CN113369492B - Quintuple twin crystal platinum nanorod and preparation method thereof - Google Patents

Quintuple twin crystal platinum nanorod and preparation method thereof Download PDF

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CN113369492B
CN113369492B CN202110641408.7A CN202110641408A CN113369492B CN 113369492 B CN113369492 B CN 113369492B CN 202110641408 A CN202110641408 A CN 202110641408A CN 113369492 B CN113369492 B CN 113369492B
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platinum
nanorod
twin
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quintuple
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CN113369492A (en
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张根磊
方延
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Hefei University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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

Abstract

The invention belongs to the field of nano catalytic materials, and discloses a quintuple twin platinum nanorod and a preparation method thereof. The preparation method has the advantages of simple process, low cost, high yield of the obtained product and good repeatability.

Description

Quintuple twin crystal platinum nanorod and preparation method thereof
Technical Field
The invention belongs to the field of nano catalytic materials, and particularly relates to a preparation method of a quintuple twin platinum nanorod.
Background
Due to excessive consumption of traditional fossil fuels, the degree of air pollution is becoming more and more serious, and the requirement for sustainable renewable clean energy is also becoming more and more urgent. Among them, Direct Ethanol Fuel Cells (DEFCs) have attracted extensive attention from researchers because of a series of advantages such as high energy density, environmental friendliness, low cost, and availability. However, the ethanol electro-oxidation process is complex and has many intermediates, so that the ethanol energy conversion efficiency is low, and the commercialization of the ethanol electro-oxidation process is not facilitated. Researchers found that only platinum (base) nano-materials can stably exist and maintain good catalytic activity under the strong acid environment of a proton exchange membrane of a direct ethanol fuel cell. In addition, the performance of the platinum (base) nano material applied to the fuel cell anode catalyst in the field of catalytic engineering is not only related to the factors such as the size, the components and the morphology of the material, but also has close relation with the dimension of the material. In the platinum (base) nano structures with different dimensions, the one-dimensional platinum (base) nano material not only has the structural advantages of unique anisotropy, higher atom utilization efficiency, rapid charge transfer, good dissolution resistance, aggregation resistance, Ostwald ripening and the like, but also can be used as a template agent for synthesizing other materials with one-dimensional structures and applied to different reaction systems to improve the catalytic performance.
Disclosure of Invention
The invention aims to provide a quintuple twin platinum nanorod and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a quintuple twin platinum nanorod is characterized by comprising the following steps:
step 1, adding glucose and hexadecyl trimethyl ammonium chloride into an oleylamine solution, and uniformly stirring;
step 2, adding platinum acetylacetonate into the solution obtained in the step 1, and ultrasonically stirring until the platinum acetylacetonate is dissolved to obtain a precursor solution;
step 3, reacting the precursor solution obtained in the step 2 at 120-250 ℃ for 4-14 hours;
and 4, after the reaction is finished, cooling to room temperature, and then carrying out centrifugal washing on the obtained product to obtain the quintuple twin platinum nanorod.
Further, in the step 1 and the step 2, the dosage ratio of the oleylamine solution, the glucose, the hexadecyltrimethylammonium chloride and the platinum acetylacetonate is 3-15 mL: 30-200 mg: 2-60 mg: 5-15 mg.
Further, in the step 4, the washing is performed by using a mixed solution of cyclohexane and ethanol, the washing frequency is 3-5 times, and the rotation speed of the centrifugation is 8000-14000 rpm.
The principle of the invention is as follows: platinum acetylacetonate is taken as a precursor, hexadecyl trimethyl ammonium chloride is taken as a morphology directing agent, glucose is taken as a reducing agent, oleylamine is taken as a solvent, and the five-twinning platinum nanorod with uniform size and morphology is synthesized through one-pot reaction.
The invention has the beneficial effects that:
1. the five-twin crystal platinum nanorod is prepared by a one-pot method, and the preparation method is simple in process, low in cost, high in yield and good in repeatability;
2. the product prepared by the method has a uniformly dispersed one-dimensional five-twin crystal structure and consistent size;
3. the one-dimensional five-twin crystal structure prepared by the invention can be used as a template to synthesize other alloy nano materials with one-dimensional structures.
Drawings
FIG. 1 shows LaB of the quintuple twinned platinum nanorod obtained in example 1 6 Transmission Electron Micrographs (TEM) where (a), (b) correspond to different magnifications.
FIG. 2 is a particle size histogram of the quintuple twinned platinum nanorods obtained in example 1.
FIG. 3 is a transmission electron microscope field emission (HRTEM) of the five-twinned platinum nanorods obtained in example 1, in which (a) and (b) correspond to different positions.
FIG. 4 is a selected area electron diffraction pattern (SAED) of the quintuple twinned platinum nanorods obtained in example 1.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
The five-twin platinum nanorod is prepared by the following steps:
step 1, adding 90mg of glucose and 8mg of hexadecyl trimethyl ammonium chloride into 5mL of oleylamine solution, and uniformly stirring;
step 2, adding 10mg of platinum acetylacetonate into the solution obtained in the step 1, and ultrasonically stirring until the platinum acetylacetonate is dissolved to obtain a precursor solution;
step 3, transferring the precursor solution obtained in the step 2 into a hydrothermal reaction kettle, and reacting for 8 hours at 160 ℃;
and 4, after the reaction is finished, cooling to room temperature, and then carrying out centrifugal washing on the obtained product three times (the centrifugal rotating speed is 12000rpm) by using a cyclohexane/ethanol mixed solution (the volume ratio is 1:3) to obtain the quintuple twin platinum nanorod with the one-dimensional structure.
LaB of quintuple twinned platinum nanorod prepared in the embodiment 6 The transmission electron micrograph, the particle size histogram, the field emission transmission electron micrograph, and the selected area electron diffraction are shown in fig. 1(a) and (b) correspond to different magnifications), fig. 2, and fig. 3(a) and (b) correspond to different positions), respectively, and fig. 4. As can be seen from FIGS. 1 to 4, the product obtained in this example has a uniform one-dimensional quintuple twin structure and consistent size, the average length is 38.48nm, and the length-diameter ratio is 6.6: 1.
Example 2
The five-twin platinum nanorod is prepared by the following steps:
step 1, adding 90mg of glucose and 12mg of hexadecyl trimethyl ammonium chloride into 5mL of oleylamine solution, and uniformly stirring;
step 2, adding 10mg of platinum acetylacetonate into the solution obtained in the step 1, and ultrasonically stirring until the platinum acetylacetonate is dissolved to obtain a precursor solution;
step 3, transferring the precursor solution obtained in the step 2 into a hydrothermal reaction kettle, and reacting for 8 hours at 160 ℃;
and 4, after the reaction is finished, cooling to room temperature, and then carrying out centrifugal washing on the obtained product three times (the centrifugal rotating speed is 12000rpm) by using a cyclohexane/ethanol mixed solution (the volume ratio is 1:3) to obtain the quintuple twin platinum nanorod with the one-dimensional structure.
The product obtained in the embodiment is characterized by a uniform one-dimensional five-twinning structure and consistent in size.
Example 3
The five-twin platinum nanorod is prepared by the following steps:
step 1, adding 90mg of glucose and 16mg of hexadecyl trimethyl ammonium chloride into 5mL of oleylamine solution, and uniformly stirring;
step 2, adding 10mg of platinum acetylacetonate into the solution obtained in the step 1, and ultrasonically stirring until the platinum acetylacetonate is dissolved to obtain a precursor solution;
step 3, transferring the precursor solution obtained in the step 2 into a hydrothermal reaction kettle, and reacting for 8 hours at 160 ℃;
and 4, after the reaction is finished, cooling to room temperature, and then carrying out centrifugal washing on the obtained product three times (the centrifugal rotating speed is 12000rpm) by using a cyclohexane/ethanol mixed solution (the volume ratio is 1:3) to obtain the quintuple twin platinum nanorod with the one-dimensional structure.
The product obtained in the embodiment is characterized by a uniform one-dimensional five-twinning structure and consistent in size.
Example 4
The five-twin platinum nanorod is prepared by the following steps:
step 1, adding 90mg of glucose and 8mg of hexadecyl trimethyl ammonium chloride into 10mL of oleylamine solution, and uniformly stirring;
step 2, adding 10mg of platinum acetylacetonate into the solution obtained in the step 1, and ultrasonically stirring until the platinum acetylacetonate is dissolved to obtain a precursor solution;
step 3, transferring the precursor solution obtained in the step 2 into a hydrothermal reaction kettle, and reacting for 8 hours at 160 ℃;
and 4, after the reaction is finished, cooling to room temperature, and then carrying out centrifugal washing on the obtained product three times (the centrifugal rotating speed is 12000rpm) by using a cyclohexane/ethanol mixed solution (the volume ratio is 1:3) to obtain the quintuple twin platinum nanorod with the one-dimensional structure.
The product obtained in the embodiment is characterized by a uniform one-dimensional five-twinning structure and consistent in size.
Example 5
In this example, a five-twin platinum nanorod was prepared as follows:
step 1, adding 90mg of glucose and 16mg of hexadecyl trimethyl ammonium chloride into 10mL of oleylamine solution, and uniformly stirring;
step 2, adding 10mg of platinum acetylacetonate into the solution obtained in the step 1, and ultrasonically stirring until the platinum acetylacetonate is dissolved to obtain a precursor solution;
step 3, transferring the precursor solution obtained in the step 2 into a hydrothermal reaction kettle, and reacting for 8 hours at 160 ℃;
and 4, after the reaction is finished, cooling to room temperature, and then carrying out centrifugal washing on the obtained product three times (the centrifugal rotating speed is 12000rpm) by using a cyclohexane/ethanol mixed solution (the volume ratio is 1:3) to obtain the quintuple twin platinum nanorod with the one-dimensional structure.
The product obtained in the embodiment is characterized by a uniform one-dimensional five-twinning structure and consistent in size.
Example 6
The five-twin platinum nanorod is prepared by the following steps:
step 1, adding 90mg of glucose and 32mg of hexadecyl trimethyl ammonium chloride into 10mL of oleylamine solution, and uniformly stirring;
step 2, adding 10mg of platinum acetylacetonate into the solution obtained in the step 1, and ultrasonically stirring until the platinum acetylacetonate is dissolved to obtain a precursor solution;
step 3, transferring the precursor solution obtained in the step 2 into a hydrothermal reaction kettle, and reacting for 8 hours at 160 ℃;
and 4, after the reaction is finished, cooling to room temperature, and then carrying out centrifugal washing on the obtained product three times (the centrifugal rotating speed is 12000rpm) by using a cyclohexane/ethanol mixed solution (the volume ratio is 1:3) to obtain the quintuple twin platinum nanorod with the one-dimensional structure.
The product obtained in the embodiment is characterized by a uniform one-dimensional five-twinning structure and consistent in size.
Example 7
The five-twin platinum nanorod is prepared by the following steps:
step 1, adding 90mg of glucose and 44mg of hexadecyl trimethyl ammonium chloride into 10mL of oleylamine solution, and uniformly stirring;
step 2, adding 10mg of platinum acetylacetonate into the solution obtained in the step 1, and ultrasonically stirring until the platinum acetylacetonate is dissolved to obtain a precursor solution;
step 3, transferring the precursor solution obtained in the step 2 into a hydrothermal reaction kettle, and reacting for 8 hours at 160 ℃;
and 4, after the reaction is finished, cooling to room temperature, and then carrying out centrifugal washing on the obtained product three times (the centrifugal rotating speed is 12000rpm) by using a cyclohexane/ethanol mixed solution (the volume ratio is 1:3) to obtain the quintuple twin platinum nanorod with the one-dimensional structure.
The product obtained by the embodiment is characterized by a uniform one-dimensional five-twinning structure and consistent size.
Example 8
The five-twin platinum nanorod is prepared by the following steps:
step 1, adding 60mg of glucose and 8mg of hexadecyl trimethyl ammonium chloride into 10mL of oleylamine solution, and uniformly stirring;
step 2, adding 10mg of platinum acetylacetonate into the solution obtained in the step 1, and ultrasonically stirring until the platinum acetylacetonate is dissolved to obtain a precursor solution;
step 3, transferring the precursor solution obtained in the step 2 into a hydrothermal reaction kettle, and reacting for 8 hours at 160 ℃;
and 4, after the reaction is finished, cooling to room temperature, and then carrying out centrifugal washing on the obtained product three times (the centrifugal rotating speed is 12000rpm) by using a cyclohexane/ethanol mixed solution (the volume ratio is 1:3) to obtain the quintuple twin platinum nanorod with the one-dimensional structure.
The product obtained by the embodiment is characterized by a uniform one-dimensional five-twinning structure and consistent size.
Example 9
The five-twin platinum nanorod is prepared by the following steps:
step 1, adding 90mg of glucose and 8mg of hexadecyl trimethyl ammonium chloride into 5mL of oleylamine solution, and uniformly stirring;
step 2, adding 10mg of platinum acetylacetonate into the solution obtained in the step 1, and ultrasonically stirring until the platinum acetylacetonate is dissolved to obtain a precursor solution;
step 3, transferring the precursor solution obtained in the step 2 into a hydrothermal reaction kettle, and reacting for 8 hours at 160 ℃;
and 4, after the reaction is finished, cooling to room temperature, and then carrying out centrifugal washing on the obtained product three times (the centrifugal rotating speed is 8000rpm) by using a cyclohexane/ethanol mixed solution (the volume ratio is 1:3) to obtain the five-twin-crystal platinum nanorod with the one-dimensional structure.
The product obtained in the embodiment is characterized by a uniform one-dimensional five-twinning structure and consistent in size.
Example 10
The five-twin platinum nanorod is prepared by the following steps:
step 1, adding 90mg of glucose and 8mg of hexadecyl trimethyl ammonium chloride into 10mL of oleylamine solution, and uniformly stirring;
step 2, adding 10mg of platinum acetylacetonate into the solution obtained in the step 1, and ultrasonically stirring until the platinum acetylacetonate is dissolved to obtain a precursor solution;
step 3, transferring the precursor solution obtained in the step 2 into a hydrothermal reaction kettle, and reacting for 8 hours at 160 ℃;
and 4, after the reaction is finished, cooling to room temperature, and then carrying out centrifugal washing on the obtained product three times (the centrifugal rotation speed is 10000rpm) by using a cyclohexane/ethanol mixed solution (the volume ratio is 1:3) to obtain the quintuple twin platinum nanorod with the one-dimensional structure.
The product obtained in the embodiment is characterized by a uniform one-dimensional five-twinning structure and consistent in size.
The present invention is not limited to the above exemplary embodiments, and any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (3)

1. A preparation method of a five-twin platinum nanorod is characterized by comprising the following steps:
step 1, adding glucose and hexadecyl trimethyl ammonium chloride into an oleylamine solution, and uniformly stirring;
step 2, adding platinum acetylacetonate into the solution obtained in the step 1, and ultrasonically stirring until the platinum acetylacetonate is dissolved to obtain a precursor solution;
step 3, reacting the precursor solution obtained in the step 2 at 120-250 ℃ for 4-14 hours;
step 4, after the reaction is finished, cooling to room temperature, and then carrying out centrifugal washing on the obtained product to obtain the quintuple twin platinum nanorod;
in the step 1 and the step 2, the dosage ratio of the oleylamine solution, the glucose, the hexadecyl trimethyl ammonium chloride and the acetylacetone platinum is 3-15 mL: 30-200 mg: 2-60 mg: 5-15 mg.
2. The method for preparing the five twin crystal platinum nanorod according to claim 1, wherein the method comprises the following steps: in the step 4, the washing is carried out by using a mixed solution of cyclohexane and ethanol, and the rotating speed of the centrifugation is 8000-14000 rpm.
3. A quintuple twin platinum nanorod prepared by the preparation method of any one of claims 1-2.
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