CN111298833A - MoS based on carbazole functionalization2Quantum dot, preparation method and application - Google Patents
MoS based on carbazole functionalization2Quantum dot, preparation method and application Download PDFInfo
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- UJOBWOGCFQCDNV-UHFFFAOYSA-N 9H-carbazole Chemical compound C1=CC=C2C3=CC=CC=C3NC2=C1 UJOBWOGCFQCDNV-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002096 quantum dot Substances 0.000 claims abstract description 80
- 239000000243 solution Substances 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000007306 functionalization reaction Methods 0.000 claims abstract description 15
- 239000001257 hydrogen Substances 0.000 claims abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 10
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 8
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000018417 cysteine Nutrition 0.000 claims abstract description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 6
- 239000010935 stainless steel Substances 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 6
- 238000005119 centrifugation Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims abstract description 3
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000000502 dialysis Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 2
- 229910052961 molybdenite Inorganic materials 0.000 abstract description 56
- 229910052982 molybdenum disulfide Inorganic materials 0.000 abstract description 56
- 230000000694 effects Effects 0.000 abstract description 10
- 238000005286 illumination Methods 0.000 abstract description 5
- 230000001052 transient effect Effects 0.000 abstract description 3
- 229910021607 Silver chloride Inorganic materials 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000002484 cyclic voltammetry Methods 0.000 description 4
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000000157 electrochemical-induced impedance spectroscopy Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910015667 MoO4 Inorganic materials 0.000 description 2
- 229910004619 Na2MoO4 Inorganic materials 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 239000011865 Pt-based catalyst Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000005516 deep trap Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004768 lowest unoccupied molecular orbital Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000276 potassium ferrocyanide Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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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
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- B01J27/051—Molybdenum
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Abstract
The invention discloses MoS based on carbazole functionalization2The quantum dot, the preparation method and the application thereof, wherein the preparation method comprises the following steps: s1: dissolving sodium molybdate and cysteine in deionized water to obtain a solution A; s2: dissolving carbazole in ethanol to obtain a solution B; s3: mixing and stirring the solution A in the S1 and the solution B in the S2, and transferring the mixed solution into a stainless steel autoclave for reaction; s4: after the reaction product in S3 is naturally cooled to room temperature, taking the supernatant for centrifugation, and purifying the centrifugate to obtain the MoS based on carbazole functionalization2A quantum dot solution. Book (I)MoS based on carbazole functionalization prepared by invention2The quantum dots have better transient photocurrent, and the current density reaches the maximum value of-2.82 mA/cm by taking the LSV stable value after 60 cycles of CV‑1Jordan of MoS2168% of the quantum dot illumination current, illustrating the carbazole-functionalized based MoS prepared herein2The quantum dots remarkably improve the photoelectric hydrogen evolution effect, compared with MoS2The quantum dot can perform photoelectric hydrogen evolution more efficiently and stably.
Description
Technical Field
The invention relates to the technical field of material synthesis, in particular to MoS based on carbazole functionalization2Quantum dot, preparation method and application.
Background
Energy and environmental challenges constitute an increasingly serious threat to the sustainable development of mankind in the 21 st century, and in order to solve the energy crisis problem, researchers have been working on finding alternative low-cost, clean and sustainable energy sources to convert solar energy into solar fuels such as hydrogen, and photoelectrochemical cells (PECs) have been widely used. The catalyst is an important part in the photoelectric hydrogen evolution reaction, however, the development of the photoelectric hydrogen evolution industry is restricted by the problems of low photoelectric conversion efficiency, low reaction activity and the like of the existing photoelectric hydrogen evolution catalyst.
MoS2The catalyst has strong small-size effect, edge effect, quantum limit effect and domain effect, has unique electrical and optical properties, is a two-dimensional non-noble metal cathode catalyst which is expected to replace a Pt-based catalyst, and still has the problems of low visible light utilization rate, high carrier recombination rate, few active sites and the like.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a MoS based on carbazole functionalization2The quantum dot, the preparation method and the application have better photoelectric hydrogen evolution effect.
The invention provides MoS based on carbazole functionalization2The preparation method of the quantum dot comprises the following steps:
s1: dissolving sodium molybdate and cysteine in deionized water to obtain a solution A;
s2: dissolving carbazole in ethanol to obtain a solution B;
s3: mixing and stirring the solution A in the S1 and the solution B in the S2, and transferring the mixed solution into a stainless steel autoclave for reaction;
s4: after the reaction product in S3 is naturally cooled to room temperature, taking the supernatant for centrifugation, and purifying the centrifugate to obtain the MoS based on carbazole functionalization2A quantum dot solution.
Preferably, the mass-to-volume ratio of the sodium molybdate, the cysteine and the deionized water in the S1 is 1g:2-3g:300-500 mL.
Preferably, the mass-to-volume ratio of carbazole to ethanol in S2 is 1g: 1.15-1.25L.
Preferably, the mass ratio of the sodium molybdate to the carbazole in the S3 is 13-16g:1 g.
Preferably, the reaction conditions of S3 are: the temperature is 180 ℃ and 200 ℃, and the time is 36-48 h.
Preferably, the centrifugation conditions in S4 are: the rotating speed is 8000-.
Preferably, the purification conditions in S4 are: purified with deionized water in a 500Da dialysis bag for 4-8 h.
MoS prepared by the method and based on carbazole functionalization2And (4) quantum dots.
The invention provides the MoS based on carbazole functionalization2The quantum dot is applied to photoelectric hydrogen evolution.
The action mechanism is as follows:
the carbazole may be in MoS2A deep trap level is formed between the valence band and the conduction band, and electrons are transited from the valence band to the conduction band by absorbing an external energy source (visible light) and then released to a defect level formed by impurity ions. The excited electrons can recombine with the holes remaining in the conduction band and can be transferred to the defect levels of copper and manganese by radiation. Thus, efficient charge transfer between particles prevents electron-hole recombination. When carbazole reacts with MoS2The quantum dots are compounded, and photoproduction electrons are transferred between a conduction band and a valence band to inhibit charge recombination. Carbazole as MoS2The organic molecule donor is beneficial to transferring photoelectrons to the surface of ITO (indium tin oxide), prolongs the service life of a photon-generated carrier, resists photocurrent corrosion and improves photocurrent stability.
Compared with the prior art, the invention has the beneficial technical effects that:
(1) MoS based on carbazole functionalization prepared by the present application2The quantum dots have better transient photocurrent, namely the LSV stable value after 60 cycles of CV and the current densityReaches the maximum value of-2.82 mA/cm-1Jordan of MoS2168% of the quantum dot illumination current, illustrating the carbazole-functionalized based MoS prepared herein2The quantum dots remarkably improve the photoelectric hydrogen evolution effect, compared with MoS2The quantum dot can perform photoelectric hydrogen evolution more efficiently and stably.
(2) The present application is in the preparation of MoS based on carbazole functionalization2In the case of quantum dots, the two solutions are directly mixed and then reacted, compared with the prior method for preparing MoS firstly2The preparation method has the advantages that the equipment and conditions are simple, other additives are not needed, the prepared product has good dispersibility, and the problems of secondary dispersion, difficult surface coating and the like are solved.
Drawings
FIG. 1 shows (a) an HRTEM image, (b) a partial magnified view of FIG. (a), and (c) carbazole-functionalized MoS2EDS spectra and elemental composition of quantum dots;
FIG. 2 is (a) carbazole functionalized MoS2Quantum dot (b) MoS2A quantum dot infrared image;
FIG. 3 shows (a)0.0084g carbazole in 10ml ethanol solution (b) MoS2Quantum dots and (c) carbazole functionalized MoS2Fluorescence emission spectra of the quantum dots;
FIG. 4 is (a) carbazole functionalized MoS2Quantum dots, (b) MoS2Ultraviolet absorption spectra of quantum dots;
FIG. 5 shows (a) bare ITO and (b) MoS2Quantum dot (c) carbazole functionalized MoS2An electrochemical impedance profile of the quantum dot;
FIG. 6 shows (a) MoS2Quantum dots, (b) carbazole functionalized MoS2Cyclic voltammetry spectra of the quantum dots;
FIG. 7 shows (a) MoS2Quantum dots, (b) carbazole functionalized MoS2The photoelectric properties of the quantum dots;
FIG. 8 shows MoS2Quantum dot, carbazole functionalized MoS2Photoelectric hydrogen evolution map of quantum dot (a) MoS2Quantum dots under dark conditions, (b) MoS2Under the illumination condition of the quantum dots, and (c) carbazole functionalized MoS2Quantum dot under dark condition, (d) carbazole functionalized MoS2The quantum dots are under the illumination condition;
FIG. 9 is carbazole functionalized MoS2The photochemical hydrogen evolution mechanism diagram of the quantum dots.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Sodium molybdate (Na) in the present application2MoO4·2H2O), cysteine (C)3H7NO2S), ethanol (C)2H5OH), potassium ferrocyanide (K)3Fe(CN)6) Are all purchased from chemical reagents of Chinese national medicine, Inc.; carbazole (C)12H9N) from Aladdin; indium Tin Oxide (ITO) sheets (type JH52, ITO coating 30 + -5 nm, sheet resistance ≤ 10 Ω) were purchased from Shenzhen south China Hunan City science and technology, Inc. (China).
HR-TEM and EDS of the application are measured by a JEM-2100F instrument; the ultraviolet-visible diffuse reflectance spectrum was measured with a UV-2550 spectrophotometer, manufactured by Shimadzu corporation, Japan; fluorescence spectroscopic measurements were obtained at room temperature using a Hitachi F-4600 fluorescence spectrophotometer with excitation at 290 nm.
Example 1
S1: mixing 0.13gNa2MoO4·2H2O and 0.26g C3H7NO2S is dissolved in 40mL of deionized water;
s2: 0.0084g of carbazole was dissolved in 10ml of ethanol;
s3: the two solutions were mixed and stirred for 30min, and the resulting suspension was transferred to a stainless steel autoclave (100ml) and reacted at 180 ℃ for 36 h.
S4: naturally cooling to room temperature, centrifuging the supernatant at 10000r/min for 12min, and purifying with deionized water in a 500Da dialysis bag for 6h to obtain the carbazole-functionalized MoS2A quantum dot solution.
The product prepared in example 1 was tested and the results were as follows:
from the HRTEM image in FIG. 1, it is clear that the carbazole-functionalized MoS2The quantum dots are uniformly dispersed and have good appearance and obvious crystal lattice stripes.
FIG. 2 shows (a) carbazole functionalized MoS2Quantum dots and (b) MoS2Infrared spectroscopy of quantum dots. In the figure, (a) is at 3463cm-1The absorption peak is-OH stretching vibration peak of crystal water, 1696cm-1Is C ═ O stretching vibration peak at 1465cm-1And 839cm-1Is caused by the asymmetric stretching vibration of C-NH-C, 1210cm-1The peak of flexural vibration of C-N (3455 cm in FIG. (b))-1The absorption peak of (2) is also the-OH tensile vibration peak of crystal water, 1643cm-1The absorption peak appeared at (1) is the bending vibration peak of N-H in-NH 2, 1453cm-1And 839cm-1The absorption peak appeared at (A) is caused by the asymmetric stretching vibration of C-NH-C, 644cm-1Is MoS2The fingerprint characteristic peak of (1). The above characteristics show that the product prepared by the method is successfully compounded into MoS by carbazole2The above.
To MoS2Quantum dot and carbazole functionalized MoS2The fluorescence emission spectra of the quantum dots were measured, and the results are shown in fig. 3. Carbazole functionalized MoS2The fluorescence intensity of the quantum dots is obviously higher than that of MoS without carbazole2And (4) quantum dots. Further, from the UV-visible absorption spectrum, carbazole functionalized MoS2The wavelength of the quantum dots is red-shifted (FIG. 4), which shows that the addition of carbazole can improve MoS2The optical property of the quantum dot can be used as a photoelectrochemical material.
The present application also relates to carbazole functionalized MoS2The electrochemical properties of the quantum dots were examined and Electrochemical Impedance Spectroscopy (EIS) was performed on an electrochemical workstation (Autolab PGSTAT 302N) with a platinum wire electrode. Ag/AgCl electrode and ITO in the concentration of 5.0 mmol.L-1K3[Fe(CN)6]/K4[Fe(CN)6](1:1) 0.1 mol. L of mixture-1KCl solution is used as redox probe, and the recording frequency range is 1Hz-100kHz, and the amplitude is 50 mv. On an electrochemical workstation (CHI 660D), a platinum wire electrode, an Ag/AgCl electrode and GCE were used in a solution containing 5.0 mmol.L-1K3[Fe(CN)6]/K4[Fe(CN)6]Cyclic voltammetry was performed in a KCl solution (1: 1). Electrochemical impedance spectroscopy further proves photogenerationSeparation efficiency of the sub-hole pairs (FIG. 5), MoS2The arc radius on the EIS-Nyquist plot for quantum dots is significantly larger than that of ITO, due to MoS2The quantum dots hinder electron transfer, but when (c) carbazole-MoS2When the quantum dots are modified on the ITO, the arc radius on the EIS-Nyquist curve is obviously smaller than that of the ITO curve. The results show that carbazole-MoS2The electron-hole pair separation rate of the quantum dot composite material is higher than that of MoS2And (4) quantum dots. Prove carbazole and MoS2The incorporation of quantum dots was successful. From MoS2Quantum dot and carbazole functionalized MoS2MoS can be calculated by cyclic voltammogram of quantum dots (FIG. 6)2Quantum dot with Homo-Lumo gap of 0.61- (-0.27) ═ 0.88eV, carbazole functionalized MoS2The Homo-Lumo gap of the quantum dot is 0.44- (-0.05) ═ 0.49 eV. The lower the HOMO-LUMO value, i.e. the lower the Eg value, the easier the molecule is excited and the easier the electrons are transferred.
In a conventional three-electrode system using an ITO sheet as a working electrode, carbazole-functionalized MoS was studied2The transient photocurrent of quantum dot is measured by using Ag/AgCl electrode as reference electrode and platinum wire as counter electrode in electrochemical workstation (CHI 660D) under 500w xenon lamp irradiation in 0.5M NaSO4The properties of the PEC were examined. The results are shown in FIG. 7, where the carbazole functionalized MoS2The photocurrent density of the quantum dots is MoS22.58 times of quantum dots, which not only means carbazole loading is successful, but also means carbazole and MoS2Efficient coupling between quantum dots.
In a conventional three-electrode system using an ITO sheet as a working electrode, the photoelectrochemical performance of the ITO sheet is studied, and an Ag/AgCl electrode is used as a reference electrode and a platinum wire is used as a counter electrode on an electrochemical workstation (CHI 660D) under the irradiation of a 500W xenon lamp and 0.5M NaSO4The properties of the PEC were examined. The variation of the catalytic current with the potential was measured by the LSV method, and the oxygen in the solution was removed by injecting nitrogen before the test. 0.1mg of sample was coated on the ITO electrode, and the initial potential was-1.2V and the final potential was 0V at a scanning speed of 2.45mv/s under dark and light conditions. Initially, MoS2The current of the quantum dot is unstable, and 60 cyclic voltammetry are takenStable value of post-LSV. As can be seen from FIG. 8, carbazole functionalized MoS2The current density of the quantum dots reaches the maximum value of-2.82 mA/cm-1Jordan of MoS2168% of the quantum dot illumination current, illustrating the carbazole-functionalized based MoS prepared herein2The quantum dots remarkably improve the photoelectric hydrogen evolution effect, compared with MoS2The quantum dot can perform photoelectric hydrogen evolution more efficiently and stably.
Example 2
S1: 0.1g of Na2MoO4·2H2O and 0.25g C3H7NO2S is dissolved in 30mL of deionized water;
s2: 0.0077g of carbazole is dissolved in 8ml of ethanol;
s3: the two solutions were mixed and stirred for 30min, and the resulting suspension was transferred to a stainless steel autoclave (100ml) and reacted at 190 ℃ for 42 h.
S4: naturally cooling to room temperature, centrifuging the supernatant at 8000r/min for 10min, and purifying with deionized water in 500Da dialysis bag for 4h to obtain MoS based on carbazole functionalization2A quantum dot solution.
Example 3
S1: 0.1g of Na2MoO4·2H2O and 0.3g C3H7NO2S is dissolved in 50mL of deionized water;
s2: 0.0062g of carbazole is dissolved in 5ml of ethanol;
s3: the two solutions were mixed and stirred for 30min, and the resulting suspension was transferred to a stainless steel autoclave (100ml) and reacted at 200 ℃ for 48 h.
S4: naturally cooling to room temperature, centrifuging the supernatant at 12000r/min for 15min, and purifying with deionized water in a 500Da dialysis bag for 8h to obtain the carbazole-functionalized MoS2A quantum dot solution.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. MoS based on carbazole functionalization2The preparation method of the quantum dot is characterized by comprising the following steps:
s1: dissolving sodium molybdate and cysteine in deionized water to obtain a solution A;
s2: dissolving carbazole in ethanol to obtain a solution B;
s3: mixing and stirring the solution A in the S1 and the solution B in the S2, and transferring the mixed solution into a stainless steel autoclave for reaction;
s4: after the reaction product in S3 is naturally cooled to room temperature, taking the supernatant for centrifugation, and purifying the centrifugate to obtain the MoS based on carbazole functionalization2A quantum dot solution.
2. The carbazole-based functionalized MoS of claim 12The preparation method of the quantum dot is characterized in that the mass volume ratio of the sodium molybdate, the cysteine and the deionized water in the S1 is 1g:2-3g:300-500 mL.
3. The carbazole-based functionalized MoS of claim 12The preparation method of the quantum dot is characterized in that the mass volume ratio of carbazole to ethanol in S2 is 1g: 1.15-1.25L.
4. The carbazole-based functionalized MoS of claim 12The preparation method of the quantum dot is characterized in that the mass ratio of sodium molybdate to carbazole in S3 is 13-16g:1 g.
5. The carbazole-based functionalized MoS of claim 12The preparation method of the quantum dot is characterized in that the reaction conditions of S3 are as follows: the temperature is 180 ℃ and 200 ℃, and the time is 36-48 h.
6. The carbazole-based functionalized MoS of claim 12The preparation method of the quantum dot is characterized in that the centrifugation conditions in the S4 are as follows:the rotating speed is 8000-.
7. The carbazole-based functionalized MoS of claim 12The preparation method of the quantum dot is characterized in that the purification conditions in S4 are as follows: purified with deionized water in a 500Da dialysis bag for 4-8 h.
8. MoS based on carbazole functionalization prepared according to the method of any one of claims 1 to 72And (4) quantum dots.
9. The carbazole-based functionalized MoS of claim 82The quantum dot is applied to photoelectric hydrogen evolution.
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| CN105271411A (en) * | 2015-11-04 | 2016-01-27 | 太原理工大学 | Preparation method for molybdenum disulfide quantum dot |
| CN107459060A (en) * | 2017-08-25 | 2017-12-12 | 徐州医科大学 | A kind of molybdenum disulfide quantum dot from bottom to top step hydrothermal preparing process |
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