CN110797543A - Multi-hole ultrathin palladium nanosheet catalyst and preparation method and application thereof - Google Patents

Multi-hole ultrathin palladium nanosheet catalyst and preparation method and application thereof Download PDF

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CN110797543A
CN110797543A CN201910958519.3A CN201910958519A CN110797543A CN 110797543 A CN110797543 A CN 110797543A CN 201910958519 A CN201910958519 A CN 201910958519A CN 110797543 A CN110797543 A CN 110797543A
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methanol
hole
ultrathin
catalyst
palladium
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张连营
欧阳伊睿
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Qingdao University
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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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
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
    • 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
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    • 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

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Abstract

The invention belongs to the technical field of direct formic acid fuel cell electrocatalysts, and relates to a multi-hole ultrathin palladium nanosheet catalyst, and a preparation method and application thereof. The method comprises the following steps: (1) introducing inert gas or nitrogen into the methanol to remove oxygen dissolved in the methanol, and then heating the methanol to a certain temperature; (2) introducing carbon monoxide into the methanol obtained in the step (1) until the methanol is saturated; (3) adding sodium chloropalladate into another part of methanol, introducing inert gas or nitrogen to remove oxygen dissolved in the solution, adding the sodium chloropalladate into the methanol saturated by the carbon monoxide obtained in the step (2), and continuing to react; (4) and (4) cleaning the product obtained in the step (3). The catalyst prepared by the invention has the advantages of super large electrochemical activity specific surface area, ultrahigh formic acid catalytic oxidation activity and excellent electrochemical stability, and the method does not relate to the use of surface active materials such as polyvinylpyrrolidone (PVP), cetyltrimethylammonium bromide (CTAB) and the like.

Description

Multi-hole ultrathin palladium nanosheet catalyst and preparation method and application thereof
Technical Field
The invention belongs to the technical field of direct formic acid fuel cell electrocatalysts, and relates to a multi-hole ultrathin palladium nanosheet catalyst, and a preparation method and application thereof.
Background
The fuel cell is a device for directly converting chemical energy into electric energy, has the characteristics of high energy conversion efficiency, environmental friendliness, easiness in assembly and the like, and has important application potential in the aspects of electric automobiles, portable power supplies and the like. The direct formic acid fuel cell is an important fuel cell. The battery takes liquid formic acid as anode fuel, has higher safety in the processes of storage, transportation, use and the like, and the formate and the perfluorosulfonate in the proton exchange membrane have electrostatic repulsion, so that the permeability of formic acid passing through the proton exchange membrane is reduced. However, the electrocatalytic oxidation kinetics of formic acid in the anode of a direct formic acid fuel cell is relatively slow, and becomes an important factor limiting the commercial development thereof. Currently, the most commonly used anode catalyst for direct formic acid fuel cells is a palladium/carbon catalyst. The catalyst has smaller electrochemical activity specific surface area, higher surface energy of palladium nano particles is easy to generate agglomeration and the like, so that the performance of the electro-catalytic oxidation of formic acid is lower. Therefore, the research and preparation of high-performance palladium catalysts are of great significance for accelerating the commercial development of direct formic acid fuel cells.
The two-dimensional electrode material has unique anisotropy and electronic performance, is applied to electrocatalysis, energy conversion, storage and other aspects, and shows great application potential. For the ultrathin palladium nanosheets, the ultrahigh specific surface area means that more surface atoms can be exposed, so that the ultrathin palladium nanosheets can contact with electrolyte and reactant molecules in a larger proportion and can also serve as catalytic active sites, and the electrooxidation catalytic performance of formic acid is greatly improved. Meanwhile, due to the unique two-dimensional structure of the ultrathin palladium nanosheet, the dissolution and Ostwald ripening of surface atoms under high potential can be inhibited to a certain extent, so that the ultrathin palladium nanosheet has high electrochemical stability. Current research indicates that ultra-thin palladium nanoplates do exhibit significant performance enhancements as electrocatalytic oxidations of formic acid over commercial palladium/carbon catalysts (Nature nanotechnology,2011,6, 28.; Journal of colloid and Interface Science,20158,532,485.). Then, in order to meet the needs of current commercialization, the performance of the electrocatalytic oxidation of formic acid of the ultrathin palladium nanosheets still needs to be further improved.
Because the formic acid electro-oxidation catalysis process relates to a diffusion control process, a multi-hole structure is designed and constructed on the basis of the ultrathin palladium nanosheets, and fast electrolyte diffusion can be realized theoretically, so that the electrode process dynamics is greatly improved, the electrochemical specific surface area is further increased, and more catalytic active sites are provided to improve the formic acid electro-catalytic oxidation current density. At present, the construction of a multi-hole ultrathin palladium nanosheet structure is not realized.
Disclosure of Invention
The invention aims to overcome the defects of the existing palladium/carbon catalyst and provides a preparation method of a multi-hole ultrathin palladium nanosheet catalyst, which is simple and convenient to operate, easy to repeat and suitable for large-scale synthesis; compared with a commercial palladium/carbon catalyst, the multi-hole ultrathin palladium nanosheet catalyst prepared by the preparation method has ultrahigh formic acid electrocatalytic oxidation peak current density and excellent electrochemical stability; the invention also aims to provide the application of the multi-hole ultrathin palladium nanosheet catalyst in the formic acid oxidation electrocatalytic reaction.
The invention is realized by adopting the following technical scheme:
the invention provides a preparation method of a multi-hole ultrathin palladium nanosheet catalyst, which comprises the following steps:
(1) introducing inert gas or nitrogen into the methanol to remove oxygen dissolved in the methanol, and then heating the methanol to a certain temperature;
(2) introducing carbon monoxide into the methanol obtained in the step (1) until the carbon monoxide is saturated;
(3) adding sodium chloropalladate into another part of methanol, introducing inert gas or nitrogen to remove oxygen dissolved in the solution, adding the sodium chloropalladate into the methanol saturated with carbon monoxide obtained in the step (2), and continuing to react;
(4) and (4) cleaning the product prepared in the step (3).
Specifically, the heating temperature range in the step (1) is 40-80 ℃.
Specifically, the flow rate of the carbon monoxide in the step (2) is 70mL/min to 120 mL/min.
Wherein the final concentration of the sodium chloropalladate in the system obtained by mixing the two parts of methanol in the step (3) is 0.05-0.3 mg/mL.
Wherein the reaction time in the step (3) is 3-30 min.
The invention also provides a multi-hole ultrathin palladium nanosheet catalyst prepared by the preparation method.
The invention also provides an application of the multi-hole ultrathin palladium nanosheet catalyst in formic acid oxidation electrocatalytic reaction.
The invention has the beneficial effects that: the invention discloses a preparation method of a multi-hole ultrathin palladium nanosheet catalyst, which is used for obtaining a two-dimensional material of a multi-hole ultrathin palladium nanosheet and effectively improving the electro-catalytic activity and stability of formic acid. Compared with a commercial palladium/carbon catalyst, the prepared multi-hole ultrathin palladium nanosheet catalyst not only has an ultra-large electrochemical activity specific surface area, but also can show more active sites to promote effective implementation of electrocatalysis reaction and improvement of electrode process dynamics, namely higher formic acid oxidation catalytic activity; the two-dimensional material has stronger Ostwald ripening resistance, so that higher stability is shown in the formic acid electrooxidation process, and the catalyst can replace a commercial palladium/carbon catalyst to be applied to the fields of direct formic acid fuel cells and other energy storage and conversion, and has higher practical value; the method does not relate to the use of surface active materials such as polyvinylpyrrolidone PVP, cetyltrimethylammonium bromide CTAB and the like, is simple and convenient to operate, has high repeatability, can be prepared in a large scale and has a potential important application prospect.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
In the drawings:
FIG. 1 is a transmission electron microscope image of the multi-hole ultrathin palladium nanosheet catalyst prepared in example 1.
FIG. 2 shows the multi-hole ultrathin palladium nanosheet catalyst prepared in example 1 and a commercial palladium/carbon catalyst at 0.5MH2SO4Comparison of cyclic voltammograms in solution.
FIG. 3 shows the multi-hole ultrathin palladium nanosheet catalyst prepared in example 1 and a commercial palladium/carbon catalyst at 0.5MH2SO4Comparative graph of catalytic activity in +0.5M HCOOH solution.
FIG. 4 shows the multi-hole ultrathin palladium nanosheet catalyst prepared in example 1 and a commercial palladium/carbon catalyst at 0.5MH2SO4Comparative graph of stability test current versus time curves in +0.5M HCOOH solution.
Fig. 5 is a transmission electron microscope image of the multi-hole ultrathin palladium nanosheet catalyst prepared in example 2.
FIG. 6 shows the multi-hole ultrathin palladium nanosheet catalyst prepared in example 2 and a commercial palladium/carbon catalyst at 0.5MH2SO4Comparison of cyclic voltammograms in solution.
FIG. 7 shows the multi-hole ultrathin palladium nanosheet catalyst prepared in example 2 and a commercial palladium/carbon catalyst at 0.5MH2SO4Comparative graph of catalytic activity in +0.5M HCOOH solution.
FIG. 8 shows the multi-hole ultrathin palladium nanosheet catalyst prepared in example 2 and a commercial palladium/carbon catalyst at 0.5MH2SO4Comparative graph of stability test current versus time curves in +0.5M HCOOH solution.
Detailed Description
In order to make the purpose and technical solution of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings. The experimental methods described in the following examples are all conventional methods unless otherwise specified; the specific techniques or conditions are not indicated in the examples, and the techniques or conditions are described in the literature in the field or according to the product specification; the reagents and materials are commercially available, unless otherwise specified.
A commercial palladium on carbon catalyst is product number P116795 available from Aladdin.
The following examples use nitrogen which has a purity of 99.999% (O)2Not more than 0.001%), is high-purity nitrogen grade, and the purity of CO is 99.999%.
Example 1
(1) Nitrogen was bubbled through 53mL of methanol for 30min to remove dissolved oxygen in the methanol, followed by adjusting the methanol to 60 ℃;
(2) introducing carbon monoxide into the methanol until the carbon monoxide is saturated, wherein the flow rate of the CO is 80 mL/min;
(3) adding 12mg of sodium chloropalladate into 2mL of methanol, introducing nitrogen to remove oxygen dissolved in the solution, quickly adding the solution into the methanol saturated with carbon monoxide obtained in the step (2), and continuously reacting for 5 min;
(4) and (4) carrying out centrifugal cleaning on the product prepared in the step (3).
FIG. 1 is a transmission electron microscope image of the multi-hole ultrathin palladium nanosheet catalyst prepared in this example 1; the prepared multi-hole ultrathin palladium nanosheet catalyst has an obvious multi-hole structure as can be clearly seen from the figure.
Formulation 0.5M H2SO4The solution was used as an electrolyte solution, nitrogen gas was introduced into the solution for ten minutes, and then a reference electrode (saturated calomel electrode), a counter electrode (platinum electrode) and a working electrode (catalyst of the present example and commercial palladium/carbon catalyst, respectively) were inserted under the protection of nitrogen gas; adjusting scanning conditions of cyclic voltammetry: the lowest scanning voltage is-0.25V, the highest scanning voltage is 1.1V, and the scanning speed is 50 mV/s; the recording of cyclic voltammograms was then started as shown in figure 2. Compared with commercial palladium/carbon catalyst (40.1 m)2/g), the catalyst of the porous ultrathin palladium nanosheet prepared in the example 1 shows higher electrochemical activity specific surface area (172.6 m)2G), demonstrating that the multi-hole ultrathin palladium nanosheet catalyst prepared in this example 1 has more catalytically active sites than commercial palladium/carbon catalysts.
Formulation 0.5M H2SO4+0.5M HCOOH solution as an electrolyte solution, and introducing nitrogen gas into the solution for ten minutes, and then inserting a reference electrode (saturated calomel electrode), a counter electrode (platinum electrode) and a working electrode (catalyst of this example and commercial palladium/carbon catalyst, respectively) under the protection of nitrogen gas; adjusting scanning conditions of cyclic voltammetry: the lowest scanning voltage is-0.25V, the highest scanning voltage is 1.1V, and the scanning speed is 50 mV/s; then, a cyclic voltammetry curve is recorded, and the current density and the potential corresponding to the highest peak in the curve are recordedAre the peak current density and the peak potential. As shown in FIG. 3, and a commercial palladium/carbon catalyst (473.8 mA/mg)pd) Compared with the catalyst prepared by the method in the embodiment 1, the catalyst prepared by the porous ultrathin palladium nanosheet has larger peak current density (2653.3 mA/mg)Pd) Meanwhile, the initial oxidation potential (-0.12V) of the multi-hole ultrathin palladium nanosheet catalyst is found to be smaller than the value of the commercial palladium/carbon catalyst (-0.07V), which indicates that the multi-hole ultrathin palladium nanosheet catalyst prepared in the embodiment 1 has higher formic acid catalytic oxidation activity compared with the commercial palladium/carbon catalyst.
Formulation 0.5M H2SO4+0.5M HCOOH solution as an electrolyte solution, and introducing nitrogen gas into the solution for ten minutes, and then inserting a reference electrode (saturated calomel electrode), a counter electrode (platinum electrode) and a working electrode (catalyst of this example and commercial palladium/carbon catalyst, respectively) under the protection of nitrogen gas; the recording of the amp-timing curve is then started as shown in fig. 4.
At the beginning of operation, the current density of the multi-hole ultrathin palladium nanosheet catalyst is 392.6mA/mg, the current density of the commercial palladium/carbon catalyst is only 125.2mA/mg, after 3000s of operation, the current density of the multi-hole ultrathin palladium nanosheet catalyst is 80.1mA/mg, the current density of the commercial palladium/carbon catalyst is only 17.9mA/mg, and the current density of the multi-hole ultrathin palladium nanosheet catalyst always shows higher current density, which indicates that the multi-hole ultrathin palladium nanosheet catalyst prepared in example 1 has higher formic acid catalytic activity and better electrochemical stability for formic acid catalytic oxidation compared with the commercial palladium/carbon catalyst.
The experimental data show that the multi-hole ultrathin palladium nanosheet catalyst prepared in the embodiment 1 has an oversized electrochemical activity specific surface area, ultrahigh formic acid catalytic oxidation activity and excellent electrochemical stability for formic acid catalytic oxidation compared with a commercial palladium/carbon catalyst, so that the catalyst can be applied to the fields of direct formic acid fuel cells and other energy conversion instead of the commercial palladium/carbon catalyst.
Example 2
(1) Nitrogen was bubbled through 48mL of methanol for 30min to remove dissolved oxygen from the methanol, then the methanol was adjusted to 40 ℃;
(2) introducing carbon monoxide into the methanol until the carbon monoxide is saturated, wherein the flow rate of the CO is 100 mL/min;
(3) adding 5mg of sodium chloropalladate into 2mL of methanol, introducing nitrogen to remove oxygen dissolved in the solution, quickly adding the solution into the methanol saturated with carbon monoxide obtained in the step (2), and continuously reacting for 10 min;
(4) and (4) carrying out centrifugal cleaning on the product prepared in the step (3).
FIG. 5 is a transmission electron microscope image of the multi-hole ultrathin palladium nanosheet catalyst prepared in this example 2; the prepared multi-hole ultrathin palladium nanosheet catalyst has an obvious multi-hole structure as can be clearly seen from the figure.
The performance test of the multi-hole ultrathin palladium nanosheet catalyst prepared in this example 2 was performed by the same test method as in example 1.
FIG. 6 shows the multi-hole ultrathin palladium nanosheet catalyst and the commercial palladium/carbon catalyst prepared in example 2 at 0.5MH2SO4A comparison graph of cyclic voltammograms in solution; found to be comparable to commercial palladium/carbon catalysts (40.1 m)2/g), the catalyst of the porous ultrathin palladium nanosheet prepared in the example 2 shows a larger electrochemical activity specific surface area (168.4 m)2G), indicating that the multi-hole ultrathin palladium nanosheet catalyst prepared in this example 2 has more catalytically active sites than the commercial palladium/carbon catalyst.
FIG. 7 shows the multi-hole ultrathin palladium nanosheet catalyst and the commercial palladium/carbon catalyst prepared in example 2 at 0.5MH2SO4Comparative plot of catalytic activity in +0.5M HCOOH solution; palladium/carbon catalysts (473.8 mA/mg) were discovered and commercializedPd) Compared with the catalyst prepared in the embodiment 2, the catalyst prepared in the embodiment 2 has higher peak current density (2470.6 mA/mg)Pd) Meanwhile, the initial oxidation potential (-0.12V) of the multi-hole ultrathin palladium nanosheet catalyst is found to be smaller than the value of the commercial palladium/carbon catalyst (-0.07V), which indicates that the multi-hole ultrathin palladium nanosheet catalyst prepared in the embodiment 2 has higher formic acid catalytic oxidation activity compared with the commercial palladium/carbon catalyst.
FIG. 8 shows the exampleThe catalyst of the multi-hole ultrathin palladium nanosheet prepared in example 2 was at 0.5M H2SO4Comparative stability testing graphs for +0.5M HCOOH solutions; at the beginning of operation, the current density of the multi-hole ultrathin palladium nanosheet catalyst is 411.4mA/mg, the current density of the commercialized palladium/carbon catalyst is only 125.2mA/mg, after 3000s of operation, the current density of the multi-hole ultrathin palladium nanosheet catalyst is 89.6mA/mg, the current density of the commercialized palladium/carbon catalyst is only 17.9mA/mg, and the current density of the multi-hole ultrathin palladium nanosheet catalyst always shows higher current density, which indicates that the multi-hole ultrathin palladium nanosheet catalyst prepared in example 2 has higher formic acid catalytic activity and better electrochemical stability for formic acid catalytic oxidation compared with the commercialized palladium/carbon catalyst.
The experimental data show that the multi-hole ultrathin palladium nanosheet catalyst prepared in the embodiment 2 has an oversized electrochemical activity specific surface area, ultrahigh formic acid catalytic oxidation activity and excellent electrochemical stability for formic acid catalytic oxidation compared with a commercial palladium/carbon catalyst, so that the catalyst can be applied to the fields of direct formic acid fuel cells and other energy conversion instead of the commercial palladium/carbon catalyst.
It should be understood that the above description is only a preferred embodiment of the present invention, and not intended to limit the present invention, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents may be made in the technical solutions described in the foregoing embodiments, or some technical features may be substituted. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. A preparation method of a multi-hole ultrathin palladium nanosheet catalyst is characterized by comprising the following steps:
(1) introducing inert gas or nitrogen into the methanol to remove oxygen dissolved in the methanol, and then heating the methanol to a certain temperature;
(2) introducing carbon monoxide into the methanol obtained in the step (1) until the carbon monoxide is saturated;
(3) adding sodium chloropalladate into another part of methanol, introducing inert gas or nitrogen to remove oxygen dissolved in the solution, adding the sodium chloropalladate into the methanol saturated with carbon monoxide obtained in the step (2), and continuing to react;
(4) and (4) cleaning the product prepared in the step (3).
2. The method for preparing a multi-hole ultrathin palladium nanosheet catalyst as recited in claim 1, wherein the heating temperature in step (1) is in a range of 40 ℃ to 80 ℃.
3. The preparation method of the multi-hole ultrathin palladium nanosheet catalyst according to claim 1, wherein the flow rate of the carbon monoxide in the step (2) is 70-120 mL/min.
4. The preparation method of the multi-hole ultrathin palladium nanosheet catalyst according to claim 1, wherein the final concentration of sodium chloropalladate in the system obtained by mixing the two parts of methanol in the step (3) is 0.05-0.3 mg/mL.
5. The preparation method of the multi-hole ultrathin palladium nanosheet catalyst according to claim 1, wherein the reaction continuing time in the step (3) is 3-30 min.
6. A multi-hole ultrathin palladium nanosheet catalyst prepared by the preparation method of any one of claims 1-5.
7. The application of the multi-hole ultrathin palladium nanosheet catalyst disclosed by claim 6 in formic acid oxidation electrocatalytic reaction.
CN201910958519.3A 2019-10-10 2019-10-10 Multi-hole ultrathin palladium nanosheet catalyst and preparation method and application thereof Withdrawn CN110797543A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114669753A (en) * 2022-01-20 2022-06-28 华东理工大学 Ultrathin palladium nanosheet with defect-rich surface and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114669753A (en) * 2022-01-20 2022-06-28 华东理工大学 Ultrathin palladium nanosheet with defect-rich surface and preparation method thereof
CN114669753B (en) * 2022-01-20 2023-11-10 华东理工大学 Ultrathin palladium nano-sheet with surface rich in defects and preparation method thereof

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Application publication date: 20200214