WO2024255063A1 - Catalyseur de pile à combustible à base de platine modifié par azote-phosphore à haute activité/stabilité et son procédé de préparation - Google Patents

Catalyseur de pile à combustible à base de platine modifié par azote-phosphore à haute activité/stabilité et son procédé de préparation Download PDF

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WO2024255063A1
WO2024255063A1 PCT/CN2023/127254 CN2023127254W WO2024255063A1 WO 2024255063 A1 WO2024255063 A1 WO 2024255063A1 CN 2023127254 W CN2023127254 W CN 2023127254W WO 2024255063 A1 WO2024255063 A1 WO 2024255063A1
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nitrogen
phosphorus
platinum
catalyst
fuel cell
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Chinese (zh)
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廖世军
李朝忠
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South China University of Technology SCUT
Guangzhou Institute of Modern Industrial Technology
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South China University of Technology SCUT
Guangzhou Institute of Modern Industrial 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
    • H01M4/92—Metals of platinum group
    • H01M4/921—Alloys or mixtures with metallic elements
    • 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
    • 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
    • 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
    • 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

Definitions

  • the present invention belongs to the technical field of new energy materials, and specifically relates to a high-activity and high-stability nitrogen-phosphorus modified carbon-supported platinum-based metal catalyst and a preparation method thereof.
  • Catalysts are one of the most core materials of fuel cells and play a decisive role in the performance of fuel cells. Developing high-performance fuel cell catalysts, reducing the use of precious metal platinum, and improving the performance of fuel cells have always been the most important research topics in the fuel cell field.
  • the widely used fuel cell catalysts are carbon-supported platinum catalysts (Pt/C) or carbon-supported platinum-based alloy catalysts (such as PtRu/C, etc.) with conductive carbon black as the carrier and platinum as the important active component.
  • Pt/C carbon-supported platinum catalysts
  • PtRu/C carbon-supported platinum-based alloy catalysts
  • conductive carbon black as the carrier
  • platinum as the important active component.
  • the activity and durability of the catalysts are in urgent need of improvement.
  • the platinum mass activity of the platinum-based intermetallic compound low-platinum catalysts (such as Umicore's Pt3Co/C catalyst) developed in recent years has been significantly improved, and the amount of platinum used has been reduced accordingly.
  • Umicore's Pt3Co/C catalyst the activity and durability of current catalysts still need to be greatly improved.
  • the development of fuel cell cathode oxygen reduction catalysts with higher activity/stability remains an important research topic in the field of fuel cells.
  • Chinese invention patent CN201310410537.0 proposed a method of modifying Pt/C catalyst with polyaniline, and found that after modification with polyaniline, the stability/durability of the catalyst was effectively improved. However, this modification method not only does not improve the activity of the catalyst, but instead causes a certain degree of decrease in activity.
  • the purpose of the present invention is to provide a type of high-activity/stability nitrogen-phosphorus modified platinum-based fuel cell catalyst and a preparation method thereof; the method first adopts impregnation of a metal precursor solution and a nitrogen-phosphorus precursor solution on a carbon carrier, freeze-drying to obtain a dry carbon carrier material containing nitrogen, phosphorus and a metal precursor, and then high-temperature heat treatment in a reducing atmosphere to obtain a high-activity/stability nitrogen-phosphorus modified platinum-based and platinum-based intermetallic compound fuel cell catalyst; the nitrogen-phosphorus modification method can also be directly used for the modification of carbon-supported platinum or carbon-supported platinum-based intermetallic compound catalysts, and platinum-carbon or intermetallic compound catalysts are impregnated with a nitrogen-phosphorus precursor solution, freeze-dried, and then high-temperature heat treatment in a reducing atmosphere to obtain a high-performance nitrogen-phosphorus modified platinum-based or platinum-based intermetallic compound catalyst.
  • a preparation method and application of a highly active/stable nitrogen-phosphorus modified platinum-based fuel cell catalyst comprising the following steps:
  • step (2) using the metal precursor solution obtained in step (1) to impregnate the pretreated carbon carrier, and ultrasonically impregnate the precursor evenly into the carbon carrier to obtain carbon containing the metal precursor; after drying, using the nitrogen and phosphorus precursor prepared in step (1) for a second impregnation;
  • step (3) drying the carbon support containing nitrogen, phosphorus and metal precursors obtained in step (2) to obtain a dried carbon support containing nitrogen, phosphorus and metal precursors;
  • step (3) placing the dried carbon support containing nitrogen, phosphorus and metal precursor obtained in step (3) in a tubular furnace in a reducing atmosphere for high-temperature thermal reduction to obtain a nitrogen-phosphorus modified platinum-based intermetallic compound;
  • a nitrogen-phosphorus-modified platinum-based catalyst can also be prepared by directly using the nitrogen-phosphorus precursor solution prepared in step (1) to impregnate a carbon-supported platinum catalyst (Pt/C) or a carbon-supported platinum-cobalt intermetallic compound catalyst (PtCo/C), followed by drying and high-temperature heat treatment in a reducing atmosphere.
  • a carbon-supported platinum catalyst Pt/C
  • a carbon-supported platinum-cobalt intermetallic compound catalyst PtCo/C
  • a platinum-carbon catalyst or a carbon-supported platinum-cobalt intermetallic compound catalyst is directly impregnated with a solution containing nitrogen and phosphorus compounds, and after freeze-drying and high-temperature treatment under a reducing atmosphere, the performance of the obtained nitrogen-phosphorus modified platinum-carbon and platinum-cobalt intermetallic compound catalysts is also improved exponentially.
  • the platinum source is an inorganic platinum salt or an organic platinum salt
  • the transition metal is an inorganic compound or an organic compound containing one or more of Co, Ni, Cu, Mn and Fe, and the molar ratio of platinum to transition metal is in the range of 3-1.
  • the platinum source is one or more of chloroplatinic acid, potassium chloroplatinate, potassium chloroplatinite or platinum acetylacetonate; and the transition metal source is one or more of chloride, nitrate, acetate and acetylacetonate.
  • the nitrogen-containing compound is any one of 2-methylimidazole, melamine, dopamine, and ammonium bicarbonate; the mass percentage of nitrogen to the catalyst is 0.5-2wt%; the phosphorus-containing compound is any one of diamine hydrogen phosphate, ammonium dihydrogen phosphate, phosphoric acid, ammonium phosphite, ammonium hypophosphite and organic phosphate, and the mass percentage of phosphorus to the catalyst is 1-8wt%.
  • the alcohol includes ethanol, n-propanol and isopropanol, and the volume ratio of water to alcohol is 1:3 to 3:1.
  • the concentration of the solution is 10-30 wt%.
  • the carbon carrier is one of XC-72R carbon black (Cabot, USA), Ketjen black (Ketjen, Japan), and Black Pearls (Cabot, USA); and the carbon carrier pretreatment method is heat treatment at 300°C for 3 hours.
  • the ultrasonic time is 30-60 min.
  • the drying in step (3) includes freeze drying and vacuum drying, and the preferred method is freeze drying, with a drying time range of 10-16 hours.
  • the reducing atmosphere is any one of H 2 /Ar, H 2 /N 2 , H 2 /He mixed gas, and ammonia; the heat treatment temperature is 650-850° C., and the time is 1-4 h.
  • the Pt/C catalyst is one of commercial Pt/C
  • the PtCo/C catalyst is Pt 3 Co/C catalyst from Umicore
  • the heat treatment temperature in the reducing atmosphere is 300-800°C.
  • the present invention also provides the use of the high-activity/stability nitrogen-phosphorus modified platinum-based fuel cell catalyst prepared by the above preparation method in fuel cell cathode oxygen reduction.
  • the present invention Compared with existing catalysts and modification technologies, the present invention has the following advantages:
  • the activity and stability of the nitrogen-phosphorus modified catalyst prepared by the present invention can be greatly improved at the same time, or the improvement can be several times; it is expected to achieve a significant improvement in the performance of fuel cell catalysts, and has great practical application prospects;
  • FIG. 1 is an XRD diagram of the PtCo/C and NP-PtCo/C intermetallic compounds prepared in Comparative Example 1 and Example 3.
  • FIG. 2 is a polarization curve diagram of the PtCo/C and NP-PtCo/C intermetallic compounds prepared in Comparative Example 1 and Example 3 before and after the oxygen reduction stability test.
  • Figure 3 is a polarization curve diagram of NP-JM Pt/C and JM Pt/C prepared in Example 6 before and after the oxygen reduction stability test.
  • Figure 4 is a polarization curve diagram of NP-Umicore PtCo/C and Umicore PtCo/C prepared in Example 7 before and after the oxygen reduction stability test.
  • 265uL of chloroplatinic acid solution and 265uL of cobalt chloride solution were respectively taken and ultrasonically mixed, and then dripped evenly into 80mg of pretreated Ketjen black drop by drop, ultrasonicated for 60min, and freeze-dried for 12h.
  • the dried product was calcined at 750°C for 2h in H 2 /Ar (the volume fraction of H 2 was 8%) atmosphere to obtain Pt 1 Co 1 /C intermetallic compound fuel cell catalyst.
  • Example 1 Except that 22.5 uL 92 mg mL -1 ammonium dihydrogen phosphate solution was used to replace 500 uL 440 mg mL -1 2-methylimidazole solution in Example 1, other steps and methods were the same as Example 1.
  • the prepared catalyst was a phosphorus-modified platinum-cobalt intermetallic compound catalyst (P-Pt 1 Co 1 /C).
  • the concentrations of chloroplatinic acid, cobalt chloride and ferrous chloride were all 0.386 mol L-1.
  • 265uL of chloroplatinic acid, 84.8uL of cobalt chloride and 21.2uL of ferrous chloride solution were respectively taken and ultrasonically mixed, and then dropwise and uniformly added to 80mg of pretreated XC-72R carbon black, and ultrasonicated for 30min.
  • the performance of the catalyst was studied using a three-electrode system, with a glassy carbon electrode with a diameter of 5 mm as the working electrode, a carbon rod as the counter electrode, and an Ag/AgCl electrode with a sodium chloride concentration of 3 mol L -1 as the reference electrode.
  • Working electrode preparation method Weigh 4 mg of the catalyst material prepared in each example, disperse it into 400 ⁇ L of a mixed solution of 0.5 wt% Nafion solution (solvent is isopropanol) and 400 ⁇ L of deionized water, and after ultrasonic dispersion, use a pipette to transfer 5 ⁇ L of catalyst slurry and drop it on the surface of the glassy carbon electrode. After drying naturally, test its oxygen reduction catalytic activity in an oxygen-saturated 0.1 M HClO 4 solution.
  • FIG1 is the XRD test result of the catalyst
  • FIG2 to FIG5 are the results of the oxygen reduction activity and durability test of the catalyst.
  • Figure 2 shows the oxygen reduction curves of PtCo/C and NP-PtCo/C intermetallic compound catalysts prepared in Comparative Example 1 and Example 3, as well as the polarization curves before and after the catalytic stability test.
  • the half-wave potential and mass activity of the NP-PtCo/C catalyst are 0.969 V vs. RHE and 1.82 A mg Pt -1 , respectively, while those of the unmodified PtCo/C intermetallic compound catalyst are 0.914 V vs. RHE and 0.38 A mg Pt -1 ; the mass activity is increased by 5 times after nitrogen and phosphorus modification.
  • the half-wave potential of the PtCo/C intermetallic compound catalyst was 0.900 V vs. RHE, a decrease of 14 mV, while the half-wave potential of the NP-PtCo/C intermetallic compound catalyst was 0.966 V vs. RHE, a decrease of only 3 mV; nitrogen and phosphorus modification reduced the attenuation of the catalyst by more than 80%;
  • the half-wave potential and mass activity of the commercial Pt/C catalyst (JM Pt/C) after nitrogen and phosphorus modification are 0.916 V (vs. RHE) and 0.47 A mg Pt -1 , respectively, and the mass activity is three times that of the unmodified catalyst (0.893 V vs. RHE and 0.18 A mg Pt -1 ).
  • the half-wave potential of the nitrogen and phosphorus modified catalyst (NP-JM Pt/C) is 0.913 V (vs. RHE), which only decreases by 3 mV
  • the half-wave potential of the unmodified JM Pt/C is 0.864 V vs. RHE, which decreases by as much as 29 mV.
  • the decrease in the modified catalyst is reduced by 90%.
  • Figure 4 shows the test results of the Umicore PtCo/C catalyst and the nitrogen-phosphorus modified catalyst (NP-Umicore PtCo/C).
  • the half-wave potential and mass activity of the nitrogen-phosphorus modified NP-Umicore PtCo/C catalyst are 0.952 V (vs. RHE) and 1.46 A mg Pt -1 , respectively, and the mass activity is about doubled (0.935 V vs. RHE and 0.85 A mg Pt -1 for the Umicore PtCo/C catalyst).
  • the half-wave potential of the NP-Umicore PtCo/C catalyst did not decrease, still at 0.952 V (vs. RHE), while the half-wave potential of the Umicore PtCo/C was 0.916 V (vs. RHE), down 19 mV. It can be seen that nitrogen-phosphorus modification can greatly improve the stability of PtCo intermetallic compounds.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
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Abstract

La présente invention concerne un catalyseur de pile à combustible à base de platine modifié par azote-phosphore à haute activité/stabilité et son procédé de préparation. Le procédé consiste à : dissoudre une source de platine et un composé source de métal de transition dans de l'eau ou un solvant mixte eau-alcool, et soumettre le mélange à un traitement par ultrasons pour obtenir une solution de précurseur métallique ; l'imprégnation d'un support de carbone prétraité avec la solution de précurseur métallique, et la réalisation d'un traitement par ultrasons et son séchage ; puis, l'imprégnation du support de carbone contenant un précurseur métallique avec une solution contenant une source d'azote et une source de phosphore pour obtenir un support de carbone contenant de l'azote, du phosphore et le précurseur métallique ; et la soumission de celui-ci à une lyophilisation, puis la réduction de celui-ci dans une atmosphère réductrice à haute température pour obtenir un catalyseur de carbone à base de platine modifié par azote-phosphore ou un catalyseur de composé intermétallique à base de platine. L'activité et la durabilité du catalyseur composé intermétallique platine-cobalt modifié par azote-phosphore sont supérieures à celles d'un catalyseur non modifié plusieurs fois. Un procédé de modification d'azote-phosphore selon la présente invention présente une importance significative pour améliorer l'activité et la durabilité du catalyseur de pile à combustible actuel.
PCT/CN2023/127254 2023-06-15 2023-10-27 Catalyseur de pile à combustible à base de platine modifié par azote-phosphore à haute activité/stabilité et son procédé de préparation Pending WO2024255063A1 (fr)

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CN120878864A (zh) * 2025-07-21 2025-10-31 济南大学 一种铂基合金负载木质碳催化剂及其制备方法与应用

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CN120878864A (zh) * 2025-07-21 2025-10-31 济南大学 一种铂基合金负载木质碳催化剂及其制备方法与应用

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