CN113921836A - Composite material for electrocatalytic hydrogen evolution of alkaline solution and preparation method thereof - Google Patents

Composite material for electrocatalytic hydrogen evolution of alkaline solution and preparation method thereof Download PDF

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CN113921836A
CN113921836A CN202111148795.7A CN202111148795A CN113921836A CN 113921836 A CN113921836 A CN 113921836A CN 202111148795 A CN202111148795 A CN 202111148795A CN 113921836 A CN113921836 A CN 113921836A
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composite material
chitosan
hydrogen evolution
solid
electrocatalytic hydrogen
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刘清雷
唐洪霆
王伟
刘慧敏
李珊珊
李雪
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Shanghai Institute of Technology
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Shanghai Institute of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Abstract

The invention discloses a composite material for electrocatalytic hydrogen evolution of an alkaline solution and a preparation method thereof. With RuCl3Is active metal Ru source, chitosan is carbon and nitrogen source, ZnCl2Respectively weighing RuCl as an activating agent and a pore-forming agent3Chitosan, ZnCl2Dispersing the mixture in deionized water to obtain a mixed solution, stirring the mixed solution at a constant temperature for reaction, and drying the mixed solution to obtain a solid; grinding the obtained solid, putting the ground solid into a tube furnace, and calcining the solid in the presence of inert gas to obtain solid powder; and adding the obtained solid powder into hydrochloric acid, etching under constant-temperature stirring, and performing suction filtration, washing and drying to obtain the composite material of the Ru nano particles loaded on the nitrogen-containing porous layered carbon material. The composite material prepared by the invention can show excellent catalytic performance in water desorption of hydrogen under alkaline conditions, and has very stable performance.

Description

Composite material for electrocatalytic hydrogen evolution of alkaline solution and preparation method thereof
Technical Field
The invention relates to a nitrogen-containing porous layered composite material for electrocatalytic hydrogen evolution of an alkaline solution and a preparation method thereof, belonging to the technical field of hydrolytic hydrogen evolution catalysis under alkaline conditions.
Background
Hydrogen fuel is considered the cleanest renewable resource and is a major alternative to fossil fuels in future energy supplies. Sustainable hydrogen production is an important prerequisite for realizing future hydrogen economy. Electrocatalytic Hydrogen Evolution (HER) as a key step in the electrolysis of water to produce hydrogen has been the subject of extensive research for the past few decades.
The production of hydrogen from water is difficult due to the high overpotential required for the water splitting reaction. Energy efficient HER must use catalysts to trigger proton reduction with minimal overpotential and enhance the kinetic process. In practice, the electrolysis of water can be carried out not only in an acidic electrolyte but also in an alkaline electrolyte. The widespread use of acidic electrolyzed water is severely hampered both technically and commercially by the slow electron transfer kinetics of the oxygen evolution reaction in acidic media and by the lack of efficient, low cost counter electrode catalysts. These problems can be alleviated if the reaction is carried out in an alkaline medium. The kinetics of hydrogen evolution in alkaline environments, including Pt-based catalysts, are two to three times slower than in acid electrolytes, due to the larger kinetic barrier of the previous hydrolysis separation step (Volmer step). Therefore, there is significant real-world and challenge to develop non-platinum HER catalysts with high activity and stability in alkaline media. In terms of performance, platinum is the best HER catalyst as an electrocatalyst for hydrogen evolution reactions with almost zero overpotential and excellent long-term durability, but unfortunately the high price of platinum-based electrocatalysts has hindered their widespread commercialization. Therefore, the search for a platinum electrocatalyst substitute with high cost performance is of great significance. Ruthenium (Ru) has a bonding strength similar to that of hydrogen, and is widely used in many important chemical reactions as an inexpensive substitute for platinum. In particular, ruthenium is much less expensive ($ 290 per ounce) than platinum group metals (e.g., platinum ($ 835 per ounce), palladium ($ 2107 per ounce), or iridium ($ 1733 per ounce)).
Disclosure of Invention
The technical problem to be solved by the invention is as follows: how to improve the catalytic performance and stability of the Ru-based electrocatalyst and improve the hydrogen evolution performance of the electrocatalyst.
In order to solve the technical problem, the invention provides a preparation method of a composite material for electrocatalytic hydrogen evolution of an alkaline solution, which comprises the following steps:
step 1): with RuCl3Is active metal Ru source, chitosan is carbon and nitrogen source, ZnCl2Respectively weighing RuCl as an activating agent and a pore-forming agent3Chitosan, ZnCl2Dispersing the mixture in deionized water to obtain a mixed solution, stirring the mixed solution at a constant temperature for reaction, and drying the mixed solution to obtain a solid;
step 2): grinding the solid obtained in the step 1), putting the ground solid into a tube furnace, and calcining the solid in the tube furnace under the protection of inert gas to obtain solid powder;
step 3): adding the solid powder obtained in the step 2) into hydrochloric acid, etching under constant-temperature stirring, and performing suction filtration, washing and drying to obtain the composite material of the Ru nano particles loaded on the nitrogen-containing porous layered carbon material.
Preferably, in the step 1), ZnCl is used2The weight ratio of the chitosan to the chitosan is 1: 4; the weight ratio of the deionized water to the chitosan is (15-20): 1; the RuCl3The weight ratio of the chitosan to chitosan is (1-4.6): 6.
more preferably, the RuCl3The weight ratio of the chitosan to the chitosan is 1: 3.
preferably, the reaction temperature in the step 1) is 80 ℃ and the reaction time is 12 hours.
Preferably, the calcining temperature in the step 2) is 900 ℃, the heating rate is 3 ℃/min, and the calcining time is 1 hour.
Preferably, the concentration of the hydrochloric acid in the step 3) is 1 mol/L.
Preferably, the weight ratio of the solid powder to the hydrochloric acid in the step 3) is (1-5): 120.
preferably, the etching temperature in the step 3) is 120 ℃ and the etching time is 12 hours.
The invention also provides the composite material for the electrocatalytic hydrogen evolution of the alkaline solution, which is prepared by the preparation method of the composite material for the electrocatalytic hydrogen evolution of the alkaline solution.
Compared with the prior art, the invention has the beneficial effects that:
(1) the nitrogen-containing porous layered composite material loaded with the Ru nanoparticles has excellent catalytic performance (low overpotential and the like) and stability under an alkaline condition.
(2) According to the invention, zinc chloride and ruthenium chloride are used as effective activating-graphitizing agents, the biomass chitosan is pyrolyzed, and zinc is removed by hydrochloric acid etching, so that the nitrogen-containing porous layered material with high graphitization degree and a similar graphene structure is prepared.
(3) The preparation process is suitable for large-scale industrial production.
Drawings
FIG. 1 is a TEM image of a nitrogen-containing porous layered composite of example 4;
FIG. 2 is a Raman plot of the nitrogen-containing porous layered composites of examples 1-5;
FIG. 3 is a plot of examples 1-5 and comparative examples and commercial 20% Pt/C polarization;
FIG. 4 is a graph of the stability of example 4 and 20% Pt/C before and after 2000 cyclic voltammetry in 1M KOH.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
The reagents used in the examples are all commercially available reagents, no other treatment is performed, the calcination process is performed in a tube furnace, and the nitrogen used is high-purity nitrogen.
Example 1
0.3g of ZnCl is weighed2Dissolving in 20mL of deionized water to obtain ZnCl2Aqueous solution, and then 1.2g of chitosan and 0.913g of RuCl are respectively weighed3Dispersing in the solution to obtain a mixtureMixing the solution, placing the mixed solution in an oil bath kettle at the temperature of 80 ℃, stirring at constant temperature for 12 hours, removing water from the obtained substance by rotary evaporation, and drying; grinding the dried solid, putting the ground solid into a tube furnace, and heating at 3 ℃ for min under the protection of nitrogen-1The temperature rising rate is increased to 900 ℃ and the mixture is calcined for 1 hour, the solid powder obtained after calcination is added into 60mL of 1M hydrochloric acid, the mixture is stirred at constant temperature in an oil bath kettle at 120 ℃ and refluxed for 12 hours to obtain a solid, and the powder obtained after washing and suction filtration is dried to obtain the Ru-doped nitrogen-containing porous layered carbon material.
Example 2
0.3g of ZnCl is weighed2Dissolving in 20mL of deionized water to obtain ZnCl2Aqueous solution, and then 1.2g of chitosan and 0.73g of RuCl are respectively weighed3Dispersing in the solution to obtain a mixed solution, placing the mixed solution in an oil bath kettle at the temperature of 80 ℃, stirring at constant temperature for 12 hours, removing water from the obtained substance by rotary evaporation, and drying; grinding the dried solid, putting the ground solid into a tube furnace, and heating at 3 ℃ for min under the protection of nitrogen-1The temperature rising rate is increased to 900 ℃ and the mixture is calcined for 1 hour, the solid powder obtained after calcination is added into 60mL of 1M hydrochloric acid, the mixture is stirred at constant temperature in an oil bath kettle at 120 ℃ and refluxed for 12 hours to obtain a solid, and the powder obtained after washing and suction filtration is dried to obtain the Ru-doped nitrogen-containing porous layered carbon material.
Example 3
0.3g of ZnCl is weighed2Dissolving in 20mL of deionized water to obtain ZnCl2Aqueous solution, then 1.2g of chitosan and 0.55g of RuCl are respectively weighed3Dispersing in the solution to obtain a mixed solution, placing the mixed solution in an oil bath kettle at the temperature of 80 ℃, stirring at constant temperature for 12 hours, removing water from the obtained substance by rotary evaporation, and drying; grinding the dried solid, putting the ground solid into a tube furnace, and heating at 3 ℃ for min under the protection of nitrogen-1The temperature rising rate is increased to 900 ℃ and the mixture is calcined for 1 hour, the solid powder obtained after calcination is added into 60mL of 1M hydrochloric acid, the mixture is stirred at constant temperature in an oil bath kettle at 120 ℃ and refluxed for 12 hours to obtain a solid, and the powder obtained after washing and suction filtration is dried to obtain the Ru-doped nitrogen-containing porous layered carbon material.
Example 4
0.3g of ZnCl is weighed2Dissolving in 20mL of deionized water to obtain ZnCl2Aqueous solution, then 1.2g of chitosan and 0.38g of RuCl are respectively weighed3Dispersing in the solution to obtain a mixed solution, placing the mixed solution in an oil bath kettle at the temperature of 80 ℃, stirring at constant temperature for 12 hours, removing water from the obtained substance by rotary evaporation, and drying; grinding the dried solid, putting the ground solid into a tube furnace, and heating at 3 ℃ for min under the protection of nitrogen-1The temperature rising rate is increased to 900 ℃ and the mixture is calcined for 1 hour, the solid powder obtained after calcination is added into 60mL of 1M hydrochloric acid, the mixture is stirred at constant temperature in an oil bath kettle at 120 ℃ and refluxed for 12 hours to obtain a solid, and the powder obtained after washing and suction filtration is dried to obtain the Ru-doped nitrogen-containing porous layered carbon material.
Example 5
0.3g of ZnCl is weighed2Dissolving in 20mL of deionized water to obtain ZnCl2Aqueous solution, then 1.2g of chitosan and 0.18g of RuCl are respectively weighed3Dispersing in the solution to obtain a mixed solution, placing the mixed solution in an oil bath kettle at the temperature of 80 ℃, stirring at constant temperature for 12 hours, removing water from the obtained substance by rotary evaporation, and drying; grinding the dried solid, putting the ground solid into a tube furnace, and heating at 3 ℃ for min under the protection of nitrogen-1The temperature rising rate is increased to 900 ℃ and the mixture is calcined for 1 hour, the solid powder obtained after calcination is added into 60mL of 1M hydrochloric acid, the mixture is stirred at constant temperature in an oil bath kettle at 120 ℃ and refluxed for 12 hours to obtain a solid, and the powder obtained after washing and suction filtration is dried to obtain the Ru-doped nitrogen-containing porous layered carbon material.
Comparative example
0.3g of ZnCl is weighed2Dissolving in 20mL of deionized water to obtain ZnCl2Aqueous solution, then 1.2g of chitosan and 0g of RuCl are respectively weighed3Dispersing in the solution to obtain a mixed solution, placing the mixed solution in an oil bath kettle at the temperature of 80 ℃, stirring at constant temperature for 12 hours, removing water from the obtained substance by rotary evaporation, and drying; grinding the dried solid, putting the ground solid into a tube furnace, and heating at 3 ℃ for min under the protection of nitrogen-1The temperature rising rate of the reaction solution is increased to 900 ℃, the mixture is calcined for 1 hour, and solid powder obtained after calcination is added into 60mLStirring in a 120 ℃ oil bath kettle at constant temperature in 1M hydrochloric acid, refluxing for 12 hours to obtain a solid, washing with water, and carrying out suction filtration to obtain powder, and drying to obtain the Ru-doped nitrogen-containing porous layered carbon material.
In order to verify the catalytic performance of the present invention, the inventors have studied the catalytic performance of the nitrogen-containing porous layered material supporting active sites, and the prepared carbon material not supporting active sites and a commercial 20% Pt/C electrode are illustrated as comparative examples. All electrocatalytic tests the electrocatalytic performance of the samples of examples 1-5, comparative example and commercial 20% Pt/C was studied at room temperature in 1M KOH medium using a standard three electrode system.
The tests of the electrocatalytic hydrogen evolution performance of all the composite materials were carried out at room temperature in a three-electrode system using an electrochemical workstation of the type Ivium vertex. A glassy carbon electrode (GCE, diameter: 3mm), a graphite rod and an Ag/AgCl (3.5M KCl) electrode were used as a working electrode, a counter electrode and a reference electrode, respectively. All test data were converted to standard hydrogen electrodes and IR corrected for, the formula:
ERHE＝EAg/AgCl+E0 Ag/AgCl+0.0591×pH-IR
wherein: eRHEIs a standard hydrogen overpotential (V); eAg/AgClThe measured electrode potential (V); e0 Ag/AgClStandard electrode potential (0.205V) for Ag/AgCl electrodes; i is scanning real-time current (A), and R is a conversion resistor (omega).
Treatment of Glassy Carbon Electrode (GCE): using Al of 0.3 μm and 0.05 μm on the flannelette respectively2O3Polishing the working electrode by the powder, then respectively ultrasonically cleaning in ethanol and ultrapure water, and finally naturally drying.
Preparation of sample slurry: accurately weighed 3.0mg of the sample (20 wt% Pt/C), dispersed in 1mL of a deionized water/isopropanol (v/v ═ 4: 1) mixed solvent along with 30 μ L of a 5 wt% Nafion solution, and the mixed solution was sonicated for 30 minutes.
The electrolyte solution was 1M KOH (basic, pH 14) and the test voltage ranged from-1.6V to-0.9V. All electrochemical measurements were performed at room temperature under N2Saturated gasIs carried out in an atmosphere.
Preparation of a working electrode: mu.L of the catalyst ink was applied to a glassy carbon electrode (GCE: diameter d 3mm) by means of a pipette and allowed to dry naturally, the catalyst loading being 0.0425mg cm-2. And the corresponding test results are summarized in table 2.
When the current density reaches 10mA cm-2The overpotentials for examples 1-5 and comparative example and commercial 20% Pt/C were 78.2, 226.1, 53.7, 50.2, 118.1 and 472.6 and 37.2mV, respectively. It can also be seen that the catalyst without the addition of Ru element during the catalyst preparation performed poorly, and that other catalyst samples with the addition of Ru element showed better performance, especially that example four showed performance approaching commercial 20% Pt/C.
As shown in fig. 1, a layered highly porous structure can be observed in the SEM image of example 4, and it can also be seen that Ru nanoparticles are uniformly distributed on the carbon nanosheets. The inset in the SEM image is a histogram of the Ru nanoparticle size distribution, showing that the average Ru nanoparticle size is about 10 nm. The formation of the porous structure is mainly left by the removal of Zn. These types of surface structures are optimal for the proper function required by the electrocatalyst.
As shown in FIG. 2, the Raman spectra of examples 1-5 and comparative example show at 1348 and 1597cm in both samples-1Two distinct peaks nearby correspond to disordered carbon (D band) and ordered graphitic carbon (G band), respectively. Wherein the ID/IG intensity ratio is about 0.9, indicating that the degree of graphitization of the prepared carbon nanosheets is higher and comparable to that of graphene (ID/IG ═ 0.8). The carbon nanosheet prepared by the method has good conductivity, and the electrocatalytic performance of the catalytic material is improved.
As shown in FIG. 3, the polarization curve in 1M KOH solution is seen to show that examples 1-5 and comparative examples, as well as commercial 20% Pt/C, all exhibit an initial potential of almost zero. When the current density reaches 10mA cm-2The overpotentials for examples 1-5 and comparative example and commercial 20% Pt/C were 78.2, 226.1, 53.7, 50.2, 118.1 and 472.6 and 37.2mV, respectively. It can also be seen that the catalyst pair without the addition of Ru element during the catalyst preparation processThe proportional catalytic performance was poor and other example samples with added Ru showed better performance especially catalyst example 4 showed performance approaching commercial 20% Pt/C, indicating that Ru and its content are key factors affecting catalyst performance. When the current density reaches 50mA cm-2The overpotentials for examples 1-5 and commercial 20% Pt/C were 196.7, 506.1, 144.7, 135.8, 320.1, and 186.2mV, respectively. From this, it is found that the current density is higher (for example, 50mA cm)-2) The potential drops of examples 4 and 3 were 135.8mV, 144.7mV, respectively, less than the overpotential of 20% Pt/C (186.2mV) at 100mA cm-2Examples 4, 3 and 20% Pt/C were 186.0mV, 196.2mV and 316.2mV, respectively, showing better catalytic performance. Meanwhile, the performance of the catalyst is not consistent with the content of Ru, the phenomenon that the content of Ru is increased and then decreased is shown, and the catalytic performance is possibly influenced by the accumulation of Ru due to the excessive content of Ru.
As shown in FIG. 4, example 4 was circulated at 100mA cm after 2000 cycles-2The overpotential during the process is shifted negatively by 15.4mV, showing excellent stability. This weak attenuation is almost negligible under alkaline conditions.
Table 1 ECSA and catalytic activity of examples 1-5 and comparative examples
Samples Cdl(mF/cm2) CDL(mF) ECSA(cm2)
Comparative example 1.91 0.1337 6.685
Example 5 10.8 0.756 37.8
Example 4 32.35 2.2645 113.225
Example 3 31.66 2.2162 110.81
Example 2 10.31 0.7217 36.085
Example 1 12.97 0.9079 45.395
CDL＝Cdl×0.07cm2；ECSA＝CDL/Cs；Cs＝0.02mF·cm-2
TABLE 2 overpotentials for examples 1-5 and comparative examples at different current densities
Samples 10mA·cm-2 50mA·cm-2 100mA·cm-2
Comparative example 472.6 -- --
Example 5 118.1 320.1 --
Example 4 50.2 135.8 186.0
Example 3 53.7 144.7 196.2
Example 2 226.1 506.1 --
Example 1 78.2 196.7 276.0
Commercial 20% Pt/C 37.2 186.2 316.2
"- -" represents a numerical value too large

Claims (9)

1. A preparation method of a composite material for electrocatalytic hydrogen evolution of an alkaline solution is characterized by comprising the following steps:
step 1): with RuCl3Is active metal Ru source, chitosan is carbon and nitrogen source, ZnCl2Respectively weighing RuCl as an activating agent and a pore-forming agent3Chitosan, ZnCl2Dispersing the mixture in deionized water to obtain a mixed solution, stirring the mixed solution at a constant temperature for reaction, and drying the mixed solution to obtain a solid;
step 2): grinding the solid obtained in the step 1), putting the ground solid into a tube furnace, and calcining the solid in the tube furnace under the protection of inert gas to obtain solid powder;
step 3): adding the solid powder obtained in the step 2) into hydrochloric acid, etching under constant-temperature stirring, and performing suction filtration, washing and drying to obtain the composite material of the Ru nano particles loaded on the nitrogen-containing porous layered carbon material.
2. The process for the preparation of a composite material for the electrocatalytic hydrogen evolution of alkaline solutions according to claim 1, characterized in that in said step 1), ZnCl is used as the hydrogen evolution catalyst2The weight ratio of the chitosan to the chitosan is 1: 4; the weight ratio of the deionized water to the chitosan is (15-20): 1; the RuCl3The weight ratio of the chitosan to chitosan is (1-4.6): 6.
3. the method for the preparation of a composite material for the electrocatalytic hydrogen evolution in alkaline solutions according to claim 2, characterized in that said RuCl is such that it is a solid, liquid, or liquid3The weight ratio of the chitosan to the chitosan is 1: 3.
4. the method for preparing a composite material for the electrocatalytic hydrogen evolution of alkaline solutions according to claim 1, characterized in that the reaction temperature in step 1) is 80 ℃ and the time is 12 hours.
5. The method for preparing a composite material for the electrocatalytic hydrogen evolution in alkaline solutions according to claim 1, characterized in that the calcination temperature in step 2) is 900 ℃, the rate of temperature rise is 3 ℃/min and the calcination time is 1 hour.
6. The method for preparing a composite material for the electrocatalytic hydrogen evolution of alkaline solutions according to claim 1, characterized in that the concentration of hydrochloric acid in the step 3) is 1 mol/L.
7. The method for preparing the composite material for the electrocatalytic hydrogen evolution of the alkaline solution according to claim 1 or 6, wherein the weight ratio of the solid powder to the hydrochloric acid in the step 3) is (1-5): 120.
8. the method for preparing a composite material for the electrocatalytic hydrogen evolution from alkaline solutions according to claim 1, wherein the etching temperature in step 3) is 120 ℃ and the etching time is 12 hours.
9. A composite material for alkaline solution electrocatalytic hydrogen evolution prepared by the method for preparing a composite material for alkaline solution electrocatalytic hydrogen evolution according to any one of claims 1 to 8.
CN202111148795.7A 2021-09-29 2021-09-29 Composite material for electrocatalytic hydrogen evolution of alkaline solution and preparation method thereof Withdrawn CN113921836A (en)

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