CN111112640A - Method for regulating and controlling Yolk-shell nano structure - Google Patents

Method for regulating and controlling Yolk-shell nano structure Download PDF

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CN111112640A
CN111112640A CN202010127005.6A CN202010127005A CN111112640A CN 111112640 A CN111112640 A CN 111112640A CN 202010127005 A CN202010127005 A CN 202010127005A CN 111112640 A CN111112640 A CN 111112640A
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solution
yolk
shell
agpt
nanorod
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邓瑶瑶
柏寄荣
向梅
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Changzhou Institute 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
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
    • 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
    • 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
    • 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

Abstract

The invention discloses a method for regulating a Yolk-shell nano structure, belonging to the technical field of new materials. According to the invention, through combining a template method and a displacement reaction, different types of surfactants are tried to be added, and the Yolk-shell-shaped Au @ AgPt nanorod with different structures is prepared by a simple method, so that a new opportunity is provided for reasonably designing and synthesizing the Yolk-shell structure. In addition, the Yolk-shell-shaped Au @ AgPt nanorod with different structures prepared by the method can be applied to different fields, such as a nano reactor, an electrocatalytic oxygen reduction reaction, a nano medicine field and the like, and the application of the Yolk-shell-shaped structure is widened.

Description

Method for regulating and controlling Yolk-shell nano structure
Technical Field
The invention relates to a method for regulating a Yolk-shell nano structure, belonging to the technical field of new materials.
Background
The Yolk-shell-like nano structure is a typical heterogeneous structure, and has large specific surface area and internal space. In recent years, the yolk-shell-like nano-structures attract the wide attention of people, not only because the yolk-shell-like nano-structures are in the frontier of material science, but also the yolk-shell-like nano-structures have strong application potential in the fields of catalysis, nano-reactors, energy storage, biomedicine and the like. Due to the unique morphological characteristics of the Yolk-shell, the Yolk-shell has the advantages of low density, large surface area, good bearing capacity and the like, and the structure not only successfully integrates various functional materials into one system, but also endows the heterogeneous nano-material with good performance in specific application. The existence of the hollow cavity enables the nano core to be fully exposed, and meanwhile, the nano shell plays a role in protection, so that the distance dependence of the core is kept. In addition, the porous structure of the shell can provide a diffusion path for guest molecules, and the reaction efficiency is improved. In addition, the yolk-shell material with the porous shell can be used in the field of electrocatalysis, and the material with the smooth shell can be used in the field of biomedicine. In short, yolk-shell like nanostructures are a specific one of the material structures that can be tailored for different applications.
At present, there are three main methods for synthesizing yolk-shell-like nanostructures: (1) a hard template method; (2) soft template method; (3) self-templated method. The hard template method is the most common strategy for synthesizing the yolk-shell-shaped nano structure and has the characteristics of simplicity, effectiveness and intuition. In a typical hard template synthesis process, a rigid material is coated on a nano core to serve as a sacrificial template, then an outer layer material is coated, and then the sacrificial template is removed. The soft template method is to use vesicles formed by self-assembly of amphiphilic molecules such as a surfactant and a block copolymer as a soft template for preparing the yolk-shell-shaped nano structure. The nanomaterial synthesized by the soft template method is not uniform well compared to the hard template method, but the vesicle template removal process is unnecessary in most of the soft template synthesis methods. The self-templating approach refers to the preparation of yolk-shell like nanostructures without the use of additional sacrificial templates. Several self-templating methods have been developed so far, such as displacement reactions, kirkendall reactions, oswald ripening and selective removal. The main disadvantage of these self-templating methods is that they usually require specific combinations. The above methods can be used either alone or in combination in order to rapidly and reproducibly obtain yolk-shell like nanostructures with controlled architecture and desirable properties.
The metathesis reaction has been considered to be self-templatedAn effective method for synthesizing a yolk-shell-shaped nano structure by a plate method, in particular to a yolk-shell-shaped nano structure of a noble metal shell. The driving force for this reaction arises from the potential difference between the two metals, one of which acts as a reducing agent (anode) and the other of which acts as an oxidizing agent (cathode). Generally, a layer of anode metal is coated on the surface of the nano-core; when the cathode metal ions are added, the anode metal is dissolved, and the cathode metal is electroplated on the outer surface of the anode template; the shape and internal pore size of the final yolk-shell-like nanostructure are determined by the anode metal template. For example, Xia et al report Ag on HAuCl4And synthesizing the Au/Ag @ Au/Ag yolk-shell-shaped nano structure through a displacement reaction. In addition, the surface of the yolk-shell structure synthesized by the method is a smooth structure, and is not beneficial to the application in the field of electrocatalysis.
Disclosure of Invention
Based on the background, the invention provides a method for preparing different Yolk-shell nano-structures, and attempts are made to synthesize Yolk-shell-shaped Au @ AgPt nano-rods with different structures by regulating the types of surfactants.
The first purpose of the invention is to provide a method for preparing Yolk-shell-shaped Au @ AgPt nanorods with different structures, which comprises the following steps:
(1) synthesizing an Au nanorod;
(2) taking the Au nanorod prepared in the step (1) as a template, coating a layer of Ag on the surface of the Au nanorod, and synthesizing the Au @ Ag nanorod;
(3) and (3) taking the Au @ Ag nanorod prepared in the step (2) as a template, adding a surfactant solution, and synthesizing the yolk-shell Au @ AgPt nanorod through a displacement reaction.
The synthesis steps are schematically shown in FIG. 1.
In one embodiment of the present invention, the specific steps of step (1) of the preparation method are as follows:
(1) and (3) synthesizing an Au nanorod:
preparing a seed solution: adding HAuCl4The solution was added to a cetyltrimethylammonium bromide (CTAB) solution to which was subsequently added freshly prepared NaBH4The solution is vigorously shaken to obtain a seed solutionStanding the solution at room temperature for 1.5-2.5 h for use;
preparing a growth solution: dissolving CTAB and NaOL, and adding AgNO3Standing the solution for 10-20 min; followed by HAuCl addition4Stirring the solution for 2-4 h, and then changing the color of the solution from orange yellow to colorless; adding HCl solution, and stirring for 10-20 min; finally adding ascorbic acid solution and stirring vigorously to obtain a growth solution;
adding a proper amount of seed solution into the growth solution, inverting, mixing, standing overnight at room temperature, purifying the Au nanorods by a centrifugal method, washing with high-purity water for multiple times to remove redundant surfactant, and dispersing the obtained Au nanorods in the high-purity water for later use.
In one embodiment of the present invention, the specific steps of step (2) of the preparation method are as follows:
(2) synthesizing Au @ Ag nanorods:
first, a prepared polyvinylpyrrolidone (PVP) solution and a CTAB solution were uniformly mixed in an oil bath pan at 60 ℃. Then adding the Au nano rod solution and AgNO prepared in the step (1)3And stirring the solution, ascorbic acid solution and NaOH solution at the temperature for 30min to react to obtain the Au @ Ag nanorod. The material was washed with ethanol and high purity water several times, and the resulting product was dispersed in 4mL of high purity water for use.
In one embodiment of the present invention, the specific steps of step (3) of the preparation method are as follows:
(3) synthesizing a Yolk-shell-shaped Au @ AgPt nanorod:
uniformly mixing the Au @ AgNRs solution prepared in the step (2) with a surfactant solution and an ascorbic acid solution, and adding H into the mixture2PtCl4The solution is stirred and reacted for a period of time at the temperature of 55-65 ℃ to obtain Au @ AgPt nano-rods, and finally the Au @ AgPt nano-rods and NH are added3·H2And O is stirred at room temperature overnight to obtain a final product of yolk-shell-shaped Au @ AgPt nano rod.
In one embodiment of the present invention, the surfactant in step (3) is any one of CTAB, F127 and PVP.
The second purpose of the invention is to provide the Yolk-shell-shaped Au @ AgPt nano rod with different structures prepared by the preparation method.
The third purpose of the invention is to provide a nano-reactor, which comprises the yolk-shell-shaped Au @ AgPt nano-rod, wherein the surfactant of the yolk-shell-shaped Au @ AgPt nano-rod is regulated and controlled to be CTAB, and the nano-shell on the surface of the yolk-shell-shaped Au @ AgPt nano-rod prepared is of a porous structure, and the internal cavity is obvious.
The fourth purpose of the invention is to provide the application of the yolk-shell-shaped Au @ AgPt nanorod in the electrocatalytic oxidation-reduction reaction, the surfactant of the yolk-shell-shaped Au @ AgPt nanorod is regulated to be F127, and the nanoshell of the yolk-shell-shaped Au @ AgPt nanorod prepared is of a porous structure and the thickness of the nanoshell on the surface is thicker.
The fifth purpose of the invention is to provide the application of the yolk-shell-shaped Au @ AgPt nanorod in the field of nano-medicines, the surfactant of the yolk-shell-shaped Au @ AgPt nanorod is regulated to be PVP, and the surface of the nanoshell of the yolk-shell-shaped Au @ AgPt nanorod prepared is of a smooth compact structure.
The invention has the beneficial effects that:
(1) the invention provides a method for preparing different Yolk-shell nano structures, which prepares Yolk-shell-shaped Au @ AgPt nano rods with different structures by combining a template method and a displacement reaction, trying to add different types of surfactants and a simple method, and provides a new opportunity for reasonably designing and synthesizing the Yolk-shell structure.
(2) The Yolk-shell-shaped Au @ AgPt nanorod with different structures is prepared by the same preparation method only by replacing the surfactant type, and can be applied to different fields, such as a nano-reactor, an electrocatalytic oxygen reduction reaction, the nano-medicine field and the like.
Drawings
FIG. 1 is a schematic diagram of the synthesis of Yolk-shell Au @ AgPt NRs.
FIG. 2 is a topographical view of AuNRs prepared in example 1; wherein (a) a TEM image of AuNRs and (b) an HRTEM image of a single AuNRs.
FIG. 3 is a topographical view of Au @ AgNRs prepared in example 1; wherein (a) is a TEM image of Au @ AgNRs, and (b) is an HRTEM image of Au @ AgNRs.
FIG. 4 is a topographical map of the Yolk-shell-like Au @ AgPtNRs prepared in example 1; wherein (a) is a TEM image of Au @ AgPtNRs, and (b) is an HRTEM image of Au @ AgPtNRs.
FIG. 5 is a topographical map of the Yolk-shell-like Au @ AgPtNRs prepared in example 2; wherein (a) is a TEM image of Au @ AgPtNRs, and (b) is an HRTEM image of Au @ AgPtNRs.
FIG. 6 is a topographical map of the Yolk-shell-like Au @ AgPtNRs prepared in example 3; wherein (a) is a TEM image of Au @ AgPtNRs, and (b) is an HRTEM image of Au @ AgPtNRs.
Detailed Description
The invention will now be further illustrated by reference to specific examples, which are intended to be illustrative only and not to limit the scope of the invention.
Example 1
(1) Synthesizing Au nanorods Au nanorodes, which is recorded as AuNRs:
preparing a seed solution: adding HAuCl4The solution (5mL, 0.5mM) was added to a cetyltrimethylammonium bromide (CTAB) solution (5mL, 0.2M) to which was subsequently added freshly prepared NaBH4The solution (0.60mL, 0.01M) was shaken vigorously, and the resulting seed solution was allowed to stand at room temperature for 2 hours before use.
Preparing a growth solution: CTAB (7g) and NaOL (1.234g) were dissolved in 250mL of warm water (40-60 ℃ C.), and AgNO was added3The solution (18mL, 4mM) was left for 15 min; followed by HAuCl addition4The solution (250mL, 1mM) is stirred for about 90min, and the color of the solution changes from orange yellow to colorless; then adding HCl solution (2.1mL), and stirring for 15 min; finally, ascorbic acid solution (1.25mL, 64mM) was added and vigorously stirred for 30s to obtain a growth solution.
0.8mL of the seed solution was added to the growth solution, mixed by inversion for 10s, and then allowed to stand at room temperature overnight. Purifying Au nano-rods (8000r/20min) by a centrifugal method, pouring out supernatant, washing the lower-layer precipitate for multiple times by high-purity water to remove redundant surfactant, and dispersing the obtained AuNRs in the high-purity water for later use.
In this system, AuNRs act as the central nucleus of yolk-shell, determining the final morphology of the product. Fig. 2 is a morphology diagram of synthesized AuNRs, and it can be seen from fig. 2 that AuNRs prepared by the method of the present invention have uniform morphology and size and high yield, and the diameter and length of AuNRs are about 20nm and 82nm, respectively.
(2) Synthesizing Au @ Ag nanorod Au @ Ag nanorods, which is recorded as Au @ AgNRs:
first, a prepared polyvinylpyrrolidone (PVP) solution (10 wt%, 8mL) and a CTAB solution (0.2M, 8mL) were mixed well in an oil bath at 60 ℃. Followed by addition of Au NRs solution (1mM, 4mL) prepared in step (1), AgNO3The solution (0.05M, 540. mu.L), ascorbic acid solution (1M, 1.2mL) and NaOH solution (1M, 2.4mL) were stirred at that temperature for 30min to obtain Au @ Ag nanorods. The material was washed 3 times with ethanol and high purity water, and the resulting product was dispersed in 4mL of high purity water for use.
FIG. 3 is a morphology chart of Au @ AgNRs prepared in example 1, from which it can be seen that the surface of Au nanorods are all successfully wrapped with a layer of Ag nanoshell, and the Au @ AgNRs have a diameter of about 46nm and a length of about 108 nm.
(3) Synthesis of Yolk-shell-like Au @ AgPt nanorods Au @ AgPtnanorudes, noted Au @ AgPtNRs:
CTAB was chosen as a surfactant for the synthesis of Au @ AgPtNRs:
5mL of H was added to the round bottom flask2O, followed by addition of Au @ AgNRs solution (1mL) prepared in step (2), CTAB solution (0.1M, 0.5mL), ascorbic acid solution (0.1M, 0.5mL), mixing the above solutions well and adding H2PtCl4The solution (10mM, 0.2mL) is stirred for another 16min at 60 ℃ to obtain the Au @ AgPt nanorod. Finally, Au @ AgPt nanorod and NH3·H2O was stirred at room temperature overnight to give the final product yolk-shell like Au @ AgPtNRs as shown in figure 4.
As can be seen from fig. 4: because the nano shell on the surface is a porous structure, the internal cavity is obvious. The yolk-shell-shaped Au @ AgPtNRs prepared in the embodiment can be used for a nano reactor.
Example 2
(1) To (2): same as steps (1) to (2) in the examples;
(3) synthesis of Yolk-shell-like Au @ AgPt nanorods Au @ AgPtnanorudes, noted Au @ AgPtNRs: au @ AgPt nanorods were synthesized by selecting F127 as a surfactant:
0.15mL of H was added to the round bottom flask2PtCl6Then HCl solution (6.0M, 30. mu.L), F127(10mg), H were added2And O (0.8mL), adding the Au @ Ag nanorod solution (2mL) synthesized in the step (2) and ascorbic acid (0.1M, 0.5mL) after F127 is completely dissolved, and then carrying out ultrasonic treatment for 2h to obtain the Au @ AgPt nanorod. Finally, Au @ AgPt nanorod and NH3·H2O was stirred at room temperature overnight to give the final product Au @ AgPt NRs as shown in figure 5.
As can be seen from fig. 5: the surfactant synthesized nanoshell is also porous in structure, but the thickness of the surface nanoshell is relatively thick. The product yolk-shell-shaped Au @ AgPtNRs prepared in the embodiment can be used in an electrocatalytic oxygen reduction reaction.
Example 3
(1) To (2): same as steps (1) to (2) in the examples;
(3) synthesis of Yolk-shell-like Au @ AgPt nanorods Au @ AgPtnanorudes, noted Au @ AgPtNRs:
PVP was chosen as the surfactant for the synthesis of Au @ AgPt nanorods:
20mL of H was added to the round bottom flask2O, followed by addition of HCl solution (0.1M, 1.32mL), PVP solution (1M, 2mL) and Au @ Ag nanorod solution (4mL) synthesized in step (2), and the above mixed solution was stirred at 45 ℃ for 5 min. Then adding K2PtCl4The solution (20mM, 8mL) is stirred for 30min to obtain the Au @ AgPt nanorod. Finally, Au @ AgPt nanorod and NH3·H2O was stirred at room temperature overnight to give the final product yolk-shell like Au @ AgPtNRs as shown in figure 6.
As can be seen from fig. 6: the nanoshell is relatively smooth under the action of the surfactant. The material yolk-shell-shaped Au @ AgPtNRs prepared in the embodiment can be used in the field of nano medicine.
According to the experimental results, the type of the surfactant seriously influences the structure of the AgPt nanoshell on the surface, and when CTAB and F127 are selected as the surfactant, a porous structure is formed on the surface; when PVP is chosen as the surfactant, the surface is a smooth, dense structure, and the reason for this may be related to the structure and properties of the surfactant.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (9)

1. A method for regulating and controlling a Yolk-shell-shaped Au @ AgPt nanorod structure is characterized by comprising the following steps:
(1) synthesizing an Au nanorod;
(2) taking the Au nanorod prepared in the step (1) as a template, coating a layer of Ag on the surface of the Au nanorod, and synthesizing the Au @ Ag nanorod;
(3) and (3) taking the Au @ Ag nanorod prepared in the step (2) as a template, adding different surfactant solutions, and regulating and controlling the structure of the yolk-shell-shaped Au @ AgPt nanorod through different surfactant types.
2. The regulation and control method according to claim 1, wherein the specific steps of the step (1) are as follows:
and (3) synthesizing an Au nanorod:
preparing a seed solution: adding HAuCl4The solution was added to a cetyltrimethylammonium bromide (CTAB) solution to which was subsequently added freshly prepared NaBH4The solution is violently oscillated, and the obtained seed solution is used after standing for 1.5-2.5 h at room temperature;
preparing a growth solution: dissolving CTAB and sodium oleate (NaOL), adding AgNO3Standing the solution for 10-20 min; followed by HAuCl addition4Stirring the solution for 2-4 h, and then changing the color of the solution from orange yellow to colorless; adding HCl solution, and stirring for 10-20 min; finally adding ascorbic acid solution and stirring vigorously to obtain growth solution；
Adding a proper amount of seed solution into the growth solution, inverting, mixing, standing overnight at room temperature, purifying the Au nanorods by a centrifugal method, washing with high-purity water for multiple times to remove redundant surfactant, and dispersing the obtained Au nanorods in the high-purity water for later use.
3. The regulation and control method according to claim 1, wherein the specific steps of the step (2) are as follows:
synthesizing Au @ Ag nanorods:
firstly, the prepared polyvinylpyrrolidone (PVP) solution and CTAB solution are mixed evenly in an oil bath kettle at 60 ℃. Then adding the Au nano rod solution and AgNO prepared in the step (1)3Stirring the solution, ascorbic acid solution and NaOH solution at the temperature for 30min to react to obtain Au @ Ag nano rods, washing the material for many times by using ethanol and high-purity water, and dispersing the obtained product in 4mL of high-purity water for later use.
4. The regulation and control method according to claim 1, wherein the specific steps of the step (3) are as follows:
synthesizing a Yolk-shell-shaped Au @ AgPt nanorod:
uniformly mixing the Au @ AgNRs solution prepared in the step (2) with a surfactant solution and an ascorbic acid solution, and adding H into the mixture2PtCl4The solution is stirred and reacted for a period of time at the temperature of 55-65 ℃ to obtain Au @ AgPt nano-rods, and finally the Au @ AgPt nano-rods and NH are added3·H2And O is stirred at room temperature overnight to obtain a final product of yolk-shell-shaped Au @ AgPt nano rod.
5. The method according to claim 1, wherein the surfactant in step (3) is any one of CTAB, F127 and PVP.
6. Yolk-shell-shaped Au @ AgPt nanorods with different structures, prepared by any one of the regulation and control methods of claims 1-5.
7. A nanoreactor comprising the Yolk-shell-like Au @ AgPt nanorod of claim 6.
8. Use of Yolk-shell like Au @ AgPt nanorods as claimed in claim 6 in electrocatalytic oxygen reduction reactions.
9. The Yolk-shell-like Au @ AgPt nanorod as claimed in claim 6, for use in the field of nanomedicine.
CN202010127005.6A 2020-02-28 2020-02-28 Method for regulating and controlling Yolk-shell nano structure Withdrawn CN111112640A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113319275A (en) * 2021-04-14 2021-08-31 深圳大学 Au @ AgNRs nanorod as well as preparation method and application thereof
CN113369494A (en) * 2021-06-11 2021-09-10 杭州电子科技大学 Hollow gold-silver-platinum trimetal material and synthesis method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113319275A (en) * 2021-04-14 2021-08-31 深圳大学 Au @ AgNRs nanorod as well as preparation method and application thereof
CN113369494A (en) * 2021-06-11 2021-09-10 杭州电子科技大学 Hollow gold-silver-platinum trimetal material and synthesis method thereof
CN113369494B (en) * 2021-06-11 2023-06-06 杭州电子科技大学 Hollow gold-silver-platinum trimetallic material and synthesis method thereof

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