CN114122436B - Preparation method of Pd-Ni/C nanosphere catalyst with diameter of 1-2nm in fuel cell - Google Patents
Preparation method of Pd-Ni/C nanosphere catalyst with diameter of 1-2nm in fuel cell Download PDFInfo
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- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
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Abstract
The invention discloses a preparation method of a Pd-Ni/C nanosphere catalyst with the diameter of 1-2nm in a fuel cell, belonging to the field of oxygen reduction catalysts of fuel cells. The preparation method comprises the following steps: (1) Mixing palladium acetylacetonate, nickel acetylacetonate, octadecyl trimethyl ammonium chloride, oleylamine and formaldehyde in proportion, and performing ultrasonic treatment to obtain a mixed solution; (2) Heating the mixed solution in a closed autoclave to obtain a heated product; (3) washing the heated product with ethanol to obtain a primary product; (4) Mixing the initial product with carbon black and ethanol, then carrying out ultrasonic treatment, stirring, centrifuging and drying to finally obtain the Pd-Ni/C nanosphere catalyst with the diameter of 1-2 nm. The small-size nano catalyst prepared by the method reduces the cost of the catalyst on the premise of ensuring the catalytic activity and stability, and the preparation method is simple and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of fuel cell electrocatalysts, and particularly relates to a preparation method of a Pd-Ni/C nanosphere catalyst with a diameter of 1-2nm in a fuel cell.
Background
Proton exchange membrane fuel cells are a type of renewable energy conversion device. Among them, the development of electrocatalysts for cathodic oxygen reduction reactions is a key material for large-scale commercial applications of fuel cells. Currently, the primary fuel cell redox catalyst on the market is Pt/C. But Pt metal reserves are scarce and poor in durability, greatly hampering the commercial development of fuel cells. Therefore, development of an efficient proton exchange membrane fuel cell electrocatalyst is an epoch-making trend.
Disclosure of Invention
The invention aims to provide an electrocatalyst applied to a cathode oxygen reduction reaction of a proton exchange membrane fuel cell, which is a Pd-Ni/C nanosphere catalyst with the diameter of 1-2nm prepared by taking palladium acetylacetonate and nickel acetylacetonate as precursors. On the premise of ensuring the catalytic activity and stability of the catalyst, the cost of the catalyst is reduced.
The catalyst has larger specific surface area and more active sites by designing the size of the catalyst, so that the catalytic performance is improved. Meanwhile, the good dispersibility also improves the utilization rate and stability of the catalyst.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a preparation method of Pd-Ni/C nanosphere catalyst with diameter of 1-2nm in fuel cell comprises the following specific steps:
(1) Mixing palladium acetylacetonate, nickel acetylacetonate, octadecyl trimethyl ammonium chloride, oleylamine and formaldehyde in proportion, and performing ultrasonic treatment to obtain a mixed solution;
(2) Heating the mixed solution in a closed autoclave to obtain a heated product;
(3) Washing the heated product with ethanol to obtain a primary product;
(4) Mixing the initial product with carbon black and ethanol, then carrying out ultrasonic treatment, stirring, centrifuging and drying to finally obtain the Pd-Ni/C nanosphere catalyst with the diameter of 1-2 nm.
Preferably, in the step (1), the mass ratio of the nickel acetylacetonate to the palladium acetylacetonate is 1:1.5-1.6.
Preferably, in the step (1), the mass ratio of the octadecyl trimethyl ammonium chloride to the palladium acetylacetonate is 25.1-25.5:1.
Preferably, in the step (1), the volume ratio of the oleylamine to the palladium acetylacetonate is 1.2-1.5:1.
Preferably, in the step (1), the volume ratio of formaldehyde to palladium acetylacetonate is 1:16.0-16.6.
Preferably, in the step (1), the ultrasonic time is 1 to 1.5 hours.
Preferably, in the step (2), the heating temperature is 190-200 ℃ and the time is 14-16 h.
Preferably, in the step (3), the centrifugation reagent is alcohol, the centrifugation speed is 9000-9500 rpm, and the centrifugation times are 3-4 times.
Preferably, in step (4), the mass ratio of the initial product to carbon black is 1:4.
The invention adopts a solvothermal method to prepare Pd-Ni nanosphere type electrocatalyst solution, and the Pd-Ni nanospheres are obtained after centrifugation and drying, and then are loaded on carbon black to obtain the Pd-Ni/C nanosphere catalyst with the diameter of 1-2 nm. The method utilizes the combined action of the size effect and the doping effect to develop the electrocatalyst with high activity, high stability and relatively low cost.
Compared with the prior art, the invention has the advantages that: the ultra-small nanostructures provide an open active surface area and more active sites. As an oxygen reduction reaction electrocatalyst, the Pd-Ni nanospheres supported on carbon black have extremely high catalytic activity, which is much higher than commercial Pt/C. The improvement in performance is attributed to the addition of small particle size nanospheres and Ni induced by octadecyl trimethyl ammonium chloride, changing the lattice parameters of Pd. The material cost of the invention is lower than that of the Pt/C sold in the market, the operation steps are simple, the requirements on equipment are low, the energy consumption is low, the resources are saved, the environment is protected, and the invention follows the concepts of sustainable development, energy conservation and emission reduction.
Drawings
FIG. 1 is a transmission electron microscope image of a Pd-Ni/C catalyst with a diameter of 1-2nm prepared in example 1, and it can be seen that nanospheres are uniformly dispersed.
FIG. 2 is a graph comparing electrocatalytic activity of Pd-Ni/C of diameter 1-2nm and commercial Pt/C prepared in example 1. It can be seen that the catalyst prepared in example 1 has a higher catalytic activity than commercial Pt/C.
FIG. 3 is a transmission electron microscope image of the Pd-Ni/C catalyst without specific morphology prepared in comparative example 1;
FIG. 4 is a graph comparing electrocatalytic activity of Pd-Ni/C without specific morphology and commercial Pt/C prepared in comparative example 1. It can be seen that the activity of Pt/C is much higher than that of the prepared catalyst.
Detailed Description
The invention will be further described with reference to the drawings and the specific examples.
Example 1
The preparation method of the Pd-Ni/C nanosphere catalyst with the diameter of 1-2nm in the fuel cell comprises the following steps:
(1) 10mg of nickel acetylacetonate, 15mg of palladium acetylacetonate, 0.9ml of formaldehyde solution, 18ml of oleylamine and 275mg of octadecyl trimethyl ammonium chloride are uniformly mixed, and then the mixture is placed in an ultrasonic cleaner for ultrasonic treatment for more than 1 hour, so that a uniform mixed solution is obtained.
(2) Heating the mixed solution in a reaction kettle at 190 ℃ for 14h;
(3) Mixing the reacted reagent with alcohol, washing and centrifuging at 9000rpm for 10min for 3 times to obtain a primary product, directly storing the primary product in a centrifuge tube, and then placing the centrifuge tube in a blast drying oven at 60 ℃ for drying overnight;
(4) Mixing the initial product with carbon black in the mass ratio of 1:4, adding ethanol, performing ultrasonic dispersion for 2h, mechanically stirring for 8h, centrifuging according to the centrifuging mode in the step (3), and drying to obtain the Pd-Ni/C nanosphere catalyst with the diameter of 1-2 nm.
As shown in FIG. 1, which is an electron microscope scanning diagram of the product, it can be seen that the product is in a very small particle shape and is uniformly distributed by adding the surfactant octadecyl trimethyl ammonium chloride. The polarization curve of the prepared catalyst was measured to evaluate its electrocatalytic activity for oxygen reduction reaction, and Pd-Ni/C having a diameter of 1-2nm showed higher activity than commercial Pt/C, as shown in FIG. 2.
Comparative example 1
The preparation method of the Pd-Ni/C alloy catalyst without specific morphology in the fuel cell specifically comprises the following steps:
(1) Uniformly mixing 10mg of nickel acetylacetonate, 15mg of palladium acetylacetonate, 0.9ml of formaldehyde solution and 18ml of oleylamine, and then placing the mixture in an ultrasonic cleaner for ultrasonic treatment for more than 1 hour to obtain a uniform mixed solution;
(2) Heating the mixed solution in a reaction kettle at 190 ℃ for 14h;
(3) Mixing the reacted reagent with alcohol, washing and centrifuging at 9000rpm for 10min for 3 times to obtain a primary product, directly storing the primary product in a centrifuge tube, and then placing the centrifuge tube in a blast drying oven at 60 ℃ for drying overnight;
(2) Mixing the initial product with carbon black in a mass ratio of 1:4, adding ethanol, performing ultrasonic dispersion for 2h, mechanically stirring for 8h, centrifuging according to the centrifuging mode in the step (3), and drying to obtain the Pd-Ni/C nanosphere catalyst without specific morphology.
As shown in fig. 3, which is an electron microscope scan of the comparative example product, comparative example 1 was free of added surfactant, and the morphology of the obtained product was irregular and the catalytic activity was inferior to that of commercial Pt/C.
From example 1 and comparative example 1, it is understood that the improvement in the performance of the catalyst for preparing Pd-Ni/C nanospheres according to the present invention is attributed to the addition of Ni and small-sized nanospheres induced by octadecyl trimethyl ammonium chloride, and the lattice parameter of Pd is changed.
Example 2
The preparation method of the Pd-Ni/C nanosphere catalyst with the diameter of 1-2nm in the fuel cell comprises the following steps:
(1) Uniformly mixing nickel acetylacetonate, palladium acetylacetonate, formaldehyde solution, oleylamine and octadecyl trimethyl ammonium chloride, and then placing the mixture in an ultrasonic cleaner for ultrasonic treatment for more than 1 hour to obtain uniform mixed solution;
wherein, the mass ratio of nickel acetylacetonate to palladium acetylacetonate is 1:1.5, the mass ratio of octadecyl trimethyl ammonium chloride to palladium acetylacetonate is 25.1:1, the volume ratio of oleylamine to palladium acetylacetonate is 1.2:1, and the volume ratio of formaldehyde to palladium acetylacetonate is 1:16.0;
(2) Heating the mixed solution in a reaction kettle at 200 ℃ for 14h;
(3) Mixing the reacted reagent with alcohol, washing and centrifuging at 9500rpm for 10min for 4 times to obtain initial product, storing the initial product in a centrifuge tube directly, and drying in a blast drying oven at 60 deg.c for overnight;
(4) Mixing the initial product with carbon black in the mass ratio of 1:4, adding ethanol, performing ultrasonic dispersion for 1.5h, mechanically stirring for 8.5h, centrifuging according to the centrifuging mode in the step (3), and drying to obtain the Pd-Ni/C nanosphere catalyst with the diameter of 1-2 nm.
Example 3
The preparation method of the Pd-Ni/C nanosphere catalyst with the diameter of 1-2nm in the fuel cell comprises the following steps:
(1) Uniformly mixing nickel acetylacetonate, palladium acetylacetonate, formaldehyde solution, oleylamine and octadecyl trimethyl ammonium chloride, and then placing the mixture in an ultrasonic cleaner for ultrasonic treatment for more than 1 hour to obtain uniform mixed solution;
wherein, the mass ratio of nickel acetylacetonate to palladium acetylacetonate is 1.6, the mass ratio of octadecyl trimethyl ammonium chloride to palladium acetylacetonate is 25.5:1, the volume ratio of oleylamine to palladium acetylacetonate is 1.5:1, and the volume ratio of formaldehyde to palladium acetylacetonate is 1:16.6;
(2) Heating the mixed solution in a reaction kettle at 190 ℃ for 16 hours;
(3) Mixing the reacted reagent with alcohol, washing and centrifuging at 9000rpm for 10min for 3 times to obtain a primary product, directly storing the primary product in a centrifuge tube, and then placing the centrifuge tube in a blast drying oven at 60 ℃ for drying overnight;
(4) Mixing the initial product with carbon black in the mass ratio of 1:4, adding ethanol, performing ultrasonic dispersion for 3h, mechanically stirring for 7h, centrifuging according to the centrifuging mode in the step (3), and drying to obtain the Pd-Ni/C nanosphere catalyst with the diameter of 1-2 nm.
Example 4
The preparation method of the Pd-Ni/C nanosphere catalyst with the diameter of 1-2nm in the fuel cell comprises the following steps:
(1) Uniformly mixing nickel acetylacetonate, palladium acetylacetonate, formaldehyde solution, oleylamine and octadecyl trimethyl ammonium chloride, and then placing the mixture in an ultrasonic cleaner for ultrasonic treatment for more than 1 hour to obtain uniform mixed solution;
wherein, the mass ratio of nickel acetylacetonate to palladium acetylacetonate is 1:1.5-1.6, the mass ratio of octadecyl trimethyl ammonium chloride to palladium acetylacetonate is 25.3:1, the volume ratio of oleylamine to palladium acetylacetonate is 1.35:1, and the volume ratio of formaldehyde to palladium acetylacetonate is 1:16.3;
(2) Heating the mixed solution in a reaction kettle at the temperature of 195 ℃ for 15 hours;
(3) Mixing the reacted reagent with alcohol, washing and centrifuging at 9000rpm for 10min for 3-4 times to obtain a primary product, directly storing the primary product in a centrifuge tube, and then placing the centrifuge tube in a blast drying oven at 60 ℃ for drying overnight;
(4) Mixing the initial product with carbon black in the mass ratio of 1:4, adding ethanol, performing ultrasonic dispersion for 2h, mechanically stirring for 8h, centrifuging according to the centrifuging mode in the step (3), and drying to obtain the Pd-Ni/C nanosphere catalyst with the diameter of 1-2 nm.
Claims (4)
1. A method for preparing a Pd-Ni/C nanosphere catalyst with a diameter of 1-2nm in a fuel cell, which is characterized by comprising the following steps:
(1) Mixing palladium acetylacetonate, nickel acetylacetonate, octadecyl trimethyl ammonium chloride, oleylamine and formaldehyde in proportion, and performing ultrasonic treatment to obtain a mixed solution;
wherein, the mass ratio of nickel acetylacetonate to palladium acetylacetonate is 1:1.5-1.6, the mass ratio of octadecyl trimethyl ammonium chloride to palladium acetylacetonate is 25.1-25.5:1, the volume ratio of oleylamine to palladium acetylacetonate is 1.2-1.5:1, and the volume ratio of formaldehyde to palladium acetylacetonate is 1:16.0-16.6;
(2) Placing the mixed solution into a closed autoclave, and heating for 14-16 h at 190-200 ℃ to obtain a heating product;
(3) Washing the heated product with ethanol to obtain a primary product;
(4) Mixing the initial product with carbon black and ethanol, then carrying out ultrasonic treatment, stirring, centrifuging and drying to finally obtain the Pd-Ni/C nanosphere catalyst with the diameter of 1-2 nm.
2. The method for preparing a Pd-Ni/C nanosphere catalyst with a diameter of 1-2nm in a fuel cell according to claim 1, wherein the ultrasonic time in the step (1) is 1-1.5 hours.
3. The method for preparing a Pd-Ni/C nanosphere catalyst with a diameter of 1-2nm in a fuel cell according to claim 1, wherein in the step (4), the centrifugation reagent is alcohol, the centrifugation rate is 9000-9500 rpm, and the centrifugation times are 3-4 times.
4. The method for preparing a Pd-Ni/C nanosphere catalyst having a diameter of 1-2nm in a fuel cell according to claim 1, wherein in the step (4), the mass ratio of the initial product to the carbon black is 1:4.
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| CN104966841A (en) * | 2015-05-11 | 2015-10-07 | 同济大学 | Method for preparing Pd / NiCu two-dimensional nanocomposite |
| CN106582736A (en) * | 2015-10-20 | 2017-04-26 | 中国科学院大连化学物理研究所 | Pillared layered zirconium phosphate loaded nickel-based catalyst, preparation method and application thereof |
| CN108311712A (en) * | 2018-05-03 | 2018-07-24 | 济南大学 | A kind of preparation method of high catalytic performance polyhedral gold-palldium alloy nano material |
| CN111129528A (en) * | 2019-12-20 | 2020-05-08 | 中国科学院过程工程研究所 | Preparation method of PdNi double-alloy catalyst in fuel cell |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104966841A (en) * | 2015-05-11 | 2015-10-07 | 同济大学 | Method for preparing Pd / NiCu two-dimensional nanocomposite |
| CN106582736A (en) * | 2015-10-20 | 2017-04-26 | 中国科学院大连化学物理研究所 | Pillared layered zirconium phosphate loaded nickel-based catalyst, preparation method and application thereof |
| CN108311712A (en) * | 2018-05-03 | 2018-07-24 | 济南大学 | A kind of preparation method of high catalytic performance polyhedral gold-palldium alloy nano material |
| CN111129528A (en) * | 2019-12-20 | 2020-05-08 | 中国科学院过程工程研究所 | Preparation method of PdNi double-alloy catalyst in fuel cell |
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