CN116443856A - Carbon quantum dot/MoS 2 Nanosheet composite material and preparation method thereof - Google Patents
Carbon quantum dot/MoS 2 Nanosheet composite material and preparation method thereof Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 239000002135 nanosheet Substances 0.000 title claims abstract description 64
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 101100069231 Caenorhabditis elegans gkow-1 gene Proteins 0.000 title description 2
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 22
- 125000000542 sulfonic acid group Chemical group 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012266 salt solution Substances 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- NFEURUSKIHJCRP-UHFFFAOYSA-N 1,2,3-trinitropyrene Chemical compound C1=CC=C2C=CC3=C([N+]([O-])=O)C([N+](=O)[O-])=C([N+]([O-])=O)C4=CC=C1C2=C43 NFEURUSKIHJCRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002064 nanoplatelet Substances 0.000 claims abstract description 8
- 238000000502 dialysis Methods 0.000 claims abstract description 7
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- QGAVSDVURUSLQK-UHFFFAOYSA-N ammonium heptamolybdate Chemical compound N.N.N.N.N.N.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Mo].[Mo].[Mo].[Mo].[Mo].[Mo].[Mo] QGAVSDVURUSLQK-UHFFFAOYSA-N 0.000 claims description 7
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 6
- IOMZCWUHFGMSEJ-UHFFFAOYSA-N 4-(azaniumylamino)benzenesulfonate Chemical compound NNC1=CC=C(S(O)(=O)=O)C=C1 IOMZCWUHFGMSEJ-UHFFFAOYSA-N 0.000 claims description 3
- RXCMFQDTWCCLBL-UHFFFAOYSA-N 4-amino-3-hydroxynaphthalene-1-sulfonic acid Chemical compound C1=CC=C2C(N)=C(O)C=C(S(O)(=O)=O)C2=C1 RXCMFQDTWCCLBL-UHFFFAOYSA-N 0.000 claims description 3
- 235000010265 sodium sulphite Nutrition 0.000 claims description 3
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 claims description 2
- FEPBITJSIHRMRT-UHFFFAOYSA-N 4-hydroxybenzenesulfonic acid Chemical compound OC1=CC=C(S(O)(=O)=O)C=C1 FEPBITJSIHRMRT-UHFFFAOYSA-N 0.000 claims description 2
- 229950000244 sulfanilic acid Drugs 0.000 claims description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052982 molybdenum disulfide Inorganic materials 0.000 abstract description 11
- 125000000524 functional group Chemical group 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000001988 toxicity Effects 0.000 abstract description 3
- 231100000419 toxicity Toxicity 0.000 abstract description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052717 sulfur Inorganic materials 0.000 abstract description 2
- 239000011593 sulfur Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 description 19
- 239000000047 product Substances 0.000 description 14
- 238000003786 synthesis reaction Methods 0.000 description 14
- -1 transition metal chalcogenide Chemical class 0.000 description 13
- 239000000463 material Substances 0.000 description 12
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 12
- 239000004810 polytetrafluoroethylene Substances 0.000 description 12
- 238000011065 in-situ storage Methods 0.000 description 6
- 239000002356 single layer Substances 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 230000007704 transition Effects 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010894 electron beam technology Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000000053 physical method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 2
- 229940010552 ammonium molybdate Drugs 0.000 description 2
- 235000018660 ammonium molybdate Nutrition 0.000 description 2
- 239000011609 ammonium molybdate Substances 0.000 description 2
- 238000004630 atomic force microscopy Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- QXYJCZRRLLQGCR-UHFFFAOYSA-N dioxomolybdenum Chemical compound O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 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 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000089 atomic force micrograph Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- 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
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
-
- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention relates to a carbon quantum dot/MoS 2 The preparation method of the nano-sheet composite material comprises the following steps: ultrasonically dissolving a sulfonic acid group precursor and trinitropyrene in water, reacting, carrying out suction filtration and dialysis on a primary product, drying the primary product to obtain solid powder of carbon quantum dots, dissolving the solid powder of carbon quantum dots, inorganic salt of Mo and inorganic salt of S in water, stirring to obtain an inorganic salt solution, reacting, centrifugally separating, washing and vacuum drying to obtain the carbon quantum dots/MoS 2 A nanosheet composite material. The carbon quantum dot has enough active sites and rich surface functional groups, and the sulfur vacancy of molybdenum disulfide is increased by influencing the electron density through different groups so as to regulate and control MoS 2 The structure forms a nanoplatelet. Compared with the prior art, the preparation method of the invention has the advantages of simplicity, easy implementation, low cost, mild reaction, small toxicity, simple post-treatment, high yield, good quality and stable structure of the prepared molybdenum disulfide, and the synthesized MoS 2 The thickness of the nanometer sheet is adjustable, and the nanometer sheet is suitable for industrial mass production of nanometer-sized MoS 2 A nano-sheet.
Description
Technical Field
The invention relates to the technical field of two-dimensional material synthesis, in particular to a carbon quantum dot/MoS 2 A nano-sheet composite material and a preparation method thereof.
Background
Molybdenum disulfide (MoS) 2 ) The most studied transition metal chalcogenide is an ideal catalyst for replacing platinum because of low price, abundant resources, no toxicity and high catalytic activity for hydrogen evolution reaction. Unlike bulk molybdenum disulfide, near-monolayer molybdenum disulfide nanosheets have attracted widespread attention due to their high specific surface area and surface activity. MoS according to the difference of S atom arrangement 2 There are mainly two different crystalline phases: 2H phase and 1T phase due to 1T MoS 2 The 4d track of Mo in (b) is not completely filled. As is well known, 1T MoS 2 The conductivity (of metal conductor nature) is 2H MoS 2 One hundred times (of semiconducting nature) this makes it a promising alternative to the catalytic electrolysis of aqueous hydrogen. However, 1T MoS 2 Cannot be directly mined from natural ores, and is difficult to mass produce by common chemical or physical methods. Hitherto, it has been reported that in 2H MoS 2 On the basis of (1) T MoS can be produced by electron beam, light irradiation and metal doping induced conversion reaction 2 . In particular, achieving such phase transitions by these experimental methods typically requires harsh experimental conditions, such as supercritical hydrothermal and high risk reagents, to overcome 2H MoS 2 To 1T MoS 2 High transformation disorder of (2).
CN 104226337B discloses a graphene-supported lamellar molybdenum disulfide nanocomposite and a preparation method thereof, the invention uses ammonium molybdate and thiourea as starting materials, and enables the ammonium molybdate and thiourea to support lamellar nano molybdenum dioxide on the surface of graphene oxide under hydrothermal conditions; the lamellar molybdenum disulfide loaded by the graphene after roasting treatment has higher crystallinity, and the photocatalytic efficiency is more than 1.7 times that of commercial nano titanium oxide, but thiourea used in the invention is decomposed into toxic gases such as hydrogen sulfide, ammonia and the like through high temperature in the reaction process.
Carbon quantum dots have become a new star in carbon-based nanomaterials due to their unique properties, such as sufficient active centers and abundant surface functional groups, and have attracted extensive attention in the electrocatalytic industry. Generally, carbon quantum dots mainly refer to nanomaterials having a size of less than 10nm and being composed of a carbonaceous backbone and surface-modified functional groups. Its carbonaceous skeleton is usually in sp 2 Hybrid C-O, C = C, O-c=o and graphitic carbon, or sp 2 And sp (sp) 3 Amorphous carbon composition of hybrid composition. In order to make the carbon quantum dot have better properties and application prospects, researchers often modify some functional groups on the surface of the carbon quantum dot, such as hydroxyl groups, carboxyl groups and the like. The carbon quantum dot has the advantages of simple preparation process, low cost, good stability, excellent photo-generated electron transfer capability and ideal electron acceptor and donor. In addition, the carbon quantum dots have the characteristics of larger than surface energy and smaller size, which effectively inhibit the aggregation of byproducts and are beneficial to the formation of nano sheets.
Therefore, there is a need for a carbon quantum dot/MoS 2 Nanosheet composite material and preparation method thereof for realizing two-dimensional MoS 2 The nano-sheet is prepared rapidly, controllably and at low cost, and realizes the conversion from 2H phase to 1T phase.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the carbon quantum dot/MoS 2 Nanometer sheet composite material and preparation method thereof, wherein carbon quantum dots are added for assisting in-situ synthesis of MoS 2 Nanosheets, carbon quantum dots used as structure regulator in preparation process, and MoS regulation and control method 2 The electronic structure of the nano sheet realizes metastable phase change and promotes the formation of two-dimensional materials, and can realize two-dimensional MoS 2 The nano-sheet is prepared rapidly, controllably and at low cost, and realizes the conversion from 2H phase to 1T phase.
The aim of the invention can be achieved by the following technical scheme:
the first object of the present invention is to provide a carbon quantum dot/MoS 2 Nanosheet composite material and preparation method thereof, and preparation method thereofThe method is an auxiliary preparation method of the carbon quantum dots, and comprises the following steps:
s1, ultrasonically dissolving a sulfonic acid group precursor and trinitropyrene in deionized water according to a certain mass ratio to obtain a mixed solution, reacting for a certain time at a certain temperature in a reaction kettle, carrying out suction filtration and dialysis on a primary product, and drying the primary product to obtain solid powder of carbon quantum dots, wherein the solid powder is used as sulfonic acid group functionalized carbon quantum dots;
s2, dissolving the sulfonic group functionalized carbon quantum dots, the inorganic salts of Mo and the inorganic salts of S obtained in the step S1 in deionized water, stirring to obtain an evenly mixed inorganic salt solution, reacting for a certain time at a certain temperature in a reaction kettle, centrifugally separating by ethanol, washing, and vacuum drying to obtain the carbon quantum dots/MoS 2 A nanosheet composite material.
Further, the reaction kettle is a polytetrafluoroethylene reaction kettle.
Further, the mass ratio of the sulfonic acid group precursor to the trinitropyrene is 0.1-1.
Further, in step S1, the sulfonic acid group precursor is selected from one or more of sodium sulfite, 4-hydrazinobenzenesulfonic acid, 4-aminobenzenesulfonic acid, 4-hydroxybenzenesulfonic acid, and 1-amino-2-naphthol-4-sulfonic acid.
Further, in step S1, the sulfonic acid group precursor is added in an amount of 100-1000mg.
In step S1, the reaction is carried out for a certain time at a certain temperature in a reaction kettle, namely transferring 20-60ml of the mixed solution into a polytetrafluoroethylene high-pressure reaction kettle for reaction, wherein the heating temperature is 150-300 ℃, and the heating time is 6-30h.
Further, in step S1, the drying temperature of the dried primary product is not higher than 60 ℃.
Further, in the step S2, the inorganic salt of Mo and the inorganic salt of S are respectively ammonium heptamolybdate and thiourea, the mass ratio of the ammonium heptamolybdate to the thiourea is 0.3-0.8, and the concentration ranges are 10-800mmol/L.
Further, in the step S2, the addition amount of the sulfonic acid group functionalized carbon quantum dots in the inorganic salt solution is 10-300mg.
Further, in step S2, the stirring time is 0.5-2h.
In step S2, the reaction is performed for a certain time at a certain temperature in the reaction kettle, specifically, 20-60ml of inorganic salt solution is transferred into the reaction kettle, the heating temperature is 150-300 ℃, and the heating time is 6-30h.
Further, the reaction kettle is a polytetrafluoroethylene reaction kettle.
Further, in the step S2, the centrifugal separation rotating speed is 8000-12000 rpm, and the centrifugal separation time is 1-20min.
A second object of the present invention is to provide a/MoS 2 Nanosheet composite material and preparation method thereof, and carbon quantum dot/MoS 2 The nano-sheet composite material is prepared by adopting the preparation method, and the carbon quantum dot/MoS 2 The average thickness of the nanoplatelet composite is not greater than 20nm.
Compared with the prior art, the invention has the following beneficial effects:
1) The invention provides the carbon quantum dot/MoS 2 The preparation method of the nano-sheet composite material is simple and feasible, low in cost, mild in reaction, small in toxicity and simple in post-treatment, and meanwhile, the prepared molybdenum disulfide has high yield, good quality and stable structure, and MoS is synthesized in situ by adding the carbon quantum dots 2 The thickness of the nano sheet is adjustable, and the method is suitable for industrial mass production of nano-sized carbon quantum dots/MoS 2 A nanosheet composite material.
2) The invention provides the carbon quantum dot/MoS 2 The nano-sheet composite material has 1T and 2H phase structures at the same time, and 1T MoS 2 Cannot be directly mined from natural ores, and is difficult to mass produce by common chemical or physical methods. Hitherto, it has been reported that in 2H MoS 2 On the basis of (1) T MoS can be produced by electron beam, light irradiation and metal doping induced conversion reaction 2 . In particular, achieving such phase transitions by these experimental methods typically requires harsh experimental conditions, such as supercritical hydrothermal and high risk reagents, to overcome 2H MoS 2 To 1T MoS 2 To improve the problem of high transformation disorderIn MoS 2 Adding carbon quantum dots in the synthesis process, regulating and controlling the addition amount of the carbon quantum dots, the reaction temperature and the filling degree of a reaction kettle so as to prepare the MoS with 1T and 2H phases coexisting 2 And a heterojunction.
3) The invention provides the carbon quantum dot/MoS 2 The nano-sheet composite material is single-layer or few-layer, compared with blocky MoS 2 Near-monolayer molybdenum disulfide nanosheets have attracted considerable attention due to their high specific surface area and surface activity. The addition of the carbon quantum dots in the method of the invention is to open MoS 2 The interlayer spacing to form a near-single-layer nano-sheet structure has important significance, and the prepared carbon quantum dot/MoS 2 The average thickness of the nano-sheet composite material can reach 2nm.
4) The invention provides the carbon quantum dot/MoS 2 Preparation method of nano-sheet composite material, and in-situ synthesis of carbon quantum dots/MoS (metal oxide semiconductor) by adding carbon quantum dots 2 Nanosheet composite material, carbon quantum dot serving as structure regulator in preparation process, and carbon quantum dot/MoS regulated and controlled 2 The electronic structure of the nano-sheet composite material realizes metastable phase change and promotes the formation of two-dimensional materials, thus realizing two-dimensional MoS 2 The nano-sheet is prepared rapidly, controllably and at low cost, and realizes the conversion from 2H phase to 1T phase.
Drawings
Fig. 1 is a field emission transmission electron microscope image of sulfonic acid group functionalized carbon quantum dots in example 1 of the present invention, and the inset is an average size image of the carbon quantum dots.
FIG. 2 is a carbon quantum dot/MoS in example 1 of the present invention 2 Transmission electron microscopy of nanoplatelets composites.
FIG. 3 is a carbon quantum dot/MoS in example 1 of the present invention 2 Nanosheet composite material and original 2H MoS 2 Is a XRD pattern of (C).
FIG. 4 is a carbon quantum dot/MoS in example 1 of the present invention 2 Atomic force microscopy of nanoplatelet composites.
FIG. 5 is a MoS of comparative example without carbon quantum dot synthesis 2 Scanning electron microscopy of nanoplatelets.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
In the technical scheme, the characteristics of preparation means, materials, structures or composition ratios and the like which are not explicitly described are regarded as common technical characteristics disclosed in the prior art.
In the following examples, the starting materials used were all commercially available.
As shown in FIG. 1, the carbon quantum dot/MoS of the present invention 2 The preparation method flow chart of the nano-sheet composite material and the preparation method thereof comprises the following steps:
s1, ultrasonically dissolving a sulfonic acid group precursor and trinitropyrene in deionized water according to a certain mass ratio to obtain a mixed solution, reacting for a certain time at a certain temperature in a polytetrafluoroethylene reaction kettle, carrying out suction filtration and dialysis on a primary product, and drying the primary product to obtain solid powder of carbon quantum dots, wherein the solid powder is used as sulfonic acid group functionalized carbon quantum dots;
s2, dissolving the sulfonic group functionalized carbon quantum dots, the inorganic salts of Mo and the inorganic salts of S obtained in the step S1 in deionized water, stirring to obtain an evenly mixed inorganic salt solution, reacting for a certain time at a certain temperature in a polytetrafluoroethylene reaction kettle, centrifugally separating with ethanol, washing, and vacuum drying to obtain the carbon quantum dots/MoS 2 A nanosheet composite material.
The conception history of the applicant is as follows: 1T MoS 2 Cannot be directly extracted from natural ores, is difficult to be produced on a large scale by common chemical or physical methods, and has been reported to date in 2H MoS 2 On the basis of (1) T MoS can be produced by electron beam, light irradiation and metal doping induced conversion reaction 2 In particular, achieving such phase transitions by these experimental methods generally requires demanding experimental conditions, such as supercritical hydrothermal and highRisk agent to overcome 2H MoS 2 To 1T MoS 2 To improve this problem, in MoS 2 Adding carbon quantum dots in the synthesis process, regulating and controlling the addition amount of the carbon quantum dots, the reaction temperature and the filling degree of a reaction kettle so as to prepare the MoS with 1T and 2H phases coexisting 2 Heterojunction, i.e. in situ synthesis of MoS assisted by the addition of carbon quantum dots 2 Nanosheets, carbon quantum dots used as structure regulator in preparation process, and MoS regulation and control method 2 The electronic structure of the nano sheet realizes metastable phase change and promotes the formation of two-dimensional materials, thus realizing two-dimensional MoS 2 The nano-sheet is prepared rapidly, controllably and at low cost, and realizes the conversion from 2H phase to 1T phase. Compared with blocky MoS 2 The near-monolayer molybdenum disulfide nanosheets are widely focused by people due to the high specific surface area and surface activity, and the addition of the carbon quantum dots is used for opening MoS 2 The interlayer spacing to form a near-monolayer nano-sheet structure is of great significance.
Example 1
In this embodiment, a carbon quantum dot/MoS is provided 2 The preparation method of the nano-sheet composite material comprises the following steps:
s1, ultrasonically dissolving 500mg of sodium sulfite and 200mg of trinitropyrene in deionized water to obtain a mixed solution, reacting for 12 hours at 160 ℃ in a polytetrafluoroethylene reaction kettle, carrying out suction filtration and dialysis on a primary product, and drying the primary product at 60 ℃ to obtain solid powder of carbon quantum dots serving as sulfonic acid group functionalized carbon quantum dots;
s2, dissolving the sulfonic functionalized carbon quantum dots (10 mg), ammonium heptamolybdate (18 mg) and thiourea (60 mg) obtained in the step S1 into 6mL of deionized water, stirring for 0.5h to obtain a uniformly mixed inorganic salt solution, reacting for 20h at 180 ℃ in a polytetrafluoroethylene reaction kettle, and centrifuging with ethanol, wherein the centrifugal separation speed is 8000 revolutions per minute, and the centrifugal separation time is 10min. Washing and vacuum drying to obtain carbon quantum dot/MoS 2 A nanosheet composite material.
The obtained carbon quantum dot/MoS 2 The nano-sheet composite material can be applied to the field of electrochemical hydrogen production.
The test analysis is as follows:
the sulfonic acid group functionalized carbon quantum dots obtained in step S1 in example 1 were observed by using a field emission transmission electron microscope, and the average size of the carbon quantum dots was found to be 2.74 nm, as shown in the inset of fig. 1. Measurement of carbon Quantum dots/MoS prepared in step S2 of this example 1 Using field emission Transmission Electron microscopy 2 The nanosheet composite material diagram shows that dense carbon quantum dots in the obtained product exist in MoS 2 Surface, which demonstrates carbon quantum dot/MoS 2 Successful synthesis of the nanoplatelet composite is illustrated in figure 2. FIG. 3 is a graph showing the carbon quantum dot/MoS obtained in example 1 2 XRD pattern of the nano-sheet composite material shows that the characteristic peak of the obtained product has better coincidence degree with the characteristic peak of the standard card JCPDS No.037-1492, which proves that MoS 2 Is a successful synthesis of (a). At the same time, it can be seen from the figure that carbon quantum dots are introduced into MoS 2 After the nano-sheet is arranged, moS is formed 2 The shift of the position of the main characteristic peak of the nano sheet indicates that the introduced carbon quantum dot can induce MoS 2 The nanoplatelets undergo a metastable phase transition, see the inset of fig. 3. As shown in FIG. 4, AFM image of the product obtained in step S2 of example 1 was examined by atomic force microscopy to find two-dimensional carbon quantum dots/MoS 2 The average thickness of the nano-sheet composite material is 1.5-2 nm.
As shown in the scanning electron microscope chart of FIG. 5, moS synthesized without adding carbon quantum dots 2 The nano-sheets are thick, no nano-sheets are formed, and the stacking phenomenon is obvious.
Comparative example
This comparative example is substantially identical to the example 1, except that:
in the synthesis of MoS 2 The sulfonic functionalized carbon quantum dots are not added into the inorganic salt solution in the material, and finally thicker MoS is prepared 2 A material.
Quick synthesis MoS 2 The preparation method of the material comprises the following steps:
dissolving ammonium heptamolybdate and thiourea in deionized water, stirring for 0.5h to obtain a uniformly mixed colorless transparent inorganic salt solution, and reacting for 20h in a polytetrafluoroethylene reaction kettle; finally, ethanol is centrifugally washed and vacuum dried to obtain MoS 2 A material.
Example 2
In this embodiment, a carbon quantum dot/MoS is provided 2 The preparation method of the nano-sheet composite material comprises the following steps:
s1, ultrasonically dissolving 100mg of 4-hydrazinobenzenesulfonic acid and 500mg of trinitropyrene in deionized water to obtain a mixed solution, reacting for 20 hours at 160 ℃ in a polytetrafluoroethylene reaction kettle, carrying out suction filtration and dialysis on a primary product, and drying the primary product at 60 ℃ to obtain solid powder of carbon quantum dots, wherein the solid powder is used as sulfonic group functionalized carbon quantum dots;
s2, dissolving the sulfonic functionalized carbon quantum dots (10 mg), ammonium heptamolybdate (15 mg) and thiourea (30 mg) obtained in the step S1 into 12mL of deionized water, stirring for 0.5h to obtain an inorganic salt solution which is uniformly mixed, reacting for 15h at 180 ℃ in a polytetrafluoroethylene reaction kettle, centrifuging by ethanol, wherein the centrifugal separation speed is 1000 revolutions per minute, the centrifugal separation time is 15min, washing and vacuum drying to obtain the carbon quantum dots/MoS 2 A nanosheet composite material.
Example 3
In this embodiment, a carbon quantum dot/MoS is provided 2 The preparation method of the nano-sheet composite material comprises the following steps:
s1, dissolving 1000mg of 1-amino-2-naphthol-4-sulfonic acid and 100mg of trinitropyrene in deionized water in an ultrasonic manner to obtain a mixed solution, reacting for 10 hours at 210 ℃ in a polytetrafluoroethylene reaction kettle, carrying out suction filtration and dialysis on a primary product, and drying the primary product at 60 ℃ to obtain solid powder of carbon quantum dots serving as sulfonic group functionalized carbon quantum dots;
s2, dissolving the sulfonic functionalized carbon quantum dots (15 mg), ammonium heptamolybdate (80 mg) and thiourea (100 mg) obtained in the step S1 into 24mL of deionized water, stirring for 0.5h to obtain an inorganic salt solution which is uniformly mixed, reacting for 24h at 220 ℃ in a polytetrafluoroethylene reaction kettle, and centrifugally separating by ethanol, wherein the centrifugal separation speed is 12000 r/min, the centrifugal separation time is 20min, washing and vacuum drying to obtain the carbon quantum dots/MoS 2 A nanosheet composite material.
The preparation methods in examples 1 to 4 described above enable carbon quantum dots/MoS 2 Nanosheet composite materialIs prepared by two-dimensional MoS 2 The auxiliary synthesis of carbon quantum dots of nanometer sheets belongs to the field of new two-dimensional material synthesizing technology. The comparative example does not prepare a composite material containing carbon quantum dots, cannot exert the function of the carbon quantum dots as a structure regulator in the use process, is unfavorable for promoting the formation of two-dimensional materials, and cannot induce MoS 2 The phase transition from 2H to 1T is achieved. In the above example 1, carbon quantum dots were synthesized by a molecular fusion method, and two-dimensional MoS with coexistence of 1T and 2H phases was prepared in situ by a top-down synthesis strategy at room temperature using carbon quantum dots as an adjuvant and an inorganic salt solution of molybdenum and sulfur 2 Nanometer sheet (carbon quantum dot/MoS) 2 Nanosheet composite material). The synthesis method of the embodiment is simple and feasible, mild in reaction, low in toxicity and simple in post-treatment, and meanwhile, the prepared molybdenum disulfide is high in yield, good in quality and stable in structure. The safe and low-cost in-situ induced phase change synthesis strategy has heuristic significance for developing the phase change of related heterostructures or other TMDs materials in electrocatalysis for energy conversion systems.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (10)
1. Carbon quantum dot/MoS 2 The preparation method of the nano-sheet composite material is characterized by comprising the following steps:
s1, ultrasonically dissolving a sulfonic acid group precursor and trinitropyrene in deionized water to obtain a mixed solution, reacting in a reaction kettle, carrying out suction filtration and dialysis on a primary product, and drying the primary product to obtain solid powder of carbon quantum dots, wherein the solid powder is used as sulfonic acid group functionalized carbon quantum dots;
s2, the step S1Dissolving the obtained sulfonic acid group functionalized carbon quantum dot, the inorganic salt of Mo and the inorganic salt of S in deionized water, stirring to obtain an inorganic salt solution which is uniformly mixed, reacting in a reaction kettle, centrifugally separating by ethanol, washing, and vacuum drying to obtain the carbon quantum dot/MoS 2 A nanosheet composite material.
2. A carbon quantum dot/MoS according to claim 1 2 The preparation method of the nano-sheet composite material is characterized in that in the step S1, the sulfonic acid group precursor is selected from one or more of sodium sulfite, 4-hydrazinobenzenesulfonic acid, 4-aminobenzenesulfonic acid, 4-hydroxybenzenesulfonic acid and 1-amino-2-naphthol-4-sulfonic acid.
3. A carbon quantum dot/MoS according to claim 1 2 The preparation method of the nano-sheet composite material is characterized in that in the step S1, the addition amount of the sulfonic acid group precursor is 100-1000mg.
4. A carbon quantum dot/MoS according to claim 1 2 The preparation method of the nano-sheet composite material is characterized in that in the step S1, the reaction in the reaction kettle is specifically that 20-60ml of mixed solution is transferred into the reaction kettle for reaction, the heating temperature is 150-300 ℃, and the heating time is 6-30h.
5. A carbon quantum dot/MoS according to claim 1 2 The preparation method of the nano-sheet composite material is characterized in that in the step S1, the drying temperature of the dried initial product is not higher than 60 ℃.
6. The carbon quantum dot according to claim 1, wherein in the step S2, the inorganic salt of Mo and the inorganic salt of S are respectively ammonium heptamolybdate and thiourea, the mass ratio of the two is 0.3-0.8, and the concentration ranges are 10-800mmol/L.
7. A carbon quantum dot/MoS according to claim 1 2 Method for preparing nanosheet composite material, and nanosheet composite materialIs characterized in that in the step S2, the addition amount of the sulfonic acid group functionalized carbon quantum dots in the inorganic salt solution is 10-300mg.
8. A carbon quantum dot/MoS according to claim 1 2 The preparation method of the nano-sheet composite material is characterized in that in the step S2, the reaction in the reaction kettle is specifically that 20-60ml of inorganic salt solution is transferred into the reaction kettle, the heating temperature is 150-300 ℃, and the heating time is 6-30h.
9. A carbon quantum dot/MoS according to claim 1 2 The preparation method of the nano-sheet composite material is characterized in that in the step S2, the centrifugal separation rotating speed is 8000-12000 r/min, and the centrifugal separation time is 1-20min.
10. A carbon quantum dot/MoS obtained by the method of any one of claims 1 to 9 2 The nano sheet composite material is characterized in that the carbon quantum dots/MoS 2 The average thickness of the nanoplatelet composite is not greater than 20nm.
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