CN105621487B - A kind of preparation method of Molybdenum Oxide Thin Films by Sol-Gel and the photoelectric device of preparation - Google Patents
A kind of preparation method of Molybdenum Oxide Thin Films by Sol-Gel and the photoelectric device of preparation Download PDFInfo
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- CN105621487B CN105621487B CN201610121111.7A CN201610121111A CN105621487B CN 105621487 B CN105621487 B CN 105621487B CN 201610121111 A CN201610121111 A CN 201610121111A CN 105621487 B CN105621487 B CN 105621487B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229910000476 molybdenum oxide Inorganic materials 0.000 title claims abstract description 16
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 239000010409 thin film Substances 0.000 title claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000010453 quartz Substances 0.000 claims abstract description 30
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000003708 ampul Substances 0.000 claims abstract description 15
- 239000011261 inert gas Substances 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 5
- 238000010792 warming Methods 0.000 claims abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910052681 coesite Inorganic materials 0.000 claims description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 229910052682 stishovite Inorganic materials 0.000 claims description 4
- 229910052905 tridymite Inorganic materials 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000005240 physical vapour deposition Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000001259 photo etching Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 229910002704 AlGaN Inorganic materials 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
-
- H—ELECTRICITY
- 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
- H01L31/08—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 in which radiation controls flow of current through the device, e.g. photoresistors
- H01L31/09—Devices sensitive to infrared, visible or ultraviolet radiation
-
- H—ELECTRICITY
- 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
- H01L31/08—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 in which radiation controls flow of current through the device, e.g. photoresistors
- H01L31/10—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 in which radiation controls flow of current through the device, e.g. photoresistors characterised by potential barriers, e.g. phototransistors
- H01L31/101—Devices sensitive to infrared, visible or ultraviolet radiation
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- General Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of preparation method of Molybdenum Oxide Thin Films by Sol-Gel and the photoelectric device of preparation, comprise the steps of：Step a, molybdenum trioxide powder is placed in quartz boat, and the S cleaned up is kept flat directly over quartz boatiO2/SiSubstrate, quartz boat is placed in the quartz ampoule of high temperature process furnances and sealed；Step b, inert gas is passed through into quartz ampoule to empty the air in pipe completely, turns the throughput of inert gas down, and high temperature process furnances is warming up to 750 850 DEG C, after complete reaction Temperature fall；Step c, sample is taken out when the temperature of quartz ampoule reaches room temperature, sample preparation is completed.By the above-mentioned means, the present invention can prepare Molybdenum Oxide Thin Films by Sol-Gel using normal pressure physical vapour deposition (PVD) mode in laboratory conditions, production method is simple, convenient.
Description
Technical field
The present invention relates to novel energy resource material technology field, more particularly to a kind of Molybdenum Oxide Thin Films by Sol-Gel for ultraviolet detector
Preparation method.
Background technology
Ultraviolet detector is widely used in military, industrial production and daily life as a kind of important photoelectric device
Etc. every field, such as ozone monitoring, fire hazard monitoring and missile defense systems；The major parameter of evaluation detector performance has switch
When speed of photoresponse, on-off ratio is bigger, the performance of the faster explanation detector of speed of photoresponse is better, has nowadays developed more
The ultraviolet detector of kind material base, such as zno-based ultraviolet detector, GaN base ultraviolet detector, AlGaN base ultraviolet detectors, but
Highly sensitive detector is the target that every field is pursued always.
Molybdenum trioxide is a kind of layered semiconductor material, its band gap is 3.2eV, can be applied to electrochromism, super electricity
The field such as appearance, Li ion batteries, solar cell and photovoltaic device；Nowadays a variety of methods prepare molybdenum trioxide thin
Film, such as the preparation method such as hydro-thermal-solvent-thermal method, sol-gal process and magnetron sputtering, but now lack one kind and prepare high quality
The method of two-dimentional molybdenum trioxide；Based on this background, applicant is prepared for high quality two using the method for normal pressure physical vapour deposition (PVD)
Tie up Molybdenum Oxide Thin Films by Sol-Gel；And photodetector is prepared for using the Molybdenum Oxide Thin Films by Sol-Gel of preparation, find molybdenum trioxide by experiment
Base detector has very high response sensitivity to ultraviolet light, is very beneficial for industry popularization.
The content of the invention
It is an object of the invention to the characteristic for molybdenum trioxide, there is provided three convenient and simple for ultraviolet detector
The preparation method of Electrochromic Molybdenum Oxide Coatings.
To achieve the above object, technical solution disclosed by the invention is：A kind of preparation method of Molybdenum Oxide Thin Films by Sol-Gel, including
Following steps：
Step a, molybdenum trioxide powder is placed in quartz boat, and the S cleaned up is kept flat directly over quartz boatiO2/
SiSubstrate, quartz boat is placed in the quartz ampoule of high temperature process furnances and sealed；
Step b, inert gas is passed through into quartz ampoule to empty the air in pipe completely, turns the air-flow of inert gas down
Measure, and high temperature process furnances is warming up to 750-850 DEG C, after complete reaction Temperature fall；
Step c, sample is taken out when the temperature of quartz ampoule reaches room temperature, sample preparation is completed；
Preferably, in the step a, S is cleanediO2/SiDuring substrate, first with acetone, each ultrasound 20-30min of isopropanol,
Then by SiO2/SiSubstrate is put into H2O2And H2SO4Mixed solution in clean 2-4h, finally cleaned with deionized water.
Preferably, the H2O2And H2SO4Volume ratio in mixed solution is 1:3.
Preferably, the inert gas used in the step b is argon gas or nitrogen.
Preferably, the heating rate of the step b high temperature tube furnaces is 20 DEG C/min-40 DEG C/min.
The invention also discloses a kind of photoelectric device, Molybdenum Oxide Thin Films by Sol-Gel prepared by the photoelectric device method described above is
Material, is prepared by modes such as photoetching, electron beam exposures.
The beneficial effects of the invention are as follows：The present invention can utilize normal pressure physical vapour deposition (PVD) mode system in laboratory conditions
Standby Molybdenum Oxide Thin Films by Sol-Gel, production method is simple, editor.
Brief description of the drawings
Fig. 1 is the Raman figures of the sample prepared in embodiment 2.
Embodiment
Presently preferred embodiments of the present invention is described in detail below in conjunction with the accompanying drawings, so that advantages and features of the invention energy
It is easier to be readily appreciated by one skilled in the art, so as to make a clearer definition of the protection scope of the present invention.
Attached drawing 1 is refer to, the embodiment of the present invention includes:
Embodiment 1：A kind of preparation method of Molybdenum Oxide Thin Films by Sol-Gel, comprises the steps of：
Step a, molybdenum trioxide powder is placed in quartz boat, and the S cleaned up is kept flat directly over quartz boatiO2/
SiSubstrate, quartz boat is placed in the quartz ampoule of high temperature process furnances and sealed；
Step b, inert gas is passed through into quartz ampoule to empty the air in pipe completely, turns the air-flow of inert gas down
Measure, and high temperature process furnances is warming up to 750-850 DEG C, after complete reaction Temperature fall；
Step c, sample is taken out when the temperature of quartz ampoule reaches room temperature, sample preparation is completed.
In the step a, S is cleanediO2/SiDuring substrate, first with acetone, each ultrasound 20-30min of isopropanol, then will
SiO2/SiSubstrate is put into H2O2And H2SO4Mixed solution in clean 2-4h, finally cleaned with deionized water.
The H2O2And H2SO4Volume ratio in mixed solution is 1:3.
The inert gas used in the step b is argon gas or nitrogen.
The heating rate of the step b high temperature tube furnaces is 20 DEG C/min-40 DEG C/min.
Embodiment 2：A kind of preparation method of Molybdenum Oxide Thin Films by Sol-Gel, is specially：S is cleaned firstiO2/SiSubstrate, with acetone,
Each ultrasound 20min of isopropanol, is then placed in H2O2：H2SO4=1:2h is cleaned in 3 mixed solution, it is finally clear with deionized water
Wash；A certain amount of molybdenum trioxide powder is placed in quartz boat, and keep flat directly over quartz boat size as 1cm × 1cm and
The S cleaned upiO2/SiSubstrate, quartz boat is placed in the quartz ampoule of high temperature process furnances and sealed；Argon is passed through into quartz ampoule
The inert gases such as gas empty the air in pipe completely；Setting high temperature process furnances are warming up to 800 DEG C with what is determined with 26 DEG C/min,
Wherein throughput is turned down after temperature reaches 400 DEG C, 1min is kept the temperature when temperature reaches 800 DEG C, Temperature fall after the reaction was complete；
Sample is taken out when the temperature of quartz ampoule reaches room temperature, sample preparation is completed.
Embodiment 3：A kind of photoelectric device, using photoetching, electron beam exposure method embodiment 1 Molybdenum Oxide Thin Films by Sol-Gel
On prepare Molybdenum Oxide Thin Films by Sol-Gel base photoelectric device.And device detection is carried out to photoelectric device：The instrument used is CHI electrochemistry work
Stand, the results showed that the device has good photoelectricity sensitivity.
The foregoing is merely the embodiment of the present invention, is not intended to limit the scope of the invention, every to utilize this hair
The equivalent structure or equivalent flow shift that bright specification and accompanying drawing content are made, is directly or indirectly used in other relevant skills
Art field, is included within the scope of the present invention.
Claims (1)
1. a kind of preparation method of Molybdenum Oxide Thin Films by Sol-Gel, it is characterised in that comprise the steps of：
Step a, molybdenum trioxide powder is placed in quartz boat, and the S cleaned up is kept flat directly over quartz boatiO2/SiBase
Bottom, quartz boat is placed in the quartz ampoule of high temperature process furnances and sealed, and cleans SiO2/SiDuring substrate, first with acetone, isopropanol
Each ultrasound 20-30min, then by SiO2/SiSubstrate is put into volume ratio as 1:3 H2O2And H2SO4Mixed solution in clean 2-
4h, is finally cleaned with deionized water；
Step b, inert gas is passed through into quartz ampoule to empty the air in pipe completely, turns the throughput of inert gas down, and
High temperature process furnances are made to be warming up to 750-850 DEG C, after complete reaction Temperature fall, inert gas is argon gas or nitrogen, high temperature pipe
The heating rate of formula stove is 20 DEG C/min -40 DEG C/min；
Step c, sample is taken out when the temperature of quartz ampoule reaches room temperature, sample preparation is completed.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610121111.7A CN105621487B (en) | 2016-03-03 | 2016-03-03 | A kind of preparation method of Molybdenum Oxide Thin Films by Sol-Gel and the photoelectric device of preparation |
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| CN201610121111.7A CN105621487B (en) | 2016-03-03 | 2016-03-03 | A kind of preparation method of Molybdenum Oxide Thin Films by Sol-Gel and the photoelectric device of preparation |
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| CN105621487B true CN105621487B (en) | 2018-05-08 |
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| CN106637089A (en) * | 2016-12-27 | 2017-05-10 | 苏州思创源博电子科技有限公司 | Preparation method of ultraviolet detecting film |
| CN115799459A (en) * | 2023-02-06 | 2023-03-14 | 昆山美淼新材料科技有限公司 | Production process of graphene modified metal electrode |
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| CN101503215A (en) * | 2009-03-10 | 2009-08-12 | 中国地质大学（武汉） | Preparation of photochromic MoO3 film |
| CN104167491B (en) * | 2014-07-02 | 2017-10-17 | 苏州大学 | Preparation method of metal oxide water-soluble film |
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