CN102097548B - Method for preparing self-supported GaN-based light emitting diode - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 8
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 28
- 239000010980 sapphire Substances 0.000 claims abstract description 28
- 239000000758 substrate Substances 0.000 claims abstract description 25
- 238000009792 diffusion process Methods 0.000 claims abstract description 20
- 238000007747 plating Methods 0.000 claims abstract description 15
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 13
- 230000007704 transition Effects 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 7
- 230000007797 corrosion Effects 0.000 claims abstract description 6
- 238000005260 corrosion Methods 0.000 claims abstract description 6
- 239000011248 coating agent Substances 0.000 claims description 26
- 238000000576 coating method Methods 0.000 claims description 26
- 238000002360 preparation method Methods 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000011065 in-situ storage Methods 0.000 claims description 5
- 238000012856 packing Methods 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000005855 radiation Effects 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract 2
- 229910044991 metal oxide Inorganic materials 0.000 abstract 1
- 150000004706 metal oxides Chemical class 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 9
- 238000009413 insulation Methods 0.000 description 8
- HQWPLXHWEZZGKY-UHFFFAOYSA-N diethylzinc Chemical compound CC[Zn]CC HQWPLXHWEZZGKY-UHFFFAOYSA-N 0.000 description 6
- 239000010409 thin film Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 3
- 238000005286 illumination Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
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Abstract
The invention relates to a method for preparing a self-supported GaN-based light emitting diode, which comprises the steps: based on the adoption of a metal-oxide chemical vapor deposition method, growing a ZnO buffer layer, a ZnO epitaxial and a GaN anticorrosive layer in sequence on a sapphire substrate at first to form a composite substrate; then growing a GaN or AlN buffer layer, a non-doped GaN transition layer, a n-type GaN epitaxial layer, a GaN/InGaN multi-quantuam-well light emitting layer, a p-type GaN epitaxial layer and a current diffusion layer in sequence on the composite substrate, plating a p-type GaN contact electrode on the current diffusion layer, and plating a n-type GaN contact electrode on the n-type GaN epitaxial layer in parallel to the GaN/InGaN multi-quantuam-well light emitting layer; and finally, peeling off the sapphire layer, the ZnO buffer layer, the ZnO epitaxial layer and the GaN anticorrosive layer by means of an acid liquor corrosion method. By using the method, radiation prominently can be improved and the light-emitting device with large power and high brightness can be obtained, and simultaneously, sapphires can be recovered and reused, which is beneficial for lowering production cost.
Description
Technical field
The present invention relates to a kind of preparation method of self-supporting GaN based light-emitting diode, belong to technical field of semiconductor luminescence.
Background technology
The GaN based light-emitting diode has important application prospects and commercial value in fields such as illumination, demonstration, scientific researches.Traditional G aN based light-emitting diode structure is as shown in Figure 1; Generally with sapphire sheet 201 as substrate; Adopt Metalorganic Chemical Vapor Deposition growing GaN or AlN resilient coating 202, non-Doped GaN transition zone 203, n type GaN epitaxial loayer 204, GaN/InGaN multiple quantum well light emitting layer 205 successively from bottom to top on substrate; P type GaN epitaxial loayer 206 and current-diffusion layer 207; And on current-diffusion layer 207, plate p type GaN contact electrode 208, on n type GaN epitaxial loayer 204, be listed in GaN/InGaN multiple quantum well light emitting layer 205 plating n type GaN contact electrode 209.
Because Sapphire Substrate has big gap at crystal structure, thermal conductivity and GaN, is easy to generate lattice mismatch and thermal stress mismatch, because the sapphire insulation and thermal insulation is functional, is unfavorable for making the high-power light-emitting device simultaneously.Sapphire Substrate must be cut after element manufacturing was accomplished, thereby accomplished follow-up packaging technology, caused Sapphire Substrate to reuse.In sum, simple Sapphire Substrate can not satisfy the preparation requirement of the high-power GaN based light-emitting diode of high-performance.
Undoubtedly, the GaN monocrystalline is the best substrate of preparation GaN base luminescent device.Yet GaN single-chip diameter is very little and cost an arm and a leg.ZnO has a lot of similar character with GaN at aspects such as crystal structure, band structures; Particularly importantly both are wurtzite structure; Have identical stacking sequence, lattice mismatch and thermal mismatching are very little simultaneously, so ZnO can be used as the template of GaN base film growth.Since with respect to GaN, the ZnO abundant raw material, cheap, be easy to corrosion, in conjunction with having the technology that Sapphire Substrate prepares the GaN base luminescent device now, can realize peeling off of GaN base film and substrate easily, thus the good high-power and high-luminance device of preparation heat radiation.
Realize above-mentioned technical two major issues that need to solve that are envisaged in: the first, for suitability for industrialized production, the selling at exorbitant prices of ZnO monocrystalline; The second, in GaN outer layer growth temperature and ammonia atmosphere, the ZnO layer is corroded easily and influences the crystal mass of subsequent growth film.So adopting ZnO single crystalline substrate or metal organic chemical vapor deposition parameter commonly used to be not suitable for growing with ZnO is the GaN based light-emitting diode of transition zone.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of self-supporting GaN based light-emitting diode, improve the heat radiation of luminescent device, be easy to obtain high-power, high brightness light-emitting devices, and can effectively reduce production cost.
The preparation method of the GaN based light-emitting diode of self-supporting of the present invention; The GaN based light-emitting diode of this self-supporting has GaN or AlN resilient coating, non-Doped GaN transition zone, n type GaN epitaxial loayer, GaN/InGaN multiple quantum well light emitting layer from bottom to top successively on the GaN etch resistant layer; P type GaN epitaxial loayer and current-diffusion layer; And on current-diffusion layer plating p type GaN contact electrode; On n type GaN epitaxial loayer, be listed in GaN/InGaN multiple quantum well light emitting layer plating n type GaN contact electrode, what its preparation was adopted is Metalorganic Chemical Vapor Deposition, and step is following:
1) Sapphire Substrate that will the pass through cleaning metal organic chemical vapor deposition device reaction chamber of packing into vacuumizes, at 250-400 ℃; Organic zinc source flow 5-100sccm; The purity oxygen flow is 10-200sccm, and air pressure is 0.01-150Torr, and growth thickness is the ZnO resilient coating of 0.1-1 micron;
2) with the step 1) goods at 700-800 ℃ of in-situ annealing 10-30 minute; In 400-600 ℃, organic zinc source flow 5-100sccm, purity oxygen flow are 10-200sccm then; Air pressure is 0.01-150Torr, and growth thickness is the ZnO epitaxial loayer of 0.5-30 micron on the ZnO resilient coating;
3) at 600-800 ℃, the organic gallium source flow is 5-100sccm, and the flow of pure ammonia is 100-2000sccm, and air pressure is 10-200Torr, and growth thickness is the GaN etch resistant layer of 0.1-1 micron on the ZnO epitaxial loayer;
4) on the compound substrate that above-mentioned sapphire, ZnO resilient coating, ZnO epitaxial loayer and GaN etch resistant layer constitute; Growing GaN or AlN resilient coating, non-Doped GaN transition zone, n type GaN epitaxial loayer, GaN/InGaN multiple quantum well light emitting layer successively; P type GaN epitaxial loayer and current-diffusion layer; And on current-diffusion layer, plate p type GaN contact electrode, on n type GaN epitaxial loayer, be listed in GaN/InGaN multiple quantum well light emitting layer plating n type GaN contact electrode;
5) adopt the acid solution chemical corrosion method, Sapphire Substrate, ZnO resilient coating and ZnO epitaxial loayer and GaN etch resistant layer are peeled off, obtain the GaN based light-emitting diode of self-supporting.
The used acid solution of above-mentioned acid solution chemical corrosion is nitric acid, phosphoric acid or the hydrofluoric acid of pH >=4.
Beneficial effect of the present invention is: it is that transition zone is made the GaN based light-emitting diode with the ZnO monocrystal thin films that the present invention has designed a kind of; Through obtaining the GaN based light-emitting diode of self-supporting at the bottom of the peeling liner; Can significantly improve heat radiation; Obtain high-power, high brightness light-emitting devices, sapphire sheet can reclaim repeated use simultaneously.The present invention is good to existing production technology compatibility, not only can significantly improve the performance of device, and help reducing production costs.
Description of drawings
Fig. 1 is present common preparation GaN based light-emitting diode structural representation;
Fig. 2 is a GaN based light-emitting diode structural representation of the present invention;
Fig. 3 is that GaN based light-emitting diode of the present invention prepares each layer sketch map in the process.
Embodiment
Be described in detail the present invention below in conjunction with accompanying drawing and embodiment.
Self-supporting GaN based light-emitting diode of the present invention is as shown in Figure 2; GaN or AlN resilient coating 202, non-Doped GaN transition zone 203, n type GaN epitaxial loayer 204, GaN/InGaN multiple quantum well light emitting layer 205 are arranged on GaN etch resistant layer 104 from bottom to top successively; P type GaN epitaxial loayer 206 and current-diffusion layer 207; And on current-diffusion layer 207 plating p type GaN contact electrode 208; On n type GaN epitaxial loayer 204, be listed in GaN/InGaN multiple quantum well light emitting layer 205 plating n type GaN contact electrode 209, its preparation process is referring to Fig. 3.
Embodiment 1.
1) the polishing Sapphire Substrate 101 that will the pass through cleaning metal organic chemical vapor deposition device reaction chamber of packing into; Vacuumize; At 250 ℃, diethyl zinc (purity >=99.9999%) flow 5sccm, oxygen (purity >=99.999%) flow is 10sccm; Air pressure is 0.01Torr, and growth thickness is 0.1 micron a ZnO resilient coating 102;
2) will grow good ZnO resilient coating 102 700 ℃ of in-situ annealing 30 minutes; Then at 400 ℃, diethyl zinc (purity >=99.9999%) flow 5sccm, oxygen (purity >=99.999%) flow is 10sccm; Air pressure is 0.01Torr, and growth thickness is 0.5 micron a ZnO epitaxial loayer 103;
3) at 600 ℃, trimethyl gallium (purity >=99.9999%) flow is 5sccm, and the flow of ammonia (purity >=99.9997%) is 100sccm, and air pressure is 10Torr, and growth thickness is 0.01 micron a GaN etch resistant layer 104 on ZnO epitaxial loayer 103;
4) adopt Metalorganic Chemical Vapor Deposition traditional processing technology growing GaN resilient coating 202, non-Doped GaN transition zone 203, n type GaN epitaxial loayer 204, GaN/InGaN multiple quantum well light emitting layer 205 successively; P type GaN epitaxial loayer 206 and current-diffusion layer 207; And on current-diffusion layer 207, plate p type GaN contact electrode 208, on n type GaN epitaxial loayer 204, be listed in GaN/InGaN multiple quantum well light emitting layer 205 plating n type GaN contact electrode 209.
5) configuration PH >=4 salpeter solutions; Its liquid level of solution is lower than the upper surface of GaN etch resistant layer 104; Corroded above-mentioned device 5 minutes; Sapphire sheet 101, ZnO resilient coating 102 and ZnO epitaxial loayer 103 are peeled off with topmost thin film, obtained the GaN based light-emitting diode of self-supporting, and the recovery sapphire reuses.
The GaN based light-emitting diode of self-supporting is because the sapphire that does not have insulation and thermal insulation as substrate, is easy to obtain photoelectric properties high-power, high brightness.The power of the GaN based light-emitting diode that obtains through above-mentioned technology is greater than 1W, and efficient is than commercial equal power product is high by 20% at present.
Embodiment 2.
1) the polishing Sapphire Substrate 101 that will the pass through cleaning metal organic chemical vapor deposition device reaction chamber of packing into; Vacuumize; At 350 ℃, diethyl zinc (purity >=99.9999%) flow 50sccm, oxygen (purity >=99.999%) flow is 100sccm; Air pressure is 75Torr, and growth thickness is 0.5 micron a ZnO resilient coating 102;
2) will grow good ZnO resilient coating 102 800 ℃ of in-situ annealing 20 minutes; Then at 500 ℃, diethyl zinc (purity >=99.9999%) flow 50sccm, oxygen (purity >=99.999%) flow is 100sccm; Air pressure is 50Torr, and growth thickness is 10 microns a ZnO epitaxial loayer 103;
3) at 700 ℃, trimethyl gallium (purity >=99.9999%) flow is 50sccm, and the flow of ammonia (purity >=99.9997%) is 1000sccm, and air pressure is 100Torr, and growth thickness is 0.5 micron a GaN etch resistant layer 104 on ZnO epitaxial loayer 103;
4) adopt Metalorganic Chemical Vapor Deposition traditional processing technology growing GaN resilient coating 202, non-Doped GaN transition zone 203, n type GaN epitaxial loayer 204, GaN/InGaN multiple quantum well light emitting layer 205 successively; P type GaN epitaxial loayer 206 and current-diffusion layer 207; And on current-diffusion layer 207, plate p type GaN contact electrode 208, on n type GaN epitaxial loayer 204, be listed in GaN/InGaN multiple quantum well light emitting layer 205 plating n type GaN contact electrode 209.
5) configuration PH >=4 hydrofluoric acid solutions; Its liquid level of solution is lower than the upper surface of GaN etch resistant layer 104; Corroded above-mentioned device 10 minutes; Sapphire sheet 101, ZnO resilient coating 102 and ZnO epitaxial loayer 103 are peeled off with topmost thin film, obtained the GaN based light-emitting diode of self-supporting, and the recovery sapphire reuses.
The GaN based light-emitting diode of self-supporting is because the sapphire that does not have insulation and thermal insulation as substrate, is easy to obtain photoelectric properties high-power, high brightness.The power of the GaN based light-emitting diode that obtains through above-mentioned technology is greater than 1W, and efficient is than commercial equal power product is high by 20% at present.
Embodiment 3
1) the polishing Sapphire Substrate 101 that will the pass through cleaning metal organic chemical vapor deposition device reaction chamber of packing into; Vacuumize; At 400 ℃, diethyl zinc (purity >=99.9999%) flow 100sccm, oxygen (purity >=99.999%) flow is 200sccm; Air pressure is 150Torr, and growth thickness is 1 micron a ZnO resilient coating 102;
2) will grow good ZnO resilient coating 102 800 ℃ of in-situ annealing 30 minutes; Then at 600 ℃, diethyl zinc (purity >=99.9999%) flow 100sccm, oxygen (purity >=99.999%) flow is 200sccm; Air pressure is 150Torr, and growth thickness is 30 microns a ZnO epitaxial loayer 103;
3) at 800 ℃, trimethyl gallium (purity >=99.9999%) flow is 100sccm, and the flow of ammonia (purity >=99.9997%) is 2000sccm, and air pressure is 200Torr, and growth thickness is 1 micron a GaN etch resistant layer 104 on ZnO epitaxial loayer 103;
4) adopt Metalorganic Chemical Vapor Deposition traditional processing technology growing AIN resilient coating 202, non-Doped GaN transition zone 203, n type GaN epitaxial loayer 204, GaN/InGaN multiple quantum well light emitting layer 205 successively; P type GaN epitaxial loayer 206 and current-diffusion layer 207; And on current-diffusion layer 207, plate p type GaN contact electrode 208, on n type GaN epitaxial loayer 204, be listed in GaN/InGaN multiple quantum well light emitting layer 205 plating n type GaN contact electrode 209.
5) configuration PH >=4 phosphoric acid solutions; Its liquid level of solution is lower than the upper surface of GaN etch resistant layer 104; Corroded above-mentioned device 5 minutes; Sapphire sheet 101, ZnO resilient coating 102 and ZnO epitaxial loayer 103 are peeled off with topmost thin film, obtained the GaN based light-emitting diode of self-supporting, and the recovery sapphire reuses.
The GaN based light-emitting diode of self-supporting is because the sapphire that does not have insulation and thermal insulation as substrate, is easy to obtain photoelectric properties high-power, high brightness.The power of the GaN based light-emitting diode that obtains through above-mentioned technology is greater than 1W, and efficient is than commercial equal power product is high by 20% at present.
Claims (2)
1. the preparation method of the GaN based light-emitting diode of a self-supporting; The GaN based light-emitting diode of this self-supporting has GaN or AlN resilient coating (202), non-Doped GaN transition zone (203), n type GaN epitaxial loayer (204), GaN/InGaN multiple quantum well light emitting layer (205) from bottom to top successively on GaN etch resistant layer (104); P type GaN epitaxial loayer (206) and current-diffusion layer (207); And at the last plating of current-diffusion layer (207) p type GaN contact electrode (208); On n type GaN epitaxial loayer (204), be listed in GaN/InGaN multiple quantum well light emitting layer (205) plating n type GaN contact electrode (209), what its preparation was adopted is Metalorganic Chemical Vapor Deposition, and step is following:
1) Sapphire Substrate (101) that will the pass through cleaning metal organic chemical vapor deposition device reaction chamber of packing into; Vacuumize; At 250-400 ℃, organic zinc source flow 5-100sccm, purity oxygen flow are 10-200sccm; Air pressure is 0.01-150Torr, and growth thickness is the ZnO resilient coating (102) of 0.1-1 micron;
2) with the step 1) goods at 700-800 ℃ of in-situ annealing 10-30 minute; In 400-600 ℃, organic zinc source flow 5-100sccm, purity oxygen flow are 10-200sccm then; Air pressure is 0.01-150Torr, and going up growth thickness at ZnO resilient coating (102) is the ZnO epitaxial loayer (103) of 0.5-30 micron;
3) at 600-800 ℃, the organic gallium source flow is 5-100sccm, and the flow of pure ammonia is 100-2000sccm, and air pressure is 10-200Torr, and going up growth thickness at ZnO epitaxial loayer (103) is the GaN etch resistant layer (104) of 0.1-1 micron;
4) on the compound substrate that above-mentioned sapphire (101), ZnO resilient coating (102), ZnO epitaxial loayer (103) and GaN etch resistant layer (104) constitute; Growing GaN or AlN resilient coating (202), non-Doped GaN transition zone (203), n type GaN epitaxial loayer (204), GaN/InGaN multiple quantum well light emitting layer (205) successively; P type GaN epitaxial loayer (206) and current-diffusion layer (207); And, on n type GaN epitaxial loayer (204), be listed in GaN/InGaN multiple quantum well light emitting layer (205) plating n type GaN contact electrode (209) at the last plating of current-diffusion layer (207) p type GaN contact electrode (208);
5) adopt the acid solution chemical corrosion method, Sapphire Substrate (101), ZnO resilient coating (102) and ZnO epitaxial loayer (103) and GaN etch resistant layer (104) are peeled off the GaN based light-emitting diode of self-supporting.
2. the preparation method of the GaN based light-emitting diode of self-supporting according to claim 1 is characterized in that the used acid solution of acid solution chemical corrosion is the nitric acid of pH >=4, the phosphoric acid of pH >=4 or the hydrofluoric acid of pH >=4.
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| CN102214748A (en) * | 2011-06-20 | 2011-10-12 | 云峰 | Epitaxial structure of LED (light-emitting diode) with GaN (gallium nitride)-based vertical structure and manufacturing method thereof |
| CN102214749A (en) * | 2011-06-20 | 2011-10-12 | 云峰 | Light emitting diode having vertical structure, and method for peeling off thin film from substrate |
| CN103022288B (en) * | 2011-09-27 | 2017-02-01 | 比亚迪股份有限公司 | Light emitting diode and manufacturing method thereof |
| CN102867892A (en) * | 2012-09-06 | 2013-01-09 | 合肥彩虹蓝光科技有限公司 | In-doped low-temperature growth P type GaN epitaxial method |
| CN103296159B (en) * | 2013-05-31 | 2015-09-16 | 华南理工大学 | Grow the InGaN/GaN Multiple Quantum Well on strontium aluminate tantalum lanthanum substrate and preparation method |
| CN103531678A (en) * | 2013-11-01 | 2014-01-22 | 杭州士兰明芯科技有限公司 | Method for removing GaN-based epitaxial layer on substrate |
| CN105322060B (en) * | 2015-10-22 | 2017-11-28 | 汤英文 | The manufacture method of chip |
| CN106601881B (en) * | 2017-02-21 | 2019-03-19 | 南京大学 | ZnO conduction covariant substrate transverse structural type GaN ultraviolet LED |
| CN109216493A (en) * | 2018-08-09 | 2019-01-15 | 镇江镓芯光电科技有限公司 | A kind of p-i-n structure ultraviolet detector and preparation method thereof based on GaN material |
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| CN101705475A (en) * | 2009-11-16 | 2010-05-12 | 浙江大学 | Method for depositing photoluminescent amorphous hydrogenated silicon carbide film on silicon chip substrate |
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| CN101705475A (en) * | 2009-11-16 | 2010-05-12 | 浙江大学 | Method for depositing photoluminescent amorphous hydrogenated silicon carbide film on silicon chip substrate |
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