CN109030453A - A kind of preparation method and application of flexible and transparent SERS substrate - Google Patents
A kind of preparation method and application of flexible and transparent SERS substrate Download PDFInfo
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- CN109030453A CN109030453A CN201810722818.2A CN201810722818A CN109030453A CN 109030453 A CN109030453 A CN 109030453A CN 201810722818 A CN201810722818 A CN 201810722818A CN 109030453 A CN109030453 A CN 109030453A
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Abstract
The invention discloses a kind of preparation method and application of flexible and transparent SERS substrate, it is by HAuCl4After aqueous solution is heated to boiling with vigorous stirring, rapidly join saline citrate, after solution colour variation is stablized, it is condensed back 13 ~ 17 min, stop heating, it is cooled to room temperature under stiring, obtain Au Nano sol, Au Nano sol is added in beaker, n-hexane and alcohol mixed solution are slowly injected into Au Nano sol with Syringe injector at room temperature, slowly form water phase and an oil phase, one layer of nanometer Au film is gradually formed at water-oil interface, after oily phase naturally volatilization to the greatest extent, the single layer nanometer Au for tearing off water phase surface is directly covered with adhesive tape, the remaining aurosol of tape surface is washed with deionized water again, flexible and transparent SERS substrate is made.The present invention can make Au nano particle have better distributing homogeneity on adhesive tape by using above-mentioned technology, maintain the flexibility and viscosity of adhesive tape itself well, can directly be measured in a manner of laser back-illuminated, realize in situ detection.
Description
Technical field
The present invention relates to a kind of preparation method and application of flexible and transparent SERS substrate.
Background technique
The problem of traditional SERS substrate is difficult to control such as Ag, Au, Pt metal electrode there are roughness, poor reproducibility；
The adjustable gold nanorods of draw ratio, the noble metals colloidal sol SERS substrate such as the controllable silver-colored cube of size and silver-colored triangle, exist
The problem of storage stability is poor, not Portable belt, and the influence vulnerable to factors such as external environments such as temperature, pH, ion concentration is interfered；
The hard SERS substrate such as metal island film, quartz, silicon wafer is still difficult to although improving stability and portability to irregular table
Determinand on face carries out effective in situ detection, and certain solvent is needed to extract processing.Therefore, flexibility SERS base is prepared
Bottom is of great significance applied to field quick detection.
Adhesive tape has flexible and sticky dual property, can make SERS substrate effectively close to determinand and firmly adherency and
Determinand surface.There is scholar that nano gold sol preparation SERS substrate is added dropwise directly on adhesive tape in the recent period, and straight with the SERS substrate
SERS signal acquisition is carried out after connecing wiping determinand surface, but due to being detached from situ environment after simple wiping, it can not be true
Reflect determinand remained on surface situation.
Summary of the invention
For the above-mentioned problems in the prior art, the purpose of the present invention is to provide a kind of flexible and transparent SERS substrates
Preparation method and application.
A kind of preparation method of the flexible and transparent SERS substrate, it is characterised in that the following steps are included:
1) HAuCl4Aqueous solution is vigorously stirred down be heated to boiling after, rapidly join saline citrate, solution colour is by shallow
Yellow gradually becomes claret, after solution colour variation is stablized, is condensed back 13 ~ 17 min, stops heating, cold under stiring
But to room temperature, Au Nano sol is obtained, it is stored refrigerated spare；
2) Au Nano sol obtained by step 1) is added in beaker, is at room temperature mixed n-hexane with ethyl alcohol with Syringe injector molten
Liquid is slowly injected into Au Nano sol, slowly forms water phase and an oil phase, and one layer of nanometer Au film is gradually formed at water-oil interface, to
Oily phase after volatilization to the greatest extent, the single layer nanometer Au for tearing off water phase surface is directly covered with adhesive tape, then adhesive tape is washed with deionized water naturally
Au MLF/Tape SERS substrate, i.e. flexible and transparent SERS substrate are completed in aurosol remained on surface, preparation.
A kind of preparation method of flexible and transparent SERS substrate, it is characterised in that HAuCl4The concentration of aqueous solution is
0.08 ~ 0.12 g/L, preferably 0.1 g/L；The concentration of sodium citrate aqueous solution is 8 ~ 12 g/L, preferably 10 g/L.
A kind of preparation method of flexible and transparent SERS substrate, it is characterised in that HAuCl4Aqueous solution and sodium citrate
The volume ratio of aqueous solution is 45 ~ 55:1, preferably 50:1.
The preparation method of a kind of flexible and transparent SERS substrate, it is characterised in that n-hexane and alcohol mixed solution
In, the volume ratio of n-hexane and ethyl alcohol is 0.5 ~ 1.5:1, preferably 1:1.
A kind of preparation method of the flexible and transparent SERS substrate, it is characterised in that in step 2, Au Nano sol and
The volume ratio of n-hexane and alcohol mixed solution is 10:6 ~ 12.
The preparation method of a kind of flexible and transparent SERS substrate, it is characterised in that citrate is potassium citrate or lemon
Lemon acid sodium, preferably sodium citrate.
Application of the flexible and transparent SERS substrate on detection malachite green.
Compared with the existing technology, the beneficial effect that the present invention obtains is:
(1) water/oil interface is assembled into from aqueous solution using alcohol induced Au nano particle directly to prepare with sequential 2 D
The nano-gold film (Au MLF) of structure, and with adhesive tape (Tape) direct transfer techniques, Au MLF/Tape SERS base is prepared
Bottom, using laser back-illuminated in situ detection mode be applied to irregular surfaces detection, have method is simple, preparation time is short,
The advantages that reinforcing effect is good, does not need additional expensive reagent, instrument, it can be realized in situ detection；Relative to Au colloidal sol is straight
The SERS substrate for being added dropwise and preparing on adhesive tape (Tape) is connect, SERS substrate by the method for the invention, Au nano particle is in adhesive tape
(Tape) there is better distributing homogeneity on；
(2) Au MLF/Tape SERS substrate is prepared in the present invention, maintains the flexibility and viscosity of adhesive tape itself well, because
This can be easy to easily be covered on irregular determinand surface, and making to be carried on tape surface can with the active Au MLF of SERS
To realize field quick detection；
(3) SERS spectra of probe molecule malachite green shows that this low cost Au MLF/Tape SERS has very high SERS
Activity, good uniformity can directly be measured in a manner of laser back-illuminated；
(4) the remaining scene of actual sample fish scale surface malachite green may be implemented immediately in this Au MLF/Tape SERS substrate
Detection, detection are limited up to 0.04 μm of ol/L, and spectral response all has good uniformity in entire effectively detection zone.
Detailed description of the invention
The SEM of Fig. 1 Au MLF/Tape SERS substrate schemes；
803 cm of Fig. 2 malachite green-1Locate feature peak intensity with the change curve of concentration；
6 groups of SERS spectras that Fig. 3 takes at random are in 803cm-1Locate characteristic peak intensity distribution；
803 cm of Fig. 4 SERS spectrogram-1Locate feature peak intensity with the change curve of gold chloride volume；
803 cm of Fig. 5 SERS spectrogram-1Locate feature peak intensity with the change curve of ethyl alcohol volume；
803 cm of Fig. 6 SERS spectrogram-1Locate feature peak intensity with the change curve of fish scale malachite green concentration remained on surface.
Specific embodiment
The present invention is further explained in the light of specific embodiments, but the scope of protection of the present invention is not limited thereto.
Embodiment 1:
The 1g bought on aladdin is filled into HAuCl4·4H2O(molecular weight 412) with ultrapure water it is configured to HAuCl4(100 g/L)
Mother liquor it is stand-by, HAuCl in mother liquor4Concentration be 2.43 × 10-1mol/L；
Prepare Au MLF/Tape SERS substrate:
1) prepared by Au colloidal sol: using classical frens method: by the HAuCl of above-mentioned preparation4The mother liquor of (100 g/L) is diluted to
Concentration is 0.1 g/L, and the solution after taking 100 mL to dilute is placed in three-necked flask, is vigorously stirred down after being heated to boiling, quickly
(directly pouring into) 2 mL(10 g/L is added) sodium citrate aqueous solution, solution colour gradually becomes claret by light yellow, to molten
After liquid color change is stablized, 15 min are condensed back, stops heating, is cooled to room temperature under stiring, obtains 2.43 × 10-4
Synthesized Au Nano sol is finally put 4 DEG C of refrigerators and saved backup by the Au Nano sol of mol/L；
2) preparation of Au MLF/Tape SERS substrate: 10 mL of Au Nano sol for taking step 1) to prepare is put into 50 ml beakers
In, with Syringe injector by 10 mL n-hexanes and alcohol mixed solution (V n-hexane: V ethyl alcohol=1:1), slowly it is injected into (about
1 minute 5 milliliters) in Au Nano sol, as n-hexane and ethyl alcohol are slowly injected into Au Nano sol, slowly form water
Oily two-phase, it can be found that water-oil interface can gradually form one layer of nano-gold film, film shows slightly light tone and with metallic luster, to oil
Mutually the single layer nanogold for tearing off water phase surface is directly covered with adhesive tape, then adhesive tape table is washed with deionized water after volatilization to the greatest extent naturally
The remaining aurosol in face prepares and completes Au MLF/Tape SERS substrate, as flexible and transparent SERS substrate, wherein Au MLF
Indicate nano-gold film, Tape indicates adhesive tape；
SEM characterization is carried out to Au MLF/Tape SERS substrate manufactured in the present embodiment, characterization result is as shown in Figure 1, can from Fig. 1
To find out nanogold particle there is no reuniting, although the gap that some of them is slightly distributed, is generally dispersed in
Tape surface, average grain diameter 30nm or so.
Embodiment 2:
Investigate influence of the malachite green concentration to SERS spectra:
Prepare malachite green standard aqueous solution: concentration is respectively 0.05,0.075,0.1,0.15,0.2,0.5,1,1.5,2 and 4 μ
mol/L；
Au MLF/Tape SERS substrate prepared by embodiment 1 detects the malachite green standard aqueous solution of above-mentioned preparation, detection knot
Fruit is as shown in Fig. 2, Fig. 2 is 803 cm of malachite green-1Locate feature peak intensity with the change curve of concentration；
Testing conditions are as follows: use the light source of 632.18 nm as exciting light to inhibit the fluorescence of sample to be tested to interfere, luminous energy quantitative change
Change range is 30 ~ 60 mW, and the time of integration is 10 s.When carrying out SERS test, first 0.4 ml sample solution is dripped in sample cell
On, Au MLF/Tape substrate is covered on sample cell mouth, shines through substrate using laser light source, directly acquisition SERS light
Spectrum signal；
Figure it is seen that SERS spectra signal gradually increases with the increase of malachite green concentration, malachite green concentration
After increasing to certain value, the SERS signal intensity increase detected slows down, and illustrates malachite green solution concentration and its SERS signal
Intensity there is certain correlation in a certain range.
When malachite green concentration is lower, the malachite green point of the Au nanoparticle absorption of Au MLF/Tape SERS substrate
Son it is less, SERS signal is very weak, and with the increase of concentration, the malachite green molecule of absorption gradually increases, SERS spectra signal by
Cumulative strong, after concentration increases to certain value, the SERS signal intensity increase detected slows down, this is because there are single layers by SERS
Effect, the only Raman signal of the nearest molecule of distance Au nano particle can adequately be enhanced, the malachite in outer layer
Since distance becomes remote, enhancement effect significantly reduces green molecule, causes SERS signal to enhance at high concentrations and gradually slows down.
Figure it is seen that malachite green concentration is drawn within the scope of 0.5 ~ 2 μm of ol/L and 0.05 ~ 0.2 μm of ol/L with it
Good linear relationship is presented in graceful feature peak intensity, acquires linear equation in 0.5 ~ 2 μm of ol/L concentration range are as follows: y=54.1x-
19.8, linearly dependent coefficient r=0.993.Linear equation y=18.7x-0.7 in 0.05 ~ 0.2 μm of ol/L concentration range is acquired, linearly
Correlation coefficient r=0.981.Above-mentioned y indicates SERS signal intensity, and x indicates malachite green concentration.
Au MLF/Tape substrate is covered on the sample cell mouth that malachite green solution is not added dropwise, is shone using laser light source
It penetrates through substrate, directly acquisition SERS spectra signal is as blank assay；By response SERS corresponding to 14 blank assays
3 times of standard deviations of spectral signal, the detection for acquiring malachite green are limited to 0.04 μm of ol/L.In addition, when concentration is greater than 2 μ
When mol/L, 803 cm-1The increase for locating feature peak intensity is in saturation trend.
To investigate Au MLF/Tape SERS substrate uniformity, Au MLF/Tape SERS substrate prepared by embodiment 1 is right
The malachite green aqueous solution of 1 μm of ol/L has carried out 6 signal acquisitions, and depict error using above-mentioned testing conditions at random
Stick, as a result as shown in figure 3, illustrate preparation transparent flexible SERS substrate have good uniformity.
Embodiment 3 investigates influence of the gold chloride volume to SERS spectra:
Take the HAuCl of different volumes4(100 g/L) 0.1 mL, 0.2 mL, 0.4 mL, 0.6 mL and 0.8 mL, add ultrapure water extremely
100 mL are in three-necked flask.The concentration for the sodium citrate aqueous solution being wherein added is respectively 20,40,60,80,160 g/L,
His condition carries out the malachite green standard aqueous solution that concentration is 1 μm of ol/L with the Au MLF/Tape SERS substrate of embodiment 1
Detection, for detection method condition with embodiment 2, testing result is shown in Fig. 4；
Gold nanoparticle density in water-oil interface can by adjust the cross-sectional area size of Au collosol concentration and container into
Row control, and Au collosol concentration can be controlled according to the volume that gold chloride is added.When the gold chloride volume of addition increases,
The color of gold nanometer film gradually deepens and has metallic luster, and the change of this color is also adjacent in single layer of gold nanometer film
The plasmon coupling effect of gold nano grain is related.In general, the gold chloride volume of addition is more, is synthetically prepared
Au collosol concentration is higher, and single layer of gold nanometer film coverage and the compactness extent for preparing completion are higher, but single layer of gold nanometer film mistake
If densification, the laser signal from back side illuminaton can be stopped, reduce final SERS signal instead；
As can be seen from Figure 4 when gold chloride small volume, SERS signal is weaker, with the increase of gold chloride volume, SERS letter
Number showing first enhances the trend weakened afterwards.When gold chloride volume is 0.4 mL, the raman spectra of malachite green is most strong, shows
The SERS substrate reinforcing effect prepared under this gold chloride volume is best.
Embodiment 4 investigates influence of the ethyl alcohol volume to SERS spectra:
Change the additional amount of ethyl alcohol, additional amount is respectively 2.5 mL, 3.0 mL, 3.5 mL, 4.0 mL, 4.5 mL and 5.0
ML, keeping the volume ratio of n-hexane and ethyl alcohol is that 1:1 is constant, other conditions with embodiment 1 Au MLF/Tape SERS substrate,
The malachite green standard aqueous solution that concentration is 1 μm of ol/L is detected, detection method condition with embodiment 2, be shown in by testing result
Fig. 5；
The addition volume for changing ethyl alcohol can have a significant impact the pattern of single layer nano-gold film, and specific rule is initially
As the additional amount of ethyl alcohol increases, single layer nano-gold film is gradually formed and area coverage gradually increases, but with continuously adding
Ethyl alcohol, single layer nano-gold film start particle and become larger, and area coverage is obviously shunk, and apparent agglomeration is formed.As can be seen that depositing
In an optimal amount of alcohol added, the area coverage of single layer nano-gold film can be made maximum.
When ethyl alcohol is added volume and is lower than 2.5 mL, rarefaction state is presented in the nano-gold film of solution surface, is not covered entire
Solution surface, and shape is arbitrarily variable, therefore think that reproducibility is bad, do not have the condition for preparing SERS substrate.And add in ethyl alcohol
When entering volume greater than 5.0 mL or more, solution surface affects the complete of monolayer surface film because nano Au particle starts to reunite
Property.
As can be seen from Figure 5 as the increase of volume is added in ethyl alcohol, SERS signal is also gradually increased.Body is added in ethyl alcohol
When product is 4.0 mL, SERS signal reaches maximum, traces it to its cause and thinks, when volume is added as 2.5 mL-4.0 mL in ethyl alcohol
It waits, although nanogold particle can be covered with entire interface, since its quantity is not very much, the mutual distance of nanogold particle
It is larger, the hot spot of enough densifications cannot be formed；When ethyl alcohol be added volume increase after, on the interface of homalographic due to foring more
More nanogold particles, nanogold particle is even closer between each other, forms mutually more hot spots than before, therefore its SERS signal
Increase.
The 5 remaining quick detection of fish scale surface malachite green of embodiment:
When carrying out analog sample SERS detection, fish is immersed in the aqueous solution of different malachite green concentration Z and is taken after 10 min
Out, Au MLF/Tape substrate prepared by embodiment 1 is directly covered on fish scale surface, shines through Au using laser light source
MLF/Tape substrate, directly acquisition SERS spectra signal, testing conditions are the same as embodiment 2；
The concentration of above-mentioned malachite green aqueous solution is respectively 0.05,0.075,0.1,0.15,0.2,0.5,1,1.5,2 and 4 μm of ol/
L；
Testing result as shown in fig. 6, through analysis malachite green concentration within the scope of 0.5-2.0 μm of ol/ with its Raman signatures peak intensity
Good linear relationship, linear equation is still presented in degree are as follows: y=2.02x+0.97, linearly dependent coefficient r=0.981, y indicate Raman
Feature peak intensity, x indicate malachite green concentration.Even if malachite green concentration is down to 0.1 μm of ol/L, still it can be observed that bright
803 aobvious cm-1Characteristic peak.Generally speaking, fish scale malachite green SERS signal intensity remained on surface is directly examined with analog sample
It surveys compared to small an order of magnitude, the matrix that this is possible as fish scale surface is more complicated, occupies most of nanogold
The hotspot location of adhesive tape substrate causes fish scale malachite green signal remained on surface greatly to weaken.
Content described in this specification is only to enumerate to inventive concept way of realization, and protection scope of the present invention is not answered
When the concrete form for being seen as limited by embodiment and being stated, protection scope of the present invention is also only in those skilled in the art's root
According to present inventive concept it is conceivable that equivalent technologies mean.
Claims (7)
1. a kind of preparation method of flexible and transparent SERS substrate, it is characterised in that the following steps are included:
HAuCl4Aqueous solution is vigorously stirred down be heated to boiling after, rapidly join saline citrate, solution colour is by light yellow
Claret is gradually become, after solution colour variation is stablized, 13 ~ 17 min is condensed back, stops heating, be cooled under stiring
Room temperature obtains Au Nano sol, stored refrigerated spare；
Au Nano sol obtained by step 1) is added in beaker, at room temperature with Syringe injector by n-hexane and alcohol mixed solution
It is slowly injected into Au Nano sol, slowly forms water phase and an oil phase, one layer of nanometer Au film is gradually formed at water-oil interface, to oil
Mutually the single layer nanometer Au for tearing off water phase surface is directly covered with adhesive tape, then adhesive tape table is washed with deionized water after volatilization to the greatest extent naturally
Au MLF/Tape SERS substrate, i.e. flexible and transparent SERS substrate are completed in the remaining aurosol in face, preparation.
2. a kind of preparation method of flexible and transparent SERS substrate according to claim 1, it is characterised in that HAuCl4Aqueous solution
Concentration be 0.08 ~ 0.12 g/L, preferably 0.1 g/L；The concentration of sodium citrate aqueous solution be 8 ~ 12 g/L, preferably 10
g/L。
3. a kind of preparation method of flexible and transparent SERS substrate according to claim 2, it is characterised in that HAuCl4Aqueous solution
Volume ratio with sodium citrate aqueous solution is 45 ~ 55:1, preferably 50:1.
4. a kind of preparation method of flexible and transparent SERS substrate according to claim 1, it is characterised in that n-hexane and second
In mixed alkoxide solution, the volume ratio of n-hexane and ethyl alcohol is 0.5 ~ 1.5:1, preferably 1:1.
5. a kind of preparation method of flexible and transparent SERS substrate according to claim 1, it is characterised in that in step 2, Au
The volume ratio of Nano sol and n-hexane and alcohol mixed solution is 10:6 ~ 12.
6. a kind of preparation method of flexible and transparent SERS substrate according to claim 1, it is characterised in that citrate is
Potassium citrate or sodium citrate, preferably sodium citrate.
7. as the flexible and transparent SERS substrate of claim 1 ~ 6 either method preparation is detecting the application on malachite green.
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| CN110625134A (en) * | 2019-09-17 | 2019-12-31 | 天津工业大学 | Preparation method of anti-counterfeiting film based on double-layer gold nanorods |
| CN110763669A (en) * | 2019-10-28 | 2020-02-07 | 江苏师范大学 | Disposable SERS paper substrate, preparation method and application thereof |
| CN110790220A (en) * | 2019-10-29 | 2020-02-14 | 深圳大学 | Surface-enhanced Raman scattering substrate, preparation method thereof and in-situ rapid detection method |
| CN112893865A (en) * | 2021-03-26 | 2021-06-04 | 江苏师范大学 | Double-layer gold nanoparticle modified flexible SERS substrate and preparation method thereof |
| CN113125409A (en) * | 2021-03-25 | 2021-07-16 | 云南省烟草质量监督检测站 | Method for rapidly detecting butralin in tobacco by surface enhanced Raman scattering |
| CN115753731A (en) * | 2022-11-21 | 2023-03-07 | 吉林大学 | Flexible wearable glove-based SERS substrate, preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110625134A (en) * | 2019-09-17 | 2019-12-31 | 天津工业大学 | Preparation method of anti-counterfeiting film based on double-layer gold nanorods |
| CN110763669A (en) * | 2019-10-28 | 2020-02-07 | 江苏师范大学 | Disposable SERS paper substrate, preparation method and application thereof |
| CN110790220A (en) * | 2019-10-29 | 2020-02-14 | 深圳大学 | Surface-enhanced Raman scattering substrate, preparation method thereof and in-situ rapid detection method |
| CN113125409A (en) * | 2021-03-25 | 2021-07-16 | 云南省烟草质量监督检测站 | Method for rapidly detecting butralin in tobacco by surface enhanced Raman scattering |
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| CN112893865A (en) * | 2021-03-26 | 2021-06-04 | 江苏师范大学 | Double-layer gold nanoparticle modified flexible SERS substrate and preparation method thereof |
| CN115753731A (en) * | 2022-11-21 | 2023-03-07 | 吉林大学 | Flexible wearable glove-based SERS substrate, preparation method and application thereof |
| CN115753731B (en) * | 2022-11-21 | 2024-05-14 | 吉林大学 | Flexible wearable glove-based SERS substrate, preparation method and application thereof |
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Application publication date: 20181218 |