CN111342060A - Preparation method of platinum-nickel/nitrogen-doped reduced graphene oxide - Google Patents
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- CN111342060A CN111342060A CN202010141658.XA CN202010141658A CN111342060A CN 111342060 A CN111342060 A CN 111342060A CN 202010141658 A CN202010141658 A CN 202010141658A CN 111342060 A CN111342060 A CN 111342060A
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
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- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
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Abstract
The invention provides a preparation method of platinum-nickel/nitrogen doped reduced graphene oxide, which comprises the following steps: graphene oxide is used as a catalyst carrier; then adding platinum-nickel as a methanol oxidation reaction catalyst to prepare a platinum-nickel/graphene oxide precursor; finally, H is introduced by plasma treatment2And N2And obtaining the platinum-nickel/nitrogen-doped reduced graphene oxide by using the platinum-nickel/graphene oxide precursor. The invention selects platinum-nickel as a methanol oxidation reaction catalyst, nitrogen-doped reduced graphene oxide as a catalyst carrier, adopts a plasma technology preparation method to obtain the platinum-nickel/nitrogen-doped reduced graphene oxide, and adopts reasonable material selection and an advanced preparation method to apply the platinum-nickel/nitrogen-doped reduced graphene oxide toThe methanol fuel cell has good electro-catalytic activity, CO poisoning resistance and long-term stability.
Description
Technical Field
The invention relates to the technical field of methanol fuel cells, in particular to a preparation method of platinum-nickel/nitrogen-doped reduced graphene oxide.
Background
Today, the rapid development of economy, the search for efficient, environment-friendly and low-cost energy resources has become a key problem. The direct methanol fuel cell is a power generation device capable of continuously and directly converting chemical energy in fuel and oxidant into electric energy, and due to the characteristics of environmental protection and high efficiency, the direct methanol fuel cell draws wide attention all over the world. Methanol fuel cells directly utilize methanol or aqueous methanol as the anode fuel and oxygen or air as the oxidant. The methanol reforming device has the characteristics of wide methanol source, convenience in carrying, storage and supplement, high specific energy of volume and mass, simple structure, no need of external reforming equipment and the like, and has wide application prospect in the aspects of portable power supplies, small-sized civil power supplies, vehicle power supplies and the like.
But the direct methanol fuel cell has the problem of low electrocatalytic activity of the methanol anode at present. Since the methanol oxidation mechanism is very complex, some unstable and insoluble intermediate products are generated in the process, and some intermediate products can be adsorbed on the surface of the catalyst, so that the activity of the catalyst is inhibited, the catalyst is poisoned, and the catalyst utilization rate is low, so that the improvement of the catalyst utilization rate is a research hotspot of direct methanol fuel cells.
Disclosure of Invention
The invention aims to: aiming at the problems in the prior art, the preparation method of the platinum-nickel/nitrogen-doped reduced graphene oxide is provided, the platinum-nickel catalyst is efficient and cheap, the nitrogen-doped reduced graphene oxide catalyst carrier can obtain better catalyst performance, and the low-temperature plasma preparation method is simple, energy-saving and efficient. The material can be better applied to methanol fuel cells, and compared with non-nitrogen-doped platinum-nickel/reduced graphene oxide (Pt-Ni/rGO) and commercial platinum/carbon catalysts (Pt/C), the material disclosed by the invention is optimal in electrocatalytic activity, CO poisoning resistance and long-term stability when applied to methanol oxidation reaction.
The invention aims to be realized by the following technical scheme:
a preparation method of platinum-nickel/nitrogen doped reduced graphene oxide is characterized by comprising the following steps: graphene oxide is used as a catalyst carrier; then adding platinum-nickel as a methanol oxidation reaction catalyst to prepare and obtain a platinum-nickel/graphene oxide precursorA body; finally, H is introduced by plasma treatment2And N2And obtaining the platinum-nickel/nitrogen-doped reduced graphene oxide by using the platinum-nickel/graphene oxide precursor.
Further, the preparation method of the graphene oxide comprises the following steps:
(1) mixing flake graphite powder with concentrated sulfuric acid, and controlling the temperature below 4 ℃; then slowly adding potassium permanganate while stirring, and reacting for 2-4 hours;
(2) putting the product obtained in the step (1) in an environment with the temperature of 35-40 ℃ for heat preservation for 1-2 hours, then gradually heating to 70-80 ℃, and slowly adding deionized water; after the reaction is finished, slowly dropping a certain amount of hydrogen peroxide until no bubbles are generated;
(3) and finally, washing the product with hydrochloric acid and deionized water, and then freeze-drying to obtain the graphene oxide of the tawny fluffy material.
Further, in the step (1), the mixing ratio of the flake graphite powder to the concentrated sulfuric acid is as follows: 50ml of concentrated sulfuric acid per 1.5g of flake graphite powder.
Further, the amount of potassium permanganate added in the step (1) is as follows: every 1.5g of the flake graphite powder corresponds to 6g of potassium permanganate.
Further, the amount of deionized water added in the step (2) is as follows: 50ml of deionized water per 50ml of concentrated sulfuric acid.
Further, the added methanol oxidation reaction catalyst is as follows: the mixed solution of the chloroplatinic acid solution and the nickel acetate solution, wherein the ratio of platinum to nickel is 3:1, and the platinum loading amount is 10 wt%.
Further, the preparation method of the platinum-nickel/graphene oxide precursor comprises the following steps: mixing and stirring graphene oxide and deionized water, and performing ultrasonic treatment to obtain a uniform graphene oxide solution; then dropwise adding a methanol oxidation reaction catalyst into the graphene oxide solution; adjusting the pH value of the solution to 9 by using ammonia water, stirring for 12-14 hours, and freeze-drying to obtain the platinum-nickel/graphene oxide precursor.
Further, H is introduced by plasma treatment2And N2The method for preparing the platinum-nickel/graphene oxide precursor comprises the following steps: precursor of platinum-nickel/graphene oxideSpreading on a quartz boat, introducing H2 and N2 under the pressure of 1.0pa, and performing plasma treatment at 150W for 10-15 min; and then taking out the sample, fully mixing, and repeating the plasma treatment step to obtain the platinum-nickel/nitrogen-doped reduced graphene oxide.
Further, the flow ratio of H2 to N2 was 2: 1.
Compared with the prior art, the invention has the following advantages:
1. the use of the platinum-nickel bimetallic catalyst can reduce the consumption of platinum and the cost, the existence of nickel enables water to form hydroxyl under lower potential, and CO intermediates are easier to oxidize and remove, so that the toxicity resistance of the catalyst is effectively improved, electrons can be transferred to platinum due to the existence of nickel, the electronic structure of the platinum is changed, the interaction between the platinum and CO is weakened, and the catalytic performance and the toxicity resistance of the catalyst are effectively improved.
2. By using the nitrogen-doped graphene carrier, on the basis of keeping unique electrical properties, large specific surface area, good mechanical strength and stability of graphene, more positions can be provided for the dispersion of catalyst particles, and the interaction between metal and the carrier is enhanced, so that the electrochemical activity and the durability are improved.
3. The low-temperature plasma preparation method avoids the use of toxic chemical reducing agents, can generate a large amount of active substances in the discharge process, and is simple in step, energy-saving, efficient and suitable for large-scale production.
Drawings
FIG. 1 shows that Pt/C, Pt-Ni/rGO and Pt-Ni/NrGO are respectively in 1M CH3OH and 0.5M H2SO4Cyclic voltammetry test curves in mixed solution;
FIG. 2 is a plot of chronoamperometric tests of Pt/C, Pt-Ni/rGO and Pt-Ni/NrGO at 0.65V, respectively;
FIG. 3 shows Pt/C, Pt-Ni/rGO and Pt-Ni/NrGO respectively at room temperature 1M H2SO4And (3) a CO adsorption and desorption experiment result graph in the solution.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Examples
The invention provides a preparation method of platinum-nickel/nitrogen doped reduced graphene oxide, which comprises the following steps: graphene oxide is used as a catalyst carrier; then adding platinum-nickel as a methanol oxidation reaction catalyst to prepare a platinum-nickel/graphene oxide precursor; finally, H is introduced by plasma treatment2And N2And obtaining the platinum-nickel/nitrogen-doped reduced graphene oxide by using the platinum-nickel/graphene oxide precursor. Wherein:
the preparation method of the graphene oxide comprises the following steps: 1.5g of flake graphite powder (325 mesh) was mixed with 50ml of concentrated sulfuric acid (H)2SO498 percent of mass percent) of the components are mixed and placed in an ice water bath, and the temperature is kept below 4 ℃; followed by slow addition of 6g of potassium permanganate
(KMnO4) Stirring and reacting for 2 hours; placing the mixture in an oil bath at 38 ℃ for heat preservation for 1 hour, then gradually heating to 75 ℃, and slowly adding 50ml of deionized water; after the reaction is finished, a certain amount of hydrogen peroxide (H) is slowly dropped2O230% by mass) until no bubbles are generated, and finally, fully washing the product with hydrochloric acid (HCl, 5% by mass) and a large amount of deionized water, and then freeze-drying to obtain the graphene oxide in the brown fluffy state.
The preparation method of the platinum-nickel/graphene oxide precursor comprises the following steps: dissolving 60mg of prepared graphene oxide in 30ml of deionized water, stirring and carrying out ultrasonic treatment to obtain a uniform graphene oxide solution; then, 1ml of chloroplatinic acid (H) was added2PtCl6) Solution and 0.3245ml of nickel acetate [ (CH)3COO)2Ni]Dropwise adding the solution (platinum-nickel ratio of 3:1 and platinum loading amount of 10 wt%) into the graphene oxide solution, adjusting the pH value of the solution to 9 by using ammonia water, stirring for 12 hours, and freeze-drying to obtain a platinum-nickel/graphene oxide precursor.
The plasma treatment method comprises the following steps: spreading the prepared platinum-nickel/graphene oxide precursor in a quartz boat as thin as possible, and introducing 20sccm H at a pressure of about 1.0pa2And N of 10sccm2Under a voltage of 150WPlasma treatment was performed for 10 minutes. And then taking out the sample, fully mixing, and repeating the plasma treatment step for 10 minutes to obtain the platinum-nickel/nitrogen-doped reduced graphene oxide. Under the same experimental conditions, only 20sccm of H was introduced2Obtaining the platinum-nickel/reduced graphene oxide.
The invention is obtained after the treatment, and is subjected to performance tests with platinum-nickel/reduced graphene oxide and a commercial platinum/carbon catalyst, as shown in figures 1 to 3:
(1) electrocatalytic activity of methanol oxidation reaction: Pt-Ni/NrGO > Pt-Ni/rGO > Pt/C.
(2) CO poisoning resistance: Pt-Ni/NrGO > Pt-Ni/rGO > Pt/C.
(3) Long-term stability: Pt-Ni/NrGO > Pt-Ni/rGO > Pt/C.
Platinum is one of the most effective catalysts found at present, but has limited storage capacity, is expensive, has poor resistance to carbon monoxide (CO) poisoning, and limits the application. The platinum-nickel bimetallic catalyst provided by the invention can reduce the consumption of platinum, and the two metals have synergistic effect, so that the catalytic performance and the toxicity resistance of the catalyst are effectively improved.
The structure, conductivity and specific surface area of the catalyst support also play a crucial role in the performance of the catalyst. Many carbon materials (such as carbon nanotubes, carbon nanofibers, and mesoporous carbon) have been used as catalyst supports, but they have poor corrosion resistance under methanol fuel cell operating conditions. The invention provides a nitrogen-doped graphene carrier, wherein graphene is a unique two-dimensional material, has unique electrical properties, a large specific surface area and good mechanical strength and stability, the nitrogen doping introduces a semiconductor behavior, the conductivity is improved, more positions are provided for the dispersion of catalyst particles, the interaction between metal and the carrier is enhanced, and the structural stability of the metal catalyst is improved, so that the electrochemical activity and the durability of the metal catalyst are improved.
The traditional methods for preparing the catalyst, such as an impregnation reduction method, a coprecipitation method, an electrodeposition method, a microwave-assisted reduction method and the like, have complicated steps, are not energy-saving and time-consuming at high temperature, and the residual surfactant is unfavorable for the performance of the catalyst. The invention provides a simple, energy-saving and efficient low-temperature plasma preparation method, which can generate a large amount of active substances such as electrons, ions, atoms, free radicals and the like in the discharge process, effectively avoids the use of toxic chemical reducing agents, can realize the combination of simplicity and environmental protection, and is suitable for large-scale production.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, it should be noted that any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. A preparation method of platinum-nickel/nitrogen doped reduced graphene oxide is characterized by comprising the following steps: graphene oxide is used as a catalyst carrier; then adding platinum-nickel as a methanol oxidation reaction catalyst to prepare a platinum-nickel/graphene oxide precursor; finally, H is introduced by plasma treatment2And N2And obtaining the platinum-nickel/nitrogen-doped reduced graphene oxide by using the platinum-nickel/graphene oxide precursor.
2. The method for preparing platinum-nickel/nitrogen doped reduced graphene oxide according to claim 1, wherein the method for preparing graphene oxide comprises the following steps:
(1) mixing flake graphite powder with concentrated sulfuric acid, and controlling the temperature below 4 ℃; then slowly adding potassium permanganate while stirring, and reacting for 2-4 hours;
(2) putting the product obtained in the step (1) in an environment with the temperature of 35-40 ℃ for heat preservation for 1-2 hours, then gradually heating to 70-80 ℃, and slowly adding deionized water; after the reaction is finished, slowly dropping a certain amount of hydrogen peroxide until no bubbles are generated;
(3) and finally, washing the product with hydrochloric acid and deionized water, and then freeze-drying to obtain the graphene oxide of the tawny fluffy material.
3. The method for preparing platinum-nickel/nitrogen doped reduced graphene oxide according to claim 2, wherein the ratio of the flake graphite powder mixed with concentrated sulfuric acid in step (1) is as follows: 50ml of concentrated sulfuric acid per 1.5g of flake graphite powder.
4. The preparation method of the platinum-nickel/nitrogen-doped reduced graphene oxide according to claim 2, wherein the amount of potassium permanganate added in the step (1) is as follows: every 1.5g of the flake graphite powder corresponds to 6g of potassium permanganate.
5. The method for preparing platinum-nickel/nitrogen doped reduced graphene oxide according to claim 2, wherein the deionized water is added in the step (2) in an amount of: 50ml of deionized water per 50ml of concentrated sulfuric acid.
6. The preparation method of the platinum-nickel/nitrogen-doped reduced graphene oxide according to claim 1, wherein the added methanol oxidation reaction catalyst is: the mixed solution of the chloroplatinic acid solution and the nickel acetate solution, wherein the ratio of platinum to nickel is 3:1, and the platinum loading amount is 10 wt%.
7. The method for preparing platinum-nickel/nitrogen-doped reduced graphene oxide according to claim 1, wherein the method for preparing the platinum-nickel/graphene oxide precursor comprises the following steps: mixing and stirring graphene oxide and deionized water, and performing ultrasonic treatment to obtain a uniform graphene oxide solution; then dropwise adding a methanol oxidation reaction catalyst into the graphene oxide solution; adjusting the pH value of the solution to 9 by using ammonia water, stirring for 12-14 hours, and freeze-drying to obtain the platinum-nickel/graphene oxide precursor.
8. The method for preparing platinum-nickel/nitrogen doped reduced graphene oxide according to claim 1, wherein H is introduced by plasma treatment2And N2The method for preparing the platinum-nickel/graphene oxide precursor comprises the following steps: spreading the platinum-nickel/graphene oxide precursor in a quartz boat, introducing H2 and N2 under the pressure of 1.0pa, and carrying out plasma treatment for 10-15 minutes under the voltage of 150W; then the sample is taken out, and the sample is taken out,fully mixing, and repeating the plasma treatment step to obtain the platinum-nickel/nitrogen doped reduced graphene oxide.
9. The method for preparing platinum-nickel/nitrogen doped reduced graphene oxide according to claim 8, wherein the flow ratio of H2 to N2 is 2: 1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113769760A (en) * | 2021-09-27 | 2021-12-10 | 安徽工业技术创新研究院六安院 | Preparation method of platinum-nickel alloy nanoparticle/graphene composite catalyst |
| CN114695908A (en) * | 2022-04-21 | 2022-07-01 | 浙江理工大学 | Preparation and application of composite hollow graphene ball-loaded platinum-nickel nanoparticles |
| WO2024170914A1 (en) * | 2023-02-17 | 2024-08-22 | Johnson Matthey Hydrogen Technologies Limited | Supported catalyst |
| RU2827645C1 (en) * | 2024-04-02 | 2024-09-30 | федеральное государственное автономное образовательное учреждение высшего образования "Казанский (Приволжский) федеральный университет" (ФГАОУ ВО КФУ) | Method of producing platinum composite on thermally treated graphene oxide support |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113769760A (en) * | 2021-09-27 | 2021-12-10 | 安徽工业技术创新研究院六安院 | Preparation method of platinum-nickel alloy nanoparticle/graphene composite catalyst |
| CN114695908A (en) * | 2022-04-21 | 2022-07-01 | 浙江理工大学 | Preparation and application of composite hollow graphene ball-loaded platinum-nickel nanoparticles |
| WO2024170914A1 (en) * | 2023-02-17 | 2024-08-22 | Johnson Matthey Hydrogen Technologies Limited | Supported catalyst |
| RU2827645C1 (en) * | 2024-04-02 | 2024-09-30 | федеральное государственное автономное образовательное учреждение высшего образования "Казанский (Приволжский) федеральный университет" (ФГАОУ ВО КФУ) | Method of producing platinum composite on thermally treated graphene oxide support |
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