CN111636057A - Silver triangular nanoparticle array/single-layer graphene film composite material - Google Patents

Silver triangular nanoparticle array/single-layer graphene film composite material Download PDF

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CN111636057A
CN111636057A CN202010410257.XA CN202010410257A CN111636057A CN 111636057 A CN111636057 A CN 111636057A CN 202010410257 A CN202010410257 A CN 202010410257A CN 111636057 A CN111636057 A CN 111636057A
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layer
silver
copper foil
graphene film
film
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何辉
程建祥
范璐瑶
杨金彭
曾祥华
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Yangzhou University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • 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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    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/184—Preparation
    • C01B32/186—Preparation by chemical vapour deposition [CVD]
    • C—CHEMISTRY; METALLURGY
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    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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    • C23C14/20—Metallic material, boron or silicon on organic substrates
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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Abstract

The invention discloses a silver triangular nanoparticle array/single-layer graphene film composite material, which comprises the following steps: growing a single-layer graphene film on a copper foil; secondly, assembling a single-layer PS sphere template and transferring the single-layer PS sphere template to a copper foil attached with single-layer graphene; then, depositing silver by thermal evaporation, wherein a sample is kept still in the deposition process; and finally, removing the PS spheres to obtain the silver triangular nanoparticle array on the single-layer graphene film. According to the invention, the silver triangular nanoparticle array is controllably grown on the single-layer graphene, the respective advantages of the silver triangular nanoparticle array and the single-layer graphene and the synergistic effect of the silver triangular nanoparticle array and the single-layer graphene are combined, so that the strong SERS performance is achieved, the graphene is prevented from being damaged due to in-situ synthesis on the copper foil on which the graphene grows, and the integrity and the cleanness of the graphene are ensured.

Description

Silver triangular nanoparticle array/single-layer graphene film composite material
Technical Field
The invention belongs to the technical field of graphene-based composite nano materials, and particularly relates to a silver triangular nanoparticle array/single-layer graphene film composite material and a preparation method thereof.
Background
Graphene has many excellent properties, such as good electrical and thermal conductivity, good toughness, large specific surface area, etc., which make graphene-based composite materials exhibit many excellent characteristics. If the graphene is used as the carrier to load the nano particles, the performances of catalysis, sensing, energy storage and the like of the particles can be improved. For example, Surface Enhanced Raman Scattering (SERS) detection is adopted, the graphene and noble metal nano structure are compounded, the chemical enhancement of the graphene, the large physical enhancement of the noble metal, the large specific surface area and the strong adsorption capacity of the graphene can be fully utilized, and therefore the concentration limit of detection molecules is improved. As is well known, micron-sized graphene oxide sheets and composite materials thereof with noble metals are widely studied due to easier synthesis and high yield by a chemical liquid phase method. However, the results show that the particles grown on the graphene oxide are disordered and the composite material is generally in a powder state after being dried, which results in uneven SERS signals. To date, the Chemical Vapor Deposition (CVD) method for growing high-quality single-layer graphene films on copper foils has matured, and provides a good choice for exerting the advantages of graphene. However, in all of the methods using such thin films, the thin films are transferred to be used as device building units, but for graphene with a thickness of only atomic scale or several nanometers, the graphene cannot be contaminated or damaged in the transfer process, and the device performance is affected.
Disclosure of Invention
The invention aims to provide a method for controllably growing a triangular nanoparticle array on a single-layer graphene film.
The technical scheme for realizing the purpose of the invention is as follows: a silver triangular nanoparticle array/single-layer graphene film composite material and a preparation method thereof are disclosed, which comprises the following steps:
(1) growing a single-layer graphene film on a copper foil by CVD;
(2) preparing a single-layer PS ball colloid film on a glass slide;
(3) transferring the single-layer PS ball colloid film to a copper foil on which a graphene film grows to obtain a single-layer PS ball template/the graphene film/the copper foil;
(4) depositing silver on the single-layer PS spherical template/graphene film/copper foil by thermal evaporation, wherein a sample is kept static in the deposition process;
(5) and removing the PS spherical template after silver deposition to obtain the single-silver triangular nanoparticle array/single-layer graphene film composite material.
Preferably, the single-layer graphene film is grown by using the copper foil as a substrate and a catalyst by using normal-pressure CVD.
Specifically, annealing is carried out in a mixed atmosphere of hydrogen and argon to remove an oxide layer on the surface of the copper foil, then methane is introduced, a single-layer graphene film is grown by CVD, and finally the single-layer graphene film is cooled to room temperature under the protection of argon.
Preferably, a single-layer PS ball colloid film is prepared on the glass slide by adopting a gas-liquid-solid phase interface self-assembly method.
Specifically, a suspension (2.5 wt%) of PS spheres (with the diameter of 1 μm) and ethanol are ultrasonically and uniformly mixed according to the volume ratio of 1:1, a clean glass slide is taken, and a single-layer PS sphere colloid film is prepared on the glass slide by adopting a gas-liquid-solid phase interface self-assembly method.
Preferably, the slide glass loaded with the single-layer PS ball colloid film is slowly heated to 45 DEG°And (3) immersing the single-layer PS spherical colloid film into water, and transferring the single-layer PS spherical colloid film onto a copper foil on which a graphene film grows to obtain a single-layer PS spherical template/graphene film/copper foil.
Preferably, the obtained single-layer PS sphere template/graphene film/copper foil is subjected to heating treatment by using a thermostat so as to change the size of a triangular gap between spheres.
Specifically, the heating treatment temperature is 110 ℃, and the time is less than 20 min.
Preferably, the silver is deposited by thermal evaporation to a thickness of 100 nm.
Preferably, the PS sphere template after silver deposition is removed by soaking in an organic solvent.
Specifically, the organic solvent is CH2Cl2The soaking time is 10 min.
Compared with the prior art, the invention has two innovative points: (1) the composite material is new: the silver triangular nanoparticle array/single-layer graphene film composite material is unique in structure, combines the respective advantages of the silver triangular nanoparticles and the single-layer graphene and the synergistic effect of the silver triangular nanoparticles and the single-layer graphene, and has better photoelectric property than a single material. (2) The preparation method is novel: the graphene is synthesized in situ on the copper foil for growing the graphene, so that the integrity and the cleanness of the graphene are ensured.
The advantages of the invention are further illustrated in the following figures and detailed description.
Drawings
Fig. 1 is a schematic process route of preparing a silver triangular nanoparticle array/single-layer graphene film composite material according to the present invention.
FIG. 2 shows the morphology (b) of a 1 μmPS diameter ball template (a) and its silver evaporated sample used in example 1 of the present invention.
Fig. 3 shows the morphology of the silver triangular nanoparticle array/graphene film/copper foil prepared in example 1 of the present invention.
Fig. 4 is a SERS spectrum of the silver triangular nanoparticle array/graphene film/copper foil pair R6G molecule in example 1 of the present invention.
Fig. 5 shows the morphology of the silver triangular nanoparticle array/graphene film/copper foil prepared in example 2 of the present invention.
Detailed Description
The silver triangular nanoparticle array/single-layer graphene film prepared by the invention is characterized in that the silver triangular nanoparticle array can be controllably grown on the single-layer graphene, and the silver triangular nanoparticle array and the single-layer graphene are combined with the respective advantages of the silver triangular nanoparticle array and the single-layer graphene and the synergistic effect of the silver triangular nanoparticle array and the single-layer graphene, so that the silver triangular nanoparticle array/single-layer graphene film has strong SERS performance. Due to in-situ synthesis on the copper foil for growing the graphene, the damage of the graphene is avoided, and the integrity and the cleanness of the graphene are ensured.
The process scheme is schematically shown in figure 1. Firstly, growing a single-layer graphene film on a copper foil; secondly, assembling a single-layer PS sphere template and transferring the single-layer PS sphere template to a copper foil attached with single-layer graphene; then, depositing silver by thermal evaporation; and finally, removing the PS spheres to obtain the silver triangular nanoparticle array on the single-layer graphene film. The structural parameters of the array can be regulated and controlled through process parameters.
Example 1
(1) CVD growth of single-layer graphene film, putting copper foil (Alfa Aesar, 99.8%) with thickness of 25 μm into a tube furnace, annealing at 1000 ℃ for 30 min in mixed atmosphere of hydrogen (100 sccm) and argon (300 sccm), removing oxide on the surface of the copper foil, then introducing methane (10 sccm), after 30 min of growth, closing hydrogen and methane, cooling to room temperature under the protection of argon, and growing a single-layer graphene film on the copper foil, (2) synthesis of PS sphere template/single-layer graphene film/copper foil, PS sphere suspension (2.5 wt%) with diameter of 1 μm, and ethanol in volume ratio of 1:1, ultrasonic mixing, adding deionized water to clean glass slide to form a large-area thin-layer water film, taking about 0.1 mL of PS sphere mixed solution to the surface of the water film, assembling PS spheres into a large-area single-layer colloidal crystal film by self-evaporation at gas-liquid-solid interface, slowly immersing the glass slide into water at 45 ℃, the colloidal sphere film can float to the water surface, and evaporate silver by heat to deposit silver 100 nm by using heat evaporation equipment, and maintain vacuum degree of silver plating by evaporation, and evaporation of silver plating the silver plating equipment, wherein the silver-4pa. The sample remained stationary during deposition. (4) Finally, the silver-plated sample is in CH2Cl2And soaking in a solvent for 10min to remove the PS balls, thus obtaining the silver triangular nanoparticle array on the single-layer graphene.
The morphology and composition of the samples were characterized using a S-4800 Field Emission Scanning Electron Microscope (FESEM) from Hitachi, Japan, and the optical properties of the samples were analyzed using an In Via laser confocal Raman spectrometer from Renishwa, UK.
FIG. 2 shows the morphology of the PS sphere template with a diameter of 1 μm and the PS sphere template after silver evaporation in example 1. Fig. 2a shows the morphology of the PS spheres template before silver deposition, from which it can be seen that the PS spheres are regularly and sequentially arranged in close proximity with triangular gaps between the spheres. Fig. 2b shows the PS sphere template morphology after silver deposition, from which it can be seen that PS spheres exhibit hexagonal close arrangement, the PS sphere surface is a shell layer composed of silver nanoparticles, and silver nanoparticles are deposited at the triangular gaps.
Fig. 3 shows the morphology of the silver triangular nanoparticle array on the single-layer graphene film prepared in example 1 of the present invention. Fig. 3a shows the silver triangular nanoparticle array morphology obtained by removing the colloidal sphere template (fig. 2 b) after silver deposition. It can be observed from fig. 3a that after the PS spheres are removed, the triangular gaps between the original PS spheres form a silver triangular nanoparticle array after silver is deposited, the whole array is uniform and ordered, and the side length of a single triangular particle is about 200 nm. FIG. 3b is a SEM image of a silver triangular nanoparticle array with high magnification.
Fig. 4 is a SERS spectrum of the silver triangular nanoparticle array on single-layer graphene to R6G molecules in example 1 of the present invention. Curves 1 and 2 correspond to SERS spectra of the silver triangular nanoparticle array/single-layer graphene film and a continuous silver film (single-layer graphene/copper foil substrate, without PS spherical template, with the same thermal evaporation process parameters), respectively, and it can be seen that the silver triangular nanoparticle array/single-layer graphene film substrate has a greater enhancing capability, and the enhancing capability comes from two aspects: the method has the advantages that the large physical enhancement of the silver triangular nanoparticles and the large chemical enhancement of the graphene are combined to enhance (multiplication relation); and secondly, the adsorption capacity of the graphene to aromatic molecules containing benzene rings is improved through pi-pi interaction between the graphene and the molecules.
Example 2
Other steps and process conditions were the same as in example 1. The difference is that before the step (3), the two single-layer PS sphere templates obtained in the step (2) are respectively subjected to heating treatment at 110 ℃/10min and 110 ℃/20min, so as to respectively obtain the silver triangular nanoparticle array/single-layer graphene film/copper foil morphology under the condition of 110 ℃/10min (figure 5 a) and the silver triangular nanoparticle array/single-layer graphene film/copper foil morphology under the heating condition of 110 ℃/20min (figure 5 b).
Comparing fig. 5a and 5b, and referring to fig. 3, we can find that the PS sphere template heat treatment has a significant effect on the triangle size, and as the heating time of the PS sphere template before depositing silver is increased, the size of the finally obtained silver triangle nanoparticle is also decreased. Therefore, the size of the silver triangular nanoparticles can be regulated and controlled by changing the heating condition of the PS sphere template before silver deposition.
From the above results, it can be seen that: the method is feasible for preparing the triangular silver nanoparticle array on the single-layer graphene film grown by CVD in situ, has the advantages of no pollution, adjustable silver size, good reproducibility, easiness in mass synthesis and the like, and is expected to be practical. SERS tests show that the graphene-based composite material has more excellent performance.

Claims (10)

1. A preparation method of a silver triangular nanoparticle array/single-layer graphene film composite material is characterized by comprising the following steps:
(1) growing a single-layer graphene film on a copper foil by CVD;
(2) preparing a single-layer PS ball colloid film on a glass slide;
(3) transferring the single-layer PS ball colloid film to a copper foil on which a graphene film grows to obtain a single-layer PS ball template/the graphene film/the copper foil;
(4) depositing silver on the single-layer PS spherical template/graphene film/copper foil by thermal evaporation, wherein a sample is kept static in the deposition process;
(5) and removing the PS spherical template after silver deposition to obtain the single-silver triangular nanoparticle array/single-layer graphene film composite material.
2. The method of claim 1, wherein the CVD growth of the single-layer graphene film on the copper foil is performed by: annealing in a mixed atmosphere of hydrogen and argon to remove an oxide layer on the surface of the copper foil, introducing methane, growing a single-layer graphene film by adopting CVD (chemical vapor deposition), and cooling to room temperature under the protection of argon.
3. The method of claim 1, wherein the monolayer PS sphere colloid film is prepared on the glass slide using a gas-liquid-solid phase interface self-assembly method.
4. The method of claim 3, wherein 2.5 wt% PS sphere suspension and ethanol are ultrasonically and uniformly mixed according to a volume ratio of 1:1, a clean glass slide is taken, and a single-layer PS sphere colloid film is prepared on the glass slide by adopting a gas-liquid-solid phase interface self-assembly method.
5. The method of claim 1, wherein the slide bearing the monolayer of PS sphere colloid film is slowly cooled to 45 ° f°And (3) immersing the single-layer PS spherical colloid film into water, and transferring the single-layer PS spherical colloid film onto a copper foil on which a graphene film grows to obtain a single-layer PS spherical template/graphene film/copper foil.
6. The method of claim 1, wherein the obtained single-layer PS sphere template/graphene film/copper foil is subjected to a heat treatment.
7. The method of claim 6, wherein the heat treatment temperature is 110 ℃ for <20 min.
8. The method of claim 1, wherein the silver is deposited by thermal evaporation to a thickness of 100 nm.
9. The method of claim 1, wherein the PS sphere template after silver deposition is removed by soaking in an organic solvent.
10. The silver triangular nanoparticle array/single layer graphene thin film composite prepared by the method of any one of claims 1-9.
CN202010410257.XA 2020-05-15 2020-05-15 Silver triangular nanoparticle array/single-layer graphene film composite material Pending CN111636057A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102180438A (en) * 2011-03-28 2011-09-14 中国科学院光电技术研究所 Manufacturing method of tunable triangular metal nano particle array structure
CN104528709A (en) * 2015-01-23 2015-04-22 华南理工大学 Preparation method of graphene having high Raman scattering intensity

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102180438A (en) * 2011-03-28 2011-09-14 中国科学院光电技术研究所 Manufacturing method of tunable triangular metal nano particle array structure
CN104528709A (en) * 2015-01-23 2015-04-22 华南理工大学 Preparation method of graphene having high Raman scattering intensity

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
彭莉岚: "石墨烯-金属复合纳米结构的制备及其表面等离激元特性研究", 《中国优秀硕士学位论文全文数据库（电子期刊） 工程科技Ⅰ辑》 *

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Application publication date: 20200908