CN118169097A - Ordered localized nano structure for realizing enrichment detection and preparation method and application thereof - Google Patents
Ordered localized nano structure for realizing enrichment detection and preparation method and application thereof Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 28
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 claims abstract description 51
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 22
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 22
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims abstract description 22
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 26
- 229910052710 silicon Inorganic materials 0.000 claims description 26
- 239000010703 silicon Substances 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 16
- 239000010410 layer Substances 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 239000000126 substance Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 5
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000001237 Raman spectrum Methods 0.000 claims description 3
- 238000007171 acid catalysis Methods 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 3
- 230000002708 enhancing effect Effects 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 238000005530 etching Methods 0.000 claims description 2
- 238000001338 self-assembly Methods 0.000 claims description 2
- 239000002356 single layer Substances 0.000 claims description 2
- 238000004070 electrodeposition Methods 0.000 abstract description 7
- 230000004048 modification Effects 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 4
- 238000004557 single molecule detection Methods 0.000 abstract description 3
- 239000002114 nanocomposite Substances 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 239000004793 Polystyrene Substances 0.000 description 16
- 239000000758 substrate Substances 0.000 description 7
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 238000003491 array Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012306 spectroscopic technique Methods 0.000 description 1
- 230000003075 superhydrophobic effect Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
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- 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
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Abstract
The invention relates to the technical field of nanocomposite materials, in particular to a preparation method for realizing enrichment detection by an ordered localized nanostructure. The method mainly comprises the following steps of 1, self-assembling PS balls; 2. removing ball corrosion; 3. electrochemical deposition; 4. and (3) modification of PDMS. The localized enrichment SERS array has the characteristics of simple preparation and strong repeatability, and has the excellent performance of conducting surface plasmons; ag 7O8NO3 is a multivalent Ag compound, and reduced Ag has good SERS detection performance; the experimental steps are simple, and the preparation period is short; the preparation cost is low; the enrichment SERS detection can realize low-concentration SERS detection, and the operation space is widened for the subsequent single-molecule detection.
Description
Technical Field
The invention relates to the technical field of nanocomposite materials, in particular to an ordered localized nanostructure for realizing enrichment detection, a preparation method and application thereof.
Background
Surface Enhanced Raman Scattering (SERS) is a Surface physical phenomenon that, based on the principle of raman scattering, significantly enhances raman signals when molecules are close to rough metal surfaces or nanostructures. This signal enhancement makes SERS an extremely sensitive spectroscopic technique that can be used to detect very low concentrations of chemicals.
Electrochemical deposition is a technique for producing and depositing metals or other substances on conductive substrates by electrolytic reactions. The method has the advantages of simple operation, low cost, strong controllability, capability of being used for surface coating of objects with complex shapes and the like, and is widely applied to material science and industrial production. In recent years, with the development of nanotechnology, electrochemical deposition on the nanoscale has been particularly attractive.
Ag 7O8NO3 has unique electrochemical and optical properties and is considered to have great potential in SERS applications, and thus can serve as a novel SERS substrate material providing high density of "hot spots" in the form of ordered nano-arrays, thereby greatly enhancing raman signals.
The SERS detection substrate is constructed through a limited area, and PDMS super-hydrophobic surfaces are combined around the substrate, so that pyridine molecules in an object to be detected can be enriched to the central area to be detected to the greatest extent. Therefore, it is necessary to construct an enrichment-SERS detection platform with high enrichment efficiency, which is particularly suitable for conventional organic solvents, and which is independent of the type of molecules to be detected, and the structure has application prospects in reduced flow single molecule detection, self-cleaning surface design, and microfluidic devices.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method based on an ordered localized nano-structure array, which can obtain the effect of enriching molecules to be detected into the localized nano-structure for SERS detection by combining electrochemical deposition of noble metal in the nano-structure array and PDMS modification, and provides a technical means with simple steps and strong operability based on the ordered localized nano-structure array, which is hopeful to realize single-molecule detection.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the preparation method of the ordered localized nano structure for realizing enrichment detection is characterized by comprising the following steps of:
(A) Self-assembling PS balls in the upper limit region of the silicon wafer, reducing the size of the PS balls through etching treatment, enabling a certain interval to exist between the PS balls, and obtaining a PS ball array on the silicon wafer;
(B) Magnetron sputtering a layer of Cr on the surface of the silicon wafer as a mask, removing the PS balls from the surface of the silicon wafer, and generating a naked silicon wafer area after the PS balls are removed; heating and soaking a silicon wafer by using NaOH solution, and obtaining an ordered array formed by a concave pyramid structure on the surface of the silicon wafer;
(C) Growing a layer of substance for improving the SERS performance in the concave pyramid structure, so as to obtain a SERS locus area on the surface of the silicon wafer;
(D) Setting a layer of PDMS film on the surface of the silicon wafer except for the SERS locus area to form an ultra-smooth surface; the super-slip surface is used for enabling the sample to be tested to concentrate towards the central SERS locus area, and as the water molecules in the sample to be tested evaporate, the molecules to be tested in the sample to be tested are continuously gathered and enriched under the action of PDMS, so that the molecules to be tested in the sample to be tested are continuously gathered in the SERS locus area.
Preferably, in the step (a), the domain-limited self-assembly specifically includes: the range of the close-packed hexagonal stacked single-layer PS ball array is controlled within the limit range of 200-300 mu m in length and width, and the diameter of the PS balls is 500nm.
Preferably, in the step (B), the step (B) is performed with heating and soaking by using NaOH solution, and specifically comprises the steps of placing the silicon wafer in NaOH solution at 80 ℃ for soaking for 1-3 min, so that a concave pyramid structure is obtained in a bare silicon wafer area; as the soaking time increases, the depth of the concave pyramid becomes gradually larger.
Preferably, in the step (C), the method for growing a layer of a substance for enhancing SERS performance specifically includes:
firstly, performing magnetron sputtering Au treatment on the concave pyramid structure;
And then, ag 7O8NO3 is electrochemically deposited in the concave pyramid structure, then Ag 7O8NO3 is reduced to Ag, and simple substance Ag with nanoscale holes on the surface is obtained in the concave pyramid.
Preferably, in the step (D), the specific method for disposing a layer of PDMS film includes:
And carrying out hydrophilization treatment on the surface of the region except the SERS site region on the surface of the silicon wafer, and grafting the surface of the hydrophilized region by using a PDMS precursor solution under the conditions of 60% of ambient humidity and acid catalysis to obtain the PDMS film.
Through dripping the substance to be detected on the sample, the ultra-smooth surface of the PDMS can lead the liquid to be more concentrated and gathered, and pyridine molecules are continuously gathered to the central area in the continuous volatilization process of the liquid. Until the water molecules in the solution are completely volatilized, the molecules to be detected in the sample are enriched to the SERS locus area to the greatest extent.
The invention also provides an ordered localized nanostructure for realizing enrichment detection, which comprises a SERS locus region and an ultra-smooth surface; the length and width of the SERS locus area are all in the range of 200-300 mu m, the periphery of the SERS locus area is an ultra-smooth surface, and the ultra-smooth surface is composed of a PDMS film;
The SERS site region consists of an array of recessed pyramids,
The spacing between the array of recessed pyramids is 20nm-100nm,
An Au layer is sputtered in the concave pyramid in a magnetron manner;
The Au layer is also provided with simple substance Ag with nanoscale holes on the surface.
Preferably, the thickness of the Au layer is 5nm.
The invention also provides an enrichment detection method of the molecules to be detected in the aqueous solution by applying the ordered localized nano structure for realizing the enrichment detection, which comprises the following steps:
Taking an aqueous solution containing molecules to be tested as a sample to be tested;
placing a sample to be detected on the surface of the ordered localized nano structure for realizing enrichment detection; the super-smooth surface is utilized to enable the sample to be tested to be concentrated towards the central SERS locus area on the super-smooth surface;
Evaporating water in the aqueous solution, and continuously gathering and enriching the sample to be detected to an SERS site area under the action of PDMS along with the evaporation of water molecules, so that molecules to be detected in the sample to be detected are continuously gathered in the SERS site area;
and after the molecules to be detected in the aqueous solution are enriched in the SERS locus region, carrying out Raman spectrum test on the molecules to be detected in the SERS locus region.
Preferably, the interval between the concave pyramid arrays is 20nm-100nm, and the molecules to be detected are pyridine molecules.
The invention has the beneficial effects that:
In the invention, the ordered localized nanostructure-based array is prepared, the preparation method is simple and easy to operate, and the prepared microstructure array has the characteristics of localized detection, strong SERS signal, enrichment effect, regular structure and the like.
The invention can enrich the sample to be detected to the central area to be detected to the greatest extent, and avoid the coffee ring in the detection process "
The effect appears to increase the concentration limit of the assay.
Drawings
Fig. 1 is a flow chart of an experiment in the specification.
Fig. 2 is a schematic diagram of PS spheres of a finite field ordered array.
Fig. 3 is an SEM image of the ordered structure.
Fig. 4 is an SEM image after electrochemical deposition of Ag 7O8NO3 in the ordered structure.
Detailed Description
Example 1:
Self-assembled PS ball
Here we select 500nm polystyrene microspheres, and obtain PS sphere arrays in localized areas on the silicon wafer by processing with a reticle; the PS balls were reduced in size to about 240nm by RIE processing at parameters 50W, 20Pa, and oxygen flux of 50sccm for 200 seconds.
Ball removing corrosion
Here we magnetron sputter a layer of Cr on the PS sphere surface as a mask, the Cr plating acting to protect the silicon wafer part from NaOH corrosion. The PS spheres are removed from the silicon wafer substrate, and the PS spheres are heated to 80 ℃ in 20mL NaOH solution to be subjected to wet chemical corrosion for 1-2 min to obtain the concave pyramid-shaped nano structures with different degrees.
Electrochemical deposition
Here we put the etched localized structure in an electrolyte solution of AgNO 3 and H 3BO3 after further magnetron sputtering plating of 5nm Au modification for electrochemical deposition. The magnetron sputtered Au is used for improving conductivity, and the deposited Ag 7O8NO3 is subjected to reduction treatment to obtain the simple substance Ag with a Ag 7O8NO3 structure and a large number of nano-scale holes on the surface.
PDMS modification
Here, the PDMS precursor dimethyl dimethoxy silane is grafted to the surface of the substrate subjected to hydrophilization treatment through acid catalysis, and water in the air also participates in the reaction during grafting, so that in order to obtain a better hydrophobic effect, the humidity in the air is required to be controlled, and therefore, the PDMS film with the functions of hydrophobic super-slip and enrichment is obtained on the surface of the substrate.
Example 2
The method for applying the ordered localized nano structure for realizing enrichment detection to the enrichment detection of the molecules to be detected in the aqueous solution comprises the following steps:
Taking an aqueous solution containing pyridine molecules as a sample to be detected;
Placing a sample to be detected on the surface of the ordered localized nano structure for realizing enrichment detection; the super-smooth surface is utilized, so that a sample to be detected can spontaneously concentrate to a central SERS locus area on the super-smooth surface;
Further evaporating water in the aqueous solution, and continuously gathering and enriching the sample to be detected to an SERS site area under the action of PDMS along with the evaporation of water molecules, so that pyridine molecules in the sample to be detected are continuously gathered in the SERS site area;
And after the pyridine molecules in the aqueous solution are enriched in the SERS locus region, carrying out Raman spectrum test on the molecules to be tested in the SERS locus region. Because of the enrichment, pyridine with low content in the aqueous solution can be enriched to enhance the signal.
The above-described embodiment is only a preferred embodiment of the present invention, and is not limited in any way, and other variations and modifications may be made without departing from the technical aspects set forth in the claims.
Claims (9)
1. The preparation method of the ordered localized nano structure for realizing enrichment detection is characterized by comprising the following steps of:
(A) Self-assembling PS balls in the upper limit region of the silicon wafer, reducing the size of the PS balls through etching treatment, enabling a certain interval to exist between the PS balls, and obtaining a PS ball array on the silicon wafer;
(B) Magnetron sputtering a layer of Cr on the surface of the silicon wafer as a mask, removing the PS balls from the surface of the silicon wafer, and generating a naked silicon wafer area after the PS balls are removed; heating and soaking a silicon wafer by using NaOH solution, and obtaining an ordered array formed by a concave pyramid structure on the surface of the silicon wafer;
(C) Growing a layer of substance for improving the SERS performance in the concave pyramid structure, so as to obtain a SERS locus area on the surface of the silicon wafer;
(D) Setting a layer of PDMS film on the surface of the silicon wafer except for the SERS locus area to form an ultra-smooth surface; the super-slip surface is used for enabling the sample to be tested to concentrate towards the central SERS locus area, and as the water molecules in the sample to be tested evaporate, the molecules to be tested in the sample to be tested are continuously gathered and enriched under the action of PDMS, so that the molecules to be tested in the sample to be tested are continuously gathered in the SERS locus area.
2. The method according to claim 1, wherein in the step (a), the domain-limited self-assembly specifically comprises: the range of the close-packed hexagonal stacked single-layer PS ball array is controlled within the limit range of 200-300 mu m in length and width, and the diameter of the PS balls is 500nm.
3. The method according to claim 1, wherein in the step (B), the step of heating and soaking with NaOH solution comprises, in particular, soaking in NaOH solution at 80 ℃ for 1-3 min to obtain a concave pyramid structure in the exposed silicon wafer area; as the soaking time increases, the depth of the concave pyramid becomes gradually larger.
4. The method of claim 1, wherein in step (C), the growing a layer of SERS enhancing material comprises:
firstly, performing magnetron sputtering Au treatment on the concave pyramid structure;
And then, ag 7O8NO3 is electrochemically deposited in the concave pyramid structure, then Ag 7O8NO3 is reduced to Ag, and simple substance Ag with nanoscale holes on the surface is obtained in the concave pyramid.
5. The method of claim 4, wherein in the step (D), the specific method for disposing a PDMS film comprises:
And carrying out hydrophilization treatment on the surface of the region except the SERS site region on the surface of the silicon wafer, and grafting the surface of the hydrophilized region by using a PDMS precursor solution under the conditions of 60% of ambient humidity and acid catalysis to obtain the PDMS film.
6. An ordered localized nanostructure for enrichment detection, the ordered localized nanostructure for enrichment detection being produced by the method of claim 5,
The ordered localized nanostructure with enrichment detection comprises a SERS locus region and an ultra-smooth surface; the length and width of the SERS locus area are all in the range of 200-300 mu m, the periphery of the SERS locus area is an ultra-smooth surface, and the ultra-smooth surface is composed of a PDMS film;
The SERS site region consists of an array of recessed pyramids,
The spacing between the array of recessed pyramids is 20nm-100nm,
An Au layer is sputtered in the concave pyramid in a magnetron manner;
The Au layer is also provided with simple substance Ag with nanoscale holes on the surface.
7. The ordered localized nanostructure of claim 6, wherein the Au layer has a thickness of 5nm to achieve enrichment detection.
8. The application of an ordered localized nanostructure having enrichment detection as claimed in claim 6 or 7 to enrichment detection of molecules to be detected in aqueous solution, comprising the steps of:
Taking an aqueous solution containing molecules to be tested as a sample to be tested;
placing a sample to be detected on the surface of the ordered localized nano structure for realizing enrichment detection; the super-smooth surface is utilized to enable the sample to be tested to be concentrated towards the central SERS locus area on the super-smooth surface;
Evaporating water in the aqueous solution, and continuously gathering and enriching the sample to be detected to an SERS site area under the action of PDMS along with the evaporation of water molecules, so that molecules to be detected in the sample to be detected are continuously gathered in the SERS site area;
and after the molecules to be detected in the aqueous solution are enriched in the SERS locus region, carrying out Raman spectrum test on the molecules to be detected in the SERS locus region.
9. The use according to claim 8, wherein the pitch between the array of recessed pyramids is 20nm-100nm and the molecule to be detected is a pyridine molecule.
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