CN114262914A - Laser-induced graphene-supported iron-doped cobalt disulfide catalyst and preparation method thereof - Google Patents
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Abstract
The invention discloses a laser-induced graphene-supported iron-doped cobalt disulfide catalyst and a preparation method thereof, and relates to the technical field of bifunctional electrolytic water catalysts, wherein the laser-induced graphene-supported iron-doped cobalt disulfide catalyst comprises a three-dimensional porous graphene substrate and Fe-doped cobalt disulfide nanoparticles loaded on the substrate; according to the invention, the LIG and the iron-doped cobalt disulfide are compounded, and the synergistic effect between the LIG and the iron-doped cobalt disulfide is utilized to improve the conductivity and further improve the stability of the catalyst; and the electronic structure is changed by doping iron, so that the catalytic efficiency is further improved.
Description
The technical field is as follows:
the invention relates to the technical field of bifunctional electrolytic water catalysts, and particularly relates to a laser-induced graphene supported iron-doped cobalt disulfide catalyst and a preparation method thereof.
Background art:
green energy is becoming more and more of a concern due to the energy crisis caused by the consumption of conventional fossil fuels and environmental pollution. Among them, hydrogen production by electrolysis of water is a technology for generating clean energy, which has received much attention. The electrolysis water reaction generates Oxygen Evolution Reaction (OER) at the anode and Hydrogen Evolution Reaction (HER) at the cathode for producing hydrogen and oxygen. However, the overpotential to be overcome during the hydrogen evolution and oxygen evolution reactions slows the reaction kinetics, thus severely hampering the efficiency of water electrolysis. To solve this problem, a high-performance catalyst has been developed to reduce the overpotential and improve the efficiency of water electrolysis.
Pt, Ir/C and RuO2The catalyst is the most advanced HER and OER performance catalyst which is recognized at present, and the noble metal catalyst can be effectively applied to both HER and OER reactions and is an effective bifunctional catalyst. However, the commercial use of the catalyst is seriously hindered due to the limited precious metal resources and high price. Therefore, the most important problem at present is to find a bifunctional catalyst with high performance, low cost and high durability.
Recently, a number of studies have shown that transition metals (Co, Fe, and Ni), etc., have excellent catalytic properties, and transition metal oxides, nitrides, and sulfides have received much research and attention. Among them, transition metal sulfides have received much attention due to their high activity and stability. Meanwhile, related researches show that the electronic structure of the transition metal sulfide can be adjusted by means of heteroatom doping and the like, so that OH in the catalytic process is influenced-And H+The adsorption energy of (b) to improve the catalytic performance. For example: king (10.1002/adfm.201701008) and the like improve CoS through Se doping2The intrinsic activity of (a) allows the catalyst to exhibit excellent HER and OER performance; sega (10.1021/acscano.7b05606) et al, by DFT calculation, revealed that7S4Co doping can accelerate electron transfer between Co and Cu sites, thereby reducing potential barrier in the OER process and improving intrinsic electrocatalytic activity. In addition, numerous studies have shown that Fe doping can be effective in improving transition metal catalyst performance. However, some transition metal catalysts are also presentProblems such as low conductivity and poor stability, etc., which can be solved by compounding carbon materials.
Currently, studies on the preparation of composite catalysts using a carbon material as a carrier are numerous, and among them, graphene is a carbon material that receives much attention. Graphene has a large specific surface area and excellent electrical conductivity, and thus can effectively affect catalyst activity. On the other hand, graphene has good stability and a fast electron transfer speed compared to other carbon materials, and thus is considered as an ideal carbon material support. At present, a Hummer method is mostly adopted for synthesizing graphene, but the method for synthesizing graphene by adopting laser induction is convenient and quick, and the cost is very low.
The graphene prepared by the current technical level has low crystal quality, the conductivity needs to be further improved, and the yield of the produced graphene is low, so that large-scale production cannot be realized. Meanwhile, the performance of the current bifunctional composite catalyst applied to HER and OER can not meet the commercial requirement, the catalyst needs to be further improved, the preparation method of the catalyst is as simple as possible, the raw material source is wide, and the catalyst can be used in a large scale.
According to the invention, the three-dimensional porous graphene is synthesized by laser induction and is used as a substrate material, then the iron-doped cobalt sulfide is loaded on the LIG by adopting a hydrothermal method, the prepared catalyst has excellent HER and OER performances, and the catalyst is respectively used as a cathode and an anode and applied to electrolytic water to show excellent electrolytic water performance.
The invention content is as follows:
the technical problem to be solved by the invention is to provide a laser-induced graphene-supported iron-doped cobalt disulfide catalyst and a preparation method thereof, wherein the prepared catalyst can be applied to hydrogen precipitation and oxygen precipitation and is applied to full water decomposition, so that the hydrogen production efficiency is improved and the like.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
the invention provides a laser-induced graphene supported iron-doped cobalt disulfide catalyst, which comprises a three-dimensional porous graphene substrate and Fe-doped cobalt disulfide nanoparticles supported on the substrate.
The substrate is three-dimensional porous graphene prepared on a polyimide film substrate by utilizing a laser induction technology.
The aperture of the three-dimensional porous graphene substrate is 0.5nm-10 mu m, and the conductivity is 0.01-10000S/m.
The Fe-doped cobalt disulfide nano particles are spherical particles, the surfaces of the particles are provided with a plurality of folds, and the particle size is 1-1000 nm.
The invention also provides a preparation method of the laser-induced graphene supported iron-doped cobalt disulfide catalyst, which comprises the following steps:
a. preparing a laser-induced three-dimensional porous graphene substrate:
washing a commercial PI membrane by using deionized water and absolute ethyl alcohol, then placing the membrane under laser, and obtaining a graphene-based substrate material through induction;
b. preparation of Fe-doped cobalt disulfide particles:
dissolving a cobalt source and a sulfur source in ultrapure water, adding an iron source, fully stirring, and placing in a reaction kettle for hydrothermal reaction to obtain Fe-CoS2；
c. Preparing a laser-induced graphene-supported iron-doped cobalt disulfide catalyst:
placing a laser-induced three-dimensional porous graphene film in a solution containing an iron source, a cobalt source and a sulfur source for hydrothermal reaction to obtain Fe-CoS2-LIG。
The light source of the laser is one or the combination of a plurality of solid-state laser, semiconductor laser, optical fiber laser and gas laser, the wavelength is 100nm-20 mu m, the power is 0.1W-100W, the pulse frequency is 1-1000KHz, and the laser scanning speed is 1-500 mm/s. Preferably, the laser is CO2The infrared laser has a wavelength of 10.6 μm, a power of 5W, a pulse frequency of 20kHz, and a laser scanning speed of 300 mm/s.
The cobalt source is at least one of cobalt nitrate, cobalt chloride and cobalt sulfate. Preferably, the cobalt source is cobalt nitrate.
The sulfur source is at least one of thiourea, thioacetamide and sodium thioacetate. Preferably, the sulfur source is thiourea.
The iron source is at least one of ferric chloride, ferric sulfate and ferric nitrate. Preferably, the iron source is ferric chloride.
The mass ratio of the cobalt source, the sulfur source and the iron source is (5-20): (10-40): 1. Preferably, the mass ratio of the cobalt source, the sulfur source and the iron source is 15:30: 1.
The hydrothermal reaction temperature is 120-200 ℃, and the hydrothermal reaction time is 10-24 h. Preferably, the hydrothermal reaction temperature is 150 ℃ and the hydrothermal reaction time is 24 h.
The area of the laser-induced three-dimensional porous graphene film is 0.01-100cm2The volume of the solution is 1-50 ml.
Characterization and optimization of the catalyst of the invention:
1. catalyst component characterization
The prepared catalyst is physically characterized, the composition, morphological characteristics, element composition and the like of the material are researched by XRD, SEM, XPS and the like, and then the morphology and dispersion are further observed by TEM.
2. Effect of different Synthesis conditions on catalyst Performance
The addition of different amounts of cobalt source and sulfur source during the synthesis will have different effects. By adding different amounts of samples, the area of the laser-induced three-dimensional porous graphene film is 1cm through performance optimization2The performance was optimal with the addition of 150mg of cobalt nitrate and 300mg of thiourea, indicating that excellent catalyst can be prepared with this amount; in addition, the ratio of cobalt nitrate and thiourea is changed, different sulfides are generated in different ratios, and the performance of the catalyst is further influenced, and performance tests conducted by changing different mass ratios can find that the catalyst has the optimal performance when the mass ratio is 1: 2. Finally, the performance of the catalyst was improved by adding varying amounts of the iron reagent, and optimization showed that the catalyst performed best when the amount of iron added was 10 mg.
HER and OER performance testing of the catalysts of the invention:
by testing the HER performance of the catalyst, Fe-CoS can be found2the/LIG has excellent HER performance compared with the pure LIG and CoS without iron doping2the/LIG is more advantageous; the double layer capacitance of the catalyst was then tested and the electrochemically active surface area of the catalyst was calculated. Fe-CoS2the/LIG has a larger active area and can expose more active sites.
Meanwhile, the Fe-CoS is found by the test2LIG has excellent OER performance compared with pure LIG and CoS without iron doping2the/LIG is more advantageous; then testing the double-layer capacitance of the catalyst, calculating the electrochemical active surface area of the catalyst, and obtaining the Fe-CoS2The double layer capacitance of LIG is larger, indicating Fe-CoS2the/LIG has a larger active area and can expose more active sites.
The full water splitting performance test of the catalyst of the invention comprises the following steps:
in order to analyze the water electrolysis capacity of the catalyst, the catalyst was used as a cathode and an anode, respectively, and tested in a 1MKOH solution, and it was found that only 1.59V was required to reach 10mA cm-2The current of (a) shows that the catalyst has good performance of electrolyzing water.
The invention has the beneficial effects that:
1. according to the invention, the LIG and the iron-doped cobalt disulfide are compounded, and the synergistic effect between the LIG and the iron-doped cobalt disulfide is utilized to improve the conductivity and further improve the stability of the catalyst.
2. The electronic structure is changed by doping iron, so that the catalytic efficiency is further improved.
3. The invention has simple operation and easily obtained raw materials, can be prepared in general chemical laboratories, is easy to popularize and is convenient to apply in various fields.
Description of the drawings:
FIG. 1 is (a) the LSV curve of OER for different amounts of cobalt nitrate; (b) the OER of different dosage of cobalt nitrate is 10mA cm-2A lower overpotential; (c) the LSV curves of HER for different amounts of cobalt nitrate; (d) HER at 10mA cm for different dosage of cobalt nitrate-2Passing throughAn electric potential;
FIG. 2 is (a) an LSV curve of HER at different cobalt to sulfur ratios; (b) HER at 10mA cm under different cobalt-sulfur ratios-2A lower overpotential; (c) LSV curves for OER at different cobalt-sulfur ratios; (d) OER at 10mA cm under different cobalt-sulfur ratios-2A lower overpotential;
FIG. 3 is (a) an LSV curve of HER at different amounts of Fe; (b) HER at 10mA cm under different Fe adding amount-2A lower overpotential; (c) the LSV curve of OER under different Fe addition; (d) the OER is 10mA cm under different Fe adding amounts-2A lower overpotential;
fig. 4 is a graph showing the full hydrolysis performance when the prepared catalyst was used as a cathode and an anode.
The specific implementation mode is as follows:
in order to make the technical means, the original characteristics, the achieved purposes and the effects of the invention easy to understand, the invention is further explained by combining the specific embodiments and the drawings.
Example 1
A preparation method of a laser-induced graphene-supported iron-doped cobalt disulfide catalyst comprises the following steps:
a. preparing a laser-induced three-dimensional porous graphene substrate:
washing commercial PI membrane with deionized water and absolute ethyl alcohol, and placing under laser, wherein the laser is CO2And infrared laser with the wavelength of 10.6 microns, the power of 5W, the pulse frequency of 20kHz and the laser scanning speed of 300mm/s is induced to obtain the graphene-based substrate material.
b. Preparation of Fe-doped cobalt disulfide particles:
dissolving cobalt nitrate and thiourea in ultrapure water, adding ferric chloride, wherein the mass ratio of the cobalt nitrate to the thiourea to the ferric chloride is 15:30:1, stirring for 30min, placing in a reaction kettle for hydrothermal reaction at the reaction temperature of 150 ℃ for 24h to obtain Fe-CoS2。
c. Preparing a laser-induced graphene-supported iron-doped cobalt disulfide catalyst:
the area is 1cm2The laser-induced three-dimensional porous graphene film is placed in 50ml of a solution containing an iron source, a cobalt source and a sulfur sourceHydrothermal reaction is carried out in the solution to obtain Fe-CoS2-LIG。
Changing the addition amount of the cobalt nitrate in the step b to 50mg, 100mg, 150mg and 200mg respectively to prepare the Fe-CoS2LIG catalyst and the HER and OER performance of the catalyst were tested and the results are shown in figure 1.
As can be seen from FIG. 1, an area of 1cm is used2When the mass of the added cobalt nitrate is 150mg, the performance of the catalyst is optimal, the over-potential of OER is 250mV, and the over-potential of HER is 230 mV. This is because when the amount of cobalt nitrate added is small, the generation of catalytically active sites is reduced, and thus sufficient catalytic activity cannot be provided; when the addition amount of the cobalt nitrate is too large, the graphene structure is damaged, and the catalytic efficiency is further influenced.
Example 2
A preparation method of a laser-induced graphene-supported iron-doped cobalt disulfide catalyst comprises the following steps:
a. preparing a laser-induced three-dimensional porous graphene substrate:
washing commercial PI membrane with deionized water and absolute ethyl alcohol, and placing under laser, wherein the laser is CO2And infrared laser with the wavelength of 10.6 microns, the power of 5W, the pulse frequency of 20kHz and the laser scanning speed of 300mm/s is induced to obtain the graphene-based substrate material.
b. Preparation of Fe-doped cobalt disulfide particles:
dissolving cobalt nitrate and thiourea in ultrapure water, adding ferric chloride, stirring for 30min, placing in a reaction kettle for hydrothermal reaction at 150 ℃ for 24h to obtain Fe-CoS2。
c. Preparing a laser-induced graphene-supported iron-doped cobalt disulfide catalyst:
the area is 1cm2The laser-induced three-dimensional porous graphene film is placed in 50ml of solution containing an iron source, a cobalt source and a sulfur source for hydrothermal reaction to obtain Fe-CoS2-LIG。
Changing the mass of the cobalt nitrate and the thiourea in the step bThe ratio is 2:1, 1:1, 1:2, 1:4 respectively, and Fe-CoS is prepared2LIG catalyst and the HER and OER performance of the catalyst were tested and the results are shown in figure 2.
As can be seen from FIG. 2, an area of 1cm is used2When the mass ratio of the cobalt nitrate to the thiourea is 1:2, the performance of the catalyst is optimal, the over-potential of the OER is 131mV, and the over-potential of the HER is 260 mV. This is because when the amount of the sulfur source added is small, insufficient vulcanization is caused and the number of generated vulcanization sites is small; when the sulfur source is too much, different sulfides are generated, and active site generation is affected, so that sufficient catalytic activity cannot be provided.
Example 3
A preparation method of a laser-induced graphene-supported iron-doped cobalt disulfide catalyst comprises the following steps:
a. preparing a laser-induced three-dimensional porous graphene substrate:
washing commercial PI membrane with deionized water and absolute ethyl alcohol, and placing under laser, wherein the laser is CO2And infrared laser with the wavelength of 10.6 microns, the power of 5W, the pulse frequency of 20kHz and the laser scanning speed of 300mm/s is induced to obtain the graphene-based substrate material.
b. Preparation of Fe-doped cobalt disulfide particles:
dissolving cobalt nitrate and thiourea in a mass ratio of 1:2 in ultrapure water, adding ferric chloride, stirring for 30min, placing in a reaction kettle for hydrothermal reaction at the reaction temperature of 150 ℃ for 24h to obtain Fe-CoS2。
c. Preparing a laser-induced graphene-supported iron-doped cobalt disulfide catalyst:
the area is 1cm2The laser-induced three-dimensional porous graphene film is placed in 50ml of solution containing an iron source, a cobalt source and a sulfur source for hydrothermal reaction to obtain Fe-CoS2-LIG。
Changing the adding amount of ferric chloride in the step b to be 1mg, 5mg, 10mg and 20mg respectively to prepare Fe-CoS2LIG catalyst and the HER and OER performance of the catalyst were tested and the results are shown in figure 3.
As can be seen from FIG. 3, an area of 1cm is used2When the mass of the added cobalt nitrate is 150mg, the mass of thiourea is 300mg and the addition amount of ferric chloride is 10mg, the performance of the catalyst is optimal, the over-potential of the OER is 86mV and the over-potential of the HER is 122 mV. This is because too little iron addition has less effect on catalyst performance; when the amount of iron added is too large, iron sulfide is generated.
Example 4
A preparation method of a laser-induced graphene-supported iron-doped cobalt disulfide catalyst comprises the following steps:
a. preparing a laser-induced three-dimensional porous graphene substrate:
washing commercial PI membrane with deionized water and absolute ethyl alcohol, and placing under laser, wherein the laser is CO2And infrared laser with the wavelength of 10.6 microns, the power of 5W, the pulse frequency of 20kHz and the laser scanning speed of 300mm/s is induced to obtain the graphene-based substrate material.
b. Preparation of Fe-doped cobalt disulfide particles:
dissolving 150mg of cobalt nitrate and 300mg of thiourea in ultrapure water, adding 10mg of ferric chloride, stirring for 30min, placing in a reaction kettle for hydrothermal reaction at the reaction temperature of 150 ℃ for 24h to obtain Fe-CoS2。
c. Preparing a laser-induced graphene-supported iron-doped cobalt disulfide catalyst:
the area is 1cm2The laser-induced three-dimensional porous graphene film is placed in 50ml of solution containing an iron source, a cobalt source and a sulfur source for hydrothermal reaction to obtain Fe-CoS2-LIG。
For the prepared Fe-CoS2The LIG catalyst was subjected to the full water splitting performance test, and the results are shown in FIG. 4.
The optimum conditions for preparing the catalyst were obtained on the basis of examples 1 to 3. The catalysts prepared under these conditions were used as an anode and a cathode, respectively, and tested in a 1M KOH solution, and it was found through the test that the prepared catalysts can reach 10mA cm in a full-hydrolysis application with only 1.59V of voltage-2The current density of the catalyst shows that the catalyst has excellent full-hydrolysis performance and can be applied to full-hydrolysis hydrogen production.
The preparation method firstly prepares the high-crystallinity high-conductivity three-dimensional porous graphene, then synthesizes Fe-doped cobalt disulfide particles by a solvothermal method, and loads the particles on LIG. The compounding of Fe-doped cobalt disulfide particles and LIG enables strong interaction between the particles, the interaction between the particles can improve the catalytic performance, and in addition, the doping of Fe enables OH-A large amount of the catalyst is enriched near the active center, so that the electron transfer distance can be shortened, and the catalytic efficiency is improved. On the other hand, the graphene synthesized by the laser induction method has high crystallinity and high conductivity, so that the graphene has high electronic conductivity after being compounded with the Fe-doped cobalt disulfide, and further the catalytic efficiency is improved. Meanwhile, the prepared catalyst is applied to HER and OER, and tests show that the catalyst has excellent HER and OER performances, small overpotential and excellent catalytic performance. Meanwhile, the catalyst is applied to the full-hydrolysis water, and has excellent full-hydrolysis performance. The composite catalyst prepared by the invention has excellent performance, simple operation and easily obtained raw materials, can meet different application requirements, and is particularly applied to the field of catalysis, thereby being convenient for popularization.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The laser-induced graphene-supported iron-doped cobalt disulfide catalyst is characterized in that: the graphene oxide nano-particle comprises a three-dimensional porous graphene substrate and Fe-doped cobalt disulfide nano-particles loaded on the substrate.
2. The laser-induced graphene supported iron-doped cobalt disulfide catalyst of claim 1, wherein: the substrate is three-dimensional porous graphene prepared on a polyimide film substrate by utilizing a laser induction technology.
3. The laser-induced graphene supported iron-doped cobalt disulfide catalyst of claim 1, wherein: the aperture of the three-dimensional porous graphene substrate is 0.5nm-10 mu m, and the conductivity is 0.01-10000S/m.
4. The laser-induced graphene supported iron-doped cobalt disulfide catalyst of claim 1, wherein: the Fe-doped cobalt disulfide nano particles are spherical particles, the surfaces of the particles are provided with a plurality of folds, and the particle size is 1-1000 nm.
5. The preparation method of the laser-induced graphene-supported iron-doped cobalt disulfide catalyst as claimed in any one of claims 1 to 4, characterized by comprising the following steps:
a. preparing a laser-induced three-dimensional porous graphene substrate:
washing a commercial PI membrane by using deionized water and absolute ethyl alcohol, then placing the membrane under laser, and obtaining a graphene-based substrate material through induction;
b. preparation of Fe-doped cobalt disulfide particles:
dissolving a cobalt source and a sulfur source in ultrapure water, adding an iron source, fully stirring, and placing in a reaction kettle for hydrothermal reaction to obtain Fe-CoS2；
c. Preparing a laser-induced graphene-supported iron-doped cobalt disulfide catalyst:
placing a laser-induced three-dimensional porous graphene film in a solution containing an iron source, a cobalt source and a sulfur source for hydrothermal reaction to obtain Fe-CoS2-LIG。
6. The preparation method of the laser-induced graphene supported iron-doped cobalt disulfide catalyst according to claim 5, wherein: the light source of the laser is one or the combination of a plurality of solid-state laser, semiconductor laser, optical fiber laser and gas laser, the wavelength is 100nm-20 mu m, the power is 0.1W-100W, the pulse frequency is 1-1000KHz, and the laser scanning speed is 1-500 mm/s.
7. The preparation method of the laser-induced graphene supported iron-doped cobalt disulfide catalyst according to claim 5, wherein: the cobalt source is at least one of cobalt nitrate, cobalt chloride and cobalt sulfate; the sulfur source is at least one of thiourea, thioacetamide and sodium thioacetate; the iron source is at least one of ferric chloride, ferric sulfate and ferric nitrate.
8. The preparation method of the laser-induced graphene supported iron-doped cobalt disulfide catalyst according to claim 5, wherein: the mass ratio of the cobalt source, the sulfur source and the iron source is (5-20): (10-40): 1. Preferably, the mass ratio of the cobalt source, the sulfur source and the iron source is 15:30: 1.
9. The preparation method of the laser-induced graphene supported iron-doped cobalt disulfide catalyst according to claim 5, wherein: the hydrothermal reaction temperature is 120-200 ℃, and the hydrothermal reaction time is 10-24 h. Preferably, the hydrothermal reaction temperature is 150 ℃ and the hydrothermal reaction time is 24 h.
10. The preparation method of the laser-induced graphene supported iron-doped cobalt disulfide catalyst according to claim 5, wherein: the area of the laser-induced three-dimensional porous graphene film is 0.01-100cm2The volume of the solution is 1-50 ml.
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