CN114411152B - AFM nano milling and chemical corrosion processing-based surface enhanced Raman substrate preparation method - Google Patents

AFM nano milling and chemical corrosion processing-based surface enhanced Raman substrate preparation method Download PDF

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CN114411152B
CN114411152B CN202210023523.2A CN202210023523A CN114411152B CN 114411152 B CN114411152 B CN 114411152B CN 202210023523 A CN202210023523 A CN 202210023523A CN 114411152 B CN114411152 B CN 114411152B
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gold
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CN114411152A (en
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耿延泉
王继强
闫永达
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Harbin Institute of Technology
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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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/30—Acidic compositions for etching other metallic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23C—MILLING
    • B23C3/00—Milling particular work; Special milling operations; Machines therefor
    • 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
    • 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
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • 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
    • 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
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • 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
    • C23C14/54—Controlling or regulating the coating process
    • C23C14/542—Controlling the film thickness or evaporation rate
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5873—Removal of material
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/44—Compositions for etching metallic material from a metallic material substrate of different composition
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons

Abstract

The invention discloses a preparation method of a surface-enhanced Raman substrate based on AFM nano milling and chemical corrosion processing, which comprises the following steps: sequentially preparing a gold film, a silver film and a gold film on the surface of a substrate by adopting a magnetron sputtering method; the step (2) is based on a nanometer milling system of AFM, and periodic nanometer structures are nanometer milled on the surface of the gold-silver-gold composite film; step (3) putting the periodic nanostructure obtained by nano milling into concentrated nitric acid, and chemically corroding a silver layer exposed at the edge of the periodic nanostructure, thereby preparing a hollow nano cavity; and (4) taking the chemically corroded composite film periodic array structure with the nano cavity as a Raman enhancement substrate. The method can be used for preparing the Raman enhancement substrate with controllable structural feature size, adjustable plasma resonance and good consistency.

Description

AFM nano milling and chemical corrosion processing-based surface enhanced Raman substrate preparation method
Technical Field
The invention relates to a preparation method of a Raman enhanced substrate, in particular to a preparation method of a surface enhanced Raman substrate based on AFM nano milling and chemical corrosion processing.
Background
The Raman detection is used as one of the label-free detection methods, has the advantages of high detection precision, high efficiency, simplicity in operation and the like, and is widely applied to the fields of biomedicine, food health, medicinal chemistry and the like. However, since raman signals are usually extremely weak, it is necessary to increase the signal intensity and thus the detection sensitivity by means of the enhancement substrate. Noble metal materials with nanostructures, such as gold, silver, etc., have been shown to be preferred materials for preparing raman-enhanced substrates, because of their ability to achieve strong surface plasmon resonance and thus enhanced raman signals.
At present, various methods have been used for preparing a noble metal raman reinforced substrate with a nanostructure, such as a colloid substitution method, a chemical etching method, a laser processing method, etc., however, the above methods have certain limitations. The substrate structure prepared by the colloid replacement method and the chemical corrosion method has poor consistency and repeatability, and the characteristic size of the target nanostructure cannot be accurately obtained. The characteristic size of the substrate structure prepared by the laser processing method is relatively large, and the reinforced substrate with the nano structure of about 10nm cannot be obtained by processing. In addition, the raman enhancement substrate cannot regulate and control the plasmon resonance by changing the characteristic size, and the raman enhancement effect cannot be further improved under the condition of fixed wavelength of the detection laser. Therefore, the preparation of raman-enhanced substrates with controllable feature sizes, good structural stability, high reproducibility and consistency becomes of great importance.
Disclosure of Invention
The invention aims to provide a preparation method of a surface-enhanced Raman substrate based on AFM nano milling and chemical corrosion processing, which can be used for rapidly and efficiently preparing a Raman enhanced substrate with controllable structural feature size, adjustable plasma resonance and good consistency.
The invention aims at realizing the following technical scheme:
a preparation method of a surface-enhanced Raman substrate based on AFM nano milling and chemical corrosion processing comprises the following steps:
sequentially preparing a gold film, a silver film and a gold film on the surface of a substrate by adopting a magnetron sputtering method, wherein:
the substrate is silicon dioxide or silicon and the like;
the thicknesses of the gold film, the silver film and the gold film are respectively 40-60 nm, 10-15 nm and 10-20 nm;
the power of the gold-plating film is 14W, the speed is 0.04nm/s, the power of the silver-plating film is 9W, and the speed is 0.025nm/s;
the step (2) is based on an AFM nanometer milling system, and nanometer milling periodic nanometer structures are formed on the surface of the gold-silver-gold composite film, wherein:
the width of the nano milling process is 280-490 nm, the rotation frequency of the probe relative to the sample is 500Hz, the processing speed is 0.66-53 mu m/s, and the feeding amount is 1.3-106 nm;
step (3) putting the periodic nanostructure obtained by nano milling into concentrated nitric acid, and chemically corroding a silver layer exposed at the edge of the periodic nanostructure to prepare a hollow nano cavity, wherein:
the mass fraction of the concentrated nitric acid is 65%;
the chemical etching time is 2min;
and (4) taking the chemically corroded composite film periodic array structure with the nano cavity as a Raman enhancement substrate.
Compared with the prior art, the invention has the following advantages:
1. the invention mainly prepares the Raman enhanced substrate with controllable characteristic size of the nanostructure by combining Atomic Force Microscope (AFM) nanometer milling processing and chemical etching processing.
2. The period of the Raman enhanced substrate prepared by the invention is determined by the width of nano milling, the plasma resonance of the substrate can be regulated and controlled, and meanwhile, the strength of Raman detection signals can be greatly improved by taking the nano cavity structure as an enhanced 'hot spot'.
Drawings
FIG. 1 is a flow chart of AFM nano milling and chemical etching process for preparing a Raman enhanced substrate; (a) Magnetron sputtering method on SiO 2 Gold plating on a substrate, (b) silver plating by a magnetron sputtering method, (c) gold plating by a magnetron sputtering method, (d) gold-silver-Jin Duoceng film TEM drawing, (e) nano milling a periodic nano structure on the surface of a gold-silver-gold multilayer film, (f) chemical etching of an intermediate silver layer by 65% nitric acid to obtain a nano cavity structure, and (G) Raman detection of rhodamine 6G by a Raman substrate;
FIG. 2 is a schematic illustration of a nano-milling process;
FIG. 3 is a schematic diagram of a periodic nanostructure and a microcavity structure, (a) a nano-milled periodic nanostructure, (b) a cross-sectional view of the periodic structure, (c) a microcavity SEM;
fig. 4 shows the results of surface enhanced raman scattering experiments, (a) periodic nanostructure dark field scattering spectra, (b) raman test results.
Detailed Description
The following description of the present invention is provided with reference to the accompanying drawings, but is not limited to the following description, and any modifications or equivalent substitutions of the present invention should be included in the scope of the present invention without departing from the spirit and scope of the present invention.
The invention provides a preparation method of a surface-enhanced Raman substrate based on AFM (atomic force microscope) nano milling and chemical corrosion processing, which comprises the steps of firstly, sequentially plating a gold film, a silver film and a gold film on the surface of silicon dioxide by utilizing a magnetron sputtering method, then, carrying out nano milling on a periodic array structure with variable width on the surface of the plated film, and carrying out chemical corrosion on the silver film with exposed nano structure edges by adopting concentrated nitric acid with the mass fraction of 65% to obtain a nano cavity, wherein the nano cavity is used as a 'hot spot' structure of the Raman-enhanced substrate. And finally, taking the chemically corroded composite film periodic array structure with the nano cavity as a Raman enhancement substrate. As shown in fig. 1, the method mainly comprises the following four steps:
step (1) magnetron sputtering method is used for preparing SiO 2 Substrate gold-silver-gold composite film:
the noble metals gold and silver are easier to generate plasmon effect, so that Raman signals are greatly enhanced, and a magnetron sputtering method is adopted to sequentially prepare a gold film, a silver film and a gold film on the surface of silicon dioxide, wherein the thickness of a film coating is determined by the film coating time and the beam current. The film plating equipment is provided with an automatic film thickness monitor, and can realize real-time monitoring of film thickness in the film plating process so as to ensure the thickness of the film plating. In the present invention, the thicknesses of the gold film, the silver film and the gold film are 50nm, 12nm and 10nm, respectively.
Step (2) nano milling processing periodic nano structure on the surface of the gold-silver-gold composite film:
FIG. 2 is a schematic diagram of an AFM-based nano-milling system. The processing system mainly comprises a signal generator, a power amplifier, a two-dimensional piezoelectric ceramic, an AFM system and the like. The signal generator generates two paths of sine signals with 90-degree phase difference, and the signals are input into the two-dimensional piezoelectric ceramic plate after passing through the power amplifier, so that the gold-silver-gold film sample fixed on the piezoelectric ceramic plate is driven to perform circular rotation movement, and therefore the relative rotation movement between the probe and the multilayer film sample is realized. And the AFM probe simultaneously performs feeding movement with a certain feeding amount to finish the processing of the periodic nanostructure. The width of the machined structure depends on the amplitude of the signal output by the signal generator. Fig. 3 (a) shows a periodic nanostructure obtained by nano-milling on the surface of a gold-silver-gold multilayer film, and fig. 3 (b) shows a cross-sectional view thereof, in which the width of the processed trench is about 495nm.
Step (3) preparing a nano cavity by chemically corroding the middle silver layer by concentrated nitric acid:
and (3) putting the periodic nanostructure obtained by the nano milling process into concentrated nitric acid with the mass fraction of 65%, and chemically corroding the exposed silver layer at the edge of the periodic nanostructure, so as to prepare a hollow nano cavity, and providing a 'hot spot' structure for the nano cavity serving as a Raman enhanced substrate. The chemical etching time of concentrated nitric acid is 2min, and the SEM of the nano cavity structure is shown in figure 3 (c), and the length and width of the nano cavity are about 45nm and 12nm respectively.
Step (4) carrying out Raman detection by rhodamine 6G to verify the Raman enhancement effect:
sample treatment: rhodamine 6G (R6G) is selected as a Raman detection object, wherein R6G is an inorganic micromolecular fluorescent dye, is a reagent commonly used in Raman detection, and is mainly used for verifying the feasibility of a processed lattice structure serving as a Raman substrate. The solution of the appropriate volume after formulation is dropped onto the sample structure.
Surface enhanced raman scattering experiments: FIG. 4 (a) shows dark field scattering spectra of periodic nanostructures I and II with widths of 495nm and 302nm, respectively, after chemical etching. For the two structures, the plasmon resonance peak is changed from 630nm to 610nm, which indicates that the plasmon resonance can be regulated by changing the nano milling width. The prepared sample was placed in a raman spectrometer (insia-Reflex, rani shao company, uk) and the detection experiment was performed by selecting appropriate parameters, and the raman detection result is shown in fig. 4 (b). From the graph, the Raman signal intensity of the gold-silver-gold composite film is far higher than that of a single-layer gold film, and the effectiveness of the method provided by the invention is proved.

Claims (8)

1. A preparation method of a surface-enhanced Raman substrate based on AFM nano milling and chemical corrosion processing is characterized by comprising the following steps:
sequentially preparing a gold film, a silver film and a gold film on the surface of a substrate by adopting a magnetron sputtering method;
the step (2) is based on a nanometer milling system of AFM, and periodic nanometer structures are nanometer milled on the surface of the gold-silver-gold composite film;
step (3) putting the periodic nanostructure obtained by nano milling into concentrated nitric acid, and chemically corroding a silver layer exposed at the edge of the periodic nanostructure, thereby preparing a hollow nano cavity;
and (4) taking the chemically corroded composite film periodic array structure with the nano cavity as a Raman enhancement substrate.
2. The method for preparing a surface-enhanced raman substrate based on AFM nano milling and chemical etching processing according to claim 1, wherein in the step (1), the substrate is silicon dioxide or silicon.
3. The method for preparing the surface-enhanced Raman substrate based on AFM nano milling and chemical etching processing according to claim 1, wherein in the step (1), the thicknesses of the gold film, the silver film and the gold film are 40-60 nm, 10-15 nm and 10-20 nm respectively.
4. The method for preparing a surface-enhanced Raman substrate based on AFM nano milling and chemical etching processing according to claim 1, wherein in the step (1), the power of the gold-plated film is 14W, the speed is 0.04nm/s, and the power of the silver-plated film is 9W, the speed is 0.025nm/s.
5. The method for preparing the surface-enhanced Raman substrate based on AFM nano milling and chemical etching processing of claim 1, wherein in the step (2), the width of nano milling processing is 280-490 nm.
6. The method for preparing the surface-enhanced Raman substrate based on AFM nano milling and chemical etching processing of claim 1, wherein in the step (2), the rotation frequency of a probe relative to a sample is 500Hz, the processing speed is 0.66-53 mu m/s, and the feeding amount is 1.3-106 nm in the nano milling processing process.
7. The method for preparing the surface-enhanced Raman substrate based on AFM nano milling and chemical etching processing according to claim 1, wherein in the step (3), the mass fraction of the concentrated nitric acid is 65%.
8. The method for preparing the surface-enhanced Raman substrate based on AFM nano milling and chemical etching processing according to claim 1, wherein in the step (3), the chemical etching time is 2min.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103604795A (en) * 2013-11-27 2014-02-26 重庆绿色智能技术研究院 Cross-scale double-metal cooperatively-enhanced raman scattering chip and preparation method thereof
CN110316697A (en) * 2019-07-11 2019-10-11 哈尔滨工业大学 A kind of preparation method of the surface enhanced Raman substrate based on AFM processing
CN110501324A (en) * 2019-09-05 2019-11-26 山东大学 A kind of surface-enhanced Raman detection substrate and its preparation method and application based on micro-nano 3D printing
CN111337474A (en) * 2020-03-19 2020-06-26 山东大学 Raman detection chip based on micro-nano composite structure and nano particles and preparation method and application thereof
CN113699481A (en) * 2021-08-25 2021-11-26 山东智微检测科技有限公司 Composite structure array loaded with gold and silver nano-film and preparation method and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103604795A (en) * 2013-11-27 2014-02-26 重庆绿色智能技术研究院 Cross-scale double-metal cooperatively-enhanced raman scattering chip and preparation method thereof
CN110316697A (en) * 2019-07-11 2019-10-11 哈尔滨工业大学 A kind of preparation method of the surface enhanced Raman substrate based on AFM processing
CN110501324A (en) * 2019-09-05 2019-11-26 山东大学 A kind of surface-enhanced Raman detection substrate and its preparation method and application based on micro-nano 3D printing
CN111337474A (en) * 2020-03-19 2020-06-26 山东大学 Raman detection chip based on micro-nano composite structure and nano particles and preparation method and application thereof
CN113699481A (en) * 2021-08-25 2021-11-26 山东智微检测科技有限公司 Composite structure array loaded with gold and silver nano-film and preparation method and application thereof

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