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CN-121976230-A - Based on Fe7S8/Ti3C2 MXene/1T MoS2Preparation method of efficient electrocatalyst of nano-sheet array

CN121976230ACN 121976230 ACN121976230 ACN 121976230ACN-121976230-A

Abstract

The invention discloses a preparation method of an Fe 7 S 8 /Ti 3 C 2 MXene/1T MoS 2 nano-sheet array based on efficient electrocatalytic application. The method adopts a two-step hydrothermal method to realize the preparation of the target product. The method takes Ti 3 C 2 MXene、(NH 4 ) 6 Mo 7 O 24 ·4H 2 O、CH 4 N 2 S、L（+）- ascorbic acid and foam iron as main raw materials, utilizes an ultrasonic cleaner to carry out ultrasonic treatment on Ti 3 C 2 MXene solution, sinters the obtained solution and pretreated foam iron at 130 ℃ for 4 h to obtain IF/Ti 3 C 2 MXene, mixes (NH 4 ) 6 Mo 7 O 24 ·4H 2 O and CH 4 N 2 S and adds L (+) -ascorbic acid by magnetic stirring, and sinters the mixed solution and the IF/Ti 3 C 2 MXene obtained in the last step at 200 ℃ for 18 h to realize the preparation of a target product.

Inventors

  • LIU XINGJIA
  • Dong Chaoxu
  • JIN DOUDOU
  • LIU QIANYU
  • CAO JIAN

Assignees

  • 吉林师范大学

Dates

Publication Date
20260505
Application Date
20251217

Claims (10)

  1. 1. The preparation method of the high-efficiency electrocatalyst based on the Fe 7 S 8 /Ti 3 C 2 MXene/1T MoS 2 nano-sheet array is characterized by comprising the following specific steps of: Firstly, preprocessing foam iron to remove impurities on the surface of the foam iron; step two, the preparation of IF/Ti 3 C 2 MXene: Adding 3.2mL-8 mL of 10 mg/mL Ti 3 C 2 MXene into 12.8mL-8 mL deionized water, dispersing uniformly, transferring into a 20 mL autoclave, inserting treated foam iron, heating for 3-5 h at 125-135 ℃, naturally cooling to room temperature, taking out the foam iron, cleaning, and drying to obtain IF/Ti 3 C 2 MXene; Step three: preparation of Fe 7 S 8 /Ti 3 C 2 MXene/1T MoS 2 electrocatalyst: Adding 0.8 mmol (NH 4 ) 6 Mo 7 O 24 ·4H 2 O and 11.2 mmol CH 4 N 2 S into 15-18 mL of deionized water, stirring and dissolving, adding 0.012 g L (+) -ascorbic acid into the solution, stirring uniformly, transferring the mixed solution into a 20 mL autoclave, inserting IF/Ti 3 C 2 MXene, heating at 195-205 ℃ for 16-20 h, naturally cooling to room temperature, taking out foam iron, cleaning, and drying to obtain the high-efficiency electrocatalyst of the Fe 7 S 8 /Ti 3 C 2 MXene/1T MoS 2 nano-sheet array.
  2. 2. The method for preparing the efficient electrocatalyst based on the Fe 7 S 8 /Ti 3 C 2 MXene/1T MoS 2 nano-sheet array, which is characterized in that the step of foam iron pretreatment in the step one is as follows, cleaning by using acetone and deionized water, removing impurities on the surface of the foam iron, and drying.
  3. 3. The method for preparing the efficient electrocatalyst based on the Fe 7 S 8 /Ti 3 C 2 MXene/1T MoS 2 nano-sheet array according to claim 2, wherein the foam iron pretreatment drying condition in the first step is 60 ℃ vacuum drying 6h.
  4. 4. The method for preparing the efficient electrocatalyst based on the Fe 7 S 8 /Ti 3 C 2 MXene/1T MoS 2 nano-sheet array according to claim 1, wherein in the second step, ti 3 C 2 MXene is dispersed by stirring for 30min and then ultrasonic dispersing for 1h.
  5. 5. The method for preparing a high-efficiency electrocatalyst based on an Fe 7 S 8 /Ti 3 C 2 MXene/1T MoS 2 nano-sheet array according to claim 1, wherein the autoclave is heated at 130 ℃ for 4h in step two.
  6. 6. The method for preparing the efficient electrocatalyst based on the Fe 7 S 8 /Ti 3 C 2 MXene/1T MoS 2 nano-sheet array according to claim 1, wherein the foam iron is taken out in the second step, washed and dried under vacuum at 60 ℃ for 6h.
  7. 7. The method for preparing an efficient electrocatalyst based on an Fe 7 S 8 /Ti 3 C 2 MXene/1T MoS 2 nanoplatelet array according to claim 1, wherein deionized water in step three is 16 mL.
  8. 8. The method for preparing a high-efficiency electrocatalyst based on an Fe 7 S 8 /Ti 3 C 2 MXene/1T MoS 2 nano-sheet array according to claim 1, wherein the autoclave is heated at 200 ℃ in step three to 18 h.
  9. 9. An efficient electrocatalyst based on an Fe 7 S 8 /Ti 3 C 2 MXene/1T MoS 2 nanoplatelet array prepared according to the method of any one of claims 1 to 8.
  10. 10. Use of a high efficiency electrocatalyst based on an array of Fe 7 S 8 /Ti 3 C 2 MXene/1T MoS 2 nanoplatelets according to claim 9, characterized in that it is supported on a cathode and/or anode for electrolysis of water.

Description

Preparation method of efficient electrocatalyst based on Fe 7S8/Ti3C2 MXene/1T MoS2 nano-sheet array Technical Field The invention belongs to the technical field of catalysts for producing hydrogen by water electrolysis. Background In recent years, clean, renewable hydrogen energy has received attention as the global energy demand continues to grow. The water electrolysis hydrogen production technology is considered as an ideal hydrogen production way because of the advantages of high efficiency, low pollution, high product purity and the like. The water electrolysis process involves mainly two half reactions, hydrogen Evolution (HER) and Oxygen Evolution (OER). To improve the overall efficiency of electrolyzed water, reduce energy consumption, it is important to develop high performance electrocatalysts to reduce the overpotential of HER and OER. At present, commercial high-efficiency electrocatalyst is mainly made of noble metal materials (Pt and RuO 2), however, the cost is high, the resources are scarce, and the large-scale industrialized application is severely restricted. Therefore, research and development of low-cost, high-activity and high-stability non-noble metal electrocatalysts has become an important direction in the field. The transition metal sulfide has the advantages of abundant resources, low price, adjustable structure and the like, and has good application prospect in the field of electrocatalysis. Among them, 1T phase molybdenum disulfide (1T MoS 2) is attracting attention due to its high electrocatalytic activity. However, the 1T MoS 2 still faces the problems of insufficient structural stability, limited active sites and the like, so that the catalytic performance of the catalyst still has a larger improvement space. MXene materials (such as Ti 3C2 MXene) have high conductivity, rich surface functional groups and unique lamellar fold structures, and are compounded with 1T MoS 2, so that the high conductivity and structural support effect of the MXene materials are expected to be utilized, the structural collapse problem of 1T MoS 2 is relieved, and the charge transmission efficiency of a compound system is improved. The foam iron has a three-dimensional framework structure, and the foam iron is used as a reaction substrate to help to construct a stable conductive structure and richer multi-stage pores, promote mass transfer process and expose more active sites. The Fe 7S8 generated by vulcanizing the iron element in the foam iron and the Ti 3C2MXene、1T MoS2 can generate stronger electronic interaction, which is beneficial to optimizing the electronic structure of the active site, thereby improving the intrinsic activity. Disclosure of Invention In order to solve the problems, the invention adopts Ti3C2MXene、(NH4)6Mo7O24·4H2O、CH4N2S、L(+)- ascorbic acid (L-Ascorbic acid) and foam iron as main raw materials by a two-step simple hydrothermal method, ti 3C2 MXene and 1T MoS 2 are grown on a foam iron substrate in situ to obtain an Fe 7S8/Ti3C2MXene/1T MoS2 array, the aim of improving the activity specific surface area of the electrocatalyst is achieved by improving the dispersibility of Ti 3C2 MXene and 1T MoS 2, and meanwhile, the high conductivity of Ti 3C2 MXene is utilized, and the electrocatalyst efficiency is improved by promoting the rapid migration of carriers. The invention provides a preparation method of an efficient electrocatalyst of an Fe 7S8/Ti3C2MXene/1T MoS2 nano-sheet array, which comprises the following specific steps: Firstly, preprocessing foam iron to remove impurities on the surface of the foam iron; step two, the preparation of IF/Ti 3C2 MXene: Adding 3.2mL-8 mL of 10 mg/mL Ti 3C2 MXene into 12.8mL-8 mL deionized water, dispersing uniformly, transferring into a 20 mL autoclave, inserting treated foam iron, heating for 3-5 h at 125-135 ℃, naturally cooling to room temperature, taking out the foam iron, cleaning, and drying to obtain IF/Ti 3C2 MXene; Step three: preparation of Fe 7S8/Ti3C2MXene/1T MoS2 electrocatalyst: Adding 0.8 mmol (NH 4)6Mo7O24·4H2 O and 11.2 mmol CH 4N2 S into 15-18 mL of deionized water, stirring and dissolving, adding 0.012 g L (+) -ascorbic acid into the solution, stirring uniformly, transferring the mixed solution into a 20mL autoclave, inserting IF/Ti 3C2 MXene, heating at 195-205 ℃ for 16-20 h, naturally cooling to room temperature, taking out foam iron, cleaning, and drying to obtain the high-efficiency electrocatalyst of the Fe 7S8/Ti3C2MXene/1T MoS2 nano-sheet array. Preferably, the foam iron pretreatment in the first step comprises the steps of cleaning by using acetone and deionized water, removing impurities on the surface of the foam iron, and drying. Further preferably, the foam iron pretreatment drying condition in the first step is 60 ℃ vacuum drying 6 h. Preferably, in the second step, ti 3C2 MXene is dispersed by stirring for 30min and then ultrasonically dispersed for 1h. Preferably, the autoclave is heated at 130 ℃ in step tw