CN114464823A - Oxygen reduction reaction catalyst and preparation method thereof - Google Patents
Oxygen reduction reaction catalyst and preparation method thereof Download PDFInfo
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- CN114464823A CN114464823A CN202210069571.5A CN202210069571A CN114464823A CN 114464823 A CN114464823 A CN 114464823A CN 202210069571 A CN202210069571 A CN 202210069571A CN 114464823 A CN114464823 A CN 114464823A
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- oxygen reduction
- reduction reaction
- phenanthroline
- reaction catalyst
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 24
- 239000001301 oxygen Substances 0.000 title claims abstract description 24
- 238000006722 reduction reaction Methods 0.000 title claims abstract description 23
- 239000007809 chemical reaction catalyst Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000002073 nanorod Substances 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 6
- 229910020427 K2PtCl4 Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- CASFCVRUBIJLBN-UHFFFAOYSA-N 2-(1,10-phenanthrolin-2-yl)ethanol Chemical compound OCCc1ccc2ccc3cccnc3c2n1 CASFCVRUBIJLBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910019029 PtCl4 Inorganic materials 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000002243 precursor Substances 0.000 abstract description 9
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010668 complexation reaction Methods 0.000 abstract description 2
- 239000008139 complexing agent Substances 0.000 abstract description 2
- 230000005518 electrochemistry Effects 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 229910052697 platinum Inorganic materials 0.000 abstract description 2
- 229910052700 potassium Inorganic materials 0.000 abstract description 2
- 239000011591 potassium Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 6
- 125000004429 atom Chemical group 0.000 description 4
- 239000010411 electrocatalyst Substances 0.000 description 4
- 239000000446 fuel Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 208000001408 Carbon monoxide poisoning Diseases 0.000 description 1
- 238000001016 Ostwald ripening Methods 0.000 description 1
- 230000010757 Reduction Activity Effects 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004502 linear sweep voltammetry Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- 238000001075 voltammogram Methods 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
- H01M4/928—Unsupported catalytic particles; loose particulate catalytic materials, e.g. in fluidised state
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
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Abstract
The invention belongs to the technical field of electrochemistry, and particularly relates to an oxygen reduction reaction catalyst and a preparation method thereof. The preparation method takes phenanthroline as a complexing agent, potassium chloroplatinite as a platinum source, ethanol and water as solvents, and utilizes Pt2+And performing strong complexation with phenanthroline, mixing at normal temperature to obtain a brown phenanthroline-Pt (II) complex precursor which has a uniform and smooth rod-shaped structure, and reducing the brown phenanthroline-Pt (II) complex precursor in a hydrogen atmosphere by using the brown phenanthroline-Pt (II) complex precursor as a template to obtain the porous Pt nanorod. The porous Pt nanorod as a catalyst shows higher catalytic activity in the aspect of catalyzing oxygen reduction reaction in an acid medium.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, and particularly relates to an oxygen reduction reaction catalyst and a preparation method thereof.
Background
The oxygen reduction reaction is the most critical half reaction in metal-air batteries and fuel batteries, and the Pt-based nano material catalytic oxygen reduction reaction is one of the most widely studied electrochemical reactions. However, some practical applications of fuel cells still face several key issues such as slow kinetics of the cathodic oxygen reduction reaction, carbon monoxide poisoning and alcohol/acid crossover at the anode and reduced activity due to catalyst dissolution, aggregation and Ostwald ripening. Therefore, improving the activity, selectivity, and durability of the cathode Pt electrocatalyst for ORR is very important to promote the commercial application of fuel cells.
The activity of the electrocatalyst is highly related to the morphology and composition thereof, and in order to improve the electrocatalytic performance, proper morphology control of the Pt-based nanostructure is an effective strategy. One-dimensional porous Pt nanorods have received much attention in catalysis and electrocatalysis due to their unique physicochemical properties. Firstly, the special one-dimensional morphology endows the Pt nanorod with high conductivity and inherent anisotropy morphology; secondly, the large number of pore structures on the surface of the nanorod increases the specific surface area of the electrocatalyst, so that the utilization rate of catalytic active sites and atoms is increased, and the porous structure can effectively promote infiltration and diffusion of reaction molecules and electrolyte solution, and accelerate mass transfer of catalytic reaction; in addition, the one-dimensional nano structure is easy to form a continuous conductive network on the surface of the electrode, so that the kinetics of various electrocatalytic reactions are promoted; finally, the self-supporting structure characteristic of the one-dimensional continuous structure has excellent self-stability, and is beneficial to improving the electrochemical stability in the catalytic reaction process. Thus, one-dimensional porous Pt nanorods generally show enhanced activity for various catalytic/electrocatalytic reactions, compared to conventional spherical nanocrystals.
At present, Pt nanorods are mainly synthesized by a hard template method, various nanowire templates such as Ag, Cu, ZnO and Te nanowires need to be synthesized in advance, and the synthesis steps are complicated. Although the prior art also adopts a self-template method to synthesize the Pt nano-rod, the adopted process is complicated in the processes of preparing the precursor and reducing the precursor. Therefore, a simple self-template method for preparing the one-dimensional porous Pt nanorod is needed.
Disclosure of Invention
The present invention is directed to an oxygen reduction catalyst and a method for preparing the same, which overcome the above-mentioned disadvantages. The catalyst is a porous Pt nanorod and is prepared by taking phenanthroline-Pt (II) complex as a template. The porous Pt nanorod as a catalyst shows higher catalytic activity in the aspect of catalyzing oxygen reduction reaction in an acid medium.
The technical scheme of the invention is as follows: a method for preparing an oxygen reduction reaction catalyst, comprising the steps of:
(1) adding phenanthroline ethanol solution to K2PtCl4To obtain a mixed solution;
(2) heating the mixed solution obtained in the step (1), and stirring for reaction to obtain a suspension;
(3) centrifugally separating the suspension obtained in the step (2), washing and drying the obtained precipitate, and then putting the precipitate into a tubular furnace for calcining; and washing, centrifugally separating and drying the calcined product to obtain the porous Pt nanorod, namely the catalyst.
K in the mixed solution in the step (1)2PtCl4The mol ratio of the compound to the phenanthroline is 1: 1.5-2.5.
The ethanol solution of phenanthroline and K in the step (1)2PdCl4The concentration of the aqueous solution is 0.01-0.05 mol/L.
Heating to 60-80 ℃ in the step (2); stirring and reacting for 1-2 hours.
And (4) washing the precipitate for 3-5 times by adopting water and ethanol in the step (3).
The calcination in the step (3) is specifically as follows: calcining for 2 hours at the temperature of 180-220 ℃ under the condition of hydrogen atmosphere.
The oxygen reduction reaction catalyst prepared by the preparation method is a porous Pt nanorod with a one-dimensional rod-shaped structure; the surface is rough, and the surface has a pore structure and grain boundary atoms.
The invention has the beneficial effects that: the preparation method takes phenanthroline as a complexing agent, potassium chloroplatinite as a platinum source, ethanol and water as solvents, and utilizes Pt2+And mixing the precursor with phenanthroline under the strong complexation effect at normal temperature to obtain a brown phenanthroline-Pt (II) complex precursor which has a uniform and smooth rod-shaped structure, reducing the precursor in a hydrogen atmosphere by taking the precursor as a template to obtain a porous Pt nanorod, wherein in the sintering process, the removal of a large amount of phenanthroline is beneficial to the formation of a pore structure on the surface of the Pt nanorod. The preparation method is simple, green and economical, can realize gram-grade preparation, and is suitable for industrial large-scale production.
The Pt nanorod prepared by the invention has rich pore structures and grain boundary atoms, shows rich active centers, shows enhanced oxygen reduction activity, can be used as a catalyst for oxygen reduction reaction, is higher than commercial Pt black, has a half-wave potential shifted by 55mV in comparison with the Pt black, and is a fuel cell cathode electrocatalyst with great development prospect.
Drawings
Fig. 1 is an XRD pattern of the porous Pt nanorods prepared in example 1.
Fig. 2 is an SEM image of the porous Pt nanorods prepared in example 1.
Fig. 3 is a partially enlarged view of fig. 2.
Fig. 4 is an SEM image of the porous Pt nanorods prepared in example 2.
Fig. 5 is a linear scanning voltammogram of the electrocatalytic oxygen reduction reaction of the porous Pt nanorods prepared in example 1 and a commercial Pt black catalyst.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1
10mL of 0.05mol/L ethanol solution of phenanthroline is added to 5mL of 0.05mol/L K2PtCl4The water solution is evenly mixed, the obtained mixed solution is heated and stirred in water bath at the temperature of 80 ℃ for reaction for 1 hour to ensure that Pt is obtained2+Fully complexing with phenanthroline to form phenanthroline-Pt (II) complex precipitate, then centrifugally washing for 4 times by using a hydrated ethanol mixed solution with the ratio of 1:1, and then pouring into a magnetic boat and drying in a 60 ℃ oven; and finally, putting the magnetic boat into a tube furnace, calcining for 2 hours at 200 ℃ under the condition of hydrogen, centrifugally separating, washing and drying in vacuum to obtain a product.
As can be seen from fig. 1, the resulting product was Pt.
As can be seen from FIG. 2, the resulting product has a one-dimensional rod-like structure.
It can be seen from the observation of FIG. 3 that the Pt nanorods have rough surfaces and many pores.
The porous Pt nanorods prepared in example 1 were used to electrocatalyze the oxygen reduction reaction at 30 c, and were measured using linear sweep voltammetry, and the results are shown in fig. 5.
As can be seen from FIG. 5, compared with commercial Johnson-Matthey Pt black (commercial Pt black for short), the porous Pt nanorod prepared by the invention has abundant pore structure and grain boundary atoms, and shows abundant active centers. Therefore, the porous Pt nanorod shows enhanced oxygen reduction reaction kinetics and area activity, the half-wave potential of the porous Pt nanorod is shifted to 55mV in comparison with commercial Pd black, and the catalytic performance is obviously improved.
Example 2
30mL of 0.05mol/L ethanol solution of phenanthroline is poured into 15mL of 0.05mol/L K2PtCl4The water solution is evenly mixed, the obtained mixed solution is heated and stirred in water bath at the temperature of 80 ℃ for reaction for 1 hour to ensure that Pt is obtained2+Fully complexing with phenanthroline to form phenanthroline-Pt (II) complex precipitate, then centrifugally washing for 4 times by using a hydrated ethanol mixed solution with the ratio of 1:1, and then pouring into a magnetic boat and drying in a 60 ℃ oven; and finally, putting the magnetic boat into a tube furnace, calcining for 2 hours at 200 ℃ under the condition of hydrogen, centrifugally separating, washing and drying in vacuum to obtain the product porous Pt nanorod, which is shown in figure 4.
Claims (7)
1. A preparation method of an oxygen reduction reaction catalyst is characterized by comprising the following steps:
(1) adding phenanthroline ethanol solution to K2PtCl4To obtain a mixed solution;
(2) heating the mixed solution obtained in the step (1), and stirring for reaction to obtain a suspension;
(3) centrifugally separating the suspension obtained in the step (2), washing and drying the obtained precipitate, and then putting the precipitate into a tubular furnace for calcining; and washing, centrifugally separating and drying the calcined product to obtain the porous Pt nanorod, namely the catalyst.
2. The method for preparing an oxygen reduction reaction catalyst according to claim 1, wherein K is contained in the mixed solution in the step (1)2PtCl4The mol ratio of the compound to the phenanthroline is 1: 1.5-2.5.
3. The oxygen reduction reaction catalyst according to claim 1The preparation method is characterized in that the ethanol solution of phenanthroline and the K in the step (1)2PdCl4The concentration of the aqueous solution is 0.01-0.05 mol/L.
4. The method for preparing the oxygen reduction reaction catalyst according to claim 1, wherein the heating in the step (2) is performed to 60 to 80 ℃; stirring and reacting for 1-2 hours.
5. The method for preparing the oxygen reduction reaction catalyst according to claim 1, wherein the precipitate is washed 3 to 5 times with water and ethanol in the step (3).
6. The method for producing an oxygen reduction reaction catalyst according to claim 1, wherein the calcination in the step (3) is specifically: calcining for 2 hours at the temperature of 180-220 ℃ under the condition of hydrogen atmosphere.
7. An oxygen reduction reaction catalyst obtained by the production method according to any one of claims 1 to 6, wherein the catalyst is a porous Pt nanorod having a one-dimensional rod-like structure; the surface is rough, and the surface has a pore structure and grain boundary atoms.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210069571.5A CN114464823B (en) | 2022-01-21 | Oxygen reduction reaction catalyst and preparation method thereof |
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| CN202210069571.5A CN114464823B (en) | 2022-01-21 | Oxygen reduction reaction catalyst and preparation method thereof |
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| CN114464823A true CN114464823A (en) | 2022-05-10 |
| CN114464823B CN114464823B (en) | 2024-07-05 |
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