CN109273729B - Solution method for in-situ preparation of molybdenum disulfide/graphite paper electrode - Google Patents

Solution method for in-situ preparation of molybdenum disulfide/graphite paper electrode Download PDF

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CN109273729B
CN109273729B CN201811133144.9A CN201811133144A CN109273729B CN 109273729 B CN109273729 B CN 109273729B CN 201811133144 A CN201811133144 A CN 201811133144A CN 109273729 B CN109273729 B CN 109273729B
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molybdenum disulfide
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黄妞
李国旺
夏芝芬
孙小华
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China Three Gorges University CTGU
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    • H—ELECTRICITY
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    • H01M4/8842—Coating using a catalyst salt precursor in solution followed by evaporation and reduction of the precursor
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Abstract

The invention discloses a preparation method of a molybdenum disulfide/graphite paper electrode, which comprises the steps of dropwise adding an ethanol solution containing molybdenum chloride and thiourea into the surface of hydrophilized graphite paper, sintering at high temperature in an inert atmosphere after drying, and taking out the sintered graphite paper after cooling to obtain the molybdenum disulfide/graphite paper electrode. The reagent used in the invention is cheap and simple to prepare; in the prepared molybdenum disulfide/graphite paper electrode, molybdenum disulfide and graphite paper are tightly combined without falling off; SEM tests show that molybdenum disulfide uniformly covers the surface of graphite paper, and related electrochemical tests show that the molybdenum disulfide/graphite paper electrode has extremely high conductivity and good electrocatalytic activity.

Description

Solution method for in-situ preparation of molybdenum disulfide/graphite paper electrode
Technical Field
The invention relates to an in-situ electrode and a preparation method thereof, belonging to the field of novel conductive and electrocatalytic materials.
Background
Due to unique chemical properties, physical properties such as light, electricity and magnetism and good stability, the molybdenum disulfide is widely used for lubricants, optoelectronic materials, vulcanized glass, luminescent materials, industrial catalysts and the like, and can also be used as electrode materials of dye-sensitized solar cells, quantum dot solar cells, lithium ion cells, sodium ion cells, supercapacitors, fuel cells and the like.
In the field of electrocatalysis, catalytic materials need to be made into electrically conductive electrodes to be used. The preparation process of the molybdenum disulfide electrode is generally powder preparation → slurry preparation → electrode preparation. The method needs to prepare the molybdenum disulfide powder and slurry thereof, has complex process, and often has the problems of uneven dispersion of the molybdenum disulfide in the slurry and weak adhesion of the molybdenum disulfide and the substrate. Therefore, it is very significant to develop a method for preparing an in-situ electrode, i.e. to simultaneously realize the loading of the transition metal sulfide on the surface of the conductive substrate in the process of forming the transition metal sulfide, or to allow the transition metal sulfide to directly grow on the surface of the conductive substrate. Few in-situ molybdenum disulfide electrode types have been reported, for example: molybdenum disulfide/fluorine-doped tin dioxide electrode and molybdenum disulfide/molybdenum electrode. The graphite paper has excellent stability and conductivity, is suitable for being used as a conductive substrate or a current collector of an electrocatalytic electrode, and has the price of only one tenth of that of fluorine-doped tin dioxide (FTO) conductive glass. Therefore, the molybdenum disulfide/graphite paper is prepared in situ by a simpler method, and has good market prospect.
Disclosure of Invention
In view of the above, the invention aims to provide a novel method for preparing a molybdenum disulfide in-situ electrode, which has the advantages of low cost of required raw materials, easy control of reaction conditions, simple production process, good consistency of formed products, small environmental pollution and the like, and has great significance for batch production of electrodes.
Therefore, the invention provides a method for preparing a molybdenum disulfide/graphite paper electrode solution with high conductivity, high catalytic activity and low cost, which comprises the following steps:
a method for preparing a molybdenum disulfide/graphite paper electrode in situ comprises the following steps:
(1) dissolving molybdenum chloride and thiourea in ethanol to form a uniform solution;
(2) and spin-coating the solution on the surface of graphite paper, drying, and annealing in an inert atmosphere to obtain the molybdenum disulfide/graphite paper electrode.
More preferably, the surface of the graphite paper contains hydrophilic functional groups, and the hydrophilic functional groups comprise-OH, -COOH and-NH2、-SO3Any two or more hydrophilic functional groups.
The molar ratio of the molybdenum chloride to the thiourea is 1: 2 to 3.
The mass concentration of the ethanol is more than 90%.
In the annealing process, the annealing temperature is 500-1000 ℃, and the annealing time is 0.3-3 h.
Dissolving the molybdenum chloride and the thiourea in ethanol to form a uniform solution, adding polyvinyl chloride, and stirring at the constant temperature of 50-70 ℃ until a uniform colloidal solution is formed to obtain a precursor solution; loading the precursor solution with the temperature of 50-70 ℃ into an injector, carrying out electrostatic spinning and spinning, and collecting tows by using graphite paper to form the graphite paper containing fiber bundles; and drying the graphite paper containing the fiber bundles in an oven at the temperature of 80-90 ℃, and sintering for 0.3-3h in a tubular furnace at the temperature of 500-1000 ℃ under the condition of nitrogen to obtain the molybdenum disulfide/graphite paper electrode material.
The ethanol can be replaced by acetone, and the mass concentration of the acetone is more than 90%. The addition amount of the polyvinyl chloride is 20-60% of the total mass of the raw materials, and the molecular weight of the polyvinyl chloride is 20000-50000.
The preparation principle of the molybdenum disulfide/graphite paper electrode is as follows: 1. utilizes the graphite paper surface containing-OH, -COOH and-NH2、-SO3The isofunctional groups are easy to uniformly disperse on the surface of the ethanol solution of molybdenum chloride and thiourea; 2. the characteristic that ethanol and acetone can be dried quickly at a lower temperature is utilized, so that the aggregation of ethanol solutions of molybdenum chloride and thiourea dripped and coated on the graphite paper in the drying process is prevented from becoming uneven; 3. reacting sulfur atoms slowly released by thiourea at high temperature with molybdenum ions in molybdenum chloride to generate molybdenum disulfide; 4. the thiourea and the molybdenum chloride form a molten state at high temperature to promote the generated molybdenum disulfide to be in good contact with the graphite paper so as to form a firm and non-shedding electrode. During sintering, polyvinyl chloride is carbonized into a porous reticular carbon fiber matrix structure, so that the volume expansion between molybdenum disulfide and graphite in the circulation process can be effectively relieved, and the integrity of the electrode is maintained. Meanwhile, the molybdenum disulfide and the graphite surface are in good contact with the conductive carbon fiber, so that the conductivity of the composite material can be obviously enhanced.
Drawings
Figure 1 is a powder XRD of the sample prepared in example 2.
FIG. 2 is a powder SEM of a sample prepared in example 2.
Fig. 3 is a graph of CV cycles of the samples prepared in example 2.
FIG. 4 is a graph of EIS cycles for the samples prepared in example 2.
Detailed description of the preferred embodiment
Example 1:
dissolving molybdenum chloride and thiourea in ethanol under stirring, wherein the molybdenum chlorideAnd thiourea with the concentration of 0.33mol/L and 0.66mol/L respectively, and then the mixed solution is dripped and coated on the surface of the graphite paper which is hydrophilically treated (the surface of the graphite paper contains a large amount of-OH, -COOH and-NH)2) And annealing at 800 ℃ for 60min in Ar after drying. And taking out the sample after natural cooling to obtain the molybdenum disulfide/graphite paper electrode.
Example 2:
dissolving molybdenum chloride and thiourea in ethanol under stirring, wherein the concentrations of the molybdenum chloride and the thiourea are respectively 0.33mol/L and 0.99mol/L, and dropwisely coating the mixed solution on the surface of hydrophilically treated graphite paper (the surface of the graphite paper contains a large amount of-OH, -COOH and-NH)2) And annealing at 800 ℃ for 60min in Ar after drying. And taking out the sample after natural cooling to obtain the molybdenum disulfide/graphite paper electrode.
Fig. 1 illustrates powder XRD of the sample prepared in this example. By matching with standard PDF cards (MoS)2PDF #37-1492) comparison showed that the sample prepared was molybdenum disulfide. Indicating that molybdenum disulfide is generated by the reaction of molybdenum chloride and thiourea through annealing at 800 ℃ in Ar.
FIG. 2 is an SEM photograph of a sample prepared in the example. The brick shape is MoS in the figure2The bottom is graphite paper, MoS can be known from the figure2Uniformly and firmly growing on the surface of the graphite paper.
FIG. 3 is a graph showing CV (MoS in the figure) of a sample prepared in the example2Graph corresponding to a paper), it can be seen that the molybdenum disulfide/graphite paper electrode (MoS) prepared in the example of the present embodiment is obtained2The redox peak shape and peak position of the/graphite paper) are similar to those of a platinum electrode (Pt-pyrolysis), which shows that the oxidation-reduction peak shape and peak position are equivalent to the electrocatalytic capability of a Pt/FTO electrode. It can also be seen from the figure that pure graphite paper (graphite paper) has substantially no catalytic I3 -Reduction to I-The ability of the cell to perform. The electrolyte used was 0.1M LiClO4，10mM LiI，1mM I2Acetonitrile solution, three-electrode method as test method, saturated Ag/AgCl electrode as reference electrode, Pt sheet as counter electrode, in-situ nickel sulfide or nickel selenide electrode as working electrode, and scanning speed of 50mV s-1The scanning range is as follows: -0.4V to 1.2V.
FIG. 4 shows EIS of the sample prepared in this example. It can be seen from the figure that the internal series resistance (Rs, high-frequency intercept between half circle and Z' axis in EIS) of the molybdenum disulfide/graphite paper electrode prepared in the embodiment is far lower than that of the Pt/FTO electrode, which means that the molybdenum disulfide and FTO are tightly adhered, and that the capability of conducting electrons of graphite paper is stronger than that of FTO glass. Secondly, as can be seen from the figure, the charge transfer resistance (half circle radius in EIS) of the molybdenum disulfide electrode/electrolyte interface is only slightly higher than that of the Pt electrode, which indicates that the prepared molybdenum disulfide/graphite paper electrode has high intrinsic electrocatalytic activity.
Table 1 shows four parameters of the cell obtained by performing a photocurrent-voltage curve test after the dye-sensitized solar cell is assembled by using the molybdenum disulfide/graphite paper electrode, the pyrolytic Pt electrode and the pure graphite paper prepared in example 2 respectively and using the same photoanode and the same electrolyte. The effectiveness of the process described in this patent in preparing electrodes can be seen in the table. Table 1:
Figure BDA0001814074010000041
example 3:
dissolving molybdenum chloride and thiourea in ethanol under stirring, wherein the concentrations of the molybdenum chloride and the thiourea are respectively 0.33mol/L and 1.32mol/L, dropwisely coating the mixed solution on the surface of the graphite paper subjected to hydrophilization treatment, drying, and annealing in Ar at 800 ℃ for 60 min. And taking out the sample after natural cooling to obtain the molybdenum disulfide/graphite paper electrode.
Example 4:
dissolving molybdenum chloride and thiourea in ethanol under stirring, wherein the concentrations of the molybdenum chloride and the thiourea are respectively 0.33mol/L and 0.99mol/L, dropwisely coating the mixed solution on the surface of the graphite paper subjected to hydrophilization treatment, drying, and annealing for 45min at 500 ℃ in Ar. And taking out the sample after natural cooling to obtain the molybdenum disulfide/graphite paper electrode.
Example 5:
dissolving molybdenum chloride and thiourea in ethanol under stirring, wherein the concentrations of the molybdenum chloride and the thiourea are respectively 0.33mol/L and 0.99mol/L, dropwisely coating the mixed solution on the surface of the graphite paper subjected to hydrophilization treatment, drying, and annealing in Ar at 1000 ℃ for 30 min. And taking out the sample after natural cooling to obtain the molybdenum disulfide/graphite paper electrode.
In the sample prepared by the method, molybdenum disulfide is loaded on graphite paper, and the difference is that the crystallinity of the molybdenum disulfide becomes better along with the increase of annealing temperature; ② the crystal size of the molybdenum disulfide becomes finer with the increase of the amount of thiourea.
Example 5:
dissolving the molybdenum chloride (0.33mol/L) and the thiourea (0.99mol/L) in ethanol to form a uniform solution, adding polyvinyl chloride (0.8g, the molecular weight of the polyvinyl chloride is 30000), and stirring at the constant temperature of 50-70 ℃ until a uniform colloidal solution is formed to obtain a precursor solution; charging the precursor solution at 50-70 deg.C into injector, and performing electrostatic spinning (distance between graphite paper and injector needle is 12cm, working voltage is 12kV, solution advancing speed is 0.4mm min-1) Collecting tows by using graphite paper to form the graphite paper containing fiber bundles; and (3) drying the graphite paper containing the fiber bundles in an oven at 85 ℃, and sintering the graphite paper in a tube furnace at 700 ℃ for 30min under the condition of nitrogen to obtain the molybdenum disulfide/graphite paper electrode material.
Figure BDA0001814074010000051
Example 6:
dissolving the molybdenum chloride (0.33mol/L) and the thiourea (0.66mol/L) in ethanol to form a uniform solution, adding polyvinyl chloride (0.6g, the molecular weight of the polyvinyl chloride is 30000), and stirring at the constant temperature of 50-70 ℃ until a uniform colloidal solution is formed to obtain a precursor solution; charging the precursor solution at 50-70 deg.C into injector, and performing electrostatic spinning (distance between graphite paper and injector needle is 12cm, working voltage is 12kV, solution advancing speed is 0.4mm min-1) Collecting tows by using graphite paper to form the graphite paper containing fiber bundles; drying graphite paper containing fiber bundles in an oven at 85 ℃, and sintering for 30min in a tubular furnace at 850 ℃ under the condition of nitrogen to obtain disulfideMolybdenum/graphite paper electrode material.
Figure BDA0001814074010000061

Claims (8)

1. A method for preparing a molybdenum disulfide/graphite paper electrode in situ is characterized by comprising the following steps:
dissolving molybdenum chloride and thiourea in ethanol to form a uniform solution, adding polyvinyl chloride, and stirring at a constant temperature of 50-70 ℃ until a uniform colloidal solution is formed to obtain a precursor solution;
putting the precursor solution with the temperature of 50-70 ℃ into an injector, carrying out electrostatic spinning and spinning, and collecting tows by adopting graphite paper to form the graphite paper containing fiber bundles;
and drying the graphite paper containing the fiber bundles in an oven at the temperature of 80-90 ℃, and sintering for 0.3-3h in a tubular furnace at the temperature of 500-1000 ℃ under the condition of nitrogen to obtain the molybdenum disulfide/graphite paper electrode material.
2. The method of claim 1, wherein the graphite paper surface contains hydrophilic functional groups comprising-OH, -COOH, -NH2、-SO3Any two or more hydrophilic functional groups.
3. The method for preparing the molybdenum disulfide/graphite paper electrode in situ according to claim 1, wherein the molar ratio of the molybdenum chloride to the thiourea is 1: 2 to 3.
4. The method for in situ preparation of a molybdenum disulfide/graphite paper electrode as claimed in claim 1, wherein the mass concentration of ethanol is greater than 90%.
5. The method for in situ preparation of the molybdenum disulfide/graphite paper electrode as claimed in claim 1, wherein the ethanol is replaced by acetone, and the mass concentration of the acetone is more than 90%.
6. The method for in situ preparation of the molybdenum disulfide/graphite paper electrode as claimed in claim 1, wherein the amount of polyvinyl chloride added is 20-60% of the total mass of the raw materials.
7. The method for in situ preparation of molybdenum disulfide/graphite paper electrode as claimed in claim 1, wherein the molecular weight of polyvinyl chloride is 20000-50000.
8. The method for in-situ preparing the molybdenum disulfide/graphite paper electrode as claimed in claim 1, wherein in the electrostatic spinning process, the distance between the graphite paper and the needle of the injector is 12-15 cm, the working voltage is 9-15 kV, and the solution advancing speed is 0.4mm min-1。
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