CN115732709A - Pt/C catalyst with ultralow Pt loading capacity and preparation method thereof - Google Patents
Pt/C catalyst with ultralow Pt loading capacity and preparation method thereof Download PDFInfo
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- CN115732709A CN115732709A CN202211420435.2A CN202211420435A CN115732709A CN 115732709 A CN115732709 A CN 115732709A CN 202211420435 A CN202211420435 A CN 202211420435A CN 115732709 A CN115732709 A CN 115732709A
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000003054 catalyst Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 238000000151 deposition Methods 0.000 claims abstract description 11
- 230000008021 deposition Effects 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 239000008151 electrolyte solution Substances 0.000 claims abstract description 8
- 238000004070 electrodeposition Methods 0.000 claims abstract description 7
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 7
- 239000010439 graphite Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 229910021607 Silver chloride Inorganic materials 0.000 claims abstract description 4
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002028 Biomass Substances 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 8
- 239000001257 hydrogen Substances 0.000 abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 239000002245 particle Substances 0.000 description 12
- 239000000446 fuel Substances 0.000 description 9
- 229910052697 platinum Inorganic materials 0.000 description 9
- 230000006911 nucleation Effects 0.000 description 5
- 238000010899 nucleation Methods 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229910002837 PtCo Inorganic materials 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000000089 atomic force micrograph Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000003921 particle size analysis Methods 0.000 description 1
- -1 platinum ions Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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 hydrogen energy, and discloses a Pt/C catalyst with ultra-low Pt loading and a preparation method thereof. The method comprises the following steps: adding a Pt precursor solution into an electrolyte solution to obtain a mixed solution, introducing inert gas into the mixed solution, adding a carbon-based carrier, performing double-pulse electrochemical deposition treatment on the mixed solution by adopting a three-electrode system, and after the deposition is finished, taking out the carbon-based carrier, washing and drying to obtain the Pt/C catalyst with ultralow Pt loading capacity; the carbon carrier is connected with the working electrode, the counter electrode is a Pt sheet, and the reference electrode is Ag/AgCl; the concentration of the Pt precursor in the mixed solution is 1-10 mmol/L. The Pt nano particles prepared by the method have the size of 1-3 nm and are mainly distributed at the edge of a graphite layer and at the defect positions on the graphite layer, and the prepared catalyst has high active specific surface area and is a catalyst with high activity and ultralow Pt loading capacity.
Description
Technical Field
The invention belongs to the technical field of hydrogen energy, and particularly relates to a Pt/C catalyst with ultralow Pt loading and a preparation method thereof.
Background
The types of catalysts in hydrogen fuel cells are mainly platinum-based catalysts, low platinum catalysts and non-platinum catalysts. The commercial catalyst commonly used in hydrogen fuel cells at present is platinum (Pt), which has good molecular adsorption and dissociation characteristics, so that the platinum catalyst is the most ideal and currently only commercialized catalyst material. Currently commercially available is the supported catalyst Pt/C (Pt nanoparticles dispersed on a carbon powder support). The Pt catalyst is one of the core materials of the fuel cell and accounts for more than 40% of the cost of the fuel cell stack. In 9 months of 2020, five departments, such as the finance department, the industry and communications department, jointly issue a notice about developing the demonstration application of the fuel cell automobile, and clearly point out that research and development breakthroughs of key materials and parts, such as catalysts, are mainly supported. In order to improve the performance and reduce the use amount, a Pt nanocrystallization dispersion preparation technology with small grain size is generally adopted. However, there are problems at present: the Pt particles with small particle size can get rid of the constraint of the carrier, migrate to larger particles and are combined to disappear, and the large particles can survive and continue to grow; the small-particle-size Pt particles are more prone to oxidation reaction and diffuse to the surface of the large-particle-size Pt particles in the form of platinum ions to be deposited, and therefore agglomeration is caused. Therefore, the carbon carrier is doped with impurity atoms such as nitrogen, oxygen, boron and the like, so that the surface adhesion of Pt particles and various transition metals (such as Co, ni, mn, fe, cu and the like) is enhanced, the durability is improved, and the anti-migration and agglomeration capabilities of the Pt-containing catalyst are enhanced. The Pt/Ir (Ta) catalyst developed by the American 3M company based on the ultrathin film catalytic technology has been realized at the cathode and the anode, and the average is as low as 0.09mg/cm 2 The amount of platinum used was 9.4kW/g (150 kPa reaction gas pressure) and 11.6kW/g (250 kPa reaction gas pressure) as catalytic power densities. The PtCo/high surface area carbon (HSC) developed by the German public automobile group also makes an important progress, and the catalytic power density and the heat dissipation capacity both exceed the planned target values set by the United states department of energy (2016-2020).
Aiming at the problems of low activity, large dosage and high cost of the platinum-based catalyst required by the preparation of the hydrogen fuel cell, the reduction of the dosage of the platinum-based catalyst and the optimized preparation of the membrane electrode based on the target are important ways for reducing the commercial cost of a hydrogen fuel cell system.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention mainly aims to provide a preparation method of a Pt/C catalyst with ultralow Pt loading.
It is still another object of the present invention to provide a Pt/C catalyst with ultra-low Pt loading prepared by the above method.
The purpose of the invention is realized by the following technical scheme:
a preparation method of an ultralow Pt loading Pt/C catalyst comprises the following steps:
adding a Pt precursor solution into an electrolyte solution to obtain a mixed solution, introducing inert gas into the mixed solution, adding a carbon-based carrier, performing double-pulse electrochemical deposition treatment on the mixed solution by adopting a three-electrode system, and after the deposition is finished, taking out the carbon-based carrier, washing and drying to obtain the Pt/C catalyst with ultralow Pt loading capacity;
wherein, the carbon-based carrier is connected with the working electrode, the counter electrode is a Pt sheet, and the reference electrode is Ag/AgCl;
the concentration of the Pt precursor in the mixed solution is 1 mmol/L-10 mmol/L.
Preferably, the voltage of the double-pulse electrochemical deposition is-0.1 v to +0.6v, and the deposition time is 5s to 200s.
Preferably, the double-pulse electrochemical deposition is firstly performed for 10 to 50ms at a voltage of-0.1 v to-0.02 v and then performed for 5 to 200s at a voltage of +0.58v to +0.6 v.
Preferably, the Pt precursor is H 2 PtCl 6 ，PtCl 4 ，K 2 PtCl 6 The electrolyte solution is perchloric acid solution or sulfuric acid solution, and the concentration of the electrolyte solution is 0.1-0.5 mol/L.
Preferably, the working electrode potential is 0.86v.
Preferably, the carbon-based carrier is one or more of Highly Oriented Pyrolytic Graphite (HOPG), carbon nanotubes, carbon black, biomass carbon and activated carbon.
Preferably, the carbon-based support is Highly Oriented Pyrolytic Graphite (HOPG), a new clean surface is exposed by pretreatment, the side length of a square is 10mm, and the thickness is 2mm.
Preferably, the inert gas is one of helium, argon and nitrogen, and the flow rate is 0.05-0.1 mL/s.
The Pt/C catalyst with ultralow Pt loading is prepared by the method.
The technical scheme of the invention is based on an electrochemical pulse deposition technology. With H 2 PtCl6 is used as a Pt precursor, an electrolyte solution is a perchloric acid solution or a sulfuric acid solution, pulse voltage is-0.1V-0.6V (relative to a standard reference electrode), and nucleation and growth time are respectively controlled to be 10-50ms and 5-200s.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) The catalyst material in the hydrogen fuel cell accounts for more than 40% of the whole fuel system, and the ultralow-load Pt/C catalyst prepared by the method can further reduce the Pt load to 0.05mg/cm 2 Compared with the technology of American 3M company, the consumption of Pt catalyst can be reduced by about 45%, the cost of catalyst can be reduced by about 45%, the loading capacity of catalyst is reduced, and the activity of unit specific surface is hardly reduced.
(2) The aqueous phase preparation method disclosed by the invention is simple to operate and has advantages in enlarged production.
(3) The stability of the Pt nanoparticles is further improved. Compared with the traditional Pt/C catalyst, the Pt nano-particles prepared by the invention have smaller particle size, and the formed sites are more at the defect sites of the carbon-based material, so that the Pt nano-particles and the carbon-based carrier have higher bonding force, and the particle agglomeration phenomenon caused by the migration of the Pt nano-particles on the surface is inhibited.
(4) The prepared Pt nano particles have the grain size of only about 1nm, and compared with the traditional Pt/C catalyst, the Pt particles have higher active surface per unit mass.
Drawings
FIG. 1 is a diagram of a potential setting process and corresponding current time distribution diagram by a two-electrochemical pulse method.
FIG. 2 is an atomic force microscope image of a catalyst product obtained by an electrochemical pulse deposition method and a surface Pt particle size analysis thereof.
FIG. 3 shows room temperature 0.5M H 2 SO 4 Comparison of performance of commercial Pt/C catalyst in electrolyte with the catalyst developed in accordance with the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto, and may be carried out with reference to conventional techniques for process parameters not particularly noted.
Example 1
The solution is based on electrochemical pulse deposition. The specific process is as follows:
(1) A carbon-based carrier was prepared, and Highly Oriented Pyrolytic Graphite (HOPG) was used in this example, with a square side of 10mm and a thickness of 2mm. The HOPG-side exposed surface was taped and pulled to expose a new clean surface, and the treated HOPG was placed in a clean container for use.
(2) Preparing 100mL of 0.1mol/L perchloric acid solution, and adding a proper amount of H 2 PtCl 6 The concentrated solution is placed in a prepared 100mL perchloric acid solution to cause H 2 PtCl 6 The concentration was 1mmol/L.
(3) Taking a clean four-neck flask, repeatedly washing with deionized water for 3 times, air drying, and mixing with the prepared solution containing H 2 PtCl 6 The perchloric acid solution was poured into a four-necked flask.
(4) And taking a clean Ag/AgCl standard reference electrode, repeatedly washing with deionized water for three times, and putting into a flask.
(5) And taking a clean Pt sheet counter electrode, repeatedly washing the counter electrode with deionized water for three times, and putting the counter electrode into a flask.
(6) The HOPG carbon support was attached to the working electrode and suspended above the solution in the flask.
(7) Argon gas was introduced into the solution at a flow rate of 0.05mL/s.
(8) Half an hour later, the HOPG carbon support was placed into solution, as illustrated in fig. 1, while setting the working electrode potential at 0.86V versus a standard hydrogen electrode.
(9) Setting the deposition time and potential of the double pulse method, adopting an electrochemical workstation (Switzerland PGSTAT 302N) during deposition, as shown in the lower graph in figure 1, the nucleation potential of the Pt nano particles is
-0.22v, a nucleation time of 10ms, a Pt nanoparticle growth potential of +0.58v, and a growth time of 180s.
(10) And after the deposition is finished, quickly taking out the HOPG carbon carrier, repeatedly washing the HOPG carbon carrier by using deionized water, and blow-drying the gas to obtain the Pt/C catalyst with the ultralow Pt loading capacity.
(11) And (3) placing the prepared Pt/C catalyst in a clean container to be characterized.
(12) The surface topography of the finished catalyst prepared in this case under an atomic force microscope is shown in fig. 2 (C), the particle size of the Pt nanoparticles on the surface is shown in red in fig. 2 (d), the particle size of the Pt nanoparticles is smaller, only about 1nm, compared with the conventional Pt/C catalyst, pt per unit mass has a higher active surface, and the formation sites are mostly at the defect sites of the carbon-based material.
Example 2
The surface topography under an atomic force microscope of the other two samples obtained using the same procedure as in example 1 with varying Pt nanoparticle nucleation and growth times is shown in fig. 2 (a) and (b), with 2 (a), 2 (b) nano nucleation and growth times of 10ms and 50s,10ms and 100s.
Example 3
Electrochemical activity test of Pt/C catalyst
0.5M H at room temperature 2 SO 4 In the electrolyte, the performances of the commercial Pt/C catalyst are compared with those of the catalyst developed by the invention, as shown in figure 3, the loading amount of the catalyst is reduced, the activity per specific surface is hardly reduced, and the performance of the catalyst is slightly better than that of the commercial Pt/C catalyst.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A preparation method of a Pt/C catalyst with ultralow Pt loading capacity is characterized by comprising the following steps:
adding a Pt precursor solution into an electrolyte solution to obtain a mixed solution, introducing inert gas into the mixed solution, adding a carbon-based carrier, performing double-pulse electrochemical deposition treatment on the mixed solution by adopting a three-electrode system, and after the deposition is finished, taking out the carbon-based carrier, washing and drying to obtain the Pt/C catalyst with ultralow Pt loading capacity;
wherein the carbon-based carrier is connected with the working electrode, the counter electrode is a Pt sheet, and the reference electrode is Ag/AgCl;
the concentration of the Pt precursor in the mixed solution is 1 mmol/L-10 mmol/L.
2. The method of claim 1, wherein the double-pulse electrochemical deposition voltage is-0.1 v to +0.6v, and the deposition time is 5s to 200s.
3. The method for preparing an ultralow Pt loading Pt/C catalyst according to claim 2 wherein the double pulse electrochemical deposition is performed for 10 to 50ms at a voltage of-0.1 v to-0.02 v and then for 5 to 200s at a voltage of +0.58v to +0.6 v.
4. The method of preparing an ultra-low Pt loading Pt/C catalyst according to claim 1, wherein the Pt precursor is H 2 PtCl 6 ，PtCl 4 ，K 2 PtCl 6 The electrolyte solution is perchloric acid solution or sulfuric acid solution, and the concentration of the electrolyte solution is 0.1-0.5 mol/L.
5. The method of making an ultra-low Pt loading Pt/C catalyst according to claim 1 or 2 or 3 or 4 wherein the working electrode potential is 0.86v.
6. The method for preparing an ultralow Pt/C catalyst as recited in claim 1, wherein said carbon-based support is one or more of highly oriented pyrolytic graphite, carbon nanotubes, carbon black, biomass carbon, activated carbon.
7. The method of claim 6, wherein the carbon-based support is highly oriented pyrolytic graphite having square sides of 10mm and a thickness of 2mm.
8. The method of preparing an ultra-low Pt loading Pt/C catalyst according to claim 1, wherein the inert gas is one of helium, argon, and nitrogen, and the flow rate is 0.05-0.1 mL/s.
9. An ultra-low Pt loaded Pt/C catalyst prepared by the process of any one of claims 1 to 8.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4490219A (en) * | 1982-10-07 | 1984-12-25 | International Business Machines Corporation | Method of manufacture employing electrochemically dispersed platinum catalysts deposited on a substrate |
| CN101259410A (en) * | 2008-04-14 | 2008-09-10 | 北京科技大学 | Method for preparing platinum catalyst by electrodeposition |
| WO2013044080A1 (en) * | 2011-09-22 | 2013-03-28 | Brookhaven Science Associates, Llc | Electrochemical synthesis of elongated noble metal nanoparticles, such as nanowires and nanorods, on high-surface area carbon supports |
| CN108155393A (en) * | 2017-12-25 | 2018-06-12 | 苏州擎动动力科技有限公司 | It is a kind of using carbon nanotube as the method for preparing catalyst of carrier |
| CN112934248A (en) * | 2021-02-01 | 2021-06-11 | 东北大学 | Mesoporous carbon matrix-based bifunctional catalyst and magnetoelectric deposition preparation method thereof |
-
2022
- 2022-11-14 CN CN202211420435.2A patent/CN115732709A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4490219A (en) * | 1982-10-07 | 1984-12-25 | International Business Machines Corporation | Method of manufacture employing electrochemically dispersed platinum catalysts deposited on a substrate |
| CN101259410A (en) * | 2008-04-14 | 2008-09-10 | 北京科技大学 | Method for preparing platinum catalyst by electrodeposition |
| WO2013044080A1 (en) * | 2011-09-22 | 2013-03-28 | Brookhaven Science Associates, Llc | Electrochemical synthesis of elongated noble metal nanoparticles, such as nanowires and nanorods, on high-surface area carbon supports |
| CN108155393A (en) * | 2017-12-25 | 2018-06-12 | 苏州擎动动力科技有限公司 | It is a kind of using carbon nanotube as the method for preparing catalyst of carrier |
| CN112934248A (en) * | 2021-02-01 | 2021-06-11 | 东北大学 | Mesoporous carbon matrix-based bifunctional catalyst and magnetoelectric deposition preparation method thereof |
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