CN103866272B - Method for improving P-type stability of zinc oxide film - Google Patents
Method for improving P-type stability of zinc oxide film Download PDFInfo
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- CN103866272B CN103866272B CN201210532370.0A CN201210532370A CN103866272B CN 103866272 B CN103866272 B CN 103866272B CN 201210532370 A CN201210532370 A CN 201210532370A CN 103866272 B CN103866272 B CN 103866272B
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 20
- 230000008021 deposition Effects 0.000 claims abstract description 39
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000011701 zinc Substances 0.000 claims abstract description 29
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 25
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 11
- 239000002131 composite material Substances 0.000 claims abstract description 9
- 229910007744 Zr—N Inorganic materials 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 238000000151 deposition Methods 0.000 claims description 27
- 239000010408 film Substances 0.000 claims description 27
- 229960001296 zinc oxide Drugs 0.000 claims description 23
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 10
- 239000010409 thin film Substances 0.000 claims description 8
- VOLGAXAGEUPBDM-UHFFFAOYSA-N $l^{1}-oxidanylethane Chemical compound CC[O] VOLGAXAGEUPBDM-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 229910001868 water Inorganic materials 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 230000002000 scavenging effect Effects 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims description 2
- 239000001117 sulphuric acid Substances 0.000 claims description 2
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 2
- 239000012498 ultrapure water Substances 0.000 claims description 2
- -1 alkyl compound Chemical class 0.000 claims 3
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims 3
- 230000001276 controlling effect Effects 0.000 claims 2
- 230000001105 regulatory effect Effects 0.000 claims 2
- 238000009423 ventilation Methods 0.000 claims 2
- 239000011592 zinc chloride Substances 0.000 claims 2
- BGGIUGXMWNKMCP-UHFFFAOYSA-N 2-methylpropan-2-olate;zirconium(4+) Chemical compound CC(C)(C)O[Zr](OC(C)(C)C)(OC(C)(C)C)OC(C)(C)C BGGIUGXMWNKMCP-UHFFFAOYSA-N 0.000 claims 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims 1
- 229910007932 ZrCl4 Inorganic materials 0.000 claims 1
- 229910008047 ZrI4 Inorganic materials 0.000 claims 1
- 125000003739 carbamimidoyl group Chemical group C(N)(=N)* 0.000 claims 1
- 125000000058 cyclopentadienyl group Chemical group C1(=CC=CC1)* 0.000 claims 1
- HQWPLXHWEZZGKY-UHFFFAOYSA-N diethylzinc Chemical compound CC[Zn]CC HQWPLXHWEZZGKY-UHFFFAOYSA-N 0.000 claims 1
- 229910001882 dioxygen Inorganic materials 0.000 claims 1
- UARGAUQGVANXCB-UHFFFAOYSA-N ethanol;zirconium Chemical group [Zr].CCO.CCO.CCO.CCO UARGAUQGVANXCB-UHFFFAOYSA-N 0.000 claims 1
- 150000004678 hydrides Chemical class 0.000 claims 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims 1
- LGRLWUINFJPLSH-UHFFFAOYSA-N methanide Chemical compound [CH3-] LGRLWUINFJPLSH-UHFFFAOYSA-N 0.000 claims 1
- 229910052594 sapphire Inorganic materials 0.000 claims 1
- 239000010980 sapphire Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 235000005074 zinc chloride Nutrition 0.000 claims 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical group Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims 1
- HONKFXPQYSOIMS-UHFFFAOYSA-J zirconium(4+) tetraiodate Chemical compound [Zr+4].[O-]I(=O)=O.[O-]I(=O)=O.[O-]I(=O)=O.[O-]I(=O)=O HONKFXPQYSOIMS-UHFFFAOYSA-J 0.000 claims 1
- XLMQAUWIRARSJG-UHFFFAOYSA-J zirconium(iv) iodide Chemical compound [Zr+4].[I-].[I-].[I-].[I-] XLMQAUWIRARSJG-UHFFFAOYSA-J 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 230000012010 growth Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000000231 atomic layer deposition Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001451 molecular beam epitaxy Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 238000004549 pulsed laser deposition Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007773 growth pattern Effects 0.000 description 1
- XEMZLVDIUVCKGL-UHFFFAOYSA-N hydrogen peroxide;sulfuric acid Chemical compound OO.OS(O)(=O)=O XEMZLVDIUVCKGL-UHFFFAOYSA-N 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- IPSRAFUHLHIWAR-UHFFFAOYSA-N zinc;ethane Chemical compound [Zn+2].[CH2-]C.[CH2-]C IPSRAFUHLHIWAR-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for improving the P-type stability of a zinc oxide film, which comprises the steps of putting a substrate into an ALD reaction chamber, heating the substrate and a chamber pipeline, and then carrying out multi-component composite deposition; the composite deposition comprises the steps of introducing doping deposition of a doping source containing a doping element Zr, zinc source deposition for the second time, nitrogen doping source deposition for the two times and oxygen source deposition for the two times respectively after zinc source deposition for the first time to form N-Zr-N codoping; the deposition sequence of the nitrogen doping source and the oxygen source is that the nitrogen doping source is deposited firstly, and then the oxygen source is deposited; the sequence of the doping source deposition containing the doping element Zr and the second zinc source deposition is that the second zinc source deposition is carried out firstly, and then the doping source deposition containing the doping element Zr is carried out. The method can carry out in-situ donor-acceptor co-doping on the zinc oxide film so as to increase the doping amount of acceptor elements and promote the p-type conversion of the zinc oxide film.
Description
Technical field
The present invention relates to the preparing technical field of zinc-oxide film, particularly to the method being used for improving zinc-oxide film P type stability.
Background technology
Semiconductive thin film has given play to highly important effect in the new high-tech industries such as microelectronics, optics, informatics, the preparation of development high-crystal quality semiconductive thin film and doping techniques, especially for the preparation of third generation semi-conducting material ZnO film, sign, adulterate extremely characteristic research, for including ultraviolet band luminescent material, ultraviolet detector, high integration photonic propulsion is of great significance towards the important applied field tool of new forms of energy with electronics device, solaode etc. Zinc oxide, as a kind of novel II-VI race direct band gap high-gap compound, has big room temperature energy gap 3.37eV, and free exciton combines and up to 60meV, increasingly can be subject to people's attention as semi-conducting material. Compared with other semiconductor material with wide forbidden band, ZnO film growth temperature is low, radiation resistance is good, stimulated radiation has relatively low threshold power and significantly high energy conversion efficiency, these advantages make ZnO just becoming the new and high technologies such as photoelectron, microelectronics, information rely after 12 continue development key foundation material. But intrinsic ZnO is due to existing defects so that ZnO is n-type, p-type ZnO film is prepared by focus and the difficult point of current ZnO correlational study. Although the preparation that the calculating that N doping is in theory makes p-type ZnO is possibly realized, but numerous experiments show that, owing to N element solid solubility in ZnO is relatively low, therefore independent N element doping can not realize the p-type ZnO film of high carrier concentration and high mobility. In order to solve this problem, being co-doped with of acceptor-donor-acceptor is considered as one of direction preparing high-quality p-ZnO thin film optimum development prospect.
In recent years, the method preparing ZnO film generally includes: such as magnetron sputtering, metal organic chemical vapor deposition (MOCVD), molecular beam epitaxy (MBE), pulsed laser deposition (PLD) and wet-chemical deposition etc.These preparation technologies are respectively arranged with pluses and minuses, and the film quality prepared with MOCVD and MBE method from crystallization situation is better. But, turbulent flow and air flow method that MOCVD exists in can not carrying out the doping of thin film in position and reacting can affect thickness and the uniformity of film. MBE technology is also difficult to for the accurate doping of specific atoms layer position.
Summary of the invention
The technical problem to be solved is to provide and a kind of zinc-oxide film can be carried out being co-doped with of original position, to increase the incorporation of recipient element, promotes the method for improving zinc-oxide film P type stability that the p-type of zinc-oxide film changes.
For solving above-mentioned technical problem, the invention provides a kind of method for improving zinc-oxide film P type stability, including substrate being put in ALD reaction chamber, substrate and chamber tube are heated, then carry out multi-component composite deposition; Described composite deposition includes after first time zinc source deposits, and introduces once the doping deposition of doped source containing doped chemical Zr, second time zinc source deposition, twice nitrogen doping source deposition and twice oxygen source deposition respectively, forms being co-doped with of N-Zr-N; The sedimentary sequence of described nitrogen doping source deposition and described oxygen source is first nitrogen doping source deposition, and rear oxygen source deposits; The described doped source deposition containing doped chemical Zr and described second time zinc source sedimentary sequence are first second time zinc source depositions, after doped source containing doped chemical Zr deposit.
Method for improving zinc-oxide film P type stability provided by the invention, utilizes the feature of ALD layer layer growth, in the process of growth of zinc oxide thin film, mixes a twice recipient element N and Zr, forms the N-Zr-N zinc-oxide film being co-doped with. The formation of N-Zr-N complex, reduces ionization energy, promotes the formation of p-type conductance. Preparation technology of the present invention is simple, and deposition and doping process are easily controllable, prepares gained and is co-doped with zinc-oxide film and is conducive to improving the stability of zinc-oxide film p-type electrical properties.
Accompanying drawing explanation
The flow chart of the method for improving zinc-oxide film P type stability that Fig. 1 provides for the embodiment of the present invention.
Detailed description of the invention
Method for improving zinc-oxide film P type stability shown in Figure 1, that the embodiment of the present invention provides, including: silicon substrate or glass substrate concentrated sulphuric acid hydrogen peroxide are processed, then is carried out with ultra-pure water ultrasound wave, N2Dry up, wherein concentrated sulphuric acid: hydrogen peroxide=4:1. Placing the substrate in the chamber of ald, open atomic layer deposition apparatus, adjust running parameter, evacuation, heating sink to the bottom, and reach the required various working environments of experiment; Carry out N-Zr and be co-doped with many groups composite deposition of zinc-oxide film, i.e. Zn (C2H5)2/N2/plasmaN2/N2/H2O/N2/Zn(C2H5)2/N2/(CH3CH2O)4Zr/N2/plasmaN2/N2/H2O/N2=0.15s/50s/10s/50s/0.07s/50s/0.08s/50s/0.08s/50s/10s/50s/ 0.07s/50s. Wherein the flow of nitrogen is 1sccm-1000sccm, it is therefore preferable to 15sccm, and inlet period is 0.04s-5s, it is therefore preferable to 0.15s, and scavenging period is 5s-150s, it is therefore preferable to 50s, and underlayer temperature is 100 DEG C-500 DEG C, it is therefore preferable to 300 DEG C; Wherein plasma discharge power is 1W-100W, it is therefore preferable to 50W, and discharge time is 1s-50s, it is preferred that for 10s. Pass through N during this period2Plasma introduces N doping, by (CH3CH2O)4Zr provides Zr atom, twice plasmaN2Once (CH3CH2O)4The deposition of Zr so that Zr replaces zinc (Zr in ZnOZn), N substitutes the position of O, forms the complex of N-Zr-N in the film, and this complex can reduce ionization energy, promotes the formation of p-type conductance.Repeat this multi-component composite deposition, it is possible to the zinc-oxide film that successively growth N-Zr-N is co-doped with.
The present invention is by the ALD growth pattern successively circulated growth Zr and the N zinc-oxide film being co-doped with, and method is simple, utilize the feature of ald monolayer cycling deposition, the process of growth of zinc oxide thin film realizes adulterate in whole membrane structure uniformly, zinc-oxide film after being co-doped with, may advantageously facilitate the formation of p-type conductance.
It should be noted last that, above detailed description of the invention is only in order to illustrate technical scheme and unrestricted, although the present invention being described in detail with reference to example, it will be understood by those within the art that, technical scheme can be modified or equivalent replacement, without deviating from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of scope of the presently claimed invention.
Claims (8)
1. the method for improving zinc-oxide film P type stability, it is characterised in that including:
Substrate is put in ALD reaction chamber, substrate and chamber tube are heated, then carry out multi-component composite deposition;
Described composite deposition includes after first time zinc source deposits, and introduces once the doping deposition of doped source containing doped chemical Zr, second time zinc source deposition, twice nitrogen doping source deposition and twice oxygen source deposition respectively, forms being co-doped with of N-Zr-N; The sedimentary sequence of described nitrogen doping source deposition and described oxygen source is first nitrogen doping source deposition, and rear oxygen source deposits; The described doped source deposition containing doped chemical Zr and described second time zinc source sedimentary sequence are first second time zinc source depositions, after doped source containing doped chemical Zr deposit; Described composite deposition includes:
Under vacuum conditions successively with first time zinc source, nitrogen doping source, oxygen source, second time zinc source, doped source containing doped chemical Zr, nitrogen doping source and oxygen source be deposited obtaining the N-Zr ZnO film being co-doped with, described first time zinc source, nitrogen doping source, oxygen source, doped source containing doped chemical Zr and second time zinc source open-assembly time in settling chamber are followed successively by 0.15s, 10s, 0.07s, 0.08s, 0.08s; Adopting high pure nitrogen to clean settling chamber after deposition every time, scavenging period is 50s.
2. preparation method according to claim 1, it is characterised in that described substrate is process through concentrated sulphuric acid and hydrogen peroxide, and through the silicon chip of the ultrasonic mistake of ultra-pure water, sapphire or glass, substrate surface is with hydroxyl.
3. the preparation method according to any one of claim 1-2, it is characterised in that described zinc source is the alkyl compound containing zinc or the halogenide containing zinc, and described oxygen source is water vapour or oxygen gas plasma; Described nitrogen doping source is N2O��N2��NO��NO2Or NH3Plasma.
4. preparation method according to claim 3, it is characterised in that the described halogenide containing zinc is zinc chloride ZnCl2, the described alkyl compound containing zinc is diethyl zinc Zn (C2H5)2Or zinc methide Zn (CH3)2��
5. preparation method according to claim 4, it is characterized in that, the described doped source containing doped chemical Zr is the halogenide containing Zr, the alcoholates containing Zr, the alkylates containing Zr, the hydride containing Zr, the cyclopentadienyl group containing Zr, the alkane amide containing Zr or the amidino groups containing Zr.
6. preparation method according to claim 5, it is characterised in that the described halogenide containing Zr is zirconium chloride ZrCl4Or iodate zirconium ZrI4, the described alcoholates containing Zr is ethanol zirconium (CH3CH2O)4Zr or zirconium tert-butoxide C16H36O4Zr��
7. the preparation method according to any one of claim 1-6, it is characterised in that also include:
The ratio of nitrogen doping source and oxygen in doping zinc-oxide thin film is regulated by controlling the duration of ventilation of described nitrogen doping source and steam.
8. preparation method according to claim 6, it is characterised in that also include:
The ratio of zirconium doped source and zinc in doping zinc-oxide thin film is regulated by controlling the duration of ventilation in doped source containing doped chemical Zr and zinc source.
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| CN201210532370.0A CN103866272B (en) | 2012-12-11 | 2012-12-11 | Method for improving P-type stability of zinc oxide film |
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| CN201210532370.0A CN103866272B (en) | 2012-12-11 | 2012-12-11 | Method for improving P-type stability of zinc oxide film |
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| CN103866272B true CN103866272B (en) | 2016-06-08 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304700A (en) * | 2011-09-23 | 2012-01-04 | 中国科学院微电子研究所 | Preparation method of nitrogen-doped zinc oxide film |
| CN102534501A (en) * | 2012-03-29 | 2012-07-04 | 山东理工大学 | Preparation method for co-doped zinc oxide transparent conductive thin film for solar cell |
| CN102694066A (en) * | 2012-04-01 | 2012-09-26 | 东旭集团有限公司 | Method for improving photoelectric conversion efficiency of solar cell panel |
| CN102781838A (en) * | 2010-02-25 | 2012-11-14 | 康宁股份有限公司 | A process for manufacturing a doped or non-doped ZnO material and said material |
-
2012
- 2012-12-11 CN CN201210532370.0A patent/CN103866272B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102781838A (en) * | 2010-02-25 | 2012-11-14 | 康宁股份有限公司 | A process for manufacturing a doped or non-doped ZnO material and said material |
| CN102304700A (en) * | 2011-09-23 | 2012-01-04 | 中国科学院微电子研究所 | Preparation method of nitrogen-doped zinc oxide film |
| CN102534501A (en) * | 2012-03-29 | 2012-07-04 | 山东理工大学 | Preparation method for co-doped zinc oxide transparent conductive thin film for solar cell |
| CN102694066A (en) * | 2012-04-01 | 2012-09-26 | 东旭集团有限公司 | Method for improving photoelectric conversion efficiency of solar cell panel |
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