CN113193206A - Preparation method of anode catalyst of ethanol fuel cell - Google Patents

Preparation method of anode catalyst of ethanol fuel cell Download PDF

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Publication number
CN113193206A
CN113193206A CN202110326200.6A CN202110326200A CN113193206A CN 113193206 A CN113193206 A CN 113193206A CN 202110326200 A CN202110326200 A CN 202110326200A CN 113193206 A CN113193206 A CN 113193206A
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fuel cell
anode catalyst
ethanol fuel
carbon cloth
bismuth
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袁小磊
黄嘉禄
杨虎
单秋磊
曹子轩
魏丛宇
徐文静
蒲岚
曹宇锋
华平
姚勇
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Nantong University
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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
    • H01M4/88—Processes of manufacture
    • H01M4/8825—Methods for deposition of the catalytic active composition
    • H01M4/8853—Electrodeposition
    • 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
    • H01M4/8825—Methods for deposition of the catalytic active composition
    • 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
    • H01M4/9041—Metals or alloys
    • 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
    • H01M4/9041—Metals or alloys
    • H01M4/905—Metals or alloys specially used in fuel cell operating at high temperature, e.g. SOFC
    • H01M4/9058—Metals or alloys specially used in fuel cell operating at high temperature, e.g. SOFC of noble metals or noble-metal based alloys
    • 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
    • H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
    • 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
    • H01M4/92—Metals of platinum group
    • H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
    • H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
    • H01M8/1011—Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
    • H01M8/1013—Other direct alcohol fuel cells [DAFC]
    • 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 provides a preparation method of an anode catalyst of an ethanol fuel cell, which comprises the following steps: s10, dissolving a certain amount of surfactant in deionized water to obtain a reaction solvent; s20, dissolving a precursor palladium salt and a precursor bismuth salt in a reaction solvent according to a preset molar ratio to obtain an electrolyte; s30 cutting a certain area of conductive carbon cloth; s40 at a certain potential for a certain time, performing electro-deposition, oxidation and reduction on palladium ions and bismuth ions in the electrolyte to conductive carbon cloth by using a chronoamperometry to obtain the load PdnConductive carbon cloth Pd of Bi alloy nano particlesnBi/CC，PdnBi/CC is an anode catalyst of the ethanol fuel cell. The invention relates to a preparation method of an ethanol fuel cell anode catalyst, which uses an electrodeposition method to electrodeposit, oxidize and reduce palladium ions and bismuth ions onto conductive carbon cloth,the anode catalyst of the ethanol fuel cell is obtained, the integral preparation method is simple, and the nucleation and growth of metal nano particles with different sizes, shapes and distributions are easy to control.

Description

Preparation method of anode catalyst of ethanol fuel cell
Technical Field
The invention relates to the technical field of new energy, in particular to a preparation method of an anode catalyst of an ethanol fuel cell.
Background
Direct Ethanol Fuel Cells (DEFCs) are electrochemical reaction devices that convert the chemical energy of ethanol liquid fuel directly into electrical energy. In order to obtain desirable cell performance, Pt-based electrocatalysts are currently used in many cases. However, the natural reserves of Pt are limited and, due to their widespread use in industry, they are becoming more and more expensive. The best way to reduce the amount of Pt is to find alternative materials that not only reduce the Pt dependence of fuel cells, but also reduce the cost and thus promote the commercialization of DEFC. The palladium has lower price than platinum and relatively abundant reserves, and has unique performance in the electrochemical fields of low-temperature fuel cells, electrolysis, sensors and the like, so that the palladium is expected to become a substitute material for the platinum.
However, from the fuel cell perspective, the price is not the primary reason Pd can replace Pt. The real attraction is that Pd has better performance than a Pt-based electrocatalyst in an alkaline environment, but in the alkaline environment, both an anode and a cathode can use a non-Pt catalyst, and if Pd is doped or modified to increase the activity of Pd and stably catalyze alcohol oxidation, the application of the catalyst in a direct ethanol fuel cell is greatly promoted.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of an anode catalyst of an ethanol fuel cell, which comprises the step of carrying out electro-deposition oxidation reduction on palladium ions and bismuth ions on conductive carbon cloth by using an electro-deposition method to obtain supported PdnConductive carbon cloth Pd of Bi alloy nano particlesnBi/CC，PdnThe Bi/CC anode catalyst of the ethanol fuel cell has simple integral preparation method and is easy to control the nucleation and the growth of metal nano particles with different sizes, shapes and distributions.
In order to achieve the above purpose, the invention adopts a technical scheme that:
a preparation method of an ethanol fuel cell anode catalyst comprises the following steps: s10, dissolving a certain amount of surfactant in deionized water to obtain a reaction solvent; s20, dissolving a precursor palladium salt and a precursor bismuth salt in a reaction solvent according to a preset molar ratio to obtain an electrolyte; s30 cutting a certain area of conductive carbon cloth; s40 at a certain potential for a certain time, performing electro-deposition, oxidation and reduction on palladium ions and bismuth ions in the electrolyte to conductive carbon cloth by using a chronoamperometry to obtain the load PdnConductive carbon cloth of Bi alloy nano particles, namely PdnBi/carbon cloth(PdnBi/CC)，PdnBi/CC is an ethanol fuel cell anode catalyst, wherein n is [0.5,10 ]]。
Further, the surfactant is Ethylene Diamine Tetraacetic Acid (EDTA), and the concentration of the EDTA in the reaction solvent is not less than 0.5 mol/L.
Furthermore, the concentration of palladium ions in the electrolyte is 0.02-0.08mol/L, and the concentration of bismuth ions is 0.02-0.08 mol/L.
Further, the molar ratio of palladium ions to bismuth ions in the electrolyte is (0.5-10): 1.
Further, the precursor palladium salt is at least one of chloropalladate or potassium chloropalladite.
Further, the precursor bismuth salt is at least one of bismuth neododecanoate or bismuth nitrate pentahydrate.
Further, the fixed potential required for the electrodeposition in the step S40 is-0.297V, and the time required for the electrodeposition is 100-.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) the invention relates to a preparation method of an ethanol fuel cell anode catalyst, which comprises the step of carrying out electro-deposition oxidation reduction on palladium ions and bismuth ions on conductive carbon cloth by using an electro-deposition method to obtain loaded PdnConductive carbon cloth Pd of Bi alloy nano particlesnBi/CC，PdnThe Bi/CC anode catalyst of the ethanol fuel cell has simple integral preparation method and is easy to control the nucleation and the growth of metal nano particles with different sizes, shapes and distributions.
(2) According to the preparation method of the anode catalyst of the ethanol fuel cell, the anode catalyst obtained through electrodeposition can improve the toxicity resistance of CO through the synergistic effect of two metals, and finally improve the activity and stability of the anode catalyst in catalyzing ethanol oxidation.
Drawings
The technical solution and the advantages of the present invention will be apparent from the following detailed description of the embodiments of the present invention with reference to the accompanying drawings.
FIG. 1 is a flow chart of a method for preparing an anode catalyst for an ethanol fuel cell according to an embodiment of the present invention;
FIG. 2 is a scanning electron microscope of an anode catalyst of an ethanol fuel cell according to an embodiment of the present invention;
FIG. 3 is an X-ray diffraction pattern of an anode catalyst for an ethanol fuel cell in accordance with an embodiment of the present invention;
FIG. 4 is an X-ray photoelectron spectrum of an anode catalyst of an ethanol fuel cell according to an embodiment of the present invention;
FIG. 5 is a graph showing the catalytic activity cyclic voltammograms of ethanol oxidation reaction of the anode catalysts of the ethanol fuel cells obtained in examples 1 and 4 of the present invention;
FIG. 6 is a graph showing the current curves of the anode catalysts of ethanol fuel cells obtained in examples 1 and 4 of the present invention when measuring the catalytic activity of ethanol oxidation reaction.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment provides a preparation method of an anode catalyst of an ethanol fuel cell, as shown in fig. 1 to 4, comprising the following steps: s10 dissolving a certain amount of surfactant in deionized water to obtain a reaction solvent. S20, dissolving a precursor palladium salt and a precursor bismuth salt in a reaction solvent according to a preset molar ratio to obtain an electrolyte; s30 cutting a certain area of conductive carbon cloth; s40 at a certain potential for a certain time, performing electro-deposition, oxidation and reduction on palladium ions and bismuth ions in the electrolyte to conductive carbon cloth by using a chronoamperometry to obtain the load PdnConductive carbon cloth of Bi alloy nano particles, namely PdnBi/carbon cloth(PdnBi/CC)，PdnBi/CC is an ethanol fuel cell anode catalyst, wherein n is [0.5,10 ]]。
In step S10, the surfactant is Ethylene Diamine Tetraacetic Acid (EDTA), and the concentration of EDTA in the reaction solvent is not less than 0.5 mol/L.
In step S20, the concentration of palladium ions in the electrolyte is 0.02-0.08mol/L, the concentration of bismuth ions is 0.02-0.08mol/L, and the molar ratio of palladium ions to bismuth ions in the electrolyte is (0.5-10): 1. The precursor palladium salt is at least one of chloropalladate or potassium chloropalladite, and the precursor bismuth salt is at least one of bismuth neododecanoate or bismuth nitrate pentahydrate.
The fixed potential required for electrodeposition in step S40 was-0.297V and the time required for electrodeposition was 100-.
Example 1
The preparation method of the anode catalyst of the ethanol fuel cell comprises the following steps
S10, dissolving 1.46g of surfactant in 100mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a reaction solvent;
s20, dissolving chloropalladate and bismuth nitrate pentahydrate in a molar ratio of 5:1 in 50mL of reaction solvent, and carrying out ultrasonic treatment for 30min to obtain an electrolyte, wherein the concentrations of palladium ions and bismuth ions in the electrolyte are both 0.02 mol/L;
s30 cutting a 2cm multiplied by 2cm conductive carbon cloth;
s40, a three-electrode system is built, conductive carbon cloth is fixed on a working electrode and is immersed in electrolyte, and electrodeposition is carried out through a chronoamperometric method. The fixed potential required by the electrodeposition is-0.297V (relative to a saturated calomel electrode, SCE), the deposition time is 2000s, the conductive carbon cloth after the electrodeposition is cleaned and dried to obtain the Pd5Conductive carbon cloth of Bi alloy nanoparticles, i.e. Pd5Bi/CC。
When the anode catalyst of the ethanol fuel cell obtained in example 1 is observed by a Scanning Electron Microscope (SEM), as shown in fig. 2, the anode catalyst of the ethanol fuel cell has a granular structure and has a rim at the periphery.
When the anode catalyst of the ethanol fuel cell was scanned by an X-ray diffractometer, as shown in fig. 3, it can be seen that all XRD spectrum peaks correspond to the face-centered cubic phase (JCPDF,46-1043) of Pd, in which diffraction peaks 2 θ of 43.4 °, 52.9 ° and 78.9 ° can be indexed as (111), (200) and (311) planes of pure Pd.
Further using X-ray photoelectron spectroscopy to detect the valence states of the components of Bi in the anode catalyst of the ethanol fuel cell, as shown in FIG. 4, for Bi element, a pair of peak patterns appeared at 159.6eV and 164.7eV, which can be attributed to Bi (OH)3Thus, it was confirmed that Bi (OH) was produced as described above3The modified Pd nano-particles are Pd5A Bi/CC catalyst.
Ethanol Oxidation Reaction (EOR) catalytic activity test:
(1) EOR testing
1mol/L NaOH +1mol/L C saturated at Ar2H5EOR measurements were performed in OH at a scan rate of 50 mV/s. At a concentration of 1mol/L C2H5OH in a 1mol/L NaOH solution at-0.2V (vs. saturated calomel electrode, SCE),the long term stability of the prepared samples was measured by chronoamperometry. For comparison, the same preparation procedure and test method were used for the Pd/CC catalyst.
Pd obtained in example 15The EOR performance of the Bi/CC catalysts was tested in a tripolar cell system using the Chenghua CHI660e workstation. In a three-electrode system, a saturated calomel electrode and a Pt net are respectively used as a reference electrode and a counter electrode.
FIG. 5 shows Pd in example 15Bi/CC catalyst in the presence of 1mol/L C2H5In a 1mol/L NaOH solution of OH, the potential range is-0.8V-0.2V (relative to a saturated calomel electrode, SCE), and the sweep rate is 50mV/s of cyclic voltammograms. From FIG. 5, Pd5EOR activity of the Bi/CC catalyst was 23.54mA cm-2In contrast, the Pd/CC catalyst had an activity of only 8.07mA cm-2。
FIG. 6 shows Pd in example 15The Bi/CC catalyst is added in a catalyst containing 1mol/L C2H5In a 1mol/L NaOH solution of OH, under the condition of a potential of-0.2V (relative to a saturated calomel electrode, SCE), the potential changes after 3600 s. From FIG. 6, it can be concluded that Pd after 3600s stability test5The activity of the Bi/CC catalyst is reduced by 70 percent. In contrast, after stability test of Pd/CC, 3600s, the activity is reduced by 90%, and the activity is nearly close to 0, namely the activity is lost.
Example 2
The preparation method of the anode catalyst of the ethanol fuel cell comprises the following steps
S10, dissolving 1.46g of surfactant in 100mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a reaction solvent;
s20, dissolving potassium chloropalladite and bismuth nitrate pentahydrate in a molar ratio of 10:1 in 50mL of reaction solvent, and performing ultrasonic treatment for 30min to obtain electrolyte;
s30 cutting a 2cm multiplied by 2cm conductive carbon cloth;
s40, a three-electrode system is built, conductive carbon cloth is fixed on a working electrode and is immersed in electrolyte, and electrodeposition is carried out through a chronoamperometric method. The fixed potential required for electrodeposition was-0.297V (vs. saturated calomel electrode, SCE) and the deposition time was 2000s, cleaning the conductive carbon cloth after electrodeposition and airing to obtain the Pd-containing conductive carbon cloth10Conductive carbon cloth of Bi alloy nanoparticles, i.e. Pd10Bi/CC。
Example 3
The preparation method of the anode catalyst of the ethanol fuel cell comprises the following steps
S10, dissolving 1.46g of surfactant in 100mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a reaction solvent;
s20, dissolving potassium chloropalladite and bismuth neododecanoate in a molar ratio of 5:1 in 50mL of reaction solvent, and carrying out ultrasonic treatment for 30min to obtain electrolyte, wherein the concentrations of palladium ions and bismuth ions in the electrolyte are both 0.08 mol/L;
s30 cutting a 2cm multiplied by 2cm conductive carbon cloth;
s40, a three-electrode system is built, conductive carbon cloth is fixed on a working electrode and is immersed in electrolyte, and electrodeposition is carried out through a chronoamperometric method. The fixed potential required by the electrodeposition is-0.297V (relative to a saturated calomel electrode, SCE), the deposition time is 100s, the conductive carbon cloth after the electrodeposition is cleaned and dried to obtain the Pd5Conductive carbon cloth of Bi alloy nanoparticles, i.e. Pd5Bi/CC。
Example 4
The preparation method of the anode catalyst of the ethanol fuel cell comprises the following steps
S10, dissolving 1.46g of surfactant in 100mL of deionized water, and carrying out ultrasonic treatment for 30min to obtain a reaction solvent;
s20, dissolving chloropalladate and bismuth neododecanoate in a molar ratio of 0.5:1 in 50mL of reaction solvent, and carrying out ultrasonic treatment for 30min to obtain electrolyte, wherein the concentrations of palladium ions and bismuth ions in the electrolyte are both 0.08 mol/L;
s30 cutting a 2cm multiplied by 2cm conductive carbon cloth;
s40, a three-electrode system is built, conductive carbon cloth is fixed on a working electrode and is immersed in electrolyte, and electrodeposition is carried out through a chronoamperometric method. The fixed potential required by the electrodeposition is-0.297V (relative to a saturated calomel electrode, SCE), the deposition time is 5000s, the conductive carbon cloth after the electrodeposition is cleaned and dried to obtain the Pd0.5Bi alloy nanoparticlesOf conductive carbon cloth, i.e. Pd0.5Bi/CC。
The above description is only an exemplary embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent structures or equivalent processes that are transformed by the content of the present specification and the attached drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (7)

1. The preparation method of the anode catalyst of the ethanol fuel cell is characterized by comprising the following steps
S10, dissolving a certain amount of surfactant in deionized water to obtain a reaction solvent;
s20, dissolving a precursor palladium salt and a precursor bismuth salt in a reaction solvent according to a preset molar ratio to obtain an electrolyte;
s30 cutting a certain area of conductive carbon cloth;
s40 at a certain potential for a certain time, performing electro-deposition, oxidation and reduction on palladium ions and bismuth ions in the electrolyte to conductive carbon cloth by using a chronoamperometry to obtain the load PdnConductive carbon cloth of Bi alloy nano particles, namely PdnBi/carbon cloth(PdnBi/CC)，PdnBi/CC is an ethanol fuel cell anode catalyst, wherein n is [0.5,10 ]]。
2. The method of claim 1, wherein the surfactant is ethylenediaminetetraacetic acid (EDTA), and the concentration of EDTA in the reaction solvent is not less than 0.5 mol/L.
3. The method of claim 1, wherein the concentration of palladium ions in the electrolyte is 0.02 to 0.08mol/L, and the concentration of bismuth ions in the electrolyte is 0.02 to 0.08 mol/L.
4. The method for preparing an anode catalyst for an ethanol fuel cell according to claim 1, wherein the molar ratio of palladium ions to bismuth ions in the electrolyte is (0.5-10): 1.
5. The method for preparing an anode catalyst for an ethanol fuel cell according to claim 1, wherein the precursor palladium salt is at least one of chloropalladic acid or potassium chloropalladite.
6. The method for preparing the anode catalyst of the ethanol fuel cell according to claim 1, wherein the precursor bismuth salt is at least one of bismuth neododecanoate or bismuth nitrate pentahydrate.
7. The method as claimed in claim 1, wherein the fixed potential required for electrodeposition in step S40 is-0.297V and the time required for electrodeposition is 100-.
CN202110326200.6A 2021-03-26 2021-03-26 Preparation method of anode catalyst of ethanol fuel cell Pending CN113193206A (en)

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