Preparation method and hydrogen evolution performance application of balsam pear epidermis-shaped 5% Co-FePS / GF catalyst

Abstract

The invention discloses a preparation method and hydrogen evolution performance application of a balsam pear epidermis-shaped 5% Co-FePS / GF catalyst, and according to the method, sucrose is used as a morphology guiding agent, Co is used as a doping agent, NaH2PO2 is used as a reducing agent, ferric salt is used as a metal precursor, and the 5% Co-FePS / GF catalyst can be obtained through hydrothermal-phosphating reduction. The 5% Co-FePS / GF catalyst prepared by the method disclosed by the invention is similar to balsam pear skin in morphology, has the advantages of large specific surface area, multiple active sites, stable structure and the like, shows excellent HER performance in different electrolytes, and has very wide commercial production application potential.

Description

Technical Field

[0001] This invention belongs to the field of electrocatalysis technology, and relates to a method for preparing a 5% Co-FePS / GF catalyst in the form of bitter gourd peel and its hydrogen evolution performance application. Background Technology

[0002] Hydrogen energy, with its high energy density and environmental friendliness, is considered an excellent energy carrier and contributes to achieving carbon neutrality. Among various hydrogen production processes, electrochemical water splitting is a recognized clean method; however, its slow kinetics are a key constraint to the industrialization of water electrolysis, and developing commercially viable high-performance electrocatalysts remains a significant challenge. Theoretically, platinum group metals are the ideal electrode materials, but their high cost limits their large-scale application. Therefore, exploring efficient, stable, and low-cost non-precious metal catalysts for electrocatalytic water splitting is of great importance.

[0003] Transition metal phosphides (TMPs) have been widely studied for HER due to their excellent stability and catalytic performance. Iron, comprising 5% of the Earth's crust, is the most abundant transition metal and forms the basis of all 3d transition metal phosphides, exhibiting high intrinsic HER activity and electronic conductivity. Therefore, iron phosphide (FeP), as a low-cost and globally abundant catalyst, has received increasing attention in recent years. Based on the above analysis, this invention prepared a cobalt-doped iron phosphide (5% Co-FePS / GF) catalyst with a bitter gourd-like surface on carbon felt fibers using hydrothermal and vapor deposition methods, and investigated its HER performance in different electrolytes. Summary of the Invention

[0004] The purpose of this invention is to provide a method for preparing a HER catalyst and to study its HER performance in different electrolytes.

[0005] To achieve the above objectives, the present invention adopts the following technical solution:

[0006] 1.35 g FeCl3·6H2O, 0.6006 g urea, a certain amount of sucrose, and CoCl2·6H2O were dissolved in 50 mL of deionized water and stirred continuously to form a clear solution. The solution and graphite felt (GF, 3*3 cm) were transferred to a 100 mL Telfon-lined high-pressure reactor and heated at 120 °C for 8 h. After natural cooling to room temperature, the reactor was removed, washed with anhydrous ethanol and deionized water, and dried under vacuum at 60 °C for 12 h to obtain 5% Co-FeS / GF. Then, 5% Co-FeS / GF and 1 g NaH2PO2 were placed in two porcelain boats, which were placed side-by-side in a tube furnace (the boat containing NaH2PO2 was upstream). The furnace was heated to 350 °C at 2 °C / min under a nitrogen atmosphere and held for 3 h. After cooling, the reactor was washed several times with ultrapure water and dried under vacuum at 60 °C for 12 h to finally obtain the catalyst 5% Co-FePS / GF.

[0007] The method for preparing the 5% Co-FePS / GF catalyst provided by this invention has the following characteristics:

[0008] 1. The method and process are simple to operate and easy to synthesize. The raw materials used are all non-toxic (low-toxic) reagents that are easy to purchase. The reaction is low-risk, the product is green and environmentally friendly, has good reproducibility, and is easy to prepare on a large scale.

[0009] 2. The prepared 5% Co-FePS / GF catalyst exhibits excellent electrocatalytic activity for HER under both acidic and alkaline conditions, and has a very broad application prospect. Attached Figure Description

[0010] Figure 1 X-ray diffraction (XRD) pattern of the 5% Co-FePS / GF catalyst prepared in Example 1 of this invention.

[0011] Figure 2 The scanning electron microscope (SEM) image of the 5% Co-FePS / GF catalyst prepared in Example 1 of this invention;

[0012] Figure 3 The image shows the HER performance of the 5% Co-FePS / GF catalyst prepared in Example 1 of this invention.

[0013] Figure 4 The image shows a chronopotential (CP) chromatogram of the 5% Co-FePS / GF catalyst prepared in Example 1 of this invention. Detailed Implementation

[0014] The embodiments of the present invention will now be described in detail with reference to the accompanying drawings. These embodiments are merely illustrative of the technical solutions of the present invention and are therefore only examples, not intended to limit the scope of protection of the present invention.

[0015] Unless otherwise specified, the experimental methods used in the following examples are conventional methods. Unless otherwise specified, the experimental materials used in the following examples were all purchased from conventional reagent stores. All quantitative experiments in the following examples were performed in triplicate, and the data are the average of the three replicates or the average ± standard deviation.

[0016] For example, a method for preparing a 5% Co-FePS / GF catalyst includes the following steps:

[0017] Example 1

[0018] 1.35 g FeCl3·6H2O, 0.6006 g urea, 0.86 g sucrose, and 0.06 g CoCl2·6H2O were dissolved in 50 mL of deionized water and stirred continuously to form a clear solution. The solution and graphite felt (GF, 3*3 cm) were transferred to a 100 mL Telfon-lined high-pressure reactor and heated at 120 °C for 8 h. After natural cooling to room temperature, the reactor was removed, washed with anhydrous ethanol and deionized water, and dried under vacuum at 60 °C for 12 h to obtain 5% Co-FeS / GF. Then, 5% Co-FeS / GF and 1 g NaH2PO2 were placed in two ceramic boats, which were placed side-by-side in a tube furnace (the boat containing NaH2PO2 was upstream). The furnace was heated to 350 °C at 2 °C / min under a nitrogen atmosphere and held for 3 h. After cooling, the reactor was washed several times with ultrapure water and dried under vacuum at 60 °C for 12 h to finally obtain the catalyst 5% Co-FePS / GF.

[0019] Example 2

[0020] 1.35 g FeCl3·6H2O and 0.6006 g urea were dissolved in 50 mL deionized water with constant stirring to form a clear solution. The solution and graphite felt (GF, 3*3 cm) were transferred to a 100 mL Telfon-lined high-pressure reactor and heated at 120 °C for 8 h. After natural cooling to room temperature, the reactor was removed, washed with anhydrous ethanol and deionized water, and dried under vacuum at 60 °C for 12 h to obtain Fe2O3 / GF. Then, Fe2O3 / GF was placed in two porcelain boats with 1 g NaH2PO2, and the boats were placed side-by-side in a tube furnace (the boat containing NaH2PO2 was upstream). The furnace was heated to 350 °C at 2 °C / min under a nitrogen atmosphere and held for 3 h. After cooling, the reactor was washed several times with ultrapure water and dried under vacuum at 60 °C for 12 h to finally obtain the catalyst FePS / GF.

[0021] Example 3

[0022] 1.35 g FeCl3·6H2O, 0.6006 g urea, and 0.86 g of urea were dissolved in 50 mL of deionized water, and the solution was stirred continuously to form a clear solution. The solution and graphite felt (GF, 3*3 cm) were transferred to a 100 mL Telfon-lined high-pressure reactor and heated at 120 °C for 8 h. After natural cooling to room temperature, the solution was removed, washed with anhydrous ethanol and deionized water, and dried under vacuum at 60 °C for 12 h to obtain Fe-S / GF. Then, 1 g of NaH2PO2 was placed in two porcelain boats, which were placed side-by-side in a tube furnace (the boat containing NaH2PO2 was upstream). The furnace was heated to 350 °C at a nitrogen atmosphere at 2 °C / min and held for 3 h. After cooling, the solution was washed several times with ultrapure water and dried under vacuum at 60 °C for 12 h to finally obtain the catalyst Fe-PS / GF.

[0023] Research findings on a 5% Co-FePS / GF catalyst:

[0024] 1. Material Structure Analysis

[0025] The 5% Co-FePS / GF catalyst prepared in Example 1 above was physically characterized using XRD and SEM. Figure 1 As can be seen from the SEM, apart from the diffraction peak of GF, there are no other obvious diffraction peaks, indicating that the sample has low crystallinity. Figure 2 As can be seen, the catalyst prepared according to the method of the present invention exhibits a bitter gourd-like morphology, which can provide more active sites for the catalytic reaction and thus improve the performance of the catalyst.

[0026] 2. HER performance

[0027] The HER performance and stability of the 5% Co-FePS / GF catalyst were tested in 1M KOH and 0.5M H2SO4. The LSV curves were obtained by linear sweep cyclic voltammetry. Figure 3 The HER performance of the 5% Co-FePS / GF catalyst was obtained as 95 and 66 mV; the catalytic stability of the 5% Co-FePS / GF catalyst was studied by chronopotential (CP) method. Figure 4 ), at 50mA cm -2 At the specified current density, the 5% Co-FePS / GF electrode can operate stably for 100 and 50 hours in alkaline and acidic environments, respectively.

[0028] In summary, the method of this invention is simple to operate and easy to synthesize. The 5% Co-FePS / GF catalyst prepared has a unique morphology and has the advantages of large specific surface area, many active sites, and stable structure, and has a very broad potential for commercial production and application.

[0029] The above description is merely a preferred embodiment of the present invention, and the scope of protection of the present invention is not limited thereto. Any simple changes or equivalent substitutions of the technical solutions that can be obviously obtained by those skilled in the art within the scope of the technology disclosed in the present invention shall fall within the scope of protection of the present invention.

Claims

1. A method for preparing a 5% Co-FePS / GF catalyst resembling the skin of bitter melon, characterized in that, Includes the following steps: Iron salts, urea, sucrose, and cobalt salts were dissolved in deionized water and stirred continuously to form a clear solution. The solution and graphite felt (GF, 3*3cm) were transferred to a Telfon-lined high-pressure reactor and heated at 120°C for 8 hours. After natural cooling to room temperature, the reactor was removed, washed with anhydrous ethanol and deionized water, and dried under vacuum at 60°C for 12 hours to obtain 5% Co-FeS / GF. Then, 5% Co-FeS / GF and 1g NaH2PO2 were placed in two ceramic boats, which were placed side-by-side in a tube furnace (the boat containing NaH2PO2 was upstream). The furnace was heated to 350°C at 2°C / min under a nitrogen atmosphere and held for 3 hours. After cooling, the reactor was washed several times with ultrapure water and dried under vacuum at 60°C for 12 hours to finally obtain the catalyst 5% Co-FePS / GF.

2. The method for preparing a 5% Co-FePS / GF catalyst in the form of bitter melon peel according to claim 1, characterized in that: The morphology guiding agent is sucrose.

3. The method for preparing a 5% Co-FePS / GF catalyst in the epidermis of bitter gourd according to claim 1, characterized in that: The iron salt is ferric chloride, ferric nitrate, or ferric sulfate.

4. The method for preparing a 5% Co-FePS / GF catalyst in the form of bitter melon epidermis according to claim 1, characterized in that: The molar ratio of ferric chloride to sucrose is 2:1 to 5:

1.

5. The method for preparing a 5% Co-FePS / GF catalyst in the epidermis of bitter gourd according to claim 1, characterized in that: The molar ratio of Co to Fe is 1%-5%.

6. The method for preparing a 5% Co-FePS / GF catalyst in the epidermis of bitter gourd according to claim 1, characterized in that: The hydrothermal reaction temperature is 120℃ and the reaction time is 8 hours.

7. The method for preparing a 5% Co-FePS / GF catalyst in the form of bitter melon epidermis according to claim 1, characterized in that: The phosphating temperature is 300-350℃ and the time is 1-3 hours.

8. The method for preparing a 5% Co-FePS / GF catalyst in the form of bitter melon epidermis according to claim 1, characterized in that: The phosphating heating rate is 2℃ / min.

9. A 5% Co-FePS / GF catalyst in the form of bitter gourd peel, prepared by the preparation method according to any one of claims 1-8.

10. The application of the 5% Co-FePS / GF catalyst in the epidermal form of bitter gourd obtained by the preparation method according to any one of claims 1-9 in hydrogen evolution performance.

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