CN115888780A - CuFeS 2 /MXene composite nano material and preparation method thereof - Google Patents
CuFeS 2 /MXene composite nano material and preparation method thereof Download PDFInfo
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- CN115888780A CN115888780A CN202211208273.6A CN202211208273A CN115888780A CN 115888780 A CN115888780 A CN 115888780A CN 202211208273 A CN202211208273 A CN 202211208273A CN 115888780 A CN115888780 A CN 115888780A
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- 239000002131 composite material Substances 0.000 title claims abstract description 53
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims description 13
- 239000002135 nanosheet Substances 0.000 claims abstract description 33
- 239000002096 quantum dot Substances 0.000 claims abstract description 20
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 20
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract description 5
- 239000011941 photocatalyst Substances 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 238000007146 photocatalysis Methods 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
- 230000000694 effects Effects 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- RKWJJKZGJHLOHV-UHFFFAOYSA-N ethane-1,2-diol;propan-2-ol Chemical compound CC(C)O.OCCO RKWJJKZGJHLOHV-UHFFFAOYSA-N 0.000 abstract 1
- 150000002505 iron Chemical class 0.000 abstract 1
- 230000033116 oxidation-reduction process Effects 0.000 abstract 1
- 239000011593 sulfur Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 10
- 238000005303 weighing Methods 0.000 description 8
- 239000012452 mother liquor Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001027 hydrothermal synthesis Methods 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 238000006243 chemical reaction 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
- 230000005540 biological transmission Effects 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
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 4
- 238000007254 oxidation 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
- 230000003647 oxidation Effects 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-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
- 238000010521 absorption reaction Methods 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
- 238000009826 distribution Methods 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
- 239000011229 interlayer Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 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
- 239000003960 organic solvent Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 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
- 238000011946 reduction process Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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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
Abstract
The invention discloses CuFeS 2 The composite nano material is prepared from CuFeS 2 Quantum dot and MXene nanosheet, cuFeS 2 The method comprises the steps of adopting a microwave method to dissolve copper salt, iron salt and sulfur source into isopropanol-ethylene glycol mixed solution, adding the MXene nanosheets, uniformly mixing, and then carrying out microwave heating for 3-8 min to obtain CuFeS 2 a/MXene composite nanomaterial; the method has the advantages of simple operation, short reaction time and low energy consumption, and the prepared composite nano material has better shapeAnd the photocatalyst has good oxidation-reduction effect when being applied to photocatalysis.
Description
Technical Field
The invention relates to a composite nano material, in particular to CuFeS 2 the/MXene composite nano material also relates to CuFeS 2 A preparation method of MXene composite nano material.
Background
Metal sulfide is a common photocatalyst, but the absorption rate of the photocatalyst to light is low, and the stability is poor, MXene is a novel 2D transition metal carbide, has high conductivity and a chemically active surface, but the application of MXene in the aspect of photoelectrocatalysis is limited because the photoproduction charge is rapidly compounded and is easily oxidized in the air. In the prior art, a method for constructing a heterojunction on MXene nano-chips is adopted to overcome the problem of photo-induced electron hole recombination, but the existing commonly used synthesis method of the composite nano-material based on MXene is a hydrothermal method, the reaction time is long, and nano-particles on MXene are easy to aggregate.
Disclosure of Invention
The purpose of the invention is as follows: one purpose of the invention is to provide CuFeS with high photocatalytic performance 2 a/MXene composite nanomaterial; another object of the present invention is to provide the above CuFeS 2 The preparation method of the MXene composite nano material has high preparation speed, the MXene nanosheet in the composite nano material has low oxidation degree, and CuFeS on the MXene nanosheet 2 The quantum dots are uniformly distributed.
The technical scheme is as follows: the CuFeS of the invention 2 the/MXene composite nano material consists of CuFeS 2 Quantum dot and MXene nanosheet, cuFeS 2 The quantum dots are loaded on the surface of the MXene nanosheet.
CuFeS 2 A heterojunction interface with strong binding force is formed between the quantum dot and the MXene nanosheet, so that the separation of photoproduction electron holes is promoted, the photocatalysis performance is improved, the separation rate of the electron holes on the MXene nanosheet under illumination is improved, and the electron holes respectively face CuFeS 2 The quantum dots and the MXene nano-chips move, and electron holes respectively participate in an oxidation reaction and a reduction reaction in a photocatalytic reaction.
Wherein the CuFeS 2 The mass ratio of the quantum dots to the MXene nanosheets is 1:1 to 100.CuFeS 2 MXene nanosheet coated CuFeS when quantum dot loading capacity is too large 2 The quantum dots are coated in a large amount, so that the specific surface area of the composite nano material is reduced, and active sites on the composite nano material are reduced.
The above CuFeS 2 The preparation method of the/MXene composite nano material comprises the following specific steps: preparation of a composition containing Cu 2+ And Fe 2+ Adding the mixed solution and thiourea into a solvent, and uniformly stirring by ultrasonic to obtain the mixed solution containing CuFeS 2 The solution of (1); to a reactor containing CuFeS 2 Adding MXene nanosheets into the solution, uniformly stirring, placing the solution in a microwave reactor for microwave for 3-8 min, taking out the solution, centrifuging, washing and drying to obtain CuFeS 2 the/MXene composite nanometer material.
CuFeS after microwave heating 2 The load forms heterojunction on MXene nano-sheet, realizes stirring on molecular level, overcomes the defect of nonuniform heating of hydrothermal method, and has the advantages of high heating speed, uniform heating, no temperature gradient, shortened reaction time and improved production efficiency.
Wherein, in the mixed solution, cu 2+ ：Fe 2+ : the molar ratio of thiourea is 1:1:2 to 4. Control of Cu 2+ ：Fe 2+ The molar ratio of (A) to (B) is equal, so that ferrous ions can be prevented from being oxidized into ferric ions; cuFeS is not easy to be synthesized when the thiourea content is too small 2 If too much thiourea is added, the MXene nanosheets may be vulcanized to form by-products.
Wherein the solvent is a mixture of the following components in a volume ratio of 1: 0.5-2 parts by weight of mixed ethylene glycol and isopropanol. Ethylene glycol with a high boiling point is selected as an organic solvent, so that the phenomenon that the solvent is excessively boiled for too long microwave time to cause a cavity in the microwave reactor is prevented; adding isopropanol with a lower boiling point, wherein the isopropanol is violently 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.
Has the beneficial effects that: compared with the prior art, the invention has the remarkable advantages that: the invention loads CuFeS 2 The composite nano material of the quantum dots has the advantages of large specific surface area and high photocatalytic performance; the CuFeS prepared by the microwave method 2 CuFeS is uniformly distributed on the surface of the/MXene composite nano material 2 The oxidation degree of the MXene nanosheets is low, so that the photocatalytic performance of the composite nanomaterial is effectively improved.
Drawings
FIG. 1 is a scanning electron microscope scan of the composite nanomaterial prepared in example 1;
FIG. 2 is a powder X-ray diffraction pattern of the composite nanomaterial prepared in example 1;
FIG. 3 is a scanned graph of the distribution of elements of the composite nanomaterial made in example 1;
FIG. 4 is a high power transmission scan of the composite nanomaterial prepared in example 1;
FIG. 5 is a scanning electron microscope scan of the composite nanomaterial prepared in example 2;
FIG. 6 is a scanning electron microscope scan of the composite nanomaterial prepared in example 3;
FIG. 7 is a scanning electron microscope scan of the composite nanomaterial prepared in comparative example 1;
FIG. 8 is a graph comparing the yields of nitrobenzene in the photocatalytic reduction processes using materials prepared in the 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, and adding 36mg of freeze-dried Ti 3 C 2 T x Stirring MXene nanosheets for 5min, adding the formed mother liquor into a 100mL flask, placing the flask into a microwave reactor for microwave reaction for 4min, taking out the mother liquor, cooling to room temperature, washing the product with water for three times and washing the product with alcohol for three times, and finally transferring the product into a drying oven at 60 ℃ for drying for 6h to obtain CuFeS 2 a/MXene composite nanomaterial; the prepared CuFeS 2 CuFeS in/MXene composite nano material 2 The mass ratio of the quantum dots to the MXene nanosheets is 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, performing ultrasonic treatment for 15min, and adding 36mg of freeze-dried Ti 3 C 2 T x Stirring MXene nanosheet for 5min, adding the formed mother liquor into a 100mL flask, placing the flask into a microwave reactor for microwave reaction for 4min, taking out the flask, cooling to room temperature, washing the product with water for three times and washing with alcohol for three times, and finally transferring the product into a drying oven at 60 ℃ for drying for 6h to obtain CuFeS 2 a/MXene composite nanomaterial; system for makingThe obtained CuFeS 2 CuFeS in/MXene composite nano material 2 The mass ratio of the quantum dots to the MXene nanosheets is 1.
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, performing ultrasonic treatment for 15min, and adding 36mg of freeze-dried Ti 3 C 2 T x Stirring MXene nanosheets for 5min, adding the formed mother liquor into a 100mL flask, placing the flask into a microwave reactor for microwave reaction for 4min, taking out the mother liquor, cooling to room temperature, washing the product with water for three times and washing the product with alcohol for three times, and finally transferring the product into a drying oven at 60 ℃ for drying for 6h to obtain CuFeS 2 a/MXene composite nanomaterial; the prepared CuFeS 2 CuFeS in/MXene composite nano material 2 The mass ratio of the quantum dots to the MXene nanosheets is 1.
Comparative example 1
Comparative example 1 preparation of CuFeS by hydrothermal method 2 a/MXene composite nano material.
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 into the mixed solution, adding 0.1mmol of thiourea, performing ultrasonic treatment for 15min, and adding 36mg of freeze-dried Ti 3 C 2 T x Stirring MXene nanosheets for 5min, adding the formed mother liquor into a 50mL polytetrafluoroethylene inner container, putting the mother liquor into a hydrothermal kettle, reacting for 8 hours in an oven at 180 ℃, cooling to room temperature, washing the product with water for three times and washing with alcohol for three times, and finally transferring the product into an oven at 60 ℃ for drying for 6 hours to obtain CuFeS prepared by a hydrothermal method 2 a/MXene composite nano material.
FIG. 1 is a transmission electron microscope photograph of the composite nanomaterial of example 1, from which it can be seen that the morphology of the sample is two-dimensional nano-sheets loaded with nano-particles and distributed relatively uniformly;
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 CuFeS 2 Characteristic peaks of quantum dots (JCPDS: 37-0471) and MXene nanosheets;
FIG. 3 is a graph of the energy spectrum analysis 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, and O elements;
FIG. 4 is a high power transmission electron micrograph of the composite nanomaterial of example 1, from which CuFeS can be seen 2 the/MXene composite nano material has the interlayer spacing (1.24 nm) of two-dimensional multilayer MXene and CuFeS 2 Lattice (112) of quantum dots, which illustrates CuFeS 2 The quantum dots are successfully loaded on the MXene nanosheets;
FIG. 5 is a transmission electron microscope image of the composite nanomaterial of example 2, from which it can be seen that the sample morphology is two-dimensional MXene nanosheets loaded with nanoparticles and distributed relatively uniformly;
FIG. 6 is a TEM image of the composite nanomaterial of example 3, from which it can be seen that the sample morphology is two-dimensional MXene nanosheets loaded with nanoparticles and relatively uniformly distributed;
FIG. 7 is a transmission electron microscope image of the composite nanomaterial obtained in comparative example 1 by hydrothermal reaction at 180 ℃ for 8 hours, from which it can be seen that the sample morphology is that CuFeS is loaded on two-dimensional MXene nanosheets 2 The nano particles have larger nano particle size and are distributed more disorderly, meanwhile, the hydrothermal method consumes long time, and the oxidation degree of the MXene nano sheets is increased along with the increase of time.
FIG. 8 shows the yields of the composite nanomaterials prepared in examples 1 to 3 and comparative example 1 participating in the photocatalytic reduction of nitrobenzene to aniline, and it can be seen that example 2, cuFeS 2 When the mass ratio of the quantum dots to the MXene nanosheets is 1.
Claims (6)
1. CuFeS 2 the/MXene composite nano material is characterized in that: the CuFeS 2 the/MXene composite nano material consists of CuFeS 2 Quantum dot and MXene nanosheet, cuFeS 2 The quantum dots are loaded on the surface of the MXene nanosheet.
2. CuFeS according to claim 1 2 the/MXene composite nano material is characterized in that: cuFeS 2 The mass ratio of the quantum dots to the MXene nanosheets is 1:1 to 100.
3. The CuFeS of claim 1 2 The preparation method of the/MXene composite nano material is characterized by comprising the following steps: preparation of a composition containing Cu 2+ And Fe 2+ Adding the mixed solution and thiourea into a solvent, and uniformly stirring by ultrasonic waves to obtain the mixed solution containing CuFeS 2 The solution of (1); to a reactor containing CuFeS 2 Adding MXene nanosheets into the solution, uniformly stirring, placing the solution in a microwave reactor for microwave for 3-8 min, taking out the solution, centrifuging, washing and drying to obtain CuFeS 2 the/MXene composite nanometer material.
4. CuFeS according to claim 3 2 The preparation method of the/MXene composite nano material is characterized by comprising the following steps: the Cu 2 + 、Fe 2+ And the molar ratio of thiourea is 1:1:2 to 4.
5. CuFeS according to claim 3 2 The preparation method of the/MXene composite nano material is characterized by comprising the following steps: the solvent is prepared from the following components in a volume ratio of 1: 0.5-2 parts by weight of mixed ethylene glycol and isopropanol.
6. CuFeS according to claim 3 2 The preparation method of the/MXene composite nano material is characterized by comprising the following steps: the drying temperature is 50-80 ℃, and the drying time is 4-8 h.
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| CN202211208273.6A CN115888780B (en) | 2022-09-30 | CuFeS2MXene composite nano material and preparation method thereof |
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| CN202211208273.6A CN115888780B (en) | 2022-09-30 | CuFeS2MXene composite nano material and preparation method thereof |
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| CN115888780A true CN115888780A (en) | 2023-04-04 |
| CN115888780B CN115888780B (en) | 2024-04-26 |
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