CN109136847A - A kind of super-absorbent Ag-Au nanostructured surface laminated film and preparation method thereof - Google Patents
A kind of super-absorbent Ag-Au nanostructured surface laminated film and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to technical field of film preparation, specially super-absorbent Ag-Au nanostructured surface laminated film and preparation method thereof.The present invention uses conventional film plating process first, successively grows Ag, Al on substrate2O3And Ag;Then once made annealing treatment;After being cooled to room temperature, regrowth layer of Au film, and carry out double annealing;Wherein, outermost metal film forms Ag-Au nano particle after annealing.The present invention makes membrane stress change to form island structure, prepares the metallic particles of different-shape by twice annealing process.Wherein, outermost metal film becomes Ag-Au nano particle after annealing, can enhance the absorbability to light.Laminated film prepared by the present invention can be used as the substrate of Surface enhanced Raman scattering, has the characteristics that absorbability is strong, light absorption range is wide, stability is good, uniformity is good, the service life is long, can be used for the detection of a variety of biochemicals.
Description
Technical field
The invention belongs to technical field of film preparation, and in particular to a kind of nanostructured surface laminated film and its preparation side
Method.
Background technique
There is the composite film material of property to have very in Surface Enhanced Raman Scattering Spectrum (SERS) technology
Important application.Surface Enhanced Raman Scattering Spectrum is a kind of detection means of high surface sensitivity, can be to various biologies, change
Credit is effectively detected, and is had in fields such as biomedicine, safety inspection, Food Monitoring, medical treatment & healths very extensive
Application.The current main direction of studying of SERS be on the basis of low cost, being suitble to large area preparation, prepare high enhancing because
Sub, uniform good, reusable substrate material.However mainstream preparation process includes electron beam lithography, nano impression etc. at present,
These method preparation costs are very high and are difficult to large area preparation production, and the SERS substrate majority of mainstream can only be at certain at present
It uses, specific some substances can only be detected under one wavelength.Therefore SERS substrate material has considerable room for improvement.
The method that Nan Zhang et al. is combined using mim structure with metal nanoparticle will excite Raman to enhance
Upper layer absorbing material of the Ag nano particles as mim structure, while utilizing 70 nm SiO2It is situated between with 150 nm Al as space
Matter layer and metal back reflection layer, can be in the detection of wider wave-length coverage progress SERS
(UltrabroadbandMetasurface for Efficient Light Trapping and Localization:A
Universal Surface-Enhanced Raman Spectroscopy Substrate for “All” Excitation
Wavelengths).This mim structure can enhance surface layer absorbing material for the absorbability of luminous energy, and furthermore total exists
The wavelength of 400-1000 nm range has very strong absorbability, can cover the full spectral limit of mainstream Raman spectrum.However this
Kind mim structure uses Ag particle as upper layer absorbing material, easily oxidation by air, to reduce its absorbent properties.And this
The spatially uniform of kind Ag particle surface is bad, can not carry out quantitative detection.
In general, the metal material that can enhance surface Raman has gold, silver and bronze etc., what different metal materials can excite
LSPR wave band is not also identical.Usually Au is able to detect a variety of different types of molecules, including antigen-antibody, DNA etc..Ag has
Better detection performance, but since Ag is easy to oxidize, the SERS substrate of Ag preparation often has lower service life, mesh
The substrate of preceding commercialization is still based on Au.Therefore, the present invention uses Ag-Au composite particles surface, and Raman detection both can be enhanced
Signal, and its service life can be improved.
Summary of the invention
The purpose of the present invention is to provide it is a kind of it is at low cost, can be mass-produced, uniformity is good, good reliability nano junction
Structure surface recombination film and preparation method thereof.
The preparation method of nanostructured surface laminated film provided by the invention, including, using conventional film plating process (such as magnetic
Control sputtering, thermal evaporation, electron beam evaporation etc.), on substrate on successively grow Ag, Al2O3And Ag, then once annealed
Processing;After being cooled to room temperature, regrowth layer of Au film, and carry out double annealing;Wherein, outermost metal film shape after annealing
At Ag-Au nano particle.The present invention is made membrane stress change to form island structure, is prepared by twice annealing process
The metallic particles of different-shape.
The preparation method of nanostructured surface laminated film provided by the invention, steps are as follows for specific steps:
(1) Ag, Al are successively grown on substrate2O3And Ag;
(2) it is made annealing treatment under ar gas environment;150-250 DEG C of temperature, time 1-1.5 h;
(3) it waits substrate to be down to room temperature, grows layer of Au film, on the basis of other conditions are identical, carry out lower temperature (100-
150 DEG C) under make annealing treatment 1-1.5 h, on the basis of the Ag nano particle formed, regrowth layer of Au nano particle.
Nanostructured surface laminated film prepared by the present invention is a kind of Ag-Al2O3Tri- layers of (metal layer-Jie of-AgAu MIM
Matter layer-metal layer) structure laminated film, wherein thicker Ag film is as first layer reflectance coating, Al2O3Film is situated between as intermediate
Matter layer.
In the present invention, using twice annealing technique, make upper layer metallic film stress variation, turns the metallic film of top layer
Metallic particles is turned to, very strong light absorption effect is generated.
In the present invention, second of annealing is dispersed in Au particle between Ag particle using the annealing compared with low temperature
In gap, the generation of Ag-Au alloy is prevented, reduces grain spacing, improves uniformity;And the presence of Au particle also can effectively inhibit
The oxidation of Ag increases the service life of film.
The method of the present invention is easy to operate, at low cost without complicated photoetching process, industrially using roll-to-roll technology
It is mass produced.
MIM laminated film prepared by the present invention has outstanding absorbing properties, can be used as a kind of novel surface enhancing drawing
Graceful spectroscopic scatterometer (SERS) substrate material, can be used for the detection of a variety of biochemicals.The MIM laminated film preparation cost
It is low, it can be mass-produced, light absorption range is wide, can carry out quantitative detection, good reliability, and long service life has wide application
Prospect.
Detailed description of the invention
Fig. 1 is the preparation flow schematic diagram of MIM laminated film.
Fig. 2 is the scanning electron microscope image of MIN trilamellar membrane structure.
Fig. 3 is Raman spectrum of two kinds of MIM laminated films as SERS substrate to vinyl bipyridyl (BPE) Molecular Detection
Figure.
Fig. 4 is the raman spectrum that MIM laminated film detects cocaine molecule as SERS substrate.
Fig. 5 is service life curve of the MIM composite film material as SERS substrate.
Specific embodiment
Preparation method of the invention is described in detail below in conjunction with Application Example and attached drawing.
Embodiment: the preparation of tri- layers of laminated film of MIM and its detection as SERS substrate to sample
Using the method for magnetron sputtering, 150 nm Ag, 50 nm Al are successively grown on clean silicon wafer2O3, 12 nm Ag,
200 DEG C are carried out under ar gas environment later, the annealing of 1 h.Vacuum breaker aoxidizes under the condition of high temperature in order to prevent, is not beating
It begins to speak to wait substrate to be down to room temperature in the case where body, replaces target, one layer of 5 nm Au film of regrowth, in other conditions phase later
150 DEG C are carried out in the case where, the annealing of 1 h lower temperature.Later we use preparation this MIM laminated film as
SERS substrate detects some molecules.For the outstanding performance for illustrating this Ag-Au composite particles surface structure film, we
(identical bottom Ag and middle layer Al also under the same conditions2O3Thickness) only by once depositing and annealing, prepare single layer Ag
The thin-film material of particle surface is as a comparison.
Vinyl bipyridyl (BPE) molecule contains pi-electron system and pyridyl nitrogen atom, it is easy to and metal bonding, it is
For characterizing the common molecule of SERS performance.By the Ag particle surface MIM laminated film substrate only by once depositing and annealing
All it is immersed in 1 mM's with the Ag-Au particle surface MIM laminated film substrate proposed by the present invention by depositing and annealing twice
10 min, take out drying later in BPE ethanol solution, after alcohol rinse, are detected, are obtained with the Raman spectrum of 785 nm wavelength
Raman spectrum it is as shown in Fig. 3.As can be seen that in 1012,1200,1340,1608,1637 cm-1There is apparent Raman at place
Peak is the characteristic signal of BPE molecule.Comparison it can be found that the Raman signal of mixing Ag-Au particle far more than single layer Ag particle,
It illustrates preparation method proposed by the present invention, reduces intergranular gap, there is stronger enhancing ability.
The present invention also carries out SERS detection to cocaine molecule using this substrate.In many countries, the abuse of drugs is
Become a serious social concern.In administration of justice test and Criminal Detecting, cocaine is a kind of important detection medicine
Object.In an experiment, we are with the cocaine acetonitrile solution dropwise of 10 μ L to substrate surface, concentration from 1 mg/mL to 1 μ g/mL,
Raman detection is carried out after drying, the raman characteristic peak of spectrogram result cocaine as shown in Fig. 4 is respectively 1001,1027,1275
With 1598 cm-1It can be observed, even if concentration is down to 10 μ g mL-1.In view of the volume of drop is 10 μ L, the area of coverage
The area approximation in domain is 20 mm2, then the averag density of cocaine is only 5 ng mm-2, this gets well than the result reported before.
Illustrate that this MIM laminated film substrate has very high sensitivity to cocaine detection in the present invention.
In the present invention, due to using Au particle to be covered on Ag particle surface, the oxidation of Ag is inhibited to a certain extent.To survey
Its effective time is tried, substrate is placed in the laboratory environment of standard by we, and for temperature at 20-23 DEG C, humidity is maintained at 20%-
60%.The BPE solution of 1 mM is added dropwise on the substrate for saving 3 months and 12 months later, as shown in Fig. 5, in 1608 cm-1
The SERS signal intensity at place only reduces 10%.Illustrate that MIM laminated film substrate of the invention has very long service life.
Claims (4)
1. a kind of preparation method of super-absorbent Ag-Au nanostructured surface laminated film, which is characterized in that specific step is as follows:
(1) Ag, Al are successively grown on substrate2O3And Ag;
(2) it is made annealing treatment under ar gas environment;150-250 DEG C of temperature, time 1-1.5 h;
(3) substrate is waited to be down to room temperature, regrowth layer of Au film, on the basis of other conditions are identical, in lower temperature 100-
1-1.5 h, on the basis of the Ag nano particle formed, regrowth layer of Au nano particle are made annealing treatment at 150 DEG C.
2. the preparation method of super-absorbent Ag-Au nanostructured surface laminated film according to claim 1, feature exist
In the substrate material is silicon wafer, quartz plate or glass slide.
3. the super-absorbent Ag-Au nanostructured surface laminated film that preparation method described in a kind of claim 1 obtains is Ag-
Al2O3- AgAu MIM three-decker, wherein Ag film is as first layer reflectance coating, Al2O3Film is as middle dielectric layer.
4. super-absorbent Ag-Au nanostructured surface laminated film as claimed in claim 3, as answering for SERS substrate material
With.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109837207A (en) * | 2019-02-28 | 2019-06-04 | 中国科学院半导体研究所 | Gene sequencing chip and method |
CN110129756A (en) * | 2019-06-10 | 2019-08-16 | 重庆大学 | Metal film coupled nanosecond island surface enhanced Raman scattering substrate and preparation method thereof |
CN110527955A (en) * | 2019-09-30 | 2019-12-03 | 长春理工大学 | A kind of step low-refraction Al2O3The preparation method of film |
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CN104746049A (en) * | 2015-04-07 | 2015-07-01 | 南京大学 | Method for preparing surface-enhanced Raman scattering base with metal nanometer gaps by utilizing ALD (atomic layer deposition) |
CN104764732A (en) * | 2015-04-09 | 2015-07-08 | 复旦大学 | Surface-enhanced raman scattering base on basis of special-material superabsorbers and preparation method thereof |
CN108277484A (en) * | 2018-01-22 | 2018-07-13 | 安徽师范大学 | A kind of preparation method of hollow Ag-Au alloys composite construction micro-nano array |
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US6149868A (en) * | 1997-10-28 | 2000-11-21 | The Penn State Research Foundation | Surface enhanced raman scattering from metal nanoparticle-analyte-noble metal substrate sandwiches |
CN103409750A (en) * | 2013-08-15 | 2013-11-27 | 南京邮电大学 | Arrayed silver nanorods with surface-modifying gold nanoparticles and preparation method thereof |
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CN109837207A (en) * | 2019-02-28 | 2019-06-04 | 中国科学院半导体研究所 | Gene sequencing chip and method |
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CN110129756B (en) * | 2019-06-10 | 2020-07-10 | 重庆大学 | Metal film coupled nano island surface enhanced Raman scattering substrate and preparation method thereof |
CN110527955A (en) * | 2019-09-30 | 2019-12-03 | 长春理工大学 | A kind of step low-refraction Al2O3The preparation method of film |
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