CN113579245A - Method for regulating and controlling morphology of nanogold assembly by one-step method - Google Patents
Method for regulating and controlling morphology of nanogold assembly by one-step method Download PDFInfo
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- CN113579245A CN113579245A CN202110813759.1A CN202110813759A CN113579245A CN 113579245 A CN113579245 A CN 113579245A CN 202110813759 A CN202110813759 A CN 202110813759A CN 113579245 A CN113579245 A CN 113579245A
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Abstract
The invention relates to a method for regulating and controlling the morphology of a nanogold assembly by a one-step method, which comprises the following steps of: s1, preparing a chloroauric acid aqueous solution, and regulating and controlling the pH value of the chloroauric acid solution; s2, adding cyclohexanone solution above the chloroauric acid aqueous solution, and sealing with a preservative film to construct a cyclohexanone/water binary system; s3, stirring the cyclohexanone/water binary system slightly by a rotor; s4, forming a nano gold particle assembly layer at the cyclohexanone/water interface; and S5, removing the preservative film, and taking out the nano gold assembly after the cyclohexanone is completely volatilized. The method realizes the direct conversion from the chloroauric acid solution to the shape-controllable nano-gold assembly, and does not use surface activity in the process. Therefore, the prepared assembly has cleaner particle surface, smaller inter-particle distance and better assembly performance.
Description
Technical Field
The invention belongs to the field of nano material self-assembly, and particularly relates to a method for regulating and controlling the appearance of a nano gold assembly by a one-step method.
Background
Assembled nanoparticles exhibit many novel or stronger properties relative to individual nanoparticles due to inter-particle coupling effects, which open new avenues for the fabrication of functional materials with specific physical and chemical properties. Furthermore, nanoparticle assembly is also an important way to connect the nanometer world with the macroscopic world.
The properties of nanoparticle assemblies are closely related to the morphology of individual nanoparticles and the spatial position between particles. The properties of a single nanoparticle are mainly determined by the size and shape of the nanoparticle, and the spatial position between the particles mainly refers to the distance between the particles, the orientation and the like. For example, gold nanoparticles (AuNPs) having a diameter of 10 nm have high catalytic activity, but cannot generate a sufficient electromagnetic field compared to AuNPs having a diameter of 50 nm. The star-shaped AuNPs have higher electromagnetic energy at the protruding tip than the spherical core due to the increased cross-section of the electromagnetic field due to plasmon hybridization. When two AuNPs are assembled very closely together, near-field coupling between their plasmons, excitons and magnetics may occur, creating a new enhancement. For example, as the gap between nanoparticles decreases from 10 nm to 2 nm, their electromagnetic field can increase by several orders of magnitude. Therefore, the synthesis of the nanoparticle assembly with ideal properties to meet the requirements of practical application by regulating the morphology of the nanoparticles in the nanoparticle assembly and the distance between the particles has important significance.
Currently, nanoparticle self-assembly strategies typically involve two major steps. Firstly, monodisperse nanoparticles with different morphologies are controllably synthesized, and then a nanoparticle assembly with a specific function is prepared. In order to prepare nanoparticles having a specific shape, which can exist stably, surfactants are often used as selective passivating agents and stabilizing agents, so that on one hand, different crystal faces are selectively adsorbed, thereby facilitating the preparation of nanoparticles having an ideal morphology, and on the other hand, the generated nanoparticles are prevented from aggregating. However, surfactants increase the charge density on the nanoparticle surface, which not only hinders the subsequent self-assembly process, but also increases the distance between the particles, impairing the inter-nanoparticle coupling effect in the assembly. Therefore, under the condition of not using a surfactant, the method has important significance for directly constructing the nanoparticle assembly with controllable morphology from the metal salt solution.
The nano gold particles are the most widely used nano particles, and are the most commonly used particles for constructing nano assemblies, and the assemblies have wide application in the fields of catalysis, sensing, SERS detection and the like. .
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for regulating and controlling the morphology of a nanogold assembly by a one-step method, so that the direct conversion from a chloroauric acid solution to the nanogold assembly is realized, the morphology of nanoparticles is controllable, and the property of the nanogold assembly can be effectively regulated and controlled. In addition, as the surfactant is not used, the activity of the nano particles is higher, the distance between the nano particles is smaller, and the coupling performance is better.
Therefore, the invention provides a method for regulating and controlling the morphology of a nanogold assembly by a one-step method, which comprises the following steps:
s1, preparing a chloroauric acid aqueous solution, and regulating and controlling the pH value of the chloroauric acid solution;
s2, adding cyclohexanone solution above the chloroauric acid aqueous solution, and sealing with a preservative film to construct a cyclohexanone/water binary system;
s3, stirring the cyclohexanone/water binary system slightly by a rotor;
s4, forming a nano gold particle assembly layer at the cyclohexanone/water interface;
and S5, removing the preservative film, and taking out the nano-gold assembly after the cyclohexanone is completely volatilized.
In some embodiments of the present invention, the specific operation of step S1 is: when the solubility of the chloroauric acid is prepared to be 0.5-10 mM, a whole self-assembly body is difficult to form on an interface when the concentration is too low, and the reverse reaction is too fast when the concentration is too high, so that the required morphology is difficult to regulate and control. HCl or NaOH solution is selected to adjust the pH value of the chloroauric acid solution, so that other substances can be introduced as little as possible. Because, chloroauric acid itself also contains Cl-And Na+The ion has small influence on the system. The pH regulation mechanism is mainly characterized in that the oxidation-reduction potential of the chloroauric acid is changed, so that the nucleation and growth processes of the nano-gold particles are changed, and the controllable morphology of the nano-particles is realized. Meanwhile, the low interfacial energy characteristic of cyclohexanone and water is combined, and the interfacial self-assembly of the nano-particle without the surfactant is promoted.
In some embodiments of the present invention, the specific operation of step S5 is: and after the cyclohexanone is completely volatilized, transferring the nano-gold assembly from the interface through a supporting material (such as a silicon wafer, glass, paper, an aluminum foil, a plastic plate and the like) to obtain the nano-gold self-assembly.
In some embodiments of the present invention, the specific operation of step S5 is: after the nano-gold assembly layer is formed and before cyclohexanone is completely volatilized, a high molecular polymer (preferably polyurethane, polyvinyl chloride, polystyrene, rubber and the like) solution is added. Premature addition of the polymer solution can cause interaction between the polymer and the chloroauric acid, and affect the shape control of the gold nanoparticles. Therefore, the polymer solution must be added after the nanogold assembly is completely formed. The optimal adding time is that after the nano gold assembly is completely formed, the macromolecular solution is slowly added before the cyclohexanone is quickly volatilized, so that the assembly is prevented from being damaged.
After the cyclohexanone is completely volatilized, the high molecular polymer forms a film on the interface, and the nano gold particles assembled on the interface are fixed to obtain the flexible self-supporting nano gold assembly. Since the nanogold assemblies are located at the interface, part of the assemblies are also in the aqueous phase. Therefore, the formed polymer film only wraps part of the nano-gold assembly, namely, part of the nano-gold particles are not wrapped by the polymer but are semi-embedded in the polymer film. Therefore, the nano gold particles still have high activity, such as high catalytic activity, high conductivity and the like. In addition, the appearance control of the nano gold particles can be influenced by adding the polymer solution too early. Therefore, the polymer solution must be added after the nano-gold assembly is completely formed, so as to prevent the appearance control from being influenced by the action between the polymer and the chloroauric acid.
In some embodiments of the present invention, no surfactant is used or other reducing agent is introduced in the method, and the prepared gold nanoparticles have no surface coating surfactant, can be closer to each other, and the assembly is more compact and ordered. The closer the particles are assembled, the stronger the conjugation effect among the particles is, so that the obtained nano gold assembly has higher conductivity and electromagnetic enhancement capability.
In some embodiments of the present invention, when the pH of the chloroauric acid solution is between 4.5 and 6.0, the nanogold assembly is a mixture of nano-sheets, nano-spheres and nano-rods, and the mixture has ultrahigh conductivity. Because the connection structure of metal in the polymer is related to the form of the conductive particles, the flaky particles are easy to form surface contact, the spherical particles are easy to form point contact, the flaky surface contact is easier to obtain good conductivity than the spherical point contact, and if the spherical particles and the flaky particles are mixed and used according to a proper proportion, the material has higher conductivity because the contact state of the conductive filler in the polymer is better than that of a pure flaky filler.
In some embodiments of the invention, when the pH of the chloroauric acid solution is 6.5-8.0, the nano-gold assembly is composed of nano-gold spheres with a heterostructure; the nano gold of the heterostructure is of a satellite structure, and a plurality of small nano gold balls are arranged on the surface of the large nano gold ball; the particle size of the large nano gold spheres is 50-100 nm, and the particle size of the small nano gold spheres is 8-25 nm; in the pH interval, the number of the small nano gold spheres is increased along with the increase of the pH; the nano-gold assembly with the heterostructure can be applied to monitoring a catalytic process, wherein small-particle nano-gold is used for catalytic reaction, and large-particle nano-gold is used for enhancing Raman signals.
In some embodiments of the present invention, when the pH of the chloroauric acid solution is greater than 8.0, the nanogold assembly is composed of nanogold spheres. The particle size of the nano gold ball is 10-50 nm, and the particle size of the nano gold ball is gradually reduced along with the increase of the pH value of the nano gold ball. Since the smaller the particle size of the nanoparticle, the higher the surface activity, the nanogold self-assembly under such conditions is suitable as a catalyst.
In some embodiments of the invention, nanoplatinum, nanopalladium assemblies may also be constructed using chloroplatinic acid, chloropalladic acid, and the like.
The invention has the beneficial effects that: the method of the invention realizes the preparation of controllable shape and appearance of the assembly by simply regulating and controlling the pH value, changing the oxidation-reduction potential of the chloroauric acid and combining the cyclohexanone-water low interface, and constructs the nano-gold assembly with controllable shape and appearance by a one-step method. According to different requirements of the application field, the pH is regulated and controlled to construct assemblies with different appearances, so that the optimization of the corresponding performance of the assemblies is realized, and the application prospect of the assemblies is expanded.
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The invention will be further explained with reference to the drawings.
Fig. 1 is an electron microscope image of the nanogold assembly prepared in example 1.
Fig. 2 is an electron microscope image of the nanogold assembly prepared in example 3.
FIG. 3 is an electron microscope image of the nano-gold assembly prepared in example 4.
FIG. 4 is an electron microscope image of the nano-gold assembly thin film prepared under the embodiment 5.
FIG. 5 is an electron microscope image of the nano-gold assembly thin film prepared under example 7.
Fig. 6 is a graph of the SERS signal collected over time for example 9.
FIG. 7 is a graph of the experiment of the finger joint movement on the change of the film resistance of the nano-gold assembly in example 10.
Detailed Description
The present invention will be described in detail below.
In order that the present invention may be more readily understood, the following detailed description will proceed with reference being made to examples, which are intended to be illustrative only and are not intended to limit the scope of the invention. The starting materials or components used in the present invention may be commercially or conventionally prepared unless otherwise specified.
Example 1: nanogold assembly under pH 5.2 condition
Adding 20 ml of 1% chloroauric acid aqueous solution and a rotor into a 25 ml beaker, adding NaOH solution to adjust the pH value to 5.2, then adding 3 ml of cyclohexanone, covering the beaker with a preservative film, stirring with the rotor to form a layer of nano-gold particles on the interface, removing the preservative film, and transferring the nano-gold assembly from a silicon wafer after the cyclohexanone is completely volatilized. The electron microscope image of the nano-gold assembly is shown in fig. 1 and consists of nano-gold sheets, rods and spheres.
Example 2: nano gold assembly film under condition of pH 5.2
Adding 20 ml of 1% chloroauric acid aqueous solution and a rotor into a 25 ml beaker, adding NaOH solution to adjust the pH value to 5.2, then adding 3 ml of cyclohexanone, covering the beaker with a preservative film, stirring with the rotor, forming a layer of nano-gold particles at an interface, removing the preservative film, slowly adding polyurethane cyclohexanone solution when the volatilization of the cyclohexanone is finished, and after the cyclohexanone is completely volatilized, forming a film by polyurethane to fix the nano-gold assembly to form the flexible nano-gold assembly film.
Example 3: the nano gold assembly is prepared under the conditions of pH 6.5, 6.8, 7.0 and 7.2
Adding 20 ml of 1% chloroauric acid aqueous solution and a rotor into a 25 ml beaker, adding NaOH solution to adjust the pH to 6.5, 6.7, 7.0 and 7.2 respectively, then adding 3 ml of cyclohexanone, covering the beaker with a preservative film, forming a layer of nano-gold particles at the interface along with the stirring of the rotor, removing the preservative film, and transferring the nano-gold assembly from a silicon wafer. The electron microscope images of the nanogold assembly under the 4 pH conditions are shown in FIG. 2, and the nanogold assembly is composed of nanogold (a large nanogold ball is provided with a plurality of small nanogold balls on the surface) with a satellite structure, and the number of the small nanogold balls is increased along with the increase of the pH.
Example 4: the nano gold assembly under the conditions of pH 9.0, 10.6 and 12.0
Adding 20 ml of 1% chloroauric acid aqueous solution and a rotor into a 25 ml beaker, adding NaOH solution to adjust the pH to 9.0, 10.6 and 12.0 respectively, then adding 3 ml of cyclohexanone, covering the beaker with a preservative film, forming a layer of nano-gold particles at an interface along with the stirring of the rotor, removing the preservative film, and transferring the nano-gold assembly out by using glass. The electron microscope image of the nano gold assembly under the 3 pH conditions is shown in FIG. 3, and the nano gold assembly is composed of nano gold spheres, and the particle size of the nano gold spheres is gradually reduced along with the increase of the pH value.
Example 5: nano gold assembly film under pH 6.7 condition
Adding 20 ml of 1% chloroauric acid aqueous solution and a rotor into a 25 ml beaker, adding NaOH solution to adjust the pH value to 6.7, then adding 3 ml of cyclohexanone, covering the beaker with a preservative film, forming a layer of nano-gold particles at an interface along with the stirring of the rotor, removing the preservative film, adding polyurethane cyclohexanone solution, and after the cyclohexanone is completely volatilized, forming a film by polyurethane to fix the nano-gold assembly to form a flexible nano-gold assembly film. The nanogold assembly is shown in figure 4 in an electron microscope.
Example 6: nano gold assembly film under pH 6.7 condition
Adding 20 ml of 1% chloroauric acid aqueous solution and a rotor into a 25 ml beaker, adding NaOH solution to adjust the pH to 6.7, then adding 3 ml of cyclohexanone and polyurethane cyclohexanone solution, covering the beaker with a preservative film, stirring the rotor all the time in time, wherein a layer of nano-gold particles cannot be formed at the interface, and after the cyclohexanone is completely volatilized, no nano-gold assembly exists on the polyurethane film.
Example 7: nano gold assembly film under pH 6.7 condition
Adding 20 ml of 1% chloroauric acid aqueous solution and a rotor into a 25 ml beaker, adding NaOH solution to adjust the pH to 6.7, then adding 3 ml of cyclohexanone and polyvinyl chloride cyclohexanone solution, stirring with the rotor, forming a layer of nano-gold particles at the interface, removing a preservative film, and after the cyclohexanone is completely volatilized, forming a film of polyvinyl chloride to fix the nano-gold assembly to form a flexible nano-gold assembly film. However, as the polyvinyl chloride is added in advance, the formed nano particles are spherical and are not satellite structure nano gold under the original condition. The nanogold assembly is shown in figure 5 in an electron microscope.
Example 8: conductivity of film of assembly with different shapes
Under the same conditions, the sheet resistances of the nanogold assembly films prepared at pH 5.2, 6.7 and 10.6 were measured and the conductivities thereof were calculated by using a four-probe method, and the results showed that the nanogold assembly prepared at pH =5.2 had the highest conductivity, followed by pH =6.7 and the worst was pH = 10.6.
Example 9: process for catalyzing and monitoring nitrothiophenol (4-NTP) to generate p-aminophenol (4-ATP) by satellite-structure nano gold assembly
The satellite structure nanogold assembly prepared in example 3 is soaked in a nitrothiophenol solution for 1 hour, after being taken out and cleaned, a sodium borohydride solution is dripped on the assembly, SERS signals on the surface of the nanogold assembly film are collected every few seconds by a Raman spectrometer, and a graph of the change of an SERS spectrum with time is drawn, as shown in FIG. 6.
Example 10: nano gold assembly film applied to tension sensing
The nanogold assembly film prepared in example 2 was attached to the knuckle portion, and when the finger was straightened or bent, the resistance of the nanogold assembly film changed significantly, and the degree of bending of the finger was reflected by the change in resistance, which was used as a tension sensor, as shown in fig. 7.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (9)
1. A method for regulating and controlling the morphology of a nanogold assembly by a one-step method comprises the following steps:
s1, preparing a chloroauric acid aqueous solution, and regulating and controlling the pH value of the chloroauric acid solution;
s2, adding cyclohexanone solution above the chloroauric acid aqueous solution, covering a preservative film, and constructing a cyclohexanone/water binary system;
s3, stirring the cyclohexanone/water binary system slightly by a rotor;
s4, forming a nano gold particle assembly layer at the cyclohexanone/water interface;
and S5, removing the preservative film, and taking out the nano-gold assembly after the cyclohexanone is completely volatilized.
2. The method of claim 1, wherein step S1 is specifically performed by preparing a chloroauric acid solubility of 0.5 mM-10 mM and adjusting the pH of the chloroauric acid solution by adding dropwise HCl or NaOH solution.
3. The method according to claim 1, wherein step S5 is specifically performed by transferring the nano-gold assembly from the interface through the supporting material after the cyclohexanone is completely volatilized; the supporting material is silicon chip, glass, paper, plastic board and aluminum foil.
4. According to the claimsThe method of claim 1, wherein the specific operation of step S5 is to slowly add the high molecular polymer solution after the formation of the nanogold assembly layer and before the complete volatilization of cyclohexanone, after the complete volatilization of cyclohexanone, the high molecular polymer forms a film at the interface, and fix the nanogold particles self-assembled at the interface to obtain a flexible self-supporting nanogold assembly; the self-supporting nano particle assembly is in a polymer semi-wrapped nano particle structure, namely part of nano particles are not wrapped by the polymer; the dosage of the polymer is 2-10 mg/cm2 。
5. The method of claim 1, wherein the nanoparticles are prepared without surface active agent, the surface of the nanoparticles is not coated by the surface active agent, the nanoparticles can be closer together, the assembly is more compact and ordered, and the electrical conductivity and electromagnetic enhancement capability of the assembly are higher.
6. The method according to claim 1, wherein the assembly is a mixture of nanoplates, rice spheres and nanorods, which has high conductivity, when the pH of the chloroauric acid solution is between 4.5 and 6.0.
7. The method according to claim 1, wherein when the pH of the chloroauric acid solution is 6.5-8.0, the assembly is composed of heterostructure gold nanospheres; the nano gold of the heterostructure is of a satellite structure, and a plurality of small nano gold balls are arranged on the surface of the large nano gold ball; the particle size of the large nano gold spheres is 50-100 nm, and the particle size of the small nano gold spheres is 8-25 nm; in the pH interval, the number of the small nano gold spheres is increased along with the increase of the pH; the nano-gold assembly with the heterostructure can be applied to monitoring a catalytic process, wherein small-particle nano-gold is used for catalytic reaction, and large-particle nano-gold is used for enhancing Raman signals.
8. The method of claim 1, wherein when the pH of the chloroauric acid solution is greater than 8.0, the assembly is comprised of nanogold spheres; the particle size of the nano gold ball is 10-50 nm, and the particle size of the nano gold ball is gradually reduced along with the increase of the pH value of the nano gold ball.
9. The method of claim 1, wherein the method is applied to chloroplatinic acid and chloropalladic acid to construct a nano platinum and nano palladium assembly.
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