CN114361477A - PdPb @ Pt cubic electrocatalyst and preparation method and application thereof - Google Patents
PdPb @ Pt cubic electrocatalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a PdPb @ Pt cubic electrocatalyst and a preparation method and application thereof. The preparation method specifically comprises the following steps: (1) dissolving a palladium source, a lead source, hexadecyl trimethyl ammonium bromide and octadecene in a solvent, and fully reacting after dissolving; (2) adding a platinum source after reacting for a period of time in step (1) and continuing the reaction; (3) and centrifuging and cleaning the obtained product, adding a proper amount of carbon powder, and drying in a vacuum oven to obtain the core-shell cubic structure containing three metals of Pd, Pb and Pt. The catalyst is used in a fuel cell. Compared with the prior art, the PdPb @ Pt disclosed by the invention has an obvious core-shell structure, can be used as an anode catalyst of a direct methanol fuel cell, and is obviously superior to the electrocatalytic activity and stability of commercial Pt/C.
Description
Technical Field
The invention relates to the technical field of fuel cells, in particular to a PdPb @ Pt cubic electrocatalyst and a preparation method and application thereof.
Background
Direct alcohol fuel cells are not limited to the carnot cycle and have attracted considerable attention by researchers through high energy conversion efficiency, portability, and operational flexibility in using a variety of fuels. However, since the anode reaction is slow, the efficiency of the anode reaction, i.e., the alcohol oxidation reaction, is low, which seriously hinders the wide use of the fuel cell. While the most important component in fuel cells is the catalyst, which is still a noble metal, Pt, at present, and although Pt has been widely used as an electrocatalyst for alcohol oxidation, it suffers from several serious problems including its scarcity, high cost and poor operational durability. The main reason for the low efficiency is the poor tolerance of Pt to toxic alcohol oxidation intermediates, especially CO.
Among various carbon-supported platinum (Pt) -based nanomaterials, small-sized Pt-based alloy Nanocrystals (NCS) are considered as a promising class of Ethanol Oxidation Reaction (EOR) electrocatalysts from the viewpoint of Pt atom utilization. While the activity of the catalyst can be improved by preparing Pt nanostructure catalysts in various forms, such as core-shell, hollow, Nanotube (NT), Nanowire (NW), nano-dendrite (ND), and porous structure. Due to the unique characteristics of the core-shell cube, the catalyst has great potential. Core-shell cubes are becoming a new class of superior electrocatalysts over commercial noble metal catalysts and most metal nanoparticle (Np) materials due to their high stability, abundant active centers and efficient mass/electron transport channels. They have excellent performance in various electrocatalytic processes such as Methanol Oxidation Reaction (MOR), Ethanol Oxidation Reaction (EOR) and Oxygen Evolution Reaction (OER).
However, small size Pt-based alloys generally exhibit poor stability and severe poisoning effects.
Disclosure of Invention
Based on the problems of poor stability and toxicity of small-size Pt-based alloys in the prior art, the invention provides a PdPb @ Pt cubic catalyst and a preparation method and application thereof.
The purpose of the invention can be realized by the following technical scheme:
the invention provides a preparation method of a PdPb @ Pt cubic catalyst, which specifically comprises the following steps:
(1) dissolving a palladium source, a lead source and a surfactant in a solvent, and reacting to generate a product after dissolving;
(2) adding Pt salt after reacting for a period of time in the step (1), and continuing to react;
(3) and (3) centrifuging and cleaning the product obtained in the step (2), adding carbon powder, and drying to obtain the catalyst with a core-shell cubic structure containing Pd, Pb and Pt, namely the PdPb @ Pt cubic catalyst.
In one embodiment of the present invention, in the step (1), the palladium source is palladium acetylacetonate (Pd (acac)2) The lead source is lead acetylacetonate (Pb (acac)2)。
In one embodiment of the present invention, in step (1), Pd (acac)2And Pb (acac)2Is 3: 1.
In one embodiment of the present invention, in step (1), the surfactant is selected from dodecyl trimethyl ammonium bromide (CTAB).
In one embodiment of the invention, in the step (1), the solvent is a mixed solvent obtained by mixing oleylamine and octadecene according to a volume ratio of 1: 1-3: 2.
In one embodiment of the invention, in step (1), ultrasonic-assisted dissolution and stirring are used to mix the components uniformly.
In one embodiment of the present invention, in the step (1), the reaction temperature is 180 ℃ and the reaction time is 3 hours.
In one embodiment of the present invention, in step (2), the Pt salt is selected to be H2PtCl6·6H2O。
In one embodiment of the present invention, in the steps (1) and (2), Pd (acac)2、Pb(acac)2And H2PtCl6·6H2The molar ratio of O is 3:1: 2.
In one embodiment of the present invention, in the step (2), the temperature for continuing the reaction is 180 ℃ and the reaction time is 3 hours.
In one embodiment of the present invention, in the step (3), the product obtained in the step (2) is washed with ethanol and cyclohexane, and the washing stirring time is 3 hours.
In one embodiment of the invention, in the step (3), a proper amount of carbon powder is added, so that the content of the noble metal Pd accounts for 20% of the total mass.
In one embodiment of the present invention, in step (3), after adding carbon powder, performing ultrasonic treatment to pulverize large-particle carbon powder, and performing stirring can make the catalyst better loaded.
In one embodiment of the invention, in the step (3), the drying is performed under a vacuum condition, the drying temperature is 50-70 ℃, and the drying time is 7-10 h.
The invention also provides the PdPb @ Pt cubic electrocatalyst prepared by the preparation method, which has a core-shell cubic structure, wherein the PdPb cube is a core, and the surface of the PdPb cube is coated with a layer of Pt shell.
The method synthesizes a PdPb cube firstly, then coats a layer of Pt shell on the surface of the PdPb cube to form a metal alloy, and Pt is alloyed with other metals to adjust the electronic structure of Pt, so that the adsorption of CO is weakened, the oxidation performance of ethanol is promoted to be greatly improved, the oxidation potential of CO on the surface of Pt is obviously reduced, and the oxidation of CO on the Pt site is promoted.
The invention also provides an application of the PdPb @ Pt cubic electrocatalyst in a fuel cell.
Compared with the prior art, the invention has the beneficial effects that:
the PdPb @ Pt cubic electrocatalyst is synthesized by a simple solvothermal method, a cubic alloy structure formed among three metals forms a more effective synergistic effect, the product performance is improved, compared with the traditional Pt/C catalyst, the catalyst provided by the invention reduces the using amount of noble metals, the utilization rate of the catalyst is improved, the electrocatalytic oxidation activity and the catalytic stability of ethanol are improved by Pt-based materials, the CO poisoning resistance is improved, the catalyst can be used as an anode catalyst of a direct ethanol fuel cell, and the preparation process is simple and safe.
Drawings
FIG. 1 is a TEM image of a transmission electron microscope of a PdPb @ Pt cubic catalyst prepared in example 1;
FIG. 2 is an energy dispersive X-ray spectroscopy (EDS) of the PdPb @ Pt cubic catalyst prepared in example 1;
FIG. 3 is an XRD pattern of the PdPb @ Pt cubic catalyst prepared in example 1;
FIG. 4a is a comparison of cyclic voltammetry tests of the catalysts of example 1 and comparative example 1 in a 1M NaOH solution;
FIG. 4b shows the results of the catalysts of example 1 and comparative example 1 in 1M NaOH +1M CH3CH2Comparison graph of cyclic voltammetry test in mixed solution of OH;
FIG. 4c shows the results of the catalysts of example 1 and comparative example 1 in 1M NaOH +1M CH3CH2Comparison of the highest mass activity in the mixed solution of OH;
FIG. 4d shows the catalysts of example 1 and comparative example 1 in 1M NaOH +1M CH3CH2Comparative plot of chronoamperometry in OH mixed solution.
Detailed Description
The invention provides a preparation method of a PdPb @ Pt cubic catalyst, which specifically comprises the following steps:
(1) general formula (Pd) (acac)2、Pb(acac)2Dissolving CTAB in solvent, dissolving with ultrasonic wave, reacting at 180 deg.C for 3 hr, and adding certain amount of H2PtCl6·6H2And O, reacting for 3 hours. In this step, Pd (acac)2And Pb (acac)2The reaction between the two to generate PdPb cubes, Pd (acac)2、Pb(acac)2And H2PtCl6·6H2The molar ratio of O is 3:1:2, and the solvent is obtained by mixing oleylamine and octadecene according to the volume ratio of 1: 1;
(2) and (2) collecting the product in the step (1), centrifuging, cleaning with ethanol and cyclohexane, adding 26mg of carbon powder, performing ultrasonic stirring, and performing suction filtration. Drying the obtained sample under a vacuum condition, wherein the drying temperature is 50-70 ℃, and the drying time is 7-10 h;
the PdPb @ Pt cubic structure catalyst obtained by the preparation method has a stable structure, particle agglomeration caused by long-time work is avoided, and the cubic structure enables the catalyst to have excellent electrocatalytic activity and CO poisoning resistance.
Use of a PdPb @ Pt cubic electrocatalyst as described above in a fuel cell.
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
A PdPb @ Pt cubic electrocatalyst for a fuel cell is prepared by the following preparation steps:
(1) the molar ratio of the components is 3:1:2, respectively taking 0.03mmol Pd (acac)2、0.01mmol Pb(acac)2Dissolving 200mg CTAB in oleylamine/octadecene mixed solvent with volume ratio of 1:1, performing ultrasonic dissolution, reacting at 180 ℃ for 3H, and adding 0.01mmol H2PtCl6·6H2And O, reacting for 3 hours to obtain the product.
(2) And centrifuging the reaction system, washing with ethanol cyclohexane, and collecting a product.
(3) The obtained dried product was placed in a flask, 18mg of carbon powder was added to perform ultrasonication for 0.5h, stirring was performed for 3h, then suction filtration was performed, and the sample was placed in a vacuum oven and dried overnight at 60 ℃.
The TEM images of the PdPb @ Pt cubes are shown in fig. 1 and 2, and it can be seen that the overall outline of the catalyst is a cube, a plurality of cubes are seen to be gathered together at a magnification of 100nm, the sizes are almost the same, and a complete cube structure is seen inside at a magnification of 50nm, and the surface is coated with a layer of Pt shell.
An XRD pattern of the PdPb @ Pt cube is shown in figure 3, and a diffraction peak at 22.765 degrees, a characteristic diffraction peak belonging to a graphitized carbon (120) crystal face, shows a relatively obvious diffraction peak of C, and peaks at 38.8 degrees, 45.1 degrees, 65.5 degrees and 78.7 degrees respectively correspond to PtxPbJCPDS 06-0374, so that the catalyst is proved to contain PtPb alloy and to have high alloying degree.
Placing PdPb @ Pt cubic catalyst in 1M NaOH +1M CH3CH2The cyclic voltammetry test was performed in a mixed solution of OH (same test conditions) as a half cell reaction using ethanol as an anode active material (same test conditions), and the test result is shown in fig. 4 b.
A-0.2V (vs SCE)3600s chronoamperometric test was performed on the PdPb @ Pt cubic catalyst, the test results of which are shown in FIG. 4 d.
Example 2
A PdPb @ Pt cubic electrocatalyst for a fuel cell is prepared by the following preparation steps:
(1) the molar ratio of the components is 3:1:2, respectively taking 0.03mmol Pd (acac)2、0.01mmol Pb(acac)2Dissolving 200mg CTAB in oleylamine/octadecene mixed solvent with volume ratio of 3:2, performing ultrasonic dissolution, reacting at 180 ℃ for 3H, and adding 0.02mmol H2PtCl6·6H2And O, reacting for 3 hours to obtain the product.
(2) And centrifuging the reaction system, washing with ethanol cyclohexane, and collecting a product.
(3) The obtained dried product was placed in a flask, 26mg of carbon powder was added to perform ultrasonication for 0.5h, stirring was performed for 3h, then suction filtration was performed, and the sample was placed in a vacuum drying oven and dried overnight at 60 ℃.
Obtaining the PdPb @ Pt cubic electrocatalyst for the fuel cell.
Example 3
A PdPb @ Pt cubic electrocatalyst for a fuel cell is prepared by the following preparation steps:
(1) the molar ratio of the components is 3:1:2, respectively taking 0.03mmol Pd (acac)2、0.01mmol Pbacac)2Dissolving 200mg CTAB in oleylamine/octadecene mixed solvent with volume ratio of 1:1, performing ultrasonic dissolution, reacting at 180 ℃ for 3H, and adding 0.03mmol H2PtCl6·6H2And O, reacting for 3 hours to obtain the product.
(2) And centrifuging the reaction system, washing with ethanol cyclohexane, and collecting a product.
(3) The obtained dried product was placed in a flask, 34mg of carbon powder was added to perform ultrasonication for 0.5h, stirring was performed for 3h, then suction filtration was performed, and the sample was placed in a vacuum oven and dried overnight at 60 ℃.
Obtaining the PdPb @ Pt cubic electrocatalyst for the fuel cell.
Comparative example 1
A commercial catalyst JM 20% Pt/C, obtained from Johnson-Matthery, was subjected to a linear cyclic voltammetry test, as shown in FIGS. 4a and b, and to a chronoamperometry test, as shown in FIG. 4 d.
As can be seen from FIG. 4a, the initial potential of the PdPb @ Pt cubic electrocatalyst shifts to the left significantly (the initial oxidation potential is the potential at which oxidation begins to occur, and the initial oxidation potential of the PdPb @ Pt cubic electrocatalyst in FIG. 4b is to the left of the initial oxidation potential of JM 20% Pt/C, indicating an increase in its CO poisoning resistance and a significant enhancement in oxidation peak current density of 6314mA mg-1 PtAbout the commercial catalyst JM 20% Pt/C (1475 mA mg)-1 Pt) 4.3 times of that of the catalyst, which shows that the unique structure of the PdPb-Pt cube can enable the catalyst to have obvious catalytic ethanol electro-oxidation activity.
Catalysts of example 1 and comparative example 1 in 1M NaOH +1M CH3CH2The highest mass activity in the OH mixed solution is shown in FIG. 4 c.
From FIG. 4d it can be seen that commercial catalyst JM 20% Pt/C is affected by CO or some intermediates (both CO and some intermediates are generated during the reaction) and that the current density is from 1475mA mg after 3600s-1 PtTending to 105mA mg-1 PtThe attenuation process of the PdPb @ Pt cubic catalyst is obviously mild, and the current density is changed from 6314mA mg after 3600s-1 PtStill as high as 1930mA mg-1 Pt. The PdPb @ Pt cubic catalyst provided by the invention is obviously improved in catalytic stability in the ethanol electrooxidation process.
In conclusion, the invention provides a PdPb @ Pt cubic electrocatalyst synthesized by a simple operation method, and the catalyst has a complete cubic structure. The catalyst can be used in the oxidation process of ethanol and shows remarkably enhanced electrochemical performance.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A preparation method of the PdPb @ Pt cubic catalyst is characterized by comprising the following steps:
(1) dissolving a palladium source, a lead source and a surfactant in a solvent, and reacting to generate a product after dissolving;
(2) adding Pt salt after reacting for a period of time in the step (1), and continuing to react;
(3) and (3) centrifuging and cleaning the product obtained in the step (2), adding carbon powder, and drying to obtain the catalyst with a core-shell cubic structure containing Pd, Pb and Pt, namely the PdPb @ Pt cubic catalyst.
2. The preparation method of the PdPb @ Pt cubic catalyst as claimed in claim 1, wherein in the step (1), the palladium source is palladium acetylacetonate, the lead source is lead acetylacetonate, and the molar ratio of the palladium acetylacetonate to the lead acetylacetonate is 3: 1.
3. The method for preparing the PdPb @ Pt cubic catalyst as claimed in claim 1, wherein in the step (1), the surfactant is dodecyl trimethyl ammonium bromide.
4. The preparation method of the PdPb @ Pt cubic catalyst as claimed in claim 1, wherein in the step (1), the solvent is a mixed solvent obtained by mixing oleylamine and octadecene according to a volume ratio of 1: 1-3: 2.
5. The preparation method of the PdPb @ Pt cubic catalyst as claimed in claim 1, wherein in the step (1), the reaction temperature is 180 ℃ and the reaction time is 3 h.
6. The method for preparing PdPb @ Pt cubic catalyst as claimed in claim 1, wherein in step (2), the Pt salt is selected from H2PtCl6·6H2O；
In the steps (1) and (2), Pd (acac)2、Pb(acac)2And H2PtCl6·6H2The molar ratio of O is 3:1: 2.
7. The method for preparing the PdPb @ Pt cubic catalyst as claimed in claim 1, wherein in the step (2), the reaction is continued at 180 ℃ for 3 h.
8. The preparation method of the PdPb @ Pt cubic catalyst as claimed in claim 1, wherein in the step (3), the product obtained in the step (2) is washed with ethanol and cyclohexane for 3 hours under stirring;
in the step (3), after adding the carbon powder, carrying out ultrasonic treatment to crush the large-particle carbon powder;
and (3) drying under a vacuum condition, wherein the drying temperature is 50-70 ℃, and the drying time is 7-10 h.
9. The PdPb @ Pt cubic electrocatalyst prepared by the preparation method of any one of claims 1-8 is characterized by having a core-shell cubic structure, wherein the PdPb cube is a core, and a Pt shell is coated on the surface of the PdPb cube.
10. Use of the PdPb @ Pt cubic electrocatalyst according to claim 9 in a fuel cell.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114959788A (en) * | 2022-06-14 | 2022-08-30 | 安徽大学 | Preparation of oxophilic metal doped network-shaped PdH/C and application thereof in ethanol electrocatalytic oxidation |
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| CN113036168A (en) * | 2021-03-04 | 2021-06-25 | 合肥工业大学 | Cubic PtPd @ Pt core-shell nano cage electrocatalyst and preparation method and application thereof |
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| CN107887619A (en) * | 2017-10-27 | 2018-04-06 | 北京航天动力研究所 | A kind of Pt Pd alloy catalysts of morphology controllable and preparation method and application |
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| CN114959788A (en) * | 2022-06-14 | 2022-08-30 | 安徽大学 | Preparation of oxophilic metal doped network-shaped PdH/C and application thereof in ethanol electrocatalytic oxidation |
| CN114959788B (en) * | 2022-06-14 | 2024-01-30 | 安徽大学 | Preparation of aerophilic metal doped network PdH/C and application thereof in electrocatalytic oxidation of ethanol |
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