CN115815617A - Self-assembled iridium nanoflower and preparation method thereof - Google Patents
Self-assembled iridium nanoflower and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of nano catalytic materials, and discloses a self-assembled iridium nanoflower and a preparation method thereof. The preparation method has the advantages of simple process, easy operation, low cost and high yield of the obtained product.
Description
Technical Field
The invention belongs to the field of nano catalytic materials, and particularly relates to a self-assembled iridium nanoflower and a preparation method thereof.
Background
The energy problem is an indispensable ring for the scientific and technological development, however, with the proposition of the "double carbon" strategy, the social demand for clean energy is more and more intense. In this context, hydrogen has been paid attention by researchers due to its advantages of high calorific value, no pollution, wide sources, and the like. Among conventional hydrogen production schemes, hydrogen production by water electrolysis is considered to be a promising approach because it completely gets rid of the dependence on fossil fuels and can be well interfaced with other renewable energy conversion devices. However, the current hydrogen production by water electrolysis faces a difficult problem, the anodic oxygen evolution reaction has an excessive overpotential, and the overpotential of the cathode is yet to be reduced, and electrode materials which can stably operate and maintain activity under the large overpotential are very scarce, so that the commercialization process of hydrogen production by water electrolysis is hindered. Iridium (based) materials have relatively excellent free energy for hydrogen adsorption, theoretically can obtain a small overpotential, and can maintain strong stability at such a large overpotential as an oxygen evolution reaction, and therefore, are considered to be one of the best electrode materials for an oxygen evolution reaction in current research, and as one of the most excellent elements in chemical stability, development of an electrode material for a hydrogen evolution reaction for an iridium (based) material is also expected to realize stable operation for a long time. Meanwhile, in the current research, the size, dimension and morphology of the catalyst electrode material can influence the final activity and stability. The self-assembled nano material has unique structural advantages such as anisotropy, excellent structural stability and strong anti-dissolving capacity, and can be used as a base material to modify or used in different systems to improve the catalytic performance and stability.
Disclosure of Invention
The invention aims to provide a self-assembled iridium nanoflower and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of self-assembled iridium nanoflower is characterized by comprising the following steps:
step 1, sequentially adding 4-20 mg of iridium trichloride hydrate and 10-30 mg of polyvinylpyrrolidone into 3-9 mL of organic solvent, uniformly stirring by magnetic force, and then performing ultrasonic treatment for 20-50 min to obtain a homogeneous solution;
step 3, transferring the precursor solution obtained in the step 2 to a polytetrafluoroethylene reaction kettle, and carrying out hydrothermal reaction for 7-9 hours in an oven preheated to 80-120 ℃;
and 4, after the reaction is finished, keeping the oven sealed, cooling the product in the oven to room temperature, and then centrifugally washing the product to obtain the self-assembled iridium nanoflower.
Further, the solvent is N-methylpyrrolidone, N-vinylpyrrolidone or N-ethylpyrrolidone.
Further, the centrifugal washing in step 4 is centrifugal washing three times at 12000rpm using acetone for 10min each time.
The principle of the invention is as follows: the self-assembly iridium nanoflower with uniform size and shape can be synthesized by a one-pot method under mild conditions by taking iridium trichloride hydrate as a precursor, polyvinylpyrrolidone as a surfactant, formic acid as a reducing agent and a surface directing agent, and N-methylpyrrolidone as a solvent (N-vinylpyrrolidone or N-ethylpyrrolidone can also be used as the solvent, but the N-methylpyrrolidone is the best in repeatability).
The invention has the beneficial effects that:
1. the self-assembled iridium nanoflower is prepared by a one-pot method, and the preparation method is simple in process, low in cost and high in yield;
2. the product prepared by the method is in a uniformly dispersed self-assembled nanometer flower shape and has consistent size;
3. the self-assembly iridium nanometer flower structure prepared by the invention can be used as a template to synthesize other alloy nanometer materials with the self-assembly nanometer flower structure.
Drawings
Fig. 1 and 2 are FESEM images of the self-assembled iridium nanoflower obtained in example 1, wherein fig. 1 and 2 correspond to different magnifications.
Fig. 3 and 4 are TEM images of the self-assembled iridium nanoflower obtained in example 1, wherein fig. 3 and 4 correspond to different magnifications.
Fig. 5 is X-ray energy spectrum EDS data of the self-assembled iridium nanoflower 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
This example prepares self-assembled iridium nanoflowers as follows:
step 1, adding 12mg of iridium trichloride hydrate and 20mg of polyvinylpyrrolidone into 6mL of N-methylpyrrolidone in sequence, uniformly stirring by magnetic force, and performing ultrasonic treatment for 40min to obtain a homogeneous solution.
And 2, quickly adding 2mL of formic acid into the homogeneous solution obtained in the step 1 to obtain a precursor solution.
And 3, transferring the precursor solution obtained in the step 2 to a polytetrafluoroethylene reaction kettle, and carrying out hydrothermal reaction for 7 hours in an oven preheated to 100 ℃.
And 4, after the reaction is finished, keeping the oven sealed, cooling the product to room temperature in the oven, and then centrifugally washing the obtained product for three times at 12000rpm by using acetone, wherein the centrifugal time is 10min each time, so that the self-assembled iridium nanoflower is obtained.
The scanning electron microscope image, the transmission electron microscope image and the X-ray energy spectrum of the self-assembled iridium nanoflower prepared in this example are shown in fig. 1 to 5, respectively. As can be seen from FIGS. 1 to 5, the product obtained in this example has a uniform self-assembled nanoflower structure and uniform size.
Example 2
The self-assembled iridium nanoflower is prepared according to the following steps:
step 1, adding 12mg of iridium trichloride hydrate and 20mg of polyvinylpyrrolidone into 3mL of N-methylpyrrolidone in sequence, uniformly stirring by magnetic force, and performing ultrasonic treatment for 40min to obtain a homogeneous solution.
And 2, quickly adding 2mL of formic acid into the homogeneous solution obtained in the step 1 to obtain a precursor solution.
And 3, transferring the precursor solution obtained in the step 2 to a polytetrafluoroethylene reaction kettle, and carrying out hydrothermal reaction for 7 hours in an oven preheated to 120 ℃.
And 4, after the reaction is finished, keeping the oven sealed, cooling the product to room temperature in the oven, and then centrifugally washing the obtained product for three times at 12000rpm by using acetone, wherein the centrifugal time is 10min each time, so that the self-assembled iridium nanoflower is obtained.
The product obtained in the embodiment is characterized by being in a uniform self-assembled iridium nanoflower structure and being consistent in size.
Example 3
The self-assembled iridium nanoflower is prepared according to the following steps:
step 1, adding 4mg of iridium trichloride hydrate and 10mg of polyvinylpyrrolidone into 9mL of N-methylpyrrolidone in sequence, uniformly stirring by magnetic force, and performing ultrasonic treatment for 40min to obtain a homogeneous solution.
And 2, quickly adding 2mL of formic acid into the homogeneous solution obtained in the step 1 to obtain a precursor solution.
And 3, transferring the precursor solution obtained in the step 2 to a polytetrafluoroethylene reaction kettle, and carrying out hydrothermal reaction for 7 hours in an oven preheated to 90 ℃.
And 4, after the reaction is finished, keeping the oven sealed, cooling the product to room temperature in the oven, and then centrifugally washing the obtained product for three times at 12000rpm by using acetone, wherein the centrifugal time is 10min each time, so that the self-assembled iridium nanoflower is obtained.
The product obtained in the embodiment is characterized by being in a uniform self-assembled iridium nanoflower structure and being consistent in size.
Example 4
The self-assembled iridium nanoflower is prepared according to the following steps:
step 1, adding 20mg of iridium trichloride hydrate and 30mg of polyvinylpyrrolidone into 6mL of N-methylpyrrolidone in sequence, uniformly stirring by magnetic force, and performing ultrasonic treatment for 40min to obtain a homogeneous solution.
And 2, quickly adding 2mL of formic acid into the homogeneous solution obtained in the step 1 to obtain a precursor solution.
And 3, transferring the precursor solution obtained in the step 2 to a polytetrafluoroethylene reaction kettle, and carrying out hydrothermal reaction for 7 hours in an oven preheated to 80 ℃.
And 4, after the reaction is finished, keeping the oven sealed, cooling the product to room temperature in the oven, and then centrifugally washing the obtained product for three times at 12000rpm by using acetone, wherein the centrifugal time is 10min each time, so that the self-assembled iridium nanoflower is obtained.
The product obtained in the embodiment is characterized by being in a uniform self-assembled iridium nanoflower structure and being consistent in size.
Example 5
The self-assembled iridium nanoflower is prepared according to the following steps:
step 1, adding 12mg of iridium trichloride hydrate and 20mg of polyvinylpyrrolidone into 6mL of N-methylpyrrolidone in sequence, uniformly stirring by magnetic force, and performing ultrasonic treatment for 40min to obtain a homogeneous solution.
And 2, quickly adding 1mL of formic acid into the homogeneous solution obtained in the step 1 to obtain a precursor solution.
And 3, transferring the precursor solution obtained in the step 2 to a polytetrafluoroethylene reaction kettle, and carrying out hydrothermal reaction for 7 hours in an oven preheated to 120 ℃.
And 4, after the reaction is finished, keeping the oven sealed, cooling the product to room temperature in the oven, and then centrifugally washing the obtained product for three times at 12000rpm by using acetone, wherein the centrifugal time is 10min each time, so that the self-assembled iridium nanoflower is obtained.
The product obtained in the embodiment is characterized by being in a uniform self-assembled iridium nanoflower structure and being consistent in size.
Example 6
The self-assembled iridium nanoflower is prepared according to the following steps:
step 1, adding 12mg of iridium trichloride hydrate and 20mg of polyvinylpyrrolidone into 3mL of N-methylpyrrolidone in sequence, uniformly stirring by magnetic force, and performing ultrasonic treatment for 40min to obtain a homogeneous solution.
And 2, quickly adding 3mL of formic acid into the homogeneous solution obtained in the step 1 to obtain a precursor solution.
And 3, transferring the precursor solution obtained in the step 2 to a polytetrafluoroethylene reaction kettle, and carrying out hydrothermal reaction for 7 hours in an oven preheated to 110 ℃.
And 4, after the reaction is finished, keeping the oven sealed, cooling the product to room temperature in the oven, and then centrifugally washing the obtained product for three times at 12000rpm by using acetone, wherein the centrifugal time is 10min each time, so that the self-assembled iridium nanoflower is obtained.
The product obtained in the embodiment is characterized by being in a uniform self-assembled iridium nanoflower structure and being consistent in size.
Example 7
The self-assembled iridium nanoflower is prepared according to the following steps:
step 1, adding 12mg of iridium trichloride hydrate and 20mg of polyvinylpyrrolidone into 6mL of N-ethyl pyrrolidone in sequence, uniformly stirring by magnetic force, and performing ultrasonic treatment for 40min to obtain a homogeneous solution.
And 2mL of formic acid is quickly added into the homogeneous solution obtained in the step 1, so as to obtain a precursor solution.
And 3, transferring the precursor solution obtained in the step 2 to a polytetrafluoroethylene reaction kettle, and carrying out hydrothermal reaction for 7 hours in an oven preheated to 100 ℃.
And 4, after the reaction is finished, keeping the oven sealed, cooling the product to room temperature in the oven, and then centrifugally washing the obtained product for three times at 12000rpm by using acetone, wherein the centrifugal time is 10min each time, so that the self-assembled iridium nanoflower is obtained.
The product obtained in the embodiment is characterized by being in a uniform self-assembled iridium nanoflower structure and being consistent in size.
Example 8
The self-assembled iridium nanoflower is prepared according to the following steps:
step 1, adding 12mg of iridium trichloride hydrate and 20mg of polyvinylpyrrolidone into 9mL of N-vinylpyrrolidone in sequence, stirring uniformly by magnetic force, and performing ultrasonic treatment for 40min to obtain a homogeneous solution.
And 2, quickly adding 1mL of formic acid into the homogeneous solution obtained in the step 1 to obtain a precursor solution.
And 3, transferring the precursor solution obtained in the step 2 to a polytetrafluoroethylene reaction kettle, and carrying out hydrothermal reaction for 7 hours in an oven preheated to 100 ℃.
And 4, after the reaction is finished, keeping the oven sealed, cooling the product to room temperature in the oven, and then centrifugally washing the obtained product for three times at 12000rpm by using acetone, wherein the centrifugal time is 10min each time, so that the self-assembled iridium nanoflower is obtained.
The product obtained in the embodiment is characterized by being in a uniform self-assembled iridium nanoflower structure and being consistent in size.
Example 9
The self-assembled iridium nanoflower is prepared according to the following steps:
step 1, adding 16mg of iridium trichloride hydrate and 20mg of polyvinylpyrrolidone into 3mL of N-methylpyrrolidone in sequence, uniformly stirring by magnetic force, and performing ultrasonic treatment for 40min to obtain a homogeneous solution.
And 2, quickly adding 2mL of formic acid into the homogeneous solution obtained in the step 1 to obtain a precursor solution.
And 3, transferring the precursor solution obtained in the step 2 to a polytetrafluoroethylene reaction kettle, and carrying out hydrothermal reaction for 7 hours in an oven preheated to 120 ℃.
And 4, after the reaction is finished, keeping the oven sealed, cooling the product to room temperature in the oven, and then centrifugally washing the obtained product for three times at 12000rpm by using acetone, wherein the centrifugal time is 10min each time, so that the self-assembled iridium nanoflower is obtained.
The product obtained in the embodiment is characterized by being in a uniform self-assembled iridium nanoflower structure and being consistent in size.
Example 10
The self-assembled iridium nanoflower is prepared according to the following steps:
step 1, adding 16mg of iridium trichloride hydrate and 20mg of polyvinylpyrrolidone into 6mL of N-methylpyrrolidone in sequence, uniformly stirring by magnetic force, and performing ultrasonic treatment for 40min to obtain a homogeneous solution.
And 2, quickly adding 4mL of formic acid into the homogeneous solution obtained in the step 1 to obtain a precursor solution.
And 3, transferring the precursor solution obtained in the step 2 to a polytetrafluoroethylene reaction kettle, and carrying out hydrothermal reaction for 7 hours in an oven preheated to 100 ℃.
And 4, after the reaction is finished, keeping the oven sealed, cooling the product to room temperature in the oven, and then centrifugally washing the obtained product for three times at 12000rpm by using acetone, wherein the centrifugal time is 10min each time, so that the self-assembled iridium nanoflower is obtained.
The product obtained in the embodiment is characterized by being in a uniform self-assembled iridium nanoflower structure and being 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 (4)
1. A preparation method of self-assembled iridium nanoflower is characterized by comprising the following steps:
step 1, sequentially adding 4-20 mg of iridium trichloride hydrate and 10-30 mg of polyvinylpyrrolidone into 3-9 mL of organic solvent, uniformly stirring by magnetic force, and then performing ultrasonic treatment for 20-50 min to obtain homogeneous solution;
step 2, quickly adding 1-4 mL of formic acid into the homogeneous solution obtained in the step 1 to obtain a precursor solution;
step 3, transferring the precursor solution obtained in the step 2 to a polytetrafluoroethylene reaction kettle, and carrying out hydrothermal reaction for 7-9 hours in an oven preheated to 80-120 ℃;
and 4, after the reaction is finished, keeping the oven sealed, cooling the product to room temperature in the oven, and then centrifugally washing the product to obtain the self-assembled iridium nanoflower.
2. The method for preparing self-assembled iridium nanoflower according to claim 1, wherein the method comprises the following steps: the solvent is N-methyl pyrrolidone, N-vinyl pyrrolidone or N-ethyl pyrrolidone.
3. The method for preparing self-assembled iridium nanoflower according to claim 1, wherein the method comprises the following steps: the centrifugal washing in step 4 was three times centrifugal washing with acetone at 12000rpm for 10min each.
4. A self-assembled iridium nanoflower prepared by the preparation method of any one of claims 1 to 3.
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| CN114990573A (en) * | 2022-06-06 | 2022-09-02 | 济南大学 | Preparation method of self-assembled two-dimensional Ir metallocene electrocatalyst |
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| CN114990573A (en) * | 2022-06-06 | 2022-09-02 | 济南大学 | Preparation method of self-assembled two-dimensional Ir metallocene electrocatalyst |
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