CN115888780B - CuFeS2MXene composite nano material and preparation method thereof - Google Patents
CuFeS2MXene composite nano material and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000002135 nanosheet Substances 0.000 claims abstract description 27
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002096 quantum dot Substances 0.000 claims abstract description 22
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 20
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 5
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 229910052717 sulfur Inorganic materials 0.000 abstract description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract 1
- 150000001879 copper Chemical class 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract 1
- 230000033116 oxidation-reduction process Effects 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 239000011593 sulfur Substances 0.000 abstract 1
- 230000005540 biological transmission Effects 0.000 description 10
- 239000002064 nanoplatelet Substances 0.000 description 9
- 238000005303 weighing Methods 0.000 description 8
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001027 hydrothermal synthesis Methods 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- MCDLETWIOVSGJT-UHFFFAOYSA-N acetic acid;iron Chemical compound [Fe].CC(O)=O.CC(O)=O MCDLETWIOVSGJT-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- NWFNSTOSIVLCJA-UHFFFAOYSA-L copper;diacetate;hydrate Chemical compound O.[Cu+2].CC([O-])=O.CC([O-])=O NWFNSTOSIVLCJA-UHFFFAOYSA-L 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 239000010949 copper Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- AZUYLZMQTIKGSC-UHFFFAOYSA-N 1-[6-[4-(5-chloro-6-methyl-1H-indazol-4-yl)-5-methyl-3-(1-methylindazol-5-yl)pyrazol-1-yl]-2-azaspiro[3.3]heptan-2-yl]prop-2-en-1-one Chemical compound ClC=1C(=C2C=NNC2=CC=1C)C=1C(=NN(C=1C)C1CC2(CN(C2)C(C=C)=O)C1)C=1C=C2C=NN(C2=CC=1)C AZUYLZMQTIKGSC-UHFFFAOYSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a CuFeS 2/MXene composite nanomaterial and a preparation method thereof, wherein the composite nanomaterial consists of CuFeS 2 quantum dots and MXene nano sheets, the CuFeS 2 quantum dots are uniformly loaded on the MXene nano sheets, a microwave method is adopted, copper salt, ferric salt and a sulfur source are dissolved in isopropanol glycol mixed solution, the MXene nano sheets are added, and after uniform mixing, the microwave is carried out for 3-8 min, so that the CuFeS 2/MXene composite nanomaterial is obtained; the method is simple to operate, short in reaction time and low in energy consumption, and the prepared composite nano material has good morphology and good oxidation-reduction effect when being applied to photocatalysis.
Description
Technical Field
The invention relates to a composite nanomaterial, in particular to a CuFeS 2/MXene composite nanomaterial and a preparation method of the CuFeS 2/MXene composite nanomaterial.
Background
Metal sulfides are common photocatalysts, but the photocatalysts have low light absorptivity and poor stability, and MXene is a novel 2D transition metal carbide with high conductivity and chemical activity surface, but the photocatalysts are rapidly compounded by photo-generated charges and are easily oxidized in air, so that the application of the photocatalysts in the aspect of photoelectrocatalysis is limited. In the prior art, a method for constructing a heterojunction on an MXene nanosheet is adopted to solve the problem of photo-generated electron-hole recombination, but the current commonly used method for synthesizing the composite nanomaterial based on MXene is a hydrothermal method, the reaction time is long, and nanoparticles on the MXene are easy to aggregate.
Disclosure of Invention
The invention aims to: one of the purposes of the invention is to provide a CuFeS 2/MXene composite nano material with high photocatalytic performance; the invention further aims to provide a preparation method of the CuFeS 2/MXene composite nanomaterial, which is high in preparation speed, low in oxidation degree of the MXene nano-sheets in the composite nanomaterial, and the CuFeS 2 quantum dots on the MXene nano-sheets are uniformly distributed.
The technical scheme is as follows: the CuFeS 2/MXene composite nano material provided by the invention consists of CuFeS 2 quantum dots and MXene nano sheets, wherein the CuFeS 2 quantum dots are loaded on the surfaces of the MXene nano sheets.
A heterojunction interface with strong binding force is formed between the CuFeS 2 quantum dot and the MXene nano-sheet, and the separation of photo-generated electron and hole is promoted, so that the photocatalysis performance of the photo-generated electron and hole is improved, the separation rate of electron and hole on the MXene nano-sheet is improved under illumination, the electron and hole respectively move to the CuFeS 2 quantum dot and the MXene nano-sheet, and in the photocatalysis reaction, the electron and hole respectively participate in the oxidation reaction and the reduction reaction.
Wherein, the mass ratio of the CuFeS 2 quantum dot to the MXene nano-sheet is 1:1 to 100. When the CuFeS 2 quantum dot load is too large, the MXene nano-sheet is largely coated by the CuFeS 2 quantum dot, so that the specific surface area of the composite nano-material is reduced, and the active sites on the composite nano-material are reduced.
The preparation method of the CuFeS 2/MXene composite nano material specifically comprises the following steps: preparing a mixed solution containing Cu 2+ and Fe 2+, adding the mixed solution and thiourea into a solvent, and uniformly stirring by ultrasonic to obtain a solution containing CuFeS 2; adding MXene nano-sheets into a solution containing CuFeS 2, uniformly stirring, placing the solution in a microwave reactor for microwave for 3-8 min, taking out, centrifuging, washing and drying to obtain the CuFeS 2/MXene composite nano-material.
After microwave heating, cuFeS 2 is loaded on the MXene nanosheets to form a heterojunction, so that stirring on a molecular level is realized, the defect of non-uniform heating by a hydrothermal method is overcome, the heating speed is high, the heating is uniform, no temperature gradient exists, the reaction time is shortened, and the production efficiency is improved.
Wherein, in the mixed solution, cu 2+：Fe2+: the molar ratio of thiourea is 1:1:2 to 4. The molar ratio of Cu 2+：Fe2+ is controlled to be equal, so that ferrous ions can be prevented from being oxidized into ferric ions; too small an amount of thiourea is not easy to synthesize CuFeS 2, and if too much thiourea is added, MXene nanoplatelets can be vulcanized to generate byproducts.
Wherein the solvent is prepared from the following components in volume ratio 1:0.5 to 2 of ethylene glycol and isopropanol. Ethylene glycol with a higher boiling point is selected as an organic solvent, so that the phenomenon that the microwave reactor cavity is caused by excessive boiling of the solvent during the microwave time is prevented; isopropanol with a lower boiling point is added, and the isopropanol is vigorously boiled in the microwave reaction, so that the solution is fully and uniformly mixed in the reaction process.
Wherein the drying temperature is 50-80 ℃ and the drying time is 4-8 h.
The beneficial effects are that: compared with the prior art, the invention has the remarkable advantages that: the composite nanomaterial loaded with CuFeS 2 quantum dots has the advantages of large specific surface area and high photocatalytic performance; the CuFeS 2 quantum dots are uniformly distributed on the surface of the CuFeS 2/MXene composite nanomaterial prepared by the microwave method, and the MXene nanosheets have low oxidation degree, so that the photocatalytic performance of the composite nanomaterial is effectively improved.
Drawings
FIG. 1 is a scanning image of a transmission electron microscope of the composite nanomaterial made in example 1;
FIG. 2 is a powder X-ray diffraction chart of the composite nanomaterial made in example 1;
FIG. 3 is a scan of the elemental distribution of the composite nanomaterial made in example 1;
FIG. 4 is a high power transmission scan of the composite nanomaterial made in example 1;
FIG. 5 is a scanning image of a transmission electron microscope of the composite nanomaterial made in example 2;
FIG. 6 is a scanning image of a transmission electron microscope of the composite nanomaterial made in example 3;
FIG. 7 is a scanning image of a transmission electron microscope of the composite nanomaterial made in comparative example 1;
FIG. 8 is a graph showing the yields of nitrobenzene participating in photocatalytic reduction by using the materials prepared in examples and comparative examples.
Detailed Description
Example 1
Weighing 15mL of ethylene glycol and 15mL of isopropanol, uniformly mixing, weighing 0.2mmol of copper acetate monohydrate and 0.2mmol of ferrous acetate, adding into the mixed solution, adding 0.4mmol of thiourea, performing ultrasonic treatment for 15min, adding 36mg of freeze-dried Ti 3C2Tx MXene nano-sheets, stirring for 5min, adding the formed mother liquor into a 100mL flask, placing into a microwave reactor for microwave reaction for 4min, cooling to room temperature after taking out, performing three water washes and three alcohol washes on the product, and finally transferring into a 60 ℃ oven for drying for 6h to obtain the CuFeS 2/MXene composite nano-material; in the prepared CuFeS 2/MXene composite nano material, the mass ratio of the CuFeS 2 quantum dot to the MXene nano sheet is 1:1.
Example 2
Weighing 15mL of ethylene glycol and 15mL of isopropanol, uniformly mixing, weighing 0.02mmol of copper acetate monohydrate and 0.02mmol of ferrous acetate, adding into the previous mixed solution, adding 0.004mmol of thiourea, carrying out ultrasonic treatment for 15min, adding 36mg of freeze-dried Ti 3C2Tx MXene nano-sheets, stirring for 5min, adding the formed mother solution into a 100mL flask, placing into a microwave reactor for microwave reaction for 4min, taking out, cooling to room temperature, carrying out three water washes and three alcohol washes on the product, and finally transferring into a 60 ℃ oven for drying for 6h to obtain the CuFeS 2/MXene composite nano-material; in the prepared CuFeS 2/MXene composite nano material, the mass ratio of the CuFeS 2 quantum dot to the MXene nano sheet is 1:100.
Example 3
Weighing 10mL of ethylene glycol and 20mL of isopropanol, uniformly mixing, weighing 0.2mmol of copper acetate monohydrate and 0.2mmol of ferrous acetate, adding into the previous mixed solution, adding 0.1mmol of thiourea, carrying out ultrasonic treatment for 15min, adding 36mg of freeze-dried Ti 3C2Tx MXene nano-sheets, stirring for 5min, adding the formed mother liquor into a 100mL flask, placing into a microwave reactor for microwave reaction for 4min, taking out, cooling to room temperature, carrying out three water washes and three alcohol washes on the product, and finally transferring into a 60 ℃ oven for drying for 6h to obtain the CuFeS 2/MXene composite nano-material; in the prepared CuFeS 2/MXene composite nano material, the mass ratio of the CuFeS 2 quantum dot to the MXene nano sheet is 1:4.
Comparative example 1
Comparative example 1a hydrothermal process was used to prepare CuFeS 2/MXene composite nanomaterial.
And (3) weighing 10mL of ethylene glycol and 20mL of isopropanol, uniformly mixing, weighing 0.05mmol of copper acetate monohydrate and 0.05mmol of ferrous acetate, adding 0.1mmol of thiourea into the mixed solution, performing ultrasonic treatment for 15min, adding 36mg of freeze-dried Ti 3C2Tx MXene nano-sheets, stirring for 5min, adding the formed mother liquor into a 50mL of polytetrafluoroethylene liner, placing into a hydrothermal kettle, reacting for 8h at 180 ℃ in an oven, cooling to room temperature, performing three water washes and three alcohol washes on the product, and finally transferring into an oven at 60 ℃ to dry for 6h to obtain the CuFeS 2/MXene composite nano-material prepared by a hydrothermal method.
FIG. 1 is a transmission electron microscope image of the composite nanomaterial of example 1, from which it can be seen that the morphology of the sample is that nanoparticles are supported on two-dimensional nanoplatelets and the distribution is relatively uniform;
FIG. 2 is a powder X-ray diffraction pattern of the composite nanomaterial of example 1, from which it can be seen that the prepared sample has characteristic peaks of CuFeS 2 quantum dots (JCPDS: 37-0471) and MXene nanoplatelets;
FIG. 3 is an analytical chart of energy spectrum of the composite nanomaterial of example 1 dispersed on a molybdenum mesh, from which it can be seen that the composite nanomaterial of example 1 contains Ti, C, S, cu, fe, O elements;
FIG. 4 is a high power transmission electron microscope image of the composite nanomaterial of example 1, from which it can be seen that the CuFeS 2/MXene composite nanomaterial has a layer spacing of two-dimensional multi-layer MXene (1.24 nm) and a lattice of CuFeS 2 quantum dots (112), which illustrates the successful loading of the CuFeS 2 quantum dots on the MXene nanoplatelets;
FIG. 5 is a transmission electron microscope image of the composite nanomaterial of example 2, from which it can be seen that the morphology of the sample is that nanoparticles are loaded on two-dimensional MXene nanoplatelets and the distribution is relatively uniform;
FIG. 6 is a transmission electron microscope image of the composite nanomaterial of example 3, from which it can be seen that the morphology of the sample is that nanoparticles are loaded on two-dimensional MXene nanoplatelets and the distribution is relatively uniform;
FIG. 7 is a transmission electron microscope image of a composite nanomaterial obtained by reacting comparative example 1 at 180℃for 8 hours by a hydrothermal method, from which it can be seen that the morphology of the sample is that the two-dimensional MXene nanoplatelets are loaded with CuFeS 2 nanoparticles, the nanoparticle size is large and the distribution is relatively disordered, and at the same time, the hydrothermal method is long in time consumption, and the oxidation degree of the MXene nanoplatelets increases with the increase of time.
Fig. 8 shows the yields of the composite nanomaterial prepared in examples 1 to 3 and comparative example 1 in the photocatalytic reduction of nitrobenzene to aniline, and it can be seen that the composite nanomaterial in example 2, i.e., the mass ratio of CuFeS 2 quantum dots to MXene nanoplatelets is 1:4, has the highest performance in the photocatalytic reduction of nitrobenzene, and the yield of aniline and the selectivity of aniline production reach 99%.
Claims (4)
1. A CuFeS 2/MXene composite nano material is characterized in that: the CuFeS 2/MXene composite nano material consists of CuFeS 2 quantum dots and MXene nano sheets, wherein the CuFeS 2 quantum dots are loaded on the surfaces of the MXene nano sheets;
The preparation method of the CuFeS 2/MXene composite nano material specifically comprises the following steps: preparing a mixed solution containing Cu 2+ and Fe 2+, adding the mixed solution and thiourea into a solvent, and uniformly stirring by ultrasonic to obtain a solution containing CuFeS 2; adding MXene nano-sheets into a solution containing CuFeS 2, uniformly stirring, placing the solution in a microwave reactor for microwave for 3-8 min, taking out, centrifuging, washing and drying to obtain a CuFeS 2/MXene composite nano-material; wherein the solvent is prepared from the following components in volume ratio 1: 0.5-2 parts of ethylene glycol and isopropanol.
2. The CuFeS 2/MXene composite nanomaterial according to claim 1, characterized in that: the mass ratio of the CuFeS 2 quantum dot to the MXene nano-sheet is 1: 1-100.
3. The CuFeS 2/MXene composite nanomaterial according to claim 1, characterized in that: the molar ratio of the Cu 2+、Fe2+ to the thiourea is 1:1: 2-4.
4. The CuFeS 2/MXene composite nanomaterial according to claim 1, characterized in that: the drying temperature is 50-80 ℃, and the drying time is 4-8 hours.
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