CN114108028B - Efficient water oxidation FeNiS 2 rGO electrocatalyst, method for its preparation and use - Google Patents
Efficient water oxidation FeNiS 2 rGO electrocatalyst, method for its preparation and use Download PDFInfo
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- CN114108028B CN114108028B CN202111514762.XA CN202111514762A CN114108028B CN 114108028 B CN114108028 B CN 114108028B CN 202111514762 A CN202111514762 A CN 202111514762A CN 114108028 B CN114108028 B CN 114108028B
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention relates to a high-efficiency water oxidation FeNiS 2 An rGO electrocatalyst, a preparation method and application thereof, belonging to the technical field of water electrolysis catalysts. The electrocatalyst is nano particle and thin layer nano composite material, and the composite material is FeNiS 2 Nanoparticle and reduced graphene oxide (rGO) thin-layer nanosheets are compounded to form FeNiS 2 The nano particles are uniformly attached to the surface of the rGO thin-layer nano sheet. FeNiS 2 The composition is Fe x Ni 1‑x S 2 (x＝0.02～0.5)，FeNiS 2 The size of the nano particles is 20-100 nm; the rGO thin-layer nano-sheet has a size of 1-2 mu m. According to the invention, graphene is introduced into the bimetallic transition metal sulfide nano-particles as a carrier, so that the dispersibility of the transition metal sulfide can be enhanced, the agglomeration of the nano-particles is inhibited, the stable particles are improved, the graphene can be used as a cocatalyst, the activity of the catalyst is improved through synergistic effect, the electron transfer rate is increased, and the overpotential is reduced. Has the advantages of good oxygen evolution performance, low overpotential, high stability and the like.
Description
Technical Field
The invention relates to a high-efficiency water oxidation FeNiS 2 An rGO electrocatalyst and a preparation method thereof, which belong to the technical field of water electrolysis catalysts.
Background
Energy is an important material basis for economic growth and social evolution. With the growth of world population and the acceleration of industrialization process, major concerns about energy crisis and environmental problems caused by excessive consumption of fossil fuel have prompted exploration of renewable and clean energy sources, such as wind energy, solar energy, hydrogen energy, and the like. The electrochemical water splitting is a novel renewable clean hydrogen energy regeneration method. In a standard state, the theoretical decomposition voltage of water is 1.23 (Δg=237.2 kJ/mol), however, in practical situations, the electrode potential deviates from the equilibrium potential due to the existence of electrochemical polarization, concentration polarization and the like, and an overpotential is generated, so that the actual decomposition voltage of water is far greater than 1.23V, and therefore, an efficient electrocatalyst is needed to reduce the overpotential of the water decomposition reaction, improve the energy conversion efficiency, reduce the consumption of electric energy and reduce the cost.
There are two key electrochemical processes in the water electrolysis process, namely oxygen evolution and hydrogen evolution. In contrast to hydrogen evolution, which is a four electron transfer process, there are multiple intermediate states, resulting in slow kinetics and a large overpotential. The oxygen evolution reaction mainly determines the overall water separation efficiency of the electrolyzer. Noble metal-based electrocatalysts are currently considered to be better oxygen evolution reaction electrocatalysts in alkaline electrocatalysts, but they have limited reserves and high cost, so that the commercial application development of the noble metal-based electrocatalysts is limited. Therefore, development of a low-cost and efficient non-noble metal electrocatalyst is imperative.
Transition metals (e.g., iron, molybdenum, nickel, tungsten, etc.) can provide unpaired d-orbital electrons and thus can open an O-H bond. Transition metal sulfides have a catalytic mechanism similar to hydrogenase and a high catalytic activity for oxygen evolution reactions, so that more and more people are beginning to study non-noble metal transition metal sulfide electrocatalysts. However, simple transition metal sulfides agglomerate easily, thus giving them a slow kinetic process and a high overpotential.
Disclosure of Invention
The invention aims to provide FeNiS for electrocatalytic oxygen evolution reaction, which has low raw material price, high catalytic activity, low overpotential and good chemical stability, aiming at the problems of the existing transition metal sulfide electrocatalyst 2 An rGO electrocatalyst.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
efficient water oxidation FeNiS 2 rGO electrocatalyst, feNiS 2 The rGO electrocatalytic material is a composite material of nano particles and thin nano sheets, and the composite material is prepared from FeNiS 2 Nanoparticle and reduced graphene oxide (rGO) thin-layer nanosheets are compounded to form FeNiS 2 The nano particles are uniformly attached to the surface of the rGO thin-layer nano sheet. The FeNiS 2 FeNiS in rGO material 2 The composition is Fe x Ni 1-x S 2 (x＝0.02～0.5)，FeNiS 2 The size of the nano particles is 20-100 nm; the rGO thin-layer nano-sheet has a size of 1-2 mu m.
Preferably, the water oxidizes FeNiS 2 In the rGO electrocatalytic material, the percentage of rGO is 5-50%.
The invention also provides the high-efficiency water oxidation FeNiS 2 The preparation method of the rGO electrocatalytic material comprises the following steps:
(1) 0.6g of lysine was weighed out, 75mL of NiCl was weighed out at 0.05mol/L 2 Continuously heating and stirring the solution in a water bath at 40 ℃ until the solution is dissolved, dropwise adding ammonia water until the pH value of the solution is 9.0, stirring for 0.5 hours, putting the obtained solution into a 100mL reaction kettle, preserving the temperature of the reaction kettle at 140-200 ℃ for 4-8 hours, naturally cooling to obtain a sample, centrifuging, washing and drying;
(2) Heating the dried sample in the step (1) to 300-500 ℃ according to the heating rate of 2 ℃/min in air atmosphere, and roasting for 2-5 hours;
(3) Weighing 0.002-0.041 g FeCl 3 Adding 0.03-0.05 g of thiourea and 0.01-0.05 g of Graphene Oxide (GO) into 60mL of deionized water, carrying out ultrasonic treatment for 20 minutes, stirring in a water bath at 40 ℃ for 0.5 hour, putting the obtained mixed solution into a 100mL reaction kettle, and carrying out heat preservation on the reaction kettle at the temperature of 140-180 ℃ for 8-16 hours; naturally cooling to obtain a sample, centrifuging, washing and drying;
(4) Weighing 0.2-0.5 g of sublimed sulfur and 0.05-0.1 g of the sample obtained by drying in the step (3), mixing and grinding the sublimed sulfur and the sample for 0.5 hour, roasting the mixture for 2-6 hours at 300-500 ℃ under the protection of inert gas, naturally cooling the mixture,namely FeNiS 2 an/rGO electrocatalytic material.
Preferably, in step (1) the incubation is carried out for 6 hours at a temperature of 180 ℃.
Preferably, in step (2) the calcination is carried out at a temperature of 350℃for 3 hours.
Preferably, feCl in step (3) 3 0.027g, 0.0457g thiourea and 0.03g GO.
Preferably, in step (3) the incubation is carried out for 12 hours at a temperature of 180 ℃.
Preferably, in step (4), the calcination is carried out at a temperature of 450℃for 4 hours.
FeNiS 2 The preparation method of the/rGO electrocatalytic electrode comprises the following steps: 10mg of FeNiS prepared in the step (4) is reacted with 2 Dispersing 50 mu L of naftifine solution in 1mL of ethanol solution, carrying out ultrasonic treatment for 25 minutes to obtain a uniform dispersion solution, uniformly coating 100 mu L of the dispersion solution on the treated foam nickel by using a micropipette, placing the foam nickel in a blast drying oven, and heating at 60 ℃ for 1 hour to obtain FeNiS 2 an/rGO electrocatalytic electrode.
Compared with the prior art, the invention has the main advantages that:
1, the raw materials used in the invention are cheap and easy to obtain, the process is relatively simple, and the manufacturing cost and the production period of the electrocatalyst are greatly reduced.
2, the composite electrocatalyst obtained by the invention has the advantages of good oxygen evolution performance, low overpotential, high stability and the like.
3. According to the invention, graphene is introduced into the bimetallic transition metal sulfide nano-particles as a carrier, so that the dispersibility of the transition metal sulfide can be enhanced, the agglomeration of the nano-particles is inhibited, the stable particles are improved, the graphene can be used as a cocatalyst, the activity of the catalyst is improved through synergistic effect, the electron transfer rate is increased, and the overpotential is reduced.
Drawings
FIG. 1 is an XRD pattern of the catalyst obtained in example 1
FIG. 2 is an SEM image of the catalyst obtained in example 1
FIG. 3a shows the catalytic performance of the catalyst obtained in example 1 for oxygen evolution in a three-electrode system: linear sweep voltammogram
FIG. 3b shows the catalytic performance of the catalyst obtained in example 1 for oxygen evolution in a three-electrode system: i-t curve obtained by constant potential step method
FIG. 4 is an electrochemical impedance spectrum of the catalyst obtained in example 1
FIG. 5a shows the catalytic performance of the catalyst obtained in example 1 for oxygen evolution in a two-electrode system: linear sweep voltammogram
FIG. 5b shows the catalytic performance of the catalyst obtained in example 1 for oxygen evolution in a two-electrode system: i-t curve obtained by constant potential step method
Detailed Description
The technical scheme of the invention is further explained and illustrated in the following form of specific examples.
Example 1:
in this example, feNiS is oxidized with water 2 The preparation method of the rGO electrocatalyst comprises the following steps:
(1) 0.6g of lysine was weighed out, 75mL of NiCl was weighed out at 0.05mol/L 2 Continuously heating and stirring the solution in a water bath at 40 ℃ until the solution is dissolved, dropwise adding ammonia water until the pH value of the solution is 9.0, stirring for 0.5 hours, putting the obtained solution into a 100mL reaction kettle, putting the reaction kettle into a baking oven, preserving heat for 6 hours at 180 ℃, naturally cooling to obtain a sample, centrifuging, washing and drying;
(2) Placing the dried sample in the step (1) into a muffle furnace, heating to 350 ℃ according to the heating rate of 2 ℃/min, and roasting for 3 hours;
(3) Weigh 0.027g FeCl 3 Adding 0.0457g of thiourea and 0.03g of Graphene Oxide (GO) into 60mL of deionized water, carrying out ultrasonic treatment for 20 minutes, stirring in a water bath at 40 ℃ for 0.5 hour, transferring the obtained mixed solution into a 100mL reaction kettle, placing the reaction kettle into an oven, carrying out heat preservation at 180 ℃ for 12 hours, naturally cooling, centrifuging the obtained sample, washing, and drying;
(4) Weighing 0.275g of sublimed sulfur and 0.055g of the sample obtained by drying in the step (3), mixing and grinding the two for 0.5 hour, and placing the mixture into a tube furnace under the protection of nitrogen inert gas at 450 DEG CRoasting for 4 hours, naturally cooling to obtain (Fe) 0.33 Ni 0.67 S 2 ) /rGO-20% electrocatalytic material.
FIG. 1 shows the XRD pattern of the sample obtained in example 1, and when the doping molar ratio of Fe is 33%, pure phase NiS can be obtained 2 And is in accordance with standard NiS 2 The standard spectrogram (JCPDS No. 65-3325) corresponds to the sample, and the sample is marked as (Fe) 0.33 Ni 0.67 S 2 )/rGO-20％。
FIG. 2 is an SEM image of a sample obtained in example 1, and it can be seen from the image that the composite material is composed of 50 nm-sized nanoparticles and rGO thin-layer nanoplatelets, and Fe with uniform particle size 0.33 Ni 0.67 S 2 Uniformly dispersed on the surface of the rGO thin-layer nano sheet, which provides guarantee for rapid electron transmission and high stability.
In example 1 (Fe 0.33 Ni 0.67 S 2 ) The preparation method of the/rGO-20% electrocatalytic electrode comprises the following steps:
10mg of the product (Fe) obtained in the above step (4) 0.33 Ni 0.67 S 2 ) Dispersing 50 μl of Nafie solution in 1mL of ethanol solution, performing ultrasonic treatment for 25 min to obtain uniform dispersion solution, uniformly coating 100 μl of dispersion solution on treated foam Ni with a pipette, placing in a forced air drying oven, and heating at 60deg.C for 1 hr to obtain (Fe) 0.33 Ni 0.67 S 2 ) /rGO-20% electrocatalytic electrode.
FIGS. 3a and 3b show the catalytic performance of the catalyst obtained in example 1 in oxygen evolution in a three-electrode system in which Hg/HgO is a reference electrode, a graphite carbon rod is a counter electrode, the catalyst electrode in example 1 is a working electrode, and the electrolyte solution is a KOH solution of 1 mol/L. FIG. 3a is a linear sweep voltammogram compared to foam Ni and RuO 2 ,(Fe 0.33 Ni 0.67 S 2 ) the/rGO-20% electrocatalyst showed better electrocatalytic activity when the current density was 10mA cm -1 ,(Fe 0.33 Ni 0.67 S 2 ) The overpotential of the/rGO-20% electrocatalyst is 142mV, which is significantly lower than that of foam Ni (422 mV) and RuO 2 (348 mV). And (Fe) 0.33 Ni 0.67 S 2 ) the/rGO-20% electrocatalyst was used at a current density of 50mA cm -1 100mA cm -1 When the overpotential is 332mV and 375mV respectively, which is obviously lower than that of foam Ni and RuO 2 Is a potential difference between the first and second electrodes. To obtain the stability of the catalyst, a constant potential (0.6V) step method was used to obtain (Fe 0.33 Ni 0.67 S 2 ) I-t curve of the/rGO-20% catalyst (FIG. 3 b), from which it can be seen that after 28800s the current density remains relatively stable, indicating that in a 1M KOH alkaline environment, (Fe 0.33 Ni 0.67 S 2 ) The rGO-20% catalyst has high stability.
FIG. 4 is an electrochemical impedance spectrum of the catalyst obtained in example 1 under a three-electrode system. With foam Ni, ruO 2 In contrast, (Fe 0.33 Ni 0.67 S 2 ) The catalyst of example 1 has a smaller electrochemical resistance value, indicating that the electron transfer is faster in the oxygen evolution reaction kinetics.
FIGS. 5a and 5b show oxygen evolution catalytic performance of the catalyst obtained in example 1 in a two-electrode system in which the catalyst electrode (Fe 0.33 Ni 0.67 S 2 ) The rGO-20%/NF is an anode (NF is foam Ni), the Pt/C/NF is a cathode, and the electrolyte solution is a KOH solution of 1 mol/L. In an electrolyzed water system, electrons are generated from (Fe 0.33 Ni 0.67 S 2 ) Transfer of the/rGO-20%/NF anode to the Pt/C/NF cathode, producing O at the anode 2 Generating H at the cathode 2 . As shown in fig. 5a, compared to RuO 2 A/NF// Pt/C/NF and Ni foam// Ni foam two-electrode catalyst system, (Fe) 0.33 Ni 0.67 S 2 ) The two electrode system of/rGO-20%/NF// Pt/C/NF has lower overpotential, which indicates that it has higher electrocatalytic activity in a full water-splitting system. In practical commercial applications, it is necessary to detect the long-term durability of the catalyst, and therefore, the stability of the catalyst under a two-electrode system was evaluated. As shown in FIG. 5b, there was no significant change in current density after 28800s, which indicates that in a 1M KOH alkaline two-electrode system, (Fe 0.33 Ni 0.67 S 2 ) The catalyst/rGO-20% also has high stability.
While the basic principles and main features of the present invention and advantages of the present invention have been shown and described, the foregoing embodiments and description are merely illustrative of the principles of the present invention, and various changes and modifications can be made without departing from the spirit and scope of the invention, which is defined in the appended claims. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (10)
1. Efficient water oxidation FeNiS 2 The preparation method of the rGO electrocatalyst is characterized by comprising the following steps:
(1) Weighing 0.6. 0.6g lysine, and weighing 75mL of 0.05mol/L NiCl 2 Continuously heating and stirring the solution in a water bath at 40 ℃ until the solution is dissolved, dropwise adding ammonia water until the pH value of the solution is 9.0, stirring for 0.5 hours, putting the obtained solution into a 100mL reaction kettle, preserving the temperature of the reaction kettle at 140-200 ℃ for 4-8 hours, naturally cooling to obtain a sample, centrifuging, washing and drying;
(2) Heating the dried sample in the step (1) to 300-500 ℃ according to the heating rate of 2 ℃/min in an air atmosphere, and roasting for 2-5 hours;
(3) Weighing 0.002~0.041 g FeCl 3 Adding the sample obtained after heat preservation in the step (2) of 0.03-0.05 g of thiourea and 0.01-0.05 g of graphene oxide and 0.03-g into 60-mL deionized water, carrying out ultrasonic treatment for 20 minutes, stirring in a water bath at 40 ℃ for 0.5 hours, putting the obtained mixed solution into a 100mL reaction kettle, and carrying out heat preservation on the reaction kettle at the temperature of 140-180 ℃ for 8-16 hours; naturally cooling to obtain a sample, centrifuging, washing and drying;
(4) Weighing 0.2-0.5 g of sublimed sulfur, 0.05-0.1 g of the sample obtained by drying in the step (3), mixing and grinding the two for 0.5 hour, roasting for 2-6 hours at 300-500 ℃ under the protection of inert gas, and naturally cooling to obtain FeNiS 2 An rGO electrocatalyst.
2.The efficient water oxidation FeNiS according to claim 1 2 A process for preparing the rGO electrocatalyst, characterized in that in step (1) it is incubated for 6 hours at a temperature of 180 ℃.
3. The efficient water oxidation FeNiS according to claim 1 2 A process for preparing an rGO electrocatalyst, characterized in that in step (2) it is calcined at a temperature of 350℃for 3 hours.
4. The efficient water oxidation FeNiS according to claim 1 2 A process for preparing the rGO electrocatalyst, characterized in that FeCl is used in step (3) 3 0.027g, 0.0457g for thiourea and 0.03g for GO.
5. The efficient water oxidation FeNiS according to claim 1 2 A process for preparing the rGO electrocatalyst, characterized in that step (3) is incubated at 180℃for 12 hours.
6. The efficient water oxidation FeNiS according to claim 1 2 A process for preparing an rGO electrocatalyst, characterized in that in step (4) it is calcined at 450℃for 4 hours.
7. An efficient water-oxidized FeNiS prepared by the preparation method according to any one of claims 1-6 2 The rGO electrocatalyst is characterized in that the electrocatalyst is a nano-particle and thin layer nano-composite material, and is prepared from FeNiS 2 Nano particles and a thin layer nano sheet of reduced graphene oxide are compounded to form FeNiS 2 The nano particles are uniformly attached to the surface of the reduced graphene oxide thin-layer nano sheet; feNiS 2 The composition is Fe x Ni 1-x S 2 ，x = 0.02~0.50；FeNiS 2 The size of the nano particles is 20-100 nm; the size of the reduced graphene oxide thin-layer nano sheet is 1-2 mu m.
8. The efficient water oxidation FeNiS according to claim 7 2 An rGO electrocatalyst characterized by reduced oxygenThe mass percentage of the graphene is 5-50%.
9. A highly effective water oxidation FeNiS according to claim 7 2 Use of an rGO electrocatalyst for the preparation of an electrocatalytic electrode.
10. The use according to claim 9, wherein 10mg of FeNiS 2 dispersing/rGO electrocatalytic material and 50 μl of naftifine solution in 1mL ethanol solution, performing ultrasound for 25 min to obtain uniform dispersion solution, uniformly coating 100 μl of the dispersion solution on the treated foam nickel with micropipette, placing in a blast drying oven, and heating at 60deg.C for 1 hr to obtain FeNiS 2 an/rGO electrocatalytic electrode.
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