CN119852425A - Ternary ordered alloy catalyst for fuel cell and preparation method thereof - Google Patents
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Abstract
本发明公开了一种燃料电池用三元有序合金催化剂及其制备方法，该方法包含：步骤1，将炭黑分散于水醇溶液和表面活性剂，得到炭黑溶液；步骤2，分别配制铂前驱体溶液、钴前驱体溶液和镧系元素前驱体溶液；步骤3，混合所述炭黑溶液、铂前驱体溶液、钴前驱体溶液和镧系元素前驱体溶液，通入还原气体进行热还原，得到三元有序合金催化剂；所述热还原的温度为700℃‑1000℃，时间为0.5h‑2h。采用上述方法制备的三元有序合金催化剂有序度高，能够大幅减缓金属的溶出，且活性和稳定性高，有助于提高燃料电池的性能。
The invention discloses a ternary ordered alloy catalyst for a fuel cell and a preparation method thereof, the method comprising: step 1, dispersing carbon black in a water-alcohol solution and a surfactant to obtain a carbon black solution; step 2, respectively preparing a platinum precursor solution, a cobalt precursor solution and a lanthanide precursor solution; step 3, mixing the carbon black solution, the platinum precursor solution, the cobalt precursor solution and the lanthanide precursor solution, passing a reducing gas for thermal reduction, and obtaining a ternary ordered alloy catalyst; the thermal reduction temperature is 700°C-1000°C, and the time is 0.5h-2h. The ternary ordered alloy catalyst prepared by the above method has a high degree of order, can greatly slow down the dissolution of metals, and has high activity and stability, which helps to improve the performance of fuel cells.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a ternary ordered alloy catalyst for a fuel cell and a preparation method thereof.
Background
The Oxygen Reduction Reaction (ORR), one of the key reactions in Proton Exchange Membrane Fuel Cells (PEMFC), acts as the primary cathode reaction, responsible for reducing oxygen to water or other oxygenates, while releasing electrons, which can then be used to generate electricity. Carbon-supported Pt nanoparticle (Pt/C) catalysts are the most widely used cathode catalysts in PEMFCs, however, pt nanoparticles are easily dissolved and migrated in the acidic working environment of PEMFCs, resulting in loss of active sites, poor Pt/C catalyst activity/durability, and thin reserves of Pt in the crust, which is expensive, resulting in Pt/C catalyst costs accounting for more than 50% of the total fuel cell costs, impeding large-scale production and application of PEMFCs.
During the last decade, pt was alloyed with other transition metals (hereinafter "M") such as Fe, co, ni, cu, etc., so that the energy of d-orbital electrons was reduced, weakening the adsorption strength of the catalyst surface with Oxygen Reduction Reaction (ORR) intermediates (such as OH, O, OOH, etc.), significantly improving the activity of the cathode catalyst and reducing the use of Pt. In the disordered face-centered cubic solid-melting structure, M and Pt are randomly distributed, the electrochemical stability of M is poor, the activity of M on the surface of an alloy is higher than that of Pt, so that M can more easily participate in the reaction in the electrochemical reaction, and the M can be easily dissolved out in the actual use process, and the activity and stability of a catalyst are reduced. In ordered intermetallic structure (such as tetragonal L10 or cubic L12 structure), M and Pt are arranged according to specific stoichiometric ratio and highly ordered mode, and have strong interatomic interaction, so that dissolution of M can be greatly slowed down, and activity and stability of the catalyst are obviously improved. CN116404182a discloses a low-platinum ternary alloy catalyst and its preparation method, but its synthesis process is complex, and a disordered solid solution alloy is synthesized, in the actual use process, the metal in the alloy can be gradually dissolved out, so that the membrane electrode performance is seriously attenuated.
Therefore, the improvement of the order of the alloy can greatly slow down the dissolution of metal, and improve the activity and stability of the catalyst, thereby improving the performance of the fuel cell.
Disclosure of Invention
The invention aims to solve the problems of reduced activity and stability of a catalyst by doping lanthanide into a platinum-cobalt binary ordered alloy catalyst, improving the degree of order and inhibiting the dissolution of metal.
In order to achieve the above object, the present invention provides a method for preparing a ternary ordered alloy catalyst for a fuel cell, the method comprising:
Step 1, dispersing carbon black in an aqueous alcohol solution and a surfactant to obtain a carbon black solution;
Step 2, preparing a platinum precursor solution, a cobalt precursor solution and a lanthanide precursor solution respectively;
and 3, mixing the carbon black solution, the platinum precursor solution, the cobalt precursor solution and the lanthanide precursor solution, and introducing reducing gas to perform thermal reduction to obtain the ternary ordered alloy catalyst, wherein the temperature of the thermal reduction is 700-1000 ℃ and the time is 0.5-2 h.
Optionally, in the step 2, the platinum precursor at least comprises one or more of H 2PtCl6、K2PtCl4, ammonium chloroplatinate and platinum acetylacetonate, the cobalt precursor at least comprises one or more of cobalt chloride, cobalt nitrate and cobalt acetate, and the lanthanide precursor is any one of lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium precursors.
Optionally, in the step 3, the molar ratio of platinum atoms, cobalt atoms and lanthanide atoms is (1-3): 0.25-4): 1-1.5.
Optionally, in the step 1, the volume ratio of water to absolute ethyl alcohol in the hydroalcoholic solution is (1-2): 1-3, and the mass ratio of carbon black to the hydroalcoholic solution is (1-2): 1-3.
Optionally, before the step 1, the method further comprises etching the carbon black by sulfuric acid, wherein the mass ratio of the carbon black to the sulfuric acid is (1-1.5): 1-2, and the etching time is 12-14 h.
Optionally, in the step 1, the surfactant at least comprises one or more of triton X-114, triton X-100, triton X-45, sodium dodecyl sulfate and tween-20.
Optionally, in the step 3, the mixing method includes ultrasonic treatment and stirring, wherein the ultrasonic treatment time is 60min-180min, and the stirring time is 10h-15h.
Optionally, in the step 3, a solvent is removed before the reducing gas is introduced, and the solvent removing method is any one of freeze-drying, natural air-drying, water bath evaporation, rotary evaporation or oil bath evaporation.
Optionally, in the step 3, the reducing gas is any one of a nitrogen-hydrogen mixture and an argon-hydrogen mixture.
The invention also provides a ternary ordered alloy catalyst for the fuel cell, which is prepared by adopting any one of the preparation methods.
Compared with the prior art, the technical scheme of the invention has at least the following beneficial effects:
1) The ternary ordered alloy catalyst is formed by doping lanthanide into platinum-cobalt binary ordered alloy catalyst, because the atomic radius of lanthanide is larger, the compressive strain of platinum-cobalt system is changed, so that the electronic structure of platinum, cobalt and lanthanide is affected, and the three are arranged according to a highly ordered mode, so that the degree of order is raised, and the three metal atoms orderly occupy the corresponding lattice points in the crystal lattice, so that more stable chemical bonds are formed between metals, the interaction is enhanced, and the dissolution of cobalt and lanthanide is greatly slowed down, thus being beneficial to raising the activity and stability of the ternary ordered alloy catalyst.
2) Further, the ternary ordered alloy catalyst is used as a cathode catalyst of the proton exchange membrane fuel cell, so that the power density of the fuel cell can be improved, and the performance of the fuel cell is improved.
Drawings
Fig. 1 is a TEM image of a ternary ordered alloy catalyst of example 1 of the present invention, wherein b is a partial enlarged view of a.
FIG. 2 is an XRD diffraction pattern of the ternary ordered alloy catalysts of comparative example 1 and examples 1-3 of the invention, where b is a partial enlargement of a.
FIG. 3 is a graph showing oxygen reduction activity test curves of the ternary ordered alloy catalysts of comparative example 1 and examples 1-3 of the present invention, wherein a is a linear voltammogram and b is a cyclic voltammogram.
Fig. 4 is a graph of stability performance test of the ternary ordered alloy catalyst of example 1 of the present invention.
Fig. 5 is a graph of power density measurements of the ternary ordered alloy catalysts of comparative example 1 and examples 1-3 of the present invention as cathode catalysts for proton exchange membrane fuel cells.
Detailed Description
The following description of the embodiments of the present invention will be made apparent and fully in view of the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be noted that the directions or positional relationships indicated by the terms "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. are directions or positional relationships based on the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
As described in the background art, pt and other transition metals M are alloyed to form a Pt-M alloy catalyst, in a disordered face-centered cubic solid-melting structure, M and Pt are randomly distributed, the electrochemical stability of M is poor, the activity of M on the surface of the alloy is higher than that of Pt, so that M can participate in the electrochemical reaction more easily, and therefore, M can be easily dissolved out in the actual use process, and the activity and stability of the catalyst are reduced. In the ordered intermetallic structure, M and Pt are arranged according to a specific stoichiometric ratio and a highly ordered mode, so that the catalyst has stronger interatomic interaction, and can greatly slow down the dissolution of metal, thereby remarkably improving the activity and stability of the catalyst.
In order to improve the activity and stability of the catalyst, the ternary ordered alloy catalyst is formed by doping lanthanide in the platinum-cobalt binary ordered alloy catalyst, the lanthanide can enable platinum, cobalt and the lanthanide to be arranged in a highly ordered mode, the degree of order is improved, meanwhile, the stronger interaction generated between ordered metals can greatly slow down the dissolution of cobalt and the lanthanide, and the activity and stability of the ternary ordered alloy catalyst are improved. Specifically, the invention provides a preparation method of a ternary ordered alloy catalyst for a fuel cell, which comprises the following steps:
And step 1, dispersing carbon black in an aqueous alcohol solution and a surfactant to obtain a carbon black solution.
In the step, the mass ratio of the carbon black to the aqueous alcohol solution is (1-2) (1-3), the volume ratio of the water in the aqueous alcohol solution to the absolute ethyl alcohol is (1-2) (1-3), the ultrasonic time for dispersing the carbon black in the aqueous alcohol solution is 60-180 min, after ultrasonic treatment is completed, the surfactant is added into the aqueous alcohol solution, the stirring time is 10-15 h, and the obtained carbon black solution is stirred at a constant temperature at 25 ℃ for standby after the stirring is completed. Because stronger interaction force exists between the carbon black particles, the carbon black particles are easy to agglomerate, the dispersibility is influenced, the interaction force between the carbon black particles can be reduced by adding the surfactant, the agglomeration tendency of the carbon black particles is weakened, and the uniform dispersion of the carbon black is realized.
In some embodiments, the surfactant comprises at least one or more of triton X-114, triton X-100, triton X-45, sodium dodecyl sulfate, tween-20.
And (2) before the step (1), the carbon black is etched by sulfuric acid, the carbon black is ultrasonically dispersed in the sulfuric acid, the mass ratio of the carbon black to the sulfuric acid is (1-1.5): 1-2, the carbon black is placed in a 60 ℃ oven for etching, the etching time is 12-14 h, centrifugal washing is carried out after the etching is finished, and the carbon black is placed in a vacuum drying oven for drying. The purpose of etching the carbon black with sulfuric acid is to remove other organic impurities and metal ions in the carbon black and improve the purity and quality of the carbon black.
And 2, preparing a platinum precursor solution, a cobalt precursor solution and a lanthanide precursor solution respectively.
In some embodiments, the platinum precursor comprises at least one or more of H 2PtCl6、K2PtCl4, ammonium chloroplatinate and platinum acetylacetonate, wherein the mass of platinum in the platinum precursor is 1-40% of the mass of the carbon carrier, the cobalt precursor comprises at least one or more of cobalt chloride, cobalt nitrate and cobalt acetate, and the lanthanide precursor is any one of lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium precursors. The mole ratio of platinum atoms, cobalt atoms and lanthanide series atoms is (1-3): (0.25-4): (1-1.5), and under the condition of said ratio the ordering degree of ternary ordered alloy can be obviously raised. Different concentrations of platinum precursor solution, cobalt precursor solution, and lanthanide precursor solution may be formulated as desired.
And 3, mixing the carbon black solution, the platinum precursor solution, the cobalt precursor solution and the lanthanide precursor solution, and introducing reducing gas to perform thermal reduction to obtain the ternary ordered alloy catalyst, wherein the temperature of the thermal reduction is 700-1000 ℃ and the time is 0.5-2 h.
Mixing the carbon black solution, the platinum precursor solution, the cobalt precursor solution and the lanthanide precursor solution, and then stirring for 10-15 h, wherein the stirring aims to ensure that the precursor solution and the carbon black solution are mixed more completely, thereby being more beneficial to the loading of the subsequent precursor on the carbon black. After the completion of the stirring, the solvent was removed and a reducing gas was introduced to carry out thermal reduction.
In some embodiments, the method of removing the solvent is any one of lyophilization, natural air drying, water bath evaporation, rotary evaporation, or oil bath evaporation.
In some embodiments, the reducing gas is any one of a nitrogen-hydrogen mixture and an argon-hydrogen mixture. The ternary ordered alloy catalyst obtained by thermal reduction is arranged in a highly ordered mode, the ordering degree is high, three metal atoms orderly occupy corresponding lattice points in a lattice, so that more stable chemical bonds are formed among metals, interaction is enhanced, dissolution of the metals is greatly slowed down, and the activity and stability of the ternary ordered alloy catalyst are improved.
Sulfuric acid, chloroplatinic acid hexahydrate, cobalt nitrate hexahydrate, and cerium nitrate in comparative example 1 and examples 1-3 were purchased from Shanghai Ala Biotechnology Co., ltd. The preparation method comprises the steps of dissolving 2.72ml of sulfuric acid (18.4 mol/L) in 1L of water to obtain 0.05mol/L of sulfuric acid, dissolving 20mg of chloroplatinic acid hexahydrate in 1ml of water to obtain 20mg/ml of chloroplatinic acid solution, dissolving 20mg of cobalt nitrate hexahydrate in 1ml of water to obtain 20mg/ml of cobalt nitrate hexahydrate solution, and dissolving 10mg of cerium nitrate in 1ml of water to obtain 10mg/ml of cerium nitrate solution.
Comparative example 1
30Mg of carbon black is placed in 30ml of sulfuric acid (0.05 mol/L) and is subjected to ultrasonic treatment for 60min, placed in a 60 ℃ oven for 12h of etching, centrifugally washed and placed in a vacuum drying oven for drying. Taking 20mg of dried carbon black, putting the dried carbon black into 20ml of aqueous alcohol solution, carrying out ultrasonic treatment for 60min, adding 5mg of triton X-114, and magnetically stirring for 10h to obtain a carbon black solution. Then adding 0.734ml of chloroplatinic acid solution hexahydrate (20 mg/ml) and 0.084ml of cobalt nitrate hexahydrate solution (20 mg/ml) into the carbon black solution in turn, magnetically stirring for 12 hours, removing the solvent by adopting a rotary evaporation method, finally carrying out thermal reduction for 2 hours at 900 ℃ in a tubular furnace under argon-hydrogen mixed gas, and cooling to obtain the binary ordered alloy catalyst.
Example 1
30Mg of carbon black is placed in 30ml of sulfuric acid (0.05 mol/L) and is subjected to ultrasonic treatment for 60min, placed in a 60 ℃ oven for 12h of etching, centrifugally washed and placed in a vacuum drying oven for drying. Taking 20mg of dried carbon black, putting the dried carbon black into 20ml of aqueous alcohol solution, carrying out ultrasonic treatment for 60min, adding 5mg of triton X-114, and magnetically stirring for 10h to obtain a carbon black solution. Then adding 0.734ml of hexahydrated chloroplatinic acid solution (20 mg/ml), 0.084ml of hexahydrated cobalt nitrate solution (20 mg/ml) and 0.068ml of cerium nitrate solution (10 mg/ml) into the carbon black solution in sequence, magnetically stirring for 12h, removing the solvent by adopting a rotary evaporation method, finally carrying out thermal reduction for 2h at 900 ℃ in a tube furnace under argon-hydrogen mixed gas, and cooling to obtain the ternary ordered alloy catalyst. As shown in fig. 1, the morphology picture of the ternary ordered alloy particles is shown.
Example 2
Ternary ordered alloy catalysts were prepared as in example 1 except that the addition amounts of cobalt nitrate hexahydrate solution (20 mg/ml) and cerium nitrate solution (10 mg/ml) were replaced with 0.269ml and 0.220ml.
Example 3
The preparation method of the ternary ordered alloy catalyst is the same as in example 2, except that the thermal reduction temperature is replaced by 1000 ℃.
Fig. 2 is an XRD diffractogram of comparative example 1 and examples 1-3 (where b is a partial enlargement of a), and the characteristic diffraction peaks of examples 1-2 are shifted compared to standard cards, indicating that cerium atoms were doped successfully, and example 3 indicates that at 700-1000 ℃, only the thermal reduction temperature was changed without affecting the characteristic diffraction peaks, and cerium atoms were doped successfully.
Example 4
And an electrochemical workstation of a three-electrode system is adopted to characterize the oxygen reduction activity of the ternary ordered alloy catalyst. The ternary ordered alloy catalyst is a working electrode, platinum is a counter electrode, saturated Ag/AgCl is a reference electrode, and the electrolyte is 0.1M HClO 4 solution. The catalyst was subjected to an oxygen reduction activity test using cyclic voltammogram test, and a potential range of +0.05 to +1.00V (compared to a reversible hydrogen electrode) was scanned by cyclic voltammogram in a nitrogen-saturated 0.1M HClO 4 solution at a scanning rate of 50mV s -1 to obtain an electrochemically active area (as shown in b in fig. 3), and further to obtain mass activity and specific activity using linear voltammogram test (as shown in a in fig. 3). the intrinsic activity parameters of the catalyst such as mass activity, specific activity, electrochemical activity area and the like can be calculated through Koutecky-Levich equation and the platinum loading in the feeding. Calculated, the ternary ordered alloy catalyst of example 1 had a mass activity of 0.57A/mg, a specific activity of 1.18mA/cm 2, an electrochemical activity area of 48.5m 2/g, the ternary ordered alloy catalyst of example 2 had a mass activity of 0.24A/mg, a specific activity of 0.35mA/cm 2, an electrochemical activity area of 68.91m 2/g, the ternary ordered alloy catalyst of example 3 had a mass activity of 0.197A/mg, a specific activity of 0.221mA/cm 2, an electrochemical activity area of 89.47m 2/g, the binary ordered alloy catalyst of comparative example 1 had a mass activity of 0.105A/mg, a specific activity of 0.035mA/cm 2, an electrochemical activity area of 84.67m 2/g, and a specific activity of the ternary ordered alloy catalyst was obtained, when the mole ratio of cobalt atoms and cerium atoms is proper, the ternary ordered alloy catalyst has better mass activity, specific activity and electrochemical activity area.
Example 5
The stability of the ternary ordered alloy catalyst of example 1 was characterized using an electrochemical workstation of a three electrode system. The ternary ordered alloy catalyst is a working electrode, platinum is a counter electrode, saturated Ag/AgCl is a reference electrode, and the electrolyte is 0.1M HClO 4 solution. The catalyst was tested for stability by linear voltammogram testing, scanning linear voltammograms in a potential range of +0.6 to +1.10V (compared to reversible hydrogen electrodes) in an oxygen saturated 0.1M HClO 4 solution at a rate of 100mV s -1 for 20000 turns. As shown in fig. 4, the current density gradually increases with the increase of the potential difference, but the difference at different scanning turns is smaller, indicating that the ternary ordered alloy catalyst of example 1 has better stability.
Example 6
The ternary ordered alloy catalyst is used as a cathode catalyst of a low-temperature proton exchange membrane fuel cell to test the power density of the fuel cell. The anode is a 20% Pt/C catalyst, the cathode is a ternary ordered alloy catalyst, the platinum loading of the anode and the cathode is 0.1 mg/cm 2, the cell temperature is 60 ℃, and the back pressure of the anode side and the cathode side is 100kPa. As shown in fig. 5, the product of the current density and the cell voltage is the power density, and the peak power densities of the proton exchange membrane fuel cells of comparative example 1 and examples 1-3 are 631mW/cm 2、738mW/cm2、646mW/cm2、582mW/cm2 respectively, and the power densities are not greatly different, which indicates that the ternary ordered alloy catalyst prepared by the method of the embodiment has good application prospect as the cathode catalyst of the proton exchange membrane fuel cell.
In conclusion, the ternary ordered alloy catalyst is formed by doping lanthanide into the platinum-cobalt binary ordered alloy catalyst, the compressive strain of a platinum-cobalt system is changed by the lanthanide, so that the electronic structures of platinum, cobalt and the lanthanide are influenced, the three are arranged in a highly ordered mode, the degree of order is improved, three metal atoms orderly occupy corresponding lattice points in a lattice, so that more stable chemical bonds are formed between metals, interaction is enhanced, the dissolution of cobalt and the lanthanide is greatly slowed down, and the activity and stability of the ternary ordered alloy catalyst are improved. The ternary ordered alloy catalyst is used as a cathode catalyst of the proton exchange membrane fuel cell, so that the power density of the fuel cell can be improved, and the performance of the fuel cell is improved.
While the present invention has been described in detail through the foregoing description of the preferred embodiment, it should be understood that the foregoing description is not to be considered as limiting the invention. Many modifications and substitutions of the present invention will become apparent to those of ordinary skill in the art upon reading the foregoing. Accordingly, the scope of the invention should be limited only by the attached claims.
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