CN115647382A - Preparation method of platinum nanorod and application of platinum nanorod in fuel cell catalyst - Google Patents
Preparation method of platinum nanorod and application of platinum nanorod in fuel cell catalyst Download PDFInfo
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- CN115647382A CN115647382A CN202211668769.1A CN202211668769A CN115647382A CN 115647382 A CN115647382 A CN 115647382A CN 202211668769 A CN202211668769 A CN 202211668769A CN 115647382 A CN115647382 A CN 115647382A
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Abstract
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of a platinum nanorod and application of the platinum nanorod in a fuel cell catalyst. The preparation method comprises the following specific steps: 1) Adding a precursor of platinum into a reducing solvent, and stirring until the precursor is dissolved to prepare a first solution; 2) Adding a dispersing agent into the obtained first solution, and stirring until the dispersing agent is dissolved to obtain a second solution; 3) Adding a morphology regulating agent into the obtained second solution, and uniformly stirring to obtain a third solution; 4) And (3) reacting the obtained third solution at high temperature and high pressure in a solvent, and separating and washing a solid-phase product to obtain the platinum nanorod. The preparation method is simple, the prepared platinum nanorod has small size and good dispersibility, and the further prepared carbon-supported platinum nanorod catalyst has high catalytic activity and is particularly well applied as a fuel cell catalyst.
Description
Technical Field
The invention belongs to the technical field of fuel cell catalysts, and particularly relates to a preparation method of a platinum nanorod and application of the platinum nanorod in a fuel cell catalyst.
Background
The platinum nano material has excellent catalytic property, and is widely applied to the fields of fuel cells, automobile exhaust purification, petrochemical industry and the like as a catalyst. However, platinum is a precious metal, is scarce in nature and expensive, and how to improve the catalytic activity of platinum nano-materials, so that the improvement of the utilization efficiency of platinum still remains a challenge.
The morphology of the noble metal nano material has an important influence on the catalytic performance of the noble metal nano material. For example, the rod-shaped noble metal nano material has the characteristics of large length-diameter ratio, unique surface atom arrangement, high surface energy, high charge transfer rate and the like, and often shows more excellent catalytic activity and durability compared with the granular nanoparticles. Some organic molecules or inorganic ions can be specifically adsorbed on a specific crystal face of the nano particles, so that the organic molecules or inorganic ions are often used as a morphology regulator to be added into a reaction system for regulating the morphology of the prepared nano particles in the synthesis process of the nano particles. In addition, the morphology of the nanoparticles is also influenced by the combination of the reaction conditions, such as the type and concentration of the reactants, the temperature and the pressure.
For example, for platinum nano materials, oleylamine is a common morphology regulator, and the platinum nano materials with unique morphologies, such as polyhedral platinum nano particles, platinum nanostars, platinum nanowires and the like, can be prepared by adding oleylamine into different reaction systems, and show excellent properties in the field of catalysis. However, the preparation of platinum nanorods of small size and good dispersibility remains a challenge.
Disclosure of Invention
Aiming at the technical problems in the background art, the invention aims to provide a preparation method of a platinum nanorod with a diameter smaller than 2nm and good dispersibility and application of the platinum nanorod in a fuel cell catalyst.
The technical scheme adopted for realizing the aim of the invention is as follows: a preparation method of a platinum nanorod comprises the following preparation steps:
1) Adding a precursor of platinum into a reducing solvent, and stirring until the precursor is dissolved to prepare a first solution;
2) Adding a dispersing agent into the first solution obtained in the step 1), and stirring until the dispersing agent is dissolved to obtain a second solution;
3) Adding a morphology regulating agent into the second solution obtained in the step 2), and uniformly stirring to obtain a third solution;
4) Reacting the third solution obtained in the step 3) under solvothermal high temperature and high pressure, and separating and washing a solid-phase product to obtain the platinum nanorod.
Preferably, the platinum nanorod in the step 4) of the invention is a single crystal, the diameter of the platinum nanorod is less than 2nm, and the length-diameter ratio of the platinum nanorod ranges from 1.5 to 20.
Preferably, the reducing solvent in step 1) of the present invention is dimethylformamide.
Preferably, the precursor of platinum in step 1) of the present invention is chloroplatinic acid or platinum acetylacetonate, and the concentration of the precursor of platinum is in the range of 0.1 to 10mmol/L.
Preferably, the dispersant in step 2) of the present invention is polyvinylpyrrolidone, and has an average molecular weight in the range of 8000 to 360000 and a concentration in the range of 0.1 to 10mg/mL.
Preferably, the morphology regulator in step 3) of the present invention is oleylamine. More preferably, the concentration of the oleylamine is 5 to 15% by volume percentage.
The invention also aims to provide the application of the platinum nanorod in the carbon-supported platinum nano-catalyst.
The technical scheme adopted for realizing the other purpose of the invention is as follows: the application of the platinum nanorods in the fuel cell catalyst, wherein the fuel cell catalyst is prepared by the following steps:
1) Ultrasonically dispersing a platinum nanorod in a micromolecular organic solvent to prepare a platinum nanorod dispersion solution;
2) Adding a carbon carrier into the platinum nanorod dispersion solution prepared in the step 1), performing ultrasonic mixing, performing centrifugal separation to obtain a solid-phase product, drying, and calcining in air to remove organic matters to obtain the fuel cell catalyst.
Preferably, the small molecule organic solvent is selected from one or more of absolute ethyl alcohol, isopropanol or n-propanol.
Preferably, the mass ratio of the platinum nanorod to the carbon carrier is (0.25-1.5): 1.
The invention has the beneficial effects that:
1) The invention takes dimethyl formamide as a solvent and a reducing agent, selects oleylamine as a morphology regulating agent, and creatively prepares the single crystal platinum nanorod with small size and good dispersibility by controlling parameters such as solvent thermal reaction temperature, raw material concentration and the like.
2) The preparation method of the platinum nanorod is simple and low in cost, the prepared platinum nanorod is small in diameter and good in dispersity, and the further prepared carbon-supported platinum nanorod catalyst has high catalytic activity and is particularly good in application as a fuel cell catalyst.
Drawings
FIG. 1 is a TEM image of Pt nanorods prepared in example 1 of the present invention.
FIG. 2 is a high-resolution TEM image of Pt nanorods prepared in example 1 of the present invention.
FIG. 3 is a graph showing oxygen reduction performance of carbon-supported platinum nanorod catalyst (PtNRs/C, 40%) and commercial platinum-carbon catalyst (Pt/C, JM 40%) prepared in example 4 of the present invention.
FIG. 4 is a TEM image of Pt nanoparticles prepared in comparative example 2 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
The invention relates to a preparation method of a platinum nanorod, which comprises the following preparation steps:
1) Adding a precursor of platinum into a reducing solvent, and stirring until the precursor is dissolved to prepare a first solution;
2) Adding a dispersing agent into the first solution obtained in the step 1), and stirring until the dispersing agent is dissolved to obtain a second solution;
3) Adding a morphology regulating agent into the second solution obtained in the step 2), and uniformly stirring to obtain a third solution;
4) Reacting the third solution obtained in the step 3) under solvothermal high temperature and high pressure, and separating and washing a solid-phase product to obtain the platinum nanorod.
Preferably, the reducing solvent in step 1) is dimethylformamide; the precursor of the platinum is selected from one of chloroplatinic acid or platinum acetylacetonate.
Preferably, the dispersant in the step 2) is polyvinylpyrrolidone, the average molecular weight is 8000-360000, and the concentration is 0.1-10 mg/mL.
Preferably, the morphology regulator in the step 3) is oleylamine; the concentration of the oleylamine is 5-15% by volume percentage.
The invention provides an application of a platinum nanorod in a carbon-supported platinum nanorod catalyst, which is used as a fuel cell catalyst.
Example 1
Adding 15.5mg of chloroplatinic acid hexahydrate, 3mg of polyethylene and pyrrolidone into 10mL of dimethylformamide, stirring for dissolving, adding 1mL of oleylamine, uniformly stirring, transferring the obtained solution to a stainless steel high-pressure reaction kettle, heating to 180 ℃, reacting for 6 hours, centrifuging the obtained solution (rotating speed of 12000 r/min, centrifuging time of 10 min) to obtain a solid-phase product, and washing with ethanol to obtain the platinum nanorod.
FIG. 1 is a TEM image of the Pt nanorod prepared in example 1 of the present invention, which has a width of less than 2nm and good dispersibility. FIG. 2 is a high-resolution TEM image of the Pt nanorod prepared in example 1 of the present invention, illustrating that the Pt nanorod prepared is a single crystal.
Example 2
Adding 0.52mg of chloroplatinic acid hexahydrate, 1mg of polyethylene and pyrrolidone into 10mL of dimethylformamide, stirring for dissolving, adding 0.5mL of oleylamine, uniformly stirring, transferring the obtained solution to a stainless steel high-pressure reaction kettle, heating to 220 ℃, reacting for 4 hours, centrifuging the obtained solution (rotating speed of 12000 r/min, centrifuging time of 10 min) to obtain a solid-phase product, and washing with ethanol to obtain the platinum nanorod.
Example 3
Adding 52mg of chloroplatinic acid hexahydrate, 100mg of polyethylene and pyrrolidone into 10mL of dimethylformamide, stirring for dissolving, adding 1.5mL of oleylamine, uniformly stirring, transferring the obtained solution to a stainless steel high-pressure reaction kettle, heating to 140 ℃, reacting for 12 hours, centrifuging the obtained solution (at the rotating speed of 12000 r/min for 10 min) to obtain a solid-phase product, and washing with ethanol to obtain the platinum nanorod.
Example 4
Adding 5mg of the platinum nanorod obtained in example 1 into 10mL of absolute ethanol to obtain an ethanol solution of the platinum nanorod, adding 7.5mg of a carbon carrier (Vulcan XC-72), ultrasonically mixing for 2h, performing centrifugal separation (4000 revolutions/min, 10 min) to obtain a solid-phase product, drying, calcining in air to remove organic matters at 220 ℃ for 1 h to obtain the carbon-supported platinum nanorod catalyst with the platinum content of 40% (PtNRs/C40%).
Example 5
5mg of the platinum nanorods prepared in example 1 were added into 25mL of absolute ethanol and 25mL of isopropanol to prepare an isopropanol solution of the platinum nanorods, 20mg of a carbon carrier (Vulcan XC-72) was added, and after ultrasonic mixing for 2 hours, centrifugal separation (4000 rpm, 10 min) was performed to obtain a solid phase product, which was dried and then calcined in air to remove organic matters at a calcination temperature of 220 ℃ for 1 hour to obtain a carbon-supported platinum nanorod catalyst with a platinum content of 20% (PtNRs/C20%).
Example 6
Adding 5mg of the platinum nanorod obtained in example 1 into 5mL of n-propanol to obtain an n-propanol solution of the platinum nanorod, adding 3.3mg of a carbon carrier (Vulcan XC-72), ultrasonically mixing for 2h, performing centrifugal separation (4000 revolutions/min, 10 min) to obtain a solid-phase product, drying, calcining in air to remove organic matters at 220 ℃ for 1 h to obtain the carbon-supported platinum nanorod catalyst with the platinum content of 60% (PtNRs/C60%).
The catalytic activity of the oxygen reduction reaction of the carbon-supported platinum nanorod catalyst of example 4 was tested by the rotating disk electrode method and compared with a commercial platinum-carbon catalyst for Johnson Matthey (Pt/C JM 40%) having the same platinum content under the same test conditions. As shown in FIG. 2, the polarization curves of the carbon-supported platinum nanorod catalyst (PtNRs/C, 40%) and the commercial platinum-carbon catalyst (Pt/C, JM 40%) for catalyzing oxygen reduction reaction are shown. According to the Koutecky-Levich formula and the corresponding current value of 0.9V in the polarization curve, the catalytic activities of the carbon-supported platinum nanorod catalyst (PtNRs/C, 40%) and the commercial platinum-carbon catalyst (Pt/C, JM 40%) on the oxygen reduction reaction are respectively 350A/gpt (0.9V vs RHE) and 225A/gpt (0.9V vs RHE) through calculation.
It can be seen that the catalytic activity of the carbon-supported platinum nanorod catalyst (PtNRs/C, 40%) for the oxygen reduction reaction is superior to that of the commercial platinum-carbon catalyst (Pt/C, JM 40%).
Comparative example 1
Adding 15.5mg of chloroplatinic acid hexahydrate, 3mg of polyethylene and pyrrolidone into 10mL of dimethylformamide, stirring for dissolving, transferring the obtained solution to a stainless steel high-pressure reaction kettle, reacting for 6 hours at 180 ℃, centrifuging the obtained solution to obtain a solid-phase product, cleaning the solid-phase product with ethanol for three times, and ultrasonically dispersing the solid-phase product in the ethanol solution again. In this comparative example, no morphology control agent oleylamine was introduced, and platinum nanorods could not be obtained.
Comparative example 2
In the chinese patent CN113369492B, platinum acetylacetonate is used as a precursor, cetyltrimethylammonium chloride is used as a morphology regulator, glucose is used as a reducing agent, and oleylamine is used as a solvent to synthesize a platinum nanorod with a quintuple twin crystal structure having a uniform size and morphology, the average length is 38.48nm, and the length-diameter ratio is 6.6:1, average width 5.8nm.
In this comparative example, cetyltrimethylammonium chloride was used as a morphology modifier, and the rest was the same as in example 1. As a result: as shown in FIG. 4, the product is a nearly spherical platinum nanoparticle, and platinum nanorods cannot be obtained.
Claims (10)
1. A preparation method of a platinum nanorod is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
1) Adding a precursor of platinum into a reducing solvent, and stirring until the precursor is dissolved to prepare a first solution;
2) Adding a dispersing agent into the first solution obtained in the step 1), and stirring until the dispersing agent is dissolved to obtain a second solution;
3) Adding a morphology regulating agent into the second solution obtained in the step 2), and uniformly stirring to obtain a third solution;
4) Reacting the third solution obtained in the step 3) under solvothermal high temperature and high pressure, and separating and washing a solid-phase product to obtain the platinum nanorod.
2. The method for preparing platinum nanorods according to claim 1, characterized in that: in the step 4), the platinum nanorod is a single crystal, the diameter of the platinum nanorod is less than 2nm, and the length-diameter ratio of the nanorod ranges from 1.5 to 20.
3. The method for preparing platinum nanorods according to claim 1, characterized in that: in the step 1), the reducing solvent is dimethylformamide, the precursor of the platinum is chloroplatinic acid or acetylacetone platinum, and the concentration range of the precursor of the platinum is 0.1-10 mmol/L.
4. The method for preparing platinum nanorods according to claim 1, characterized in that: in the step 2), the dispersant is polyvinylpyrrolidone, the average molecular weight range is 8000-360000, and the concentration range is 0.1-10 mg/mL.
5. The method for preparing platinum nanorods according to claim 1, characterized in that: the morphology regulating agent in the step 3) is oleylamine, and the concentration range of the oleylamine is 5-15% by volume percentage.
6. The method for preparing platinum nanorods according to claim 1, characterized in that: the solvent reacts under high temperature and high pressure, the reaction temperature is 140-220 ℃, and the reaction time is 4-12 hours.
7. Use of platinum nanorods prepared according to the method of any one of claims 1 to 6, characterized in that: for use in fuel cell catalysts.
8. Use according to claim 7, characterized in that: the fuel cell catalyst is prepared by the following steps:
1) Ultrasonically dispersing the platinum nanorods in a micromolecular organic solvent to prepare a platinum nanorod dispersion solution;
2) Adding a carbon carrier into the platinum nanorod dispersion solution prepared in the step 1), performing ultrasonic mixing, performing centrifugal separation to obtain a solid-phase product, drying, and calcining in air to remove organic matters to obtain the fuel cell catalyst.
9. Use according to claim 8, characterized in that: the small molecular organic solvent is selected from one or more of absolute ethyl alcohol, isopropanol or n-propanol.
10. Use according to claim 8, characterized in that: the mass ratio of the platinum nano-rod to the carbon carrier is (0.25-1.5) to 1.
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