CN111180750B - AgPdIr nano alloy and preparation and use method thereof - Google Patents
AgPdIr nano alloy and preparation and use method thereof Download PDFInfo
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Abstract
The invention relates to an AgPdIr nano alloy and a preparation and use method thereof. The AgPdIr ternary nano alloy is used as a catalyst, so that the catalytic activity and stability of the formate oxidation reaction are improved, the initial potential and the peak potential position of the formate oxidation reaction are moved to the negative potential direction, and the discharge voltage and the energy efficiency of the direct formate fuel cell are improved. The AgPdIr nano alloy is used as a formate oxidation reaction catalyst, the initial potential of the formate oxidation reaction is 0.16-0.2V, the peak potential is 0.5-0.8V, and the potential is referred to a reversible hydrogen electrode. The catalytic activity of the formate oxidation reaction is 2.09-5.14 A.mg ‑1 Pd The catalytic activity of the formate oxidation reaction is 0.82 to 1.54A. mg after a 4000s durability test ‑1 Pd 1.29-3.17 times and 7.45-14 times the activity and durability of the commercial Pd/C.
Description
Technical Field
The invention belongs to the technical field of fuel cells, relates to an AgPdIr nano alloy and preparation and use methods thereof, and particularly relates to an anode catalyst for a direct formate fuel cell and a preparation method thereof.
Background
With the growing energy crisis and environmental deterioration problems, it has been urgent to develop a clean new energy source to replace the conventional fossil fuel. The direct formate fuel cell is a green and efficient energy conversion device, and has the advantages of no toxicity, high conversion efficiency, good safety and the like. In general, the alkaline condition of the working environment of the direct formic acid fuel cell, the oxidation reaction of formate occurs at the anode, and the reduction reaction of oxygen occurs at the cathode, and the theoretical voltage and the theoretical power density of the direct formic acid fuel cell are higher than those of other types of fuel cells. Therefore, in recent years, the research of direct formate fuel cells has received increasing attention.
At present, the problem of restricting the development of the direct formate fuel cell is that a formate oxidation reaction catalyst with high catalytic activity and good stability is lacked. Currently, the formate oxidation catalysts widely used are commercial Pt/C or Pd/C. The Pt/C catalyst has low catalytic activity for formate oxidation reaction and is easy to generate poisoning phenomenon in the catalytic reaction process. Compared with Pt/C, the commercial Pd/C catalyst has low price, high catalytic activity and no poisoning phenomenon, and becomes a research hotspot of formate oxidation reaction catalysts. However, the metallic Pd surface has a strong binding energy for the adsorbed hydrogen generated during the formate oxidation reaction. The intermediate hydrogen adsorbed on the surface of Pd occupies the catalytic active sites of Pd/C, so that the catalytic activity of the intermediate hydrogen rapidly decreases, resulting in poor stability. Therefore, in order to accelerate the commercialization of direct formate fuel cells, the development of Pd-based catalysts with higher catalytic activity and stability is required.
Generally, the main method for improving the catalytic activity and stability of Pd-based catalysts for formate oxidation reactions is alloying. The novel Pd-based nano alloy catalyst is formed by combining metal Pd with other different types of metals, so that the catalytic activity and the stability of the Pd-based formate oxidation reaction catalyst are improved.
Chinese invention patent CN107017409A discloses a combined production of an alkali salt and a direct formate fuel cell. In such cell systems, PdAu bimetallic metals are used as anode catalysts in place of conventional Pt-based catalysts. Although PdAu bimetallic catalysts reduce the cost of the cell, the cost remains high.
Chinese patent CN108417854A discloses a high-efficiency silver-palladium nano-alloy formate oxidation reaction electrocatalyst and a preparation method thereof. The AgPd nano alloy provided by the invention ensures the oxidation catalytic activity of high-efficiency formate, and simultaneously improves the Pd poisoning problem through the alloying of Ag, thereby improving the stability of the catalytic material and prolonging the service life of the material.
Chinese invention patent CN108746659A discloses a flower-shaped AgPd nano alloy and a preparation and use method thereof. In the invention, the Apzc is used as a morphology control agent to synthesize the flower-shaped AgPd nano-alloy catalyst, and the excellent catalytic activity and stability are shown.
The Chinese invention patent CN108598508A discloses an AgPd nano-alloy formate oxidation catalyst and a treatment method for improving catalytic activity without a surfactant. The invention provides an in-situ electrochemical potential cycling method for improving the oxidation catalytic activity of the Ag-Pd nano alloy formate on the basis of the alloyed Pd-based nano catalyst.
In summary, despite the extensive research on Pd-based bimetallic nanoalloy formate oxidation catalysts, the current Pd-based nanoalloys suffer from the following drawbacks: the initial potential of the formate oxidation reaction is low, the peak potential of the formate oxidation reaction is biased to the positive potential direction, and when the direct formate fuel cell works, the output voltage of the cell is low, and the fuel conversion efficiency is not high.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides an AgPdIr nano alloy and a preparation and use method thereof, which overcome the defects of a Pd-based nano formate oxidation reaction catalyst in the prior art.
Technical scheme
An AgPdIr nanoalloy, which is characterized in that: adding Ir into AgPd nano alloy to form an AgPdIr ternary nano alloy catalyst, wherein the shape of the AgPdIr ternary nano alloy catalyst is a three-dimensional porous spherical structure assembled by nanocrystals, and the AgPd ternary nano alloy catalyst is characterized in that: the atomic percentage ranges of the components are Ag: 23-46, Pd: 49-73, Ir: 1 to 8.
The diameter of the ball in the three-dimensional porous spherical structure is 30-100 nanometers.
The size of the nanocrystal is 3-7 nanometers.
The method for preparing the AgPdIr nano alloy is characterized by comprising the following steps:
step 2: the concentration is 0.01 mol.L -1 Sequentially adding 0.2-0.3 mL of sodium chloropalladate, 0.12-0.32 mL of chloroiridic acid and 0.1-0.2 mL of silver nitrate precursor solution into the cetylpyridinium chloride solution obtained in the step 1, and stirring for 10-15 minutes to uniformly mix the materials
And step 3: adding an ascorbic acid solution into the solution obtained in the step 2, stopping stirring, and standing and reacting for 2-4 hours at the temperature of 25-50 ℃;
and 4, step 4: processing the solution in the step 3 through centrifugal separation, deionized water cleaning and freeze drying to obtain the AgPdIr nano alloy formate oxidation reaction catalyst;
the proportion of each component in the reaction is each part, and is multiplied according to the requirement.
The use method of the AgPdIr nano alloy is characterized by comprising the following steps: the AgPdIr nano alloy is used as a formate oxidation reaction catalyst, the initial potential of the formate oxidation reaction is 0.16-0.2V, the peak potential is 0.5-0.8V, and the potential is referred to a reversible hydrogen electrode. The catalytic activity of the formate oxidation reaction is 2.09-5.14 A.mg -1 Pd The catalytic activity of the formate oxidation reaction is 0.82 to 1.54A. mg after a 4000s durability test -1 Pd 1.29-3.17 times and 7.45-14 times the activity and durability of the commercial Pd/C.
Advantageous effects
The AgPdIr nano alloy and the preparation and use method thereof provided by the invention are characterized in that Ir is added into the AgPd nano alloy to form the AgPdIr ternary nano alloy. The AgPdIr ternary nano alloy is used as a catalyst, so that the catalytic activity and stability of the formate oxidation reaction are improved, the initial potential and the peak potential position of the formate oxidation reaction are moved to the negative potential direction, and the discharge voltage and the energy efficiency of the direct formate fuel cell are improved.
In the invention, the AgPdIr ternary nano-alloy catalyst has excellent catalytic activity and stability, and the attached figure 2 shows that the AgPdIr ternary nano-alloy catalyst and the commercialized Pd/C have N in the presence of N 2 From the cyclic voltammetry curve in the saturated 1M KOH +1M KCOOH solution, the catalytic activity of the AgPdIr ternary nano-alloy catalyst is higher than that of the commercial Pd/C catalyst, and the catalyst is represented by a negative-shifted initial potential and a negative-shifted peak potential. The current density of the AgPdIr ternary nano-alloy catalyst is 5.14 A.mg at 0.5V (vs RHE) -1 Pd 3.17 times that of commercial Pd/C. FIG. 3 shows the long-range durability test of the AgPdIr ternary nano-alloy catalyst on formate oxidation reaction, and the test result shows that under the test condition that the potential is 0.624V (vs RHE), the current density of the formate oxidation reaction is still 347 mA-mg after 20000s long-time test -1 Pd . FIG. 4 shows the regeneration capacity of the AgPdIr ternary nanoalloy catalyst for formate oxidation reactions. As can be seen from the figure, after the 4000s test process is finished, the AgPdIr ternary nano-alloy catalyst is cleaned by deionized water and is put into new electrolyte, and formate of the catalyst is obtainedThe oxidation reaction activity is restored to the initial state. Fig. 5 shows a cycle stability test of the AgPdIr ternary nano-alloy catalyst on formate oxidation reaction, and it can be known from the test result that after 500 cycles, the formate oxidation reaction activity is 41% of the initial value.
Drawings
FIG. 1: preparation flow chart of AgPdIr ternary nano-alloy catalyst
FIG. 2: different kinds of catalysts in N 2 Cyclic voltammetry curves in a saturated 1M KOH +1M KCOOH solution, wherein a curve 1 in the figure is a cyclic voltammetry curve of an AgPdIr ternary nano-alloy catalyst; curve 2 is the cyclic voltammogram of commercial Pd/C.
FIG. 3: the long-range durability test of the formate oxidation reaction of the AgPdIr ternary nano alloy catalyst adopts a time-current curve as a test means, the test potential is 0.624V (vs RHE), and the test time is 20000 s.
FIG. 4: the regeneration capability of the AgPdIr ternary nano alloy catalyst on formate oxidation reaction is tested, the test means is a time-current curve, the test potential is 0.624V (vs RHE), and the test time is 4000 s. Curve 1 is the 1 st time-current curve, curve 2 is the 2 nd time-current curve, curve 3 is the 3 rd time-current curve, and curve 4 is the 4 th time-current curve.
FIG. 5: and (3) testing the cycling stability of the AgPdIr ternary nano alloy catalyst by adopting a cyclic voltammetry curve with a scanning rate of 50 mV/s. Curve 1 is the cyclic voltammetry curve of circle 1; curve 2 is the cyclic voltammogram at turn 200; curve 3 is the cyclic voltammogram at turn 500.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
the main components of the formate oxidation reaction electrocatalyst are Ag, Pd and Ir, and the atomic percentage ranges of the components are Ag: 23-46, Pd: 49-73, Ir: 1-8. The AgPdIr nano alloy is a single-phase solid solution alloy. The AgPdIr nano alloy has a three-dimensional porous spherical structure assembled by nanocrystals, the diameter of the sphere is 30-100 nanometers, and the size of the nanocrystals is 3-7 nanometers.
The AgPdIr nano alloy is used as a catalyst for formate oxidation reaction, the initial potential of the formate oxidation reaction is 0.16-0.2V (vs RHE), the peak potential is 0.5-0.8V (vs RHE), and the catalytic activity of the formate oxidation reaction is 2.09-5.14A. mg -1 Pd The catalytic activity of the formate oxidation reaction is 0.82 to 1.54A. mg after a 4000s durability test -1 Pd 1.29-3.17 times and 7.45-14 times the activity and durability of the commercial Pd/C.
The specific embodiment is as follows:
example 1
Dissolving 18mg of cetylpyridinium chloride surfactant in 5mL of deionized water, sonicating for 10 minutes, and stirring for 10 minutes to form an aqueous cetylpyridinium chloride solution. 0.267mL of sodium chloropalladate (0.01 mol. L) are taken in turn respectively -1 ) 0.12mL of chloroiridic acid (0.01 mol. L) -1 ) And 0.13mL silver nitrate (0.01 mol. L) -1 ) The aqueous solution was added dropwise to the aqueous solution of cetylpyridinium chloride obtained above, and stirred for 10 minutes to form an aqueous precursor solution. 0.3mL of the solution was prepared at a concentration of 0.1 mol. L -1 Quickly dripping the ascorbic acid aqueous solution into the precursor aqueous solution, stopping stirring, and standing for reaction for 3 hours at the temperature of 35 ℃. After the reaction is finished, centrifuging the obtained black solution, washing the black solution with deionized water for three times, and finally freeze-drying the black solution for 12 hours to obtain the final Ag 32 Pd 66 Ir 2 A ternary nano-alloy catalyst. In N 2 Electrochemical test results in saturated 1M KOH +1M KCOOH solutions showed that Ag was present at 0.5V (vs RHE) 32 Pd 66 Ir 2 The current density of the ternary nano-alloy catalyst for the oxidation reaction of the formate is 1.29 times that of the commercial Pd/C catalyst.
Example 2
Dissolving 18mg of cetylpyridinium chloride surfactant in 5mL of deionized water, sonicating for 10 minutes, and stirring for 10 minutes to form an aqueous cetylpyridinium chloride solution. 0.267mL of sodium chloropalladate (0.01 mol. L) are taken in turn respectively -1 ) 0.2mL of chloroiridic acid (0.01 mol. L) -1 ) And 0.13mL silver nitrate (0.01 mol. L) -1 ) Dropwise adding the aqueous solution to the obtained cetylpyridinium chloride aqueous solutionIn the solution, the solution was stirred for 10 minutes to form an aqueous precursor solution. 0.3mL of the solution was prepared at a concentration of 0.1 mol. L -1 Quickly dripping the ascorbic acid aqueous solution into the precursor aqueous solution, stopping stirring, and standing for reaction for 3 hours at the temperature of 35 ℃. After the reaction is finished, centrifuging the obtained black solution, washing the black solution with deionized water for three times, and finally freeze-drying the black solution for 12 hours to obtain the final Ag 30 Pd 66 Ir 4 A ternary nano-alloy catalyst. In N 2 Electrochemical test results in saturated 1M KOH +1M KCOOH solutions showed that Ag was present at 0.5V (vs RHE) 31 Pd 65 Ir 4 The current density of the ternary nano-alloy catalyst for the oxidation reaction of the formate is 3.17 times that of the commercial Pd/C catalyst.
Example 3
Dissolving 18mg of cetylpyridinium chloride surfactant in 5mL of deionized water, sonicating for 10 minutes, and stirring for 10 minutes to form an aqueous cetylpyridinium chloride solution. 0.267mL of sodium chloropalladate (0.01 mol. L) are taken in turn respectively -1 ) 0.32mL of chloroiridic acid (0.01 mol. L) -1 ) And 0.13mL silver nitrate (0.01 mol. L) -1 ) The aqueous solution was added dropwise to the aqueous solution of cetylpyridinium chloride obtained above, and stirred for 10 minutes to form an aqueous precursor solution. 0.3mL of the solution was prepared at a concentration of 0.1 mol. L -1 Quickly dripping the ascorbic acid aqueous solution into the precursor aqueous solution, stopping stirring, and standing for reaction for 3 hours at the temperature of 35 ℃. After the reaction is finished, centrifuging the obtained black solution, washing the black solution with deionized water for three times, and finally freeze-drying the black solution for 12 hours to obtain the final Ag 28 Pd 65 Ir 7 A ternary nano-alloy catalyst. In N 2 Electrochemical test results in saturated 1M KOH +1M KCOOH solutions showed that Ag was present at 0.5V (vs RHE) 28 Pd 65 Ir 7 The current density of the ternary nano-alloy catalyst for the oxidation reaction of the formate is 2.54 times that of the commercial Pd/C catalyst.
Example 4
Dissolving 18mg of cetylpyridinium chloride surfactant in 5mL of deionized water, performing ultrasonic treatment for 10 minutes, and stirring for 10 minutes to form cetylpyridinium chloride waterAnd (3) solution. 0.3mL of sodium chloropalladate (0.01 mol. L) was sequentially and respectively taken -1 ) 0.2mL of chloroiridic acid (0.01 mol. L) -1 ) And 0.1mL silver nitrate (0.01 mol. L) -1 ) The aqueous solution was added dropwise to the aqueous solution of cetylpyridinium chloride obtained above, and stirred for 10 minutes to form an aqueous precursor solution. 0.3mL of the solution was prepared at a concentration of 0.1 mol. L -1 Quickly dripping the ascorbic acid aqueous solution into the precursor aqueous solution, stopping stirring, and standing for reaction for 3 hours at the temperature of 35 ℃. After the reaction is finished, centrifuging the obtained black solution, washing the black solution with deionized water for three times, and finally freeze-drying the black solution for 12 hours to obtain the final Ag 23 Pd 73 Ir 4 A ternary nano-alloy catalyst. In N 2 Electrochemical test results in saturated 1M KOH +1M KCOOH solutions showed that Ag was present at 0.5V (vs RHE) 23 Pd 73 Ir 4 The current density of the ternary nano-alloy catalyst for the oxidation reaction of the formate is 2.41 times that of the commercial Pd/C catalyst.
Example 5
Dissolving 18mg of cetylpyridinium chloride surfactant in 5mL of deionized water, sonicating for 10 minutes, and stirring for 10 minutes to form an aqueous cetylpyridinium chloride solution. 0.2mL of sodium chloropalladate (0.01 mol. L) was sequentially and respectively taken -1 ) 0.2mL of chloroiridic acid (0.01 mol. L) -1 ) And 0.2mL silver nitrate (0.01 mol. L) -1 ) The aqueous solution was added dropwise to the aqueous solution of cetylpyridinium chloride obtained above, and stirred for 10 minutes to form an aqueous precursor solution. 0.3mL of the solution was prepared at a concentration of 0.1 mol. L -1 Quickly dripping the ascorbic acid aqueous solution into the precursor aqueous solution, stopping stirring, and standing for reaction for 3 hours at the temperature of 35 ℃. After the reaction is finished, centrifuging the obtained black solution, washing the black solution with deionized water for three times, and finally freeze-drying the black solution for 12 hours to obtain the final Ag 46 Pd 49 Ir 5 A ternary nano-alloy catalyst. In N 2 Electrochemical test results in saturated 1M KOH +1M KCOOH solutions showed that Ag was present at 0.5V (vs RHE) 46 Pd 49 Ir 5 The current density of the ternary nano-alloy catalyst for the oxidation reaction of the formate is 1.89 times that of the commercial Pd/C catalyst.
Claims (3)
1. An AgPdIr nanoalloy, which is characterized in that: adding Ir into AgPd nano alloy to form an AgPdIr ternary nano alloy catalyst, wherein the shape of the AgPdIr ternary nano alloy catalyst is a three-dimensional porous spherical structure assembled by nanocrystals, and the AgPd ternary nano alloy catalyst is characterized in that: the diameter of the ball in the three-dimensional porous spherical structure is 30-100 nanometers, the size of the nanocrystal is 3-7 nanometers, and the atomic percentage ranges of the components are Ag: 23-46, Pd: 49-73, Ir: 1 to 8.
2. A method for preparing the AgPdIr nanoalloy of claim 1, characterized by the following steps:
step 1: completely dissolving 17-25 mg of cetylpyridinium chloride surfactant into 5-7 mL of deionized water to form a transparent cetylpyridinium chloride aqueous solution;
step 2: the concentration is 0.01 mol.L -1 Sequentially adding 0.2-0.3 mL of sodium chloropalladate, 0.12-0.32 mL of chloroiridic acid and 0.1-0.2 mL of silver nitrate precursor solution into the cetylpyridinium chloride solution obtained in the step 1, and stirring for 10-15 minutes to uniformly mix the materials
And step 3: adding an ascorbic acid solution into the solution obtained in the step 2, stopping stirring, and standing and reacting for 2-4 hours at the temperature of 25-50 ℃;
and 4, step 4: processing the solution in the step 3 through centrifugal separation, deionized water cleaning and freeze drying to obtain the AgPdIr nano alloy formate oxidation reaction catalyst;
the proportion of each component in the reaction is each part, and is multiplied according to the requirement.
3. The use method of the AgPdIr nanoalloy according to claim 1, characterized in that: the AgPdIr nano alloy is used as a formate oxidation reaction catalyst, the initial potential of the formate oxidation reaction is 0.16-0.2V, the peak potential is 0.5-0.8V, and the potential is referred to a reversible hydrogen electrode; the catalytic activity of the formate oxidation reaction is 2.09-5.14 A.mg -1 Pd The catalytic activity of the formate oxidation reaction is 0.82 to 1.54 A.mg after a 4000s durability test -1 Pd Is prepared from1.29-3.17 times and 7.45-14 times the activity and durability of commercial Pd/C.
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