CN112047308A - In2Se3Quantum dot and preparation method thereof - Google Patents
In2Se3Quantum dot and preparation method thereof Download PDFInfo
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- CN112047308A CN112047308A CN201910486169.5A CN201910486169A CN112047308A CN 112047308 A CN112047308 A CN 112047308A CN 201910486169 A CN201910486169 A CN 201910486169A CN 112047308 A CN112047308 A CN 112047308A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000002096 quantum dot Substances 0.000 claims abstract description 65
- 239000013078 crystal Substances 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000006228 supernatant Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 3
- 238000005191 phase separation Methods 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 abstract description 7
- 239000007788 liquid Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000000703 high-speed centrifugation Methods 0.000 abstract 1
- 239000002798 polar solvent Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 7
- 239000012071 phase Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 238000012876 topography Methods 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- PHPKKGYKGPCPMV-UHFFFAOYSA-N [SeH-]=[Se].[In+3].[SeH-]=[Se].[SeH-]=[Se] Chemical compound [SeH-]=[Se].[In+3].[SeH-]=[Se].[SeH-]=[Se] PHPKKGYKGPCPMV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- VSXOUQNLLPQTQK-UHFFFAOYSA-N selanylideneindium;selenium Chemical compound [Se].[In]=[Se].[In]=[Se] VSXOUQNLLPQTQK-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal chalcogenide Chemical class 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0573—Selenium; Compounds thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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Abstract
The invention discloses an In2Se3The quantum dot and the preparation method thereof comprise the following steps: in is formed by2Se3Taking crystal powder as raw material, and ultrasonically stripping In polar solvent to obtain In-containing2Se3The dispersion liquid of the quantum dots is firstly centrifuged at a low rotating speed, then supernatant liquid is taken, and then the quantum dots in the dispersion liquid are precipitated through high-speed centrifugation; washing the precipitate with absolute ethanol and drying at low temperature to obtain In2Se3A quantum dot powder. In provided by the invention2Se3The quantum dots have simple preparation conditions and low cost, and the obtained In2Se3The quantum dots have uniform size less than 5nm and high quality.
Description
Technical Field
The present invention relates to an In2Se3A quantum dot and a preparation method thereof belong to the field of preparation of two-dimensional crystal materials.
Background
Indium diselenide (In)2Se3) The alpha phase is a room temperature stable phase and has a layered structure, adjacent atoms in an atomic layer are combined through strong covalent bonds, and layers are connected through weak van der Waals force. In2Se3The material is a direct narrow-band-gap semiconductor material, and the band gap of the material can be changed within the range of 1.3eV to 2eV along with the difference of the number of atomic layers; has high carrier mobility (the theoretical value can reach 0.96 multiplied by 10)3cm2•V−1•s−1) The material has the characteristics of strong absorption and high photoresponse of a light wave band, good stability, in-plane anisotropy and the like, and has unique advantages which are not possessed by other two-dimensional crystal materials such as graphene, transition metal chalcogenide, black phosphorus and the like in the fields of microelectronics and photoelectrons.
Disclosure of Invention
It is an object of the present invention to provide an In2Se3Quantum dots and methods of making the same.
The technical solution for realizing the above purpose is as follows: in2Se3Quantum dot and preparation method thereof, In with uniform shape and controllable particle size is prepared on large scale by liquid phase stripping method2Se3Quantum dots, and obtaining In by centrifugal drying2Se3A quantum dot powder. The method specifically comprises the following steps:
in is separated by liquid phase separation2Se3Carrying out ultrasonic treatment on the crystal powder in an Isopropanol (IPA) solvent for 6h at the power of 450-600W, centrifuging for 20-30 min at 5000-8000 rmp/min to obtain a quantum dot supernatant, and centrifuging for 20-30 min at the centrifugation speed of 10000-11000 rmp/min to precipitate the quantum dots in the solution; washing the precipitate with anhydrous ethanol, and drying at a temperature of not higher than 100 deg.C.
Further, In2Se3The ratio of crystal powder to IPA was 0.2g:100 ml.
Further, the quantum dot supernatant was obtained after centrifugation at 7000 rmp/min for 20 min.
Further, the solution was centrifuged at a centrifugation rate of 10000rmp/min for 30min to precipitate the quantum dots in the solution.
Further, drying was carried out at 40 ℃.
Compared with the prior art, the invention has the advantages that: in is compared with nano material such as nano sheet2Se3The specific surface area of the quantum dot is increased, the absorption of light is increased, surface unsaturated bonds are increased, the activity is high, and more active sites are provided for catalytic reaction; the band gap of the material is widened, the reduction capability of conduction band electrons or the oxidation capability of valence band holes are increased, and In can be greatly improved2Se3Photocatalytic performance.
Drawings
FIG. 1 shows In prepared In example 12Se3XRD pattern of crystal powder of raw material used for quantum dot.
FIG. 2 shows In prepared In example 12Se3Raman diagram of crystal powder of raw materials used for quantum dots.
FIG. 3 shows In prepared In example 12Se3A physical diagram of the quantum dot dispersion.
FIG. 4 shows In prepared In example 12Se3And (3) carrying out a physical diagram on the quantum dot dispersion liquid under laser irradiation.
FIG. 5 shows In prepared In example 12Se3TEM topography of quantum dots.
FIG. 6 shows In prepared In example 12Se3Particle size statistical chart of quantum dots.
FIG. 7 shows In prepared In example 22Se3TEM topography of quantum dots.
FIG. 8 shows In prepared In example 22Se3Particle size statistical chart of quantum dots.
FIG. 9 shows In prepared In example 22Se3AFM topography of quantum dots.
FIG. 10 shows a portion of In prepared In example 22Se3Height map of quantum dots.
FIG. 11 shows In prepared In example 22Se3Height statistics of quantum dots.
Detailed Description
The invention will be described in more detail with reference to the following examples and the accompanying drawings
[ example 1 ]
Getting In2Se3Crystal powder (commercially available, J)&K) Putting 200 mg into a wide-mouth bottle, adding 100ml IPA solvent, performing ultrasonic accumulation for 6h at the power of 450W, centrifuging for 20min at 7000 rmp/min to obtain quantum dot supernatant, and centrifuging for 30min at the centrifugation rate of 10000rmp/min to precipitate the quantum dots in the solution; washing the precipitate with anhydrous ethanol for 3 times and drying at 40 deg.C to obtain In2Se3And (4) quantum dots.
Due to In2Se3Has a plurality of crystal phases and crystal forms, so that In is prepared2Se3Before quantum dots, it is necessary to determine the crystal phase and crystal form of the raw material crystal powder used. FIG. 1 and FIG. 2 show the preparation of In the present invention2Se3XRD and Raman patterns of the crystal raw material used for the quantum dots; as can be seen from FIG. 1, In was used as a raw material2Se3The crystal powder is matched with the rhombus alpha phase of a laminated structure, has high orientation along the c axis and has good crystallization. The Raman data of FIG. 2 further confirms that alpha phase In is present2Se3。
FIGS. 3 and 4 show In2Se3And (3) a quantum dot dispersion liquid object diagram. As can be seen from FIG. 3, In was prepared2Se3The quantum dot dispersion liquid is free of any obvious small particles and impurities; and no precipitate appears after long-time storage, and the product is stable. FIG. 4 shows In under laser irradiation2Se3The quantum dot dispersion has an obvious Tyndall phenomenon. The resulting mixed system was shown to be homogeneous and a colloid with particle size in the nanometer range dispersed in the supernatant.
FIGS. 5 and 6 show In2Se3TEM morphology and particle size statistic of quantum dots. As can be seen from FIG. 5, after being subjected to ultrasonic treatment for 6h at 450W and centrifugal screening at 7000 rmp/min, the quantum dots are relatively uniform in distribution and clear in morphology, the shape of each quantum dot is approximately spherical, the particle sizes of 100 quantum dots in the quantum dots are counted to obtain a graph 6, the particle size distribution of the quantum dots is in accordance with normal distribution, most of the particle sizes are between 1.6nm and 3.0nm and are about 1.6nm to 3.0nm90% of the total, In2Se3The average grain diameter of the quantum dots is 2.3 nm.
[ example 2 ]
Getting In2Se3Putting 200 mg of crystal powder into a wide-mouth bottle, adding 100ml of IPA solvent, performing ultrasonic accumulation for 6 hours at the power of 600W, centrifuging for 20 minutes at 7000 rmp/min to obtain quantum dot supernatant, and centrifuging for 30 minutes at the centrifugation rate of 10000rmp/min to precipitate the quantum dots in the solution; washing the precipitate with anhydrous ethanol for 3 times and drying at 40 deg.C to obtain In2Se3And (4) quantum dots.
FIGS. 7 and 8 show In2Se3TEM morphology and particle size statistic of quantum dots. As can be seen from FIG. 7, after being subjected to ultrasonic treatment for 6h at 600W, the quantum dots are relatively uniformly distributed and have clear morphology after being subjected to centrifugal screening at 7000 rmp/min, the shape of each quantum dot is approximately spherical, the particle sizes of 100 quantum dots In the quantum dots are counted to obtain a graph 8, the particle size distribution of the quantum dots is known to be In accordance with normal distribution, most of the particle sizes are between 1.4nm and 2.2nm, the particle sizes account for about 85 percent of the total number, and In2Se3The average grain diameter of the quantum dots is 1.8 nm.
FIG. 9, FIG. 10, FIG. 11 are In prepared2Se3AFM topography of quantum dots and their height data. FIG. 10 shows In through which three straight lines In FIG. 9 pass2Se3The quantum dot height diagram shows that the curve has obvious step shape corresponding to the layered structure. FIG. 11 shows 100 In2Se3From the high statistical data obtained for the quantum dots, it can be seen that In2Se3The height of the quantum dots is mostly between 1nm and 3nm, and the average height is about 2 nm. Due to a single layer of In2Se3(Se-In-Se 5 layer atoms) thickness was about 1nm, so that In was prepared2Se3The quantum dots are 2 layers on average.
Claims (7)
1. In2Se3The preparation method of the quantum dot is characterized by comprising the following steps:
in is separated by liquid phase separation2Se3Crystalline powder in isopropylCarrying out ultrasonic treatment for 6h in an alcohol solvent at the power of 450-600W, centrifuging for 20-30 min at the speed of 5000-8000 rmp/min to obtain a quantum dot supernatant, and centrifuging for 20-30 min at the centrifugal speed of 10000-11000 rmp/min to precipitate the quantum dots in the solution; washing the precipitate with anhydrous ethanol, and drying at a temperature of not higher than 100 deg.C.
2. The method of claim 1, wherein In2Se3The ratio of the crystal powder to isopropanol was 0.2g to 100 ml.
3. The method of claim 1, wherein the quantum dot supernatant is obtained after 20min of 7000 rmp/min centrifugation.
4. The method of claim 1, wherein the quantum dots in the solution are precipitated by centrifugation at a centrifugation rate of 10000rmp/min for 30 min.
5. The method of claim 1, wherein drying is at 40 ℃.
6. In prepared by the method of any one of claims 1 to 52Se3And (4) quantum dots.
7. In according to claim 62Se3Quantum dot characterized by In2Se3The quantum dot size is less than 5 nm.
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| CN201910486169.5A CN112047308B (en) | 2019-06-05 | 2019-06-05 | In 2 Se 3 Quantum dot and preparation method thereof |
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| CN201910486169.5A CN112047308B (en) | 2019-06-05 | 2019-06-05 | In 2 Se 3 Quantum dot and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102445223A (en) * | 2011-09-23 | 2012-05-09 | 苏州大学 | Photoelectric sensor |
| CN107234244A (en) * | 2017-06-23 | 2017-10-10 | 南京理工大学 | A kind of ultrasonic liquid-phase strip preparation method of big yield antimony alkene quantum dot |
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2019
- 2019-06-05 CN CN201910486169.5A patent/CN112047308B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102445223A (en) * | 2011-09-23 | 2012-05-09 | 苏州大学 | Photoelectric sensor |
| CN107234244A (en) * | 2017-06-23 | 2017-10-10 | 南京理工大学 | A kind of ultrasonic liquid-phase strip preparation method of big yield antimony alkene quantum dot |
Non-Patent Citations (3)
| Title |
|---|
| LIQIANG LU等: "Large-scale synthesis of defect-selective graphene quantum dots by ultrasonic-assisted liquid-phase exfoliation", 《CARBON》 * |
| XIAO FU等: "Tunable UV-Visible Absorption of SnS2 Layered Quantum Dots Produced by Liquid Phase Exfoliation", 《NANOSCALE》 * |
| XIAO ZHANG等: "Black Phosphorus Quantum Dots", 《ANGEWANDTE CHEMIE INTERNATIONAL EDITION》 * |
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