KR20140065686A - Preparation method of carbon-supported palladium-platinum alloy nanoparticles with core-shell structure for the application to fuel cells - Google Patents
Preparation method of carbon-supported palladium-platinum alloy nanoparticles with core-shell structure for the application to fuel cells Download PDFInfo
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- KR20140065686A KR20140065686A KR1020120131497A KR20120131497A KR20140065686A KR 20140065686 A KR20140065686 A KR 20140065686A KR 1020120131497 A KR1020120131497 A KR 1020120131497A KR 20120131497 A KR20120131497 A KR 20120131497A KR 20140065686 A KR20140065686 A KR 20140065686A
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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Abstract
The present invention relates to core-shell palladium-platinum alloy nanoparticles and a method for producing a carbon-supported catalyst for fuel cells. More particularly, the present invention relates to a method for preparing a metal precursor, comprising: ultrasonically mixing a platinum (Pt) precursor, a second metal precursor, and a carrier in an aqueous solution; Adding a reducing agent to the mixed solution containing the metal precursor and the support obtained after the ultrasonic treatment to reduce the solution while stirring; The present invention also relates to a method for preparing a highly dispersed core-shell palladium-platinum alloy nanoparticle and a carbon-supported catalyst for a fuel cell, by filtering and washing the resulting mixed solution.
The present invention can provide a carbon-supported catalyst for a fuel cell, which is economical and excellent in performance, by preparing a core-shell type palladium-platinum alloy nano-particle and a carbon-supported catalyst.
Description
The present invention relates to a method for producing palladium (Pd) -platinum (Pt) alloy nanoparticles. More specifically, the core-shell nanoparticles are synthesized and used as a catalyst for a polymer electrolyte fuel cell.
Polymer Electrolyte Membrane Fuel Cell (PEMFC) is an electrochemical energy conversion device that directly converts the chemical energy of hydrogen and oxygen into electrical energy. Compared with conventional internal combustion engines, it has high energy conversion efficiency and is not attracting pollutant emissions, and is attracting attention as a next generation clean alternative power source. Despite the many advantages of PEMFCs, one of the reasons for the delay in commercialization is the high manufacturing cost. In the case of mass production of the stack, the cost of the electrode catalyst is higher than other materials. Since the cathode reaction of the PEMFC is relatively complicated and slow compared with the anode reaction, a large amount of platinum catalyst or a platinum supported catalyst supported on carbon is used in order to obtain a desired output. Because of the limited reserves of platinum, commercialization of PEMFC is expected to increase the cost of catalysts as demand increases. Therefore, in order to improve the economical efficiency of the PEMFC, a study is required to improve the oxygen reduction performance of the platinum catalyst so as to obtain a high output with a small amount of platinum.
In order to improve the oxygen reduction performance, an alloy platinum catalyst such as Pt-Co, Pt-Cu, Pt-Co-Cu, or Pt-Pd is used together with a platinum catalyst and cobalt, In recent years, fuel cell catalysts have been developed that dramatically improve the durability and catalyst performance of fuel cell catalysts by designing nanocatalyst structures in the form of a core-shell structure.
In the prior art related to the present invention, Fadlilatul Taufany, Chun-Jern Pan, John Rick, Hung-Lung Chou, Mon-Che Tsai, Bing-Joe Hwang, Din-Goa Liu, , Mau-Tsu Tang, Yao-Chang Lee, and Ching-lue Chen, ACS NaNo publications, 2011, Vol 5, 12, page 9370-9381) discloses a Kinetically Controlled Autocatalytic Chemical Process for Bulk Production of Bimetallic Core- Nanoparticles. There are also platinum-based electrocatalysts with core-shell nanostructures (Hong Yang, Angewandte Chemie International Edition, 2011, Vol. 50, page 2674-2676).
However, since the conventional core-shell structure is manufactured by growing a shell using a surfactant in advance of core particles synthesized in advance, or by carrying a shell on the surface of the core by an electrolytic deposition method, The technical composition is different.
Conventional core-shell nanoparticles were prepared by growing a shell using a surface active agent on a previously synthesized core particle or by carrying a shell on the core surface by electrolytic deposition. However, these methods are not suited for mass production because of the difficult synthesis conditions, the influence of surfactants affecting the performance of the catalyst to be produced, the synthesis of inert atmosphere, and many other sensitive and limited conditions. Therefore, there is a need for a technique capable of mass production of a catalyst for low-cost-high-performance oxygen reduction reaction, which solves the above-mentioned limited conditions in manufacturing core-shell nanoparticles.
In order to synthesize a conventional core-shell type nanoparticle catalyst, a surfactant has been used or an electrolytic deposition method has been used. However, the present invention selects palladium-platinum nanoparticles which form a core-shell structure by employing a conventionally applied coacervation method in which a ligand is strongly bound to platinum ions and a relatively difficult to reduce platinum precursor, The interaction between the platinum layer and the palladium in the core modifies the electronic structure, and in the oxygen reduction reaction, the adsorption of oxidized species is suppressed, thereby improving the performance and durability of the catalyst. Therefore, the constraints described above can be solved, the process can be simplified and mass production is possible, and a low-cost-high-performance oxygen reduction reaction catalyst can be mass-produced, thereby contributing to the economical improvement of the fuel cell.
The co-sputtering method is a method widely applied to the manufacture of alloy catalysts by supporting two or more kinds of metal precursors together by reducing them. In the present invention, palladium-platinum nanoparticles which form a core-shell structure by a co-precipitation method are selected by selecting a platinum precursor having a strong ligand binding to platinum ions and relatively difficult to reduce, and a palladium- It was confirmed that the electron structure was modified by the interaction and the adsorption of oxidized species was suppressed in the oxygen reduction reaction, thereby improving the performance and durability of the catalyst. In addition, it can solve the sensitive factors affecting the performance of the catalyst, simplify the process and enable mass production, thereby contributing to improvement of economical efficiency of the fuel cell catalyst.
Fig. 1 is a schematic view showing that core-shell nanoparticles are supported on carbon.
2 is a transmission electron microscope image of a core-shell structure nanoparticle catalyst.
FIG. 3 shows the result of qualitative analysis of a core-shell structure nanoparticle catalyst by EDX.
4 shows XRD pattern analysis results of a core-shell structure nanoparticle catalyst and a commercial platinum catalyst.
FIG. 5 shows the oxygen reduction reaction polarization curve of a core-shell structure nanoparticle catalyst and a conventional platinum catalyst.
FIG. 6 shows current-voltage curves in a unit cell experiment of a core-shell structure nanoparticle catalyst and a commercial platinum catalyst.
The present invention shows a method for producing a carbon-supported catalyst for a fuel cell.
The present invention relates to a method for preparing a palladium complex, which comprises mixing an aqueous solution of a platinum (Pt) precursor, palladium (Pd) precursor and a carrier, and subjecting the mixture to ultrasonic treatment; Adding a reducing agent to the mixed solution containing the platinum (Pt) precursor, the palladium (Pd) precursor and the carrier obtained after the ultrasonic treatment, and stirring and reducing the mixture; And a step of washing and washing the mixed solution obtained after the above-mentioned reduction process, to thereby produce a carbon-supported catalyst for a fuel cell, wherein the palladium-platinum alloy nanoparticles are supported.
In order to synthesize palladium-platinum nanoparticles supported on carbon by coacervation, a platinum precursor and palladium, which are relatively difficult to reduce, are used because amine ligands are strongly bonded to platinum ions.
The platinum precursor may be a platinum compound containing an amine (NH 3 ) ligand of tetraamine platinum (II) nitrate (Pt (NH 3 ) 4 (NO 3 ) 2 ]
The palladium precursor may be palladium (Pd) or palladium nitrate (Pd (NO 3 ) 2 ).
The carrier may be any one selected from carbon black, Ketjen black, carbon nanotube, carbon nanofiber, graphite carbon, and graphene.
The reducing agent may be at least one selected from the group consisting of NaBH 4 , LiBH 4 and LiAlH 4 .
The present invention includes a carbon-supported catalyst for a fuel cell produced by the above-mentioned method.
The present invention includes a fuel cell containing a carbon-supported catalyst for a fuel cell manufactured by the above-mentioned method.
In order to accomplish the object of the present invention, palladium-platinum alloy nanoparticles according to the present invention were produced under various conditions under the conditions of producing the carbon-supported catalyst for a fuel cell carrying the palladium-platinum alloy nanoparticles of the present invention. It is desirable to provide a supported carbon-supported catalyst for a fuel cell.
Hereinafter, the present invention will be described in detail with reference to Examples and Test Examples. However, these are for the purpose of illustrating the present invention in more detail, and the scope of the present invention is not limited thereto.
<Examples>
Add tetraamine platinum (II) nitrate (0.25 mmol) and palladium (II) nitrate (0.25 mmol) to the third distilled water (150 ml) at room temperature. Then, the suspension was charged with commercial carbon (Vulcan XC-72R carbon black, 0.3 g) as a carrier and thoroughly dispersed by stirring at 100 rpm and ultrasonic treatment at 50 kHz for 1 hour in a suspension state.
NaBH 4 (sodium borohydride, 0.003 mol) is dissolved in tertiary distilled water to be supported on the carrier for supporting the platinum precursor and the palladium precursor on the support, and then the solution is dropped on the suspension.
The above process will be described with reference to FIG. 1, and the
FIG. 2 shows a transmission electron microscope image of a core-shell type palladium-platinum nanoparticle catalyst uniformly dispersed and has a size of about 3-4 nm.
FIG. 3 is a scanning electron microscope image of a core-shell type palladium-platinum nanoparticle catalyst. It was confirmed that the nanoparticles had a core-shell structure composed of palladium at the core and platinum at the shell, and palladium and platinum And it is confirmed that this alloy exists in the form of the alloy.
≪ Test Example 1 >
(PdPt / C, hereinafter abbreviated as a core-shell type nanoparticle catalyst) having a core-shell structure of palladium-platinum alloy nanoparticles supported on a carbon carrier and a commercially available platinum The X-ray diffraction pattern of the catalyst (Pt / C commercial) was measured and the results are shown in Fig.
In the X-ray diffraction pattern of FIG. 4, the characteristic peak of the (220) plane of the platinum catalyst was 67.4 ㅀ, and the characteristic peak of the core-shell type nanoparticle catalyst migrated to a slightly higher angle than that of the commercial platinum catalyst have. This is because the lattice constant of the platinum atom becomes small and the platinum layer is formed on the surface, so that the degree of formation of the alloy of palladium-platinum in the particles is relatively low.
≪ Test Example 2 &
The core-shell type nanoparticle catalyst (PdPt / C) and the platinum catalyst (Pt / C commercial) obtained in the above example were measured by a linear principle preliminary method (LSV) using potentiostat as an oxygen reduction polarization curve, The results are shown in Fig.
In the LSV measurement, 0.1 M HClO 4 aqueous solution purged with oxygen for 1 hour was used. The working electrode rotation speed was 1600 rpm and the measurement range was 1.115-0.315 (V vs. RHE ), And the catalyst amount of the electrode was set to 15 ug / cm 2 .
As shown in FIG. 5, the core-shell type nanoparticle catalyst obtained in the embodiment of the present invention showed superior performance to that of the commercial platinum catalyst.
≪ Test Example 3 >
The current-voltage curves of the unit cells prepared using the core-shell type nanoparticle catalyst (PdPt / C) and the commercial platinum catalyst (Pt / C commercial) obtained in the above examples as the anode catalysts for the polymer electrolyte fuel cell And the results are shown in Fig.
When measuring the current-voltage curve of the unit cells, the area of the electrode was 5 cm 2. In both cases, the commercial platinum catalyst was used in an amount of 0.3 mg / cm 2. The positive electrode was a core-shell type nanoparticle catalyst and the commercial platinum catalyst 0.5 mg / cm < 2 > The fuel used was hydrogen at the anode and oxygen at the anode. The stoichiometric ratio was 1: 1.5 and the temperature was measured at 65 ° C.
As shown in FIG. 6, the current density and the voltage density of the core-shell nanoparticle catalyst were higher than those of the conventional platinum catalyst.
From the results of Test Examples 1, 2, 3 and especially Test Examples 2 and 3, the carbon-supported catalyst for a fuel cell carrying the palladium-platinum alloy nanoparticles of the present invention exhibited excellent activity as a catalyst of a fuel cell as compared with the conventional platinum catalyst And it was found.
Although the present invention has been described and illustrated in detail, it should be understood by those skilled in the art that various changes and modifications may be made without departing from the scope of the present invention as defined by the appended claims. It will be understood that various modifications and changes may be made in the present invention.
The present invention synthesizes palladium-platinum nanoparticles forming a core-shell structure by a co-precipitation method, so that the adsorption of oxidized species is suppressed, thereby improving the performance and durability of the catalyst, thereby solving a sensitive factor affecting the performance of the catalyst. Therefore, it is possible to simplify the process and mass-produce the fuel cell, thereby contributing to the improvement of the economical efficiency of the fuel cell catalyst, which is industrially applicable.
Claims (7)
Adding a reducing agent to the mixed solution containing the platinum (Pt) precursor, the palladium (Pd) precursor and the carrier obtained after the ultrasonic treatment, and stirring and reducing the mixture;
A method for producing a carbon-supported catalyst for a fuel cell, which comprises palladium-platinum alloy nanoparticles supported thereon, which comprises filtering and washing the mixed solution obtained after the reduction process
Wherein the platinum precursor is a platinum compound comprising an amine (NH 3 ) ligand of tetraamine platinum (II) nitrate (Pt (NH 3 ) 4 (NO 3 ) 2 ]
Wherein the palladium precursor is palladium (Pd) or palladium nitrate (Pd (NO 3 ) 2 ).
Characterized in that the support is any one selected from carbon black, Ketjen black, carbon nanotube, carbon nanofiber, graphite carbon and graphene.
Wherein the reducing agent is at least one selected from the group consisting of NaBH 4 , LiBH 4 and LiAlH 4 .
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| WO2017052222A1 (en) * | 2015-09-25 | 2017-03-30 | 주식회사 엘지화학 | Carrier-nanoparticle complex, preparation method therefor, and membrane electrode assembly including same |
| WO2018056774A3 (en) * | 2016-09-26 | 2018-08-09 | 충남대학교산학협력단 | Manufacturing method for carbon dot-platinum-palladium composite, carbon dot-platinum-palladium catalyst manufactured thereby, and fuel cell using same |
| KR20180117808A (en) * | 2017-04-20 | 2018-10-30 | 현대자동차주식회사 | Carbon-Platinum Core-Shell Type Catalysts for Fuel Cell and Method for Preparing the Same |
| CN110743571A (en) * | 2019-12-03 | 2020-02-04 | 清华大学 | By using H2Method for preparing carbon-supported Pt shell core catalyst by liquid phase reduction |
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| CN109792060B (en) * | 2016-09-26 | 2021-09-28 | 忠南大学校产学协力团 | Method for preparing carbon dot-platinum-palladium complex |
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| CN110743571A (en) * | 2019-12-03 | 2020-02-04 | 清华大学 | By using H2Method for preparing carbon-supported Pt shell core catalyst by liquid phase reduction |
| KR20220072508A (en) * | 2020-11-25 | 2022-06-02 | 충남대학교산학협력단 | Platinum Based Catalyst for Oxygen Reduction Reaction and Preparation Method thereof |
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