CN107235471B - A kind of surface enhanced Raman scattering substrate and its preparation method and application - Google Patents
A kind of surface enhanced Raman scattering substrate and its preparation method and application Download PDFInfo
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- CN107235471B CN107235471B CN201710261949.0A CN201710261949A CN107235471B CN 107235471 B CN107235471 B CN 107235471B CN 201710261949 A CN201710261949 A CN 201710261949A CN 107235471 B CN107235471 B CN 107235471B
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Abstract
The invention belongs to LR laser raman detection technique field, a kind of surface enhanced Raman scattering substrate and its preparation method and application is disclosed.The surface of the substrate is covered with orderly etching silver nanowire film, the orderly etching silver nanowires film is formed by the etching silver nanowires ordered arrangement being parallel to each other, the average headway 0-15nm between silver nanowires is etched, the roughness on single etching silver nanowires surface is in 0-20nm.Preparation method is to be performed etching using chemical method on silver nanowires surface, then this etching silver nanowires is carried out self assembly by three phase boundary method, is then transferred into substrate surface.This method not only have many advantages, such as method it is simple, it is low in cost, be easily achieved.The substrate is used for SERS detection, minimum detection limit is up to 10 when detection sensitivity with higher with rhodamine B is probe molecule‑11M has extensive potential application foreground in fields such as food, environment, medical treatment, biologies.
Description
Technical field
The invention belongs to nano science, analysis science, life science, environmental science, Food Science and LR laser raman inspection
A kind of survey technology field, and in particular to surface enhanced Raman scattering substrate and its preparation method and application.
Background technique
Surface enhanced Raman scattering (Surface-enhanced Raman scattering, SERS), due to high
Sensitivity, it can be achieved that Single Molecule Detection to sample molecule, has become highly important fast trace detection means.SERS
The activity of substrate is largely related to the size of metal nanoparticle, shape, surface roughness and spacing.Therefore,
Preparing high-performance SERS substrate is quite high for the control synthesis of the shape of metal nanoparticle and distance regulation requirement.
With the development of nano science, nano material of different shapes is synthesized, through frequently as composition SERS substrate
Nano material includes gold and silver nanosphere, nano cubic, nano wire etc., and wherein silver nanowires is the relatively broad nanometer used
Material or one of, however silver nanowires as composition SERS substrate material when, hot spot is distributed mainly on the tip of silver nanowires
Place, and surface signal is uneven, while the silver nanowire film of disorderly and unsystematic arrangement causes the weight of SERS substrate each point signal linear
It is poor.Limit its extensive use.
Summary of the invention
In order to overcome the disadvantages and deficiencies of the prior art, the primary purpose of the present invention is that providing a kind of surface-enhanced Raman
Scatter substrate.
Another object of the present invention is to provide a kind of preparation methods of above-mentioned surface enhanced Raman scattering substrate.This method
The surface of silver nanowires is performed etching using chemical etchant, assembles novel etching silver nanoparticle with three phase boundary self-assembly method
Line is transferred to substrate surface later, is formed and orderly etches silver nanowire film as surface enhanced Raman scattering substrate, the method system
In standby orderly etching silver wire film substrate, hot spot is not only present at silver nanowires tip, and is formed after existing in etching
Rough surface and orientation after at the nanoscale gap that is formed, stronger Raman enhancing signal can be generated；And ordered structure
After formation, the reproducibility of substrate surface SERS signal is also greatly improved.
A further object of the present invention is to provide the applications of above-mentioned surface enhanced Raman scattering substrate.
The purpose of the invention is achieved by the following technical solution:
A kind of surface enhanced Raman scattering substrate, the surface of the substrate are covered with orderly etching silver nanowire film, this is orderly
Etching silver nanowire film is formed by the etching silver nanowires ordered arrangement being parallel to each other, and is etched between average between silver nanowires
Away from 0-15nm, the roughness on single etching silver nanowires surface is in 0-20nm.
We provide the roughness (R) on single etching silver nanowires surface:
Wherein Xn represents the height at silver nanowires any point along long axis direction cross section,It represents silver-colored on the cross section
The average height of nano wire.
Etch the average headway (D) between silver nanowires:
DmaxiFor the maximum spacing of adjacent two silver nanowiress.
The preparation method of above-mentioned surface enhanced Raman scattering substrate, comprising the following steps:
(1) etching silver nanowires colloidal sol is formed to silver nanowires surface etching treatment by etching agent；
(2) orderly etching silver nanowires film is formed at three phase boundary by interface self-assembly method；
(3) the orderly etching silver nanowires film of self assembly on interface is transferred to substrate surface, forms surface enhanced and draws
Graceful scattering substrate.
Step (1) etching agent is the concentrated ammonia liquor and dioxygen aqueous mixtures of volume ratio (10:1)-(1:1).
Step (1) is specific according to the following steps: it is water-soluble that the etching agent of fresh configuration is added to the PVP that concentration is 5mg/mL
In liquid, silver nanowires is added under 3000rmp-6000rmp stirring condition, solution changes color releases gas, continues to stir, and is formed and is carved
Lose silver nanowires colloidal sol.
Step (2) is specific according to the following steps: in a wide mouth glassware, silver nanowires will be etched obtained by step (1)
Colloidal sol is added to the surface of oil-phase solution, forms contact surface between immiscible two liquid and air three-phase, is then carving
Orientation silver nanowires that the third solvent is formed at oil-water interfaces is added gradually from oil-water interfaces in erosion silver nanowires sol surface
It is finally formed on water air interface to water air interface migration and is orientated silver nanowires film.
The volume ratio of the third solvent and etching silver nanowires colloidal sol is 1:1~1:20.
The oil-phase solution is chloroform, methylene chloride or chlorobenzene；The third described solvent is ethyl alcohol, acetone or tetrahydro furan
It mutters.
Application of the above-mentioned surface enhanced Raman scattering substrate in rhodamine B detects.
The present invention has the following advantages and effects with respect to the prior art:
The present invention provides the preparation method of SERS active-substrate, is performed etching using chemical method on silver nanowires surface,
This etching silver nanowires is subjected to self assembly by three phase boundary method again, substrate surface is then transferred into, is orderly etched
Silver nanowires film substrate, this substrate preparation method not only facilitate simply, but also low in cost, can be real without special installation
It is existing；And the roughness on silver nanowires surface can be greatly increased by this kind of method, increase surface hot spot, to improve SERS letter
Number intensity, so that the substrate carries out having good detection sensitivity and higher reproducibility when Raman detection；This method is available
In the detection of super low concentration molecule, it is expected in life science, the fields great Zhan such as environmental science and Food Science application；By the substrate
It is detected for SERS, detection sensitivity with higher, minimum detection limit is up to 10 when with rhodamine B being probe molecule-11M,
There is extensive potential application foreground in the fields such as food, environment, medical treatment, biology.
Detailed description of the invention
Fig. 1 is the preparation flow schematic diagram of surface-enhanced Raman scattering activity substrate used in case study on implementation of the present invention.
Fig. 2 is the SEM figure for the surface-enhanced Raman scattering activity substrate that the embodiment of the present invention 1,2,3 provides, and wherein a is real
The disorderly and unsystematic silver nanowires for applying the offer of example 1 is schemed as the SEM of surface-enhanced Raman scattering activity substrate, and b is that embodiment 2 provides
Orientation do not etch silver nanowires as surface-enhanced Raman scattering activity substrate SEM scheme, c embodiment 3 provide orientation carve
The SEM for losing silver nanowires as surface-enhanced Raman scattering activity substrate schemes.
Fig. 3 is the atomic force microscopy diagram spectrum for not etching silver nanowires in the embodiment of the present invention 1,3 and etching silver nanowires
(AFM), wherein a is that the AFM figure for not etching silver nanowires and b that the embodiment of the present invention 1 provides etch silver nanowires to apply in example 3
AFM figure, c is the height ratio along long axis direction by silver nanowires along the cross section of diameter of silver nanowires in above-mentioned two figure
Compared with.
Fig. 4 is that the progress concentration of surface-enhanced Raman scattering activity substrate provided by case study on implementation 1,2,3 of the present invention is 10- 7SERS spectra figure when M rhodamine B detects, wherein a has surface-enhanced Raman scattering activity substrate for what embodiment 1 provided
SERS spectra figure, b is the SERS spectra figure with surface-enhanced Raman scattering activity substrate that provides of embodiment 2, c embodiment
The 3 SERS spectra figures with surface-enhanced Raman scattering activity substrate provided.Raman determination condition: Surface enhanced Raman spectroscopy
It is measured using laser Raman spectrometer (HORIBA Jobin Yvon), is furnished with 1.mWAr+ laser, excitation wavelength uses
633nm, CCD detector, peak position is calibrated with silicon wafer before Raman spectroscopy, and the measurement cumulative time is 20s, by sieve of 0.02mL
Red bright B ethanol solution is added dropwise in 7 × 7mm2Substrate on, testing conditions carry out under identical conditions.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
For ease of description, in the examples below, we are said with diameter 100nm and 20 μm of length of silver nanowires
Bright, certainly, in other embodiments, initial silver nanowires is also possible to other sizes, and the scale of reaction uses 500 μ L, 5mg/
The amount of mL silver nanowires, the amount of certain single reaction and the concentration of silver nanowires are also adjustable, and base material removes monocrystalline
Also glass, metal etc. can be used outside silicon.
The process that following embodiment prepares surface-enhanced Raman scattering activity substrate is as shown in Figure 1.
Embodiment 1
By the 500 μ direct drop coatings of L silver nanowires suspension in substrate material surface, the scanning electricity of obtained silver nanowires
Mirror is as shown in Figure 2 a, and the single atomic force microscope for not etching silver nanowires is shown in Fig. 3 a, to rhodamine B (10-7Mol/L) Raman light
Spectrogram is shown in Fig. 4 a.
Embodiment 2
In a wide mouth glassware, the 5mL silver nanowires hydrosol is added to 15mL chloroform surface, immiscible two
Contact surface is formed between liquid and air three-phase, then, is carefully added into 1mL acetone on etching silver nanowires hydrosol surface,
The orderly silver nanowires formed at oil-water interfaces is gradually migrated from oil-water interfaces to water air interface, is finally formed on water air interface
Silver nanowires monofilm is not etched orderly.
It is transferred to substrate surface by orderly silver nanowire film is not etched, to obtain Ordered Silver nanowire surface enhancing Raman
Scatter active substrate.
The scanning electron microscope for etching silver nanowires by orientation prepared by this method is as shown in Figure 2 b, to rhodamine B (10- 7Mol/L) Raman spectrogram is shown in Fig. 4 b.
Embodiment 3
A) processing is performed etching to silver wire surface: chooses concentrated ammonia liquor and 30% hydrogen peroxide (volume ratio 9:1) as etching
Agent, etching agent fresh configuration before the use, and be stored in ice-water bath, it is water-soluble that the etching agent of 400 μ L is added to 4.5ml PVP
In liquid (5mg/mL), 500 μ L silver nanowiress are added under 3000rmp intense agitation.Solution, which changes colour rapidly, releases gas, after
Continuous stirring 5min.
B) above-mentioned etching silver nanowires is carried out by interface self assembly by three phase boundary method: in a wide mouth glassware,
5mL etching silver nanowires solution is added to 25mL chloroform surface, is formed and is connect between immiscible two liquid and air three-phase
Then contacting surface is carefully added into 1mL ethyl alcohol on etching silver nanowires hydrosol surface, the Ordered Silver formed at oil-water interfaces is received
Rice noodles are gradually migrated from oil-water interfaces to water air interface, and orderly etching silver nanowires monofilm is finally formed on water air interface.
C) by the silver wire film transfer of orientation to substrate surface, to obtain surface-enhanced Raman scattering activity substrate.
The single silver wire diameter in SERS active-substrate prepared by this method is about 80nm, and length is 20 μm, etching silver
Average distance 5mn between nano wire is 10 as the detectable concentration limit of the SERS substrate to rhodamine B-11M.It is obtained to take
To etching silver nanowires scanning electron microscope (SEM) photograph as shown in 2c.The atomic force microscopy diagram 3b of single etching silver nanowires, to Luo Dan
Bright B (10-7Mol/L) Raman spectrogram is shown in Fig. 4 c.By by Fig. 3 it can be concluded that silver nanowires etching front and back silver nanowires surface
Degree of roughness has notable difference, show that the surface roughness of etching silver wire is 0.5nm by Fig. 3 c, and it is coarse to etch rear surface
Degree obviously increases, and the roughness of single silver nanowires is up to 10.8nm.In addition to this we have also carried out rambling silver and have received
Rice noodles are orientated silver nanowires, and are orientated the detection that same concentrations rhodamine B is carried out when etching silver nanowires as SERS substrate,
Compare from Fig. 4 a, 4b, 4c and show that Fig. 4 c SERS intensity is significantly stronger than Fig. 4 a and Fig. 4 b, and repeatedly measure the result shows that,
Differing greatly between the signal point of Fig. 4 a, and SERS signal difference when substrate in this example carries out SERS detection is compared with example 1
Small is more.The result shows that the orientation etching silver nanowires in the present invention is as the more rambling silver nanowires substrate of SERS substrate
It is had great advantages with orientation silver nanowires substrate.
Embodiment 4
A) processing is performed etching to silver wire surface: chooses concentrated ammonia liquor and 30% hydrogen peroxide (volume ratio 1:1) as etching
Agent, etching agent fresh configuration before the use, and be stored in ice-water bath, it is water-soluble that the etching agent of 250 μ L is added to 4.5mL PVP
In liquid (5mg/mL), 500 μ L silver nanowiress are added under 5000rmp intense agitation.Solution, which changes colour rapidly, releases gas, after
Continuous stirring 10min.
B) above-mentioned etching silver wire is carried out by interface self assembly by interface method: in a wide mouth glassware, 5mL is added and carves
Erosion silver nanowires solution is added to 35mL methylene chloride liquid surface, is formed between immiscible two liquid and air three-phase
Then contact surface is carefully added into 3mL tetrahydrofuran on etching silver nanowires hydrosol surface, what is formed at oil-water interfaces has
Sequence silver nanowires is gradually migrated from oil-water interfaces to water air interface.Orderly etching silver nanowires list is finally formed on water air interface
Tunic.
C) by the silver wire film transfer of orientation to substrate surface, to obtain surface-enhanced Raman scattering activity substrate.
The single silver wire diameter in SERS active-substrate prepared by this method is about 90nm, and length is 20 μm, etching silver
Average distance 6nm between nano wire, the roughness of single silver nanowires examine rhodamine B as SERS substrate up to 5.4nm
The limit for surveying concentration is 10-10M。
Embodiment 5
A) processing is performed etching to silver wire surface: chooses concentrated ammonia liquor and 30% hydrogen peroxide (volume ratio 5:1) as etching
Agent, etching agent fresh configuration before the use, and be stored in ice-water bath, it is water-soluble that the etching agent of 100 μ L is added to 4.5mLPVP
In liquid (5mg/mL), 500 μ L silver nanowiress are added under 6000rmp intense agitation.Solution, which changes colour rapidly, releases gas, after
Continuous stirring 15min.
B) above-mentioned etching silver wire is carried out by interface self assembly by interface method: in a wide mouth glassware, 5mL is added and carves
Erosion silver nanowires solution is added to 25mL chlorobenzene liquid surface, and contact is formed between immiscible two liquid and air three-phase
Then face on etching silver nanowires hydrosol surface, is carefully added into 0.05mL ethyl alcohol, the Ordered Silver formed at oil-water interfaces
Nano wire is gradually migrated from oil-water interfaces to water air interface.Orderly etching silver nanowires single layer is finally formed on water air interface
Film.
C) by the silver wire film transfer of orientation to substrate surface, to obtain surface-enhanced Raman scattering activity substrate.
The single silver wire diameter in SERS active-substrate prepared by this method is about 97nm, and length is 20 μm, etching silver
The distance between nano wire 10nm, the roughness of single silver nanowires detect rhodamine B as SERS substrate up to 3.1nm
The limit of concentration is 10-9M。
In conclusion the preparation method of surface enhanced Raman scattering substrate provided by the invention, utilizes chemical etching legal system
The silver nanowires of standby surface roughening will etch silver nanowires using three phase boundary self-assembly method and be assembled into ordered structure, and will
The orderly etching silver wire film is transferred in substrate.This method is not only simple, at low cost, easily operated to be not required to special installation,
And this method preparation has preferable Raman signal intensity, detection sensitivity and reproducibility with higher, Ke Yiying
SERS for super low concentration molecule is detected, and has wide use scope.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (5)
1. a kind of preparation method of surface enhanced Raman scattering substrate, it is characterised in that the following steps are included:
(1) etching silver nanowires colloidal sol is formed to silver nanowires surface etching treatment by etching agent；
(2) orderly etching silver nanowires film is formed at three phase boundary by interface self-assembly method, specifically according to the following steps:
In a wide mouth glassware, etching silver nanowires colloidal sol obtained by step (1) is added to the surface of oil-phase solution, in mutually not phase
Contact surface is formed between molten two liquid and air three-phase, the third solvent then is added in etching silver nanowires sol surface and exists
The orientation silver nanowires formed at oil-water interfaces is gradually finally formed on water air interface from oil-water interfaces to water air interface migration
It is orientated silver nanowires film；
(3) the orderly etching silver nanowire film of self assembly on interface is transferred to substrate surface, forms Surface enhanced Raman scattering
Substrate；The surface of the substrate is covered with orderly etching silver nanowires film, and it is by being parallel to each other that this, which orderly etches silver nanowire film,
Etching silver nanowires ordered arrangement form, etch silver nanowires between average headway 0-15nm, single etching silver nanowires
The roughness on surface is in 0-20nm.
2. preparation method according to claim 1, it is characterised in that: step (1) etching agent is volume ratio (10:1)-
The concentrated ammonia liquor and dioxygen aqueous mixtures of (1:1).
3. preparation method according to claim 1, it is characterised in that: step (1) is specific according to the following steps: matching fresh
The etching agent set is added in the PVP aqueous solution that concentration is 5mg/mL, is added under 3000 revs/min of -6000 revs/min of stirring conditions
Silver nanowires, solution changes color release gas, continue to stir, and form etching silver nanowires colloidal sol.
4. preparation method according to claim 1, it is characterised in that: the body of the third solvent and etching silver nanowires colloidal sol
Product is than being 1:1~1:20.
5. preparation method according to claim 1, it is characterised in that: the oil-phase solution is chloroform, methylene chloride or chlorine
Benzene；The third described solvent is ethyl alcohol, acetone or tetrahydrofuran.
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| CN108226130A (en) * | 2017-12-28 | 2018-06-29 | 浙江大学 | For the soft light Meta Materials laminated film and method of nitrite detection |
| CN108318473A (en) * | 2018-01-12 | 2018-07-24 | 暨南大学 | A kind of surface-enhanced Raman scattering activity substrate and its preparation method and application |
| CN109686496B (en) * | 2018-10-30 | 2021-02-09 | 苏州诺菲纳米科技有限公司 | Etching method of silver nanowire, transparent conductive electrode and preparation method of transparent conductive electrode |
| CN109520992B (en) * | 2018-11-08 | 2021-02-05 | 南京光声超构材料研究院有限公司 | SERS substrate of silver bromide nanowire and preparation method thereof |
| CN110379561A (en) * | 2019-06-27 | 2019-10-25 | 顾氏纳米科技（浙江）有限公司 | A kind of preparation method of silver nanowires self assembly conductive film |
| CN110927140A (en) * | 2019-11-27 | 2020-03-27 | 浙江工业大学 | Method for rapidly preparing nano Ag film surface enhanced Raman substrate through liquid-liquid interface |
| CN116539584B (en) * | 2023-03-28 | 2024-02-09 | 浙江大学 | Ultra-high sensitivity SERS hydrogen sulfide detection method |
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