CN104409337B - The preparation method of sulphur and silver-colored codoped p type zinc oxide optoelectronic film - Google Patents
The preparation method of sulphur and silver-colored codoped p type zinc oxide optoelectronic film Download PDFInfo
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- CN104409337B CN104409337B CN201410614869.5A CN201410614869A CN104409337B CN 104409337 B CN104409337 B CN 104409337B CN 201410614869 A CN201410614869 A CN 201410614869A CN 104409337 B CN104409337 B CN 104409337B
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 34
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000005864 Sulphur Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 230000005693 optoelectronics Effects 0.000 title claims abstract description 8
- 230000003647 oxidation Effects 0.000 claims abstract description 19
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 239000005083 Zinc sulfide Substances 0.000 claims abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001301 oxygen Substances 0.000 claims abstract description 9
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 238000000151 deposition Methods 0.000 claims abstract description 3
- 230000008021 deposition Effects 0.000 claims abstract description 3
- 238000004544 sputter deposition Methods 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 23
- 239000011701 zinc Substances 0.000 description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 7
- 229910052725 zinc Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 125000004430 oxygen atom Chemical group O* 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000003775 Density Functional Theory Methods 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0623—Sulfides, selenides or tellurides
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
- C23C14/5853—Oxidation
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- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/0296—Inorganic materials including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe
- H01L31/02963—Inorganic materials including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe characterised by the doping material
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Abstract
The present invention relates to the preparation method of a kind of sulphur and silver-colored codoped p type zinc oxide optoelectronic film, prepared using magnetron sputtering and thermal oxidation technique, magnetron sputtering chamber is extracted under vacuum environment, and heat the substrate through strictly cleaning, it is more than 99.99% zinc sulphide target and silver-colored target using purity, the method deposition ZnS sputtered jointly with double targets:Ag films;By the ZnS of acquisition:Ag is placed on thermal oxidation under oxygen atmosphere.Preparation method of the present invention, parameter is easily-controllable, and repeatability is high, and the control of doping concentration can be achieved, and is applicable industrialization production environment.
Description
Technical field
The invention belongs to p-type ZnO semiconductor optoelectronic thin film materials arts, and in particular to a kind of sulphur and silver-colored codoped p type
The preparation method of ZnO optoelectronic films and application.
Background technology
As the representative material of semiconductor material with wide forbidden band, ZnO has up to 3.37eV energy gap and up to 60meV
Exciton bind energy, and ZnO has abundant raw materials concurrently, the characteristics of green non-poisonous so that ZnO is particularly ultraviolet in semiconductor industry
Field of photoelectric devices receives extensive concern.But being difficult to of p-type ZnO film is increasingly becoming restriction ZnO material device
Bottleneck.Because 1)ZnO acceptor level is very deep, and itself there is Shi zhiming has strong auto-compensation so that intrinsic
ZnO shows weak n-type, hinders the formation of shallow acceptor energy level.2)Solid solubility of most recipient elements in ZnO is very low, greatly
Limit the raising of hole concentration.But be still at present by adulterate I races element such as sodium, potassium, lithium or V group element nitrogen, phosphorus etc. by
Main mode prepares p-type ZnO.Recently, theoretical research is confirmed:In excess oxygen, Ag doping ZnO is easily formed zinc displacement, it was demonstrated that
Ag doping is the effective ways for obtaining p-type ZnO.But Yan etc. is pointed out simultaneously, the acceptor level that Ag doping is introduced is deeper(About
0.4eV), this to hardly result in the hole concentration needed for transition at room temperature.Therefore silver how is reduced as the ionization energy of acceptor,
As the major issue for obtaining low temperature lower p-type ZnO.Yan etc. shows through theoretical research:Ag can be effectively reduced by codope sulphur to make
For the ionization energy of acceptor.But density functional theory is confirmed:After Ag displacements Zn, it will be bonded with the four of surrounding O atoms.If will
The O atom of surrounding is replaced with S atom, then forms AgZn-nSO, n is the number for replacing O atom.As n increases, AgZn-
nSOThe ionization energy of defect will be reduced, therefore it is deeper by silver and sulphur codope can effectively to reduce independent Ag acceptor level of adulterating
Problem, to realizing that n-type ZnO is significant.But to how to realize the Effective Doping of two kinds of elements and effectively control it to adulterate
Ratio there is no further research.
The content of the invention
The problem of present invention is difficult to for p-type ZnO is prepared there is provided one kind by magnetron sputtering and thermal oxidation technique
Silver and sulphur co-doping p-type ZnO optoelectronic film method and application, the p-type ZnO photoelectric properties of preparation are excellent.
A kind of preparation method of sulphur and silver-colored codoped p type zinc oxide optoelectronic film, it is characterised in that using magnetron sputtering and
Prepared by thermal oxidation technique, comprise the following steps:
(1)Magnetron sputtering chamber is extracted under vacuum environment, and heats the substrate through strictly cleaning, is more than using purity
99.99% zinc sulphide target and silver-colored target, the method deposition ZnS sputtered jointly with double targets:Ag films;
(2)By step(1)The ZnS of middle acquisition:Ag is placed on thermal oxidation under oxygen atmosphere.
Environment initial depression is prepared using magnetron sputtering and is not less than 10-4The order of magnitude, the argon flow amount being passed through should be controlled
50-100sccm, sputtering pressure is in 3-5Pa, and base reservoir temperature is 250-350 DEG C.
When carrying out thermal oxidation under oxygen-enriched environment, its temperature is 600-1000 DEG C, and thermal oxidation time is 4-10 hours.
The ZnS of different proportion can be obtained by the sputtering power for adjusting ZnS and Ag:Ag films, wherein zinc sulphide target
Sputtering power control in 50-100W, the sputtering power of silver-colored target target is in 5-20W.
The features of the present invention and gain effect are as follows:
The inventive method is easy to the ratio that is co-doped with of regulation and control silver and sulphur, satisfaction by the way of zinc sulphide and silver-colored target cosputtering
Different demands, can effectively reduce production cost consumption;
The even particle distribution of p-type ZnO film prepared by sulphur and silver-colored codope prepared by the present invention, electrical properties are excellent,
Electrical property such as resistivity as little as 10-2Magnitude, p-type carrier concentration is up to 1021The order of magnitude, mobility is between 1-10.
Preparation method technique of the present invention is simple, and parameter is easily-controllable, and repeatability is high, and process is easily controllable, can be achieved
Large-scale industrialization production.
Brief description of the drawings
ZnSs of the Fig. 1 without thermal oxidation:The AFM figures of Ag films, it can be seen that ZnS:Ag particles are uniform sequential, favorably
In the ZnO for forming codope.
The AFM figures that Fig. 2 is the sulphur and silver-colored codope ZnO obtained after thermal oxidation, it can be seen that through high-temperature thermal oxidation
Afterwards, codope ZnO film is made up of uniform crystal grain, compared with before oxidation, and crystal grain is significantly increased.
Fig. 3 is the sulphur obtained after thermal oxide and the X-ray diffraction spectrum of the ZnO film of silver-colored codope
Embodiment
Heretofore described method need to use magnetic control sputtering system and thermal oxidation instrument, below with reference to embodiment
Technical scheme is elaborated.All embodiments are implemented lower premised on technical solution of the present invention, give
Detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following embodiments.
Embodiment 1:
(1) silicon after surface is strictly cleaned is put into the position of sample 1, heating substrate is to 300 DEG C, by magnetic control as substrate
The vacuum of sputtering chamber is evacuated to 10-4After the Pa orders of magnitude, it is 80sccm, (stable gas pressure 4.1- to control argon flow amount meter parameter
4.3Pa), the radio-frequency power for setting zinc sulphide target is 80W, and the sputtering power of silver-colored target is 10W, and sputtering obtains Ag doping
Ratio is 3.9% ZnS:Ag films.
(2) by the ZnS of acquisition:Ag films carry out thermal oxidation under oxygen atmosphere, and temperature is 800 DEG C, and the time is 6
Hour.Obtain sulphur and zinc co-doped p-type ZnO film that thickness is about 985nm.
As shown in table 1, resistivity is 0.0389 to the room temperature electric property of the sulphur of acquisition and zinc co-doped p-type ZnO film
Ω cm, mobility is 7.85cm2/ Vs, carrier concentration is 2.69 × 1019。
Embodiment 2:
(1) quartz by strictly cleaning is put into the position of sample 2, base reservoir temperature is set to 250 DEG C as substrate;Will
The vacuum of magnetron sputtering chamber is evacuated to 10-4After the Pa orders of magnitude, it is 50sccm, (stable gas pressure 3.- to control argon flow amount meter parameter
3.3Pa), the radio-frequency power for setting zinc sulphide target is 50W, and the sputtering power of silver-colored target is 5W, and sputtering obtains Ag doping
Ratio is 2.9% ZnS:Ag films.
(2) by the ZnS of acquisition:Ag films carry out thermal oxidation under oxygen atmosphere, and temperature is 1000 DEG C, and the time is 8
Hour.Obtain sulphur and zinc co-doped p-type ZnO film that thickness is about 818nm.
As shown in table 2, resistivity is 0.054 Ω to the room temperature electric property of the sulphur of acquisition and zinc co-doped p-type ZnO film
Cm, mobility is 20.78cm2/ Vs, carrier concentration is 5.46 × 1018。
Embodiment 3:
(1) silicon using surface by strictly cleaning is put into the position of sample 2, base reservoir temperature is set to 350 DEG C as substrate;Will
The vacuum of magnetron sputtering chamber is evacuated to 10-4After the Pa orders of magnitude, it is 100sccm, (stable gas pressure to control argon flow amount meter parameter
4.8.-5.0Pa), the radio-frequency power for setting zinc sulphide target is 100W, and the sputtering power of silver-colored target is 20W, and sputtering is obtained
Ag doping ratios are 7.2% ZnS:Ag films.
(2) by the ZnS of acquisition:Ag films carry out thermal oxidation under oxygen atmosphere, and temperature is 600 DEG C, and the time is 8
Hour.Obtain sulphur and zinc co-doped p-type ZnO film that thickness is about 1132nm.
As shown in table 3, resistivity is 0.054 Ω to the room temperature electric property of the sulphur of acquisition and zinc co-doped p-type ZnO film
Cm, mobility is 0.082cm2/ Vs, carrier concentration is 3.24 × 1021。
Claims (1)
1. the preparation method of a kind of sulphur and silver-colored codoped p type zinc oxide optoelectronic film, it is characterised in that use magnetron sputtering and heat
Prepared by oxidation technology, comprise the following steps:
(1)Magnetron sputtering chamber is extracted under vacuum environment, and heats the substrate through strictly cleaning, is more than 99.99% using purity
Zinc sulphide target and silver-colored target, the method deposition ZnS sputtered jointly with double targets:Ag films;
(2)By step(1)The ZnS of middle acquisition:Ag is placed on thermal oxidation under oxygen atmosphere;
Environment initial depression is prepared using magnetron sputtering and is not less than 10-4The order of magnitude, the argon flow amount being passed through should be controlled in 50-
100sccm, sputtering pressure is in 3-5Pa, and base reservoir temperature is 250-350 DEG C;
When carrying out thermal oxidation under oxygen-enriched environment, its temperature is 600-1000 DEG C, and thermal oxidation time is 4-10 hours;
The ZnS of different proportion can be obtained by the sputtering power for adjusting ZnS and Ag:Ag films, wherein zinc sulphide target splash
Power Control is penetrated in 50-100W, the sputtering power of silver-colored target target is in 5-20W.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101798672A (en) * | 2009-12-18 | 2010-08-11 | 湛江师范学院 | Method for preparing P-type zinc oxide film from in situ low-pressure oxidized aluminum-doped zinc nitride |
CN102503162A (en) * | 2011-11-01 | 2012-06-20 | 昆明理工大学 | Preparation method for Ag-Al co-doped p type ZnO film |
CN102719893A (en) * | 2012-06-18 | 2012-10-10 | 中国科学院福建物质结构研究所 | Method for preparing p-type zinc oxide material |
CN103103478A (en) * | 2013-01-16 | 2013-05-15 | 浙江工业大学 | Ag-S co-doped p-type ZnO film and preparation method thereof |
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CN101798672A (en) * | 2009-12-18 | 2010-08-11 | 湛江师范学院 | Method for preparing P-type zinc oxide film from in situ low-pressure oxidized aluminum-doped zinc nitride |
CN102503162A (en) * | 2011-11-01 | 2012-06-20 | 昆明理工大学 | Preparation method for Ag-Al co-doped p type ZnO film |
CN102719893A (en) * | 2012-06-18 | 2012-10-10 | 中国科学院福建物质结构研究所 | Method for preparing p-type zinc oxide material |
CN103103478A (en) * | 2013-01-16 | 2013-05-15 | 浙江工业大学 | Ag-S co-doped p-type ZnO film and preparation method thereof |
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