CN111298833B - MoS based on carbazole functionalization 2 Quantum dot, preparation method and application - Google Patents

MoS based on carbazole functionalization 2 Quantum dot, preparation method and application Download PDF

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CN111298833B
CN111298833B CN202010146257.3A CN202010146257A CN111298833B CN 111298833 B CN111298833 B CN 111298833B CN 202010146257 A CN202010146257 A CN 202010146257A CN 111298833 B CN111298833 B CN 111298833B
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石建军
黄垚
庞卫国
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Anhui University of Science and Technology
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Abstract

The invention discloses a carbazole-based functionalized MoS 2 The preparation method and application of the quantum dot comprise the following steps: s1: dissolving sodium molybdate and cysteine in deionized water to obtain a solution A; s2: carbazole is dissolved in ethanol to obtain a solution B; s3: mixing and stirring the solution A in the step S1 and the solution B in the step S2, and transferring the mixed solution into a stainless steel autoclave for reaction; s4: after the reaction product in the S3 is naturally cooled to room temperature, taking supernatant, centrifuging, and purifying centrifugate to obtain the carbazole-based functionalized MoS 2 Quantum dot solution. The carbazole-based functionalized MoS prepared by the invention 2 The quantum dot has better transient photocurrent, takes the LSV stable value after 60 circles of CV, and the current density reaches the maximum value of-2.82 mA/cm ‑1 About occupied MoS 2 168% of illumination current of quantum dots, which illustrates carbazole-functionalization-based MoS prepared by the method 2 The quantum dot obviously improves the photoelectric hydrogen evolution effect compared with MoS 2 The quantum dot can more efficiently and stably perform photoelectric hydrogen evolution.

Description

MoS based on carbazole functionalization 2 Quantum dot, preparation method and application
Technical Field
The invention relates to the technical field of material synthesis, in particular to a carbazole functionalization-based MoS 2 Quantum dots, a preparation method and application.
Background
Energy and environmental challenges pose an increasing threat to the sustainable development of the 21 st century human beings, and researchers have been working on finding alternative low-cost, clean and sustainable energy sources to convert solar energy into solar fuels such as hydrogen, photoelectrochemical cells (PECs) have found widespread use in order to solve the energy crisis problem. In the photoelectric hydrogen evolution reaction, the catalyst is an important part, however, the development of the photoelectric hydrogen evolution industry is restricted due to the problems of low photoelectric conversion efficiency, low reaction activity and the like of the existing photoelectric hydrogen evolution catalyst.
MoS 2 The 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, but 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 existing in the background technology, the invention provides a carbazole-based functionalized MoS 2 The quantum dot, the preparation method and the application have better photoelectric hydrogen evolution effect.
The invention provides a carbazole functionalization-based MoS 2 The 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: carbazole is dissolved in ethanol to obtain a solution B;
s3: mixing and stirring the solution A in the step S1 and the solution B in the step S2, and transferring the mixed solution into a stainless steel autoclave for reaction;
s4: after the reaction product in the S3 is naturally cooled to room temperature, taking supernatant, centrifuging, and purifying centrifugate to obtain the carbazole-based functionalized MoS 2 Quantum dot solution.
Preferably, the mass volume ratio of the sodium molybdate, the cysteine and the deionized water in the S1 is 1g:2-3g:300-500mL.
Preferably, the mass volume ratio of carbazole to ethanol in the S2 is 1g:1.15-1.25L.
Preferably, the mass ratio of sodium molybdate to carbazole in S3 is 13-16g to 1g.
Preferably, the reaction conditions of S3 are: the temperature is 180-200 ℃ and the time is 36-48h.
Preferably, the centrifugation in S4 is performed under the following conditions: the rotating speed is 8000-12000r/min, and the time is 10-15min.
Preferably, the conditions for purification in S4 are: purification with deionized water was performed in a 500Da dialysis bag for 4-8 hours.
The carbazole-based functionalized MoS prepared by the method provided by the invention 2 Quantum dots.
The invention provides the MoS based on carbazole functionalization 2 The quantum dot is applied to photoelectric hydrogen evolution.
Mechanism of action:
carbazole can be in MoS 2 A deep trap level is formed between the valence band and the conduction band, and electrons are transferred 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 either recombine with holes remaining in the conduction band or transfer to the defect level of copper-manganese by radiation. Thus, efficient inter-particle charge transfer prevents electron-hole recombination. When carbazole and MoS 2 Quantum dots are compounded, photo-generated electrons are transferred between a conduction band and a valence band, and charge recombination is inhibited. Carbazole as MoS 2 The organic molecular donor is favorable for photoelectron transfer to the ITO surface, prolongs the service life of a photo-generated carrier, resists photocurrent corrosion and improves the photocurrent stability.
Compared with the prior art, the invention has the beneficial technical effects that:
(1) Carbazole functionalization-based MoS prepared by the method 2 The quantum dot has better transient photocurrent, takes the LSV stable value after 60 circles of CV, and the current density reaches the maximum value of-2.82 mA/cm -1 About occupied MoS 2 168% of illumination current of quantum dots, which illustrates carbazole-functionalization-based MoS prepared by the method 2 The quantum dot obviously improves the photoelectric hydrogen evolution effect compared with MoS 2 The quantum dot can more efficiently and stably perform photoelectric hydrogen evolution.
(2) The application is used for preparing MoS based on carbazole functionalization 2 When quantum dots are prepared, the two solutions are directly mixed and then reacted, compared with the prior MoS preparation method 2 The preparation method and the conditions are simple, other additives are not needed, and the prepared product has good dispersibility, so that the problems of secondary dispersion, difficult surface coating and the like are avoided.
Drawings
FIG. 1 shows (a) an HRTEM image, (b) a partial enlargement of the image (a), and (c) carbazole-functionalized MoS 2 EDS energy spectrum and element composition of the quantum dot;
FIG. 2 is (a) carbazole-functionalized MoS 2 Quantum dot (b) MoS 2 Quantum dot infrared map;
FIG. 3 is (a) 0.0084g carbazole in 10ml ethanol solution (b) MoS 2 Quantum dot and (c) carbazole functionalized MoS 2 Fluorescence emission spectrum of quantum dots;
FIG. 4 is (a) carbazole-functionalized MoS 2 Quantum dot, (b) MoS 2 Ultraviolet absorption spectrum of quantum dot;
FIG. 5 is (a) MoS 2 Quantum dot, (b) carbazole functionalized MoS 2 Cyclic voltammograms of quantum dots;
FIG. 6 is (a) MoS 2 Quantum dot, (b) carbazole functionalized MoS 2 Photoelectric properties of quantum dots;
FIG. 7 is MoS 2 Quantum dot and carbazole functionalized MoS 2 Photoelectric hydrogen-evolution spectrum of quantum dot (a) MoS 2 Under dark condition, (b) MoS 2 Under the illumination condition, the quantum dot (c) carbazole functionalized MoS 2 Under dark condition, the quantum dot (d) carbazole functionalized MoS 2 The quantum dots are under the illumination condition;
FIG. 8 is carbazole functionalized MoS 2 A photochemical hydrogen evolution mechanism diagram of quantum dots.
Detailed Description
The invention is further illustrated below in connection with specific embodiments.
Sodium molybdate (Na) 2 MoO 4 ·2H 2 O), cysteine (C) 3 H 7 NO 2 S), ethanol (C) 2 H 5 OH), potassium ferrocyanide (K) 3 Fe(CN) 6 ) All purchased from chinese national chemical reagent limited; carbazole (C) 12 H 9 N) purchased from aladine; indium Tin Oxide (ITO) sheets (type JH52, ITO coating 30+ -5 nm, sheet resistance 10 Ω or less) were purchased from Shenen Huanan Hunan City science and technology Co., ltd (China).
HR-TEM, EDS of the present application are measured by a JEM-2100F instrument; the UV-visible diffuse reflectance spectrum was measured by using a Japanese Shimadzu UV-2550 spectrophotometer; fluorescence spectroscopy was obtained at room temperature using a Hitachi F-4600 fluorescence spectrophotometer at 290nm excitation.
Example 1
S1: will be 0.13g Na 2 MoO 4 ·2H 2 O and 0.26gC 3 H 7 NO 2 S is dissolved in 40mL of deionized water;
s2: 0.0084g carbazole was dissolved in 10ml ethanol;
s3: the two solutions were mixed and stirred for 30min, and the resulting suspension was transferred to a stainless steel autoclave (100 ml) and reacted at 180℃for 36h.
S4: naturally cooling to room temperature, centrifuging the supernatant at 10000r/min for 12min, and purifying with deionized water in 500Da dialysis bag for 6 hr to obtain carbazole-based functionalized MoS 2 Quantum dot solution.
The product prepared in example 1 was tested and the results were as follows:
from the HRTEM image in fig. 1, carbazole functionalized MoS 2 The quantum dots are uniformly dispersed, and the good appearance and the obvious lattice stripes are obtained.
FIG. 2 shows (a) carbazole-functionalized MoS 2 Quantum dots and (b) MoS 2 Infrared spectra of quantum dots. In the figure, (a) at 3463cm -1 The absorption peak at the position is the-OH stretching vibration peak of crystal water, 1696cm -1 At C=O stretching vibration peak, 1465cm -1 And 839cm -1 Is caused by asymmetric stretching vibration of C-NH-C, 1210cm -1 The bending vibration peak of C-N, 3455cm in the graph (b) -1 The absorption peak of (C) is also the-OH stretching vibration peak of crystal water, 1643cm -1 The absorption peak appearing at this point is the bending vibration peak of N-H in-NH 2, 1453cm -1 And 839cm -1 The absorption peak at which occurs is caused by asymmetric stretching vibration of C-NH-C, 644cm -1 Is MoS 2 Is a fingerprint characteristic peak of (2). The above characterization shows that the product prepared by the application is successfully compounded to MoS by carbazole 2 And (3) upper part.
For MoS 2 MoS functionalized by quantum dots and carbazole 2 The measurement of the fluorescence emission spectrum of the quantum dot is shown in fig. 3. Carbazole functionalized MoS 2 The fluorescence intensity of the quantum dot is obviously higher than MoS without carbazole 2 Quantum dots. Furthermore, from the UV-visible absorption spectrum, carbazole functionalized MoS is known 2 The wavelength red shift of the quantum dots (FIG. 4) illustrates that the addition of carbazole can increase MoS 2 The optical property of the quantum dot can be used as photoelectrochemical material.
The application also relates to a carbazole functionalized MoS 2 The electrochemical properties of the quantum dots were examined on an electrochemical workstation (CHI 660D) using platinum wire electrode, ag/AgCl electrode and GCE at a concentration of 5.0 mmol.L -1 K 3 [Fe(CN) 6 ]/K 4 [Fe(CN) 6 ]Cyclic voltammetry experiments were performed in KCl solution (1:1). From MoS 2 MoS functionalized by quantum dots and carbazole 2 The cyclic voltammogram of the quantum dots (FIG. 5) can calculate MoS 2 Homo-Lumo gap of quantum dot=0.61- (-0.27) =0.88 eV, carbazole functionalized MoS 2 The 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 more easily the molecule is excited and the more easily the electrons are transferred.
In a conventional three-electrode system using an ITO sheet as a working electrode, carbazole-functionalized MoS was studied 2 Transient photocurrent of quantum dot, on electrochemical workstation (CHI 660D), with Ag/AgCl electrode as reference electrode, platinum wire as counter electrode, under 500w xenon lamp irradiation, under 0.5M NaSO 4 PEC properties were examined. The test results are shown in FIG. 6, where carbazole functionalized MoS 2 The photocurrent density of the quantum dots is MoS 2 2.58 times of quantum dot, which means not only successful carbazole loading, but also carbazole and MoS 2 Efficient coupling between quantum dots.
In a conventional three-electrode system using an ITO sheet as a working electrode, photoelectrochemical properties were studied, on an electrochemical workstation (CHI 660D), using an Ag/AgCl electrode as a reference electrode, a platinum wire as a counter electrode, and under 500w xenon lamp irradiation, at 0.5M NaSO 4 PEC properties were examined. The change of catalytic current with potential was measured by LSV method, in solutionOxygen was vented by nitrogen injection prior to the test. A sample of 0.1mg was applied to the ITO electrode, and the initial potential was-1.2V and the final potential was 0V under dark and light conditions at a scan rate of 2.45 mv/s. Initially, moS 2 The current of the quantum dot is unstable, and the stable value of LSV after 60 times of cyclic voltammetry is taken. As can be seen from FIG. 7, carbazole-functionalized MoS 2 The current density of the quantum dot reaches the maximum value of-2.82 mA/cm -1 About occupied MoS 2 168% of illumination current of quantum dots, which illustrates carbazole-functionalization-based MoS prepared by the method 2 The quantum dot obviously improves the photoelectric hydrogen evolution effect compared with MoS 2 The quantum dot can more efficiently and stably perform photoelectric hydrogen evolution.
Example 2
S1: will be 0.1g Na 2 MoO 4 ·2H 2 O and 0.25gC 3 H 7 NO 2 S is dissolved in 30mL of deionized water;
s2: 0.0077g carbazole was dissolved in 8ml ethanol;
s3: the two solutions were mixed and stirred for 30min, and the resulting suspension was transferred to a stainless steel autoclave (100 ml) and reacted at 190℃for 42h.
S4: naturally cooling to room temperature, centrifuging the supernatant at 8000r/min for 10min, and purifying with deionized water in 500Da dialysis bag for 4 hr to obtain carbazole-based functionalized MoS 2 Quantum dot solution.
Example 3
S1: will be 0.1g Na 2 MoO 4 ·2H 2 O and 0.3gC 3 H 7 NO 2 S is dissolved in 50mL of deionized water;
s2: 0.0062g carbazole was dissolved in 5ml ethanol;
s3: the two solutions were mixed and stirred for 30min, and the resulting suspension was transferred to a stainless steel autoclave (100 ml) and reacted at 200℃for 48h.
S4: naturally cooling to room temperature, centrifuging supernatant at 12000r/min for 15min, and purifying with deionized water in 500Da dialysis bag for 8 hr to obtain carbazole-based functionalized MoS 2 Quantum dot solution.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims (5)

1. MoS based on carbazole functionalization 2 The application of the quantum dot in photoelectric hydrogen evolution is characterized in that the carbazole functionalization-based MoS 2 The preparation method of the quantum dots comprises the following steps:
s1: dissolving sodium molybdate and cysteine in deionized water to obtain a solution A;
s2: carbazole is dissolved in ethanol to obtain a solution B;
s3: mixing and stirring the solution A in the step S1 and the solution B in the step S2, and transferring the mixed solution into a stainless steel autoclave for reaction;
s4: after the reaction product in the S3 is naturally cooled to room temperature, taking supernatant, centrifuging, and purifying centrifugate to obtain the carbazole-based functionalized MoS 2 A quantum dot solution;
in the S3, the mass ratio of the sodium molybdate to the carbazole is 13-16g to 1g;
the reaction conditions of the S3 are as follows: the temperature is 180-200 ℃ and the time is 36-48h.
2. The carbazole-based functionalized MoS of claim 1 2 The application of the quantum dot in photoelectric hydrogen evolution is characterized in that the mass volume ratio of sodium molybdate, cysteine and deionized water in S1 is 1g:2-3g:300-500mL.
3. The carbazole-based functionalized MoS of claim 1 2 The application of the quantum dot in photoelectric hydrogen evolution 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 1 2 Application of quantum dot in photoelectric hydrogen evolutionThe method is characterized in that the centrifugation conditions in the step S4 are as follows: the rotating speed is 8000-12000r/min, and the time is 10-15min.
5. The carbazole-based functionalized MoS of claim 1 2 The application of the quantum dot in photoelectric hydrogen evolution is characterized in that the purification conditions in the S4 are as follows: purification with deionized water was performed in a 500Da dialysis bag for 4-8 hours.
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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
CN108404938A (en) * 2018-04-05 2018-08-17 哈尔滨工业大学 A kind of electrocatalytic hydrogen evolution MoS2Nano flower sphere catalyst and preparation method thereof
CN110079317A (en) * 2019-04-17 2019-08-02 安徽理工大学 The synthetic method and application of molybdenum disulfide fluorescence quantum

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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
CN108404938A (en) * 2018-04-05 2018-08-17 哈尔滨工业大学 A kind of electrocatalytic hydrogen evolution MoS2Nano flower sphere catalyst and preparation method thereof
CN110079317A (en) * 2019-04-17 2019-08-02 安徽理工大学 The synthetic method and application of molybdenum disulfide fluorescence quantum

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