CN113275555B - Metal nano frame with array structure and preparation method and application thereof - Google Patents
Metal nano frame with array structure and preparation method and application thereof Download PDFInfo
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- CN113275555B CN113275555B CN202110397677.3A CN202110397677A CN113275555B CN 113275555 B CN113275555 B CN 113275555B CN 202110397677 A CN202110397677 A CN 202110397677A CN 113275555 B CN113275555 B CN 113275555B
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a metal nanometer frame with an array structure, which comprises a gold nanometer bipyramid and an outer layer frame body, wherein the outer layer frame body comprises silver atoms and gold atoms, and the array structure is uniformly distributed on the outer layer frame body. The invention also discloses a preparation method of the metal nanometer frame with the array structure, which comprises the following steps: adding the metal nano-frame solution into a cetylpyridinium chloride solution, and then adding a chloropalladate solution or a chloroplatinic acid solution and an ascorbic acid solution; and shaking the obtained solution uniformly, and reacting in an oven at the temperature of 30-90 ℃ to obtain the metal nano frame with the array structure. The invention also discloses application of the metal nanometer frame with the array structure in photoelectrocatalysis. The metal nano frame structure of the array structure prepared by the invention has high purity and high repeatability, and has potential application in the fields of photoelectrocatalysis, sensing and photochemistry; the preparation conditions are simple, mild and strong in operability.
Description
Technical Field
The invention belongs to a metal nano frame and a preparation method and application thereof, and particularly relates to a metal nano frame with an array structure and a preparation method and application thereof.
Background
Due to the unique optical and electric field characteristics of the noble metal nanoparticles, the noble metal nanoparticles have wide application values in the fields of catalysis, electronics, photonics and the like. In recent years, many research results show that the physicochemical properties of the nanoparticles are related to the size, shape and surface atomic species of the nanoparticles, so that the purpose of adjusting the properties of the nanoparticles can be achieved by adjusting the morphology size of the nanoparticles and the surface modification species. However, the noble metals are expensive, and the elemental catalytic metals (platinum, palladium, etc.) have weak toxicity resistance and low stability. To overcome these limitations, improvements in catalytic activity and catalytic metal utilization need to be achieved by controlling the structure and size of the catalyst. In recent years, researchers have developed strategies to increase the catalytic activity of noble metal nanocrystals and reduce their loading in catalysts. Since the edge and corner positions of the catalyst usually have higher activity, the synthesis of porous structures, tree structures, hollow structures, etc. is an effective strategy for maximizing the utilization of edge catalytic metals, which is reported in many literatures (Part Syst char, 2018,35, 1800258; Nanoscale,2017,9, 18881-.
However, the synthesis of these alloy structures is complex. In order to enhance the stability of the catalyst, a large number of complex processes are used, and a long time is required for structure evolution, and the processing means is complex, which greatly restricts the large-scale application of the unique nano-structure (such as Science,2014,343, 1339-. In addition, in the frame structure, the advantages of the plasmonic metal (such as gold) are not fully utilized, so that the competitiveness of the structure in the field of photocatalysis is restricted.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention aims to provide the metal nano frame with the array structure and the plasmon resonance performance and high purity, the invention also aims to provide the preparation method of the metal nano frame with the array structure, which is simple in preparation, mild in condition and strong in operability, and the invention also aims to provide the application of the metal nano frame with the array structure in photoelectrocatalysis.
The technical scheme is as follows: the metal nanometer frame with the array structure comprises gold nanometer bipyramids and an outer layer frame body, wherein the outer layer frame body comprises silver atoms and gold atoms, and the array structure is uniformly distributed on the outer layer frame body.
Further, the array structure is a palladium array or a platinum array, preferably a palladium array. The single length of the array structure is 2-5 nm. When the single length of the array structure is less than 2nm, the catalytic performance is weaker; the single length of the array structure is larger than 5nm, the array growth is uneven, and the outer frame body is easy to deform.
Further, outer framework includes point portion one, point portion two and connecting rod, and point portion one, point portion two are regular pentagonal pyramid and set up about the connecting rod symmetry, and the connecting rod links to each other with point portion one, point portion two respectively. The width of the connecting rod is 2-6 nm. When the width of the connecting rod is less than 2nm, the frame body is too thin, and the stability is not high; when the width of the connecting rod is larger than 6nm, the influence on the plasmon effect of the structure is large.
The preparation method of the metal nanometer frame with the array structure comprises the following steps:
adding a metal nano-frame solution into a cetylpyridinium chloride solution, and then adding a chloropalladate solution or a chloroplatinic acid solution and an ascorbic acid solution;
and step two, shaking the solution obtained in the step one evenly, and reacting in an oven at the temperature of 30-90 ℃ to obtain the metal nanometer frame with the array structure.
Further, in the first step, the concentration of the surfactant cetyl pyridinium chloride is 1-20 mmol/L. The cetyl pyridinium chloride has the functions of a blocking agent and a soft template, and can realize an array structure deposited at uniform intervals. Too low or too high a concentration of cetylpyridinium results in uneven growth of the array. The concentration of the palladium chloride acid is 1-5 mmol/L, and the concentration of the ascorbic acid is 10-30 mmol/L.
Further, in the second step, the reaction time is 0.5-17 h.
The metal nanometer frame with the array structure is applied to photoelectrocatalysis.
The preparation principle is as follows: the metal precursor and the silver atoms on the surface of the metal nanometer frame are subjected to displacement reaction under the action of ascorbic acid and cetylpyridinium chloride; since the cetylpyridinium chloride acts as a capping agent, palladium atoms are selectively deposited on the metal nano-frame to form a palladium array structure.
Has the advantages that: compared with the prior art, the invention has the following remarkable characteristics:
1. the prepared metal nanometer frame structure of the array structure has high purity and high repeatability, and has potential application in the fields of photoelectrocatalysis, sensing and photochemistry;
2. the preparation conditions of the metal nanometer frame structure of the array structure are simple, mild and strong in operability;
3. the prepared metal nanometer frame structure of the array structure has abundant catalytic active sites, and the utilization rate of catalytic metal is high;
4. the prepared metal nanometer frame structure of the array structure has better plasmon effect.
Drawings
FIG. 1 is a schematic diagram of the preparation of the present invention;
FIG. 2 is a schematic representation of a metal nanobox of the present invention;
FIG. 3 is a transmission electron micrograph of a product obtained in example 1 of the present invention;
FIG. 4 is a transmission electron microscope image of a first tip 21 of a product obtained in example 1 of the present invention;
FIG. 5 is an energy spectrum of the product obtained in example 1 of the present invention;
FIG. 6 is a graph showing a UV-VIS absorption spectrum of a product obtained in example 1 of the present invention;
FIG. 7 is a graph comparing the mass activity of the product obtained in example 1 of the present invention and commercial palladium on carbon in an alkaline ethanol electrocatalytic reaction.
Detailed Description
The raw materials and the apparatus in the following examples were all purchased and used directly.
The purity of the metal nano frame is 99 percent, and the absorbance is 2. The preparation method of the metal nano frame solution comprises the following steps:
(1) adding 1mL of gold nano bipyramid 1 solution into 10mL of 0.08mol/L hexadecyl trimethyl ammonium chloride solution, and adding 125 mu L of 0.1mol/L ascorbic acid solution and 250 mu L of 0.01mol/L AgNO solution3Uniformly shaking the mixed solution, putting the mixed solution into a 60 ℃ oven, and reacting for 5 hours to obtain silver nanorods;
(2) centrifuging the silver nanorods obtained in the step (1) at 5000rpm for 10min, then dispersing the silver nanorods into 4mL of hexadecyl trimethyl ammonium bromide solution with the concentration of 0.05mol/L, respectively adding 1mL of ascorbic acid solution with the concentration of 0.1mol/L and 1mL of NaOH solution with the concentration of 0.2mol/L, slowly dropwise adding 1.6mL of chloropalladate reaction solution with the concentration of 0.1mmol/L at room temperature according to the speed of 20 mu L/min, and reacting for 2 h;
(3) centrifuging the sample obtained in the step (2) at 6000rpm for 10min, dispersing the sample into 3mL of hexadecyl trimethyl ammonium bromide solution and 0.005mol/L of hexadecyl trimethyl ammonium bromide solution, respectively adding 2mL of hydrogen peroxide solution and 5mol/L of hydrogen peroxide solution and 0.1mL of ammonia water solution and 14mol/L of ammonia water solution, and reacting at room temperature for 12h to obtain a metal nano frame;
(4) and (4) dispersing the metal nano frame prepared in the step (3) into water to obtain a metal nano frame solution.
Example 1
Referring to fig. 1, a method for preparing a metal nano frame of an array structure 3 includes the following steps:
(a) adding 1mL of metal nano-frame solution into 10mL of 10mmol/L surfactant cetylpyridinium chloride solution, and then adding 90 mu L of 1mmol/L chloropalladate solution and 90 mu L of 10mmol/L ascorbic acid solution;
(b) and d, shaking the solution obtained in the step a uniformly, and reacting in a 65 ℃ oven for 0.5h to obtain the metal nano frame with the palladium array structure 3.
Referring to fig. 2, the metal nano frame manufactured in this embodiment includes a gold nano bipyramid 1 and an outer frame 2, the outer frame 2 is made of a gold-silver alloy composed of silver atoms and gold atoms, and palladium array structures 3 are uniformly distributed on the outer frame 2. The outer frame body 2 comprises a first tip portion 21, a second tip portion 22 and a connecting rod 23, wherein the first tip portion 21 and the second tip portion 22 are regular pentagonal pyramids and are symmetrically arranged relative to the connecting rod 23, and the connecting rod 23 is respectively connected with the first tip portion 21 and the second tip portion 22.
The metal nano frame prepared in this embodiment is subjected to morphology analysis, as shown in fig. 3 to 5, which are a transmission electron microscope image, a high-resolution transmission electron microscope image and an energy spectrum image of the palladium array structure 3 based on the metal nano frame, respectively. As can be seen from fig. 3 to 5, the prepared product is a nano-frame structure supported by the gold nano-bipyramid 1, the width of the connecting rod 23 is 2nm, and the single length of the palladium array structure 3 is 2 nm. The palladium array structure 3 is mainly grown on the surface of the outer layer frame body 2, and a very small amount of palladium array structure is likely to grow on the surface of the gold nanometer bipyramid 1.
Fig. 4 is a comparison graph of absorption spectra of the metal nano frame and the original metal nano frame manufactured in this embodiment, after the surface is covered with palladium, the plasmon resonance performance of the entire structure preserves forty percent of the plasmon resonance performance of the metal nano frame, and the peak position is red-shifted, so that the metal nano frame of the array structure 3 has both plasmon resonance performance and catalytic performance.
Example 2
A preparation method of a metal nanometer frame of an array structure 3 comprises the following steps:
(a) adding 1mL of metal nano-frame solution into 10mL of 1mmol/L surfactant cetylpyridinium chloride solution, and then adding 90 mu L of 5mmol/L chloroplatinic acid solution and 90 mu L of 30mmol/L ascorbic acid solution;
(b) and d, shaking the solution obtained in the step a uniformly, and reacting for 17 hours in a drying oven at the temperature of 30 ℃ to obtain the metal nanometer frame with the platinum array structure 3.
The metal nano frame manufactured in the embodiment includes a gold nano bipyramid 1 and an outer layer frame body 2, the outer layer frame body 2 is made of gold-silver alloy, and a single platinum array structure 3 with the length of 5nm is uniformly distributed on the outer layer frame body 2. The outer frame body 2 comprises a first tip portion 21, a second tip portion 22 and a connecting rod 23, wherein the first tip portion 21 and the second tip portion 22 are regular pentagonal pyramids and are symmetrically arranged relative to the connecting rod 23, and the connecting rod 23 is respectively connected with the first tip portion 21 and the second tip portion 22. The width of the tie bar 23 is 6 nm.
Example 3
A preparation method of a metal nanometer frame of an array structure 3 comprises the following steps:
(a) adding 1mL of metal nano-frame solution into 10mL of 20mmol/L surfactant cetylpyridinium chloride solution, and then adding 90 mu L of 3mmol/L chloropalladate solution and 90 mu L of 20mmol/L ascorbic acid solution;
(b) and d, shaking the solution obtained in the step a uniformly, and reacting in a drying oven at 90 ℃ for 9h to obtain the metal nano frame with the palladium array structure 3.
The metal nano frame manufactured in the embodiment comprises a gold nano bipyramid 1 and an outer layer frame body 2, wherein the outer layer frame body 2 is made of gold-silver alloy, and a single palladium array structure 3 with the length of 3nm is uniformly distributed on the outer layer frame body 2. The outer frame body 2 comprises a first tip portion 21, a second tip portion 22 and a connecting rod 23, wherein the first tip portion 21 and the second tip portion 22 are regular pentagonal pyramids and are symmetrically arranged relative to the connecting rod 23, and the connecting rod 23 is respectively connected with the first tip portion 21 and the second tip portion 22. The width of the tie bar 23 is 3 nm.
Example 4
A preparation method of a metal nanometer frame of an array structure 3 comprises the following steps:
(a) adding 1mL of metal nano-frame solution into 10mL of 5mmol/L surfactant cetylpyridinium chloride solution, and then adding 90 mu L of 2mmol/L chloroplatinic acid solution and 90 mu L of 15mmol/L ascorbic acid solution;
(b) and d, shaking the solution obtained in the step a uniformly, and reacting for 4 hours in a baking oven at the temperature of 45 ℃ to obtain the metal nanometer frame with the platinum array structure 3.
The metal nano frame manufactured in the embodiment includes a gold nano bipyramid 1 and an outer layer frame body 2, the outer layer frame body 2 is made of gold-silver alloy, and a single platinum array structure 3 with a length of 4nm is uniformly distributed on the outer layer frame body 2. The outer frame body 2 comprises a first tip portion 21, a second tip portion 22 and a connecting rod 23, wherein the first tip portion 21 and the second tip portion 22 are regular pentagonal pyramids and are symmetrically arranged relative to the connecting rod 23, and the connecting rod 23 is respectively connected with the first tip portion 21 and the second tip portion 22. The width of the tie bar 23 is 4 nm.
Example 5
A preparation method of a metal nanometer frame of an array structure 3 comprises the following steps:
(a) adding 1mL of metal nano-frame solution into 10mL of 15mmol/L surfactant cetylpyridinium chloride solution, and then adding 90 mu L of 4mmol/L chloropalladite solution and 90 mu L of 25mmol/L ascorbic acid solution;
(b) and d, shaking the solution obtained in the step a uniformly, and reacting for 13 hours in a 75 ℃ oven to obtain the metal nanometer frame with the palladium array structure 3.
The metal nano frame manufactured in the embodiment comprises a gold nano bipyramid 1 and an outer layer frame body 2, wherein the outer layer frame body 2 is made of gold-silver alloy, and a single palladium array structure 3 with the length of 3nm is uniformly distributed on the outer layer frame body 2. The outer frame body 2 comprises a first tip portion 21, a second tip portion 22 and a connecting rod 23, wherein the first tip portion 21 and the second tip portion 22 are regular pentagonal pyramids and are symmetrically arranged relative to the connecting rod 23, and the connecting rod 23 is respectively connected with the first tip portion 21 and the second tip portion 22. The width of the tie bar 23 is 4 nm.
Example 6
The application of the gold nano-frame structure of the array structure in the embodiment 1 to the ethanol oxidation reaction in the potassium hydroxide solution comprises the following steps:
(a) mixing the catalyst with a 0.5 wt% membrane solution, wherein the mass ratio of N, N-dimethylformamide to carbon black is 950: 1, and dropwise adding the mixed solution on a glassy carbon electrode to test the catalytic performance, wherein the volume ratio of the membrane solution, the mixed solution of N, N-dimethylformamide-carbon black, the catalyst and water is 1: 1: 5: 20;
(b) electrocatalysis experiments are carried out in a mixed solution of 0.5mol/L potassium hydroxide and 0.5mol/L ethanol.
Electrocatalytic efficiency as shown in fig. 7, the area activity of the gold nano-frame structure (25.9942 a/m)2) Much higher than commercial palladium on carbon (6.3926A/m)2) About 4 times that of commercial palladium on carbon.
Comparative example 1
The remaining steps of this example are the same as example 1, except that: replacement of the surfactant cetylpyridinium chloride with cetyltrimethylammonium bromide failed to achieve a uniformly spaced-apart growth of the array structure 3.
Claims (9)
1. A metal nanometer frame of an array structure is characterized in that: the gold nanometer double-cone array structure comprises a gold nanometer double-cone (1) and an outer layer frame body (2), wherein the outer layer frame body (2) comprises silver atoms and gold atoms, and array structures (3) are uniformly distributed on the outer layer frame body (2); the outer frame body (2) comprises a first tip part (21), a second tip part (22) and a connecting rod (23), wherein the first tip part (21) and the second tip part (22) are regular pentagonal pyramids and are symmetrically arranged relative to the connecting rod (23), and the connecting rod (23) is connected with the first tip part (21) and the second tip part (22) respectively.
2. The metal nanobrame of claim 1, wherein: the array structure (3) is a palladium array or a platinum array.
3. The metal nanobrame of claim 1, wherein: the single length of the array structure (3) is 2-5 nm.
4. The metal nanobrame of claim 1, wherein: the width of the connecting rod (23) is 2-6 nm.
5. The method for preparing the metal nano frame with the array structure according to any one of claims 1 to 4, comprising the following steps:
adding a metal nano-frame solution into a cetylpyridinium chloride solution, and then adding a chloropalladate solution or a chloroplatinic acid solution and an ascorbic acid solution;
step two, shaking the solution obtained in the step one evenly, and reacting in an oven at the temperature of 30-90 ℃ to obtain a metal nano frame of an array structure (3);
the preparation method of the metal nano frame solution comprises the following steps:
(1) adding 1mL of gold nano bipyramid (1) solution into 10mL of 0.08mol/L hexadecyl trimethyl ammonium chloride solution, and adding 125 mu L of 0.1mol/L ascorbic acid solution and 250 mu L of 0.01mol/L AgNO solution3Uniformly shaking the mixed solution, putting the mixed solution into a 60 ℃ oven, and reacting for 5 hours to obtain silver nanorods;
(2) centrifuging the silver nanorods obtained in the step (1) at 5000rpm for 10min, then dispersing the silver nanorods into 4mL of hexadecyl trimethyl ammonium bromide solution with the concentration of 0.05mol/L, respectively adding 1mL of ascorbic acid solution with the concentration of 0.1mol/L and 1mL of NaOH solution with the concentration of 0.2mol/L, slowly dropwise adding 1.6mL of chloropalladate reaction solution with the concentration of 0.1mmol/L at room temperature according to the speed of 20 mu L/min, and reacting for 2 h;
(3) centrifuging the sample obtained in the step (2) at 6000rpm for 10min, dispersing the sample into 3mL of hexadecyl trimethyl ammonium bromide solution and 0.005mol/L of hexadecyl trimethyl ammonium bromide solution, respectively adding 2mL of hydrogen peroxide solution and 5mol/L of hydrogen peroxide solution and 0.1mL of ammonia water solution and 14mol/L of ammonia water solution, and reacting at room temperature for 12h to obtain a metal nano frame;
(4) and (4) dispersing the metal nano frame prepared in the step (3) into water to obtain a metal nano frame solution.
6. The method for preparing a metal nano frame of an array structure according to claim 5, wherein: in the first step, the concentration of the cetylpyridinium chloride is 1-20 mmol/L.
7. The method for preparing a metal nano frame of an array structure according to claim 5, wherein: in the first step, the concentration of the palladium chloride acid is 1-5 mmol/L, and the concentration of the ascorbic acid is 10-30 mmol/L.
8. The method for preparing a metal nano frame of an array structure according to claim 5, wherein: in the second step, the reaction time is 0.5-17 h.
9. The use of the metal nano-frame of an array structure according to any one of claims 1 to 4 in photoelectrocatalysis.
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| US11045874B2 (en) * | 2015-06-08 | 2021-06-29 | The University Of Chicago | Bipyramid-templated synthesis of monodisperse noble metal nanocrystals |
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| WO2014005147A2 (en) * | 2012-06-29 | 2014-01-03 | Northeastern University | Three-dimensional crystalline, homogenous, and hybrid nanostructures fabricated by electric field directed assembly of nanoelements |
| CN110137317A (en) * | 2019-04-29 | 2019-08-16 | 南京航空航天大学 | A kind of novel electroluminescent device and preparation method thereof |
| CN111647871A (en) * | 2019-10-17 | 2020-09-11 | 山东省科学院新材料研究所 | Super-assembly controllable growth method of metal nano grain boundary surface carbon-based material |
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