CN112179886A - SERS detection transparent flexible substrate of metal nano hemispherical shell array and preparation method - Google Patents
SERS detection transparent flexible substrate of metal nano hemispherical shell array and preparation method Download PDFInfo
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- 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 metal nano hemispherical shell array SERS detection transparent flexible substrate and a preparation method thereof, wherein the preparation method comprises the following steps: laying single-layer polystyrene nanospheres on the surface of the hard substrate by using a self-assembly method; depositing a layer of metal nickel film on the surface of the polystyrene nano-spheres by adopting an evaporation method; annealing treatment is carried out to ensure that the polystyrene spheres are completely volatilized, and then a metal nickel nano hollow hemispherical shell array is formed on the surface of the substrate; depositing a metal silver film on the surface of the metal nickel nano hollow hemispherical shell by a thermal evaporation method; covering the viscous transparent adhesive tape on the metal nano hollow hemispherical shell, and taking off the viscous transparent adhesive tape to obtain the SERS detection transparent flexible substrate based on the metal nano hemispherical shell array. The preparation method has the advantages of low cost, high repeatability, simple process and the like, and can be used for batch production in short period at low cost in industrial production.
Description
Technical Field
The invention belongs to the field of nano material preparation, and particularly relates to a SERS detection transparent flexible substrate of a metal nano hemispherical shell array and a preparation method thereof.
Background
The Surface Enhanced Raman Scattering (SERS) effect can greatly increase the raman signal intensity of adsorbates on the surface of certain nanostructures. The surface Raman enhanced spectrum technology developed by the method becomes an ultrasensitive surface detection technology and is successfully applied to the fields of electrochemistry and analytical science. However, the excitation line of SERS research is substantially concentrated in the wavelength range from visible light to near infrared, and the transition metal such as nickel can broaden the excitation line to the ultraviolet region, which will substantially expand the application system of SERS.
The metal spherical shell/hemispherical shell array can excite the surface-enhanced Raman scattering effect due to the surface plasmon enhancement effect of the metal spherical shell/hemispherical shell array. At present, a preparation method of a metal spherical shell/hemispherical shell array mostly adopts a chemical method for synthesis, the process is complex, the cost is high, and the formed metal spherical shell/hemispherical shell array has poor appearance.
Disclosure of Invention
The invention aims to provide a SERS detection transparent flexible substrate of a metal nano hemispherical shell array and a preparation method thereof; the preparation method has the advantages of simple process, strong operability and high repeatability; the prepared substrate can excite the surface enhanced Raman scattering effect and has wide application prospect in the fields of electrochemistry and analytical science.
In order to achieve the purpose, the invention adopts the following technical scheme:
SERS of metal nanometer hemisphere shell array detects transparent flexible base includes:
the nickel metal film is in a metal nickel nanometer hollow hemispherical shell array structure which is connected with each other and is in hexagonal close packing;
the silver metal film is arranged on the nickel metal film and has a hexagonal close-packed metal silver nano hollow hemispherical shell array structure;
and the flexible transparent substrate is arranged on the silver metal film.
The invention further improves the following steps: the thickness of the nickel metal film is 20-50 nm.
The invention further improves the following steps: the thickness of the silver metal film is 10-30 nm.
The invention further improves the following steps: the diameter of each hemispherical shell in the nickel nano hemispherical shell array is 200-700 nm.
The invention further improves the following steps: the diameter of each hemispherical shell in the metal silver nano hollow hemispherical shell array structure is 200-700 nm.
The invention further improves the following steps: the nickel metal film and the silver metal film are prepared in a vapor deposition mode.
The preparation method of the SERS detection transparent flexible substrate of the metal nano hemispherical shell array comprises the following steps:
laying a single-layer polystyrene bead template on the surface of the hard substrate;
depositing nickel metal on the polystyrene small ball template by using an evaporation method;
annealing the small ball template with the nickel metal deposited on the surface, and removing the polystyrene small ball template to obtain a nickel metal film; the nickel metal film is in a metal nickel nanometer hollow hemispherical shell array structure which is connected with each other and is in hexagonal close packing;
depositing silver metal on the nickel metal film by an evaporation method to obtain a silver metal film; the silver metal film is in a metal silver nano hemispherical shell array structure which is connected with each other and is in hexagonal close packing;
and the nickel metal film and the silver metal film are peeled off from the surface of the hard substrate through the flexible transparent substrate with the adhesive and the adhesive, so that the SERS detection transparent flexible substrate based on the metal nano hemispherical shell array is obtained.
The invention further improves the following steps: the hard substrate is a silicon wafer, a quartz wafer, a sapphire substrate or a gallium nitride substrate.
The invention further improves the following steps: the polystyrene sphere template is completely removed by an annealing method.
The invention further improves the following steps: the annealing treatment is carried out under the protective atmosphere of inert gas.
The invention further improves the following steps: the flexible transparent substrate with the adhesive and capable of being pasted is PDMS or PET.
Compared with the prior art, the invention has the following beneficial effects:
1. the single-layer polystyrene nanospheres are used as a template, so that the prepared array structure is regular and has good appearance;
2. the metal is deposited by adopting an evaporation coating method, the method is a physical vapor deposition method, and compared with a chemical synthesis method, the method has the advantages of simple operation process and stable film forming quality;
3. the polystyrene nano-bead template is removed by adopting an annealing method, and the method is simple, convenient and good in removal effect;
4. the substrate is simple in preparation method, low in cost, strong in operability, convenient to carry and use, and beneficial to realizing simple and rapid sampling of samples in an actual analysis and test scene.
The preparation method adopting the polystyrene spheres as the template has the advantages of simple process, low cost and regular appearance, and further promotes the application of the structure.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a flow chart of the preparation of the method of the present invention; wherein, 1 is a hard substrate; 2-polystyrene beads; 3-a nickel metal film; 4-silver metal thin film; 5-transparent flexible substrate.
FIG. 2 is a surface representation of a scanning electron microscope of a metal nano-hemispherical shell array structure prepared by the method of the present invention.
FIG. 3 is a cross-sectional representation of a scanning electron microscope of a metal nano-hemispherical shell array structure prepared by the method of the present invention.
FIG. 4 shows a Raman spectrum obtained by performing surface enhanced Raman spectrum testing on the SERS detection transparent flexible substrate based on the metal nano-hemispherical shell array, which is prepared by the method disclosed by the invention, after the SERS detection transparent flexible substrate is treated by crystal violet solutions with different concentrations.
Detailed Description
The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The following detailed description is exemplary in nature and is intended to provide further details of the invention. Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention.
Example 1:
step 1) preparing a small ball template with single-layer polystyrene
Step 1.1), pretreatment of the hard substrate 1:
placing the hard substrate 1 (silicon substrate) in absolute ethyl alcohol, ultrasonically cleaning the substrate in a fume hood for 20 minutes, removing the substrate, cleaning the substrate with deionized water for three times, and blow-drying the substrate with nitrogen for later use;
step 1.2), carrying out hydrophilic treatment after the pretreatment of the hard substrate 1:
placing the hard substrate 1 in a plasma degumming machine, and vacuumizing the chamber when the vacuum degree is less than 1 multiplied by 10-1Introducing oxygen gas at Pa, and performing oxygen plasma treatment at the power of 100W for 3 minutes;
step 1.3), preparing a single-layer polystyrene bead film:
mixing a dispersion containing polystyrene spheres with the diameter of 500nm and absolute ethyl alcohol according to the volume ratio of 1: 1, mixing, namely performing ultrasonic treatment on the mixed solution for 10 minutes to uniformly disperse the mixed solution to form polystyrene microsphere dispersion liquid;
extending a first hard substrate 1 subjected to hydrophilic treatment in the step 1.2) into a culture dish containing deionized water at an inclination angle of 45 degrees, slowly dripping a uniform polystyrene bead solution onto the first hard substrate 1 to enable the polystyrene bead solution to naturally slide down into the deionized water, and adding 1-2 mL of surfactant sodium dodecyl sulfate into the deionized water to enable the polystyrene beads to be self-assembled on a water surface to form a single-layer polystyrene bead film;
step 1.4), preparing a single-layer polystyrene small ball template:
slowly extending the second hard substrate 1 subjected to hydrophilic treatment into deionized water, fishing up the polystyrene bead film to transfer the polystyrene bead film to the surface of the second hard substrate 1, and naturally air-drying the polystyrene bead film to obtain the hard substrate with the single-layer polystyrene bead template;
step 2) depositing a metal film on the surface of the polystyrene small ball template
Fixing a hard substrate 1 with a single-layer polystyrene small ball template on a target position of an evaporation chamber for electron beam evaporation, and forming a nickel metal film 3 on the surface of the single-layer polystyrene small ball template; the evaporation target material is nickel, and the vacuum degree of the evaporation chamber needs to reach 2 multiplied by 10 before evaporation-3The electron gun current is 1.06-1.08A below Pa, and the coating thickness is 30 nm;
step 3), removing the small ball template:
taking out the hard substrate 1 after the evaporation, and placing the hard substrate in an RTP rapid alloy furnace for rapid heat treatment, wherein the annealing temperature is 500 ℃, and the heat preservation time is 20 minutes; taking out the hard substrate 1 subjected to annealing treatment, and removing the polystyrene pellet template to obtain a metal nickel nano hemispherical shell array;
step 4), fixing the annealed hard substrate 1 on a target position of an evaporation chamber for thermal evaporation, and evaporating a silver metal film 4 on the surface of the nickel metal film 3; the evaporation target material is silver, and the vacuum degree of the evaporation chamber needs to reach 2 multiplied by 10 before evaporation- 3The vapor deposition current is 107A and the thickness of the coating film is 20nm below Pa;
and 5), taking out the hard substrate 1 after the silver evaporation is finished, covering a transparent flexible substrate 5 (viscous transparent adhesive tape) on the silver metal film 4, and taking off to obtain the SERS detection flexible substrate of the metal nano hemispherical shell array (step 6 in the figure 1).
The whole preparation process is shown in figure 1. The metal nano hemispherical shell array structure prepared in example 1 is characterized in morphology by a field emission scanning electron microscope, and a scanning electron microscope surface characterization map of the metal nano hemispherical shell array structure shown in fig. 2 and a scanning electron microscope cross-sectional characterization map of the metal nano hemispherical shell array structure shown in fig. 3 are obtained. As can be seen from FIG. 2, the radius of the metal nano-hemispherical shell is uniformly distributed and is in a regular hexagonal close-packed shape; it can be seen from fig. 3 that after the polystyrene bead template is removed, a hollow bowl-shaped metal nano hemispherical shell array is formed.
The SERS detection flexible substrate of the prepared metal nano hemispherical shell array comprises:
the nickel metal film 3 is in a mutually connected metal nickel nano hollow hemispherical shell array structure;
the silver metal film 4 is arranged on the nickel metal film 3 and has a mutually connected metal silver nano hollow hemispherical shell array structure; and the flexible transparent substrate is arranged on the silver metal film 4.
Example 2:
step 1) preparing a small ball template with single-layer polystyrene
Step 1.1), pretreatment of the hard substrate 1:
placing the hard substrate 1 (quartz plate) in absolute ethyl alcohol, ultrasonically cleaning for 20 minutes in a fume hood, removing the substrate, cleaning for three times by using deionized water, and drying for later use by using nitrogen;
step 1.2), carrying out hydrophilic treatment after the pretreatment of the hard substrate 1:
placing the hard substrate 1 in a plasma degumming machine, and vacuumizing the chamber when the vacuum degree is less than 1 multiplied by 10-1Introducing oxygen gas at Pa, and performing oxygen plasma treatment at the power of 100W for 3 minutes;
step 1.3), preparing a single-layer polystyrene bead film:
mixing a dispersion containing polystyrene spheres with the diameter of 200nm and absolute ethyl alcohol according to the volume ratio of 1: 1, mixing, namely performing ultrasonic treatment on the mixed solution for 10 minutes to uniformly disperse the mixed solution to form polystyrene microsphere dispersion liquid;
extending a first hard substrate 1 subjected to hydrophilic treatment in the step 1.2) into a culture dish containing deionized water at an inclination angle of 45 degrees, slowly dripping a uniform polystyrene bead solution onto the first hard substrate 1 to enable the polystyrene bead solution to naturally slide down into the deionized water, and adding 1-2 mL of surfactant sodium dodecyl sulfate into the deionized water to enable the polystyrene beads to be self-assembled on a water surface to form a single-layer polystyrene bead film;
step 1.4), preparing a single-layer polystyrene small ball template:
slowly extending the second hard substrate 1 subjected to hydrophilic treatment into deionized water, fishing up the polystyrene bead film to transfer the polystyrene bead film to the surface of the second hard substrate 1, and naturally air-drying the polystyrene bead film to obtain the hard substrate with the single-layer polystyrene bead template;
step 2) depositing a metal film on the surface of the polystyrene small ball template
Fixing a hard substrate 1 with a single-layer polystyrene small ball template on a target position of an evaporation chamber for electron beam evaporation, and forming a nickel metal film 3 on the surface of the single-layer polystyrene small ball template; the evaporation target material is nickel, and the vacuum degree of the evaporation chamber needs to reach 2 multiplied by 10 before evaporation-3The electron gun current is 1.06-1.08A below Pa, and the coating thickness is 50 nm;
step 3), removing the small ball template:
taking out the hard substrate 1 after the evaporation, and placing the hard substrate in an RTP rapid alloy furnace for rapid heat treatment, wherein the annealing temperature is 500 ℃, and the heat preservation time is 20 minutes; taking out the hard substrate 1 subjected to annealing treatment, and removing the polystyrene pellet template to obtain a metal nickel nano hemispherical shell array;
step 4), fixing the annealed hard substrate 1 on a target position of an evaporation chamber for thermal evaporation, and evaporating a silver metal film 4 on the surface of the nickel metal film 3; the evaporation target material is silver, and the vacuum degree of the evaporation chamber needs to reach 2 multiplied by 10 before evaporation- 3The vapor deposition current is 107A and the thickness of the coating film is 10nm below Pa;
and 5), taking out the hard substrate 1 after the silver evaporation is finished, covering the transparent flexible substrate 5 (viscous PET) on the silver metal film 4, and taking off to obtain the SERS detection flexible substrate of the metal nano hemispherical shell array (step 6 in the figure 1).
Example 3:
step 1) preparing a small ball template with single-layer polystyrene
Step 1.1), pretreatment of the hard substrate 1:
placing the hard substrate 1 (sapphire substrate) in absolute ethyl alcohol, ultrasonically cleaning the substrate in a fume hood for 20 minutes, removing the substrate, cleaning the substrate with deionized water for three times, and drying the substrate with nitrogen for later use;
step 1.2), carrying out hydrophilic treatment after the pretreatment of the hard substrate 1:
placing the hard substrate 1 in a plasma degumming machine, and vacuumizing the chamber when the vacuum degree is less than 1 multiplied by 10-1Introducing oxygen gas at Pa, and performing oxygen plasma treatment at the power of 100W for 3 minutes;
step 1.3), preparing a single-layer polystyrene bead film:
mixing a dispersion containing polystyrene spheres with the diameter of 700nm and absolute ethyl alcohol according to the volume ratio of 1: 1, mixing, namely performing ultrasonic treatment on the mixed solution for 10 minutes to uniformly disperse the mixed solution to form polystyrene microsphere dispersion liquid;
extending a first hard substrate 1 subjected to hydrophilic treatment in the step 1.2) into a culture dish containing deionized water at an inclination angle of 45 degrees, slowly dripping a uniform polystyrene bead solution onto the first hard substrate 1 to enable the polystyrene bead solution to naturally slide down into the deionized water, and adding 1-2 mL of surfactant sodium dodecyl sulfate into the deionized water to enable the polystyrene beads to be self-assembled on a water surface to form a single-layer polystyrene bead film;
step 1.4), preparing a single-layer polystyrene small ball template:
slowly extending the second hard substrate 1 subjected to hydrophilic treatment into deionized water, fishing up the polystyrene bead film to transfer the polystyrene bead film to the surface of the second hard substrate 1, and naturally air-drying the polystyrene bead film to obtain the hard substrate with the single-layer polystyrene bead template;
step 2) depositing a metal film on the surface of the polystyrene small ball template
Fixing a hard substrate 1 with a single-layer polystyrene small ball template on a target position of an evaporation chamber for electron beam evaporation, and forming a nickel metal film 3 on the surface of the single-layer polystyrene small ball template; the evaporation target material is nickel, and the vacuum degree of the evaporation chamber needs to reach 2 multiplied by 10 before evaporation-3The electron gun current is 1.06-1.08A below Pa, and the coating thickness is 20 nm;
step 3), removing the small ball template:
taking out the hard substrate 1 after the evaporation, and placing the hard substrate in an RTP rapid alloy furnace for rapid heat treatment, wherein the annealing temperature is 500 ℃, and the heat preservation time is 20 minutes; taking out the hard substrate 1 subjected to annealing treatment, and removing the polystyrene pellet template to obtain a metal nickel nano hemispherical shell array;
step 4), fixing the annealed hard substrate 1 on a target position of an evaporation chamber for thermal evaporation, and evaporating a silver metal film 4 on the surface of the nickel metal film 3; the evaporation target material is silver, and the vacuum degree of the evaporation chamber needs to reach 2 multiplied by 10 before evaporation- 3The vapor deposition current is 107A and the thickness of the coating film is 30nm below Pa;
and 5), taking out the hard substrate 1 after the silver evaporation is finished, covering the transparent flexible substrate 5 (viscous PDMS) on the silver metal film 4, and taking off to obtain the SERS detection flexible substrate of the metal nano hemispherical shell array (step 6 in the figure 1). Example 4:
the SERS detection flexible substrate based on the metal nano-hemispherical shell array prepared in example 1 was tested with Crystal Violet (CV) as a detection object:
(1) weighing crystal violet solid by using an electronic precision analytical balance, taking deionized water as a solvent, and preparing the crystal violet solid with the concentration of 10 respectively-7mol/L、10-8mol/L、10-9mol/L、10-10mol/L、10-11A mol/L crystal violet solution;
(2) placing the prepared substrate to be detected in crystal violet solutions with different concentrations for soaking for 8 hours, taking out the substrate and naturally airing;
(3) carrying out Surface Enhanced Raman Spectroscopy (SERS) detection on the substrate treated by the crystal violet solution; wherein the type of the used laser Raman spectrometer is HR Evolution, the laser source is a 325nm HeCd laser (power is 25mW), the exposure time is 10s, and the scanning range is 100-1800 cm-1The data were processed by LabSpec6 to give the Raman spectrum shown in FIG. 4.
As can be seen from the Raman spectrum shown in FIG. 4, the characteristic peak intensity of the crystal violet molecules decreases with decreasing concentration of the crystal violet solution, when the concentration of the crystal violet solution is lowTo 10-11Still, a more obvious characteristic peak of crystal violet can be seen at mol/L.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of or equivalence to the invention are intended to be embraced therein.
Claims (9)
1. SERS of metal nanometer hemisphere shell array detects transparent flexible substrate, its characterized in that includes:
the nickel metal film (3) is in a metal nickel nano hollow hemispherical shell array structure which is connected with each other and is in hexagonal close packing;
the silver metal film (4) is arranged on the nickel metal film (3) and is in a metal silver nano hollow hemispherical shell array structure which is connected with each other and is in hexagonal close packing;
and the flexible transparent substrate is arranged on the silver metal film (4).
2. The SERS detection transparent flexible substrate of the metal hemispherical nanoshell array according to claim 1, wherein the nickel metal film (3) is 20-50 nm thick.
3. A SERS detection transparent flexible substrate of a metal nano hemispherical shell array according to claim 1, wherein the thickness of the silver metal film (4) is 10-30 nm.
4. The SERS detection transparent flexible substrate of the metal nano hemispherical shell array according to claim 1, wherein the diameter of each hemispherical shell in the nickel nano hemispherical shell array is 200-700 nm.
5. The SERS detection transparent flexible substrate of the metal hemispherical nanoshell array according to claim 1, wherein the nickel metal film (3) and the silver metal film (4) are prepared by evaporation.
6. The preparation method of the SERS detection transparent flexible substrate with the metal nano hemispherical shell array as claimed in any one of claims 1 to 5, characterized by comprising the following steps:
laying a single-layer polystyrene bead template on the surface of the hard substrate;
depositing nickel metal on the polystyrene small ball template by using an evaporation method;
annealing the small ball template with the nickel metal deposited on the surface, and removing the polystyrene small ball template to obtain a nickel metal film (3); the nickel metal film (3) is in a metal nickel nano hollow hemispherical shell array structure which is connected with each other and is in hexagonal close packing;
depositing silver metal on the nickel metal film (3) by an evaporation method to obtain a silver metal film (4); the silver metal film (4) is in a metal silver nano hemispherical shell array structure which is connected with each other and is in hexagonal close packing;
and the nickel metal film (3) and the silver metal film (4) are peeled off from the surface of the hard substrate through the flexible transparent substrate with the adhesive and the adhesive, so that the SERS detection transparent flexible substrate based on the metal nano hemispherical shell array is obtained.
7. The method according to claim 6, wherein the hard substrate is a silicon wafer, a quartz wafer, a sapphire substrate, or a gallium nitride substrate.
8. The method according to claim 6, wherein the polystyrene pellet template is completely removed by an annealing process, and the annealing process is performed under an inert gas atmosphere.
9. The method of claim 6, wherein the flexible adhesive transparent substrate is PDMS or PET.
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Application publication date: 20210105 |