CN105551946A - Preparation method for stannous sulfide nanosheet and photoelectric detector prepared based on stannous sulfide nanosheet - Google Patents
Preparation method for stannous sulfide nanosheet and photoelectric detector prepared based on stannous sulfide nanosheet Download PDFInfo
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- CN105551946A CN105551946A CN201610013223.0A CN201610013223A CN105551946A CN 105551946 A CN105551946 A CN 105551946A CN 201610013223 A CN201610013223 A CN 201610013223A CN 105551946 A CN105551946 A CN 105551946A
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- DZXKSFDSPBRJPS-UHFFFAOYSA-N tin(2+);sulfide Chemical compound [S-2].[Sn+2] DZXKSFDSPBRJPS-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000002135 nanosheet Substances 0.000 title abstract 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 96
- 239000010453 quartz Substances 0.000 claims abstract description 86
- 239000000758 substrate Substances 0.000 claims abstract description 21
- 239000011261 inert gas Substances 0.000 claims abstract description 19
- 239000007789 gas Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000009413 insulation Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- 239000003708 ampul Substances 0.000 claims description 53
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 5
- 238000007669 thermal treatment Methods 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001259 photo etching Methods 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 76
- 238000000034 method Methods 0.000 abstract description 15
- 229910052681 coesite Inorganic materials 0.000 abstract description 5
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 5
- 239000000377 silicon dioxide Substances 0.000 abstract description 5
- 229910052682 stishovite Inorganic materials 0.000 abstract description 5
- 229910052905 tridymite Inorganic materials 0.000 abstract description 5
- 238000001816 cooling Methods 0.000 abstract 2
- 238000005240 physical vapour deposition Methods 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000005273 aeration Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical group Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/20—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy
- H01L21/203—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy using physical deposition, e.g. vacuum deposition, sputtering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
-
- 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
- H01L31/0248—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
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
-
- 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
Abstract
The invention discloses a preparation method for a stannous sulfide nanosheet and a photoelectric detector prepared based on the stannous sulfide nanosheet. The preparation method comprises the following steps of putting stannous sulfide powder into a clean quartz boat; enabling a completely washed SiO2/Si substrate to be horizontally placed above the quartz boat; then putting the quartz boat in a middle position of a quartz tube heating region, and sealing the quartz tube; pumping inert gas to the quartz tube and maintaining for 10-30min so as to completely exhaust air from the quartz tube; heating the quartz tube to 700-750 DEG C, and reducing gas flow of the inert gas in the heating process; performing thermal insulation for a high temperature region at a temperature of 700-720 DEG C of the quartz tube for 6-12min, and then naturally cooling; after the temperature of the quartz tube is naturally cooled to 560-600 DEG C, pushing the whole quartz tube out of a tubular furnace, and performing rapid cooling; and when the quartz tube is cooled to room temperature, opening the quartz tube and taking out a sample to finish the preparation of the sample. By adoption of the preparation method, the high-quality stannous sulfide nanosheet can be prepared by a simple physical vapor deposition method.
Description
Technical field
The present invention relates to novel energy resource material technology field, the preparation method being specifically related to a kind of stannous sulfide nanometer sheet and the photodetector prepared based on it.
Background technology
In recent years, the discovery of stratified nano materials Graphene, makes two-dimensional layer nano material obtain extensive concern and the research of people.And as the representative of two-dimensional layer semi-conducting material, laminated metal chalcogenide has unique property and structure because of it, at opto-electronic device, photovoltaic industry, catalysis, the aspect such as stored energy and conversion has application prospect widely.
Stannous sulfide is as the important a member in the sulfide of laminated metal, be a kind of cavity type there is rhombic layered semiconductor compound, combined by relatively weak Van der Waals force between layers, it has optics direct band gap 1.2-1.5eV and indirect band gap 1.0-1.2eV.Because stannous sulfide has narrower band gap, rich content, the advantages such as price is low and non-toxic, stannous sulfide is widely used in solar cell, photodetection, air-sensitive, the field such as ultracapacitor and lithium ion battery.Nowadays the method preparing stannous sulfide is a lot, as hydro-thermal-solvent thermal process, and sputtering method, chemical vapour deposition technique etc.But lack the method for the high-quality stannous sulfide nanometer sheet of simple preparation.Although the people such as J.Ahn deliver on NANOLETTER " DeterministicTwo-DimensionalPolymorphismGrowthofHexagona ln-TypeSnS2andOrthorhombicp-TypeSnSCrystals; 2015; 15; 3703-3708; " the high-quality stannous sulfide nanometer sheet that utilized the method for chemical vapour deposition (CVD) to prepare in paper, but this preparation method's process is complicated, and uses inflammable and explosive hydrogen as reducing gas, and operational danger is high.
Therefore, be badly in need of utilizing straightforward procedure to prepare high-quality stannous sulfide nanometer sheet in Infrared Detectors, and utilize this nanometer sheet to prepare the photodetector with good photoelectric respone.
Summary of the invention
For the deficiency in above-mentioned existing research, main purpose of the present invention is to provide a kind of method of the high-quality stannous sulfide nanometer sheet that utilized simple physical gas-phase deposite method to prepare, and on the basis of this high-quality stannous sulfide nanometer sheet, prepared corresponding photodetector, and find that this photodetector has extraordinary photoelectric respone to infrared light through experiment test, be very beneficial for business-like applying.
For achieving the above object, technical scheme disclosed by the invention is: a kind of preparation method of stannous sulfide nanometer sheet, described preparation method comprises the steps:
Step 1, stannous sulfide powder is placed in clean quartz boat, by the SiO cleaned up
2/ Si substrate lies in a horizontal plane in directly over quartz boat.Then quartz boat is placed on the centre position of the quartz ampoule thermal treatment zone, closed quartz tube;
Step 2, pass in quartz ampoule inert gas and continue 10-30min so that by the air emptying in quartz ampoule;
Step 3, by quartz ampoule heating rise to 700-750 DEG C; The throughput of inert gas is turned down in temperature-rise period;
Step 4, be the high-temperature region insulation 6-12min of 700-720 DEG C in temperature by quartz ampoule, then allow its Temperature fall;
Step 5, after quartz ampoule Temperature fall is to 560-600 DEG C, by quartz ampoule entirety release tube furnace lower the temperature rapidly outward;
Step 6, when quartz ampoule temperature is down to room temperature, open quartz ampoule take out sample, sample preparation completes, and obtains stannous sulfide nanometer sheet.
Preferably, SiO described in step 1
2the cleaning operation of/Si substrate is: first by SiO
2/ Si substrate is at H
2sO
4: H
2o
2in 3:(1-1.5) the mixed liquor that is made into of ratio in soak 1-2h, then use the ultrasonic cleaning successively of deionized water, acetone, alcohol, deionized water, finally obtain clean SiO
2/ Si substrate.
Preferably, the flow of the inert gas passed in step 2 is between 270-300sccm.
Preferably, turn the throughput of inert gas in the temperature-rise period described in step 3 down, concrete operations are: when quartz ampoule is heated to 380-400 DEG C, throughput are turned down to 18-22sccm; When quartz ampoule is heated to 580-610 DEG C, throughput is turned down to 4-6sccm.
Preferably, the inert gas passed in step 2 is argon gas or nitrogen.
The invention also discloses a kind of photoelectric device prepared according to above-mentioned stannous sulfide nanometer sheet, utilize the technology such as photoetching to be prepared into photoelectric device stannous sulfide nanometer sheet, and utilize the testing photoelectronic devices such as CHI660D electrochemical workstation to the photoresponse of infrared light.
Compare with reported in literature with prior art, the advantage that the present invention has is: what the inventive method adopted is easy high temperature process furnances, low production cost, and the gas adopted in experiment preparation process is argon gas or the nitrogen of inertia, has higher processing safety compared to inflammable and explosive property gases such as the application hydrogen reported in other technologies or document.And the stannous sulfide nanometer sheet obtained to have crystalline quality high, the advantages such as yardstick is large; And the photoelectric device made has extraordinary response to infrared light.
The invention has the beneficial effects as follows: the method for the present invention's high-quality stannous sulfide nanometer sheet that utilized simple physical gas-phase deposite method to prepare, and on the basis of this high-quality stannous sulfide nanometer sheet, prepared corresponding photodetector, and find that this photodetector has extraordinary photoelectric respone to infrared light through experiment test, be very beneficial for business-like applying.
Accompanying drawing explanation
Fig. 1 is the light microscope figure of the stannous sulfide nanometer sheet of preparation in embodiment 1;
Fig. 2 is the Raman figure of the stannous sulfide nanometer sheet of preparation in embodiment 1;
Fig. 3 is infrared light (638nm) response curve of the device made in embodiment 1.
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
Please refer to accompanying drawing 1-3, the embodiment of the present invention comprises:
Embodiment 1: a kind of preparation method of stannous sulfide nanometer sheet, specifically comprises the steps:
Step 1: first by SiO
2/ Si substrate is at H
2sO
4: H
2o
2soak 1h in the mixed liquor be made in the ratio of 3:1, then once use deionized water, acetone, alcohol, deionized water ultrasonic cleaning, obtain clean SiO2/Si substrate.Then 0.02g stannous sulfide powder is placed in clean quartz boat, the SiO2/Si substrate cleaned up is lain in a horizontal plane in directly over quartz boat; Quartz boat is placed on the centre position of the quartz ampoule thermal treatment zone, closed quartz tube;
Step 2: pass into inert gas argon gas or nitrogen as protective gas in quartz ampoule, the throughput passed into is 300sccm, and the air in quartz ampoule is discharged by Continuous aeration for 20 minutes completely;
Step 3: heated quarty tube: by quartz ampoule heat temperature raising, and in temperature-rise period, when temperature rises to 400 DEG C, turns down throughput to 20sccm; When temperature rises to 600 DEG C, again throughput is turned down to 5sccm; Quartz ampoule is finally made to be warming up to 720 DEG C;
Step 4: by quartz ampoule 720 DEG C of insulations 10 minutes, make it react completely and deposit nanometer sheet in substrate; Then its Temperature fall is allowed.
Step 5: quartz ampoule entirety, to after 600 DEG C, is released tube furnace rapidly and lowered the temperature outward by quartz ampoule Temperature fall;
Step 6: when quartz ampoule temperature is down to room temperature, open quartz ampoule and take out sample, sample preparation completes.
The light microscope figure of the stannous sulfide nanometer sheet prepared in this embodiment is shown in Fig. 1; The Raman figure of the stannous sulfide nanometer sheet prepared in this embodiment is shown in Fig. 2.
Embodiment 2: a kind of photoelectric device prepared by stannous sulfide nanometer sheet, stannous sulfide nanometer sheet embodiment 1 prepared utilizes the technological means such as photoetching to be made into photoelectric device, and utilize the testing photoelectronic devices such as CHI660D electrochemical workstation to the photoresponse of infrared light, infrared light (638nm) response curve of the photoelectric device made in the present embodiment is shown in Fig. 3, and result shows that this device has extraordinary photodetection performance.
Embodiment 3: a kind of preparation method of stannous sulfide nanometer sheet, described preparation method comprises the steps:
Step 1, stannous sulfide powder is placed in clean quartz boat, by the SiO cleaned up
2/ Si substrate lies in a horizontal plane in directly over quartz boat.Then quartz boat is placed on the centre position of the quartz ampoule thermal treatment zone, closed quartz tube;
Step 2, pass in quartz ampoule inert gas and continue 10-30min so that by the air emptying in quartz ampoule;
Step 3, by quartz ampoule heating rise to 700-750 DEG C; The throughput of inert gas is turned down in temperature-rise period;
Step 4, be the high-temperature region insulation 6-12min of 700-720 DEG C in temperature by quartz ampoule, then allow its Temperature fall;
Step 5, after quartz ampoule Temperature fall is to 560-600 DEG C, by quartz ampoule entirety release tube furnace lower the temperature rapidly outward;
Step 6, when quartz ampoule temperature is down to room temperature, open quartz ampoule take out sample, sample preparation completes, and obtains stannous sulfide nanometer sheet.
Embodiment 4: the difference of the present embodiment and embodiment 3 is, in the present embodiment, SiO described in step 1
2the cleaning operation of/Si substrate is: first by SiO
2/ Si substrate is at H
2sO
4: H
2o
2in 3:(1-1.5) the mixed liquor that is made into of ratio in soak 1-2h, then use the ultrasonic cleaning successively of deionized water, acetone, alcohol, deionized water, finally obtain clean SiO
2/ Si substrate.
Embodiment 5: the difference of the present embodiment and embodiment 3 is, in the present embodiment, the flow of the inert gas passed in step 2 is between 270-300sccm.
Embodiment 6: the difference of the present embodiment and embodiment 3 is, in the present embodiment, turn the throughput of inert gas in the temperature-rise period described in step 3 down, concrete operations are: when quartz ampoule is heated to 380-400 DEG C, throughput are turned down to 18-22sccm; When quartz ampoule is heated to 580-610 DEG C, throughput is turned down to 4-6sccm.
Embodiment 7: the difference of the present embodiment and embodiment 3 is, in the present embodiment, the inert gas passed in step 2 is argon gas or nitrogen.
Embodiment 8: a kind of preparation method of stannous sulfide nanometer sheet, specifically comprises the steps:
Step 1: first by SiO
2/ Si substrate is at H
2sO
4: H
2o
2soak 1h in the mixed liquor be made in the ratio of 3:1, then once use deionized water, acetone, alcohol, deionized water ultrasonic cleaning, obtain clean SiO2/Si substrate.Then 0.04g stannous sulfide powder is placed in clean quartz boat, the SiO2/Si substrate cleaned up is lain in a horizontal plane in directly over quartz boat; Quartz boat is placed on the centre position of the quartz ampoule thermal treatment zone, closed quartz tube;
Step 2: pass into inert gas argon gas or nitrogen as protective gas in quartz ampoule, the throughput passed into is 270sccm, and the air in quartz ampoule is discharged by Continuous aeration for 30 minutes completely;
Step 3: heated quarty tube: by quartz ampoule heat temperature raising, and in temperature-rise period, when temperature rises to 380 DEG C, turns down throughput to 22sccm; When temperature rises to 580 DEG C, again throughput is turned down to 6sccm; Quartz ampoule is finally made to be warming up to 720 DEG C;
Step 4: by quartz ampoule 720 DEG C of insulations 12 minutes, make it react completely and deposit nanometer sheet in substrate; Then its Temperature fall is allowed.
Step 5: quartz ampoule entirety, to after 500 DEG C, is released tube furnace rapidly and lowered the temperature outward by quartz ampoule Temperature fall;
Step 6: when quartz ampoule temperature is down to room temperature, open quartz ampoule and take out sample, sample preparation completes.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize specification of the present invention and accompanying drawing content to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (6)
1. a preparation method for stannous sulfide nanometer sheet, is characterized in that, described preparation method comprises the steps:
Step 1, stannous sulfide powder is placed in clean quartz boat, by the SiO cleaned up
2/ Si substrate lies in a horizontal plane in directly over quartz boat.Then quartz boat is placed on the centre position of the quartz ampoule thermal treatment zone, closed quartz tube;
Step 2, pass in quartz ampoule inert gas and continue 10-30min so that by the air emptying in quartz ampoule;
Step 3, by quartz ampoule heating rise to 700-750 DEG C; The throughput of inert gas is turned down in temperature-rise period;
Step 4, be the high-temperature region insulation 6-12min of 700-720 DEG C in temperature by quartz ampoule, then allow its Temperature fall;
Step 5, after quartz ampoule Temperature fall is to 560-600 DEG C, by quartz ampoule entirety release tube furnace lower the temperature rapidly outward;
Step 6, when quartz ampoule temperature is down to room temperature, open quartz ampoule take out sample, sample preparation completes, and obtains stannous sulfide nanometer sheet.
2. the preparation method of stannous sulfide nanometer sheet according to claim 1, is characterized in that, SiO described in step 1
2the cleaning operation of/Si substrate is: first by SiO
2/ Si substrate is at H
2sO
4: H
2o
2in 3:(1-1.5) the mixed liquor that is made into of ratio in soak 1-2h, then use the ultrasonic cleaning successively of deionized water, acetone, alcohol, deionized water, finally obtain clean SiO
2/ Si substrate.
3. the preparation method of stannous sulfide nanometer sheet according to claim 1, is characterized in that, the flow of the inert gas passed in step 2 is between 270-300sccm.
4. the preparation method of stannous sulfide nanometer sheet according to claim 1, it is characterized in that, turn the throughput of inert gas in temperature-rise period described in step 3 down, concrete operations are: when quartz ampoule is heated to 380-400 DEG C, throughput are turned down to 18-22sccm; When quartz ampoule is heated to 580-610 DEG C, throughput is turned down to 4-6sccm.
5., according to the preparation method of described stannous sulfide nanometer sheet arbitrary in claim 1-4, it is characterized in that, the inert gas passed in step 2 is argon gas or nitrogen.
6. the photoelectric device prepared according to described stannous sulfide nanometer sheet arbitrary in claim 1-5, it is characterized in that, utilize the technology such as photoetching to be prepared into photoelectric device stannous sulfide nanometer sheet, and utilize the testing photoelectronic devices such as CHI660D electrochemical workstation to the photoresponse of infrared light.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107555401A (en) * | 2017-08-08 | 2018-01-09 | 广东工业大学 | A kind of method for preparing stannous sulfide/Si oxide nuclear shell structure nano line |
CN115000233A (en) * | 2022-04-28 | 2022-09-02 | 华南师范大学 | Photodiode based on stannous sulfide/indium selenide heterojunction and preparation method and application thereof |
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