CN109713323B - Preparation method of PtNi/C alloy catalyst - Google Patents
Preparation method of PtNi/C alloy catalyst Download PDFInfo
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- CN109713323B CN109713323B CN201811469538.1A CN201811469538A CN109713323B CN 109713323 B CN109713323 B CN 109713323B CN 201811469538 A CN201811469538 A CN 201811469538A CN 109713323 B CN109713323 B CN 109713323B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 45
- 229910002844 PtNi Inorganic materials 0.000 title claims abstract description 33
- 229910001339 C alloy Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000002904 solvent Substances 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- SHWZFQPXYGHRKT-FDGPNNRMSA-N (z)-4-hydroxypent-3-en-2-one;nickel Chemical compound [Ni].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O SHWZFQPXYGHRKT-FDGPNNRMSA-N 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 23
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000006722 reduction reaction Methods 0.000 claims 2
- 238000002525 ultrasonication Methods 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 13
- 239000000446 fuel Substances 0.000 abstract description 5
- 238000007598 dipping method Methods 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 44
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 30
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 15
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 15
- 239000001301 oxygen Substances 0.000 description 15
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 229920006395 saturated elastomer Polymers 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000009210 therapy by ultrasound Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 230000004913 activation Effects 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 229910021397 glassy carbon Inorganic materials 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 230000010757 Reduction Activity Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000002604 ultrasonography Methods 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 discloses a preparation method of a PtNi/C alloy catalyst. The invention takes Pt/C and nickel acetylacetonate which are commercialized at present as precursors, takes ethanol as a solvent, adopts the methods of dipping and thermal reduction to prepare the PtNi/C alloy catalyst, and is applied to the ORR reaction of a fuel cell cathode. The catalyst exhibited performance in half cell testing of the ORR reaction that exceeded that of the current commercial Pt/C catalyst.
Description
Technical Field
The invention relates to a preparation method of a PtNi/C alloy catalyst, which can be applied to the cathode Oxygen Reduction (ORR) Reaction of a fuel cell.
Background
Pt/C has long been recognized as the best catalyst for low temperature fuel cells. Both for the HOR reaction at its anode and for the ORR at its cathode have excellent catalytic activity. However, the platinum reserves are rare and expensive, which seriously affects the application of the Pt/C catalyst in the fuel cell industrialization. The invention adopts a metal alloy catalyst of Pt and Ni to replace the traditional Pt/C. Research shows that the Pt-based alloy catalyst not only can reduce the consumption of platinum, but also can improve the catalytic activity of Pt by changing the d-energy band electron state of the Pt.
Disclosure of Invention
The invention aims to provide a preparation method of a PtNi/C alloy catalyst, aiming at overcoming the defects of the prior art, the method prepares the PtNi/C alloy catalyst by dipping reduction, and can effectively reduce the use amount of Pt and improve the activity of the catalyst.
The preparation method of the PtNi/C alloy catalyst comprises the following steps: dissolving nickel acetylacetonate in ethanol, adding a commercial Pt/C catalyst, forming a uniformly distributed colloid-like solution by the system through ultrasonic dispersion, volatilizing the solvent to obtain powder, reducing the powder by hydrogen heat, washing and drying to obtain the PtNi/C alloy catalyst.
In the above scheme, the molar ratio of nickel acetylacetonate to nickel and Pt in the commercial Pt/C catalyst is preferably 1: 1.
The ultrasound should generally be not less than 1 hour.
The hydrogen thermal reduction refers to heat treatment under an atmosphere containing hydrogen. The atmosphere is preferably a mixture of hydrogen and argon, with hydrogen being present in a proportion of 5% by volume.
The heat treatment specifically comprises the following steps: heating from room temperature to 350 ℃ at a heating rate of 2-5 ℃/min, standing at the temperature for 1h, heating to 600 ℃ at 2-5 ℃/min, standing at 600 ℃ for 1h, heating to 700 ℃ at 2-5 ℃/min, standing at the temperature for 2-3 h, and naturally cooling.
Compared with the prior art, the invention has the beneficial effects that:
the PtNi/C alloy catalyst is prepared by taking the currently commercialized Pt/C catalyst and nickel acetylacetonate as precursors and ethanol as a solvent and adopting an immersion thermal reduction method, can be applied to the ORR reaction of a fuel cell cathode, shows the performance superior to that of the currently commercialized Pt/C catalyst in a half-cell test of the ORR reaction, namely the catalyst prepared by the invention has higher activity compared with the commercial Pt/C catalyst, can effectively reduce the metal dosage of platinum, particularly adopts a slow-heating three-stage heat preservation treatment method, and is more favorable for obtaining the high-activity PtNi/C alloy catalyst.
Drawings
FIG. 1 is an HR-TEM image of a PtNi/C alloy catalyst prepared by the present invention;
FIG. 2 shows PtNi/C prepared in example 1 under an atmosphere of argon and oxygen and 0.1M HClO4Electrochemical performance in solution;
FIG. 3 is a commercial Pt/C0.1M HClO in argon and oxygen atmosphere4Electrochemical performance in solution;
FIG. 4 shows 0.1M HClO in an oxygen atmosphere for PtNi/C obtained in comparative example 24Electrochemical performance in solution;
FIG. 5 shows 0.1M HClO in an oxygen atmosphere for PtNi/C obtained in comparative example 34Electrochemical performance in solution;
FIG. 6 is0.1M HClO of PtNi/C obtained in comparative example 4 in an oxygen atmosphere4Electrochemical performance in solution;
detailed description of the preferred embodiments
Example 1
Preparing a PtNi/C alloy catalyst:
1) 13.2mg of nickel acetylacetonate was dissolved in 100mL of an anhydrous ethanol solution, and 40mg of Johnson Matthey Pt/C with a metal loading of 20% was dispersed in the solution.
2) And (2) carrying out ultrasonic treatment on the solution obtained in the step 1) for at least 1 hour to form a uniformly distributed colloid-like solution (i.e. ink solution).
3) Heating the solution in the step 2) and electromagnetically stirring to volatilize the solvent, and finally obtaining solvent-free mixture powder.
4) Placing the mixture powder obtained in the step 3) in a quartz boat, and placing in a hydrogen atmosphere to carry out heating reduction according to a set temperature-raising program; the temperature rising procedure is as follows:
the initial temperature is room temperature, the temperature is raised to 350 ℃ at the heating rate of 2-5 ℃/min, the temperature is kept for 1h at the temperature, then the temperature is raised to 600 ℃ at the heating rate of 2-5 ℃/min, the temperature is kept for 1h at the temperature, then the temperature is raised to 700 ℃ at the heating rate of 2-5 ℃/min, the temperature is kept for 2-3 h at the temperature, and the PtNi/C alloy catalyst is obtained after natural cooling.
FIG. 1 is an HR-TEM image of the catalyst prepared in this example, in which a superlattice peak (001) is clearly observed, demonstrating that an alloy has been formed and that an Ordered alloy Ordered-PtNi/C (O-PtNi/C) is formed with a particle size of 5 to 10 nm.
Taking a mixture of isopropanol and water as a solvent, dispersing the prepared PtNi/C in a mixed solution of isopropanol and water, performing ultrasonic treatment for several hours, and dropping the mixture on a glassy carbon electrode after the mixture is uniformly dispersed so that the metal loading of the catalyst is 30 mu g/cm2. Half-cell testing was performed on an electrochemical workstation after evaporation of its solvent in an atmosphere of isopropanol. HClO with an environment of 0.1M was tested4The solution was first saturated with argon HClO4In solution, the activation is performed by scanning back and forth in a voltage range of 0V to 1.1V. Then in HClO saturated with oxygen4Testing of redox in solutionThe activity was then measured by half-wave potential at 900 rpm. The test results are shown in FIG. 2. The half-wave potential thereof was 0.91V.
Comparative example 1
Taking a Johnson Matthey commercial Pt/C catalyst with the metal loading of 20 percent, taking a mixture of isopropanol and water as a solvent, dispersing Pt/C in a mixed solution of isopropanol and water, carrying out ultrasonic treatment for several hours, dripping the Pt/C on a glassy carbon electrode after the Pt/C is uniformly dispersed, and enabling the metal loading of the catalyst to be 30 mu g/cm2. Half-cell testing was performed on an electrochemical workstation after evaporation of its solvent in an atmosphere of isopropanol. HClO with an environment of 0.1M was tested4The solution was first saturated with argon HClO4In solution, the activation is performed by scanning back and forth in a voltage range of 0V to 1.1V. Then in HClO saturated with oxygen4The solution was tested for oxygen reduction activity, and then tested for half-wave potential at 900rpm for revolutions. The test results are shown in FIG. 3. The half-wave potential thereof was 0.90V.
Comparative example 2
Preparing a PtNi/C alloy catalyst:
1) 13.2mg of nickel acetylacetonate was dissolved in 100mL of an anhydrous ethanol solution, and 40mg of Johnson Matthey Pt/C with a metal loading of 20% was dispersed in the solution.
2) And (2) carrying out ultrasonic treatment on the solution obtained in the step 1) for at least 1 hour to form a uniformly distributed colloid-like solution (i.e. ink solution).
3) Heating the solution in the step 2) and electromagnetically stirring to volatilize the solvent, and finally obtaining solvent-free mixture powder.
4) Placing the mixture powder obtained in the step 3) in a quartz boat, and placing in a hydrogen atmosphere to carry out heating reduction according to a set temperature-raising program; the temperature rising procedure is as follows:
the initial temperature is room temperature, the temperature is raised to 350 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 1h at the temperature, then the temperature is raised to 600 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 1h at the temperature, then the temperature is raised to 700 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 2-3 h at the temperature, and the PtNi/C alloy catalyst is obtained after natural cooling.
Using a mixture of isopropanol and water asSolvent, dispersing the prepared PtNi/C in a mixed solution of isopropanol and water, performing ultrasonic treatment for several hours, and dripping the mixture on a glassy carbon electrode after the mixture is uniformly dispersed to ensure that the metal loading of the catalyst is 30 mu g/cm2. Half-cell testing was performed on an electrochemical workstation after evaporation of its solvent in an atmosphere of isopropanol. HClO with an environment of 0.1M was tested4The solution was first saturated with argon HClO4In solution, the activation is performed by scanning back and forth in a voltage range of 0V to 1.1V. Then in HClO saturated with oxygen4The solution was tested for oxygen reduction activity, and then tested for half-wave potential at 900rpm for revolutions. The test results are shown in FIG. 4. The half-wave potential thereof was 0.87V.
Comparative example 3
Preparing a PtNi/C alloy catalyst:
1) 13.2mg of nickel acetylacetonate was dissolved in 100mL of an anhydrous ethanol solution, and 40mg of Johnson Matthey Pt/C with a metal loading of 20% was dispersed in the solution.
2) And (2) carrying out ultrasonic treatment on the solution obtained in the step 1) for at least 1 hour to form a uniformly distributed colloid-like solution (i.e. ink solution).
3) Heating the solution in the step 2) and electromagnetically stirring to volatilize the solvent, and finally obtaining solvent-free mixture powder.
4) Placing the mixture powder obtained in the step 3) in a quartz boat, and placing in a hydrogen atmosphere to carry out heating reduction according to a set temperature-raising program; the temperature rising procedure is as follows:
the initial temperature is room temperature, the temperature is raised at the rate of 2-5 ℃/min to 350 ℃, the temperature is kept for 1h at 350 ℃, then the temperature is raised at the rate of 2-5 ℃/min to 700 ℃, the temperature is kept for 2-3 h, and the PtNi/C alloy catalyst is obtained after natural cooling.
Taking a mixture of isopropanol and water as a solvent, dispersing the prepared PtNi/C in a mixed solution of isopropanol and water, performing ultrasonic treatment for several hours, and dropping the mixture on a glassy carbon electrode after the mixture is uniformly dispersed so that the metal loading of the catalyst is 30 mu g/cm2. Half-cell testing was performed on an electrochemical workstation after evaporation of its solvent in an atmosphere of isopropanol. HClO with an environment of 0.1M was tested4The solution is first saturated with argonAnd HClO of4In solution, the activation is performed by scanning back and forth in a voltage range of 0V to 1.1V. Then in HClO saturated with oxygen4The solution was tested for oxygen reduction activity, and then tested for half-wave potential at 900rpm for revolutions. The test results are shown in FIG. 5. The half-wave potential thereof was 0.875V.
Comparative example 4
Preparing a PtNi/C alloy catalyst:
1) 13.2mg of nickel acetylacetonate was dissolved in 100mL of an anhydrous ethanol solution, and 40mg of Johnson Matthey Pt/C with a metal loading of 20% was dispersed in the solution.
2) And (2) carrying out ultrasonic treatment on the solution obtained in the step 1) for at least 1 hour to form a uniformly distributed colloid-like solution (i.e. ink solution).
3) Heating the solution in the step 2) and electromagnetically stirring to volatilize the solvent, and finally obtaining solvent-free mixture powder.
4) Placing the mixture powder obtained in the step 3) in a quartz boat, and placing in a hydrogen atmosphere to carry out heating reduction according to a set temperature-raising program; the temperature rising procedure is as follows:
the initial temperature is room temperature, the temperature is raised at the rate of 2-5 ℃/min to 600 ℃, the temperature is kept for 1h at the temperature of 600 ℃, then the temperature is raised at the rate of 2-5 ℃/min to 700 ℃, the temperature is kept for 2-3 h, and the PtNi/C alloy catalyst is obtained after natural cooling.
Taking a mixture of isopropanol and water as a solvent, dispersing the prepared PtNi/C in a mixed solution of isopropanol and water, performing ultrasonic treatment for several hours, and dropping the mixture on a glassy carbon electrode after the mixture is uniformly dispersed so that the metal loading of the catalyst is 30 mu g/cm2. Half-cell testing was performed on an electrochemical workstation after evaporation of its solvent in an atmosphere of isopropanol. HClO with an environment of 0.1M was tested4The solution was first saturated with argon HClO4In solution, the activation is performed by scanning back and forth in a voltage range of 0V to 1.1V. Then in HClO saturated with oxygen4The solution was tested for oxygen reduction activity, and then tested for half-wave potential at 900rpm for revolutions. The test results are shown in FIG. 6. The half-wave potential thereof was 0.89V.
Claims (4)
1. A preparation method of a PtNi/C alloy catalyst is characterized by comprising the following steps: dissolving nickel acetylacetonate in ethanol, adding a commercial Pt/C catalyst with 20% of metal load, forming a uniformly distributed colloid-like solution by the system through ultrasonic dispersion, volatilizing the solvent to obtain powder, carrying out hydrogen thermal reduction, washing and drying to obtain the PtNi/C alloy catalyst; the hydrogen thermal reduction refers to heat treatment in an atmosphere containing hydrogen; the heat treatment specifically comprises the following steps: heating from room temperature to 350 ℃ at a heating rate of 2-5 ℃/min, standing at the temperature for 1h, heating to 600 ℃ at 2-5 ℃/min, standing at 600 ℃ for 1h, heating to 700 ℃ at 2-5 ℃/min, standing at the temperature for 2-3 h, and naturally cooling.
2. The method of claim 1, wherein the molar ratio of nickel acetylacetonate to Pt in the commercial Pt/C catalyst is 1: 1.
3. The method for preparing a PtNi/C alloy catalyst according to claim 1, wherein the ultrasonication is not less than 1 hour.
4. The method of claim 1, wherein the hydrogen-containing atmosphere is a mixture of hydrogen and argon, and the volume ratio of hydrogen is 5%.
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