CN106567119A - Polymer based nanometer cone structure SERS substrate and preparation method - Google Patents
Polymer based nanometer cone structure SERS substrate and preparation method Download PDFInfo
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- CN106567119A CN106567119A CN201610912964.2A CN201610912964A CN106567119A CN 106567119 A CN106567119 A CN 106567119A CN 201610912964 A CN201610912964 A CN 201610912964A CN 106567119 A CN106567119 A CN 106567119A
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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 invention discloses a polymer based nanometer cone structure SERS substrate which is prepared from a polymer with a nanometer cone structure and a three-dimensional noble metal nanometer particle array; and noble metal nanometer particles are uniformly inlaid in the polymer nanometer cone structure surface. The SERS substrate has the advantages of excellent transparency, excellent flexibility, excellent uniformity, high sensitivity, light weight, foldable ability, portability and liability in treatment and can be applied to the field of in-situ detection of pesticide residues on the surfaces of vegetables and pollutants in an aqueous solution. The invention also discloses a preparation method of the SERS substrate. The preparation method comprises the following steps: preparing a conical porous alumina template by utilizing a multistep anodic oxidation method; depositing the noble metal nanometer particles on the conical porous alumina template; and copying the nanometer cone structure of the conical porous alumina template on the polymer by utilizing a nanometer imprinting technology, and transferring the noble metal nanometer particles onto the polymer to obtain the SERS substrate. The method is simple in preparation process and lower in cost and is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to optics field, more particularly to a kind of nanocone structures SERS substrates and system based on polymer
Preparation Method.
Background technology
SERS (SERS) technology, is that a kind of strong analytical chemistry, electrochemistry, catalysis, medical science are examined
Disconnected instrument, can provide nondestructive, overdelicate sign, and detectable limit can arrive unimolecule rank.SERS is unique
Performance attracted the concern of vast researcher, increasing new SERS substrates to be reported.Even so, before
The most of work of research is concentrated on and designs new substrate to obtain higher Raman enhancer, but is less focused on more
Actual application.The SERS substrates of flexible and transparent can be good at realizing, in-situ Raman detection real-time to various samples.Up till now
Till, have concurrently excellent transparency with it is flexible, while substrate with higher SERS sensitivity is less being reported.In addition, can be just
Victory preparation low cost, uniform, repeatability are good, large area has highly sensitive SERS substrates concurrently simultaneously, still fill at present
Full challenge.This is probably the research direction of a great prospect in Raman spectroscopy, the real world applications to promoting SERS technologies
It is significant.
Porous alumina formwork is excellent because its distinctive regularly arranged, low cost, production efficiency are high and structure is adjustable etc.
Point, is widely used in the preparation of various nano materials and device.The anti-reflective effect of its taper nanostructured, can make it is more enter
Penetrate light to enter in structure and then absorbed, to produce more emergent lights；On the other hand, emergent light can run into many in outgoing
Pore structure, is transmitted away can more light.On the one hand increase absorbing incident light absorption efficiency, on the other hand increase scattered light
Outgoing efficiency, the substrate prepared based on this kind of structure can preferably improve in theory SERS performances.However, tapered, porous oxidation
The few studied report of research application of the aluminum alloy pattern plate in SERS fields.
The content of the invention
For problems of the prior art, the present invention is to provide a kind of low cost, easily prepare, suitable for extensive
Industrial flexible and transparent based on polymer nanocomposite wimble structure SERS substrates and preparation method thereof.
As an aspect of of the present present invention, the invention provides a kind of nanocone structures SERS substrates based on polymer, bag
The polymer with nanocone structures and three-dimensional noble metal nano-particle array are included, noble metal nano particles are uniformly embedded in nanometer
Wimble structure surface.
The characteristics of flexible, transparent because polymer has so that the nanocone structures SERS substrates based on polymer can
, in-situ Raman detection real-time to various samples is realized well.
Further, have a good SERS performances to guarantee nanocone structures SERS substrates, noble metal nano particles it is big
It is little for 5nm～20nm.
As another aspect of the present invention, the invention provides a kind of nanocone structures SERS substrates based on polymer
Preparation method, 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；
(3) using nano-imprinting method the nanocone structures of tapered, porous alumina formwork are copied on polymer and is incited somebody to action
Noble metal granule is transferred on polymer；
(4) tapered, porous alumina formwork is separated with polymer, is obtained based on the nanocone structures SERS bases of polymer
Bottom.
Preferably, nano-imprinting method comprises the steps in step (3)：
(31) the tapered, porous alumina formwork that polymer there are noble metal nano particles with deposition is placed on sample stage, is taken out
After vacuum, 155 DEG C～220 DEG C are heated to；
(32) 30bar～40bar is progressively pressurized to, and keeps 10min～20min；
(33) pressure is decreased to into 10bar～20bar, keeps 1min～2min；
(34) again pressure risen to into 30bar～40bar, and keeps 10min～20min；
(35) after being cooled to below polymer glass temperature, decompression step by step.
Preferably, in step (4) tapered, porous alumina formwork is separated with polymer using mechanical stripping, the method work
Skill is simple, and tapered, porous alumina formwork can 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, possesses following technology compared with prior art, mainly according to the above-mentioned technology design of the present invention excellent
Point：
1st, due to using polymer as carrier so that the SERS substrates have flexible, transparent, light weight, it is foldable, portable,
The advantage such as disposable, can be widely used in the original of pollutant in the in-situ investigation of gourd, fruit and vegetable surface residues of pesticides, the aqueous solution
Position detection, the rapid field analysis of microorganism real-time detection and chemical reaction etc. field, and its Fluorescence Increasing, etc. from
Also there is potential using value in the fields such as daughter waveguide, catalysis, sensing, transparent electrode material.
2nd, the preparation method realizes the transfer of three-dimensional nanoparticles.By nanometer embossing, not only by tapered, porous
Nanocone structures on alumina formwork have been copied on polymer, while will be deposited on tapered, porous alumina formwork three
Dimension metal nanoparticle array has completely been transferred on polymer.
3rd, the preparation process is simple, cost are relatively low, be suitable for large-scale industrial production；After mechanical stripping, tapered, porous oxygen
Change aluminium nano-imprint stamp reusable.
Description of the drawings
The schematic diagram of the nanocone structures SERS substrates based on polymer that Fig. 1 is provided for the present invention；
The flow chart of the preparation method of the nanocone structures SERS substrates based on polymer that Fig. 2 is provided for the present invention；
Fig. 3 is the schematic diagram of the tapered, porous alumina formwork prepared by multistep anodic oxidation method；
Fig. 4 is the schematic diagram of the tapered, porous alumina formwork that deposition has silver nano-grain；
Fig. 5 is the schematic diagram through nano impression post-consumer polymer and tapered, porous alumina formwork；
The electronic display of nanocone structures SERS substrates based on polymer of the Fig. 6 to be prepared using the method for providing of the invention
Micro mirror photo.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only the embodiment of a part of embodiment of the present invention rather than whole.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
As shown in figure 1, the nanocone structures SERS substrates based on polymer that the present invention is provided, 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 interact and produce metal surface etc.
Ion resonance body, so as to cause local Electromagnetic enhancement, greatly strengthens the Raman signal that material is detected in substrate or near substrate.
The SERS performance good to guarantee the nanocone structures SERS substrates for being based on polymer, prepares preferably three-dimensional your gold
Category nano-array, the size of noble metal granule is 5nm～20nm.
As shown in Fig. 2 the present invention is provided based on the preparation method of polymer nanocomposite wimble structure SERS substrates, including following step
Suddenly：
(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) using nano-imprinting method the nanocone structures of tapered, porous alumina formwork are copied on polymer and is incited somebody to action
Noble metal nano particles are transferred on polymer；
(4) tapered, porous alumina formwork is separated with polymer, is obtained based on the nanocone structures SERS bases of polymer
Bottom.
Tapered, porous anodic oxidation aluminium formwork is prepared by multistep anodic oxidation method, and in nanocone structures surface deposition
Noble metal nano particles, by nano-imprinting method by the nanocone structures complete copy on tapered, porous alumina formwork to poly-
On compound, and it is transferred to noble metal nano particles are complete on polymer so that there is rule in array arrangement on polymer
Nanocone structures, and noble metal nano particles are evenly distributed on the nanocone structures of polymer, are provided by the present invention
Nanocone structures SERS substrate function admirables prepared by method, this method preparation process is simple, cost are relatively low, be suitable for extensive
Industrial production.
The first embodiment of the preparation method of the nanocone structures SERS substrates based on polymer that the present invention is provided, including
Following steps：
(1) tapered, porous alumina formwork is prepared by multistep anodic oxidation method, is comprised the steps：
(11) aluminium foil that mass percent is more than 99.99% is put in the oxalic acid solution of 0.3mol/L carries out the first step
Oxidation, oxidation voltage is 40V, and oxidizing temperature is 3 DEG C, and first step oxidization time is 4h.
(12) the anodised aluminium foil of the first step will be carried out and is placed in leaching in the mixed liquor of 6wt% phosphoric acid and 1.8wt% chromic acid
Bubble 12h, the temperature 60 C of mixed liquor；For removing the oxide layer of aluminium foil.
(13) aluminium foil after oxide layer is put in the oxalic acid solution of 0.3mol/L carries out second step oxidation, oxidation
Voltage is 40V, and oxidizing temperature is 10 DEG C, and oxidization time is 15s.
(14) aluminium foil aoxidized through second step is expanded in the mass percent that temperature is 30 DEG C is 5% phosphoric acid solution
Hole, pore-enlargement is 8min.
(15) repeat step (13) and step (14), number of repetition is 5 times.
(16) repeat step (13) once, and after deionized water is rinsed, obtain tapered, porous aluminum oxide as shown in Figure 3
Template, including the Woelm Alumina 4 with pyramidal structure and aluminium foil 3.
(2) using the method for plasma sputtering, in the silver nano-grain of tapered, porous alumina formwork surface depositing homogeneous.
Tapered, porous alumina formwork is placed in vacuum room, silver nano-grain, sputtering current 2mA, sputtering time are sputtered after vacuumizing
3min, obtaining deposition as shown in Figure 4 has the tapered, porous alumina formwork of silver nano-grain, including the porous with pyramidal structure
Aluminum oxide 4, silver nano-grain 2 and aluminium foil 3.
(3) nanocone structures of tapered, porous alumina formwork are copied on PMMA films simultaneously using nano-imprinting method
Silver nano-grain is transferred on PMMA films, is comprised the steps：
(31) polymethyl methacrylate (PMMA) film and deposition are had the tapered, porous oxidation aluminum dipping form of silver nano-grain
Plate is placed on sample stage, after vacuumizing, is heated to 180 DEG C；
(32) 40bar is progressively pressurized to, and keeps 10min；
(33) pressure is decreased to into 20bar, keeps 1min；
(34) again pressure risen to into 40bar, 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 through hot nano-imprinting method
On PMMA films 5, the silver nano-grain 2 being deposited on nanocone structures is also transferred on PMMA films 5.
(4) after cooling down, by PMMA films from tapered, porous alumina formwork surface mechanical stripping, base as shown in Figure 1 is obtained
In the SERS substrates of the nanocone structures of polymer.
Taper nano-pore structure is prepared on aluminium foil by multistep anodic oxidation method, obtained nanostructured 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 films, and it is thin that silver nano-grain is transferred to into PMMA
Nanocone structures surface on film, is obtained based on the nanocone structures SERS substrates of PMMA films.The method system that the present invention is provided
Standby process is simple, and preparation cost is relatively low, is conducive to large-scale popularization and application.
The second embodiment of the preparation method of the nanocone structures SERS substrates based on polymer that the present invention is provided, 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) using the method for plasma sputtering, in the gold nano grain of tapered, porous alumina formwork surface depositing homogeneous.
Tapered, porous alumina formwork is placed in vacuum room, gold nano grain, sputtering current 3mA, sputtering time are sputtered after vacuumizing
2min, obtains depositing the tapered, porous alumina formwork of gold nano grain.
(3) nanocone structures of tapered, porous alumina formwork are copied on PMMA films simultaneously using nano-imprinting method
Gold nano grain is transferred on PMMA films, is comprised the steps；
(31) the tapered, porous alumina formwork that PMMA films have gold nano grain with deposition is placed on sample stage, takes out true
After sky, 200 DEG C are heated to；
(32) 35bar is progressively pressurized to, and keeps 15min；
(33) pressure is decreased to into 15bar, keeps 1.5min；
(34) again pressure risen to into 35bar, and keeps 15min；
(35) after being cooled to 80 DEG C, decompression step by step.
(4) after cooling down, by PMMA films from tapered, porous alumina formwork surface mechanical stripping, that is, obtain thin based on PMMA
The nanocone structures SERS substrates 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 films by nano-imprinting method, and by Jenner
Rice grain is transferred on PMMA films, is obtained based on the nanocone structures SERS substrates of PMMA films.
The 3rd embodiment of the metal nano sieve series Preparation Method based on polymer that the present invention is provided, comprises the steps：
(1) tapered, porous alumina formwork is prepared by multistep anodic oxidation method, with first embodiment step (1) phase
Together.
(2) using the method for plasma sputtering, on tapered, porous alumina formwork surface gold nano grain is deposited.By taper
Porous alumina formwork is placed in vacuum room, and gold nano grain, sputtering current 5mA, sputtering time 2min are sputtered after vacuumizing.I.e.
Obtain depositing the tapered, porous alumina formwork of gold nano grain.
(3) nanocone structures of tapered, porous alumina formwork are copied on PMMA films simultaneously using nano-imprinting method
Gold nano grain is transferred on PMMA films, is comprised the steps：
(31) the tapered, porous alumina formwork that PMMA films have gold nano grain with deposition is placed on sample stage, takes out true
After sky, 220 DEG C are heated to；
(32) 30bar is progressively pressurized to, and keeps 20min；
(33) pressure is decreased to into 10bar, keeps 2min；
(34) again pressure risen to into 30bar, and keeps 20min；
(35) after being cooled to 80 DEG C, decompression step by step.
(4) after cooling down, by PMMA films from tapered, porous alumina formwork surface mechanical stripping, that is, obtain being inlaid with gold
The polymer nanocomposite wimble structure SERS substrates 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 films by nano-imprinting method, and by your gold
Metal nano-particle is transferred on PMMA films, is obtained based on the nanocone structures SERS substrates of PMMA films.
The fourth embodiment of the preparation method based on polymer nanocomposite wimble structure SERS substrates that the present invention is provided, 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) using the method for plasma sputtering, in tapered, porous alumina surface gold nano grain is deposited.By tapered, porous
Alumina formwork is placed in vacuum room, and gold nano grain, sputtering current 3mA, sputtering time 1.5min are sputtered after vacuumizing.Obtain final product
There is the tapered, porous alumina formwork of gold nano grain to deposition.
(3) using nano-imprinting method the nanocone structures of tapered, porous alumina formwork are copied on polymer and is incited somebody to action
Noble metal nano particles are transferred on polyolefin resin film；
(31) the tapered, porous alumina formwork that polyolefin resin film has gold nano grain with deposition is placed in into sample stage
On, after vacuumizing, it is heated to 155 DEG C；
(32) 40bar is progressively pressurized to, and keeps 20min；
(33) pressure is decreased to into 10bar, keeps 1min；
(34) again pressure risen to into 40bar, and keeps 20min；
(35) after being cooled to 50 DEG C, decompression step by step.
(4) after cooling down, by polyolefin resin film from tapered, porous alumina formwork surface mechanical stripping, that is, it is based on
The nanocone structures SERS substrates 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, are obtained based on the nanocone structures SERS of polyolefin resin film
Substrate.
It is illustrated in figure 6 the nanocone structures SERS substrates based on polymer prepared by the method provided by the present invention
Electron micrograph, the nanocone structures SERS underlying structures based on polymer are uniform, and tapered, porous oxygen is replicated exactly
Change the nanocone structures of aluminium, and successfully inlay gold nano grain.Its transmissivity in visible-range can reach 70%；
To the enhancer of R6G (rhodamine 6G) up to 108The order of magnitude, R6G concentration is 10-12Remain to measure obvious Raman letter during M
Number.Excellent repeatability is shown based on the nanocone structures SERS substrates of polymer, the intensity of the main Raman peaks of six R6G
Relative standard deviation value is respectively less than 11%.And nanocone structures SERS substrates have extraordinary flexible characteristic, through up to a hundred
After secondary bending R6G tests are remained to obtain stable Raman signal.
As it will be easily appreciated by one skilled in the art that the foregoing is only presently preferred embodiments of the present invention, not to
The present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc. are limited, all should be included
Within protection scope of the present invention.
Claims (8)
1. a kind of nanocone structures SERS substrates based on polymer, it is characterised in that include with nanocone structures 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. nanocone structures SERS substrates according to claim 1, it is characterised in that the noble metal nano particles it is big
It is little for 5nm～20nm.
3. a kind of preparation method of nanocone structures SERS substrates as claimed in claim 1, it is characterised in that including following step
Suddenly：
(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 by your gold using nano-imprinting method
Metal particles are transferred on polymer；
(4) tapered, porous alumina formwork is separated with polymer, is obtained based on the nanocone structures SERS substrates of polymer.
4. preparation method according to claim 3, it is characterised in that in the step (3) nano-imprinting method include as
Lower step：
(31) the tapered, porous alumina formwork that polymer there are noble metal nano particles with deposition is placed on sample stage, is vacuumized
Afterwards, 155 DEG C～220 DEG C are heated to；
(32) 30bar～40bar is progressively pressurized to, and keeps 10min～20min；
(33) pressure is decreased to into 10bar～20bar, keeps 1min～2min；
(34) again pressure risen to into 30bar～40bar, and keeps 10min～20min；
(35) after being cooled to below polymer glass temperature, decompression step by step.
5. the preparation method according to claim 3 or 4, it is characterised in that be by mechanically pulling off and will bore in the step (4)
Shape porous alumina formwork is separated with polymer.
6. the preparation method according to claim 3 or 4, it is characterised in that the nanocone knot of the porous alumina formwork
The depth-to-width ratio of structure is 0.5～5.0.
7. the preparation method according to claim 3 or 4, it is characterised in that the noble metal nano particles are gold nano
Grain or silver nano-grain.
8. the preparation method according to claim 3 or 4, it is characterised in that the polymer is thermoplastic macromolecule material.
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| CN107991281A (en) * | 2017-11-23 | 2018-05-04 | 华中农业大学 | The preparation method of flexible SERS substrates and its for specific detection PAT |
| CN108046211A (en) * | 2017-11-23 | 2018-05-18 | 中国科学院合肥物质科学研究院 | A kind of preparation method and applications of silicon substrate thorniness shape nanocone oldered array |
| CN108375567A (en) * | 2018-02-24 | 2018-08-07 | 国家纳米科学中心 | A kind of surface-enhanced Raman substrate and preparation method thereof |
| CN108436253A (en) * | 2018-02-26 | 2018-08-24 | 北京航空航天大学 | A kind of preparation method of SERS- fluorescent dual modules formula metal enhancing substrate |
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| CN111455319A (en) * | 2020-05-15 | 2020-07-28 | 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 |
| CN114888276A (en) * | 2022-05-12 | 2022-08-12 | 集美大学 | Preparation method and application of chain-like high polymer modified nano particles |
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