CN107014799A - A kind of graphene/silver nano flower-like/PMMA " sandwich " structural flexibility SERS substrates and preparation method thereof - Google Patents
A kind of graphene/silver nano flower-like/PMMA " sandwich " structural flexibility SERS substrates and preparation method thereof Download PDFInfo
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Abstract
The invention discloses a kind of graphene/silver nano flower-like/PMMA " sandwich " structural flexibility SERS substrates and preparation method thereof, the rigid basement for which solving SERS in the prior art is difficult in adapt to realize between a variety of surface topographies, noble metal nano structure and substrate and combined closely, the problem of noble metal nano structure is easily aoxidized, allow prepared SERS substrates to conform to the surface of the various patterns in situ detection with flexible structure, carry out the effect of the in situ detection of Raman signal.Concrete scheme is：Flexible SERS substrates, including single-layer graphene, be grown on the silver nano flower-like layer on single-layer graphene surface and be covered in the PMMA films of silver nano flower-like layer surface so that silver nano flower-like layer is clipped between single-layer graphene and PMMA films.
Description
Technical field
The invention belongs to flexible SERS substrates preparation field, and in particular to a kind of graphene/silver nano flower-like/PMMA " Sanming City
Control " structural flexibility SERS substrates and preparation method thereof.
Background technology
SERS (SERS) realizes overdelicate single point due to can effectively amplify intrinsic Raman signal
Son detection, since the advent of the world just causes the extensive concern of people, and is gradually applied to chemical detection, food security and environment prison
The multiple fields such as survey.What SERS mechanism was widely accepted have two kinds of physics enhancing and Chemical enhancement, physics enhancing mainly by
Caused by the surface plasma resonance caused by electric-field enhancing, Chemical enhancement is mainly due to substrate and intermolecular charge-exchange
It is caused.Universal says, coarse precious metal surface and noble metal nano structure is mainly physics and strengthened, and noble metal plane,
Some semiconductors and New Two Dimensional stratified material are mainly Chemical enhancement.And the SERS bases that two kinds of enhancing principles are be combined with each other
Bottom is the big focus direction of one studied now.
In recent years, research shows that graphene has the SERS effects based on Chemical enhancement, and graphene has much in itself
Advantage：(1) the good biomolecule compatibility of graphene allows it as biological molecule concentration layer；(2) it is graphene-based in
The SERS effects of Chemical enhancement allow graphene as additional enhancement layer；(3) the good chemical inertness of graphene causes
Graphene can be used as the natural protective layer of noble metal nano structure；(4) property of graphene quenching fluorescence allows it to make
For fluorescent quenching layer.Graphene and metal Nano structure are be combined with each other and make compound SERS substrates, was studied in recent years
Hot fields, and achieve good achievement.Most SERS substrates are all rigid basements, this unyielding rigid material
Substrate is expected, it is difficult to adapt to a variety of surface topographies, it is more difficult to trace detection in situ is carried out to material.In rigid basement
Noble metal nano structure (gold, silver, copper etc.) is typically all after preparing, to be transferred in rigid basement.But pass through transfer
The process that method prepares the compound SERS substrates of graphene-metal Nano structure is extremely complex, and physics is combined and can not realized
Graphene-metal Nano structure is combined closely, and traditional noble metal nano structure is usually nano particle, nano particle
Signal enhancing less effective, the sensitvity constraint of detection.In addition, the oxygen of noble metal nano structure (gold, silver, copper etc.) used
Change problem is also one of the problem of being difficult to overcome.
To sum up shown, SERS of the prior art rigid basement is difficult in adapt to a variety of surface topographies, noble metal
It can not realize and combine closely, the problem of noble metal nano structure is easily aoxidized between nanostructured and substrate, still lack has at present
The solution of effect.
The content of the invention
Flexible SERS substrates have the advantages that it is many rare, such as：Flexible SERS substrates can conform to different shape
The outer surface of object carries out the in situ detection of Raman signal, and the good SERS flexible substrates of translucency can be placed on liquid surface
Carry out lossless Raman signal detection.These advantages cause flexible SERS substrates to have very strong practical application, have greatly
Potentiality can carry out trace detection in situ to real world object.
Although graphene is used for the preparation of flexibility SERS substrates by current also non-someone, the pliability of graphene causes
It can as flexibility SERS substrates material, so inventor begin attempt to by graphene be used for flexibility SERS substrates system
It is standby.
For technical problem present in above-mentioned prior art, it is an object of the invention to provide a kind of graphene/silver nanoparticle
Flower/PMMA " sandwich " structural flexibility SERS substrates.
It is a further object to provide above-mentioned graphene/silver nano flower-like/PMMA " sandwich " structural flexibilities SERS
The preparation method of substrate.
In order to solve the above technical problems, the technical scheme is that：
A kind of graphene/silver nano flower-like/PMMA " sandwich " structural flexibility SERS substrates, including single-layer graphene, growth
In single-layer graphene surface silver nano flower-like layer and be covered in the PMMA films of silver nano flower-like layer surface so that silver nano flower-like layer
It is clipped between single-layer graphene and PMMA films.
Compared to traditional graphene-noble metal nano structure SERS substrates and rigidity SERS substrates, stone of the invention
The advantage of black alkene/silver nano flower-like/PMMA flexibility SERS substrates is：One, in graphenic surface direct growth silver nano flower-like so that
Silver nano flower-like can firmly be attached to graphenic surface；Secondly, PMMA (polymethyl methacrylate) on the one hand have it is certain
Intensity, can as flexibility SERS substrates holder；On the other hand, with good translucency, SERS bases are not interfered with
The enhancing effect at bottom；The third aspect, silver nano flower-like is secured firmly between single-layer graphene and PMMA films, silver is both improved
The fastness of nano flower attachment, has completely cut off air, effectively prevent the oxidation of silver nano flower-like, and then improved SERS substrates again
Life-span.Thirdly, nano flower-like silver huge SERS effects can be provided, its signal enhancing effect is far better than silver nano-grain
Etc. structure；Four, single-layer graphene has preferable pliability, and PMMA has preferable pliability, and with certain intensity,
So the SERS substrates prepared are flexible substrates, flexible SERS substrates have wider applicability, it is possible to achieve trace in situ
Detection.
The preparation method of above-mentioned graphene/silver nano flower-like/PMMA " sandwich " structural flexibility SERS substrates, including following step
Suddenly：Single-layer graphene is grown on copper foil, the chemical reduction method aided in micro-current is in one layer of silver of single-layer graphene superficial growth
Nano flower, then covers one layer of PMMA film on silver nano flower-like layer, and final etching removes copper foil, produced.
Silver nano flower-like is grown directly upon single-layer graphene surface, and silver nano flower-like can be caused firmly to be attached to graphene table
Face；Silver nano flower-like prepared by the chemical reduction method of micro-current auxiliary has bigger specific surface area, strengthens with stronger Raman
Can occur chimeric between effect, and the silver nano flower-like and single-layer graphene of generation, further increase silver nano flower-like and individual layer
Bond strength between graphene.
Further, the growing method of single-layer graphene is CVD (chemical vapor deposition) growing method.
Further, the size of current of the chemical reduction method of the micro-current auxiliary is 50~200 μ A/cm-1, during growth
Between be 10~70s.Copper foil with graphene is inserted AgNO3Displacement can occur in solution, between copper atom and silver ion anti-
Should, silver nanoparticle island is formed, this is the brilliant nucleation first and growth course of silver nanoparticle, in order to form the silver nanoparticle with cutting-edge structure
Flower, silver nanoparticle brilliant second of nucleation and growth course are carried out with micro-current electric plating method, now, the Yin Na of silver atoms formation
Rice cluster is oriented on silver nanoparticle island surface grows nonparasitically upon another plant, and forms the cutting-edge structure with excellent SERS effects.
Further, size of current is 140~180 μ A/cm-1, growth time is 40~60s.
When electric current and growth time is the scopes, the silver nano flower-like prepared has stronger Raman signal enhancing effect
Really.
Further, the electrolyte of the chemical reduction method of the micro-current auxiliary is AgNO3Solution, the concentration of electrolyte
For 1.5~2g/L.
Further, the chemical reduction method of micro-current auxiliary grows the method for silver nano flower-like, specifically include as
Lower step：Using graphene/copper foil compound as negative pole, using silver foil as positive pole, size of current is 50~200 μ A/cm-1, it is auxiliary
Help the AgNO that electrolyte concentrations are 1.5~2g/L3The citric acid mixed liquor of solution and 10~15g/L, reacts 10~70s, obtains silver
Nano flower layer.
Further, the corrosive liquid used in erosion removal copper foil is FeCl3Solution, the concentration of corrosive liquid is 0.5~1M, rotten
It is 10~20 DEG C to lose reaction temperature.
A kind of biology sensor, including above-mentioned graphene/silver nano flower-like/PMMA " sandwich " structural flexibility SERS substrates.
Above-mentioned graphene/silver nano flower-like/PMMA " sandwich " structural flexibility SERS substrates are in material trace detection in situ
Application.
The present invention advantageous effects be：
(1) in graphenic surface direct growth silver nano flower-like so that silver nano flower-like can firmly be attached to graphene table
Face；
(2) PMMA as flexible SERS substrates holder, with good translucency；
(3) silver of nano flower-like can provide huge SERS effects, and its signal enhancing effect is far better than silver nanoparticle
The structures such as grain；
(4) silver nano flower-like is firmly fixed between graphene and PMMA films with " sandwich " structure, can be effectively
Prevent the oxidation of silver so that floor life is greatly enhanced.
(5) flexible structure allows prepared SERS substrates to conform to the tables of the various patterns in situ detection
Face, carries out the in situ detection of Raman signal.
Brief description of the drawings
The Figure of description for constituting the part of the application is used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its illustrate be used for explain the application, do not constitute the improper restriction to the application.
Fig. 1 is the scanning electron microscope image that embodiment 1 prepares forerunner's substrate copper foil/graphene/silver nano flower-like；
Fig. 2 is the scanning electron microscope image that embodiment 1 prepares graphene/silver nano flower-like/PMMA.
In Fig. 3, (a) is the detects schematic diagram that embodiment 1 prepares graphene/silver nano flower-like/PMMA flexibility SERS substrates；
(b) for embodiment 1 prepare graphene/silver nano flower-like/PMMA flexibility SERS substrates to 10-12M concentration rhodamine 6G (R6G)
Raman enhancing effect figure.
Embodiment
It is noted that described further below is all exemplary, it is intended to provide further instruction to the application.Unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in this manual using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
Term explains part：
Flexible substrates, refer to the substrate of bending rigidity very little, can deform and arbitrarily bend with the body surface of laminating；Rigidity
The bending rigidity of substrate is big, it is impossible to deform any bending with the body surface of laminating.
Copper foil, is to be made and formed by copper plus other a certain proportion of metals, typically there is two kinds of 90 paper tinsels and 88 paper tinsels, i.e. copper content
For 90% and 88%.Copper foil herein can be any one in both copper foils, the copper used in embodiment
Paper tinsel is the copper foil that copper content is 90%, purchased from United Copper Foils Huizhou Co., Ltd..
Embodiment 1
1. single-layer graphene is grown with CVD technology, carbon source is methane, and growing substrate is as catalyst with high-purity copper foil
Copper foil, growth conditions：Air pressure is 105Pa, growth temperature is 1100 DEG C, and growth time is 1h.
2. the chemical reduction method aided in micro-current grows one layer of silver nano flower-like in graphenic surface, it is specially：With stone
Black alkene/copper foil is as negative pole, using silver foil as positive pole, and size of current is 150 μ A/cm-1, electrolyte is that concentration is 2g/L's
AgNO3The citric acid mixed liquor of solution and 10g/L, the reaction time is 50s.
3. the FeCl for being 1M with concentration3Solution is corrosive liquid, and copper foil substrate is removed in 20 DEG C of environment.
The scanning electron microscope image of forerunner's substrate copper foil/graphene/silver nano flower-like of preparation as shown in figure 1, from this
Figure can be seen that：A diameter of 80~120nm of silver nano flower-like, nano flower spacing be 50~150nm, branch length be 40~
60nm.Graphene/silver nano flower-like/PMMA of preparation scanning electron microscope image is as shown in Fig. 2 as can be seen from this figure：
Chip shape is presented in the bottom of silver nano flower-like, and diameter is in 80~120nm, and thin slice spacing is 50~150nm.Prepare graphene/silver
The detects schematic diagram of nano flower/PMMA flexibility SERS substrates, using the flexible SERS substrates to 10-12M concentration rhodamine 6Gs
(R6G) carry out in Raman enhancing, such as Fig. 3 shown in (a), wherein 1 is silica substrate, 2 be R6G molecular layers, and 3 be silver nanoparticle
Flower, 4 be PMMA films, and 5 be graphene, and R6G molecular layers 2 are located between silica substrate 1 and flexibility SERS substrates, from flexibility
The top projection laser of SERS substrates, and obtained enhanced Raman scattering signal is detected.Graphene/silver nanoparticle
Flower/PMMA flexibility SERS substrates are to 10-12The Raman enhancing effect figure of M concentration rhodamine 6G (R6G), can from figure such as shown in (b)
To find out：For R6G concentration as little as 10-12M, the Detection results of the flexible SERS substrates are still fine, and raman characteristic peak clearly may be used
See, 1578cm-1For the Raman peaks of graphene, R6G most strong Raman peaks are located at 614cm-1, intensity is 2300counts.
Embodiment 2
1. single-layer graphene is grown with CVD technology, carbon source is methane, and growing substrate is as catalyst with high-purity copper foil
Copper foil, growth conditions：Air pressure is 105Pa, growth temperature is 1100 DEG C, and growth time is 1h.
2. the chemical reduction method aided in micro-current grows one layer of silver nano flower-like in graphenic surface, it is specially：With stone
Black alkene/copper foil is as negative pole, using silver foil as positive pole, and size of current is 200 μ A/cm-1, electrolyte is that concentration is 1.5g/L's
AgNO3The citric acid mixed liquor of solution and 15g/L, the reaction time is 55s.
3. the FeCl for being 0.5M with concentration3Solution is corrosive liquid, and copper foil substrate is removed in 10 DEG C of environment.
Embodiment 3
1. single-layer graphene is grown with CVD technology, carbon source is methane, and growing substrate is as catalyst with high-purity copper foil
Copper foil, growth conditions：Air pressure is 105Pa, growth temperature is 1100 DEG C, and growth time is 1h.
2. the chemical reduction method aided in micro-current grows one layer of silver nano flower-like in graphenic surface, it is specially：With stone
Black alkene/copper foil is as negative pole, using silver foil as positive pole, and size of current is 50 μ A/cm-1, electrolyte is that concentration is 1.5g/L's
AgNO3The citric acid mixed liquor of solution and 10g/L, the reaction time is 60s.
3. the FeCl for being 0.8M with concentration3Solution is corrosive liquid, and copper foil substrate is removed in 20 DEG C of environment.
The preferred embodiment of the application is the foregoing is only, the application is not limited to, for the skill of this area
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. a kind of graphene/silver nano flower-like/PMMA " sandwich " structural flexibility SERS substrates, it is characterised in that：Including individual layer stone
Black alkene, the silver nano flower-like layer for being grown on single-layer graphene surface and the PMMA films for being covered in silver nano flower-like layer surface so that
Silver nano flower-like layer is clipped between single-layer graphene and PMMA films.
2. the preparation method of graphene/silver nano flower-like/PMMA " sandwich " structural flexibility SERS substrates described in claim 1,
It is characterized in that：Comprise the following steps：Single-layer graphene is grown on copper foil, the chemical reduction method aided in micro-current is in individual layer
Graphenic surface grows one layer of silver nano flower-like, then covers one layer of PMMA film on silver nano flower-like layer, copper removal is removed in final etching
Paper tinsel, is produced.
3. preparation method according to claim 2, it is characterised in that：The growing method of single-layer graphene is CVD growth side
Method.
4. preparation method according to claim 3, it is characterised in that：The electricity of the chemical reduction method of the micro-current auxiliary
Stream size is 50~200 μ A/cm-1, growth time is 10~70s.
5. preparation method according to claim 4, it is characterised in that：Size of current is 140~180 μ A/cm-1, during growth
Between be 40~60s.
6. preparation method according to claim 3, it is characterised in that：The electricity of the chemical reduction method of the micro-current auxiliary
Solution liquid is AgNO3Solution, the concentration of electrolyte is 1.5~2g/L.
7. preparation method according to claim 2, it is characterised in that：The chemical reduction method growth of the micro-current auxiliary
The method of silver nano flower-like, specifically includes following steps：Using graphene/copper foil compound as negative pole, using silver foil as positive pole, electricity
Stream size is 50~200 μ A/cm-1, assisted electrolysis concentration is 1.5~2g/L AgNO3Solution and 10~15g/L citric acid are mixed
Liquid is closed, 10~70s is reacted, silver nano flower-like layer is obtained.
8. preparation method according to claim 2, it is characterised in that：Corrosive liquid used in erosion removal copper foil is FeCl3It is molten
Liquid, the concentration of corrosive liquid is 0.5~1M, and corrosion reaction temperature is 10~20 DEG C.
9. a kind of biology sensor, it is characterised in that：Including above-mentioned graphene/silver nano flower-like/PMMA " sandwich " structural flexibility
SERS substrates.
10. graphene/silver nano flower-like/PMMA " sandwich " structural flexibility SERS substrates described in claim 1 are in situ in material
Application in trace detection.
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| CN112378893A (en) * | 2020-11-11 | 2021-02-19 | 长春理工大学 | Preparation method of composite SERS substrate for pesticide detection |
| CN115819817A (en) * | 2022-12-22 | 2023-03-21 | 西安交通大学 | Flexible SERS film and preparation method and application thereof |
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