CN116565042B - Preparation method of self-assembled tin oxide and cadmium oxide nanostructure superlattice - Google Patents
Preparation method of self-assembled tin oxide and cadmium oxide nanostructure superlattice Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 46
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 title claims abstract description 35
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 title claims abstract description 35
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910001887 tin oxide Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 38
- 239000000843 powder Substances 0.000 claims abstract description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- VJQAXQXVZOKZSM-UHFFFAOYSA-N [O-2].[Cd+2].[Sn+2]=O.[O-2] Chemical compound [O-2].[Cd+2].[Sn+2]=O.[O-2] VJQAXQXVZOKZSM-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002244 precipitate Substances 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000000047 product Substances 0.000 claims abstract description 12
- QOYRNHQSZSCVOW-UHFFFAOYSA-N cadmium nitrate tetrahydrate Chemical compound O.O.O.O.[Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QOYRNHQSZSCVOW-UHFFFAOYSA-N 0.000 claims abstract description 10
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004246 zinc acetate Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- KHMOASUYFVRATF-UHFFFAOYSA-J tin(4+);tetrachloride;pentahydrate Chemical compound O.O.O.O.O.Cl[Sn](Cl)(Cl)Cl KHMOASUYFVRATF-UHFFFAOYSA-J 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 16
- 238000001514 detection method Methods 0.000 abstract description 8
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 abstract description 4
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 abstract description 4
- 238000003837 high-temperature calcination Methods 0.000 abstract description 2
- 230000000737 periodic effect Effects 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 3
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910002601 GaN Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BEQNOZDXPONEMR-UHFFFAOYSA-N cadmium;oxotin Chemical compound [Cd].[Sn]=O BEQNOZDXPONEMR-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005489 elastic deformation Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000003362 semiconductor superlattice Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- 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
- H01L31/0328—Inorganic materials including, apart from doping materials or other impurities, semiconductor materials provided for in two or more of groups H01L31/0272 - H01L31/032
- H01L31/0336—Inorganic materials including, apart from doping materials or other impurities, semiconductor materials provided for in two or more of groups H01L31/0272 - H01L31/032 in different semiconductor regions, e.g. Cu2X/CdX hetero-junctions, X being an element of Group VI of the Periodic System
- H01L31/03365—Inorganic materials including, apart from doping materials or other impurities, semiconductor materials provided for in two or more of groups H01L31/0272 - H01L31/032 in different semiconductor regions, e.g. Cu2X/CdX hetero-junctions, X being an element of Group VI of the Periodic System comprising only Cu2X / CdX heterojunctions, X being an element of Group VI of the Periodic System
-
- 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
- H01L31/0352—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 their shape or by the shapes, relative sizes or disposition of the semiconductor regions
- H01L31/035236—Superlattices; Multiple quantum well structures
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention belongs to the technical field of photoelectric detection, and particularly relates to a preparation method of a self-assembled tin oxide and cadmium oxide nano-structure superlattice, which comprises the following steps: zinc acetate, sodium hydroxide, stannic chloride pentahydrate and cadmium nitrate tetrahydrate are added into deionized water to be uniformly mixed, and completely dissolved to obtain precursor liquid; heating the precursor liquid at high temperature, and cooling to room temperature to obtain an initial white precipitate product; washing and centrifuging an initial white precipitate by alcohol and deionized water, and drying to obtain tin oxide cadmium oxide nano-structure superlattice precursor powder; and placing the tin oxide and cadmium oxide nano-structure superlattice precursor powder in a tube furnace for high-temperature calcination to obtain a target product. The superlattice structure obtained by the method has a short size and thickness, electrons have an energy level structure of ultraviolet bands in a quantum well formed by two materials alternately through artificial regulation, and the superlattice structure has very important significance in ultraviolet band detection.
Description
Technical Field
The invention belongs to the technical field of photoelectric detection, and particularly relates to a preparation method of a self-assembled tin oxide and cadmium oxide nano-structure superlattice.
Background
The semiconductor material is used as a particularly important part in photoelectric detection, and the change of the energy band structure can be realized by manually regulating the composition and structure of the semiconductor material. The semiconductor superlattice is an extremely important artificial lattice structure in a low-dimensional material, and after the periodic arrangement of the nano-scale thickness is realized through the artificial regulation and control of different materials, the coupling and the like among multiple quantum wells can be realized, the interaction between light and substances is promoted, and excellent and unique physical properties such as electron transmission, optical absorption and the like are shown. In addition, through regulating and controlling the thickness of the periodical nano material forming the superlattice, the binding effect of electrons can be realized, the energy level is further increased, and through further reducing the thickness, the utilization of photons of the electron energy level structure in an ultraviolet band can be realized, and the further development of a third class wide forbidden band semiconductor similar to silicon carbide, gallium nitride, zinc oxide and the like is expected to be realizedAnd (5) displaying. Early superlattice research was focused mainly on GaAs/Al x Ga 1-x As material, e.g. Ga, is also present thereafter x In 1-x As/GaAs、Ga x In 1-x As/InP、Si/Ge x Si 1-x The synthesis method of the strain superlattice composed of lattice elastic deformation mainly comprises the synthesis technologies of molecular beam epitaxy, metal organic chemical vapor deposition, electron beam exposure and the like, and the synthesis technologies still have the problems of complex operation, long preparation period and the like.
Disclosure of Invention
The invention provides a preparation method of a nano-structure superlattice material formed by self-assembly of tin oxide and cadmium oxide with close lattice constants. The preparation method is simple and efficient, has low cost, and can slowly and orderly form the superlattice material with periodic distribution and small material size and thickness in a high-temperature and high-pressure environment through van der Waals interaction force between the tin oxide and the cadmium oxide. The prepared self-assembled tin oxide and cadmium oxide nano-structure superlattice has the absorption characteristic in the ultraviolet band, and is a new generation of ultraviolet photoelectric detection semiconductor material with wide application prospect.
The invention is realized by the following technical scheme:
the preparation method of the self-assembled tin oxide and cadmium oxide nano-structure superlattice comprises the following steps:
step one: adding zinc acetate, sodium hydroxide, tin tetrachloride pentahydrate and cadmium nitrate tetrahydrate powder into deionized water, uniformly mixing, and continuously stirring the mixture at room temperature until the mixture is completely dissolved to obtain a required precursor solution;
step two: transferring the precursor liquid prepared in the first step into a reaction kettle for high-temperature heating, and obtaining an initial white precipitate product after the reaction kettle is cooled to room temperature;
step three: washing and centrifuging the initial white precipitate obtained in the second step by deionized water and alcohol, and drying to obtain tin oxide and cadmium oxide nano-structure superlattice precursor powder;
step four: and placing the tin oxide and cadmium oxide nano-structure superlattice precursor powder in a tube furnace for high-temperature calcination to obtain a target product.
Further, in the first step, analytically pure zinc acetate, sodium hydroxide, stannic chloride pentahydrate and cadmium nitrate tetrahydrate are added in a molar ratio of 1: 53-55: 10-12: 4-6.
In the second step, the precursor solution prepared in the first step is transferred to a reaction kettle, heated to 180-200 ℃ in a muffle furnace at a heating rate of 2 ℃/min, and then reacted for 16-20h.
Further, in the third step, the white precipitate is washed and centrifuged by deionized water for three times, and then centrifuged by ethanol for three times, and the centrifugation is carried out at 6000-9000rpm/min for 5-10min, and then dried in an oven for 2-4h, and the drying temperature is kept at 60 ℃.
In the fourth step, the superlattice precursor powder of the tin oxide and cadmium oxide nano structure is placed in a tube furnace, heated to 400-450 ℃ at a heating rate of 2 ℃/min, calcined at a high temperature for 1-2h, and naturally cooled.
In the fourth step, nitrogen is introduced into the tube furnace, so that the tin oxide and cadmium oxide nano-structure superlattice precursor powder is calcined at a high temperature in a nitrogen environment.
The beneficial effects of the invention are as follows:
1. according to the preparation method of the self-assembled tin oxide and cadmium oxide nano-structure superlattice, the materials with small mismatch degree of the two lattices of tin oxide and cadmium oxide are utilized, so that the materials are slowly and orderly embedded together under the action of Van der Waals force in a high-temperature and high-pressure environment to form a periodic superlattice structure with small size and thickness, and compared with the traditional semiconductor material, the preparation method has the advantages of high light utilization rate and good photoelectric conversion efficiency;
2. the preparation method has the advantages of simple process, high repeatability and easily available raw materials;
3. the self-assembled tin oxide and cadmium oxide nano-structure superlattice prepared by the invention has better application in photoelectric detection, and is especially suitable for photoelectric detection in ultraviolet band.
Drawings
FIG. 1 is a transmission electron microscope electron diffraction diagram of a self-assembled tin oxide cadmium oxide nanostructure superlattice prepared in accordance with the invention.
FIG. 2 is an X-ray diffraction pattern of a self-assembled cadmium tin oxide nanostructure superlattice prepared in accordance with the invention.
Fig. 3 and 4 are transmission electron microscope images of self-assembled tin oxide and cadmium oxide nanostructure superlattice prepared by the invention.
Fig. 5 is an ultraviolet-visible absorption spectrum of a self-assembled tin oxide cadmium oxide nanostructured superlattice prepared in accordance with the invention.
Detailed Description
The invention will be further described with reference to the drawings and the detailed description.
Embodiment one:
the preparation method of the self-assembled tin oxide and cadmium oxide nano-structure superlattice comprises the following steps:
step one, preparing a precursor liquid:
deionized water was weighed in a graduated cylinder, analytically pure zinc acetate was weighed using an electronic balance, added to deionized water, and magnetically stirred at room temperature until fully dissolved.
Analytically pure sodium hydroxide solid was weighed using an electronic balance, added to the above solution and magnetically stirred at room temperature until it was completely dissolved.
The analytically pure tin tetrachloride pentahydrate is weighed by using an electronic balance, added into the solution and magnetically stirred at room temperature until the solution is fully dissolved.
And weighing the analytically pure cadmium nitrate tetrahydrate by using an electronic balance, adding the analytically pure cadmium nitrate tetrahydrate into the solution, and fully magnetically stirring the solution at room temperature until the solution is fully dissolved.
The molar ratio of the weighed analytically pure zinc acetate, sodium hydroxide, stannic chloride pentahydrate and cadmium nitrate tetrahydrate is 1: 53-55: 10-12: 4-6.
And carrying out ultrasonic treatment on the obtained solution for 10 minutes to uniformly disperse the solution, thereby obtaining the precursor liquid required by the reaction.
Step two, preparing self-assembled tin oxide and cadmium oxide nano-structure superlattice precursor powder:
transferring the precursor liquid prepared in the step one into a 100ml polytetrafluoroethylene reaction kettle, placing the reaction kettle in a muffle furnace, heating the reaction kettle for 16 hours at the temperature rising rate of 2 ℃/min to 180 ℃ in the muffle furnace, and waiting for the hydrothermal reaction kettle to cool to room temperature to obtain a white precipitate product.
And washing and centrifuging the obtained white precipitate by deionized water for three times, centrifuging by ethanol for three times, keeping the centrifuging speed at 6000-9000rpm/min for 5-10min, transferring to an oven, drying for 2h, and keeping the drying temperature at 60 ℃ to obtain self-assembled tin oxide and cadmium oxide nano-structure superlattice precursor powder.
Step three, preparing a self-assembled tin oxide and cadmium oxide nano-structure superlattice:
grinding the precursor powder, placing the ground precursor powder into a crucible, transferring the crucible into a tube furnace, introducing nitrogen into the tube furnace, setting the heating rate of the tube furnace to be 2 ℃/min to 400 ℃, calcining at a high temperature for 1h, naturally cooling to room temperature, and obtaining the self-assembled tin oxide and cadmium oxide nano-structure superlattice.
Embodiment two:
the preparation method of the self-assembled tin oxide and cadmium oxide nano-structure superlattice comprises the following steps:
step one, preparing a precursor liquid:
deionized water was weighed in a graduated cylinder, analytically pure zinc acetate was weighed using an electronic balance, added to deionized water, and magnetically stirred at room temperature until fully dissolved.
Analytically pure sodium hydroxide solid was weighed using an electronic balance, added to the above solution and magnetically stirred at room temperature until it was completely dissolved.
The analytically pure tin tetrachloride pentahydrate is weighed by using an electronic balance, added into the solution and magnetically stirred at room temperature until the solution is fully dissolved.
And weighing the analytically pure cadmium nitrate tetrahydrate by using an electronic balance, adding the analytically pure cadmium nitrate tetrahydrate into the solution, and fully magnetically stirring the solution at room temperature until the solution is fully dissolved.
The molar ratio of the weighed analytically pure zinc acetate, sodium hydroxide, stannic chloride pentahydrate and cadmium nitrate tetrahydrate is 1: 53-55: 10-12: 4-6.
And carrying out ultrasonic treatment on the obtained solution for 10 minutes to uniformly disperse the solution, thereby obtaining the precursor liquid required by the reaction.
Step two, preparing self-assembled tin oxide and cadmium oxide nano-structure superlattice precursor powder:
transferring the precursor liquid prepared in the step one into a 100ml polytetrafluoroethylene reaction kettle, placing the reaction kettle in a muffle furnace, heating the reaction kettle for 20 hours at the temperature rising rate of 2 ℃/min to 200 ℃ in the muffle furnace, and waiting for the hydrothermal reaction kettle to cool to room temperature to obtain a white precipitate product.
And washing and centrifuging the obtained white precipitate by deionized water for three times, centrifuging by ethanol for three times, keeping the centrifuging speed at 6000-9000rpm/min for 5-10min, transferring to an oven, drying for 4h, and keeping the drying temperature at 60 ℃ to obtain self-assembled tin oxide and cadmium oxide nano-structure superlattice precursor powder.
Step three, preparing a self-assembled tin oxide and cadmium oxide nano-structure superlattice:
grinding the precursor powder, placing the ground precursor powder into a crucible, transferring the crucible into a tube furnace, introducing nitrogen into the tube furnace, setting the heating rate of the tube furnace to be 2 ℃/min to 450 ℃, calcining at a high temperature for 2 hours, naturally cooling to room temperature, and obtaining the self-assembled tin oxide and cadmium oxide nano-structure superlattice.
FIG. 1 is a transmission electron microscope electron diffraction diagram of a self-assembled tin oxide cadmium oxide nanostructure superlattice prepared according to the invention, wherein the existence of tin oxide and cadmium oxide heterostructures can be confirmed by the diffraction radius.
FIG. 2 is an X-ray diffraction pattern of a self-assembled tin oxide cadmium oxide nanostructure superlattice prepared in accordance with the invention, as compared to XRD peaks of standard tin oxide and cadmium oxide, to determine the tin oxide cadmium oxide heterostructure.
Fig. 3 and 4 are transmission electron microscope images of self-assembled tin oxide cadmium oxide nano-structure superlattice prepared by the invention, from which the superlattice structure of the tin oxide cadmium oxide nano-structure can be determined.
FIG. 5 is a graph of the ultraviolet-visible absorption spectrum of the self-assembled tin oxide cadmium oxide nanostructured superlattice prepared according to the invention, from which it can be seen that the prepared material has excellent ultraviolet absorption efficiency.
According to the invention, two materials of tin oxide and cadmium oxide with close lattice constants are selected to form an ordered periodic superlattice structure through van der Waals force self-assembly in a high-temperature and high-pressure environment, the periodic superlattice structure has a short size and thickness, electrons have an energy level structure of ultraviolet bands in a quantum well formed by the two materials alternately through artificial regulation, and the periodic superlattice structure has very important significance in ultraviolet band detection.
Claims (4)
1. The preparation method of the self-assembled tin oxide and cadmium oxide nano-structure superlattice is characterized by comprising the following steps of:
step one: analytically pure zinc acetate, sodium hydroxide, tin tetrachloride pentahydrate and cadmium nitrate tetrahydrate powder are mixed according to the molar ratio of 1: 53-55: 10-12: adding the solution into deionized water, uniformly mixing, and continuously stirring the mixture at room temperature until the mixture is completely dissolved to obtain a required precursor solution;
step two: transferring the precursor liquid prepared in the first step into a reaction kettle, heating to 180-200 ℃ in a muffle furnace at a heating rate of 2 ℃/min, reacting for 16-20h, and waiting for the reaction kettle to cool to room temperature to obtain an initial white precipitate product;
step three: washing and centrifuging the initial white precipitate obtained in the second step by alcohol and deionized water, and drying to obtain tin oxide cadmium oxide nano-structure superlattice precursor powder;
step four: placing the tin oxide cadmium oxide nano-structure superlattice precursor powder in a tube furnace, introducing nitrogen into the tube furnace, heating the tin oxide cadmium oxide nano-structure superlattice precursor powder to 400-450 ℃ at a heating rate of 2 ℃/min in a nitrogen environment, calcining at a high temperature for 1-2h, and naturally cooling to obtain a target product.
2. The method for preparing a self-assembled tin oxide-cadmium oxide nano-structure superlattice according to claim 1, wherein in the third step, the white precipitate is washed and centrifuged three times by deionized water and then centrifuged three times by ethanol, and the white precipitate is kept at 6000-9000rpm/min for 5-10min, and then dried in an oven for 2-4h, and the drying temperature is kept at 60 ℃.
3. The method for preparing a self-assembled tin oxide and cadmium oxide nano-structure superlattice according to claim 2, wherein the second step is as follows: transferring the precursor liquid prepared in the first step into a reaction kettle, heating to 180 ℃ in a muffle furnace at a heating rate of 2 ℃/min, reacting for 16 hours, and waiting for the reaction kettle to cool to room temperature to obtain an initial white precipitate product;
the third step is as follows: washing and centrifuging the white precipitate by deionized water for three times, centrifuging by ethanol for three times, keeping the centrifuging speed at 6000-9000rpm/min for 5-10min, drying in an oven for 2h, and keeping the drying temperature at 60 ℃ to obtain tin oxide and cadmium oxide nano-structure superlattice precursor powder;
the fourth step is as follows: placing the tin oxide cadmium oxide nano-structure superlattice precursor powder in a tube furnace, introducing nitrogen into the tube furnace, heating the tin oxide cadmium oxide nano-structure superlattice precursor powder to 400 ℃ at a heating rate of 2 ℃/min in a nitrogen environment, calcining at a high temperature for 1h, and naturally cooling to obtain a target product.
4. The method for preparing a self-assembled tin oxide and cadmium oxide nano-structure superlattice according to claim 2, wherein the second step is as follows: transferring the precursor liquid prepared in the first step into a reaction kettle, heating to 200 ℃ in a muffle furnace at a heating rate of 2 ℃/min, reacting for 20 hours, and waiting for the reaction kettle to cool to room temperature to obtain an initial white precipitate product;
the third step is as follows: washing and centrifuging the white precipitate by deionized water for three times, centrifuging by ethanol for three times, keeping the centrifuging speed at 6000-9000rpm/min for 5-10min, drying in an oven for 4h, and keeping the drying temperature at 60 ℃ to obtain tin oxide and cadmium oxide nano-structure superlattice precursor powder;
the fourth step is as follows: placing the tin oxide cadmium oxide nano-structure superlattice precursor powder in a tube furnace, introducing nitrogen into the tube furnace, heating the tin oxide cadmium oxide nano-structure superlattice precursor powder to 450 ℃ at a heating rate of 2 ℃/min in a nitrogen environment, calcining at a high temperature for 2 hours, and naturally cooling to obtain a target product.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102321917A (en) * | 2011-06-18 | 2012-01-18 | 中国科学院合肥物质科学研究院 | Preparation method for Si-doped alpha-Fe2O3 super-lattice nanostructure |
| CN102324320A (en) * | 2011-07-29 | 2012-01-18 | 上海奥威科技开发有限公司 | High-performance super capacitor |
| CN103303968A (en) * | 2013-04-28 | 2013-09-18 | 中国科学技术大学 | CdSnO3 nanometer material as well as preparation method and application thereof |
| CN103433038A (en) * | 2013-08-19 | 2013-12-11 | 江苏大学 | Hetero-structured copper oxide-composited titanium oxide nanowire array synthesized by hydrothermal method |
| KR20190115236A (en) * | 2018-04-02 | 2019-10-11 | 고려대학교 산학협력단 | 1-dimensional CdS/CdO core/shell nanostructured photoelectrodes for hydrogen generation via a solution process and the method for manufacturing the same |
| CN111239205A (en) * | 2020-01-30 | 2020-06-05 | 吉林大学 | Based on CdSnO3Isopropyl alcohol gas sensor of sensitive layer and preparation method thereof |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102321917A (en) * | 2011-06-18 | 2012-01-18 | 中国科学院合肥物质科学研究院 | Preparation method for Si-doped alpha-Fe2O3 super-lattice nanostructure |
| CN102324320A (en) * | 2011-07-29 | 2012-01-18 | 上海奥威科技开发有限公司 | High-performance super capacitor |
| CN103303968A (en) * | 2013-04-28 | 2013-09-18 | 中国科学技术大学 | CdSnO3 nanometer material as well as preparation method and application thereof |
| CN103433038A (en) * | 2013-08-19 | 2013-12-11 | 江苏大学 | Hetero-structured copper oxide-composited titanium oxide nanowire array synthesized by hydrothermal method |
| KR20190115236A (en) * | 2018-04-02 | 2019-10-11 | 고려대학교 산학협력단 | 1-dimensional CdS/CdO core/shell nanostructured photoelectrodes for hydrogen generation via a solution process and the method for manufacturing the same |
| CN111239205A (en) * | 2020-01-30 | 2020-06-05 | 吉林大学 | Based on CdSnO3Isopropyl alcohol gas sensor of sensitive layer and preparation method thereof |
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