and fall expensive lithographic equipment, processing cost reduction is a lot；And relative to non-PSS processing procedure, this processing procedure is formed on sapphire
Pit pattern be conducive to growing high-quality epitaxial layer of gallium nitride, be conducive to improve outer quantum effect；LED inspires simultaneously
Light reflect at these pit pattern, scattered light can be formed, be conducive to increasing light extraction efficiency.
Accompanying drawing explanation
Fig. 1 is one nanoscale PSS substrate preparation method structural representation of the present invention
P1: sapphire；
P2:SiO2Film；
P3:ITO or ZnO；
The substrat structure pattern of A～G: processing procedure corresponding steps.
Detailed description of the invention
Figure 1A～G display present invention forms nanoscale PPS substrate implementing procedure in emitting components；
Step 1: deposit one layer of SiO in Sapphire Substrate2Film；
Step 2: at SiO2One layer of ITO or ZnO film is deposited on film；
Step 3: the substrate of one layer of ITO or ZnO of deposition is put in annealing furnace and annealed, SiO2Generate uniformly on film surface
ITO or ZnO crystal grain
Step 4: after c step annealing effect, then dry etching falls the SiO failing to be blocked by ITO or ZnO particle2Film, will be all
ITO or the ZnO particle figure of even nanometer shape transfer to SiO2Film layer；, form the SiO of nanometer shape2Granule；
Step 5: the sulphuric acid placing into high temperature after Step d erodes not by SiO in phosphoric acid mixed solution2Granule blocks
Blue precious substrate；
Step 6: remove SiO with HF acid after step e2Mask, forms nanoscale PSS substrate.
Embodiment 1
One layer of SiO is deposited the most on a sapphire substrate by PECVD device2Film, thickness about 2000～5000 angstroms；
Then at SiO2One layer of ITO or ZnO film, thickness about 1000～3000 angstroms is deposited on film；Annealing furnace temperature 300～
600 DEG C of annealing 0.5 to ITO or ZnO film～2 hours, at SiO2Generate on film surface uniform ITO or ZnO crystal grain (80～
300 angstroms)；Then with RIE equipment (parameter: CF4: 30～60sccm；Reaction pressure: 20～100mTorr；Power: 300～
500W, etch period: 10～30 minutes), then with sulphuric acid and phosphoric acid mixed volume ratio: 3:1；Mixing of temperature (230～350 DEG C)
Close in solution and corrode 10～30 minutes；Finally with HF acid corrosion SiO2Mask 10～30 minutes.
Claims (7)
1. a simple nanoscale PSS substrate fabrication method, preparation process is as follows:
One layer of SiO is deposited in (a) Sapphire Substrate2Film；
B () is at SiO2One layer of ITO or ZnO is deposited on film；
C the substrate of step b one layer of ITO or ZnO of deposition is put in annealing furnace by (), anneal, SiO2Generate uniformly on film surface
ITO or ZnO crystal grain；
D () is after c step annealing effect, then dry etching falls the SiO failing to be blocked by ITO or ZnO particle2Film, by uniform nanometer
ITO or the ZnO particle figure of shape transfer to SiO2Film layer, forms the SiO of nanometer shape2Granule；
E () places into sulphuric acid after Step d and erodes not by SiO in phosphoric acid mixed solution2The Sapphire Substrate that granule blocks；
F () removes SiO with HF acid after step e2Mask, forms nanoscale PSS substrate.
Simple nanoscale PSS substrate fabrication method the most according to claim 1, it is characterised in that: (a) step sapphire serves as a contrast
One layer of SiO is deposited by PECVD device at the end2Film, thickness 2000～5000 angstroms.
Simple nanoscale PSS substrate fabrication method the most according to claim 1, it is characterised in that: (b) step is at SiO2Film
One layer of ITO or ZnO of upper evaporation, thickness 1000～3000 angstroms.
Simple nanoscale PSS substrate fabrication method the most according to claim 1, it is characterised in that: (c) step is by step b
The substrate 300 of one layer of ITO or ZnO of evaporation～600 DEG C of annealing furnaces carry out annealing 0.5～2 hour, SiO2Generate all on film surface
Even ITO or ZnO crystal grain.
Simple nanoscale PSS substrate fabrication method the most according to claim 1, it is characterised in that: (d) is at step c chemistry
After effect, re-use RIE equipment, etch away the SiO failing to be blocked by ITO or ZnO particle2Film, make uniform nanometer shape ITO or
ZnO particle figure transfers to SiO2Film layer, forms the SiO of nanometer shape2Granule；The parameter of RIE etching is: CF4: 30～60sccm；
Reaction pressure: 20～100mTorr；Power: 300～500W, etch period: 10～30 minutes.
Simple nanoscale PSS substrate fabrication method the most according to claim 1, it is characterised in that: (e) after Step d again
Put into sulphuric acid to erode not by SiO in phosphoric acid mixed solution2The Sapphire Substrate that granule blocks；Its sulphuric acid mixes molten with phosphoric acid
The proportioning of liquid is: H2SO4:H3PO4=3:1；Its corrosion temperature is 230～350 DEG C；Its etching time is 10～30 minutes.
Simple nanoscale PSS substrate fabrication method the most according to claim 1, it is characterised in that: (f) uses after step e
HF acid corrosion 10～30 minutes, remove SiO2Mask, forms nanoscale PSS substrate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110330647.7A CN102368518B (en) | 2011-10-27 | A kind of simple nanoscale PSS substrate fabrication method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110330647.7A CN102368518B (en) | 2011-10-27 | A kind of simple nanoscale PSS substrate fabrication method |
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| CN102368518A CN102368518A (en) | 2012-03-07 |
| CN102368518B true CN102368518B (en) | 2016-12-14 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6844569B1 (en) * | 2003-12-20 | 2005-01-18 | Samsung Electro-Mechanics Co., Ltd. | Fabrication method of nitride-based semiconductors and nitride-based semiconductor fabricated thereby |
| CN101159307A (en) * | 2007-11-16 | 2008-04-09 | 北京工业大学 | Emitting surface semiconductor LED with nanostructure and its preparing process |
| CN101456579A (en) * | 2008-12-05 | 2009-06-17 | 天津大学 | Method for synthesizing zinc oxide nano tube array by low-temperature hydrothermal method |
| CN101740702A (en) * | 2009-12-02 | 2010-06-16 | 武汉华灿光电有限公司 | ZnO nanosphere-based GaN-based light emitting diode surface roughening method |
| CN102184842A (en) * | 2011-03-30 | 2011-09-14 | 华灿光电股份有限公司 | Method for patterning sapphire by combining wet etching and dry etching |
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6844569B1 (en) * | 2003-12-20 | 2005-01-18 | Samsung Electro-Mechanics Co., Ltd. | Fabrication method of nitride-based semiconductors and nitride-based semiconductor fabricated thereby |
| CN101159307A (en) * | 2007-11-16 | 2008-04-09 | 北京工业大学 | Emitting surface semiconductor LED with nanostructure and its preparing process |
| CN101456579A (en) * | 2008-12-05 | 2009-06-17 | 天津大学 | Method for synthesizing zinc oxide nano tube array by low-temperature hydrothermal method |
| CN101740702A (en) * | 2009-12-02 | 2010-06-16 | 武汉华灿光电有限公司 | ZnO nanosphere-based GaN-based light emitting diode surface roughening method |
| CN102184842A (en) * | 2011-03-30 | 2011-09-14 | 华灿光电股份有限公司 | Method for patterning sapphire by combining wet etching and dry etching |
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