CN115016045B - Universal assembling method for plasmon nanometer super structure - Google Patents

Universal assembling method for plasmon nanometer super structure Download PDF

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CN115016045B
CN115016045B CN202210492705.4A CN202210492705A CN115016045B CN 115016045 B CN115016045 B CN 115016045B CN 202210492705 A CN202210492705 A CN 202210492705A CN 115016045 B CN115016045 B CN 115016045B
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plasmon
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CN115016045A (en
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李剑锋
杨晶亮
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Xiamen University
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    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/002—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials
    • 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
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    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/008—Surface plasmon devices
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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Abstract

The invention discloses a general assembly method of a plasmon nanometer super structure, which specifically comprises the following steps: (1) synthesizing nanoparticles with plasmonic activity; (2) producing modified positively charged particles; and (3) forming the plasmon nanometer super structure. The invention selectively modifies positively charged molecules at one end of nano particles with plasmon activity; the nano particles with different plasmon activities are assembled together in an electrostatic self-assembly mode to form a plasmon super structure, so that the method can be prepared into a SERS substrate for SERS rapid detection, can be directly placed in a photocatalytic reaction device for direct photocatalysis experiments, can be also used for solar cells, plasmon enhanced photoelectric detectors, plasmon enhanced fluorescence and the like, and is simple and rapid to operate and capable of synthesizing in batches.

Description

Universal assembling method for plasmon nanometer super structure
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a general assembly method of a plasmon nano super structure.
Background
The plasmon nano material has large scattering and absorption cross sections, and is widely applied to various fields such as plasmon enhanced photocatalysis, plasmon enhanced photoelectric detectors, surface enhanced Raman scattering spectrums, plasmon enhanced solar cells and the like. In addition, the improvement of the absorption efficiency of the plasmon nano material in the full spectrum range of sunlight can be realized by changing the size, the shape and the composition of the plasmon nano material. Particularly, when two or more plasmon nano particles are close to each other, the local electromagnetic field intensity around the plasmon nano particles is greatly improved due to the coupling effect of the plasmon nano particles, so that the utilization efficiency of sunlight is remarkably improved. However, the plasmonic nano material prepared by the synthesis method generally adopted by people often exists in a single particle form, so that the utilization efficiency of sunlight is still low. Along with the continuous development of technology, the periodic arrangement of the plasmon nanometer materials is realized by adopting technical means such as photoetching, micro-nano processing and the like, and the utilization efficiency of the materials to sunlight is improved to a certain extent. However, the application of the plasmon nanometer material in the actual life is greatly limited due to the expensive technical means.
On the other hand, in the practical environment, two or more plasmon nanometer materials are often required to cooperate with each other to furthest promote the efficient utilization of the materials to sunlight. This makes it particularly difficult to prepare multicomponent plasmonic nanomaterials by means of photolithography, micro-nano processing, etc.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a general assembly method of a plasmon nano super structure, which is used for solving the problem that a single plasmon nano material cannot meet the requirements of actual complex conditions for a long time.
In order to achieve the above object, one of the technical solutions of the present invention is: the general assembly method of the plasmon nanometer super structure specifically comprises the following steps:
(1) Synthesizing nano particles with plasmon activity;
(2) Immersing the nano particles synthesized in the step (1) in positively charged modification molecules to obtain modified positively charged particles;
(3) And (3) simply and physically mixing the synthesized nano particles in the step (1) with the modified positively charged particles obtained in the step (2), so as to obtain the plasmon nano super structure composed of different materials.
Further, the assembly method further comprises the step of preparing the plasmon nanometer super structure into a SERS substrate, or directly placing the plasmon nanometer super structure into a photocatalysis 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 cetyltrimethoxyammonium chloride.
Further, in the step (3), only the modified positively charged plasmonic nanoparticles and the unmodified plasmonic nanoparticles are 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 and the like.
Further, the synthesized nano particles in the step (3) are mixed with modified positively charged particles according to a volume ratio of 1:1.
In order to achieve the above object, a second technical scheme of the present invention is as follows: the plasmon nanometer super structure is prepared by a general assembly method of the plasmon nanometer super structure.
In order to achieve the above object, a third aspect of the present invention is: the use of plasmonic superstructures as SERS substrates not only for drugs such as: the quick detection of the icetoxin, K powder, morphine, synthetic cannabinoids, fentanyl and the like can also be carried out on pollutants in the environment such as: toluene, methylene blue, malachite green, methyl orange and the like can be detected rapidly, and meanwhile, the pesticide residue can be detected as follows: and (5) rapidly detecting paraquat and methamidophos. In addition, the substrate not only can detect single component samples, but also can detect multiple types of mixtures rapidly.
Further, the plasmon nanometer superstructure in the step (4) is prepared into a SERS substrate, so that SERS detection can be performed on the object to be detected, and the molecules which can be detected by the SERS substrate comprise various molecules with SERS activity such as toluene, toxity, methylene blue, paraquat and the like.
Further, the molecules of the object to be detected are dripped on the surface of the assembled plasmon super structure before SERS detection.
In order to achieve the above object, the fourth technical scheme of the present invention is as follows: the application of the plasmon super structure can be directly placed in a photocatalysis reaction device to perform photocatalysis hydrogen production or photocatalysis 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 nano super structure which meets the actual requirement and has the property different from single particle nano particles.
2. The synthesized plasmon super-structure nano-particles can be prepared into SERS substrates for quick detection of SERS, and can be directly placed in a photocatalysis reaction device to directly carry out photocatalysis experiments.
3. The synthesized plasmon super-structure assembly can also be used for solar cells, plasmon enhanced photoelectric detectors, plasmon enhanced fluorescence and the like, and the method is simple and quick 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 of Au plasmonic superstructures;
FIG. 2 is a graph of Ag@SiO of example 1 2 The Au plasmon super structure is prepared into a SERS graph of the SERS substrate for rapidly detecting paraquat molecules;
FIG. 3 is a SERS diagram of a rapid detection of paraquat molecules by a common Au nanoparticle;
FIG. 4 is Ag@SiO prepared in example 2 2 -transmission electron microscopy and scanning electron microscopy images of au@cds plasmonic superstructures;
FIG. 5 is Ag@SiO prepared in example 2 2 And (3) directly placing the Au@CdS plasmon super structure in a photocatalytic reaction device to perform an activity data diagram of a photocatalytic hydrogen production experiment.
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 an activity data graph of the photocatalytic hydrogen production experiment in which the au@cds-au@pt plasmonic super structure prepared in example 3 is directly placed in a photocatalytic reaction device.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in more detail with reference to the accompanying drawings and specific embodiments, but the scope of the present invention is not limited to these embodiments.
The general assembly method of the plasmon nanometer super structure is characterized by comprising the following steps of:
(1) Synthesizing nano particles with plasmon activity;
(2) Immersing the nano particles synthesized in the step (1) in positively charged modification molecules to obtain modified positively charged particles;
(3) And (3) mixing the synthesized nano particles in the step (1) with the modified positively charged particles obtained in the step (2) to obtain the plasmon nano super structure composed of different materials.
And preparing the plasmon nano super structure into a SERS substrate, or directly placing the plasmon nano super structure into 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 super structure 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 nano particles with modified positively charged particles according to a volume ratio of 1:1.
The plasmon nanometer super structure is prepared by a general assembly method of the plasmon nanometer super structure.
The application of the plasmon nanometer super structure is used as a SERS substrate for rapidly detecting drug molecules, pollutants in the environment and pesticide residues.
The drug molecules comprise glacial toxins, 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.
And before the rapid detection, the molecules of the object to be detected are dripped on the surface of the assembled plasmon super-structure.
The SERS substrate is used for rapid detection of single component samples and multiple types of mixtures.
The application of the plasmon nanometer super structure is used for photocatalysis experiments including photocatalysis hydrogen production or photocatalysis oxygen production experiments.
Example 1
The invention relates to a general assembly method of a plasmon nanometer super structure, which is used for preparing Ag@SiO 2 The Au plasmon super-structure transmission electron microscope and the scanning electron microscope are shown in figure 1,
(1) The large-size Ag nano particles are synthesized by adopting a seed growth method: the specific operation steps are as follows:
1) Taking 2ml of HAuCl with mass fraction of 1% 4 Adding the mixture into 200ml of ultrapure water, adding 2ml of sodium citrate solution with the mass fraction of 1% after boiling the solution, and reacting for 30 minutes to obtain the Au seed with the size of 45 nm. The Au nano-particles with the synthetic size of 16nm only need to increase the amount of sodium citrate to 6 ml.
2) 10ml of Au seeds at 45nm are taken, 60ml of water is added, 1.2ml of sodium citrate and ascorbic acid solution with a molar concentration of 20mM are respectively added, and then 10ml of AgNO with a molar concentration of 10mM is added under normal temperature conditions 3 The solution can obtain Ag nano particles with the size of 120 nm.
(2) 60ml of the Ag nanoparticle obtained in the step (1) was added with 1ml of 3-aminopropyl trimethoxysilane with a molar concentration of 10mM and stirred for 15 minutes. Then adding 3.2ml of sodium silicate solution with the mass fraction of 0.54% into the mixture, and reacting for 30 minutes under the condition of 90 ℃ to obtain Ag@SiOwith the shell thickness of 2nm 2 And (3) nanoparticles.
(3) Taking Ag@SiO synthesized in the step (2) 2 10ml of nano particles are mixed with 0.02ml of polyallylamine hydrochloride with the molar concentration of 10mM for 10 minutes, 10ml of Au nano particles with the size of 16nm are added into the mixture, and the mixture is subjected to ultrasonic treatment for 30 minutes to obtain Ag@SiOI 2 -Au plasmonic superstructures.
(4) The Ag@SiO assembled in the step (3) is treated 2 And (3) centrifugally concentrating the Au plasmon super-structure, and then dripping the concentrated Au plasmon super-structure on a gold sheet for drying to prepare the SERS chip.
(5) Taking a piece of vegetable leaves with paraquat remained, wiping the surfaces of the vegetable leaves with a cotton swab soaked with alcohol, dipping the alcohol on the cotton swab into the alcohol obtained in the step (4) to obtain Ag@SiOO 2 On an Au plasmon super-structure SERS chip, a 785nm hand-held Raman spectrometer is used for testing to obtain the SERS light of FIG. 2A spectrogram. The substrate can be seen from the graph to be capable of well and rapidly detecting drugs, and meanwhile, the detection sensitivity of the substrate is surprisingly lower than 0.05ppb, so that the on-site detection requirement can be well met. The SERS enhancement substrate prepared by the method has more excellent SERS enhancement ability than the general Au nanoparticles (fig. 3).
Example 2
The invention relates to a general assembly method of a plasmon nanometer super structure, which is used for preparing Ag@SiO 2 The Au@CdS plasmon super-structure transmission electron microscope and scanning electron microscope images are shown in figure 4,
(1)Ag@SiO 2 synthetic reference example 1 of (c).
(2) The synthesis steps of Au@CdS are as follows: 30ml of Au nanoparticles of 16nm are taken and 3ml of a mixed solution of cadmium nitrate and L-cysteine with a molar concentration of 10mM is added. Then transferring the mixture into a reaction kettle to react for 6 hours at 130 ℃, thus obtaining the Au@CdS nano-particles.
(3) Taking the Ag@SiO synthesized in the step (1) 2 10ml of nanoparticle, 0.02ml of 4-dimethylaminopyridine was added thereto at a molar concentration of 20 mM.
(4) 10ml of Au@CdS nano particles prepared in the step (2) are taken and added 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 superstructures.
(5) The Ag@SiO assembled in the step (4) is treated 2 The Au@CdS plasmon super structure is directly placed in a photocatalytic reaction device to perform 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 to Au@CdS alone 2 The Au@CdS plasmon super structure shows extremely high photocatalytic activity.
Example 3
The general assembly method for the plasmon nanometer super structure prepares the Au@CdS-Au@Pt plasmon super structure transmission electron microscope and a scanning electron microscope image are shown in figure 6,
(1) Taking 2ml of HAuCl with mass fraction of 1% 4 Adding into 200ml of superAnd (3) adding 1.5ml of sodium citrate solution with the mass fraction of 1% into pure water after the solution is boiled, and reacting for 30 minutes to obtain Au nano-particles with the size of 55 nm.
(2) Taking 2ml of HAuCl with mass fraction of 1% 4 To 200ml of ultrapure water, 6ml of a sodium citrate solution having a mass fraction of 1% was added. Subsequently, 1ml of a sodium borohydride solution with a molar concentration of 38mM was rapidly added, and Au nanoparticles with a size of 5-8nm were obtained.
(3) 200ml of the 55nm Au nanoparticle obtained in the step (1) was taken, and 3ml of sodium citrate with a mass fraction of 1% and 5ml of CdCl with a molar concentration of 20mM were added thereto, respectively 2 The pH was adjusted to 10.2 with concentrated aqueous ammonia. And then transferring the reaction solution to 70 ℃ water bath for reaction for 6 hours, and obtaining the Au@CdS nano-particles.
(4) 30ml of the Au nanoparticle of 5-8nm prepared in the step (2) was taken, and 3ml of sodium citrate and 3ml of ascorbic acid were added thereto. Subsequently, 1ml of HPtCl with a mass fraction of 0.1% was slowly added dropwise thereto 4 The Au@Pt nano particles can be obtained.
(5) 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 into the mixture, mixing for 10 minutes, adding 10ml of the Au@Pt nano particles into the mixture, and carrying out ultrasonic treatment for 30 minutes to obtain the Au@CdS-Au@Pt plasmon super structure.
(6) And (3) directly placing the Au@CdS-Au@Pt plasmon super structure assembled in the step (5) in a photocatalysis reaction device to perform photocatalysis hydrogen production experiments, wherein the obtained photocatalysis hydrogen production data are shown in figure 7. From the figure, compared with pure Au@CdS, the Au@CdS-Au@Pt plasmon super-structure has a larger flexible selective assembly structure, so that the structure has excellent performances in the SERS detection field, the photocatalysis field, the photoelectric detection field, the solar cell field and the like. The preparation method is simple, convenient and quick. Meanwhile, the assembly can be batched. Therefore, the invention has great commercial application prospect.
The above embodiments are merely preferred embodiments of the present invention to illustrate the principles and the effects of the present invention, and are not intended to limit the invention. It should be noted that modifications to the above-described embodiments may be made by one skilled in the art without departing from the spirit and scope of the invention, and such modifications should also be considered as being within the scope of the invention.

Claims (9)

1. The general assembly method of the plasmon nanometer super structure is characterized by comprising the following steps of:
step (1) synthesizing nano particles with plasmon activity;
step (2) immersing the nano particles synthesized in the step (1) in positively charged modified molecules to obtain modified positively charged particles; the positively charged modified molecule is one of polyallylamine hydrochloride, 4-dimethylaminopyridine and hexadecyl trimethoxy ammonium chloride;
and (3) mixing the synthesized nano particles in the step (1) with the modified positively charged particles obtained in the step (2) to obtain the plasmon nano super structure, and preparing the plasmon nano super structure into a SERS substrate or directly placing the plasmon nano super structure in a photocatalysis reaction device.
2. The method of claim 1, wherein the nanoparticles in 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 plasmon nanometer super structure 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.
3. The method for universal assembly of plasmonic nano-superstructures of claim 1, wherein the synthesized nanoparticles of step (3) are mixed with modified positively charged particles in a volume ratio of 1:1.
4. A plasmonic nano-superstructure prepared by a general assembly method of plasmonic nano-superstructure as claimed in any one of claims 1 to 3.
5. The use of a plasmonic nano-superstructure according to claim 4 as a SERS substrate for the rapid detection of drug-like molecules, pollutants in the environment, pesticide residues.
6. The use of a plasmonic nano-superstructure according to claim 5, wherein the drug molecules comprise glaciers, K-powders, morphine, synthetic cannabinoids, fentanyl, the environmental pollutants comprise methylene blue, malachite green, methyl orange, and the pesticide residues comprise paraquat, methamidophos.
7. The use of a plasmonic nano-superstructure according to claim 5, wherein the rapid detection is preceded by a drop of the analyte molecule onto the assembled plasmonic super-structure surface.
8. The use of claim 5, wherein the SERS substrate is used for rapid detection of single component samples and multiple classes of mixtures.
9. The use of a plasmonic nano-superstructure according to claim 4, for photocatalytic experiments comprising photocatalytic hydrogen production or photocatalytic oxygen production experiments.
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