CN115016045A - Universal assembling method for plasmon nanometer superstructure - Google Patents
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- CN115016045A CN115016045A CN202210492705.4A CN202210492705A CN115016045A CN 115016045 A CN115016045 A CN 115016045A CN 202210492705 A CN202210492705 A CN 202210492705A CN 115016045 A CN115016045 A CN 115016045A
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Abstract
The invention discloses a general assembly method of a plasmon nanometer superstructure, which comprises the following steps: (1) synthesizing nanoparticles with plasmon activity; (2) preparing modified positively charged particles; (3) and forming the plasmon nanometer superstructure. The invention selectively modifies positively charged molecules at one end of a nanoparticle with plasmon activity; the method has the advantages that nanoparticles with different plasmon activities are assembled together to form the plasmon superstructure in an electrostatic self-assembly mode, the SERS substrate can be prepared into the plasmon super-structure for rapid detection of SERS, and can be directly placed in a photocatalytic reaction device for direct photocatalytic experiments, and can also be used for solar cells, plasmon-enhanced photodetectors, plasmon-enhanced fluorescence and the like.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a general assembling method of a plasmon nanometer superstructure.
Background
The plasmon nanometer material has large scattering and absorption cross sections, and is widely applied to the fields of plasmon enhanced photocatalysis, plasmon enhanced photoelectric detectors, surface enhanced Raman scattering spectroscopy, plasmon enhanced solar cells and the like. In addition, the absorption efficiency of the plasmon nanometer material in the full spectrum range of sunlight can be improved by changing the size, the shape and the composition of the plasmon nanometer material. Particularly, when two or more plasmon nanoparticles are close to each other, the local electromagnetic field strength around the plasmon nanoparticles is greatly improved due to the coupling effect between the plasmon nanoparticles, so that the utilization efficiency of sunlight is remarkably improved. However, the plasmonic nanomaterial prepared by a synthesis method generally adopted by people often exists in a single particle form, so that the utilization efficiency of the plasmonic nanomaterial to sunlight is still low. With the continuous development of the technology, people adopt technical means such as photoetching and micro-nano processing to realize the periodic arrangement of the plasmon nanometer materials, and the utilization efficiency of the materials to sunlight is improved to a certain extent. However, the technical means is expensive, so that the application of the plasmon nanometer material in real life is greatly limited.
On the other hand, in an actual environment, two or more plasmon nanomaterials are often required to cooperate with each other to improve the efficient utilization of sunlight by the materials to the maximum extent. The preparation of the multi-component plasmon nanometer material by means of photoetching, micro-nano processing and the like is particularly difficult.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a general assembling method of a plasmon nanometer superstructure, which is used for solving the problem that a single plasmon nanometer material cannot meet the requirements of actual complex conditions for a long time.
In order to achieve the above purpose, one of the technical solutions of the present invention is: a general assembling method of a plasmon nanometer superstructure specifically comprises the following steps:
(1) synthesizing nanoparticles with plasmon activity;
(2) soaking the nanoparticles synthesized in the step (1) in positively charged modified molecules to obtain modified positively charged particles;
(3) and (3) simply and physically mixing the nanoparticles synthesized in the step (1) and the modified positively charged particles obtained in the step (2) to obtain the plasmon nanometer superstructure made of different materials.
In a further scheme, the assembling method further comprises the step of preparing the plasmon nanometer superstructure into an SERS substrate, or directly placing the plasmon nanometer superstructure in a photocatalytic reaction device.
Further, the particles for synthesizing the specific plasmon nanometer material in the step (1) comprise Au, Ag, Au @ SiO 2 、Ag@SiO 2 、Au@TiO 2 、Au@CdS、Ag@TiO 2 One or more of Au @ Pt, Au @ Pd and AuPt alloy.
In a further scheme, the positively charged modified molecule in the step (2) is one of polyallylamine hydrochloride, 4-dimethylaminopyridine and hexadecyl trimethoxy ammonium chloride.
Further, in the step (3), only the positively-modified plasmonic nanoparticles and the non-modified plasmonic nanoparticles need to be simply mixed to obtain plasmonic nano superstructures with various unique properties, such as: ag @ SiO 2 -Au@CdS、Au@SiO 2 -Au@CdS、Au-AuPt、Au@TiO 2 AuAg, Au @ Pt-Au, Au @ CdS-Au @ Pt, etc.
In a further scheme, the nanoparticles synthesized in the step (3) are mixed with the modified positively charged particles according to the volume ratio of 1: 1.
In order to achieve the above purpose, the second technical solution of the present invention is: a plasmon nanometer superstructure is prepared by a general assembly method of the plasmon nanometer superstructure.
In order to achieve the above purpose, the third technical scheme of the invention is as follows: use of a plasmonic superstructure as a SERS substrate capable of targeting not only drug-like molecules such as: the kit can be used for rapidly detecting the methamphetamine, K powder, morphine, synthetic cannabinoids, fentanyl and the like, and can also be used for detecting pollutants in the environment such as: toluene, methylene blue, malachite green, methyl orange etc. carry out short-term test, can also be to pesticide residue like simultaneously: and (4) carrying out rapid detection on paraquat and methamidophos. In addition, the substrate can be used for detecting a single-component sample and also can be used for quickly detecting a multi-class mixture.
According to a further scheme, the plasmon nanometer superstructure in the step (4) is prepared into an SERS substrate, and SERS detection can be carried out on the object to be detected, wherein molecules capable of being detected by the SERS substrate comprise various molecules with SERS activity, such as toluene, methamphetamine, methylene blue, paraquat and the like.
In a further scheme, before SERS detection, molecules of an object to be detected are dripped on the surface of the assembled plasmon superstructure.
In order to achieve the above purpose, the fourth technical scheme of the invention is as follows: the application of the plasmon superstructure can be directly placed in a photocatalytic reaction device to carry out photocatalytic hydrogen production or photocatalytic oxygen production experiments.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention can change the composition components in the plasmon assembly structure according to the actual situation, thereby obtaining the novel plasmon nanometer superstructure which meets the actual requirement and has the property different from that of single-particle nanometer particles.
2. The plasmon super-structure nano particle synthesized by the invention can be prepared into an SERS substrate for rapid detection of SERS, and can also be directly placed in a photocatalytic reaction device for direct photocatalytic experiments.
3. The plasmon superstructure assembly synthesized by the invention can also be used for solar cells, plasmon enhanced photodetectors, plasmon enhanced fluorescence and the like, and the method is simple and rapid to operate and can be synthesized in batches.
Drawings
FIG. 1 is Ag @ SiO prepared in example 1 2 -transmission electron microscopy and scanning electron microscopy images of Au plasmonic superstructure;
FIG. 2 is a graph of Ag @ SiO in example 1 2 Preparing an SERS graph of the SERS substrate for rapidly detecting paraquat molecules by using the Au plasmon superstructure;
FIG. 3 is a SERS diagram of the rapid detection of paraquat molecules by common Au nanoparticles;
FIG. 4 is the Ag @ SiO film prepared in example 2 2 -transmission electron microscopy and scanning electron microscopy images of Au @ CdS plasmonic superstructure;
FIG. 5 is Ag @ SiO prepared in example 2 2 -Au @ CdS plasmonic superstructure directly placed in lightAnd (3) an activity data chart of a photocatalytic hydrogen production experiment in the catalytic reaction device.
FIG. 6 is a transmission electron microscope and scanning electron microscope image of the Au @ CdS-Au @ Pt plasmonic superstructure prepared in example 3;
FIG. 7 is a graph of activity data for a photocatalytic hydrogen production experiment in which the Au @ CdS-Au @ Pt plasmonic superstructure prepared in example 3 was directly placed in a photocatalytic reaction device.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in more detail below with reference to the accompanying drawings and specific embodiments, but the scope of the present invention is not limited to these embodiments.
A general assembling method of a plasmon nanometer superstructure is characterized by comprising the following steps:
(1) synthesizing nanoparticles with plasmon activity;
(2) soaking the nanoparticles synthesized in the step (1) in positively charged modified molecules to obtain modified positively charged particles;
(3) and (3) mixing the nanoparticles synthesized in the step (1) with the modified positively charged particles obtained in the step (2) to obtain the plasmon nanometer superstructure made of different materials.
And preparing the plasmon nanometer superstructure into an SERS substrate, or directly placing the plasmon nanometer superstructure in a photocatalytic reaction device.
The nano particles in the step (1) comprise Au, Ag and Au @ SiO 2 、Ag@SiO 2 、Au@TiO 2 、Au@CdS、Ag@TiO 2 One or more of Au @ Pt, Au @ Pd and AuPt alloy; the positively-charged modified molecule in the step (2) is one of polyallylamine hydrochloride, 4-dimethylaminopyridine and hexadecyl trimethoxy ammonium chloride; the plasmon nanometer superstructure in the step (3) comprises Ag @ SiO 2 -Au@CdS、Au@SiO 2 -Au@CdS、Au-AuPt、Au@TiO 2 -one of AuAg, Au @ Pt-Au, Au @ CdS-Au @ Pt.
And (3) mixing the synthesized nanoparticles with the modified positively charged particles according to the volume ratio of 1: 1.
A plasmon nanometer superstructure is prepared by a general assembly method of the plasmon nanometer superstructure.
The application of the plasmon nanometer superstructure is used as an SERS substrate for rapid detection of drug molecules, pollutants in the environment and pesticide residues.
The drug molecules comprise methamphetamine, K powder, morphine, synthetic cannabinoids and fentanyl, the pollutants in the environment comprise methylene blue, malachite green and methyl orange, and the pesticide residues comprise paraquat and methamidophos.
Before the rapid detection, the molecules of the object to be detected are dripped on the surface of the assembled plasmon superstructure.
The SERS substrate is used for rapidly detecting single-component samples and multi-class mixtures.
The application of the plasmon nanometer superstructure is used for photocatalytic experiments including photocatalytic hydrogen production experiments or photocatalytic oxygen production experiments.
Example 1
The invention relates to a general assembling method of a plasmon nanometer superstructure, and Ag @ SiO is prepared 2 -transmission electron microscopy and scanning electron microscopy of Au plasmonic superstructure as shown in FIG. 1,
(1) the large-size Ag nano particles are synthesized by adopting a seed growth method: the specific operation steps are as follows:
1) 2ml of HAuCl with the mass fraction of 1 percent is taken 4 Adding the solution into 200ml of ultrapure water, adding 2ml of 1% sodium citrate solution after the solution is boiled, and reacting for 30 minutes to obtain the Au seed with the size of 45 nm. The Au nano-particles with the size of 16nm are synthesized only by increasing the amount of the sodium citrate to 6 ml.
2) Adding 10ml of 45nm Au seed into 60ml of water, adding 1.2ml of sodium citrate and ascorbic acid solution with molar concentration of 20mM respectively, and adding 10ml of AgNO with molar concentration of 10mM into the solution at normal temperature 3 And (4) obtaining Ag nano particles with the size of 120nm by using the solution.
(2) 60ml of Ag nanoparticles obtained in step (1) were added with 1ml of 10mM molar 3-aminopropyltrimethoxysilane and stirred for 15 minutes. Then, 3.2ml of 0.54% sodium silicate solution was added thereto and reacted at 90 ℃ for 30 minutes to obtain Ag @ SiO with a shell thickness of 2nm 2 Nanoparticles.
(3) Taking the Ag @ SiO synthesized in the step (2) 2 Mixing 10ml of nano particles with 0.02ml of polyallylamine hydrochloride with the molar concentration of 10mM for 10 minutes, adding 10ml of Au nano particles with the size of 16nm, and carrying out ultrasonic treatment for 30 minutes to obtain Ag @ SiO 2 -an Au plasmonic superstructure.
(4) The Ag @ SiO assembled in the step (3) is added 2 And dripping the Au plasmon superstructure after centrifugal concentration on a gold sheet, and drying to prepare the SERS chip.
(5) Taking a vegetable leaf with paraquat residue, wiping the surface of the vegetable leaf with a cotton swab soaked with alcohol, and dipping the alcohol on the cotton swab into the Ag @ SiO prepared in the step (4) 2 On the Au plasmon superstructure SERS chip, a 785nm handheld Raman spectrometer is used for testing to obtain the SERS spectrogram shown in the figure 2. The figure shows that the substrate can well and rapidly detect the drugs, and meanwhile, the detection sensitivity of the substrate reaches below 0.05ppb which is surprising, and the substrate can well meet the field detection requirement. The SERS enhanced substrate prepared by the method has more excellent SERS enhancing capability than common Au nanoparticles (figure 3).
Example 2
The invention relates to a general assembling method of a plasmon nanometer superstructure, and Ag @ SiO is prepared 2 -Au @ CdS plasmonic superstructure transmission electron microscope and scanning electron microscope images are shown in FIG. 4,
(1)Ag@SiO 2 reference example 1.
(2) The synthesis steps of Au @ CdS are as follows: 30ml of 16nm Au nano particles are taken and added with 3ml of mixed solution of cadmium nitrate and L-cysteine with the molar concentration of 10 mM. And then, transferring the Au @ CdS nanoparticles into a reaction kettle to react for 6 hours at 130 ℃, so as to obtain the Au @ CdS nanoparticles.
(3) Taking the step (1) Well synthesized Ag @ SiO 2 10ml of nanoparticles, to which 0.02ml of 4-dimethylaminopyridine with a molar concentration of 20mM was added.
(4) Taking 10ml of Au @ CdS nano particles prepared in the step (2), and adding the Au @ CdS nano particles into Ag @ SiO modified with 4-dimethylaminopyridine molecules in the step (3) 2 In the nano particles, Ag @ SiO can be obtained 2 -Au @ CdS plasmonic superstructure.
(5) The Ag @ SiO assembled in the step (4) is processed 2 the-Au @ CdS plasmon superstructure is directly placed in a photocatalytic reaction device to carry out a photocatalytic hydrogen production experiment, and the obtained photocatalytic hydrogen production data are shown in figure 5. From the figure, it can be seen that Ag @ SiO is compared with Au @ CdS alone 2 the-Au @ CdS plasmon superstructure shows extremely high photocatalytic activity.
Example 3
The invention discloses a general assembling method of plasmon nanometer superstructure, preparing Au @ CdS-Au @ Pt plasmon superstructure transmission electron microscope and scanning electron microscope images as shown in figure 6,
(1) 2ml of HAuCl with the mass fraction of 1 percent is taken 4 Adding the solution into 200ml of ultrapure water, adding 1.5ml of 1% sodium citrate solution after the solution is boiled, and reacting for 30 minutes to obtain the Au nano particles with the size of 55 nm.
(2) 2ml of HAuCl with the mass fraction of 1 percent is taken 4 Added to 200ml of ultrapure water, and 6ml of a 1% by mass sodium citrate solution was added thereto. Then, 1ml of 38mM sodium borohydride solution is rapidly added to obtain 5-8nm Au nanoparticles.
(3) Taking 200ml of the 55nm Au nano particles in the step (1), and respectively adding 3ml of sodium citrate with the mass fraction of 1% and 5ml of CdCl with the molar concentration of 20mM into the Au nano particles 2 Then, the pH was adjusted to 10.2 with concentrated ammonia water. And then, transferring the reaction solution to a 70-degree water bath for reaction for 6 hours to obtain the Au @ CdS nano particles.
(4) 30ml of the 5-8nm Au nanoparticles prepared in the step (2) are taken, and 3ml of sodium citrate and 3ml of ascorbic acid are added into the Au nanoparticles. Then, 1ml of a solution containing 0.1% by mass of a solvent was slowly added dropwise theretoHPtCl 4 And obtaining the Au @ Pt nano particles.
(5) And (3) taking 10ml of the Au @ CdS nano particles synthesized in the step (3), adding 0.02ml of polyallylamine hydrochloride with the molar concentration of 10mM, mixing for 10 minutes, adding 10ml of Au @ Pt nano particles, and performing ultrasonic treatment for 30 minutes to obtain the Au @ CdS-Au @ Pt plasmon superstructure.
(6) And (3) directly placing the Au @ CdS-Au @ Pt plasmon superstructure assembled in the step (5) in a photocatalytic reaction device to perform a photocatalytic hydrogen production experiment, wherein the obtained photocatalytic hydrogen production data are shown in FIG. 7. The photo-catalytic activity of the Au @ CdS-Au @ Pt plasmon superstructure compared with that of pure Au @ CdS is larger and flexible in selecting and assembling structure, so that the Au @ CdS plasmon super-structure has excellent performance in the SERS detection field, the photo-catalytic field, the photoelectric detection field, the solar cell field and the like. The preparation method is simple, convenient and rapid. Meanwhile, the assembly can be carried out in batch. Therefore, the invention has great commercial application prospect.
The above embodiments are merely preferred embodiments of the present invention, which are provided for illustrating the principles and effects of the present invention and not for limiting the present invention. It should be noted that modifications to the above-described embodiments can be made by persons skilled in the art without departing from the spirit and scope of the invention, and such modifications should also be considered as within the scope of the invention.
Claims (10)
1. A general assembling method of a plasmon nanometer superstructure is characterized by comprising the following steps:
(1) synthesizing nanoparticles with plasmon activity;
(2) soaking the nano particles synthesized in the step (1) in positively charged modified molecules to obtain modified positively charged particles;
(3) and (3) mixing the nanoparticles synthesized in the step (1) with the modified positively charged particles obtained in the step (2) to obtain the plasmon nanometer superstructure.
2. The method for universal assembly of plasmonic nano-superstructures according to claim 1, further comprising the steps of: and preparing the plasmon nanometer superstructure into an SERS substrate, or directly placing the plasmon nanometer superstructure in a photocatalytic reaction device.
3. The method for assembling a plasmonic nanostructure of claim 1, wherein said nanoparticles of step (1) comprise Au, Ag, Au @ SiO 2 、Ag@SiO 2 、Au@TiO 2 、Au@CdS、Ag@TiO 2 One or more of Au @ Pt, Au @ Pd and AuPt alloy; the positively-charged modified molecule in the step (2) is one of polyallylamine hydrochloride, 4-dimethylaminopyridine and hexadecyl trimethoxy ammonium chloride; the plasmon nanometer superstructure in the step (3) comprises Ag @ SiO 2 -Au@CdS、Au@SiO 2 -Au@CdS、Au-AuPt、Au@TiO 2 -one of AuAg, Au @ Pt-Au, Au @ CdS-Au @ Pt.
4. The method for assembling a plasmonic nano superstructure according to claim 1, wherein the nanoparticles synthesized in step (3) are mixed with the modified positively charged particles in a volume ratio of 1: 1.
5. The plasmonic nano superstructure prepared by the general assembly method of any one of claims 1 to 4.
6. Use of the plasmonic nanostructural according to claim 5 as a SERS substrate for rapid detection of drug like molecules, environmental pollutants, pesticide residues.
7. Use of a plasmonic nanostructural according to claim 6, wherein said poison based molecules comprise methamphetamine, K powder, morphine, synthetic cannabinoids, fentanyl, said environmental contaminants comprise methylene blue, malachite green, methyl orange, said pesticide residues comprise paraquat, methamidophos.
8. Use of a plasmonic nanostructure according to claim 6, wherein the rapid detection is preceded by dropping analyte molecules onto the surface of the assembled plasmonic superstructure.
9. The use according to claim 6, wherein the SERS substrate is used for rapid detection of single-component samples and multi-class mixtures.
10. Use of a plasmonic nano-superstructure according to claim 5 for photocatalytic experiments including photocatalytic hydrogen or photocatalytic oxygen production experiments.
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