CN114792817B - Co@Pt core-shell fuel cell catalyst with Au doped subsurface layer and preparation method thereof - Google Patents
Co@Pt core-shell fuel cell catalyst with Au doped subsurface layer and preparation method thereof Download PDFInfo
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- CN114792817B CN114792817B CN202210523674.4A CN202210523674A CN114792817B CN 114792817 B CN114792817 B CN 114792817B CN 202210523674 A CN202210523674 A CN 202210523674A CN 114792817 B CN114792817 B CN 114792817B
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Abstract
The invention provides a Co@Pt core-shell fuel cell catalyst with Au doped on a subsurface layer and a preparation method thereof, belonging to the technical field of fuel cells, wherein the proportion of Co, pt and Au atoms is (3-5): 1: (0.001-0.05); the metal loading in the catalyst is between 20% and 80%. According to the preparation method of the catalyst, the catalyst is prepared by combining the gas phase reduction method and the displacement reaction, the cobalt core can be prevented from being oxidized by the gas phase reduction method in the preparation process, the displacement reaction operation is simpler and more convenient, and the prepared fuel cell catalyst is beneficial to improving the activity of the catalyst by doping transition metal, so that the fuel cell can operate more efficiently.
Description
Technical Field
The invention relates to the technical field of fuel cells, in particular to a Co@Pt core-shell fuel cell catalyst with Au doped on a subsurface layer and a preparation method thereof.
Background
Fuel cells produce electricity by electrochemical reaction of hydrogen and oxygen. The product generated by the power generation of the fuel cell is in principle only water. Therefore, little burden is imposed on the global environment, and attention is paid as a clean power generation system.
The fuel cell obtains electromotive force by supplying a fuel gas containing hydrogen to the anode (fuel electrode) side and an oxidizing gas containing oxygen to the cathode (air electrode) side. Here, the oxidation reaction represented by the following formula (1) is performed on the anode side, the reduction reaction represented by the following formula (2) is performed on the cathode side, and the reaction represented by the formula (3) is performed as a whole, thereby providing an electromotive force to the external circuit.
H 2 →2H + + 2e - （1）
(1/2)O 2 +2H+ +2e - →H 2 O （2）
H 2 +(1/2)O 2 →H 2 O （3）
Fuel cells are classified into solid polymer type (PEFC), phosphoric acid type (PAFC), molten carbonate type (MCFC), solid oxide type (SOFC) and the like according to the kind of electrolyte. Fuel cells and other types of devices typically utilize electroactive materials. For example, a typical fuel cell may include an anode catalyst layer, a cathode catalyst layer, and an electrolyte between the anode and cathode catalyst layers to generate an electrical current in a known electrochemical reaction between a fuel and an oxidant. The catalyst layer typically includes a catalytic material, such as platinum, supported on carbon particles. However, the catalytic material is only active when it can contact protons, electrons and the corresponding reactant fuel or oxidant. The areas of the catalyst layer that can be contacted by protons, electrons, and corresponding reactants are referred to as three-phase boundaries.
The existing fuel cell catalyst has low activity, and the platinum consumption is increased, so that the cost is high. The catalyst has poor stability, is easy to dissolve and agglomerate in the operation environment of the fuel cell, and causes the problems of insufficient service life of the membrane electrode, etc., so the development of a novel fuel cell catalyst has wide application prospect.
Disclosure of Invention
The invention provides an Au-doped Co@Pt core-shell fuel cell catalyst and a preparation method thereof.
The technical scheme of the invention is realized as follows:
the invention provides a Co@Pt core-shell fuel cell catalyst with Au doped on a subsurface layer, wherein the proportion of Co, pt and Au atoms is (3-5): 1: (0.001-0.05); the metal loading in the catalyst is between 20% and 80%.
As a further improvement of the invention, the method comprises the following steps:
s1, preparation of Co/C kernel: mixing cobalt salt, a carbon carrier and water uniformly under stirring, drying the water to obtain carbon-supported cobalt powder, and heating and calcining the carbon-supported cobalt powder in a hydrogen environment to obtain Co/C core powder;
s2. Preparation of Co@Au@Pt/C catalyst: adding deoxidized deionized water into the Co/C core powder prepared in the step S1, carrying out ultrasonic crushing to uniformly mix the solution, adding chloroauric acid solution under stirring, stirring for reacting for a first time period, then dropwise adding chloroplatinic acid solution, continuously stirring for reacting for a second time period, centrifuging, carrying out suction filtration, and drying to obtain the Co@Au@Pt/C catalyst, namely the Co@Pt core-shell fuel cell catalyst with Au doped on the subsurface.
As a further improvement of the present invention, the cobalt salt in step S1 is at least one selected from cobalt chloride, cobalt sulfate, and cobalt nitrate.
As a further improvement of the invention, the calcination temperature in the step S1 is 200-500 ℃ and the time is 1-4h.
As a further improvement of the present invention, the mass ratio of cobalt salt, carbon carrier and water in step S1 is (5-6): (7-10): 1.
as a further improvement of the invention, the mass ratio of cobalt salt, carbon support and water in step S1 is 5.5:8:1.
As a further improvement of the present invention, the first period of time in step S2 is 5-15min; the second time period is 10-30min.
As a further improvement of the invention, the content of the chloroauric acid solution in the step S2 is 0.01-0.03g/mL; the content of the chloroplatinic acid solution is 0.03-0.05g/mL.
As a further improvement of the invention, the mass ratio of the Co/C core powder, the deoxidized deionized water, the chloroauric acid and the chloroplatinic acid in the step S2 is (5-10): 2: (0.03-0.04): (3-5).
As a further improvement of the invention, the mass ratio of the Co/C core powder, the deoxidized deionized water, the chloroauric acid and the chloroplatinic acid in the step S2 is 8:2:0.032:4.
In order to improve the activity of the catalyst, transition metal cobalt is doped in the platinum catalyst, the metal atom spacing is shortened, the electronic structure of the catalyst is regulated and controlled, and then the oxygen adsorption energy is optimized, so that the catalytic activity is improved.
In the catalyst, only platinum atoms exposed on the surface can play a role in catalysis, and in order to improve the utilization rate of the platinum atoms, the core-shell catalyst is prepared by using non-noble metal cobalt as an inner core and platinum atoms as an outer shell, so that the platinum atoms are utilized as much as possible.
In the fuel cell operating environment, with potential cycling, alternating temperature and humidity, and the like, cobalt atoms are more likely to dissolve in an acidic environment, and the catalyst structure is more likely to be destroyed, resulting in reduced activity. In order to improve the durability of the catalyst and the service life of the fuel cell, the catalyst is doped with inert metal to improve the chemical stability, and gold element has been proved to be capable of improving the durability of the platinum-based catalyst, but the oxygen reduction activity of gold atoms is lower, so that the activity reduction caused by doping gold atoms is avoided.
The invention has the following beneficial effects:
1. the fuel cell catalyst prepared by the method is beneficial to improving the activity of the catalyst by doping transition metal, so that the fuel cell can operate more efficiently.
2. This patent adopts core-shell structure, makes platinum atom expose on the catalyst surface, improves the utilization ratio of platinum.
3. Increasing activity and platinum utilization can reduce the amount of platinum used and reduce fuel cell costs.
4. The gold atoms are doped on the subsurface layer, so that the catalyst durability can be improved, the service life of the fuel cell can be prolonged, and the cost can be reduced without reducing the catalytic activity.
5. The preparation method of the catalyst utilizes a mode of combining a gas phase reduction method and a displacement reaction to prepare the catalyst, and the gas phase reduction method can avoid the cobalt core from being oxidized in the preparation process, so that the displacement reaction operation is simpler and more convenient.
The summary is provided to introduce a selection of concepts in a simplified form that are further described below in the detailed description. This summary is not intended to identify key features or essential features of the disclosure, nor is it intended to be used to limit the scope of the disclosure.
Drawings
The foregoing and other objects, features and advantages of the disclosure will be apparent from the following more particular descriptions of exemplary embodiments of the disclosure as illustrated in the accompanying drawings wherein like reference numbers generally represent like parts throughout the exemplary embodiments of the disclosure.
FIG. 1 shows a preparation process flow diagram of a Co@Pt core-shell fuel cell catalyst with Au doped subsurface layers;
FIG. 2 shows a schematic structural diagram of a subsurface Au-doped Co@Pt core-shell fuel cell catalyst prepared by the method;
FIG. 3 shows an SEM image of Co/C core powder prepared in example 1 of the invention;
FIG. 4 shows an SEM image of a subsurface Au-doped Co@Pt core-shell fuel cell catalyst prepared in example 1 of the present invention;
FIG. 5 shows electrochemical test characterization graphs of the subsurface Au-doped Co@Pt core-shell fuel cell catalyst prepared in example 1 of the invention.
Detailed Description
Embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While embodiments of the present disclosure are illustrated in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
The term "comprising" and variations thereof as used herein means open ended, i.e., "including but not limited to. The term "or" means "and/or" unless specifically stated otherwise. The term "based on" means "based at least in part on". The terms "one example embodiment" and "one embodiment" mean "at least one example embodiment. The term "another embodiment" means "at least one additional embodiment". The terms "first," "second," and the like, may refer to different or the same object. Other explicit and implicit definitions are also possible below.
Example 1
Referring to fig. 1, the embodiment provides a preparation method of a subsurface Au doped co@pt core-shell fuel cell catalyst, which specifically includes the following steps:
s1, preparation of Co/C kernel: firstly, 550mg of cobalt chloride hexahydrate and 800mg of carbon carrier are weighed and placed in a beaker, then 100mL of deionized water is measured and added into the beaker, the mixture is fully mixed under stirring, then the moisture is dried in an oven, the dried powder is placed in a porcelain boat and placed in a tube furnace, hydrogen is introduced, the temperature is raised to 250 ℃, and the mixture is kept at the temperature for 2 hours, so that Co/C core powder is prepared, and an SEM (scanning electron microscope) diagram of the Co/C core powder is shown in figure 3.
S2. Preparation of Co@Au@Pt/C catalyst: 800mg of the powder prepared in the step S1 is taken, 200mL of deoxidized deionized water is added, the solution is uniformly mixed by ultrasonic crushing, 0.16mL of chloroauric acid solution (the concentration is 0.02 g/mL) is slowly added under stirring, au element is reduced to the surface of a cobalt kernel by a displacement reaction, after stirring for 10min, 10mL of chloroplatinic acid solution (the concentration is 0.04 g/mL) is slowly dripped, stirring is continued for 20min, and platinum atoms are reduced to the surface of the kernel by the displacement reaction. After the reaction is finished, preparing the Co@Pt core-shell fuel cell catalyst with the subsurface layer doped with Au through operations such as centrifugation, suction filtration and drying, wherein the structure schematic diagram of the prepared catalyst is shown in fig. 2, and the SEM (scanning electron microscope) diagram is shown in fig. 4.
Example 2
Referring to fig. 1, the embodiment provides a preparation method of a subsurface Au doped co@pt core-shell fuel cell catalyst, which specifically includes the following steps:
s1, preparation of Co/C kernel: firstly, weighing 500mg of cobalt chloride hexahydrate and 700mg of carbon carrier, placing the cobalt chloride hexahydrate and 700mg of carbon carrier into a beaker, then weighing 100mL of deionized water, adding the cobalt chloride hexahydrate and the carbon carrier into the beaker, fully mixing the cobalt chloride hexahydrate and the carbon carrier under stirring, then drying the water in an oven, placing the dried powder into a porcelain boat, placing the porcelain boat into a tubular furnace, introducing hydrogen, heating to 200 ℃, and keeping the temperature for 1h to obtain Co/C core powder.
S2. Preparation of Co@Au@Pt/C catalyst: taking 500mg of the powder prepared in the step S1, adding 200mL of deoxidized deionized water, uniformly mixing the solution through ultrasonic crushing, slowly adding 0.3mL of chloroauric acid solution (with the concentration of 0.01 g/mL) under stirring, reducing the Au element to the surface of a cobalt core through a displacement reaction, stirring for 5min, slowly adding 10mL of chloroplatinic acid solution (with the concentration of 0.03 g/mL) under stirring, continuously stirring for 10min, and reducing the Pt atoms to the surface of the core through the displacement reaction. After the reaction is finished, preparing the Co@Pt core-shell fuel cell catalyst with the subsurface layer doped with Au through operations such as centrifugation, suction filtration, drying and the like.
Example 3
Referring to fig. 1, the embodiment provides a preparation method of a subsurface Au doped co@pt core-shell fuel cell catalyst, which specifically includes the following steps:
s1, preparation of Co/C kernel: firstly, 600mg of cobalt chloride hexahydrate and 1000mg of carbon carrier are weighed and placed in a beaker, then 100mL of deionized water is measured and added into the beaker, the mixture is fully mixed under stirring, then the moisture is dried in an oven, the dried powder is placed in a porcelain boat and placed in a tube furnace, hydrogen is introduced, the temperature is raised to 500 ℃, and the mixture is kept at the temperature for 4 hours, so that Co/C inner core powder is prepared.
S2. Preparation of Co@Au@Pt/C catalyst: 1000mg of the powder prepared in the step S1 is taken, 200mL of deoxidized deionized water is added, the solution is uniformly mixed by ultrasonic crushing, 0.13mL of chloroauric acid solution (the concentration is 0.03 g/mL) is slowly added under stirring, au element is reduced to the surface of a cobalt kernel by a displacement reaction, after stirring for 15min, 10mL of chloroplatinic acid solution (the concentration is 0.05 g/mL) is slowly dripped, stirring is continued for 30min, and platinum atoms are reduced to the surface of the kernel by the displacement reaction. After the reaction is finished, preparing the Co@Pt core-shell fuel cell catalyst with the subsurface layer doped with Au through operations such as centrifugation, suction filtration, drying and the like.
Comparative example 1
In contrast to example 1, chloroauric acid was not added in step S2, and the other conditions were not changed.
The method specifically comprises the following steps:
s1, preparation of Co/C kernel: firstly, 550mg of cobalt chloride hexahydrate and 800mg of carbon carrier are weighed and placed in a beaker, then 100mL of deionized water is measured and added into the beaker, the mixture is fully mixed under stirring, then the moisture is dried in an oven, the dried powder is placed in a porcelain boat and placed in a tube furnace, hydrogen is introduced, the temperature is raised to 250 ℃, and the temperature is kept for 2 hours, so that Co/C inner core powder is prepared.
S2. Preparation of Co@Pt/C catalyst: 800mg of the powder prepared in the step S1 was taken, 200mL of deionized water after oxygen removal was added, and the solution was uniformly mixed by ultrasonic disruption, 10.08mL of an aqueous solution of chloroplatinic acid (concentration: 0.04 g/mL) was slowly added under stirring, and stirring was continued for 20 minutes, and platinum atoms were reduced to the surface of the core by substitution reaction. After the reaction is finished, the Co@Pt/C catalyst is prepared through operations such as centrifugation, suction filtration, drying and the like.
Comparative example 2
In contrast to example 1, no chloroplatinic acid was added in step S2, and the other conditions were not changed.
The method specifically comprises the following steps:
s1, preparation of Co/C kernel: firstly, 550mg of cobalt chloride hexahydrate and 800mg of carbon carrier are weighed and placed in a beaker, then 100mL of deionized water is measured and added into the beaker, the mixture is fully mixed under stirring, then the moisture is dried in an oven, the dried powder is placed in a porcelain boat and placed in a tube furnace, hydrogen is introduced, the temperature is raised to 250 ℃, and the temperature is kept for 2 hours, so that Co/C inner core powder is prepared.
S2. Preparation of Co@Au/C catalyst: 800mg of the powder prepared in the step S1 is taken, 200mL of deoxidized deionized water is added, the solution is uniformly mixed through ultrasonic crushing, 20.16mL of chloroauric acid solution (the concentration is 0.02 g/mL) is slowly added under stirring, au element is reduced to the surface of a cobalt core through substitution reaction, and after stirring for 10min, the Co@Au/C catalyst is prepared through operations such as centrifugation, suction filtration, drying and the like.
Test example 1
The catalyst prepared in example 1 was dispersed in a 20% isopropyl alcohol solution (isopropyl alcohol: deionized water: nafion 25:74.5:0.5) to a concentration of 1 mg mL -1 Then 20 mu L of catalyst slurry is sucked and slowly dropped on the surface of the platinum carbon electrode, the liquid is evaporated at normal temperature, and a flat catalyst film is left, thus the catalyst film can be used as a working electrode to be tested. Linear Scanning Voltammogram (LSV), also known as polarization curve test, was carried out using a perchloric acid solution at a concentration of 0.1. 0.1M in the electrolyte, and O was introduced 2 Saturated for half an hour at room temperature at 10 mV s -1 Potential scan at a rate between 0.2V and 1.05V, setting the electrode speed to 16 using PINE00 rpm, one-way scanning and recording data. The half-wave potential can be obtained according to the curve, and the activity of the catalyst is estimated preliminarily. And after 10000 circles of voltage scanning are carried out at 0.6-1.1V, carrying out polarization curve test again to obtain comparative data before and after durability test.
As shown in FIG. 5, the half-wave potential of the initial polarization curve is 0.92V through electrochemical test characterization, and the attenuation after the durability test is 12mV, so that the activity and the stability are better.
Test example 2
The catalysts prepared in examples 1-3 and comparative examples 1-2 were subjected to performance tests according to the relevant national standards, and the results are shown in Table 1. Wherein catalyst activity is measured in terms of the conversion of fuel cell oxygen.
TABLE 1
| Group of | Storage stability for 7 days | Catalytic Activity (A/mg) PGM ） | Performance decay after durability test (%) |
| Example 1 | Good quality | 0.63 | 13.1 |
| Example 2 | Good quality | 0.57 | 14.3 |
| Example 3 | Good quality | 0.52 | 11.7 |
| Comparative example 1 | Qualified product | 0.55 | 29.4 |
| Comparative example 2 | Qualified product | 0.11 | 12.2 |
As can be seen from Table 1, the catalysts prepared in examples 1 to 3 have significantly better performance than the comparative examples, and have better catalytic effect, better durability and better stability.
The foregoing description of the embodiments of the present disclosure has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described. The terminology used herein was chosen in order to best explain the principles of the embodiments, the practical application, or the technical improvement of the technology in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
Claims (9)
1. A preparation method of a Co@Pt core-shell fuel cell catalyst with Au doped on a subsurface layer comprises the following steps of: 1: (0.001-0.05), wherein the metal loading in the catalyst is between 20% and 80%, characterized in that the preparation method comprises the following steps:
s1, preparation of Co/C kernel: mixing cobalt salt, a carbon carrier and water uniformly under stirring, drying the water to obtain carbon-supported cobalt powder, and heating and calcining the carbon-supported cobalt powder in a hydrogen environment to obtain Co/C core powder;
s2. Preparation of Co@Au@Pt/C catalyst: adding deoxidized deionized water into the Co/C core powder prepared in the step S1, carrying out ultrasonic crushing to uniformly mix the solution, adding chloroauric acid solution under stirring, stirring for reacting for a first time period, then dropwise adding chloroplatinic acid solution, continuously stirring for reacting for a second time period, centrifuging, carrying out suction filtration, and drying to obtain the Co@Au@Pt/C catalyst, namely the Co@Pt core-shell fuel cell catalyst with Au doped on the subsurface.
2. The method according to claim 1, wherein the cobalt salt in step S1 is at least one selected from the group consisting of cobalt chloride, cobalt sulfate and cobalt nitrate.
3. The method according to claim 1, wherein the calcination temperature in step S1 is 200 to 500 ℃ for 1 to 4 hours.
4. The preparation method according to claim 1, wherein the mass ratio of cobalt salt, carbon carrier and water in step S1 is (5-6): (7-10): 1.
5. the method according to claim 1, wherein the mass ratio of cobalt salt, carbon support and water in step S1 is 5.5:8:1.
6. The method according to claim 1, wherein the first period of time in step S2 is 5-15min; the second time period is 10-30min.
7. The preparation method according to claim 1, wherein the chloroauric acid solution in step S2 has a content of 0.01-0.03g/mL; the content of the chloroplatinic acid solution is 0.03-0.05g/mL.
8. The preparation method according to claim 1, wherein in the step S2, the mass ratio of the Co/C core powder, the deoxidized deionized water, the chloroauric acid and the chloroplatinic acid is (5-10): 2: (0.03-0.04): (3-5).
9. The method according to claim 8, wherein the mass ratio of the Co/C core powder, deoxidized deionized water, chloroauric acid, chloroplatinic acid in step S2 is 8:2:0.032:4.
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| WO2011081619A1 (en) * | 2009-12-28 | 2011-07-07 | Utc Power Corporation | Platinum-palladium catalyst with intermediate layer |
| CN102500365A (en) * | 2011-10-19 | 2012-06-20 | 华南理工大学 | Preparation method of catalyst with core-shell structure for low-temperature fuel cell |
| CN103165914B (en) * | 2011-12-15 | 2015-02-11 | 中国科学院大连化学物理研究所 | Pt/Au/PdCo/C catalyst, and preparation and application thereof |
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| CN104475126B (en) * | 2014-12-11 | 2017-10-20 | 北京化工大学 | Fuel cell carbon supported core-shell platinum cobalt platinum catalyst and preparation method thereof |
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| KR102291160B1 (en) * | 2018-11-08 | 2021-08-19 | 한국과학기술원 | Au doped Pt alloy catalysts for fuel cell and method thereof |
| CN110890558B (en) * | 2019-11-05 | 2021-05-04 | 中新国际联合研究院 | Supported platinum-based core-shell catalyst and preparation method thereof |
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| CN109461945A (en) * | 2018-10-15 | 2019-03-12 | 南京博星科技有限公司 | A kind of fuel cell nuclear shell on carbon dense form copper iron/copper-platinum catalyst |
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