CN114108028A - Efficient water oxidation FeNiS2rGO electrocatalyst and its preparation method and use - Google Patents
Efficient water oxidation FeNiS2rGO electrocatalyst and its preparation method and use Download PDFInfo
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- CN114108028A CN114108028A CN202111514762.XA CN202111514762A CN114108028A CN 114108028 A CN114108028 A CN 114108028A CN 202111514762 A CN202111514762 A CN 202111514762A CN 114108028 A CN114108028 A CN 114108028A
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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 high-efficiency water oxidation FeNiS2A/rGO electrocatalyst, a preparation method and application thereof belong to the technical field of water electrolysis catalysts. The electrocatalyst in the invention is a nano-particle and thin layer nano composite material, and the composite material is made of FeNiS2Nanoparticles and reduced graphene oxide (rGO) thin-layer nanosheets, FeNiS2Nanoparticles are uniformly attached to the surface of rGO thin-layer nanosheets. FeNiS2Has the composition of FexNi1‑xS2(x＝0.02～0.5)，FeNiS2The size of the nano particles is 20-100 nm; the size of the rGO thin-layer nanosheet is 1-2 mu m. The invention relates to a method for preparing bimetal transition metal sulfideThe graphene is introduced into the rice particles as a carrier, so that the dispersity of transition metal sulfide can be enhanced, the agglomeration of nano particles is inhibited, stable particles are improved, the graphene can be used as a catalyst promoter, the activity of the catalyst is improved through a 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 high-efficiency water oxidation FeNiS2A/rGO electrocatalyst and a preparation method thereof belong to the technical field of water electrolysis catalysts.
Background
Energy is an important material basis for economic growth and social revolution. With the growth of the world population and the acceleration of the industrialization process, the significant concern of energy crisis and environmental problems caused by the excessive consumption of fossil fuels has pushed the exploration of renewable and clean energy sources, such as wind energy, solar energy, hydrogen energy and the like. 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(Δ G is 237.2kJ/mol), however, in an actual situation, the existence of electrochemical polarization, concentration polarization and the like causes the electrode potential to deviate from the equilibrium potential, and an overpotential is generated, so that the actual decomposition voltage of water is much larger than 1.23V, and therefore, an efficient electrocatalyst is required to be adopted 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 reaction and hydrogen evolution reaction. Compared to hydrogen evolution reactions, oxygen evolution reactions are a four electron transfer process with multiple intermediate states resulting in slow kinetics and larger overpotentials. The oxygen evolution reaction mainly determines the overall water dividing efficiency of the electrolytic cell. At present, noble metal-based electrocatalysts are considered to be better oxygen evolution reaction electrocatalysts in alkaline electrocatalysts, but the reserves of the noble metal-based electrocatalysts are limited, the cost is high, and the commercial application development of the noble metal-based electrocatalysts is limited. Therefore, the development of low-cost and high-efficiency non-noble metal electrocatalysts is imperative.
Transition metals (e.g., iron, molybdenum, nickel, tungsten, etc.) can provide unpaired d-orbital electrons and can therefore open O-H bonds. Transition metal sulfides have a hydrogenase-like catalytic mechanism and a high catalytic activity for oxygen evolution reactions, and thus more and more people are beginning to study non-noble metal transition metal sulfide electrocatalysts. However, simple transition metal sulfides are easily agglomerated, so that they have slow kinetics and high overpotentials.
Disclosure of Invention
The invention aims to provide FeNiS for electrocatalytic oxygen evolution reaction with low raw material price, high catalytic activity, low overpotential and good chemical stability aiming at the problems of the existing transition metal sulfide electrocatalyst2a/rGO electrocatalyst.
In order to achieve the purpose, the invention adopts the following technical scheme:
efficient water oxidation FeNiS2/rGO electrocatalyst, the FeNiS2the/rGO electro-catalytic material is a nano-particle and thin-layer nano-sheet composite material, and the composite material is made of FeNiS2Nanoparticles and reduced graphene oxide (rGO) thin-layer nanosheets, FeNiS2Nanoparticles are uniformly attached to the surface of rGO thin-layer nanosheets. The FeNiS2In the/rGO material, FeNiS2Has the composition of FexNi1-xS2(x＝0.02～0.5)，FeNiS2The size of the nano particles is 20-100 nm; the size of the rGO thin-layer nanosheet is 1-2 mu m.
Preferably, the aqueous oxidation FeNiS2In the/rGO electro-catalytic material, the percentage of rGO is 5-50%.
The invention also provides the high-efficiency water oxidation FeNiS2The preparation method of the/rGO electro-catalytic material comprises the following steps:
(1) 0.6g of lysine was weighed out and 75mL of 0.05mol/L NiCl was measured2Continuously 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 hour, putting the obtained solution into a 100mL reaction kettle, keeping 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 sample dried in the step (1) to 300-500 ℃ at a heating rate of 2 ℃/min in an air atmosphere, and roasting for 2-5 hours;
(3) weighing 0.002-0.041 g FeCl30.03-0.05 g of thiourea and 0.01-0.05 g of Graphene Oxide (GO), and 0.03g of the catalyst in the step (2)Adding the sample obtained after the temperature is increased into 60mL of deionized water, performing 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 keeping the temperature of the reaction kettle at 140-180 ℃ for 8-16 hours; naturally cooling and 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 in the step (3), mixing and grinding the two samples for 0.5 hour, roasting for 2-6 hours at 300-500 ℃ under the protection of inert gas, and naturally cooling to obtain FeNiS2a/rGO electrocatalytic material.
Preferably, the incubation in step (1) is carried out at a temperature of 180 ℃ for 6 hours.
Preferably, the calcination in step (2) is carried out at a temperature of 350 ℃ for 3 hours.
Preferably, FeCl is used in step (3)30.027g, 0.0457g thiourea and 0.03g GO.
Preferably, the incubation in step (3) is carried out at a temperature of 180 ℃ for 12 hours.
Preferably, the calcination in step (4) is carried out at a temperature of 450 ℃ for 4 hours.
FeNiS2The preparation method of the/rGO electrocatalytic electrode comprises the following steps: 10mg of FeNiS prepared in the step (4) above is added2Dispersing 50 mu L of naphthylene solution in 1mL of ethanol solution to obtain a uniform dispersion solution by ultrasonic treatment for 25 minutes, uniformly coating 100 mu L of the dispersion solution on the treated foam nickel by using a micro liquid transfer gun, placing the foam nickel in a blast drying oven, and heating for 1 hour at 60 ℃ to obtain FeNiS2a/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 easily available, 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, the graphene is introduced into the bimetallic transition metal sulfide nano particles as a carrier, so that the dispersity 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 a 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 photograph of the catalyst obtained in example 1
FIG. 3a shows the oxygen evolution catalytic performance of the catalyst obtained in example 1 in a three-electrode system: linear sweep voltammogram
FIG. 3b shows the oxygen evolution catalytic performance of the catalyst obtained in example 1 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 oxygen evolution catalytic performance of the catalyst obtained in example 1 in a two-electrode system: linear sweep voltammogram
FIG. 5b shows the oxygen evolution catalytic performance of the catalyst obtained in example 1 in a two-electrode system: i-t curve obtained by constant potential step method
Detailed Description
The technical solution of the invention is further explained and illustrated in the form of specific embodiments.
Example 1:
in this example, FeNiS is an efficient water oxidation2the/rGO electrocatalyst and the preparation method thereof are carried out according to the following steps:
(1) 0.6g of lysine was weighed out and 75mL of 0.05mol/L NiCl was measured2Continuously 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 hour, putting the obtained solution into a 100mL reaction kettle, putting the reaction kettle into an oven, keeping the temperature of the reaction kettle at 180 ℃ for 6 hours, naturally cooling to obtain a sample, centrifuging, washing and drying;
(2) putting the sample dried 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 FeCl30.0457g of thiourea and 0.03g of oxygenDissolving Graphene (GO), adding 0.03g of the sample obtained after heat preservation in the step (2) into 60mL of deionized water, performing 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, putting the reaction kettle into an oven, performing heat preservation at 180 ℃ for 12 hours, naturally cooling to obtain a sample, centrifuging, washing and drying;
(4) weighing 0.275g of sublimed sulfur and 0.055g of the sample obtained in the step (3), mixing and grinding the two samples for 0.5 hour, roasting the mixture for 4 hours at 450 ℃ in a tubular furnace under the protection of nitrogen inert gas, and naturally cooling to obtain (Fe)0.33Ni0.67S2) /rGO-20% electrocatalytic material.
FIG. 1 is the XRD pattern of the sample obtained in example 1, when the doping molar ratio of Fe is 33%, NiS in pure phase can be obtained2And is in accordance with standard NiS2The standard spectrum (JCPDS No:65-3325) corresponds to the standard spectrum, and the sample is marked as (Fe)0.33Ni0.67S2)/rGO-20％。
FIG. 2 is an SEM image of a sample obtained in example 1, and it can be seen from the SEM image that the composite material is formed by compounding nanoparticles with the size of 50nm and rGO thin-layer nanosheets, and Fe with uniform particle size0.33Ni0.67S2The nano-particles are uniformly dispersed on the surface of the rGO thin-layer nanosheet, so that the rapid electron transmission and high stability are guaranteed.
In example 1 (Fe)0.33Ni0.67S2) The preparation method of the/rGO-20% electrocatalytic electrode comprises the following steps:
10mg of (Fe) prepared in the above step (4)0.33Ni0.67S2) The preparation method comprises the following steps of dispersing 50 mu L of naphthylene solution in 1mL of ethanol solution of/rGO-20% electro-catalytic material, carrying out ultrasonic treatment for 25 minutes to obtain a uniform dispersion solution, uniformly coating 100 mu L of the dispersion solution on treated foam Ni by using a liquid transfer gun, then placing the foam Ni in a blast drying oven, and heating at 60 ℃ for 1 hour to obtain (Fe)0.33Ni0.67S2) a/rGO-20% electrocatalytic electrode.
FIGS. 3a and 3b show the oxygen evolution catalytic performance of the catalyst obtained in example 1 in a three-electrode system with Hg/HgO as referenceThe electrode, graphite carbon rod as the counter electrode, the catalyst electrode in example 1 as the working electrode, and the electrolyte solution was 1mol/L KOH solution. FIG. 3a is a linear sweep voltammogram compared to foamed Ni and RuO2,(Fe0.33Ni0.67S2) the/rGO-20% electrocatalyst shows better electrocatalytic activity, and when the current density is 10mA cm-1,(Fe0.33Ni0.67S2) The overpotential of/rGO-20% electrocatalyst is 142mV, which is obviously lower than that of foamed Ni (422mV) and RuO2(348 mV). And (Fe)0.33Ni0.67S2) /rGO-20% electrocatalyst at a Current Density of 50mA cm-1And 100mA cm-1When the nickel-copper alloy is used, the overpotential is respectively 332mV and 375mV, which are obviously lower than that of foamed Ni and RuO2Over-potential of (c). To obtain the stability of the catalyst, (Fe) was obtained by potentiostatic (0.6V) step method0.33Ni0.67S2) I-t curve for/rGO-20% catalyst (FIG. 3b), it can be seen that the current density remains relatively stable after 28800s, indicating that under 1M KOH alkaline environment, (Fe)0.33Ni0.67S2) the/rGO-20% catalyst has high stability.
FIG. 4 is an electrochemical impedance spectrum of the catalyst obtained in example 1 in a three-electrode system. With foamed Ni, RuO2In contrast, (Fe)0.33Ni0.67S2) the/rGO-20% catalyst has a much smaller electrochemical impedance value, indicating that the catalyst of this example 1 has faster electron transfer in the kinetics of the oxygen evolution reaction.
FIGS. 5a and 5b show the oxygen evolution catalytic performance of the catalyst obtained in example 1 in a two-electrode system, i.e., a two-electrode full-hydrolysis system, and the catalyst electrode (Fe) in example 10.33Ni0.67S2) the/rGO-20%/NF is used as an anode (NF is foam Ni), the Pt/C/NF is used as a cathode, and the electrolyte solution is a KOH solution of 1 mol/L. In an electrolytic water system, electrons are driven from (Fe)0.33Ni0.67S2) Transfer of/rGO-20%/NF anodes to Pt/C/NF cathodes to produce O on the anodes2Generating H on the cathode2. As shown in fig. 5a, in comparison to RuO2Two-electrode catalysis of/NF// Pt/C/NF and Ni foam// Ni foamSystem of (Fe)0.33Ni0.67S2) the/rGO-20%/NF// Pt/C/NF two-electrode system has lower overpotential, which shows that the electrode system has higher electrocatalytic activity in a full-hydrolytic system. In practical commercial applications, it is necessary to examine 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, after 28800s, there was no significant change in current density, indicating that in a 1M KOH alkaline environment two-electrode system, (Fe)0.33Ni0.67S2) the/rGO-20% catalyst also has high stability.
While the foregoing shows and describes the principles of the present invention, together with the general features and advantages thereof, the foregoing embodiments and description merely illustrate the principles of the invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is further defined in the appended claims. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. Efficient water oxidation FeNiS2The preparation method of the/rGO electrocatalyst is characterized by comprising the following steps:
(1) 0.6g of lysine was weighed out and 75mL of 0.05mol/L NiCl was measured2Continuously 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 hour, putting the obtained solution into a 100mL reaction kettle, keeping 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 sample dried in the step (1) to 300-500 ℃ at a heating rate of 2 ℃/min in an air atmosphere, and roasting for 2-5 hours;
(3) weighing 0.002-0.041 g FeCl30.03-0.05 g of thiourea and 0.01-0.05 g of graphene oxide, 0.03g of the sample obtained in the step (2) after heat preservation is added into 60mL of deionized water, ultrasonic treatment is carried out for 20 minutes, stirring is carried out in a water bath at 40 ℃ for 0.5 hour, the obtained mixed solution is placed into a 100mL reaction kettle, and the mixture is subjected to vacuum dryingThe reaction kettle is subjected to heat preservation for 8-16 hours at the temperature of 140-180 ℃; naturally cooling and 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 in the step (3), mixing and grinding the two samples for 0.5 hour, roasting for 2-6 hours at 300-500 ℃ under the protection of inert gas, and naturally cooling to obtain FeNiS2a/rGO electrocatalyst.
2. The high efficiency aqueous oxidation FeNiS of claim 12The preparation method of the/rGO electrocatalyst is characterized in that in the step (1), the temperature is kept at 180 ℃ for 6 hours.
3. The high efficiency aqueous oxidation FeNiS of claim 12The preparation method of the/rGO electrocatalyst is characterized in that in the step (2), the calcination is carried out for 3 hours at the temperature of 350 ℃.
4. The high efficiency aqueous oxidation FeNiS of claim 12The preparation method of the/rGO electrocatalyst is characterized in that FeCl is adopted in the step (3)30.027g, 0.0457g thiourea and 0.03g GO.
5. The high efficiency aqueous oxidation FeNiS of claim 12The preparation method of the/rGO electrocatalyst is characterized in that the temperature in the step (3) is kept at 180 ℃ for 12 hours.
6. The high efficiency aqueous oxidation FeNiS of claim 12The preparation method of the/rGO electrocatalyst is characterized in that in the step (4), the calcination is carried out for 4 hours at 450 ℃.
7. High-efficiency water oxidation FeNiS prepared by the preparation method of any one of claims 1 to 62the/rGO electrocatalyst is characterized in that the electrocatalyst is a nano-particle and thin layer nano composite material and is prepared from FeNiS2The nano particles and the reductive graphene oxide thin-layer nanosheets are compounded to form FeNiS2The nanoparticles are uniformly attachedOn the surface of the reducing graphene oxide thin-layer nanosheet; FeNiS2Has the composition of FexNi1-xS2，x＝0.02～0.50；FeNiS2The size of the nano particles is 20-100 nm; the size of the reducing graphene oxide thin-layer nanosheet is 1-2 microns.
8. The high efficiency water oxidation FeNiS of claim 72the/rGO electrocatalyst is characterized in that the mass percentage of the reductive graphene oxide is 5-50%.
9. The high efficiency aqueous oxidation FeNiS as claimed in claim 72Use of/rGO electrocatalyst for the preparation of an electrocatalytic electrode.
10. The high efficiency aqueous oxidation FeNiS of claim 92Use of/rGO electrocatalyst, characterised in that 10mg FeNiS is added2Dispersing the/rGO electro-catalytic material and 50 mu L of naphthylene solution in 1mL of ethanol solution, performing 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 micro liquid transfer gun, placing the foam nickel in a blast drying oven, and heating at 60 ℃ for 1 hour to obtain FeNiS2a/rGO electrocatalytic electrode.
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