CN105821379A - Method for preparing single-phase transparent conductive cuprous oxide film - Google Patents
Method for preparing single-phase transparent conductive cuprous oxide film Download PDFInfo
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- CN105821379A CN105821379A CN201610409769.8A CN201610409769A CN105821379A CN 105821379 A CN105821379 A CN 105821379A CN 201610409769 A CN201610409769 A CN 201610409769A CN 105821379 A CN105821379 A CN 105821379A
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- oxide film
- cuprous oxide
- transparent conductive
- sputtering
- phase transparent
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- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 53
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229940112669 cuprous oxide Drugs 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 30
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000000758 substrate Substances 0.000 claims abstract description 39
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000010949 copper Substances 0.000 claims abstract description 36
- 229910052802 copper Inorganic materials 0.000 claims abstract description 35
- 238000004544 sputter deposition Methods 0.000 claims abstract description 32
- 229910052786 argon Inorganic materials 0.000 claims abstract description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000007789 gas Substances 0.000 claims abstract description 21
- 239000001301 oxygen Substances 0.000 claims abstract description 21
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 21
- 238000000151 deposition Methods 0.000 claims abstract description 13
- 230000008021 deposition Effects 0.000 claims abstract description 10
- 239000012495 reaction gas Substances 0.000 claims abstract description 10
- 238000005477 sputtering target Methods 0.000 claims abstract description 9
- 239000013077 target material Substances 0.000 claims abstract description 8
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003945 anionic surfactant Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000001276 controlling effect Effects 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000011941 photocatalyst Substances 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 239000002887 superconductor Substances 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000011540 sensing material Substances 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 5
- 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 3
- 230000003287 optical effect Effects 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 229960004643 cupric oxide Drugs 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
-
- 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
- C23C14/08—Oxides
- C23C14/087—Oxides of copper or solid solutions thereof
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing Of Electric Cables (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention provides a method for preparing a single-phase transparent conductive cuprous oxide film. A direct current reaction magnetron sputtering method is adopted at the room temperature, a copper target serves as a sputtering target material, oxygen serves as reaction gas, argon serves as sputtering gas, the cuprous oxide film is deposited on a substrate, and deposition of the cuprous oxide film is conducted in a vacuum chamber with the vacuum degree being 6.0*10<4> Pa or above; the copper target sputtering power is 40-150 W, and the deposition time is 1-30 minutes; oxygen flow is 2-30 sccm, and argon flow is 5-100 sccm. The cuprous oxide film prepared from the method is transparent, conductive, high in deposition rate and high in controllability, has a single phase, good adhesiveness, uniformity and stability and has wide application prospect in the fields of heterojunction solar cells, photoelectric devices, gas sensing materials, photocatalysts, high-temperature superconductor materials, environmental purification and the like.
Description
Technical Field
The invention belongs to the field of semiconductor materials, relates to a film, and particularly relates to a method for preparing a single-phase transparent conductive cuprous oxide film.
Background
With the development of modern science and technology, information, energy and materials become three fundamental stones for the development of science and technology, and among them, the research of semiconductor materials plays a very important role.
Cuprous oxide is a direct band gap semiconductor material which can be excited by visible light and has a regular octahedral cubic crystal structure, and has the characteristics of a P-type semiconductor. The forbidden band width is about 2.17eV, the energy band is in the optimal energy gap (1.5-3.0eV) of solar power generation, the photoelectric conversion efficiency is as high as 20% under the irradiation of visible light, and the practical value is high.
The cuprous oxide material is non-toxic, low in preparation cost, rich in resources and good in process repeatability, is a very promising semiconductor material, and is widely applied to the fields of heterojunction solar cells, photoelectric devices, gas sensing materials, photocatalysts, colorants, high-temperature superconductor materials, environmental purification and the like.
The cuprous oxide film can be prepared by thermal evaporation, sputtering, chemical vapor deposition, electrochemical deposition, sol-gel, pulsed laser deposition, molecular beam epitaxy, electron beam evaporation, solution growth, vacuum evaporation, etc. The methods have great limitations, namely the prepared cuprous oxide film usually has copper and cupric oxide components, so that the crystallinity of the film is poor, the film is easy to be oxidized, the growth mechanism and the photoelectric characteristic of the film cannot be accurately analyzed, and the most critical point is that the single-phase transparent conductive cuprous oxide film is difficult to obtain.
Chinese patent application CN 102623521 a (title of the invention, "a method for preparing cuprous oxide film") discloses a method for preparing cuprous oxide film, which has certain advantages but still has the following defects: 1) the preparation process is time-consuming and tedious, and the experimental conditions are extremely harsh; 2) the cuprous oxide film prepared is not a single phase; 3) the high-temperature environment in the film preparation process is difficult to realize, the cost is high, and large-scale preparation cannot be carried out.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a method for preparing a single-phase transparent conductive cuprous oxide film, which aims to solve the technical problems that the cuprous oxide film prepared by the method in the prior art is not a single phase, the preparation process is complex and the conditions are harsh.
The invention provides a method for preparing a single-phase transparent conductive cuprous oxide film, which is characterized in that a direct-current reactive magnetron sputtering method is adopted at room temperature, a copper target material is used as a sputtering target material, oxygen is used as a reaction gas, argon is used as a sputtering gas, and a cuprous oxide film is deposited on a substrate and is deposited at the vacuum degree of 6.0 × 10-4Pa and above in a vacuum chamber; wherein the sputtering power of the copper target is 40-150W, and the deposition time is 1-30 min; the oxygen flow is 2-30sccm, and the argon flowThe amount is 5-100 sccm.
The invention also provides a method for preparing the single-phase transparent conductive cuprous oxide film, which comprises the following steps:
1) firstly, adopting an anionic surfactant to pre-clean a substrate;
2) sequentially carrying out ultrasonic cleaning on the substrate by adopting acetone, alcohol and deionized water, and regulating and controlling the temperature to be 0 ℃;
3) taking metal copper as a cathode target, connecting an anode with a vacuum chamber, mounting the substrate subjected to ultrasonic cleaning on a substrate fixture, and placing a movable baffle between the substrate fixture and the copper target;
4) the vacuum degree of the vacuum chamber is pumped to 6.0 × 10-4Pa and above, then introducing oxygen and argon into the vacuum chamber to ensure that the working pressure in the vacuum chamber is 0.8 Pa;
5) after the working air pressure and the gas flow are stable, sputtering the copper target for 10-15min in advance to remove oxides and impurities on the surface of the copper target;
6) and rotating the substrate fixture, moving the movable baffle plate, starting sputtering the film, and closing the movable baffle plate after sputtering is finished to obtain the single-phase transparent conductive cuprous oxide film.
Further, the flow rate of the introduced oxygen is 5-30sccm, and the flow rate of the argon is 5-100 sccm;
further, the sputtering target material is metal copper with the purity of more than 99.99 percent;
further, the purity of the argon gas is 99.99 percent;
further, the purity of the oxygen is 99.99%;
further, the substrate may be quartz, silicon wafer, crystal or glass.
The invention adopts a direct current reactive magnetron sputtering method at room temperature, takes a copper target material as a sputtering target material, takes high-purity oxygen as reaction gas and takes high-purity argon as sputtering gas, and the cuprous oxide film is deposited on the substrate. Compared with the prior art, the film preparation method provided by the invention has the advantages that the deposition rate is high, the controllability is strong, the prepared film has good crystallinity, good adhesiveness, uniformity and thermal stability, and the most important point is that the cuprous oxide film with a single phase and transparent conductivity can be obtained. The test result of the XRD diffractometer shows that the cuprous oxide film obtained by the invention is a single phase, and the intensity of the diffraction peak gradually becomes stronger. The square resistance of the film is tested by using an RTS-9 type double-electric-test four-probe tester, and the result shows that the resistance value of the square resistance of the cuprous oxide film obtained by the invention is gradually reduced, and the cuprous oxide film has good electric conductivity.
Compared with the prior art, the invention has remarkable technical progress. The cuprous oxide film obtained by the method is transparent and conductive, has a single phase, high deposition rate, strong controllability, good adhesiveness, uniformity and stability, is nontoxic in material, low in preparation cost, rich in resources and good in process repeatability, and has wide application prospects in the fields of heterojunction solar cells, photoelectric devices, gas induction materials, photocatalysts, colorants, high-temperature superconductor materials, environmental purification and the like.
Drawings
Fig. 1 is an X-ray diffraction pattern of a transparent conductive cuprous oxide film measured according to the present invention.
Fig. 2 is a plot of the square resistance of a transparent conductive cuprous oxide film measured according to the present invention.
Fig. 3 is a graph of an optical transmittance curve of a transparent conductive film measured according to the present invention.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the following embodiments are specifically described in the method for preparing the single-phase transparent conductive cuprous oxide film according to the present invention with reference to the attached drawings.
Examples
1
And adopting a direct-current reactive magnetron sputtering method at room temperature. Depositing a cuprous oxide film on a substrate by taking a copper target as a sputtering target, high-purity oxygen as a reaction gas and high-purity argon as a sputtering gas; wherein,
the sputtering power of the copper target is 40W, and the deposition time is 5 min;
the oxygen flow is 5sccm, and the argon flow is 5 sccm.
The specific operation steps are as follows:
1. pre-washing the substrate with a dilute solution of an anionic surfactant (sodium aliphatate, etc., available as soapy water);
2. sequentially carrying out ultrasonic cleaning on the substrate for 10 minutes by adopting acetone, alcohol and deionized water, and regulating the temperature to be 0 ℃;
3. taking metal copper with the purity of 99.99 percent as a cathode target, connecting an anode with a vacuum chamber, installing the quartz substrate after ultrasonic cleaning on a substrate fixture, and arranging a movable baffle between the substrate fixture and the copper target;
4. the vacuum degree of the vacuum chamber is pumped to 6.0 × 10-4Pa and above, introducing reaction gas oxygen and sputtering gas argon into the vacuum chamber, so that the working pressure in the vacuum chamber is 0.8Pa, and the sputtering power is 40W;
5. after the working pressure and the gas flow are stable, the copper target is sputtered for 10-15min in advance to remove oxides and impurities on the surface of the copper target.
6. And rotating the substrate fixture, moving the movable baffle plate, starting sputtering the film, and closing the movable baffle plate after sputtering for 5 minutes to obtain the single-phase transparent conductive cuprous oxide film.
Examples
2
And adopting a direct-current reactive magnetron sputtering method at room temperature. Depositing a cuprous oxide film on a substrate by taking a copper target as a sputtering target, high-purity oxygen as a reaction gas and high-purity argon as a sputtering gas; wherein,
the sputtering power of the copper target is 80W, and the deposition time is 8 min;
the oxygen flow rate was 15sccm, and the argon flow rate was 50 sccm.
The specific operation steps are as follows:
1. pre-cleaning the substrate with a diluted solution of an anionic surfactant (sodium aliphatate, etc., soap water is available), and then sequentially performing ultrasonic cleaning on the substrate for 10 minutes by using acetone, alcohol and deionized water, wherein the temperature is controlled at 0 ℃;
2. taking metal copper with the purity of 99.99 percent as a cathode target, connecting an anode with a vacuum chamber, installing the quartz substrate after ultrasonic cleaning on a substrate fixture, and arranging a movable baffle between the substrate fixture and the copper target;
3. the vacuum degree of the vacuum chamber is pumped to 6.0 × 10-4Pa and above, introducing reaction gas oxygen and sputtering gas argon into the vacuum chamber, so that the working pressure in the vacuum chamber is 0.8Pa, and the sputtering power is 80W;
4. after the working pressure and the gas flow are stable, the copper target is sputtered for 10-15min in advance to remove oxides and impurities on the surface of the copper target.
5. And rotating the substrate fixture, moving the movable baffle plate, starting sputtering the film, and closing the movable baffle plate after sputtering for 8 minutes to obtain the single-phase transparent conductive cuprous oxide film.
Examples
3
And adopting a direct-current reactive magnetron sputtering method at room temperature. Depositing a cuprous oxide film on a substrate by taking a copper target as a sputtering target, high-purity oxygen as a reaction gas and high-purity argon as a sputtering gas; wherein,
the sputtering power of the copper target is 150W, and the deposition time is 10 min;
the flow rate of the oxygen gas is 30sccm, and the flow rate of the argon gas is 100 sccm.
The specific operation steps are as follows:
1. pre-cleaning the substrate with a diluted solution of an anionic surfactant (sodium aliphatate, etc., soap water is available), and then sequentially performing ultrasonic cleaning on the substrate for 10 minutes by using acetone, alcohol and deionized water, wherein the temperature is controlled at 0 ℃;
2. taking metal copper with the purity of 99.99 percent as a cathode target, connecting an anode with a vacuum chamber, installing the quartz substrate after ultrasonic cleaning on a substrate fixture, and arranging a movable baffle between the substrate fixture and the copper target;
3. the vacuum degree of the vacuum chamber is pumped to 6.0 × 10-4Pa and above, introducing reaction gas oxygen and sputtering gas argon into the vacuum chamber, so that the working pressure in the vacuum chamber is 0.8Pa, and the sputtering power is 150W;
4. after the working air pressure and the gas flow are stable, the copper target is pre-sputtered for 10-15min to remove oxides and impurities on the surface of the copper target.
5. And rotating the substrate fixture, moving the movable baffle plate, starting sputtering the film, and closing the movable baffle plate after sputtering for 10 minutes to obtain the single-phase transparent conductive cuprous oxide film.
Wherein, fig. 1 is an X-ray diffraction pattern of the transparent conductive cuprous oxide film measured according to the present invention, the intensity of the diffraction peak of which gradually becomes stronger; FIG. 2 is a graph of the square resistance of a transparent conductive cuprous oxide film according to the present invention, wherein the resistance of the square resistance becomes gradually smaller; fig. 3 is a graph showing an optical transmittance curve of the transparent conductive film according to the present invention, in which the optical transmittance is gradually decreased.
The above embodiments are merely basic illustrations of the concept of the present invention, and do not limit the present invention. Any equivalent changes made according to the technical scheme of the invention belong to the protection scope of the invention.
Claims (7)
1. A method for preparing a single-phase transparent conductive cuprous oxide film is characterized in that a direct-current reactive magnetron sputtering method is adopted at room temperature, a copper target material is used as a sputtering target material, oxygen is used as a reaction gas, argon is used as a sputtering gas, a cuprous oxide film is deposited on a substrate, and the cuprous oxide film is deposited under the condition that the vacuum degree is 6.0 × 10-4Pa and above in a vacuum chamber; wherein the sputtering power of the copper target is 40-150W, and the deposition time is 1-30 min; the flow rate of the oxygen is 2-30sccm, and the flow rate of the argon is 5-100 sccm.
2. The method of preparing a single-phase transparent conductive cuprous oxide film according to claim 1, comprising the steps of:
1) firstly, adopting an anionic surfactant to pre-clean a substrate;
2) sequentially carrying out ultrasonic cleaning on the substrate by adopting acetone, alcohol and deionized water, and regulating and controlling the temperature to be 0 ℃;
3) taking metal copper as a cathode target, connecting an anode with a vacuum chamber, mounting the substrate subjected to ultrasonic cleaning on a substrate fixture, and placing a movable baffle between the substrate fixture and the copper target;
4) the vacuum degree of the vacuum chamber is pumped to 6.0 × 10-4Pa and above, then introducing oxygen and argon into the vacuum chamber to ensure that the working pressure in the vacuum chamber is 0.8 Pa;
5) after the working air pressure and the gas flow are stable, sputtering the copper target for 10-15min in advance to remove oxides and impurities on the surface of the copper target;
6) and rotating the substrate fixture, moving the movable baffle plate, starting sputtering the film, and closing the movable baffle plate after sputtering is finished to obtain the single-phase transparent conductive cuprous oxide film.
3. The method of preparing a single-phase transparent conductive cuprous oxide film according to claim 1, wherein said single-phase transparent conductive cuprous oxide film comprises: the flow rate of the introduced oxygen is 5-30sccm, and the flow rate of the argon is 5-100 sccm.
4. The method of preparing a single-phase transparent conductive cuprous oxide film according to claim 1, wherein said single-phase transparent conductive cuprous oxide film comprises: the sputtering target is metallic copper with the purity of more than 99.99 percent.
5. The method of preparing a single-phase transparent conductive cuprous oxide film according to claim 1, wherein said single-phase transparent conductive cuprous oxide film comprises: the purity of the argon gas was 99.99%.
6. The method of preparing a single-phase transparent conductive cuprous oxide film according to claim 1, wherein said single-phase transparent conductive cuprous oxide film comprises: the purity of the oxygen was 99.99%.
7. The method of preparing a single-phase transparent conductive cuprous oxide film according to claim 1, wherein said single-phase transparent conductive cuprous oxide film comprises: wherein the substrate can be quartz, silicon wafer, crystal or glass.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106191797A (en) * | 2016-08-10 | 2016-12-07 | 上海理工大学 | A kind of preparation method of the tunable cuprous oxide film of preferred orientation |
CN106884144A (en) * | 2017-03-20 | 2017-06-23 | 广东工业大学 | The preparation method of N-shaped CuO films, transoid hetero-junctions |
CN109023284A (en) * | 2018-09-30 | 2018-12-18 | 广东工业大学 | A kind of complex multi layer films material and its preparation method and application with optical characteristics and rectifying effect |
CN109536990A (en) * | 2018-10-15 | 2019-03-29 | 华南理工大学 | A kind of flat thin-film electro catalyst operation electrode and its preparation method and application |
CN111364006A (en) * | 2020-04-03 | 2020-07-03 | 中国科学院长春应用化学研究所 | Method for preparing multi-valence metal oxide |
-
2016
- 2016-06-13 CN CN201610409769.8A patent/CN105821379A/en active Pending
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106191797A (en) * | 2016-08-10 | 2016-12-07 | 上海理工大学 | A kind of preparation method of the tunable cuprous oxide film of preferred orientation |
CN106884144A (en) * | 2017-03-20 | 2017-06-23 | 广东工业大学 | The preparation method of N-shaped CuO films, transoid hetero-junctions |
CN109023284A (en) * | 2018-09-30 | 2018-12-18 | 广东工业大学 | A kind of complex multi layer films material and its preparation method and application with optical characteristics and rectifying effect |
CN109536990A (en) * | 2018-10-15 | 2019-03-29 | 华南理工大学 | A kind of flat thin-film electro catalyst operation electrode and its preparation method and application |
CN111364006A (en) * | 2020-04-03 | 2020-07-03 | 中国科学院长春应用化学研究所 | Method for preparing multi-valence metal oxide |
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