CN107589103A - A step solution assemble method of the silver nano flower-like on fiber - Google Patents
A step solution assemble method of the silver nano flower-like on fiber Download PDFInfo
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Abstract
The present invention relates to a kind of implementation method of high-efficiency fiber shape SERS substrates, and in particular to a kind of self-assembling method of silver nano flower-like rich in nanometer gap on the fibers such as graphene.Method adds deionized water, fiber, which is suspended in midair to lucky, to be totally submerged in reaction solution using beaker as reaction vessels；Under conditions of ice-water bath and magnetic stirring, silver nano flower-like and the package assembly of fiber are synthesized in 5min using four kinds of silver nitrate, PVP, citric acid and ascorbic acid medicines.The composite fibre has the characteristics of flexible light and good mechanical stability, is a kind of high-efficiency soft SERS substrates, to Luo Dan names 6G detection limit up to 10‑12M.Ice-water bath and magnetic stirring condition of the present invention can be replaced with normal temperature and hand operated mixing, and in the case of using natural fiber, the cost of SERS substrates is reduced to 5 points/.This method has simple and quick, inexpensive and the advantages of can be mass, and great application advantage be present in resource-constrained region.
Description
Technical field
The present invention relates to a kind of direct-assembling method of silver nano flower-like on fiber, a kind of efficient fibre rich in nanometer gap
Tie up the implementation method of shape SERS (SERS) substrate, a kind of simple and quick, the inexpensive and fibre that can be mass
Tie up SERS substrate processing methods.More particularly to an a kind of " step of silver nano flower-like rich in nanometer gap on the fibers such as graphene
Solution " self-assembling method.Present invention would apply in Raman detection, realized using the fiber rich in nanometer gap of synthesis fast
The overdelicate SERS detections of speed.
Background technology
SERS (Surface Enhanced Raman Spectroscopy, SERS), because it can be fast
The immanent structure information of molecule is provided fast hypersensitive, is widely used in sensing, ring as a kind of strong analysis tool
The field such as border detection, biomedicine, food security, trace analysis or even Single Molecule Detection.Generally, the Raman signal of probe molecule
Can be by realizing being greatly enhanced for signal with two kinds of mechanism of substrate chemical bonding and/or electromagnetic interaction.Wherein, electromagnetism
Enhancing mechanism is to strengthen Raman signal using the surface plasmon oscillations of metal nanoparticle, is deposited in SERS field of detecting
It is being widely applied.Metal can produce the collective oscillation of surface phasmon-free electron in the presence of incident light.Work as gold
When belonging to the gap that nanoscale is rich in nanostructured, great local Electromagnetic enhancement can be produced at nanometer gap, is formed
" focus " effect, is advantageously implemented the enhancing of surface-enhanced Raman signals, so " focus " effect of metal Nano structure is wide
It is used for lifting local SERS detectivities generally.By introducing hot spot-effect, SERS detection spirit in micronano optical structure
Sensitivity can be horizontal close to single-molecule detection.However, the preparation of SERS substrates still exist complex process, to equipment requirement compared with
It is high, be difficult to the limitation produced in batches, limit further practical application.
The performance of SERS substrates greatly influences and determined the detection performance of Raman signal.It is highly sensitive in order to realize
SERS is detected, and various SERS substrates rich in nanometer gap are devised and implemented.According to the pattern of carrier, it is substantially divided
For two classes：Two dimensional surface carrier micro-nano structure and one dimension fibre carrier micro-nano structure.For two dimensional surface carrier, researcher's exploitation
Manufacturing process, these means such as nanolithographic, self assembly and mould plate technique respectively have advantage and disadvantage.Nanolithography can realize essence
Fine tuning control and orderly metal array structure, but be unfavorable for largely producing；Self-assembling method has inexpensive, simple to operate excellent
Point, but it is slightly inadequate in terms of regulation and control；Mould plate technique technology have can largely produce with finely regulating advantage, but post-processing fiber crops
Tired, technological process is complicated, the nanostructured being easily destroyed in template.
Because fiber has the advantages of flexible, flexibly light, inexpensive, surface utilisation is high, realized based on fiber
Micro-nano structure is also favored by SERS researchers.By using the guide-lighting feature of optical fiber, researchers are by different end faces
Optical fiber is combined with metal nanoparticle, is prepared into flexibly compact SERS probes or small-sized Raman spectrometer and (is referred to non-patent
Document 1-4).In addition, cheap chemical fibre is combined with metal nanoparticle and prepares the methods of fibrous SERS substrates and also enjoy
Concern.Jonathan Mbah adsorb 0 valency silver particles in carbon fiber surface using constant-temperature shaking culture method and make SERS substrates,
The problem of Argent grain concentration is less than normal, spot concentrations are relatively low (referring to non-patent literature 5) be present；Sudip Malik groups utilize submergence
In polyaniline fiber adsorption, some synthetic silver nano-grains realize SERS substrates to method, and this method needs two
Step is completed and the packaging efficiency of silver nano-grain is relatively low (referring to non-patent literature 6)；Sputtering is had silver nanoparticle by Wang et al.
The porous zinc bloom nanometer sheet of grain is grafted onto on flexible carbon cloth, and efficient SERS substrates (referring to non-patent literature 7) are made,
This method complex process, and need to use the large scale equipments such as ald (ALD)；Pan et al. is in PmPD and PAN nanofibers
On realize the SERS substrates (referring to non-patent literature 8) of Nano silver piece package assembly.Generally speaking, fibrous SERS substrates " heat
Point " quantity and the uniformity all have much room for improvement, and existing preparation method is mostly complicated multi-step synthetic method, is being produced in batches
Aspect also has to be optimized, limits its practical application.
To sum up, the invention provides a kind of simple and quick, the inexpensive and high-efficiency fiber shape SERS substrates that can be mass
Implementation method, i.e., using fibers such as graphenes as carrier, with reference to silver nano flower-like, using a step solution synthesis method directly in fiber
Upper silver nano flower-like of the growth rich in nanometer gap, obtains efficient fibrous SERS substrates.Method therefor of the present invention
Non-patent literature 1：
Xie Zhiguo, the fibre optical sensor research of metal nanoparticle, China Science ＆ Technology University, Ph.D. Dissertation.
Non-patent literature 2：
David L.Stokes,Tuan Vo-Dinh,Development of an integrated single-fiber
SERS sensor,Sensors and Actuators B,2000.69:p.28–36.
Non-patent literature 3：
Carmen Viets,Wieland Hill*,Single-fibre surface-enhanced Raman
sensorswith angled tips,J.Raman Spectrosc.,2000.31:p.625–631.
Non-patent literature 4：
Carmen Viets,Wieland Hill,Journal of Molecular Structure,2001.563:
163.
Non-patent literature 5：
Jonathan Mbah,etal.,A rapid technique for synthesis of metallic
nanoparticles for surface enhanced Raman spectroscopy,J.Raman Spectrosc.,
2013.44:p.723–726
Non-patent literature 6：
Mondal,S.,U.Rana,and S.Malik,Facile decoration of polyaniline fiber
with Ag nanoparticles for recyclable SERS substrate,ACS applied materials&
interfaces,2015.7(19):p.10457-10465.
Non-patent literature 7：
Zhiwei Wang,etal.,Ag-nanoparticle-decorated porous ZnO-nanosheets
grafted on a carbon fiber cloth as effective SERS substrates,Nanoscale,
2014.6:p.15280–15285
Non-patent literature 8：
Peng Jia,etal.,Fabrication and Formation Mechanism of Ag Nanoplate-
Decorated Nanofiber Mats and Their Application in SERS,Chem.Asian J.,2016.11:
86–92.
The content of the invention
The invention provides a kind of direct self assembly side of silver nano flower-like rich in nanometer gap on the fibers such as graphene
Method, this method is simple, cost is cheap, batch production can be achieved.Package assembly based on this method synthesis has abundant nanometer
Gap, be widely distributed between nano flower " petal ", between adjacent nano flower and nano flower with interfibrous gap, Ke Yishi
Now to the detection of low concentration SERS signal；Silver nano flower-like and the package assembly of fiber there is very strong absorption to make probe molecule
With the quick detection of SERS signal can be realized；Silver nano flower-like and the package assembly of fiber have good mechanical stability, are expected to
It is applied to flexible field of detecting.
The technical scheme is that：" a step solution synthesis method " realizes silver nano flower-like and the package assembly of fiber.Choosing
It is reaction vessels to select beaker, adds deionized water, fiber, which is suspended in midair to lucky, to be totally submerged in deionized water, such as Fig. 1 institutes
Show；Under conditions of ice-water bath and magnetic stirring, four kinds of silver nitrate, PVP, citric acid and ascorbic acid medicines are sequentially added, are controlled
Reaction time is 5min；Fiber is taken out, is rinsed with deionized water/ethanol, (80 DEG C) is dried in vacuum drying oven, obtains Yin Na
The package assembly of popped rice and fiber.
The reaction condition being related in technical solution of the present invention can adjust, with normal temperature and hand operated mixing replace ice-water bath and
Magnetic stirring condition, as shown in Fig. 2 to meet energy-conservation or the hypodynamic specific demand of outlying mountain area's electricity.
Technical scheme can meet the needs of mass production, can be with using experimental provision as shown in Figure 3
Substantial amounts of silver nano flower-like and the package assembly of fiber are disposably obtained, realizes the batch production of high-performance SERS substrates.
The large scale that technical scheme can be directly realized by silver nano flower-like and fiber assembles, as shown in figure 4, can be with
Directly obtain the fiber of silver nano flower-like parcel.
In such scheme, have chosen graphene fiber, carbon fiber, string, aramid fiber and the hair that authorizes be used as from
Assemble the fibrous substrate of silver nano flower-like structure；
In such scheme, ice water bath environment, its temperature control is at 0~10 DEG C；Magnetic stirring condition, is carried by magnetic stirring apparatus
For；Drying preserves equipment, and using vacuum drying oven, temperature control is at 80 DEG C.
In such scheme, the changeability of reaction condition, normal temperature condition temperature is at 25~30 DEG C, and hand operated mixing is by glass bar
Carry out.
Compared with prior art, the advantage of the invention is that：
1st, silver nano flower-like is directly grown on fiber using a step solution synthesis method herein, realized fibrous efficient
The preparation of SERS substrates.This is a kind of new technology for preparing SERS substrates, prepares simple and quick, and can meet to produce in batches
(accompanying drawing 3), there is potential application prospect in the industrial production.
2nd, the package assembly based on this method synthesis has abundant nanometer gap, is widely distributed in nano flower " petal "
Between, between adjacent nano flower and nano flower and interfibrous gap, it is possible to achieve the detection to low concentration SERS signal, to sieve
Red bright 6G detectable limit is up to 10-12M, such as accompanying drawing 6；Silver nano flower-like and the package assembly of fiber have good mechanically stable
Property, it is 5x10 in rhodamine 6G concentration-7In the case of M, Characteristic Raman peak 611.5cm-1Peak strength as shown in Figure 7, table
The bright SERS substrates have good mechanical stability, are expected to be applied to flexible field of detecting.
3rd, ice-water bath and magnetic stirring condition are replaced with normal temperature and hand operated mixing, controls the reaction time, can also be successfully realized
High-efficiency fiber shape SERS substrates, to the detection limit of rhodamine 6G up to 10-12M, such as accompanying drawing 15.This allows for this method and disobeyed
Rely in electric power, be expected to be applied to electric power deficient field or region.
4th, this method is applied to the fiber that nature obtains, such as string and the hair to come off, fine using nature
In the case of dimension, the cost of SERS substrates is reduced to 5 points/, has obvious price advantage.
Brief description of the drawings
Fig. 1 is the schematic diagram of explanation synthesis silver nano flower-like according to embodiments of the present invention and the method for fiber package assembly；
Fig. 2 is the schematic diagram of explanation synthesis silver nano flower-like according to embodiments of the present invention and the method for fiber package assembly；
Fig. 3 is the schematic diagram of explanation synthesis silver nano flower-like according to embodiments of the present invention and the method for fiber package assembly；
Fig. 4 is the schematic diagram of explanation synthesis silver nano flower-like according to embodiments of the present invention and the method for fiber package assembly；
The package assembly of Fig. 5 silver nano flower-likes and graphene fiber；
The SERS design sketch of the silver nano flower-like and graphene fiber package assembly of Fig. 6 synthesis；
The SERS detection stability of the silver nano flower-like of Fig. 7 synthesis and graphene fiber package assembly；
The silver nano flower-like and graphene fiber package assembly of Fig. 8 batch synthesis；
The SERS design sketch of the silver nano flower-like and graphene fiber package assembly of Fig. 9 batch synthesis；
The package assembly of Figure 10 silver nano flower-likes and carbon fiber；
The SERS design sketch of the silver nano flower-like and carbon fiber package assembly of Figure 11 synthesis；
The package assembly of Figure 12 silver nano flower-likes and the hair to come off；
The SERS design sketch of the silver nano flower-like and hair package assembly of Figure 13 synthesis；
The silver nano flower-like realized under the conditions of Figure 14 room temperatures and hand operated mixing and graphene fiber package assembly；
The SERS effects of the silver nano flower-like realized under the conditions of Figure 15 room temperatures and hand operated mixing and graphene fiber package assembly
Figure.
Embodiment
In order to be better understood from the present invention, with reference to the example content that the present invention is furture elucidated.
Example 1：The preparation flow of silver nano flower-like and the package assembly of graphene fiber：The first step, graphene fiber is (wet
Method textile technology obtains, and is provided by Suzhou nanometer) 8mm length is uniformly cut into, it is clean with deionized water and alcohol flushing, dry,
Then it is fixed in advance on ready PET sheet, it is standby；Second step, ice-water bath condition is kept, added in 25mL beaker
Enter 10mL deionized waters, the graphene fiber got ready is suspended in midair and immersed, then, it is dense that 1mL is added into reaction beaker with pipettor
Spend the silver nitrate (AgNO3 for 0.5M：99.9999%, Aldrich), carry out magnetic agitation；3rd step, after 5min, continue with moving
Liquid device adds the PVP (PVP that 1mL concentration is 0.3M into beaker:Mw=1,300,000, Aladdin), wait
15min；4th step, the citric acid (CA that 0.1mL concentration is 0.25M is added into beaker with pipettor：Aldrich), continue
Treat 10min；5th step, the ascorbic acid (AA that 1mL concentration is 0.5M is added into beaker with pipettor：99.9%,
Aladdin), reaction solution is quickly turned to Dark grey by transparent, reacts five minutes, stops magnetic agitation, takes out reaction product, uses second
Alcohol and deionized water rinsing, are placed in 80 degree of vacuum drying oven and dry, that is, obtain silver nano flower-like and graphene fiber package assembly
SERS substrates, air-isolation preserve.ESEM is as shown in Figure 5, it can be seen that silver nano flower-like is uniformly wrapped in graphene fiber
Surface.
The preparation of SERS test samples：It is as substrate, rhodamine 6G using silver nano flower-like and the package assembly of graphene fiber
It is introduced exemplified by probe molecule：The rhodamine 6G aqueous solution of 1mL various concentrations is taken to be placed on 1mL small test tube with pipettor
In, prepare substrate sample is dipped into small test tube, controls soak time 12h, takes out, is fixed on clean aluminium foil
On, it is placed on drying (80 degree) in vacuum drying oven, you can carry out Raman test.With the spectrometer of Horiba Jobin Yivon companies
LabRAM Araims are tested, and excitation source chooses 532nm green (light) laser, and about 3 μm of spot diameter, power is elected as
1mW, it is 500-1800cm to adopt spectral limit-1, time for exposure 2s, integral number of times is 2 times.Obtain Raman spectrum as shown in Figure 6
Figure.
Example 2：The batch preparation flow of silver nano flower-like and the package assembly of graphene fiber：The first step, graphene is fine
Dimension (wet method textile technology obtains, and is provided by Suzhou nanometer) is uniformly cut into 8mm length, clean with deionized water and alcohol flushing,
They, are then fixed in advance on ready PET sheet by drying, standby；Second step, ice-water bath condition is kept, 25mL's
10mL deionized waters are added in beaker, the graphene fiber array got ready is suspended in midair and immersed, then, with pipettor to reaction beaker
Middle addition 1mL concentration is 0.5M silver nitrate (AgNO3：99.9999%, Aldrich), carry out magnetic agitation；3rd step, 5min
Afterwards, continue to add the PVP (PVP that 1mL concentration is 0.3M into beaker with pipettor:Mw=1,300,000,
Aladdin), 15min is waited；4th step, the citric acid (CA that 0.1mL concentration is 0.25M is added into beaker with pipettor：
Aldrich), 10min is continued waiting for；5th step, the ascorbic acid (AA that 1mL concentration is 0.5M is added into beaker with pipettor：
99.9%, Aladdin), reaction solution is quickly turned to Dark grey by transparent, reacts five minutes, stops magnetic agitation, takes out reaction production
Thing, with ethanol and deionized water rinsing, it is placed in 80 degree of vacuum drying oven and dries, that is, obtain large quantities of silver nano flower-likes and graphene
Fiber package assembly SERS substrates (as shown in Figure 8).
With the SERS detection methods as example 1, the Raman signal of stable performance can obtain (such as to each sample
Shown in Fig. 9).
Example 3：The preparation of silver nano flower-like and the package assembly of carbon fiber：(provided using carbon fiber by Suzhou nanometer),
Using the technical step as example 1, silver nano flower-like and carbon fiber package assembly (as shown in Figure 10) are obtained.
With the SERS detection methods as example 1, the Raman signal (as shown in figure 11) of stable performance can obtain.
Example 4：The preparation of silver nano flower-like and the package assembly of dropped hair：Using the hair to come off naturally, deionization is used
Water and alcohol flushing are clean, drying, then they are fixed in advance on ready PET sheet, using the skill as example 1
Art step, obtain silver nano flower-like and the package assembly (as shown in figure 12) of hair.
With the SERS detection methods as example 1, the Raman signal (as shown in figure 13) of stable performance can obtain.
Example 5：Silver nano flower-like and the package assembly of fiber are realized in the case of room temperature and hand operated mixing.Utilize graphene
Fiber (is provided) by Suzhou nanometer, at ambient temperature, magnetic stick is replaced with hand operated mixing, and other are used and example 1 one
The technical step of sample, obtain silver nano flower-like and graphene fiber package assembly (as shown in figure 14).
With the SERS detection methods as example 1, the Raman signal (as shown in figure 15) of stable performance can obtain.
Claims (6)
1. the present invention relates to a kind of simple and quick, the inexpensive and realization side of high-efficiency fiber shape SERS substrates that can be mass
A kind of method, and in particular to self-assembling method of silver nano flower-like rich in nanometer gap on the fibers such as graphene.Method choice burns
Cup is reaction vessels, and fiber, which is suspended in midair to lucky, to be totally submerged in reaction solution；Under conditions of ice-water bath and magnetic stirring, according to
Secondary that reaction reagent is added into beaker, it is 5min to control the reaction time, is reacted with a large amount of frozen water Quick stops；Fiber is taken out, is used
Deionized water/ethanol is rinsed, and is dried, and is preserved.In addition, it is related to the change of reaction condition in the present invention, with normal temperature and manually
Stirring successfully obtains high-efficiency fiber shape SERS substrates instead of ice-water bath and magnetic stirring condition.
2. the fiber according to claim one, graphene fiber, carbon fiber, string aramid fiber are have chosen in invention and is awarded
The natural dropped hair weighed.
3. the reaction reagent according to claim one, silver nitrate (oxidant), polyvinylpyrrolidone (PVP) (dispersant,
End-capping reagent), citric acid (end-capping reagent), ascorbic acid (reducing agent).
4. the terminating reaction condition according to claim one, real process is quick into reaction beaker when reacting 5min
The frozen water for adding about 20 times of total volume of reaction solution comes significantly diluting reaction concentration, Quick stop reaction.
5. the ice water bath environment according to claim one, its temperature control is at 0~10 DEG C；Magnetic stirring condition, is stirred by magnetic force
Device offer is provided；Drying preserves equipment, and using baking oven, temperature control is at 80 DEG C.
6. the changeability of the reaction condition according to claim one, normal temperature condition temperature at 25~30 DEG C, borrow by hand operated mixing
Glass bar is helped to carry out.
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| CN113877643A (en) * | 2021-09-18 | 2022-01-04 | 重庆市益康环保工程有限公司 | Cellulose 3D enhanced Raman spectrum microfluidic chip for detecting water pollution and application thereof |
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| CN113877643A (en) * | 2021-09-18 | 2022-01-04 | 重庆市益康环保工程有限公司 | Cellulose 3D enhanced Raman spectrum microfluidic chip for detecting water pollution and application thereof |
| CN113877643B (en) * | 2021-09-18 | 2022-09-13 | 重庆市益康环保工程有限公司 | Cellulose 3D enhanced Raman spectrum microfluidic chip for detecting water pollution and application thereof |
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