CN111485210A - graphene/Au composite material with enhanced SERS activity - Google Patents
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- 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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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
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- 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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- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
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- 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
- C23C14/34—Sputtering
- C23C14/3471—Introduction of auxiliary energy into the plasma
- C23C14/3478—Introduction of auxiliary energy into the plasma using electrons, e.g. triode sputtering
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Abstract
The invention relates to a graphene/Au composite material which comprises a two-dimensional structure array template formed on a silicon chip by utilizing polystyrene microsphere arrangement, Au and graphene are alternately deposited on the template, and the deposition thicknesses of the Au and the graphene are respectively 50-100nm and 2-10 nm. The method takes a polystyrene colloid ball template with original micron-scale or micro-nanometer-scale roughness as a substrate, and an Au layer and a graphene layer are respectively deposited by magnetron sputtering and electron cyclotron plasma sputtering, so that the signal intensity of the detected probe molecules can be obviously enhanced, the dependence of the detected probe molecules on an excitation light source is overcome, and the Raman analysis application range of the detected probe molecules is widened.
Description
Technical Field
The invention relates to the technical field of surface enhanced Raman scattering spectroscopy (SERS) detection, and particularly relates to a graphene/Au composite material.
Background
The surface-enhanced raman scattering spectroscopy detection technology is based on the raman effect, and is developed based on the near-field enhancement property of Surface Plasmon Resonance (SPR). SERS is a common analysis technology, has the advantages of high sensitivity, strong selectivity, good repeated stability and the like, and has wide application in the fields of environmental science, bioscience, trace analysis and the like.
In a specific SERS assay, the resonance frequency of the surface plasmon varies with the kind, size, shape, etc. of the metal nanoparticle, and thus, a surface enhanced raman signal can be obtained by controlling these factors. Among them, the roughness of the substrate surface of the placed analyte is an important factor for the generation of surface plasmon and the enhancement of raman signal. Accordingly, a large number of researchers have developed various techniques for roughening the surface of a substrate using nanotechnology to provide nanostructures, such as nanoscale pillars, linear fracture surfaces, or nanoparticles. Although these methods can control the size and shape of particles well, high production costs are required and there are limitations to large-scale implementation.
In addition, in practical applications, users also find that the dependence on an excitation light source is strong only by virtue of the surface plasmon resonance property of the noble metal nanoparticle, so that the application limitation is serious.
Therefore, the invention aims to provide the SERS substrate with low production cost and wide application range.
Disclosure of Invention
Aiming at the problems of an SERS substrate used in the existing SERS detection technology, the invention provides a graphene/Au composite material with enhanced SERS activity, wherein Au and graphene are sequentially deposited on the surface of a polystyrene colloid ball template directly by a sputtering method to obtain the graphene/Au composite material.
Namely, the graphene/Au composite material with enhanced SERS activity provided by the invention comprises a two-dimensional structure array template formed on a silicon chip by arranging polystyrene microspheres, Au and graphene are sequentially deposited on the template, and the deposition thicknesses of the Au and the graphene are respectively 50-100nm and 2-10 nm.
The preparation method of the graphene/Au composite material with enhanced SERS activity comprises the following steps:
firstly, preparing a two-dimensional periodic structure array by using polystyrene microspheres through a self-assembly technology to obtain a polystyrene colloid sphere template;
secondly, preparing an Au layer by magnetron sputtering;
and thirdly, depositing the graphene layer by electron cyclotron plasma sputtering.
Wherein, the first step is specifically as follows:
(1) soaking the silicon wafer in 1-3% sodium dodecyl sulfate solution for 12-36 hours to make the silicon wafer have hydrophilic property;
(2) another silicon slice is taken and cut to 2 × 2cm2After the size is increased, putting the mixture into a mixed solution of ammonia water, hydrogen peroxide and deionized water with the volume ratio of 1:2:6, heating at the temperature of 250-350 ℃ for 5-10min, cooling, sequentially adding deionized water and ethanol for ultrasonic treatment, and then putting the mixture into an ethanol solution for later use;
(3) mixing an ethanol solution of polystyrene microspheres according to the volume ratio of 1: 0.5-2 of the polystyrene microspheres to the ethanol solution, and then carrying out ultrasonic treatment to uniformly disperse the polystyrene microspheres;
(4) dropping the solution of the polystyrene ethanol on a hydrophilic silicon wafer, spreading the liquid uniformly, inserting the liquid into water in an inclined manner, and diffusing the liquid on the water surface to form a single-layer closely-arranged structural array;
(5) and fishing out the liquid surface by using the cleaned silicon wafer after the liquid surface is static, washing away the redundant water by using filter paper, and placing the silicon wafer in an inclined mode until the silicon wafer is completely dried.
Wherein, the second step is specifically as follows:
placing the silicon chip with polystyrene bead array in magnetron sputtering cavity, vacuumizing to make background air pressure reach 10- 4Below Pa, setting the flow rate of argon as working gas to make the working pressure reach 10-2And carrying out magnetron sputtering on the Au layer after Pa, wherein the sputtering power is 50W, and the sputtering time is 10-30 min.
Wherein, the third step is specifically as follows:
transferring the polystyrene colloid ball template with the Au layer deposited in the second step into an electron cyclotron plasma sputtering deposition chamber through a transition chamber, and vacuumizing to 3 × 10-4Introducing argon gas at Pa to maintain the gas pressure at 1 × 10-2Pa; applying current to a magnetic coil, introducing microwaves, generating argon plasma through the coupling action of a magnetic field and the microwaves, applying target bias voltage of-200V to-500V, bombarding a carbon target, applying bias voltage of +100V to +200V to an Au layer, and performing sputtering deposition for 1-5 min.
The invention has the following beneficial effects:
1. the polystyrene microsphere is utilized to prepare a two-dimensional periodic structure array through a self-assembly technology, and a polystyrene colloid sphere template is obtained to be used as a substrate for subsequent sputtering deposition, so that the obtained graphene/Au composite material has original micron-scale or micro-nanometer-scale roughness, and the signal intensity of detected probe molecules can be enhanced.
2. The subsequent Au layer and graphene layer are both subjected to sputtering deposition, the quality and thickness of the film layer are controllable, the method is simple and convenient, batch preparation is easy, and the cost is low.
3. Through electron cyclotron plasma sputtering deposition, a stable graphene layer can be obtained on the surface of the Au layer, and the graphene layer is high in adhesion stability to the Au layer. And the deposited graphene layer is graphene nanocrystalline, so that the graphene nano-crystal has excellent conductivity and can further remarkably enhance the signal intensity of the detected probe molecules.
4. Due to the composite action of the graphene layer and Au, the substrate can realize Raman enhancement under various excitation wavelengths, the dependence of the substrate on an excitation light source is overcome to a certain extent, and the Raman analysis application range is widened.
Detailed Description
The present invention will be described in detail with reference to specific examples. Of course, the described embodiments are merely inventive in part, and not in whole. Other examples, which would be obtained by one of ordinary skill in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
A graphene/Au composite material with enhanced SERS activity is prepared by the following steps:
(1) soaking the silicon wafer in 1% sodium dodecyl sulfate solution for 36 hr to make it have hydrophilic characteristic;
(2) another silicon slice is taken and cut to 2 × 2cm2After the size is increased, putting the mixture into a mixed solution of ammonia water, hydrogen peroxide and deionized water with the volume ratio of 1:2:6, heating the mixture at 250 ℃ for 10min, cooling the mixture, sequentially adding deionized water and ethanol, performing ultrasonic treatment, and then putting the mixture into an ethanol solution for later use;
(3) mixing an ethanol solution of polystyrene microspheres according to the volume ratio of 1:2 of the polystyrene microspheres to the ethanol solution, and then carrying out ultrasonic treatment to uniformly disperse the polystyrene microspheres;
(4) dropping the solution of the polystyrene ethanol on a hydrophilic silicon wafer, spreading the liquid uniformly, inserting the liquid into water in an inclined manner, and diffusing the liquid on the water surface to form a single-layer closely-arranged structural array;
(5) after the liquid level is static, fishing out the silicon wafer which is cleaned, washing away the redundant water by using filter paper, and placing the silicon wafer in an inclined way until the silicon wafer is completely dried;
(6) placing the silicon chip with polystyrene bead array in magnetron sputtering cavity, vacuumizing to make background air pressure reach 10-4Below Pa, setting the flow rate of argon as working gas to make the working pressure reach 10-2Carrying out magnetron sputtering on the Au layer after Pa, wherein the sputtering power is 50W, and the sputtering time is 15 min;
(7) transferring the polystyrene colloid ball template with the Au layer deposited in the second step into an electron cyclotron plasma sputtering deposition chamber through a transition chamber, and vacuumizing to 3 × 10-4Introducing argon gas at Pa to maintain the gas pressure at 1 × 10-2Pa; applying current to the magnetic coil and introducing microwaves, generating argon plasma through the coupling action of the magnetic field and the microwaves, applying a target bias of-200V to bombard the carbon target, applying a bias of +100V to the Au layer, and performing sputtering deposition for 1 min.
Example 2
A graphene/Au composite material with enhanced SERS activity is prepared by the following steps:
(1) soaking a silicon wafer in a 3% sodium dodecyl sulfate solution for 12 hours to ensure that the silicon wafer has hydrophilic characteristics;
(2) another silicon slice is taken and cut to 2 × 2cm2After the size is increased, putting the mixture into a mixed solution of ammonia water, hydrogen peroxide and deionized water with the volume ratio of 1:2:6, heating the mixture for 5min at 350 ℃, cooling the mixture, sequentially adding deionized water and ethanol, performing ultrasonic treatment, and then putting the mixture into an ethanol solution for later use;
(3) mixing an ethanol solution of polystyrene microspheres according to the volume ratio of the polystyrene spheres to the ethanol solution of 1:0.5, and then carrying out ultrasonic treatment to uniformly disperse the polystyrene microspheres;
(4) dropping the solution of the polystyrene ethanol on a hydrophilic silicon wafer, spreading the liquid uniformly, inserting the liquid into water in an inclined manner, and diffusing the liquid on the water surface to form a single-layer closely-arranged structural array;
(5) after the liquid level is static, fishing out the silicon wafer which is cleaned, washing away the redundant water by using filter paper, and placing the silicon wafer in an inclined way until the silicon wafer is completely dried;
(6) placing the silicon chip with polystyrene bead array in magnetron sputtering cavity, vacuumizing to make background air pressure reach 10-4Below Pa, setting the flow rate of argon as working gas to make the working pressure reach 10-2Carrying out magnetron sputtering on the Au layer after Pa, wherein the sputtering power is 50W, and the sputtering time is 30 min;
(7) transferring the polystyrene colloid ball template with the Au layer deposited in the second step into an electron cyclotron plasma sputtering deposition chamber through a transition chamber, and vacuumizing to 3 × 10-4Introducing argon gas at Pa to maintain the gas pressure at 1 × 10-2Pa; applying current to the magnetic coil and introducing microwaves, generating argon plasma through the coupling action of the magnetic field and the microwaves, applying a target bias of-500V to bombard the carbon target, applying a bias of +200V to the Au layer, and performing sputtering deposition for 3 min.
Example 3
A graphene/Au composite material with enhanced SERS activity is prepared by the following steps:
(1) soaking the silicon wafer in 2% sodium dodecyl sulfate solution for 20 hours to make the silicon wafer have hydrophilic characteristic;
(2) another silicon slice is taken and cut to 2 × 2cm2After the size is increased, putting the mixture into a mixed solution of ammonia water, hydrogen peroxide and deionized water with the volume ratio of 1:2:6, heating the mixture at 300 ℃ for 7min, cooling the mixture, sequentially adding deionized water and ethanol, performing ultrasonic treatment, and then putting the mixture into an ethanol solution for later use;
(3) mixing an ethanol solution of polystyrene microspheres according to the volume ratio of 1:1 of the polystyrene microspheres to the ethanol solution, and then carrying out ultrasonic treatment to uniformly disperse the polystyrene microspheres;
(4) dropping the solution of the polystyrene ethanol on a hydrophilic silicon wafer, spreading the liquid uniformly, inserting the liquid into water in an inclined manner, and diffusing the liquid on the water surface to form a single-layer closely-arranged structural array;
(5) after the liquid level is static, fishing out the silicon wafer which is cleaned, washing away the redundant water by using filter paper, and placing the silicon wafer in an inclined way until the silicon wafer is completely dried;
(6) placing the silicon chip with polystyrene bead array in magnetron sputtering cavity, vacuumizing to make background air pressure reach 10-4Below Pa, setting the flow rate of argon as working gas to make the working pressure reach 10-2Carrying out magnetron sputtering on the Au layer after Pa, wherein the sputtering power is 50W, and the sputtering time is 10 min;
(7) transferring the polystyrene colloid ball template with the Au layer deposited in the second step into an electron cyclotron plasma sputtering deposition chamber through a transition chamber, and vacuumizing to 3 × 10-4Introducing argon gas at Pa to maintain the gas pressure at 1 × 10-2Pa; applying current to the magnetic coil, introducing microwave, generating argon plasma through the coupling action of the magnetic field and the microwave, applying a target bias of-300V to bombard the carbon target, applying a bias of +150V to the Au layer, and performing sputtering deposition for 5 min.
Example 4
A graphene/Au composite material with enhanced SERS activity is prepared by the following steps:
(1) soaking the silicon wafer in 2% sodium dodecyl sulfate solution for 28 hours to make the silicon wafer have hydrophilic characteristic;
(2) another silicon slice is taken and cut to 2 × 2cm2After the size is increased, putting the mixture into a mixed solution of ammonia water, hydrogen peroxide and deionized water with the volume ratio of 1:2:6, heating the mixture at 280 ℃ for 8min, cooling the mixture, sequentially adding deionized water and ethanol, performing ultrasonic treatment, and then putting the mixture into an ethanol solution for later use;
(3) mixing an ethanol solution of polystyrene microspheres according to the volume ratio of 1:1.5 of the polystyrene spheres to the ethanol solution, and then carrying out ultrasonic treatment to uniformly disperse the ethanol solution;
(4) dropping the solution of the polystyrene ethanol on a hydrophilic silicon wafer, spreading the liquid uniformly, inserting the liquid into water in an inclined manner, and diffusing the liquid on the water surface to form a single-layer closely-arranged structural array;
(5) after the liquid level is static, fishing out the silicon wafer which is cleaned, washing away the redundant water by using filter paper, and placing the silicon wafer in an inclined way until the silicon wafer is completely dried;
(6) placing the silicon chip with polystyrene bead array in magnetron sputtering cavity, vacuumizing to make background air pressure reach 10-4Below Pa, setting the flow rate of argon as working gas to make the working pressure reach 10-2Carrying out magnetron sputtering on the Au layer after Pa, wherein the sputtering power is 50W, and the sputtering time is 25 min;
(7) transferring the polystyrene colloid ball template with the Au layer deposited in the second step into an electron cyclotron plasma sputtering deposition chamber through a transition chamber, and vacuumizing to 3 × 10-4Introducing argon gas at Pa to maintain the gas pressure at 1 × 10-2Pa; applying current to the magnetic coil and introducing microwaves, generating argon plasma through the coupling action of the magnetic field and the microwaves, applying a target bias of 400V to bombard the carbon target, applying a bias of 100V to the Au layer, and performing sputtering deposition for 2 min.
The graphene/Au composite material of the present invention was described above. It should be noted that the content of the present invention, other examples obtained by a person of ordinary skill in the art without any creative effort, is covered within the protection scope of the present invention.
Claims (6)
1. A graphene/Au composite material with enhanced SERS activity comprises a two-dimensional structure array template formed on a silicon chip by utilizing polystyrene microsphere arrangement, Au and graphene are sequentially deposited on the template, and the deposition thicknesses of the Au and the graphene are 50-100nm and 2-10nm respectively.
2. The graphene/Au composite with enhanced SERS activity of claim 1, wherein Au is deposited by magnetron sputtering and graphene is deposited by electron cyclotron plasma sputtering.
3. The method for preparing the graphene/Au composite material with enhanced SERS activity as claimed in claim 1, comprising:
firstly, preparing a two-dimensional periodic structure array by using polystyrene microspheres through a self-assembly technology to obtain a polystyrene colloid sphere template;
secondly, preparing an Au layer by magnetron sputtering;
and thirdly, depositing the graphene layer by electron cyclotron plasma sputtering.
4. The method according to claim 3, wherein step one is specifically:
(1) soaking the silicon wafer in 1-3% sodium dodecyl sulfate solution for 12-36 hours to make the silicon wafer have hydrophilic property;
(2) another silicon slice is taken and cut to 2 × 2cm2After the size is increased, putting the mixture into a mixed solution of ammonia water, hydrogen peroxide and deionized water with the volume ratio of 1:2:6, heating at the temperature of 250-350 ℃ for 5-10min, cooling, sequentially adding deionized water and ethanol for ultrasonic treatment, and then putting the mixture into an ethanol solution for later use;
(3) mixing an ethanol solution of polystyrene microspheres according to the volume ratio of 1: 0.5-2 of the polystyrene microspheres to the ethanol solution, and then carrying out ultrasonic treatment to uniformly disperse the polystyrene microspheres;
(4) dropping the solution of the polystyrene ethanol on a hydrophilic silicon wafer, spreading the liquid uniformly, inserting the liquid into water in an inclined manner, and diffusing the liquid on the water surface to form a single-layer closely-arranged structural array;
(5) and fishing out the liquid surface by using the cleaned silicon wafer after the liquid surface is static, washing away the redundant water by using filter paper, and placing the silicon wafer in an inclined mode until the silicon wafer is completely dried.
5. The preparation method according to claim 3, wherein the second step is specifically:
placing the silicon chip with polystyrene bead array in magnetron sputtering cavity, vacuumizing to make background air pressure reach 10-4Below Pa, setting the flow rate of argon as working gas to make the working pressure reach 10-3And carrying out magnetron sputtering on the Au layer after Pa, wherein the sputtering power is 50W, and the sputtering time is 10-30 min.
6. The preparation method according to claim 3, wherein the third step is specifically:
will be passedTransferring the polystyrene colloid ball template with the Au layer deposited in the step two into an electron cyclotron plasma sputtering deposition chamber through a transition chamber, and vacuumizing to 3 × 10-4Introducing argon gas at Pa to maintain the gas pressure at 1 × 10-2Pa; applying current to a magnetic coil, introducing microwaves, generating argon plasma through the coupling action of a magnetic field and the microwaves, applying target bias voltage of-200V to-500V, bombarding a carbon target, applying bias voltage of +100V to +200V to an Au layer, and performing sputtering deposition for 1-5 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112763473A (en) * | 2020-12-07 | 2021-05-07 | 福建师范大学 | Urea-modified paper-based SERS substrate and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103512875A (en) * | 2013-09-23 | 2014-01-15 | 武汉大学 | Preparation method for surface-enhanced Raman spectrum compound substrate |
| CN104528709A (en) * | 2015-01-23 | 2015-04-22 | 华南理工大学 | Preparation method of graphene having high Raman scattering intensity |
| EP3073251A1 (en) * | 2015-03-24 | 2016-09-28 | Agri-Food and Biosciences Institute | A multi-layered substrate for spectroscopy and manufacturing process thereof |
| CN107313046A (en) * | 2017-05-12 | 2017-11-03 | 北京邮电大学 | A kind of SERS substrates and preparation method thereof |
| CN110136996A (en) * | 2019-05-31 | 2019-08-16 | 西安理工大学 | The manufacturing method of micro super capacitor based on graphene nano-crystal carbon film electrodes |
-
2020
- 2020-04-29 CN CN202010359308.0A patent/CN111485210A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103512875A (en) * | 2013-09-23 | 2014-01-15 | 武汉大学 | Preparation method for surface-enhanced Raman spectrum compound substrate |
| CN104528709A (en) * | 2015-01-23 | 2015-04-22 | 华南理工大学 | Preparation method of graphene having high Raman scattering intensity |
| EP3073251A1 (en) * | 2015-03-24 | 2016-09-28 | Agri-Food and Biosciences Institute | A multi-layered substrate for spectroscopy and manufacturing process thereof |
| CN107313046A (en) * | 2017-05-12 | 2017-11-03 | 北京邮电大学 | A kind of SERS substrates and preparation method thereof |
| CN110136996A (en) * | 2019-05-31 | 2019-08-16 | 西安理工大学 | The manufacturing method of micro super capacitor based on graphene nano-crystal carbon film electrodes |
Non-Patent Citations (2)
| Title |
|---|
| LIFENG HANG ET AL.: "Copper nanoparticle@graphene composite arrays and their enhanced catalytic performance", 《ACTA MATERIALIA》 * |
| 杨景海等: "自组装单层和多层衬底制备纳米碗的对比研究", 《吉林师范大学学报( 自然科学版)》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112763473A (en) * | 2020-12-07 | 2021-05-07 | 福建师范大学 | Urea-modified paper-based SERS substrate and preparation method thereof |
| CN112763473B (en) * | 2020-12-07 | 2023-07-07 | 福建师范大学 | Urea-modified paper-based SERS substrate and preparation method thereof |
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