CN106567119B - A kind of nanocone structures SERS substrate and preparation method based on polymer - Google Patents
A kind of nanocone structures SERS substrate and preparation method based on polymer Download PDFInfo
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- CN106567119B CN106567119B CN201610912964.2A CN201610912964A CN106567119B CN 106567119 B CN106567119 B CN 106567119B CN 201610912964 A CN201610912964 A CN 201610912964A CN 106567119 B CN106567119 B CN 106567119B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/045—Anodisation of aluminium or alloys based thereon for forming AAO templates
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/006—Nanoparticles
Abstract
The nanocone structures SERS substrate based on polymer that the invention discloses a kind of includes that there is the polymer of nanocone structures and three-dimensional noble metal nano-particle array, noble metal nano particles to be uniformly embedded in polymer nanocomposite wimble structure surface.The SERS substrate has excellent transparency, flexibility, uniformity and high sensitivity, and has light weight, foldable, portable and easy to handle advantage, can be applicable to the in-situ investigation field of pollutant in vegetable surface pesticide residue and aqueous solution.And a kind of preparation method of SERS substrate is disclosed, tapered, porous alumina formwork is prepared including the use of the method for multistep anodic oxidation；The depositing noble metal nano particle on tapered, porous alumina formwork；The nanocone structures of tapered, porous alumina formwork are copied on polymer using nanometer embossing, and noble metal nano particles are transferred on polymer, obtain SERS substrate.This method preparation process is simple, and cost is relatively low, is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to optical device field, in particular to a kind of nanocone structures SERS substrate and system based on polymer
Preparation Method.
Background technique
Surface enhanced Raman scattering (SERS) technology is that a kind of strong analytical chemistry, electrochemistry, catalysis, medicine are examined
Disconnected tool, can provide nondestructive, overdelicate characterization, detectable limit can arrive unimolecule rank.SERS is unique
Performance attracted the concern of vast researcher, more and more novel SERS substrates are reported.Nevertheless, before
The most of work of research concentrates on designing new substrate to obtain higher Raman enhancement factor, but less focuses on more
Actual application.The SERS substrate of flexible and transparent can be good at realizing that real-time, in-situ Raman detects to various samples.To current
Until, excellent transparency and flexibility are had both, while having the substrate of higher SERS sensitivity is less to be reported.In addition, can be just
Victory preparation low cost, uniform, reproducibility is good, large area has both highly sensitive SERS substrate simultaneously, still fills at present
Full challenge.This may be the research direction of a great prospect in Raman spectroscopy, to the practical application for pushing SERS technology
It is of great significance.
Porous alumina formwork is adjustable etc. excellent due to its distinctive regularly arranged, at low cost, high production efficiency and structure
Point is widely used in the preparation of various nano materials and device.The anti-reflective effect of its taper nanostructure can make more to enter
It penetrates light to enter in structure and then be absorbed, to generate more emergent lights；On the other hand, emergent light can encounter more in outgoing
Pore structure can be such that more light are transmitted away.On the one hand increase absorbing incident light absorption efficiency, on the other hand increase scattering light
Outgoing efficiency, the substrate based on the preparation of such structure theoretically can preferably improve SERS performance.However, tapered, porous aoxidizes
The few studied report of research application of the aluminum alloy pattern plate in the field SERS.
Summary of the invention
Aiming at the problems existing in the prior art, it prepares, be suitable on a large scale the present invention is to provide a kind of low cost, easily
Industrial flexible and transparent based on polymer nanocomposite wimble structure SERS substrate and preparation method thereof.
As an aspect of of the present present invention, the nanocone structures SERS substrate based on polymer that the present invention provides a kind of, packet
It includes polymer and three-dimensional noble metal nano-particle array, noble metal nano particles with nanocone structures and is uniformly embedded in nanometer
Wimble structure surface.
Since polymer has the characteristics that flexible, transparent, enable the nanocone structures SERS substrate based on polymer
Realize that real-time, in-situ Raman detects to various samples well.
Further, to ensure that nanocone structures SERS substrate has a good SERS performance, noble metal nano particles it is big
Small is 5nm~20nm.
As another aspect of the present invention, the nanocone structures SERS substrate based on polymer that the present invention provides a kind of
Preparation method, comprising the following steps:
(1) tapered, porous alumina formwork is prepared by multistep anodic oxidation method；
(2) in the noble metal nano particles of tapered, porous alumina formwork surface depositing homogeneous；
(3) nanocone structures of tapered, porous alumina formwork are copied on polymer and is incited somebody to action using nano-imprinting method
Noble metal granule is transferred on polymer；
(4) tapered, porous alumina formwork is separated with polymer, the nanocone structures SERS base based on polymer is made
Bottom.
Preferably, nano-imprinting method includes the following steps: in step (3)
(31) polymer is placed on sample stage with the tapered, porous alumina formwork for being deposited with noble metal nano particles, is taken out
After vacuum, it is heated to 155 DEG C~220 DEG C；
(32) it is gradually pressurized to 30bar~40bar, and keeps 10min~20min；
(33) pressure is decreased to 10bar~20bar, keeps 1min~2min；
(34) pressure is risen into 30bar~40bar again, and keeps 10min~20min；
(35) after being cooled to polymer glass temperature or less, decompression step by step.
Preferably, tapered, porous alumina formwork is separated with polymer using mechanical stripping in step (4), this method work
Skill is simple, and tapered, porous alumina formwork may be reused.
Preferably, the depth-to-width ratio of the nanocone structures of tapered, porous alumina formwork is 0.5~5.0, in order to pass through nanometer
Method for stamping gain freedom standing polymer nanocomposite cone array.
Preferably, the noble metal nano particles are gold nano grain or silver nano-grain.
Preferably, the polymer is thermoplastic macromolecule material.
In general, above-mentioned technical concept according to the invention compared with prior art, it is excellent mainly to have technology below
Point:
1, due to using polymer as carrier so that the SERS substrate have flexible, transparent, light weight, it is foldable, portable,
The advantages such as easy to handle, can be widely used in the in-situ investigation of gourd, fruit and vegetable surface pesticide residue, in aqueous solution pollutant original
Rapid field analysis etc. the field of position detection, microorganism real-time detection and chemical reaction, and its fluorescence enhancement, etc. from
Also there is potential using value in the fields such as daughter waveguide, catalysis, sensing, transparent electrode material.
2, the preparation method realizes the transfer of three-dimensional nanoparticles.By nanometer embossing, not only by tapered, porous
Nanocone structures on alumina formwork have copied on polymer, while three will be deposited on tapered, porous alumina formwork
Dimension metal nanoparticle array has completely been transferred on polymer.
3, the preparation process is simple, cost is relatively low, is suitable for large-scale industrial production；After mechanical stripping, tapered, porous oxygen
It is reusable to change aluminium nano-imprint stamp.
Detailed description of the invention
Fig. 1 is the schematic diagram of the nanocone structures SERS substrate provided by the invention based on polymer；
Fig. 2 is the flow chart of the preparation method of the nanocone structures SERS substrate provided by the invention based on polymer；
Fig. 3 is the schematic diagram of the tapered, porous alumina formwork prepared by multistep anodic oxidation method；
Fig. 4 is the schematic diagram for being deposited with the tapered, porous alumina formwork of silver nano-grain；
Fig. 5 is the schematic diagram by nano impression post-consumer polymer and tapered, porous alumina formwork；
Fig. 6 is the electronic display using the nanocone structures SERS substrate based on polymer of method provided by the invention preparation
Micro mirror photo.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiment be only a part of the embodiments of the present invention instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
As shown in Figure 1, the nanocone structures SERS substrate provided by the invention based on polymer, including with nanocone knot
The polymer 1 of structure and three-dimensional noble metal nano-particle array 2, noble metal nano particles are uniformly embedded in nanocone structures surface,
Form three-dimensional noble metal nano-particle array.Due to noble metal nano structure can exciting light interaction generate metal surface etc.
Ion resonance body greatly enhances in substrate so as to cause local Electromagnetic enhancement or substrate nearby detects the Raman signal of substance.
To ensure the good SERS performance of nanocone structures SERS substrate based on polymer, your preferable three-dimensional gold prepared
Belong to nano-array, the size of noble metal granule is 5nm~20nm.
As shown in Fig. 2, the present invention provides the preparation method based on polymer nanocomposite wimble structure SERS substrate, including following step
It is rapid:
(1) tapered, porous alumina formwork is prepared by multistep anodic oxidation method；
(2) in the noble metal nano particles of tapered, porous alumina formwork surface depositing homogeneous；
(3) nanocone structures of tapered, porous alumina formwork are copied on polymer and is incited somebody to action using nano-imprinting method
Noble metal nano particles are transferred on polymer；
(4) tapered, porous alumina formwork is separated with polymer, the nanocone structures SERS base based on polymer is made
Bottom.
Tapered, porous anodic oxidation aluminium formwork is prepared by multistep anodic oxidation method, and is deposited on nanocone structures surface
Noble metal nano particles, by nano-imprinting method by the nanocone structures complete copy on tapered, porous alumina formwork to poly-
It closes on object, and noble metal nano particles is completely transferred on polymer, so that on polymer there is rule to arrange in array
Nanocone structures, and noble metal nano particles are evenly distributed on the nanocone structures of polymer, are provided through the invention
The nanocone structures SERS substrate function admirable of method preparation, this method preparation process is simple, cost is relatively low, it is extensive to be suitable for
Industrial production.
The first embodiment of the preparation method of nanocone structures SERS substrate provided by the invention based on polymer, including
Following steps:
(1) tapered, porous alumina formwork is prepared by multistep anodic oxidation method, included the following steps:
(11) aluminium foil that mass percent is 99.99% or more is put into the oxalic acid solution of 0.3mol/L and carries out the first step
Oxidation, oxidation voltage 40V, oxidizing temperature are 3 DEG C, and first step oxidization time is 4h.
(12) aluminium foil for carrying out first step anodic oxidation is placed in the mixed liquor of 6wt% phosphoric acid and 1.8wt% chromic acid and is soaked
Steep 12h, the temperature 60 C of mixed liquor；For removing the oxide layer of aluminium foil.
(13) aluminium foil after oxide layer is put into progress second step oxidation in the oxalic acid solution of 0.3mol/L, oxidation
Voltage is 40V, and oxidizing temperature is 10 DEG C, oxidization time 15s.
It (14) is to expand in 5% phosphoric acid solution in the mass percent that temperature is 30 DEG C by the aluminium foil by second step oxidation
Hole, pore-enlargement 8min.
(15) step (13) and step (14) are repeated, number of repetition is 5 times.
(16) it repeats step (13) once, and after being rinsed with deionized water, obtains tapered, porous aluminium oxide as shown in Figure 3
Template, including porous aluminas 4 and aluminium foil 3 with pyramidal structure.
(2) method for using plasma sputtering, in the silver nano-grain of tapered, porous alumina formwork surface depositing homogeneous.
Tapered, porous alumina formwork is placed in vacuum chamber, silver nano-grain, sputtering current 2mA, sputtering time are sputtered after vacuumizing
3min is deposited with the tapered, porous alumina formwork of silver nano-grain, including with the porous of pyramidal structure as shown in Figure 4
Aluminium oxide 4, silver nano-grain 2 and aluminium foil 3.
(3) nanocone structures of tapered, porous alumina formwork are copied on PMMA film simultaneously using nano-imprinting method
Silver nano-grain is transferred on PMMA film, is included the following steps:
(31) polymethyl methacrylate (PMMA) film is aoxidized into aluminum dipping form with the tapered, porous for being deposited with silver nano-grain
Plate is placed on sample stage, after vacuumizing, is heated to 180 DEG C；
(32) it is gradually pressurized to 40bar, and keeps 10min；
(33) pressure is decreased to 20bar, keeps 1min；
(34) pressure is risen into 40bar again, and keeps 10min；
(35) after being cooled to 90 DEG C, decompression step by step.
As described in Figure 5, the nanocone structures 4 of tapered, porous alumina formwork are copied to by hot nano-imprinting method
On PMMA film 5, the silver nano-grain 2 being deposited on nanocone structures is also transferred on PMMA film 5.
(4) after cooling, by PMMA film from tapered, porous alumina formwork surface mechanical stripping, base as shown in Figure 1 is obtained
In the SERS substrate of the nanocone structures of polymer.
Taper nano-pore structure is prepared on aluminium foil by multistep anodic oxidation method, nanostructure obtained is neatly advised
Then, then by plasma sputtering processes silver nano-grain is deposited on tapered, porous alumina formwork, by hot nano impression side
Method copies to the nanocone structures of tapered, porous alumina formwork on PMMA film, and it is thin that silver nano-grain is transferred to PMMA
The nanocone structures SERS substrate based on PMMA film is made in nanocone structures surface on film.Method system provided by the invention
Standby simple process, and preparation cost is lower, is conducive to promote and apply on a large scale.
The second embodiment of the preparation method of nanocone structures SERS substrate provided by the invention based on polymer, including
Following steps:
(1) tapered, porous alumina formwork is prepared by multistep anodic oxidation method, with (1) phase the step of first embodiment
Together.
(2) method for using plasma sputtering, in the gold nano grain of tapered, porous alumina formwork surface depositing homogeneous.
Tapered, porous alumina formwork is placed in vacuum chamber, gold nano grain, sputtering current 3mA, sputtering time are sputtered after vacuumizing
2min obtains the tapered, porous alumina formwork for being deposited with gold nano grain.
(3) nanocone structures of tapered, porous alumina formwork are copied on PMMA film simultaneously using nano-imprinting method
Gold nano grain is transferred on PMMA film, is included the following steps；
(31) PMMA film is placed on sample stage with the tapered, porous alumina formwork for being deposited with gold nano grain, is taken out true
After sky, it is heated to 200 DEG C；
(32) it is gradually pressurized to 35bar, and keeps 15min；
(33) pressure is decreased to 15bar, keeps 1.5min；
(34) pressure is risen into 35bar again, and keeps 15min；
(35) after being cooled to 80 DEG C, decompression step by step.
(4) after cooling, by PMMA film from tapered, porous alumina formwork surface mechanical stripping to get thin to PMMA is based on
The nanocone structures SERS substrate of film.
Tapered, porous alumina formwork is prepared by multistep anodic oxidation method, and in the gold nano of surface depositing homogeneous
Grain, is copied to the nanocone structures of tapered, porous alumina formwork on PMMA film by nano-imprinting method, and by Jenner
Rice grain is transferred on PMMA film, and the nanocone structures SERS substrate based on PMMA film is made.
The 3rd embodiment of metal nano sieve preparation method provided by the invention based on polymer, includes the following steps:
(1) tapered, porous alumina formwork is prepared by multistep anodic oxidation method, with first embodiment step (1) phase
Together.
(2) method for using plasma sputtering deposits gold nano grain on tapered, porous alumina formwork surface.By taper
Porous alumina formwork is placed in vacuum chamber, and gold nano grain, sputtering current 5mA, sputtering time 2min are sputtered after vacuumizing.I.e.
Obtain the tapered, porous alumina formwork for being deposited with gold nano grain.
(3) nanocone structures of tapered, porous alumina formwork are copied on PMMA film simultaneously using nano-imprinting method
Gold nano grain is transferred on PMMA film, is included the following steps:
(31) PMMA film is placed on sample stage with the tapered, porous alumina formwork for being deposited with gold nano grain, is taken out true
After sky, it is heated to 220 DEG C；
(32) it is gradually pressurized to 30bar, and keeps 20min；
(33) pressure is decreased to 10bar, keeps 2min；
(34) pressure is risen into 30bar again, and keeps 20min；
(35) after being cooled to 80 DEG C, decompression step by step.
(4) after cooling, by PMMA film from tapered, porous alumina formwork surface mechanical stripping to get to being inlaid with gold
The polymer nanocomposite wimble structure SERS substrate of grain.
Tapered, porous alumina formwork is prepared by multistep anodic oxidation method, and in the gold nano of surface depositing homogeneous
Grain, is copied to the nanocone structures of tapered, porous alumina formwork on PMMA film by nano-imprinting method, and by your gold
Metal nano-particle is transferred on PMMA film, and the nanocone structures SERS substrate based on PMMA film is made.
The fourth embodiment of preparation method provided by the invention based on polymer nanocomposite wimble structure SERS substrate, including such as
Lower step:
(1) tapered, porous alumina formwork is prepared by multistep anodic oxidation method, with first embodiment step (1) phase
Together.
(2) method for using plasma sputtering deposits gold nano grain in tapered, porous oxidation aluminium surface.By tapered, porous
Alumina formwork is placed in vacuum chamber, and gold nano grain, sputtering current 3mA, sputtering time 1.5min are sputtered after vacuumizing.To obtain the final product
To the tapered, porous alumina formwork for being deposited with gold nano grain.
(3) nanocone structures of tapered, porous alumina formwork are copied on polymer and is incited somebody to action using nano-imprinting method
Noble metal nano particles are transferred on polyolefin resin film；
(31) polyolefin resin film is placed in sample stage with the tapered, porous alumina formwork for being deposited with gold nano grain
On, after vacuumizing, it is heated to 155 DEG C；
(32) it is gradually pressurized to 40bar, and keeps 20min；
(33) pressure is decreased to 10bar, keeps 1min；
(34) pressure is risen into 40bar again, and keeps 20min；
(35) after being cooled to 50 DEG C, decompression step by step.
(4) after cooling, by polyolefin resin film from tapered, porous alumina formwork surface mechanical stripping to get to being based on
The nanocone structures SERS substrate of polyolefin resin film.
Tapered, porous alumina formwork is prepared by multistep anodic oxidation method, and in the gold nano of surface depositing homogeneous
Grain, is copied to the nanocone structures of tapered, porous alumina formwork on polyolefin resin film by nano-imprinting method, and
Noble metal nano particles are transferred on polyolefin resin film, the nanocone structures SERS based on polyolefin resin film is made
Substrate.
The nanocone structures SERS substrate based on polymer of the method preparation provided through the invention is provided
Electron micrograph, the nanocone structures SERS underlying structure based on polymer is uniform, accurately replicates tapered, porous oxygen
Change the nanocone structures of aluminium, and successfully inlays gold nano grain.Its transmissivity in visible-range can achieve 70%；
To the enhancement factor of R6G (rhodamine 6G) up to 108The order of magnitude, R6G concentration are 10-12It remains to measure apparent Raman letter when M
Number.Nanocone structures SERS substrate based on polymer shows excellent repeatability, the intensity of six main Raman peaks of R6G
Relative standard deviation value is respectively less than 11%.And nanocone structures SERS substrate has extraordinary flexible characteristic, process is up to a hundred
R6G test is remained to obtain stable Raman signal after secondary bending.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (6)
1. a kind of preparation method of nanocone structures SERS substrate, which comprises the following steps:
(1) tapered, porous alumina formwork is prepared by multistep anodic oxidation method；
(2) in the noble metal nano particles of tapered, porous alumina formwork surface depositing homogeneous；
Your (3) using nano-imprinting method the nanocone structures of tapered, porous alumina formwork are copied on polymer and by gold
Metal particles are transferred on polymer；
(4) tapered, porous alumina formwork is separated with polymer, the nanocone structures SERS substrate based on polymer is made；
Nano-imprinting method includes the following steps: in the step (3)
(31) polymer is placed on sample stage with the tapered, porous alumina formwork for being deposited with noble metal nano particles, is vacuumized
Afterwards, 155 DEG C~220 DEG C are heated to；
(32) it is gradually pressurized to 30bar, and keeps 20min；
(33) pressure is decreased to 10bar, keeps 2min；
(34) pressure is risen into 30bar again, and keeps 20min；
(35) after being cooled to polymer glass temperature or less, decompression step by step；
It include: with nanocone structures polymer using the nanocone structures SERS substrate made from above-mentioned steps based on polymer
(1) and three-dimensional noble metal nano-particle array (2), the noble metal nano particles are uniformly embedded in the nanocone structures table
Face.
2. preparation method according to claim 1, which is characterized in that the size of the noble metal nano particles be 5nm~
20nm。
3. preparation method according to claim 1, which is characterized in that be by mechanically pulling off in the step (4) by taper
Porous alumina formwork is separated with polymer.
4. preparation method according to claim 1, which is characterized in that the nanocone structures of the porous alumina formwork
Depth-to-width ratio is 0.5~5.0.
5. preparation method according to claim 1, which is characterized in that the noble metal nano particles are gold nano grain
Or silver nano-grain.
6. preparation method according to claim 1, which is characterized in that the polymer is thermoplastic macromolecule material.
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| CN111455319B (en) * | 2020-05-15 | 2022-07-01 | 中国科学院合肥物质科学研究院 | Gold-silver nanocone array with body-enhanced Raman scattering effect and preparation method and application thereof |
| CN112618803A (en) * | 2020-12-17 | 2021-04-09 | 大连理工大学 | Preparation method of temperature response type bionic nanocone dual-functional antibacterial surface |
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| CN106567119A (en) | 2017-04-19 |
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