CN114411152A - Surface enhanced Raman substrate preparation method based on AFM nano milling and chemical corrosion processing - Google Patents

Surface enhanced Raman substrate preparation method based on AFM nano milling and chemical corrosion processing Download PDF

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CN114411152A
CN114411152A CN202210023523.2A CN202210023523A CN114411152A CN 114411152 A CN114411152 A CN 114411152A CN 202210023523 A CN202210023523 A CN 202210023523A CN 114411152 A CN114411152 A CN 114411152A
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nano
milling
film
gold
afm
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CN114411152B (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 surface enhanced Raman substrate preparation method based on AFM nano milling and chemical corrosion processing, which comprises the following steps: preparing a gold film, a silver film and a gold film on the surface of a substrate in sequence by adopting a magnetron sputtering method; step (2) based on a nano milling system of AFM, nano milling periodic nano structure on the surface of the gold-silver-gold composite film; step (3) putting the periodic nano structure obtained by nano milling into concentrated nitric acid, and chemically corroding the silver layer exposed at the edge of the periodic nano structure, so as to prepare 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 quickly and efficiently preparing the Raman enhanced substrate with controllable structural feature size, adjustable plasma resonance and good consistency.

Description

Surface enhanced Raman substrate preparation method based on AFM nano milling and chemical corrosion processing
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 one of the label-free detection methods, has the advantages of high detection precision, high efficiency, simple operation and the like, and is widely applied to the fields of biomedicine, food health, medical chemistry and the like. However, the raman signal is usually very weak, so that it is necessary to increase the signal intensity and thus the detection sensitivity by means of the enhancing substrate. Noble metal materials with nanostructures, such as gold, silver, etc., which can obtain a strong surface plasmon resonance effect to enhance raman signals, have proven to be preferred materials for preparing raman-enhanced substrates.
At present, various methods have been used to prepare a noble metal raman-enhanced substrate with a nanostructure, such as a colloid replacement method, a chemical etching method, a laser processing method, and the like, but all of the methods have certain limitations. The substrate prepared by the colloid replacement method and the chemical corrosion method has poor structural consistency and repeatability, and the characteristic dimension of the target nano structure cannot be accurately obtained. The substrate prepared by the laser processing method has a relatively large characteristic dimension, and a reinforced substrate with a nano structure of about 10nm cannot be obtained by processing. In addition, the raman enhancement substrate cannot regulate and control plasma resonance by changing the characteristic size, and the raman enhancement effect cannot be further improved under the condition that the wavelength of the detection laser is fixed. Therefore, the preparation of raman-enhanced substrates with controllable feature size, good structural stability, high reproducibility and consistency becomes of paramount importance.
Disclosure of Invention
The invention aims to provide a surface enhanced Raman substrate preparation method based on AFM nano milling and chemical corrosion processing, which can be used for quickly and efficiently preparing a Raman enhanced substrate with controllable structural feature size, adjustable plasma resonance and good consistency.
The purpose of the invention is realized by the following technical scheme:
a surface enhanced Raman substrate preparation method based on AFM nano milling and chemical corrosion processing comprises the following steps:
the method comprises the following steps of (1) preparing a gold film, a silver film and a gold film on the surface of a substrate in sequence 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 40-60 nm, 10-15 nm and 10-20 nm respectively;
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 0.025 nm/s;
and (2) based on the nano milling system of the AFM, nano milling a periodic nano structure on the surface of the gold-silver-gold composite film, wherein:
the width of the nano milling is 280-490 nm, the rotation frequency of the probe relative to the sample is 500Hz, the processing speed is 0.66-53 μm/s, and the feeding amount is 1.3-106 nm;
and (3) putting the periodic nano structure obtained by nano milling into concentrated nitric acid, and chemically corroding the silver layer exposed at the edge of the periodic nano structure, so as to prepare a hollow nano cavity, wherein:
the mass fraction of the concentrated nitric acid is 65 percent;
the chemical etching time is 2 min;
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 nano-structure characteristic dimension by combining Atomic Force Microscope (AFM) nano milling processing and chemical corrosion processing.
2. The period of the Raman enhancement substrate prepared by the invention is determined by the width of nano milling, the plasma resonance of the substrate can be regulated, and meanwhile, the strength of Raman detection signals can be greatly improved by taking the nano cavity structure as an enhancement '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 on SiO2Gold plating a substrate, (b) silver plating by a magnetron sputtering method, (c) gold plating by a magnetron sputtering method, (d) a gold-silver-gold multilayer film TEM image, (e) nano-milling a periodic nano-structure on the surface of the gold-silver-gold multilayer film, (f) chemically corroding a middle silver layer by 65% nitric acid to obtain a nano-cavity structure, and (G) carrying out Raman detection on rhodamine 6G by a Raman substrate;
FIG. 2 is a schematic view of a nano-milling process;
FIG. 3 is a periodic nanostructure and a nanocavity structure, (a) a nanomilling periodic nanostructure, (b) a cross-sectional view of the periodic structure, and (c) a nanocavity SEM image;
FIG. 4 shows the results of the surface enhanced Raman scattering experiment, (a) the periodic nanostructure dark field scattering spectrum, and (b) the Raman test results.
Detailed Description
The technical solution of the present invention is further described below with reference to the accompanying drawings, but not limited thereto, and any modification or equivalent replacement of the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention shall be covered by the protection scope of the present invention.
The invention provides a surface enhanced Raman substrate preparation method based on AFM nano milling and chemical corrosion processing, which comprises the steps of firstly plating a gold film, a silver film and a gold film on the surface of silicon dioxide in sequence by a magnetron sputtering method, then nano milling a periodic array structure with variable width on the surface of the plated film, and chemically corroding the silver film exposed at the edge of the nano structure by using concentrated nitric acid with the mass fraction of 65% to obtain a nano cavity which 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 on SiO2Substrate gold-plated-silver-gold composite film:
noble metal gold and silver are easier to generate a plasmon effect so as to greatly enhance Raman signals, and a gold film, a silver film and a gold film are sequentially prepared on the surface of silicon dioxide by adopting a magnetron sputtering method, wherein the coating thickness is determined by the coating time and the beam size. The coating equipment is provided with an automatic film thickness monitor, and can realize real-time monitoring of the film thickness in the coating process so as to ensure the thickness of the coating film. 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 the periodic nano-structure on the surface of the gold-silver-gold composite film:
fig. 2 is a schematic diagram of a nano-milling system based on AFM. The processing system mainly comprises a signal generator, a power amplifier, two-dimensional piezoelectric ceramics, an AFM system and the like. The signal generator generates two paths of sinusoidal signals with the phase difference of 90 degrees, the sinusoidal signals are input into the two-dimensional piezoelectric ceramic piece after passing through the power amplifier, and therefore the gold-silver-gold film sample fixed on the piezoelectric ceramic piece is driven to perform circular rotation motion, and therefore the relative rotation motion between the probe and the multilayer film sample is achieved. And the AFM probe simultaneously performs feeding movement with a certain feeding amount to complete the processing of the periodic nano structure. The width of the processing structure depends on the amplitude of the signal generator output signal. Fig. 3 (a) shows the periodic nanostructure obtained by nano-milling on the surface of the au-ag-au multilayer film, and fig. 3 (b) is a cross-sectional view thereof, which shows that the width of the processed trench is about 495 nm.
And (3) chemically corroding the intermediate silver layer by concentrated nitric acid to prepare a nano cavity:
and putting the periodic nano structure obtained by the nano milling processing into concentrated nitric acid with the mass fraction of 65%, and chemically corroding the silver layer exposed at the edge of the periodic nano structure, so as to prepare a hollow nano cavity and provide a 'hot spot' structure for the nano cavity serving as a Raman enhancement substrate. The chemical etching time of concentrated nitric acid is 2min, the SEM of the structure of the nano cavity is shown in figure 3 (c), and the length and the width of the nano cavity are respectively about 45nm and 12 nm.
And (4) carrying out Raman detection by using 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 common reagent in Raman detection, and is mainly used for verifying the feasibility of the processed lattice structure as a Raman substrate. A suitable volume of solution after formulation was dropped onto the sample structure.
Surface enhanced raman scattering experiments: FIG. 4 (a) shows dark field scattering spectra of periodic nanostructures I and periodic nanostructures II with nanotmill widths of 495nm and 302nm, respectively, after chemical etching. For the two structures, the plasmon resonance peak is changed from 630nm to 610nm, which shows that the plasmon resonance can be regulated and controlled by changing the nano milling width. The prepared sample was placed in a raman spectrometer (InVia-Reflex, renisha, uk) and appropriate parameters were selected for the detection experiment, with the raman detection results shown in fig. 4 (b). As can be seen from the figure, 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 surface enhanced Raman substrate preparation method based on AFM nano milling and chemical corrosion processing is characterized by comprising the following steps:
preparing a gold film, a silver film and a gold film on the surface of a substrate in sequence by adopting a magnetron sputtering method;
step (2) based on a nano milling system of AFM, nano milling periodic nano structure on the surface of the gold-silver-gold composite film;
step (3) putting the periodic nano structure obtained by nano milling into concentrated nitric acid, and chemically corroding the silver layer exposed at the edge of the periodic nano structure, so as to prepare 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 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 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 according to claim 1, wherein in the step (1), the power of the gold-plated film is 14W at a rate of 0.04nm/s, and the power of the silver-plated film is 9W at a rate of 0.025 nm/s.
5. The method for preparing the surface-enhanced Raman substrate based on AFM nano-milling and chemical etching according to claim 1, wherein in the step (2), the width of the nano-milling is 280-490 nm.
6. The method for preparing the surface-enhanced Raman substrate based on AFM nano-milling and chemical etching according to claim 1, wherein in the step (2), the rotational frequency of the probe relative to the sample during nano-milling is 500Hz, the processing speed is 0.66-53 μm/s, and the feeding amount is 1.3-106 nm.
7. The method for preparing a surface-enhanced Raman substrate based on AFM nano-milling and chemical etching according to claim 1, wherein the mass fraction of the concentrated nitric acid in the step (3) is 65%.
8. The method for preparing a surface-enhanced Raman substrate based on AFM nano-milling and chemical etching according to claim 1, wherein in the step (3), the chemical etching time is 2 min.
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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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