CN114105107A - Highly monodisperse MoSe with different morphologies2Preparation method of nano material - Google Patents
Highly monodisperse MoSe with different morphologies2Preparation method of nano material Download PDFInfo
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- CN114105107A CN114105107A CN202111675326.0A CN202111675326A CN114105107A CN 114105107 A CN114105107 A CN 114105107A CN 202111675326 A CN202111675326 A CN 202111675326A CN 114105107 A CN114105107 A CN 114105107A
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- 229910016001 MoSe Inorganic materials 0.000 title claims abstract description 32
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 54
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 8
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 8
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 7
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 10
- 239000012300 argon atmosphere Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 239000011669 selenium Substances 0.000 claims description 3
- 229910052711 selenium Inorganic materials 0.000 claims description 2
- 238000004729 solvothermal method Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 3
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- 235000019441 ethanol Nutrition 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 5
- 229910052750 molybdenum Inorganic materials 0.000 description 5
- 239000011733 molybdenum Substances 0.000 description 5
- 239000002077 nanosphere Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 229910004619 Na2MoO4 Inorganic materials 0.000 description 4
- 239000004809 Teflon Substances 0.000 description 4
- 229920006362 Teflon® Polymers 0.000 description 4
- 238000007605 air drying Methods 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- UGSPLKDPMABWOB-UHFFFAOYSA-N selenium;hydrate Chemical compound O.[Se] UGSPLKDPMABWOB-UHFFFAOYSA-N 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007810 chemical reaction solvent Substances 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000006276 transfer reaction Methods 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005285 chemical preparation method Methods 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
- 238000004146 energy storage Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 150000002751 molybdenum Chemical class 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 239000003586 protic polar solvent Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal chalcogenides Chemical class 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides highly monodisperse MoSe with different morphologies2A method for preparing nano material. The technical scheme provided comprises the following steps: firstly, dissolving sodium molybdate in a mixed solution of dimethyl formamide (DMF), an organic solvent and a trace amount of deionized water to form a solution A, dissolving selenium powder in a hydrazine hydrate solution to form a solution B, then mixing the two solutions AB together, and synthesizing the highly monodisperse MoSe by a solvent thermal-wet chemical method2And (3) nano materials. MoSe prepared by the invention2The nano material has the characteristics of controllable appearance, uniform size and high conductivity, and can effectively relieve MoSe2The agglomeration phenomenon among the nano particles forms highly monodisperse MoSe with various shapes2And (3) nano materials.
Description
Technical Field
The invention belongs to the field of solvent heat-wet chemical synthesis processes, and particularly relates to highly monodisperse MoSe with different morphologies2A method for preparing nano material.
Background
In recent years, transition metal chalcogenides (TMDs) have shown great potential for development in the fields of microelectronics, photodetectors, catalytic energy conversion, solar cells, energy storage, sensors, and biomedicine. MoSe, one of the most studied materials in TMDs2Has a MoS ratio2Smaller forbidden band width and larger interlayer spacing, and Mo-Se bond is oxidized than molybdenum metalThe weakness of the substance or sulfide homologue will favor the kinetic behavior of the conversion reaction. On the other hand, the morphology of the material has a significant impact on the performance of the device, while the uniformity of morphology and size will have a significant impact on the stability of the device. Thus, highly monodisperse MoSe2The controllable synthesis of the nano material has wide application prospect and profound research value.
MoSe is currently prepared by wet chemical methods2The nano material mainly adopts water as a solvent, and also adopts dimethyl formamide (DMF) as a solvent. Water is a typical protic solvent, the proton autodelivery reaction is fast, while Dimethylformamide (DMF) is an aprotic polar solvent, the proton autodelivery reaction is extremely weak. The use of two solutions alone or a mixture of two solutions as a solvent to dissolve sodium molybdate is not conducive to the preparation of monodisperse MoSe2And (3) nano materials.
Disclosure of Invention
The invention aims to provide highly monodisperse MoSe with different morphologies2The preparation method of the nano material overcomes the problem of insufficient effective control of the reaction rate in the prior art.
In order to achieve the purpose of the invention, the invention adopts the technical scheme that: highly monodisperse MoSe with different morphologies2The preparation method of the nano material comprises the following steps:
the method comprises the following steps: adding selenium powder into 80% hydrazine hydrate solution, standing and dissolving to form the solution with the concentration of 0.1-0.5 mol.L-1The hydrated selenium precursor solution A; dissolving sodium molybdate in a mixed solution of DMF, an organic solvent and deionized water to form a solution with the concentration of 0.5-2 mmol.L-1The volume of the deionized water is 0.4 to 1.6 percent of the mixed solution;
step two: uniformly mixing and stirring the solution A and the solution B in the step one, and transferring the mixture into a reaction kettle to perform hydrothermal reaction on the mixed solution in a closed high-temperature high-pressure environment;
step three: centrifuging, washing and drying the product obtained in the second step to obtain the highly monodisperse MoSe2Precursor sodiumRice material.
Step four: MoSe obtained in the third step2The precursor nanomaterial is annealed at high temperature in an argon atmosphere.
Further, the organic solvent used in the first step is ethanol, and the volume mixing ratio of ethanol to DMF is 2: 3-3: 2.
Further, the organic solvent used in the first step is methanol, and the volume mixing ratio of the methanol to the DMF is 2: 1-4: 1.
Further, in the second step, in the process of mixing the solution A and the solution B, the solution A is added into the solution B at a dropping speed of 12-15 drops/MIN, and stirring is continuously carried out for 15-30 minutes.
Further, the reaction time of the solvothermal reaction in the second step is 15-24 hours, and the reaction temperature is 180-220 ℃.
Furthermore, the annealing temperature in the fourth step is 400-600 ℃, and the annealing time is 1-5 hours.
Compared with the prior art, the preparation process has the following advantages:
(1) the product MoSe obtained by the invention2The particle size of the nano material has high monodispersity, high crystallization quality and controllable morphology, can efficiently avoid agglomeration of nano particles, and has important effects on improving the performance, stability, precision and the like of related microelectronic or optoelectronic devices.
(2) The solvent thermal-wet chemical preparation method adopted by the invention combines hydroxyl-containing organic (methanol or ethanol) with moderate proton self-transfer reaction and DMF solution with weak proton self-transfer reaction, mixes the two solutions in a proper mixing proportion, and introduces a trace amount of aqueous solution for fully dissolving molybdenum salt in order to further ensure the uniformity of the reaction, thereby ensuring the preparation of MoSe2High monodispersity of the nanomaterial.
(3) The invention can realize the controllability of the appearance by simply changing the components of the solvent. When DMF and ethanol are used as mixed reaction solvent, monodisperse MoSe with smooth surface can be synthesized2Nanospheres; when DMF and methanol are taken as mixed reaction solvent, the monodisperse flower-shaped assembled by nano-sheets can be synthesizedMoSe2A nanostructure.
(4) The preparation and synthesis process is simple, low in cost and high in repeatability, and can realize large-scale production.
Drawings
FIG. 1 shows the monodisperse flower-like MoSe prepared in example 12A Scanning Electron Microscope (SEM) image of the nanomaterial;
FIG. 2 shows the monodisperse MoSe prepared in example 22SEM image of nanospheres;
FIG. 3 shows the monodisperse flower-like MoSe prepared in example 12X-ray diffraction profile of the nanomaterial.
Detailed Description
Example 1: in a room temperature environment of 20-25 ℃, firstly, 0.5mmol selenium powder is added into 4ml of 80% hydrazine hydrate solution, and the solution is kept stand for 1 hour to form a selenium hydrate precursor solution A; secondly, 0.25mmol of Na2MoO4·2H2Dissolving O in a mixed solvent consisting of 20ml of ethanol, 20ml of DMF solution and 0.2ml of deionized water under the stirring of strong magnetic force to form a molybdenum source solution B; then slowly dripping the solution A into the solution B at the dripping speed of 12-15 drops/MIN under the stirring of strong magnetic force, and continuously stirring for 15 minutes; finally, the final mixed solution was transferred to a 100ml teflon lined hydrothermal reaction kettle, sealed and covered tightly, and the reaction kettle was placed in an air-blast drying oven for reaction at 200 ℃ for 15 hours. After the reaction kettle is naturally cooled, the precipitate is sequentially centrifugally cleaned for 5 times by deionized water and absolute ethyl alcohol, finally the obtained powder material is put into a forced air drying oven to be dried for 12 hours at the temperature of 60 ℃, and then is annealed for 5 hours at the temperature of 500 ℃ in an argon atmosphere, and finally the MoSe with highly monodisperse and smooth surface is obtained2Nanospheres. Referring to FIG. 1, the MoSe obtained2The nanospheres have uniform particle size and high monodispersity, and the particle size is about 200 nm. Referring to FIG. 3, it can be seen that the monodisperse flower-like MoSe prepared in this example2X-ray diffraction Pattern (XRD) of nanomaterials and MoSe in PDF card2Corresponds to the standard diffraction peak (PDF # 72-1420).
Example 2: in the room temperature environment of 20-25 ℃,firstly, adding 0.5mmol selenium powder into 4ml 80% hydrazine hydrate solution, standing and dissolving for 1 hour to form selenium hydrate precursor solution A; secondly, 0.25mmol of Na2MoO4·2H2Adding O into a mixed solvent consisting of 30ml of methanol, 10ml of DMF solution and 0.2ml of deionized water under the stirring of strong magnetic force to form a molybdenum source solution B; then slowly dripping the solution A into the solution B at the dripping speed of 12-15 drops/MIN under the stirring of strong magnetic force, and continuously stirring for 15 minutes; finally, the final mixed solution was transferred to a 100ml teflon lined hydrothermal reaction kettle, sealed and covered tightly, and the reaction kettle was placed in an air-blast drying oven for reaction at 200 ℃ for 15 hours. After the reaction kettle is naturally cooled, the precipitate is sequentially centrifugally cleaned for 5 times by deionized water and absolute ethyl alcohol, finally the obtained powder material is put into a forced air drying oven to be dried for 12 hours at the temperature of 60 ℃, and then is annealed for 5 hours at the temperature of 500 ℃ in an argon atmosphere, and finally the flower-shaped MoSe with high monodispersity is obtained2And (3) nano materials. Flower-shaped MoSe2The SEM image of the nanomaterial is shown in FIG. 2, and the flower-like MoSe is obtained from the SEM image2The nano material has uniform particle size and high monodispersity, and the particle size is about 250 nm.
Example 3 in a room temperature environment of 20 ℃ to 25 ℃, 2.0mmol of selenium powder is firstly added into 4ml of 80% hydrazine hydrate solution, and the solution is kept stand for 1 hour to form a selenium hydrate precursor solution A; secondly, 1.0mmol of Na2MoO4·2H2Dissolving O in a mixed solvent consisting of 20ml of ethanol, 20ml of DMF solution and 0.8ml of deionized water under the stirring of strong magnetic force to form a molybdenum source solution B; then slowly dripping the solution A into the solution B at the dripping speed of 12-15 drops/MIN under the stirring of strong magnetic force, and continuously stirring for 15 minutes; finally, the final mixed solution was transferred to a 100ml teflon lined hydrothermal reaction kettle, sealed and covered tightly, and the reaction kettle was placed in an air-blast drying oven for reaction at 200 ℃ for 15 hours. After the reaction kettle is naturally cooled, the precipitate is sequentially centrifugally cleaned for 5 times by deionized water and absolute ethyl alcohol, finally the obtained powder material is put into a forced air drying oven to be dried for 12 hours at the temperature of 60 ℃, then the powder material is annealed for 5 hours at the temperature of 500 ℃ in an argon atmosphere, and finally the reaction kettle is cooledObtaining smooth-surfaced MoSe with high monodispersity2Nanospheres.
Example 4: in a room temperature environment of 20-25 ℃, firstly, adding 2.0mmol of selenium powder into 4ml of 80% hydrazine hydrate solution, standing for dissolving for 1.5 hours to form a selenium hydrate precursor solution A; secondly, 1.0mmol of Na2MoO4·2H2Adding O into a mixed solvent consisting of 25ml of methanol, 15ml of DMF solution and 0.8ml of deionized water under the stirring of strong magnetic force to form a molybdenum source solution B; then slowly dripping the solution A into the solution B at the dripping speed of 12-15 drops/MIN under the strong magnetic stirring, and continuously stirring for 30 minutes; finally, the final mixed solution was transferred to a 100ml teflon lined hydrothermal reaction kettle, sealed and covered tightly, and the reaction kettle was placed in an air-blast drying oven for reaction at 180 ℃ for 24 hours. After the reaction kettle is naturally cooled, the precipitate is sequentially centrifugally cleaned for 5 times by deionized water and absolute ethyl alcohol, finally the obtained powder material is put into a forced air drying oven to be dried for 12 hours at the temperature of 60 ℃, and then the powder material is annealed for 1 hour at the temperature of 600 ℃ in an argon atmosphere, and finally the flower-shaped MoSe with high monodispersity is obtained2And (3) nano materials.
Claims (6)
1. Highly monodisperse MoSe with different morphologies2The preparation method of the nano material is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: adding selenium powder into 80% hydrazine hydrate solution, standing and dissolving to form the solution with the concentration of 0.1-0.5 mol.L-1The hydrated selenium precursor solution A; dissolving sodium molybdate in a mixed solution of DMF, an organic solvent and deionized water to form a solution with the concentration of 0.5-2 mmol.L-1The volume of the deionized water is 0.4 to 1.6 percent of the mixed solution;
step two: uniformly mixing and stirring the solution A and the solution B in the step one, and transferring the mixture into a reaction kettle to perform hydrothermal reaction on the mixed solution in a closed high-temperature high-pressure environment;
step three: centrifuging, washing and drying the product obtained in the second step to obtain the highly monodisperse MoSe2A precursor nanomaterial.
Step four: MoSe obtained in the third step2The precursor nanomaterial is annealed at high temperature in an argon atmosphere.
2. Highly monodisperse MoSe with different morphologies according to claim 12The preparation method of the nano material is characterized by comprising the following steps: the organic solvent used in the first step is ethanol, and the volume mixing ratio of the ethanol to the DMF is 2: 3-3: 2.
3. Highly monodisperse MoSe with different morphologies according to claim 12The preparation method of the nano material is characterized by comprising the following steps: the organic solvent used in the first step is methanol, and the volume mixing ratio of the methanol to the DMF is 2: 1-4: 1.
4. Highly monodisperse MoSe with different morphologies according to claim 2 or 32The preparation method of the nano material is characterized by comprising the following steps: and in the second step, in the process of mixing the solution A and the solution B, adding the solution A into the solution B at the dropping speed of 12-15 drops/MIN, and continuously stirring for 15-30 minutes.
5. Highly monodisperse MoSe with different morphologies according to claim 42The preparation method of the nano material is characterized by comprising the following steps: in the second step, the solvothermal reaction lasts for 15-24 hours, and the reaction temperature is 180-220 ℃.
6. Highly monodisperse MoSe with different morphologies according to claim 22The preparation method of the nano material is characterized by comprising the following steps: the annealing temperature in the fourth step is 400-600 ℃, and the annealing time is 1-5 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117244566A (en) * | 2023-11-16 | 2023-12-19 | 内蒙古工业大学 | Photocatalyst 1T/2H MoSe 2 ZIS and method for the production thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117244566A (en) * | 2023-11-16 | 2023-12-19 | 内蒙古工业大学 | Photocatalyst 1T/2H MoSe 2 ZIS and method for the production thereof |
| CN117244566B (en) * | 2023-11-16 | 2024-02-09 | 内蒙古工业大学 | Photocatalyst 1T/2H MoSe 2 ZIS and method for the production thereof |
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