CN111286752A - Nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material and preparation method thereof - Google Patents
Nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material and a preparation method thereof. The method adopts a one-step hydrothermal method, and g-C prepared by an alternative vapor deposition method3N4The nano-sheets are subjected to hydrothermal reaction with urea, sodium molybdate dihydrate and thioacetamide to realize compounding and element doping. The invention has simple process and low cost, and when the prepared nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material is used as a catalyst, the current density is 10mA/cm2When the electrochemical hydrogen evolution catalyst is used, the overpotential is 187.2mV, the Tafel slope is 44mV/dec, and the electrochemical hydrogen evolution performance and the stability are excellent.
Description
Technical Field
The invention belongs to the technical field of electrocatalysis materials, and relates to a nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material and a preparation method thereof.
Background
Hydrogen has the highest mass energy density and renewability, and can be used as a clean renewable energy source to replace fossil fuels. Electrochemical Hydrogen Evolution Reaction (HER), 2H++2e-→H2It is one of the methods for efficiently and continuously producing hydrogen. The key to the production of hydrogen using electrochemical catalysis techniques is the production of efficient and inexpensive electrocatalysts. Platinum (Pt) has suitable Gibbs free energy of adsorption of hydrogen atoms and minimumIs an effective catalyst for hydrogen evolution reactions. However, the scarcity and high cost of Pt greatly limit its applications.
Molybdenum disulfide (MoS)2) The high activity and good stability to hydrogen production make it a potential candidate for replacing Pt. MoS2The hydrogen evolution catalyst has a layered structure similar to graphite, the interior of the sheets are bonded by strong covalent bonds, the sheets are interacted by weak van der Waals force, the resource is rich, the price is low, and the hydrogen evolution catalyst is widely applied to electrocatalytic hydrogen evolution reaction. However, there are two disadvantages that limit MoS2The practical application of (1): (1) MoS2The interaction of van der waals force between layers inevitably causes a stacking phenomenon, and active sites are reduced, thereby reducing the catalytic activity; (2) MoS2Due to electrons along the MoS2The lateral transfer of the nanosheet layered structure limits effective electron transfer and associated electrochemical kinetic performance. Thus MoS with more edge active sites and good conductivity2The base material is an effective method for improving the electrocatalytic hydrogen evolution efficiency.
The carbon material has good conductivity and MoS2Combined with carbon to form a composite material capable of improving MoS2The conductivity of the electrolyte improves the electrochemical performance of the electrolyte. MoS is prepared by the Solvothermal method of the professor Dacron2Loaded on reduced graphene oxide to obtain MoS2the/RGO material is composed of thin MoS2The nanolayers and a high graphite conductive network. The existence of the reduced graphene oxide in the composite electrocatalyst greatly improves the electron conduction rate in the electrocatalysis process, and effectively reduces MoS2The initial overpotential and tafel slope of the electrocatalyst and higher electrochemical stability is achieved. The reduced graphene oxide not only increases the conductivity of the material, but also acts as a MoS2The support of (3) so that it is distributed on the surface of the graphene in the form of highly dispersed nanosheets. The catalyst shows excellent electrochemical hydrogen evolution activity and can reach the current density of 10mA cm-2When the voltage is higher than the predetermined value, the overpotential is only 140mV, and the Tafel slope is 41mV/dec (Li Y G, Wang H L, Liang Y, et2nanoparticles grown on graphene:an advanced catalyst for the hydrogenevolution reaction[J].Journal of the American Chemical Society,2011,133(19):7296-7299.)。
Disclosure of Invention
The invention aims to provide a nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material for electrochemical hydrogen evolution and a preparation method thereof. The method adopts a one-step hydrothermal method to mix graphite phase carbon nitride (g-C)3N4) The nano-sheets are subjected to hydrothermal reaction with urea, sodium molybdate dihydrate and thioacetamide to realize compounding and element doping.
The technical solution for realizing the purpose of the invention is as follows:
the preparation method of the nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material comprises the following specific steps:
in the presence of sodium molybdate dihydrate (Na)2MoO4·2H2O) and thioacetamide (CH)3CSNH2) Adding g-C to the mixed solution3N4Uniformly stirring and mixing the nanosheets, adding urea, carrying out hydrothermal reaction at 180-220 ℃, cooling to room temperature after the reaction is finished, respectively centrifugally cleaning the suspension with ethanol and water, and drying to obtain the nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material.
Preferably, said g-C3N4The mass ratio of the nanosheets, urea, sodium molybdate dihydrate and thioacetamide is 0.05: 0.05: 1.70: 1.05.
preferably, the reaction time is 20-24 h.
Preferably, said g-C3N4The nanosheet is prepared by the following steps: roasting urea at 550 deg.C for 2 hr, and heating at 5 deg.C for min-1Collecting the vapor deposition to obtain g-C3N4Nanosheets.
The invention also provides the nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material prepared by the preparation method.
Further, the invention also provides application of the nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material in electrochemical hydrogen evolution.
Compared with the prior art, the invention has the following advantages:
(1) nitrogen-doped g-C of the invention3N4The nano-sheet/molybdenum disulfide composite material is characterized in that molybdenum disulfide nanoflowers are loaded on nitrogen-doped g-C3N4On the nano sheet, the nano flower is formed by stacking a large number of nano sheets and can be used as an electrochemical hydrogen evolution catalyst.
(2) In the composite material, g-C3N4The unique edge effect of the nanosheets can provide more active sites for the growth of the molybdenum disulfide nanosheets, and the active edges of the molybdenum disulfide nanosheets can be more fully exposed; nitrogen doped g-C3N4The conductivity of the nano sheets is beneficial to the transmission of electrons, so that the overall conductivity of the composite material is improved; when the composite material of the invention is used as a catalyst, the current density is 10mA/cm2When the electrochemical hydrogen evolution catalyst is used, the overpotential is 187.2mV, the Tafel slope is 44mV/dec, and the electrochemical hydrogen evolution performance is excellent.
Drawings
FIG. 1 shows g-C3N4Nanosheet, MoS2、MoS2/g-C3N4、N-MoS2、MoS2XRD pattern of/NCN;
FIG. 2 shows g-C3N4Nanosheet, MoS2、MoS2TEM image of/NCN;
FIG. 3 is g-C3N4Nanosheet, MoS2、MoS2/CN、N-MoS2、MoS2Linear sweep voltammetry curve graph of/NCN (the working electrode is a glassy carbon electrode, the loading of the catalyst is 0.285 mg/cm)2)；
FIG. 4 shows g-C3N4Nanosheet, MoS2、MoS2/CN、N-MoS2、MoS2Tafel polarization plot for/NCN;
FIG. 5 shows MoS2Stability plot of/NCN.
Detailed Description
The present invention will be described in more detail with reference to the following examples and the accompanying drawings.
g-C3N4Reference to preparation of nanosheets [ Shihai Cao, BinFan3N4nanosheets with carbon vacancies:General synthesis and improved activityfor simulated solar-light photocatalytic nitrogen fixation[J]Chemical engineering Journal,2018,353(1): 147-:
placing urea into a crucible, sleeving a large crucible and a small crucible in the large crucible, roasting at 550 ℃ for 2h in a muffle furnace, and raising the temperature for 5 ℃ for min-1Collecting the vapor deposited on the wall of the large crucible to obtain g-C3N4Nanosheets.
Example 1
Preparation of nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material
1.6937g of sodium molybdate dihydrate (Na)2MoO4·2H2O) and 1.0518g of thioacetamide (CH)3CSNH2) Dissolving in 50ml water, stirring to obtain uniform transparent solution, and adding 0.05g g-C3N4Stirring the nano-sheets for 10min, adding 0.05g of urea, stirring for 10min, placing the solution in a stainless steel reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle in an oven, keeping the temperature at 180 ℃ for 24h, cooling to room temperature after the reaction is finished to obtain a turbid liquid, respectively centrifugally cleaning the turbid liquid for 3 times by using ethanol and deionized water, drying and collecting to obtain the nitrogen-doped graphite phase carbon nitride nano-sheet/molybdenum disulfide composite material (MoS)2/NCN)。
Fig. 1 is an XRD chart of the nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite hydrogen evolution catalytic material, which shows that the materials all present a typical hexagonal crystal structure of molybdenum sulfide, and diffraction peaks at 14.2 °, 32.1 °, 42.9 ° and 56.0 ° respectively correspond to (002), (100), (105) and (110) crystal faces of molybdenum disulfide, and are correspondingly consistent with those of a standard card (JCPDS 37-1492). MoS2The diffraction peak of molybdenum disulfide (002) at a diffraction angle equal to 14.2 ° was found to be diminished by the NCN, indicating that there was no significant stacking of molybdenum disulfide and a reduced number of layers of the composite was synthesized. FIG. 2 shows g-C3N4、MoS2And MoS2TEM image of/NCN hydrogen evolution catalytic material,in the figure, g-C can be seen3N4The molybdenum disulfide is in a two-dimensional nanosheet structure, pure molybdenum disulfide is in a flower-shaped structure, and the molybdenum disulfide is formed by stacking layered molybdenum disulfide. In MoS2In the/NCN material, a part of single layer or few layers of molybdenum disulfide are grown in g-C3N4Of (2) is provided. FIG. 3 is a linear sweep voltammetry characteristic curve of the nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite hydrogen evolution catalytic material, FIG. 4 is a Tafel polarization curve of the nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite hydrogen evolution catalytic material, and it can be seen from FIGS. 3 and 4 that the current density of the composite hydrogen evolution catalytic material is 10mA/cm2The overpotential was 187.2mV, and the Tafel slope was 44 mV/dec. Compared with the commercialized Pt/C (32mV/dec), the difference is only 12mV/dec, and the result is obviously better than the result reported by a plurality of literatures and patents. Fig. 5 is a stability test chart of the nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite hydrogen evolution catalytic material, which shows that the material still has good HER stability after long-time circulation.
Electrocatalytic application:
the electrochemical hydrogen evolution performance of the nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material is tested by adopting a three-electrode system, a Pt sheet is taken as a counter electrode, an Ag/AgCl electrode is taken as a reference electrode, a working electrode is a glassy carbon electrode of which the surface is dropwise coated with the nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material, and an electrolyte is 0.5M H2SO4The solution and the testing instrument are electrochemical workstations of CHI660e model Shanghai, Chenghua, the linear volt-ampere scanning range is between-0.2V and-0.8V, the scanning speed is 10mV/s, and all the tests are carried out at constant temperature.
The working electrode is prepared by a dropping-coating method, and the specific process is as follows: and (3) taking out 80 mu L of Nafion solution, mixing and dissolving in 1ml of water-ethanol mixed solution (V water: V ethanol is 1:1), mixing 5mg of nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide catalyst with the former solution, and performing ultrasonic treatment for 1 hour to obtain a uniform mixed solution. 6. mu.L (catalyst content: 24. mu.g) of the black solution was pipetted directly onto the surface of a glassy carbon electrode (loading: 0.285 mg/cm)2) Finally, the modified electrode is naturally dried or heated in a far infrared box for standby。
Comparative example 1
g-C3N4Preparation of nanosheets
Placing urea into a crucible, sleeving a large crucible and a small crucible in the large crucible, roasting at 550 ℃ for 2h in a muffle furnace, and raising the temperature for 5 ℃ for min-1Collecting the vapor deposited on the wall of the large crucible to obtain g-C3N4Nanosheets.
Electrocatalytic application: the electrodes were prepared and tested as in example 1. The current density of the sample was 10mA/cm2The overpotential was 529.2mV, and the Tafel slope was 89 mV/dec. The electrocatalytic hydrogen evolution performance is obviously inferior to that of MoS2a/NCN material.
Comparative example 2
Pure MoS2Preparation of
1.6937g of sodium molybdate dihydrate (Na)2MoO4·2H2O) and 1.0518g of thioacetamide (CH)3CSNH2) Dissolving the solution in 50ml of water, stirring to form a uniform and transparent solution, placing the solution in a stainless steel reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle in an oven, keeping the temperature at 180 ℃ for 24 hours, cooling to room temperature after the reaction is finished to obtain a turbid liquid, respectively centrifugally cleaning the turbid liquid for 3 times by using ethanol and deionized water, drying and collecting to obtain the pure molybdenum disulfide material.
Electrocatalytic application: the electrodes were prepared and tested as in example 1. The current density of the sample was 10mA/cm2The overpotential was 425.2mV, and the Tafel slope was 74 mV/dec. The electrocatalytic hydrogen evolution performance is obviously inferior to that of MoS2a/NCN material.
Comparative example 3
Preparing a nitrogen-free molybdenum disulfide/graphite phase carbon nitride nanosheet composite material:
(1)g-C3N4preparation of nanosheets
Placing urea into a crucible, sleeving a large crucible and a small crucible in the large crucible, roasting at 550 ℃ for 2h in a muffle furnace, and raising the temperature for 5 ℃ for min-1Collecting the vapor deposited on the wall of the large crucible to obtain g-C3N4Nanosheets;
(2) preparation of graphite phase carbon nitride nanosheet/molybdenum disulfide composite material
1.6937g of sodium molybdate dihydrate (Na)2MoO4·2H2O) and 1.0518g of thioacetamide (CH)3CSNH2) Dissolving in 50ml water, stirring to obtain uniform transparent solution, and adding 0.05g g-C3N4Stirring the nanosheets for 10min, placing the solution in a stainless steel reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle in an oven, keeping the temperature at 180 ℃ for 24h, cooling to room temperature after the reaction is finished to obtain a suspension, respectively centrifugally cleaning the suspension for 3 times by using ethanol and deionized water, drying and collecting to obtain the molybdenum disulfide/graphite phase carbon nitride nanosheet composite material.
Electrocatalytic application: the electrodes were prepared and tested as in example 1. The current density of the sample was 10mA/cm2The overpotential was 357.2mV, and the Tafel slope was 74 mV/dec. The electrocatalytic hydrogen evolution performance is obviously inferior to that of MoS2a/NCN material.
Comparative example 4
Preparation of nitrogen-doped molybdenum disulfide
1.6937g of sodium molybdate dihydrate (Na)2MoO4·2H2O) and 1.0518g of thioacetamide (CH)3CSNH2) Dissolving the mixed solution in 50ml of water, stirring to form a uniform and transparent solution, continuously adding 0.05g of urea into the solution, stirring for 10min, placing the solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle into an oven, keeping the temperature of the reaction kettle at 180 ℃ for 24h, cooling to room temperature after the reaction is finished to obtain a suspension, respectively centrifugally cleaning the suspension for 3 times by using ethanol and deionized water, drying and collecting to obtain the nitrogen-doped molybdenum disulfide material.
Electrocatalytic application: the electrodes were prepared and tested as in example 1. The current density of the sample was 10mA/cm2The overpotential was 357.2mV, and the Tafel slope was 68 mV/dec. The electrocatalytic hydrogen evolution performance is obviously inferior to that of MoS2a/NCN material.
Claims (6)
1. The preparation method of the nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material is characterized by comprising the following specific steps of:
in two waterAdding g-C into the mixed solution of sodium molybdate and thioacetamide3N4Uniformly stirring and mixing the nanosheets, adding urea, carrying out hydrothermal reaction at 180-220 ℃, cooling to room temperature after the reaction is finished, respectively centrifugally cleaning the suspension with ethanol and water, and drying to obtain the nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material.
2. The method according to claim 1, wherein g-C is3N4The mass ratio of the nanosheets, urea, sodium molybdate dihydrate and thioacetamide is 0.05: 0.05: 1.70: 1.05.
3. the preparation method according to claim 1, wherein the reaction time is 20-24 hours.
4. The method according to claim 1, wherein g-C is3N4The nanosheet is prepared by the following steps: roasting urea at 550 deg.C for 2 hr, and heating at 5 deg.C for min-1Collecting the g-C obtained by vapor deposition3N4Nanosheets.
5. The nitrogen-doped graphite-phase carbon nitride nanosheet/molybdenum disulfide composite material prepared by the preparation method according to any one of claims 1 to 4.
6. The use of the nitrogen-doped graphite-phase carbon nitride nanosheet/molybdenum disulfide composite of claim 5 in electrochemical hydrogen evolution.
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| CN114005985A (en) * | 2021-10-18 | 2022-02-01 | 湖南理工学院 | Molybdenum disulfide composite nitrogen-doped carbon material and preparation method and application thereof |
| CN114768530A (en) * | 2022-04-29 | 2022-07-22 | 中国工程物理研究院材料研究所 | Application of molybdenum disulfide in hydrogen isotope electrolytic separation |
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| CN112647094B (en) * | 2020-12-21 | 2023-03-10 | 陕西科技大学 | Molybdenum disulfide modified sulfur and molybdenum codoped graphite phase carbon nitride heterostructure material for full-pH electrocatalytic hydrogen evolution and preparation method thereof |
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| CN114768530A (en) * | 2022-04-29 | 2022-07-22 | 中国工程物理研究院材料研究所 | Application of molybdenum disulfide in hydrogen isotope electrolytic separation |
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