CN113083328A - MoS2Preparation method and application of Ag-In-Zn-S quantum dot co-modified with hole extraction functionalized carbon quantum dot - Google Patents
MoS2Preparation method and application of Ag-In-Zn-S quantum dot co-modified with hole extraction functionalized carbon quantum dot Download PDFInfo
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 62
- 229910007609 Zn—S Inorganic materials 0.000 title claims abstract description 34
- 238000000605 extraction Methods 0.000 title claims abstract description 34
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 8
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 146
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 83
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- 238000005406 washing Methods 0.000 claims abstract description 44
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 42
- 239000002243 precursor Substances 0.000 claims abstract description 34
- 238000002360 preparation method Methods 0.000 claims abstract description 33
- 239000001257 hydrogen Substances 0.000 claims abstract description 31
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 claims abstract description 31
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 230000001699 photocatalysis Effects 0.000 claims abstract description 29
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 23
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 23
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 23
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 21
- 238000001816 cooling Methods 0.000 claims abstract description 19
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims abstract description 9
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004246 zinc acetate Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 239000004201 L-cysteine Substances 0.000 claims abstract description 3
- 235000013878 L-cysteine Nutrition 0.000 claims abstract description 3
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 90
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000004809 Teflon Substances 0.000 claims description 3
- 229920006362 Teflon® Polymers 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims 1
- 239000011941 photocatalyst Substances 0.000 abstract description 30
- 238000005215 recombination Methods 0.000 abstract description 3
- 230000006798 recombination Effects 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 230000005284 excitation Effects 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract 1
- 230000003000 nontoxic effect Effects 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 19
- 229910052799 carbon Inorganic materials 0.000 description 19
- 238000011156 evaluation Methods 0.000 description 17
- PWKSKIMOESPYIA-UHFFFAOYSA-N 2-acetamido-3-sulfanylpropanoic acid Chemical compound CC(=O)NC(CS)C(O)=O PWKSKIMOESPYIA-UHFFFAOYSA-N 0.000 description 16
- 238000005303 weighing Methods 0.000 description 16
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 description 15
- 238000000926 separation method Methods 0.000 description 10
- GPRSOIDYHMXAGW-UHFFFAOYSA-N cyclopenta-1,3-diene cyclopentanecarboxylic acid iron Chemical compound [CH-]1[CH-][CH-][C-]([CH-]1)C(=O)O.[CH-]1C=CC=C1.[Fe] GPRSOIDYHMXAGW-UHFFFAOYSA-N 0.000 description 6
- 239000002131 composite material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000005424 photoluminescence Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000004770 highest occupied molecular orbital Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002057 nanoflower Substances 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000002211 L-ascorbic acid Substances 0.000 description 1
- 235000000069 L-ascorbic acid Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000005525 hole transport Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910000337 indium(III) sulfate Inorganic materials 0.000 description 1
- XGCKLPDYTQRDTR-UHFFFAOYSA-H indium(iii) sulfate Chemical compound [In+3].[In+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGCKLPDYTQRDTR-UHFFFAOYSA-H 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 description 1
- 229910000367 silver sulfate Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
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Abstract
The invention belongs to the technical field of nano material preparation, relates to a photocatalyst, and particularly relates to a MoS2The preparation method of the Ag-In-Zn-S quantum dot co-modified with the hole extraction functionalized carbon quantum dots (fCDs) comprises the following steps: dissolving silver nitrate, indium nitrate, zinc acetate and L-cysteine in water, and adjusting the pH value to 8.5 by using a NaOH solution; continuously adding an fCDs precursor and thioacetamide, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110-140 ℃ for 2-4 h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs; the prepared AIZS/fCDs and MoS2Dissolving the precursor in water, mechanically stirring for 8-16 h, centrifuging, and washing to obtain the product. The invention also relates to the prepared MoS2the/AIZS/fCDs photocatalyst is applied to photocatalytic hydrogen production. The invention has simple process, low cost and easy obtainmentIs convenient for batch production, is nontoxic and harmless, and meets the environment-friendly requirement. Under the excitation of visible light, photogenerated holes and electrons are respectively and rapidly transferred to MoS2And the recombination occurrence is reduced on the fCDs, so that more electrons can be used for hydrogen production reaction, and the photocatalytic performance is improved.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, relates to a photocatalyst, and particularly relates to a MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method and application of/AIZS/fCDs).
Background
Photocatalytic water splitting is considered to be one of the most desirable methods for producing hydrogen directly from continuous solar energy and water. Visible light accounts for about 43% of sunlight, plays a key role in better utilization of solar energy, and the utilization rate is far lower than expected. Quantum Dots (QDs) are considered to be the most promising visible light active photocatalyst candidate particles due to unique Quantum confinement effects, desirable optical properties and large specific surface area. Compared with the traditional II-VI quantum dots, the cadmium-free I-III-VI quantum dots attract wide attention in the field of photocatalysis due to the adjustable forbidden bandwidth and low toxicity of the components, and are the most promising visible light activity candidate quantum dots. However, the charge separation efficiency is low, and the improvement of the catalytic activity is severely limited, so that the further improvement of the charge separation efficiency of the photocatalyst is particularly important.
In photocatalytic research, the promoter plays an important role in improving charge separation efficiency, such as molybdenum disulfide (MoS) with high conductivity2) Nanosheets, which have excellent conductivity making them excellent electron promoters; carbon quantum dots (CDs) for theirThe existence of multiple energy levels can be used as an electron donor and an electron acceptor (electron mediator) and can play a key role in designing the photocatalyst, and CDs are expected to be used as hole transport materials by adjusting the Highest Occupied Molecular Orbital (HOMO) energy level to realize efficient hole transfer.
In view of the analysis, the invention modifies ferrocenecarboxylic acid (FcA) In CDs to form hole extraction functionalized carbon dots (fCDs) with a hole extraction effect, compounds the carbon dots with Ag-In-Zn-S quantum dots In an In-situ synthesis mode to construct AIZS/fCDs, and loads the AIZS/fCDs on MoS by a mechanical stirring method2The nano-chip is used for research in the field of photocatalytic hydrogen production.
Disclosure of Invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2/AIZS/fCDs).
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. dissolving silver nitrate, indium nitrate, zinc acetate and L-cysteine in water, and adjusting the pH value to 8.5 by using a 1M NaOH solution, wherein the weight ratio of the silver nitrate: indium nitrate: zinc acetate: l-cysteine: the molar volume ratio of water is 0.17-0.51 mmol: 0.17-1.7 mmol: 0.17-0.85 mmol: 5 mmol: 5.5mL, preferably 0.34 mmol: 1.7 mmol: 0.85 mmol: 5 mmol: 5.5 mL;
B. continuously adding an fCDs precursor and thioacetamide into the solution, performing ultrasonic stirring uniformly, performing hydrothermal reaction at 110-140 ℃ for 2-4 h, preferably at 110 ℃ for 4h, cooling to room temperature, centrifuging, and washing to obtain AIZS/fCDs, wherein the fCDs precursor: thioacetamide: the molar volume ratio of water is 3.48-17.4 mmol: 0.4-3.2 mmol: 5.5mL, preferably 14 mmol: 3.2 mmol: 5.5mL, wherein the water is the water in the step A;
C. the prepared AIZS/fCDs and MoS2Dissolving the precursor in water, mechanically stirring for 8-16 h, preferably 12h, centrifuging and washing to obtain MoS2/AIZS/fCDs, whichThe AIZS/fCDs of (1): MoS2Precursor: the mass volume ratio of water is 100 mg: 3-15 mg: 10mL, preferably 100 mg: 9 mg: 10 mL.
In a preferred embodiment of the present invention, the preparation method of the fCDs precursor in step B is: dissolving carbon quantum dots (CDs) and FcA in dimethyl sulfoxide, carrying out constant volume to 20mL, carrying out a solvothermal reaction at 110-140 ℃ for 2-4 h, preferably at 140 ℃ for 4h, centrifuging, and washing to obtain the carbon quantum dots (CDs): FcA, the mass-to-volume ratio is 3-15 mg: 0.48-2.4 mg, preferably 12 mg: 1.92 mg.
In a preferred embodiment of the present invention, in step C, the MoS is described2A precursor, a method of making the same: 1mmol of (NH)4)6Mo7O24 4H2O and 30mmol of CH4N2Dissolving S in 35mL of deionized water, stirring vigorously for 20min to form a uniform solution, placing the uniform solution into a 50mL stainless steel high pressure apparatus with a Teflon lining, carrying out hydrothermal reaction at 160-240 ℃ for 12-24 h, preferably at 220 ℃ for 18h, and washing with 0.1M HCl to completely remove NH4 +And drying at 60 ℃ in vacuum to obtain the product.
MoS prepared by the invention2the/AIZS/fCDs photocatalyst is in the shape that quantum dots are attached to nanoflowers.
Another object of the present invention is to provide the obtained MoS2the/AIZS/fCDs photocatalyst is applied to photocatalytic hydrogen production.
Evaluation of photocatalytic activity:
0.02g (MoS) is weighed2the/AIZS/fCDs) photocatalyst, 0.528g (L-ascorbic acid) hole sacrificial agent and 15ml distilled water are added into the photoreactor to be completely dissolved, and N is introduced at a large flow rate2Exhausting gas in the gas waiting reactor; under magnetic stirring, turning on a white light LED lamp with the power of 300W for continuous illumination for 5h, and sampling and analyzing once every 1 h; the hydrogen production rate is calculated.
The invention utilizes the higher visible light response capability of Ag-In-Zn-S quantum dots and adopts an electronic cocatalyst (MoS)2) And the hole promoters (fCDs) respectively accelerate the extraction of electrons and holes, greatly reduce the charge recombination probability, realize high-efficiency charge separation efficiency, and improveThe hydrogen production efficiency by photolysis of water. MoS2The AIZS quantum dots and the fCDs can be uniformly loaded on MoS for nanoflower2So as to fix the composite photocatalyst and effectively increase the catalytic active sites.
Advantageous effects
The invention has simple process, low price, easy obtainment, convenient batch production, no toxicity and no harm, and meets the environment-friendly requirement. Realize at MoS2Under the modification of the fCDs double-promoter, an electron hole synergistic effect is formed to improve the charge separation efficiency and research of photocatalytic efficient hydrogen production. Under the excitation of visible light, photogenerated holes and electrons are respectively and rapidly transferred to MoS2And the fCDs, the recombination is greatly reduced, so that more electrons can be used for hydrogen production reaction, and the photocatalytic performance is improved.
Drawings
FIG. 1.MoS2/AIZS/fCDs、MoS2And XRD diffractogram of AIZS photocatalyst;
FIG. 2.MoS2/AIZS/fCDs、AIZS/fCDs、AIZS/MoS2And ultraviolet-visible absorption (a) and photoluminescence (b) patterns of the AIZS photocatalyst;
FIG. 3.MoS2Transmission plot of/AIZS/fCDs;
FIG. 4.MoS2/AIZS/fCDs、AIZS/fCDs、AIZS/MoS2And a photocatalytic hydrogen production curve (a) and a hydrogen production rate map (b) for AIZS;
FIG. 5.MoS2/AIZS/fCDs、AIZS/fCDs、AIZS/MoS2And the electrochemical impedance plot of AIZS.
Detailed Description
The present invention will be described in detail below with reference to examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
The preparation method of the fCDs precursor comprises the following steps: dissolving carbon quantum dots (CDs) and FcA in dimethyl sulfoxide, carrying out constant volume to 20mL, carrying out a solvothermal reaction at 110-140 ℃ for 2-4 h, preferably reacting at 140 ℃ for 4h, centrifuging, and washing to obtain the carbon quantum dots (CDs): FcA, the mass-to-volume ratio is 3-15 mg: 0.48-2.4 mg, preferably 12 mg: 1.92 mg.
The MoS of the invention2The preparation method of the precursor comprises the following steps: 1mmol of (NH)4)6Mo7O24 4H2O and 30mmol of CH4N2Dissolving S in 35mL of deionized water, stirring vigorously for 20min to form a uniform solution, placing the uniform solution into a 50mL stainless steel high pressure apparatus with a Teflon lining, carrying out hydrothermal reaction at 160-240 ℃ for 12-24 h, preferably at 220 ℃ for 18h, and washing with 0.1M HCl to completely remove NH4 +And drying at 60 ℃ in vacuum.
Example 1
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. weighing 0.34mmol of silver nitrate, 1.7mmol of indium nitrate, 0.85mmol of zinc acetate dihydrate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using a 1M NaOH solution;
B. continuously adding 3.48mmol of fCDs precursor and 3.2mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 9mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: calculated, the MoS obtained in this example2The hydrogen production rate was 5.1 mmol/g/h/AIZS/fCDs.
Example 2
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. weighing 0.34mmol of silver nitrate, 1.7mmol of indium nitrate, 0.85mmol of zinc acetate dihydrate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using a 1M NaOH solution;
B. continuously adding 6.96mmol of fCDs precursor and 3.2mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 9mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: calculated, the MoS obtained in this example2The hydrogen production rate was 5.8 mmol/g/h/AIZS/fCDs.
Example 3
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. weighing 0.34mmol of silver nitrate, 1.7mmol of indium nitrate, 0.85mmol of zinc acetate dihydrate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using a 1M NaOH solution;
B. continuously adding 10.44mmol of fCDs precursor and 3.2mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 9mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: calculated, the MoS obtained in this example2The hydrogen production rate per AIZS/fCDs was 6.3 mmol/g/h.
Example 4
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. weighing 0.34mmol of silver nitrate, 1.7mmol of indium nitrate, 0.85mmol of zinc acetate dihydrate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using a 1M NaOH solution;
B. continuously adding 13.92mmol of fCDs precursor and 3.2mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 9mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: calculated, the MoS obtained in this example2The hydrogen production rate per AIZS/fCDs was 8.2 mmol/g/h.
Example 5
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. weighing 0.34mmol of silver nitrate, 1.7mmol of indium nitrate, 0.85mmol of zinc acetate dihydrate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using a 1M NaOH solution;
B. continuously adding 17.4mmol of fCDs precursor and 3.2mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 9mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: calculated, the MoS obtained in this example2The hydrogen production rate was 5.4 mmol/g/h/AIZS/fCDs.
Example 6
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. weighing 0.17mmol of silver nitrate, 1.7mmol of indium nitrate, 0.85mmol of zinc acetate dihydrate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using a 1M NaOH solution;
B. continuously adding 13.92mmol of fCDs precursor and 3.2mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 9mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: calculated, the MoS obtained in this example2The hydrogen production rate per AIZS/fCDs was 4.2 mmol/g/h.
Example 7
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. weighing 0.51mmol of silver nitrate, 1.7mmol of indium nitrate, 0.85mmol of zinc acetate dihydrate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using a 1M NaOH solution;
B. continuously adding 13.92mmol of fCDs precursor and 3.2mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 9mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: calculated, the MoS obtained in this example2The hydrogen production rate was 7.1 mmol/g/h/AIZS/fCDs.
Example 8
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. weighing 0.51mmol of silver nitrate, 1.7mmol of indium nitrate, 0.85mmol of zinc acetate dihydrate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using a 1M NaOH solution;
B. continuously adding 13.92mmol of fCDs precursor and 0.8mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 9mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: is calculated byMoS made in this example2The hydrogen production rate was 1.4 mmol/g/h/AIZS/fCDs.
Example 9
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. weighing 0.51mmol of silver nitrate, 1.7mmol of indium nitrate, 0.85mmol of zinc acetate dihydrate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using a 1M NaOH solution;
B. continuously adding 13.92mmol of fCDs precursor and 1.6mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 9mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: calculated, the MoS obtained in this example2The hydrogen production rate was 3.8 mmol/g/h/AIZS/fCDs.
Example 10
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. weighing 0.51mmol of silver nitrate, 1.7mmol of indium nitrate, 0.85mmol of zinc acetate dihydrate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using a 1M NaOH solution;
B. continuously adding 13.92mmol of fCDs precursor and 2.4mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 9mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: calculated, the MoS obtained in this example2The hydrogen production rate per AIZS/fCDs was 6.4 mmol/g/h.
Example 11
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. weighing 0.51mmol of silver nitrate, 1.7mmol of indium nitrate, 0.85mmol of zinc acetate dihydrate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using a 1M NaOH solution;
B. continuously adding 13.92mmol of fCDs precursor and 3.2mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 3mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: calculated, the MoS obtained in this example2The hydrogen production rate per AIZS/fCDs was 4.1 mmol/g/h.
Example 12
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. weighing 0.51mmol of silver nitrate, 1.7mmol of indium nitrate, 0.85mmol of zinc acetate dihydrate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using a 1M NaOH solution;
B. continuously adding 13.92mmol of fCDs precursor and 3.2mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 6mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: calculated, the MoS obtained in this example2The hydrogen production rate per AIZS/fCDs was 6.4 mmol/g/h.
Example 13
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. weighing 0.51mmol of silver nitrate, 1.7mmol of indium nitrate, 0.85mmol of zinc acetate dihydrate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using a 1M NaOH solution;
B. continuously adding 13.92mmol of fCDs precursor and 3.2mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 9mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: calculated, the MoS obtained in this example2The hydrogen production rate per AIZS/fCDs was 8.2 mmol/g/h.
Example 14
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. weighing 0.51mmol of silver nitrate, 1.7mmol of indium nitrate, 0.85mmol of zinc acetate dihydrate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using a 1M NaOH solution;
B. continuously adding 13.92mmol of fCDs precursor and 3.2mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 12mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: calculated, the MoS obtained in this example2The hydrogen production rate was 7.0 mmol/g/h/AIZS/fCDs.
Example 15
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2/AIZS/fCDs), comprising:
A. weighing 0.51mmol of silver nitrate, 1.7mmol of indium nitrate, 0.85mmol of zinc acetate dihydrate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using a 1M NaOH solution;
B. continuously adding 13.92mmol of fCDs precursor and 3.2mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 15mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: calculated, the MoS obtained in this example2The hydrogen production rate per AIZS/fCDs was 4.2 mmol/g/h.
Example 16
MoS2Co-modifying Ag-In-Zn-S quantum dots (MoS) with hole extraction functionalized carbon quantum dots2A preparation method of/AIZS/fCDs), comprising the following steps:
A. weighing 0.51mmol of silver sulfate, 1.7mmol of indium sulfate, 0.85mmol of zinc sulfate and 5mmol of L-cysteine, dissolving in 5.5mL of water, and adjusting the pH value to 8.5 by using 1M NaOH solution;
B. continuously adding 13.92mmol of fCDs precursor and 3.2mmol of thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110 ℃ for 4h, cooling to room temperature, centrifuging and washing to obtain AIZS/fCDs;
C. 100mg of the AIZS/fCDs and 3mg of MoS prepared were transferred2Dissolving in 10mL water, mechanically stirring for 12h, centrifuging, and washing to obtain MoS2/AIZS/fCDs。
Evaluation of photocatalytic activity of photocatalyst: calculated, the MoS obtained in this example2The hydrogen production rate was 7.9 mmol/g/h/AIZS/fCDs.
FIG. 1.MoS2/AIZS/fCDs、MoS2And XRD diffractogram of AIZS photocatalyst; the XRD diffractogram shows that MoS is a good candidate for MoS2When the mass fraction of (2) is 9%, MoS does not appear2When the mass fraction reached 13%, a clear peak appearedApparent MoS2Diffraction peaks to illustrate MoS2MoS of/AIZS/fCDs2Successful composition of the composite; and the diffraction peak of AIZS is also in MoS2The appearance in/AIZS/fCDs demonstrates the successful synthesis of the composite.
FIG. 2.MoS2/AIZS/fCDs、AIZS/fCDs、AIZS/MoS2And ultraviolet-visible absorption (a) and photoluminescence (b) patterns of the AIZS photocatalyst; as can be seen from FIG. 2a, the AIZS is loaded with MoS2After fCDs, the light absorption intensity is obviously improved, and the improvement is in MoS2More pronounced in/AIZS/fCDs. In fig. 2b, a lower photoluminescence intensity indicates a better separation efficiency. As can be seen, MoS2The strength of/AIZS/fCDs is lower than that of the material, indicating that MoS2the/AIZS/fCDs have better separation efficiency compared with other materials.
FIG. 3.MoS2Transmission plot of/AIZS/fCDs; MoS is seen in FIG. 32Presence of composite materials, but due to MoS2The presence of quantum dots cannot be seen clearly.
FIG. 4.MoS2/AIZS/fCDs、AIZS/fCDs、AIZS/MoS2And a photocatalytic hydrogen production curve (a) and a hydrogen production rate map (b) for AIZS; as seen in FIG. 4, MoS2The hydrogen production rate of/AIZS/fCDs reaches 8.2mmol g-1h-120.5 times of pure AIZS quantum dots, 5.7 times of AIZS-fCDs and AIZS-MoS26.5 times of the total weight of the powder. Demonstration of MoS2And fCDs function to effectively promote charge separation.
FIG. 5.MoS2/AIZS/fCDs、AIZS/fCDs、AIZS/MoS2And the electrochemical impedance plot of AIZS. The radial size of the electrochemical impedance represents the separation efficiency of the sample charge, and MoS is shown in the figure2The radius of the/AIZS/fCDs is much smaller than that of the remaining material, illustrating on the other hand the MoS2The charge separation efficiency of/AIZS/fCDs is the best.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (10)
1.MoS2The preparation method of the Ag-In-Zn-S quantum dot co-modified with the hole extraction functionalized carbon quantum dot is characterized by comprising the following steps:
A. dissolving silver nitrate, indium nitrate, zinc acetate and L-cysteine in water, and adjusting the pH value to 8.5 by using a 1M NaOH solution, wherein the weight ratio of the silver nitrate: indium nitrate: zinc acetate: l-cysteine: the molar volume ratio of water is 0.17-0.51 mmol: 0.17-1.7 mmol: 0.17-0.85 mmol: 5 mmol: 5.5 mL;
B. continuously adding an fCDs precursor and thioacetamide into the solution, uniformly stirring by ultrasonic, carrying out hydrothermal reaction at 110-140 ℃ for 2-4 h, cooling to room temperature, centrifuging, and washing to obtain AIZS/fCDs, wherein the fCDs precursor: thioacetamide: the molar volume ratio of water is 3.48-17.4 mmol: 0.4-3.2 mmol: 5.5mL, wherein the water is the water in the step A;
C. the prepared AIZS/fCDs and MoS2Dissolving the precursor in water, mechanically stirring for 8-16 h, centrifuging and washing to obtain MoS2(ii)/AIZS/fCDs, wherein the AIZS/fCDs: MoS2Precursor: the mass volume ratio of water is 100 mg: 3-15 mg: 10 mL.
2. The MoS of claim 12The preparation method of the Ag-In-Zn-S quantum dot co-modified with the hole extraction functionalized carbon quantum dot is characterized by comprising the following steps: step A, silver nitrate: indium nitrate: zinc acetate: l-cysteine: the molar volume ratio of water is 0.34 mmol: 1.7 mmol: 0.85 mmol: 5 mmol: 5.5 mL.
3. The MoS of claim 12The preparation method of the Ag-In-Zn-S quantum dot co-modified with the hole extraction functionalized carbon quantum dot is characterized by comprising the following steps: and B, continuously adding the fCDs precursor and thioacetamide into the solution, uniformly stirring by ultrasonic, and carrying out hydrothermal reaction at 110 ℃ for 4 hours.
4. The MoS of claim 12And hole extractionThe preparation method of the functionalized carbon quantum dot co-modified Ag-In-Zn-S quantum dot is characterized by comprising the following steps: step B the fCDs precursor: thioacetamide: the molar volume ratio of water is 14 mmol: 3.2 mmol: 5.5 mL.
5. The MoS of claim 12The preparation method of the Ag-In-Zn-S quantum dot co-modified with the hole extraction functionalized carbon quantum dot is characterized by comprising the following steps: the preparation method of the fCDs precursor in the step B comprises the following steps: dissolving carbon quantum dots CDs and FcA in dimethyl sulfoxide, carrying out constant volume to 20mL, carrying out a thermal reaction for 2-4 h in a 110-140 ℃ solvent, preferably carrying out a reaction for 4h at 140 ℃, centrifuging, and washing to obtain the carbon quantum dots CDs: FcA, the mass-to-volume ratio is 3-15 mg: 0.48-2.4 mg, preferably 12 mg: 1.92 mg.
6. The MoS of claim 12The preparation method of the Ag-In-Zn-S quantum dot co-modified with the hole extraction functionalized carbon quantum dot is characterized by comprising the following steps: step C, the prepared AIZS/fCDs and MoS2Dissolved in water and mechanically stirred for 12 h.
7. The MoS of claim 12The preparation method of the Ag-In-Zn-S quantum dot co-modified with the hole extraction functionalized carbon quantum dot is characterized by comprising the following steps: step C said AIZS/fCDs: MoS2: the mass volume ratio of water is 100 mg: 9 mg: 10 mL.
8. The MoS of claim 12The preparation method of the Ag-In-Zn-S quantum dot co-modified with the hole extraction functionalized carbon quantum dot is characterized In that the MoS In the step C is2The preparation method of the precursor comprises the following steps: 1mmol of (NH)4)6Mo7O24 4H2O and 30mmol of CH4N2Dissolving S in 35mL of deionized water, stirring vigorously for 20min to form a uniform solution, placing the uniform solution into a 50mL stainless steel high-pressure apparatus lined with Teflon, carrying out hydrothermal reaction at 160-240 ℃ for 12-24 h, preferably at 220 ℃ for 18h, and washing with 0.1M HCl to completely remove NH4 +And drying at 60 ℃ in vacuum to obtain the product.
9. MoS made according to the method of any of claims 1-82And modifying the Ag-In-Zn-S quantum dots together with the hole extraction functionalized carbon quantum dots.
10. The MoS of claim 92The application of the Ag-In-Zn-S quantum dot co-modified with the hole extraction functionalized carbon quantum dot is characterized In that: the method is applied to photocatalytic hydrogen production.
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