CN112047308B - In 2 Se 3 Quantum dot and preparation method thereof - Google Patents
In 2 Se 3 Quantum dot and preparation method thereof Download PDFInfo
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- CN112047308B CN112047308B CN201910486169.5A CN201910486169A CN112047308B CN 112047308 B CN112047308 B CN 112047308B CN 201910486169 A CN201910486169 A CN 201910486169A CN 112047308 B CN112047308 B CN 112047308B
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000006228 supernatant Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 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 14
- 238000005119 centrifugation Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 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 5
- 238000000703 high-speed centrifugation Methods 0.000 abstract 1
- 239000002798 polar solvent Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 16
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 150000001875 compounds Chemical class 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
- 238000004519 manufacturing process Methods 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
- 230000003287 optical effect Effects 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 238000001556 precipitation 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
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- 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
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- 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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Abstract
The invention discloses an In 2 Se 3 The quantum dot and the preparation method thereof comprise the following steps: in is formed by 2 Se 3 Taking crystal powder as raw material, and ultrasonically stripping In polar solvent to obtain In-containing 2 Se 3 The dispersion liquid of the quantum dots is firstly centrifuged at a lower 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 In 2 Se 3 A quantum dot powder. In provided by the invention 2 Se 3 The quantum dots have simple preparation conditions and low cost, and the obtained In 2 Se 3 The quantum dots have uniform size less than 5nm and high quality.
Description
Technical Field
The present invention relates to an In 2 Se 3 A quantum dot and a preparation method thereof belong to the field of preparation of two-dimensional crystal materials.
Background
Indium diselenide (In) 2 Se 3 ) The compound is an important III-VI main group compound and has various crystal forms, wherein an 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 the layers are connected through weak van der Waals force. In 2 Se 3 The 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) 3 cm 2 •V −1 •s −1 ) For the visible light waveThe section has the properties of strong absorption, high optical response, 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 In 2 Se 3 Quantum dots and methods of making the same.
The technical solution for realizing the above purpose is as follows: in 2 Se 3 Quantum dot and preparation method thereof, in with uniform shape and controllable particle size is prepared on large scale by liquid phase stripping method 2 Se 3 Quantum dots, and obtaining In by centrifugal drying 2 Se 3 A quantum dot powder. The method specifically comprises the following steps:
in is separated by liquid phase separation 2 Se 3 Ultrasonically treating the crystal powder in Isopropanol (IPA) solvent for 6h at the power of 450-600W, centrifuging for 20-30min at the power of 5000-8000rmp/min to obtain a quantum dot supernatant, and centrifuging for 20-30min 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, in 2 Se 3 The ratio of crystalline powder to IPA was 0.2g.
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 sheet 2 Se 3 The 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 improved 2 Se 3 Photocatalytic performance.
Drawings
FIG. 1 shows In prepared In example 1 2 Se 3 XRD pattern of crystal powder of raw material used for quantum dot.
FIG. 2 shows In prepared In example 1 2 Se 3 Raman diagram of crystal powder of raw materials used for quantum dots.
FIG. 3 shows In prepared In example 1 2 Se 3 Physical image of quantum dot dispersion.
FIG. 4 shows In prepared In example 1 2 Se 3 And carrying out real object diagram of the quantum dot dispersion liquid under laser irradiation.
FIG. 5 shows In prepared In example 1 2 Se 3 TEM topography of quantum dots.
FIG. 6 shows In prepared In example 1 2 Se 3 Particle size statistical graph of quantum dots.
FIG. 7 shows In prepared In example 2 2 Se 3 TEM topography of quantum dots.
FIG. 8 shows In prepared In example 2 2 Se 3 Particle size statistical chart of quantum dots.
FIG. 9 shows In prepared In example 2 2 Se 3 AFM topography of quantum dots.
FIG. 10 shows a portion of In prepared In example 2 2 Se 3 Height map of quantum dots.
FIG. 11 shows In prepared In example 2 2 Se 3 Height 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 In 2 Se 3 Crystal 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 In 2 Se 3 And (4) quantum dots.
Due to In 2 Se 3 Has a plurality of crystal phases and crystal forms, so that In is prepared 2 Se 3 Before 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 invention 2 Se 3 XRD and Raman patterns of the crystal feedstock used for quantum dots; as can be seen from FIG. 1, in was used as a raw material 2 Se 3 The 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 is further confirmed as alpha phase In 2 Se 3 。
FIG. 3 and FIG. 4 show In prepared 2 Se 3 And (3) a quantum dot dispersion liquid object diagram. As can be seen from FIG. 3, in was prepared 2 Se 3 The quantum dot dispersion liquid is free of any obvious small particles and impurities; and no precipitation appears after long-time standing, and the product is stable. FIG. 4 shows In under laser irradiation 2 Se 3 The quantum dot dispersion has an obvious Tyndall phenomenon. The obtained mixed system is uniform and is a colloid, and the particle size dispersed in the supernatant is in a nanometer level.
FIGS. 5 and 6 show In 2 Se 3 TEM 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, the particle sizes account for about 90 percent of the total number, and In 2 Se 3 The average particle size of the quantum dots is 2.3nm.
[ example 2 ] A method for producing a polycarbonate
Getting In 2 Se 3 Putting 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 speed of 10000rmp/min to precipitate the quantum dots in the solution; washing the precipitate with anhydrous ethanol for 3 times, and oven drying at 40 deg.C to obtain In 2 Se 3 And (4) quantum dots.
FIGS. 7 and 8 show In 2 Se 3 TEM morphology image and particle size statistical image 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 In 2 Se 3 The average grain diameter of the quantum dots is 1.8nm.
FIG. 9, FIG. 10, FIG. 11 show In prepared 2 Se 3 AFM topography of quantum dots and their height data. FIG. 10 shows In through which three straight lines In FIG. 9 pass 2 Se 3 The curve of the quantum dot height diagram can be seen to have obvious ladder shape corresponding to the layered structure. FIG. 11 shows 100 In 2 Se 3 From the high statistical data obtained for the quantum dots, it can be seen that In 2 Se 3 The height of the quantum dots is mostly between 1nm and 3nm, and the average height is about 2nm. Due to a single layer of In 2 Se 3 (Se-In-Se 5 layer atoms) thickness was about 1nm, so that In was prepared 2 Se 3 The quantum dots are 2 layers on average.
Claims (6)
1. In (I) 2 Se 3 The preparation method of the quantum dot is characterized by comprising the following steps:
in is separated by liquid phase separation 2 Se 3 Carrying out ultrasonic treatment on the crystal powder in an isopropanol solvent for 6h at the power of 450-600W, centrifuging for 20-30min at the power of 5000-8000rmp/min to obtain a quantum dot supernatant, and centrifuging for 20-30min 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;
In 2 Se 3 the ratio of crystalline powder to isopropanol was 0.2g.
2. The method of claim 1, wherein the quantum dot supernatant is obtained after 20min of 7000 rmp/min centrifugation.
3. 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.
4. The method of claim 1, wherein drying is at 40 ℃.
5. In prepared by the method of any one of claims 1 to 4 2 Se 3 And (4) quantum dots.
6. In according to claim 5 2 Se 3 Quantum dot characterized by In 2 Se 3 The quantum dot size is less than 5nm.
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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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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 |
|---|
| Black Phosphorus Quantum Dots;Xiao Zhang等;《Angewandte Chemie International Edition》;20150203;第54卷(第12期);第3653-3657页 * |
| Large-scale synthesis of defect-selective graphene quantum dots by ultrasonic-assisted liquid-phase exfoliation;Liqiang Lu等;《carbon》;20160813;第109卷;第373-383页 * |
| Tunable UV-Visible Absorption of SnS2 Layered Quantum Dots Produced by Liquid Phase Exfoliation;Xiao Fu等;《Nanoscale》;20170103;第9卷(第5期);第1820-1826页 * |
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