CN106501232A - A kind of compound particle SERS active-substrate of sandwich structure and preparation method thereof - Google Patents
A kind of compound particle SERS active-substrate of sandwich structure and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to LR laser raman detection technique field, and in particular to a kind of SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure and preparation method thereof.A kind of SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure, including carrier, is followed successively by flower-shaped silver granuel sublayer, graphene oxide particle layer and gold nano star particle layer from bottom to top on the carrier.Sandwich structure substrate constructed by the present invention, the plasma resonance coupling effect of each layer in gold nano star particle and flower-shaped silver particles is not only existed, but also there is the plasma resonance coupling effect of each interlayer gold nano star and flower-shaped silver particles so that the sandwich structure substrate of the present invention has the surface enhanced Raman scattering effect more excellent than single layer substrates.
Description
Technical field
The invention belongs to LR laser raman detection technique field, and in particular to a kind of flower-shaped silver/graphene oxide/gold nano star
SERS active-substrate of sandwich structure and preparation method thereof.
Background technology
SERS（SERS）Technology is that a kind of sensitivity is high, molecular detection technology quick and precisely, lossless,
There is very wide application prospect at aspects such as analytical chemistry, biological medicine, environment measurings.Generally believe SERS mechanisms of production
Be mainly derived from Electromagnetic enhancement (EM) that nano-particle local surface plasma resonance effect causes and detection molecules with
Chemical enhancement (CM) effect caused by electric charge transfer between SERS substrates.Electromagnetic enhancement can be produced with the summation of Chemical enhancement
About 109-1011Raman strengthen signal.SERS excellent performance is built using noble metals such as gold, silver
SERS substrates are simultaneously carried out theoretical research and practical application and have become a big focus of research.
Three dimensional composite structure substrate is a kind of surface-enhanced Raman scattering activity substrate with excellent SERS performances.Pass through
The sandwich composite construction SERS substrates that the layer assembly of gold, silver particle is built, do not only exist the plasma between particle in layer
Resonance body coupling effect, but also there is the interparticle plasma resonance coupling effect of interlayer so as to than individual layer particle
More excellent surface enhanced Raman scattering effect.At present, using different gold, silver particles build sandwich structure SERS substrates into
New direction for SERS research field.
Graphene oxide has two-dimensional slice structure of the surface rich in oxygen-containing functional group, grinding in SERS
Study carefully and there is in application unique advantage：（1）Graphene oxide has Chemical enhancement effect；（2）Containing rich on graphene oxide
Rich big π keys, by π-π interaction adsorption and enrichment aromatic series detection molecules, can improve sensitivity and the weight of SERS detections
Renaturation；（3）Graphene oxide is attached to silver particles surface, silver particles can be made to be hedged off from the outer world, prevented silver particles from aoxidizing, carry
The stability of high silver particles.Graphene oxide is combined with gold, silver particle composite is prepared as SERS
Substrate incomparable advantage with uniqueness.
At present, graphene oxide is combined with gold, silver particle, plays respective advantage and build sandwich structure surface enhanced
Raman scattering substrate is also rarely reported.Using flower-shaped silver particles as bottom, graphene oxide has the present invention as intermediate course
Numerous tip gold branches gold nano star as upper strata, in conjunction with excellent plasma resonance between gold nano star and flower-shaped silver particles
The Chemical enhancement of coupling effect and graphene oxide, molecule enrichment, passivation protection effect, have been prepared a kind of with excellent first
The sandwich composite substrate of different surface enhanced Raman scattering effect.The preparation method of the present invention is simple, mild condition, increases on surface
The theoretical research of strong Raman scattering is significant with application aspect.
Content of the invention
The present invention is intended to provide a kind of new SERS active-substrate, specifically a kind of flower-shaped silver/graphene oxide/gold nano
SERS active-substrate of star sandwich structure and preparation method thereof.
The present invention is achieved by the following technical solutions：A kind of flower-shaped silver/graphene oxide/gold nano star sandwich knot
The SERS active-substrate of structure, including carrier, is followed successively by flower-shaped silver granuel sublayer, graphene oxide particle from bottom to top on the carrier
Layer and gold nano star particle layer.
Compared with prior art, the present invention has the advantage that and beneficial effect：
The present invention using gold nano star as sandwich structure outermost layer.Gold nano star particle has numerous tapering golden branches, etc.
Gas ions performance is adjustable, with the gold particle than other patterns（Gold nanosphere, gold nanorods etc.）More excellent plasma is altogether
Coupling effect of shaking and more rich " focus " so as to which sandwich structure compound particle has more excellent SERS effects.This
Bright constructed sandwich structure substrate, does not only exist the plasma resonance of gold nano star particle and flower-shaped silver particles in each layer
Coupling effect, but also there is the plasma resonance coupling effect of each interlayer gold nano star and flower-shaped silver particles so that this
Bright sandwich structure substrate has the surface enhanced Raman scattering effect more excellent than single layer substrates.The present invention will be with chemistry
Strengthen, the graphene oxide that molecule enrichment and passivation protection are acted on is added in sandwich composite construction, can further improve
The sensitivity of SERS detections, stability and repeatability, have highly important using value in SERS fields.
Further, described carrier is silicon chip.When being embodied as certainly, described carrier can adopt the load of other forms
Body.
For the further description present invention, the invention provides a kind of flower-shaped silver/graphene oxide/gold nano star three
The preparation method of the SERS active-substrate of Mingzhi's structure, comprises the steps：
（1）The preparation of flower-shaped silver particles：With ascorbic acid as reducing agent, with polyvinylpyrrolidone as protective agent, by liquid phase
Reducing process prepares flower-shaped silver particles；
（2）The preparation of gold nano star：With sodium borohydride as reducing agent, sodium citrate is protective agent, is prepared by liquid phase reduction
Silver-colored seed；Gold chloride is added in silver-colored seed solution, and is rapidly added ascorbic acid, silver nitrate simultaneously, prepare gold nano star；
（3）The preparation of flower-shaped SERS substrate：Silicon chip is successively placed in Piranha solution, 3- mercaptopropyl trimethoxysilanes to be carried out
Immersion modification；Silicon chip after by modification is dipped into step（1）In prepared flower-shaped silver-colored solution, flower-shaped silver granuel is formed on silicon chip
Sublayer, obtains flower-shaped SERS substrate；
（4）The preparation of flower-shaped silver/graphene oxide substrate：Graphene oxide solution is dripped to step（3）The flower-shaped silver-based for preparing
On bottom and carry out spin coating；Spin coating rotating speed 1000r/min, spin-coating time 30s, form graphene oxide in flower-shaped silver granuel sublayer
Layer, obtains flower-shaped silver/graphene oxide substrate；
（5）The preparation at flower-shaped silver/graphene oxide/gold nano satellite-based bottom：By step（4）Flower-shaped silver/the graphene oxide for preparing
Substrate is dipped in diallyl dimethyl ammoniumchloride solution and is modified；Subsequently step is immersed in（2）The gold of preparation
In nanometer star solution, by gold nano star particle load to flower-shaped silver/graphene oxide substrate, gold is formed on graphene oxide layer
Nanometer star particle layer, obtains the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure.
During use, the branch number of gold nano star can be controlled by the consumption of control gold chloride（Branch density）And the major diameter of golden branch
Than（Tapering degree）；When being embodied as, when the consumption of gold chloride is more, the branch number of gold nano star is more, and the draw ratio of golden branch is got over
Greatly.Certainly, the outermost load capacity of the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure can be led to
The consumption for crossing gold nano star is controlled.Above-mentioned regulating measure or control device are that those skilled in the art can realize.
Preparation method of the present invention is using 3- mercaptopropyl trimethoxysilanes（MPTMS）Modification silicon chip, then will repair
Silicon chip after decorations is immersed in flower-shaped silver-colored solution, and flower-shaped silver is assembled into formation sandwich in silicon chip substrate by the effect of Ag-S keys
The bottom of structure；Graphene oxide is attached to by flower-shaped silver particles surface by spin-coating method and forms intermediate course；With polydiene third
Base alkyl dimethyl ammonium chloride（PDDA）The substrate for walking preparation in modification makes its surface positively charged, and it is molten to be immersed in gold nano star
In liquid, gold nano star is made to be attached to the upper strata that surface of graphene oxide forms sandwich structure by electrostatic interaction, finally
Form flower-shaped silver/graphene oxide/gold nano star sandwich composite construction.
And, the preparation method of the present invention is very easy, and reaction condition is gentle, favorable reproducibility, is further SERS inspections
Survey and provide advantage.
Description of the drawings
Fig. 1 is the stereoscan photograph of flower-shaped silver/graphene oxide/gold nano star sandwich structure prepared by the present invention.
Fig. 2 is respectively with flower-shaped silver particles, flower-shaped silver/graphene oxide, flower-shaped silver/graphene oxide/gold nano star three
Mingzhi's structure is substrate, with concentration as 10-5Raman spectrograms of the R6G of M for detection molecules.As can be seen from Figure：Flower-shaped silver/oxidation
Graphene/gold nano star sandwich structure substrate has than individual layer silver particles and flower-shaped silver/graphene oxide binary core-shell particles
There is more excellent SERS effects.
Fig. 3 is with flower-shaped silver/graphene oxide/gold nano star sandwich structure as substrate, with concentration as 10-5The R6G of M is
Detection molecules, randomly select 20 points, carry out basal signal repeatability detection Raman spectrogram.As can be seen from Figure：20 random
The Raman signal intensity of point is basically identical, is 5% by being calculated its relative standard deviation, less than literature values 10%, tool
Illustrate that its substrate has good repeatability.
Specific embodiment
Below by specific embodiment, the present invention is expanded on further.
Embodiment 1：
The preparation of flower-shaped silver/graphene oxide substrate, specifically includes following steps：
（1）The preparation of flower-shaped silver particles：Under room temperature, 1M silver nitrates, 1M ascorbic acid, 1M polyvinylpyrrolidones is respectively configured
Solution.The 0.3mL silver nitrate solutiones for preparing and 2mL polyvinylpyrrolidonesolution solutions are added in 10mL deionized waters, are stirred
Mix, subsequently the ascorbic acid solution that 0.2mL is prepared is added rapidly in mixed solution, continue stirring 15 minutes, spent
Shape silver particles.By the flower-shaped silver particles eccentric cleaning for preparing 3 times, treat that next step is used.
（2）The preparation of flower-shaped SERS substrate：Silicon chip is put in the Piranha solution for preparing, place 2 hours at 90 DEG C.
With clean water, 3- mercaptopropyl trimethoxysilanes will be placed into after silicon chip extracting（MPTMS）Soak 1 hour in solution, obtain
The silicon chip of 3- mercaptopropyl trimethoxysilanes modification.The silicon chip that 3- mercaptopropyl trimethoxysilanes are modified is dipped into 10mL steps
（1）30 minutes in prepared flower-shaped silver-colored solution, after taking-up, deionized water cleaning, forms flower-shaped silver granuel sublayer on silicon chip,
Treat that next step is used.
（3）The preparation of flower-shaped silver/graphene oxide substrate：Graphene oxide is prepared with Hummers methods, ultrasonic disperse is prepared
Into 0.25mg/mL graphene oxide solutions.20 μ L graphene oxides are added drop-wise to step（2）Go forward side by side on the flower-shaped SERS substrate for preparing
Row spin coating.Spin coating rotating speed 1000r/min, spin-coating time 30s, in flower-shaped silver granuel sublayer form graphene oxide layer, are spent
Shape silver/graphene oxide substrate.
Embodiment 2：
The preparation method of gold nano star particle silver seed kernel, specifically includes following steps：
Under room temperature, 50 mM silver nitrates, 1%wt sodium citrate solutions is respectively configured.By the 1mL silver nitrate solutiones for having configured and 1mL
Sodium citrate solution is added in 48 mL deionized waters, strong stirring, adds 0.005g sodium borohydrides, continues stirring 15 minutes,
Obtain silver-colored seed.Centrifugation（1200 revs/min, 15 minutes）Upper solution is taken, treats that next step is used.
Embodiment 3
The preparation method of gold nano star particle, specifically includes following steps：
Under room temperature, 1mM silver nitrates, 0.1 M ascorbic acid, 0.1 mM chlorauric acid solutions is respectively configured.Will be molten for 10mL gold chlorides
Liquid is added in the 0.1mL silver seed solutions of the preparation of embodiment 2, stirring, and rapidly joins 0.05 mL ascorbic acid solutions simultaneously
With 0.5 mL silver nitrate solutiones, continue stirring 1 minute, obtain gold nano star solution.
Embodiment 4：
The preparation method of gold nano star particle, specifically includes following steps：
Under room temperature, 1mM silver nitrates, 0.1 M ascorbic acid, 0.15 mM chlorauric acid solutions is respectively configured.By 10 mL gold chlorides
Solution is added in the 0.1mL silver seed solutions of the preparation of embodiment 2, stirring, and it is molten to rapidly join 0.05 mL ascorbic acid simultaneously
Liquid and 0.5 mL silver nitrate solutiones, continue stirring 1 minute, obtain gold nano star solution.
Embodiment 5：
The preparation method of gold nano star particle, specifically includes following steps：
Under room temperature, 1 mM silver nitrates, 0.1 M ascorbic acid, 0.2 mM chlorauric acid solutions is respectively configured.By 10 mL gold chlorides
Solution is added in 0.1 mL silver seed solutions prepared by embodiment 2 and stirs, and it is molten to rapidly join 0.05mL ascorbic acid simultaneously
Liquid and 0.5 mL silver nitrate solutiones, continue stirring 1 minute, obtain gold nano star solution.
Embodiment 6：
The preparation method of gold nano star particle, specifically includes following steps：
Under room temperature, 1mM silver nitrates, 0.1 M ascorbic acid, 0.25 mM chlorauric acid solutions is respectively configured.By 10 mL gold chlorides
Solution is added in 0.1 mL silver seed solutions prepared by embodiment 2 and stirs, and it is molten to be quickly simultaneously introduced 0.05 mL ascorbic acid
Liquid and 0.5 mL silver nitrate solutiones continue stirring 1 minute, obtain gold nano star solution.
Embodiment 7：
The preparation method of the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure, specifically includes following
Step：
Flower-shaped silver/graphene oxide substrate prepared by embodiment 1 is dipped into 2 hours in PDDA solution, deionized water is cleaned；
Then gold nano star solution prepared by embodiment 3 is dipped into again（20 times of concentration）In 3 hours, shape on graphene oxide layer
Into gold nano star particle layer, the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure is obtained.
Embodiment 8：
The preparation method of the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure, specifically includes following
Step：
Flower-shaped silver/graphene oxide substrate prepared by embodiment 1 is dipped into 2 hours in PDDA solution, deionized water is cleaned；
Then gold nano star solution prepared by embodiment 4 is dipped into again（20 times of concentration）In 3 hours, shape on graphene oxide layer
Into gold nano star particle layer, the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure is obtained.
Embodiment 9：
The preparation method of the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure, specifically includes following
Step：
Flower-shaped silver/graphene oxide substrate prepared by embodiment 1 is dipped into 2 hours in PDDA solution, deionized water is cleaned；
Then gold nano star solution prepared by embodiment 5 is dipped into again（20 times of concentration）In 3 hours, shape on graphene oxide layer
Into gold nano star particle layer, the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure is obtained.
Embodiment 10：
The preparation method of the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure, specifically includes following
Step：
Flower-shaped silver/graphene oxide substrate prepared by embodiment 1 is dipped into 2 hours in PDDA solution, deionized water is cleaned；
Then gold nano star solution prepared by embodiment 6 is dipped into again（20 times of concentration）In 3 hours, shape on graphene oxide layer
Into gold nano star particle layer, the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure is obtained.
Embodiment 11：
The preparation method of the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure, specifically includes following
Step：
Flower-shaped silver/graphene oxide substrate prepared by embodiment 1 is dipped into 2 hours in PDDA solution, deionized water is cleaned；
Then gold nano star solution prepared by embodiment 6 is dipped into again（5 times of concentration）In 3 hours, shape on graphene oxide layer
Into gold nano star particle layer, the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure is obtained.
Embodiment 12：
The preparation method of the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure, specifically includes following
Step：
Flower-shaped silver/graphene oxide substrate prepared by embodiment 1 is dipped into 2 hours in PDDA solution, deionized water is cleaned；
Then gold nano star solution prepared by embodiment 6 is dipped into again（10 times of concentration）In 3 hours, shape on graphene oxide layer
Into gold nano star particle layer, the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure is obtained.
The above specific embodiment for the present invention.Technical scheme is not limited to above specific embodiment party
Formula, person skilled in art can carry out some nonessential adjustment on the premise of the know-why without departing from the present invention and change
Dynamic, this has no effect on the flesh and blood of the present invention.
Claims (4)
1. a kind of SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure, it is characterised in that include
Carrier, is followed successively by flower-shaped silver granuel sublayer, graphene oxide particle layer and gold nano star particle layer from bottom to top on the carrier.
2. SERS active groups of a kind of flower-shaped silver/graphene oxide/gold nano star sandwich structure according to claim 1
Bottom, it is characterised in that described carrier is silicon chip.
3. a kind of preparation method of the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure, its feature
It is, comprises the steps：
（1）The preparation of flower-shaped silver particles：With ascorbic acid as reducing agent, with polyvinylpyrrolidone as protective agent, by liquid phase
Reducing process prepares flower-shaped silver particles；
（2）The preparation of gold nano star：With sodium borohydride as reducing agent, sodium citrate is protective agent, is prepared by liquid phase reduction
Silver-colored seed；Gold chloride is added in silver-colored seed solution, and is rapidly added ascorbic acid, silver nitrate simultaneously, prepare gold nano star；
（3）The preparation of flower-shaped SERS substrate：Silicon chip is successively placed in Piranha solution, 3- mercaptopropyl trimethoxysilanes to be carried out
Immersion modification；Silicon chip after by modification is dipped into step（1）In prepared flower-shaped silver-colored solution, flower-shaped silver granuel is formed on silicon chip
Sublayer, obtains flower-shaped SERS substrate；
（4）The preparation of flower-shaped silver/graphene oxide substrate：Graphene oxide solution is dripped to step（3）The flower-shaped silver-based for preparing
On bottom and carry out spin coating；Spin coating rotating speed 1000r/min, spin-coating time 30s, form graphene oxide in flower-shaped silver granuel sublayer
Layer, obtains flower-shaped silver/graphene oxide substrate；
（5）The preparation at flower-shaped silver/graphene oxide/gold nano satellite-based bottom：By step（4）Flower-shaped silver/the graphene oxide for preparing
Substrate is dipped in diallyl dimethyl ammoniumchloride solution and is modified；Subsequently step is immersed in（2）The gold of preparation
In nanometer star solution, by gold nano star particle load to flower-shaped silver/graphene oxide substrate, gold is formed on graphene oxide layer
Nanometer star particle layer, obtains the SERS active-substrate of flower-shaped silver/graphene oxide/gold nano star sandwich structure.
4. SERS active groups of a kind of flower-shaped silver/graphene oxide/gold nano star sandwich structure according to claim 3
The preparation method at bottom, it is characterised in that the branch density and tapering degree of the gold nano star particle of gold nano star particle layer can pass through
The consumption for adjusting gold chloride is regulated.
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| CN107167464A (en) * | 2017-05-25 | 2017-09-15 | 南京大学 | A kind of two-dimension flexible device for quantifying and being imaged for Raman and preparation method thereof |
| CN107598182A (en) * | 2017-07-24 | 2018-01-19 | 西北工业大学 | Gold nano grain molybdenum disulfide gold hypersensitive SERS base materials and preparation method |
| CN110887828A (en) * | 2019-12-04 | 2020-03-17 | 济南大学 | SERS mechanism based on Glass/AuNSts-SLG for detecting rhodamine B in solution |
| CN111017872A (en) * | 2019-11-25 | 2020-04-17 | 西安邮电大学 | Preparation method of sandwich structure composite nano array substrate |
| CN111781188A (en) * | 2020-07-02 | 2020-10-16 | 南通大学 | Preparation method of SERS substrate with aluminum-based flower-shaped composite nanostructure and SERS substrate |
| CN115508331A (en) * | 2022-09-02 | 2022-12-23 | 哈尔滨工程大学 | Raman sensor for rapidly detecting new coronavirus based on integrated optical flow control type microstructure optical fiber and SERS substrate |
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|---|---|---|---|---|
| CN107167464A (en) * | 2017-05-25 | 2017-09-15 | 南京大学 | A kind of two-dimension flexible device for quantifying and being imaged for Raman and preparation method thereof |
| CN107598182A (en) * | 2017-07-24 | 2018-01-19 | 西北工业大学 | Gold nano grain molybdenum disulfide gold hypersensitive SERS base materials and preparation method |
| CN111017872A (en) * | 2019-11-25 | 2020-04-17 | 西安邮电大学 | Preparation method of sandwich structure composite nano array substrate |
| CN111017872B (en) * | 2019-11-25 | 2022-03-04 | 西安邮电大学 | Preparation method of sandwich structure composite nano array substrate |
| CN110887828A (en) * | 2019-12-04 | 2020-03-17 | 济南大学 | SERS mechanism based on Glass/AuNSts-SLG for detecting rhodamine B in solution |
| CN111781188A (en) * | 2020-07-02 | 2020-10-16 | 南通大学 | Preparation method of SERS substrate with aluminum-based flower-shaped composite nanostructure and SERS substrate |
| CN115508331A (en) * | 2022-09-02 | 2022-12-23 | 哈尔滨工程大学 | Raman sensor for rapidly detecting new coronavirus based on integrated optical flow control type microstructure optical fiber and SERS substrate |
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