CN110082341A - SERS substrate preparation based on nanosphere etching and its application in explosive TNT detection - Google Patents

SERS substrate preparation based on nanosphere etching and its application in explosive TNT detection Download PDF

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CN110082341A
CN110082341A CN201910465736.9A CN201910465736A CN110082341A CN 110082341 A CN110082341 A CN 110082341A CN 201910465736 A CN201910465736 A CN 201910465736A CN 110082341 A CN110082341 A CN 110082341A
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solution
raman
aminothiophenol
substrate
tnt
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CN110082341B (en
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高荣科
宋雪飞
毛元朔
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Hefei University of Technology
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Hefei University of Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65Raman scattering
    • G01N21/658Raman scattering enhancement Raman, e.g. surface plasmons

Abstract

The invention discloses the SERS substrate etched based on nanosphere preparation and its applications in explosive TNT detection, it is related to Surface enhanced Raman spectroscopy detection field, it solves since explosive TNT raman scattering cross section is small, it is difficult to the problem of carrying out direct trace detection, now propose following scheme, it is the following steps are included: S1, the spin coating of single layer polystyrene microsphere in PET film: first to PET film hydrophilic treated, then PS ball mother solution is centrifuged and is moved in the mixed solution containing ethyl alcohol and methanol that volume ratio is 2:1, and PS solution concentration is finally adjusted to 2.5 w/v%, surfactant TX-100 is added in final mixture with 0.5 volume %, then the PS solution that a drop volume is about 8 μ l is spin-coated on pure PET film.The present invention realizes quick, efficient, lossless decomposition, and operates without professional person, and detection operating process is simple, by the way of detecting indirectly, can achieve lower detection limit.

Description

SERS substrate based on nanosphere etching prepares and its in explosive TNT detection Using
Technical field
The present invention relates to Surface enhanced Raman spectroscopy detection fields, more particularly to the SERS substrate system based on nanosphere etching Application standby and its in explosive TNT detection.
Background technique
Surface enhanced Raman spectroscopy (Surface-Enhanced Raman Spectroscopy) is used as a kind of highly sensitive inspection Substance tool is surveyed, Fleischmann et al. is obtained for the first time after 1974 are roughened smooth silver electrode surface It is adsorbed on the Raman spectrum of the high quality of monolayer Pyridine Molecules in silver electrode surface.But Fleishmann it is thought that due to The roughening of electrode surface, electrode real table area increase and make absorption Pyridine Molecules amount increase caused by, without anticipate Rough surface is known to the humidification of the raman spectral signal of binding molecule.Until 1977, Van Duyne and Creighton Liang Ge study group finds each independently, is adsorbed on the Raman letter of each Pyridine Molecules of coarse silver electrode surface It is number about stronger by 10 than the Raman signal of Pyridine Molecules single in solution6, it is indicated that this is a kind of surface relevant to rough surface Enhancement effect, referred to as SERS effect.SERS detection mode overcomes the contact measurement of traditional chemical detection mode, realizes Harmless, trace materials detection, there is quick detection speed, sample pre-treatments operation summary, scene may be implemented and When detection, the advantages that spectrogram reaction information is obvious.With the further development of science and technology, Raman spectrum detecting device of new generation is more Sample, portability, intelligence have become a kind of powerful species analysis detection means, have been widely cited and lead in various industries Domain.
Trinitrotoluene (English: Trinitrotoluene, abbreviation: TNT) is a kind of colourless or light yellow crystal, odorless, Have hygroscopicity, fusing point is 354K(80.9 °C), it, with explosivity, is one of common Explosive ingredients.Trinitrotoluene is medium Toxicity, can percutaneous, respiratory tract, alimentary canal intrusion, main harm is slow poisoning, and local skin stimulation generates dermatitis.TNT is simultaneously It is also the important component of a variety of explosives, the main dress explosive of our countries is still TNT at present, so detection TNT In the presence of being Main way to explosive detection.Since the production of TNT, preparation, transport and using can all make in natural environment There are a small amount of TNT, this can cause the pollution of serious pollution, especially soil and water resource to environment.
Trace explosive detection technique mainly detects explosive and distributes the remaining explosive particle trace in steam With remaining trace on the people or object that were contacted with explosive.Currently, the detection method of micro explosive mainly has Ion transfer Spectroscopic methodology, chemiluminescence, gas chromatography, infra-red sepectrometry, mass spectrography etc..Because of above-mentioned detection technique or unsuitable scene Detection needs test sample to do a large amount of pre-treatment and prepares, can not achieve the sample of non-destructive testing;Detection device is expensive, Be not suitable for popularizing in an all-round way.The characteristics of Raman detection technology is due to its quick detection and non-destructive testing, becomes a kind of ideal Detection technique.Since the raman scattering cross section of TNT molecule is smaller, directly detection is difficult to detect the spectrogram of low concentration, and TNT molecule can not be effectively connected with each other with gold, silver nanoparticle, so cannot be needed by the way of directly detecting to inspection The Raman substrate of survey is modified, and so that Raman substrate is effectively adsorbed more TNT molecules, is reached the water of trace detection It is flat.Common modification reagent has cysteine, polydiacetylene, p-Mercaptoaniline etc. to form complex compound with TNT molecule, to facilitate inspection It surveys and determines.
Reactive ion etching technology is the dry etching technology that a kind of anisotropy is very strong, selectivity is high.It is in vacuum It is performed etching in system using molecular gas plasma, ion induction chemical reaction is utilized to realize that anisotropy is carved Erosion is that made to be etched using the ion energy surface of layer is formed the damaging layer for being easy etching and promotes chemical reaction, simultaneously Ion can also remove surface resultant to expose the effect of clean etching surface.
Summary of the invention
The purpose of the present invention is to solve due to explosive TNT raman scattering cross section it is small, it is difficult to carry out direct trace inspection The problem of survey, and the SERS substrate preparation based on nanosphere etching proposed and its application in explosive TNT detection.
To achieve the goals above, present invention employs following technical solutions:
SERS substrate preparation based on nanosphere etching and its application in explosive TNT detection, comprising the following steps:
S1, the spin coating of single layer polystyrene microsphere in PET film: first to PET film hydrophilic treated, then by PS ball mother solution It is centrifuged and moves in the mixed solution containing ethyl alcohol and methanol that volume ratio is 2:1, and PS solution concentration is finally adjusted to 2.5 Surfactant TX-100 is added in final mixture by w/v% with 0.5 volume %, is then about 8 μ l by a drop volume PS solution be spin-coated on pure PET film, rotated 15 seconds at 650 rpm, then 1000 rpm spin coating 1 second, excessive to remove Film is kept for a few minutes in the heater so that solvent seasoning, obtains the PET film with single layer PS ball in this way by liquid;
Reactive ion etching: S2 the PET film with single layer PS ball is placed in the etch chamber of reactive ion etching machine and is carried out Etching, adjusting etch period are 5min, finally obtain the cyclic array containing nanocone on PET film surface, obtain the period Property nano-cone array film substrate;
S3, electron beam deposition gold nano grain: by the periodic nanometer cone array film substrate of acquisition in electron beam deposition system In gold-plated, the Raman substrate with a thickness of 30nm of finally obtained gold nanoparticle carried out with the rate of 0.02 ~ 0.03nm/s;
The modification of PET film substrate: S4 4- aminothiophenol is dissolved in ethanol solution for 10-5mol/L as 4- using concentration Then 4- aminothiophenol original solution is taken and a certain amount of ethyl alcohol is used to be diluted to 10- as solvent by aminothiophenol original solution 7mol/L, then will be gold-plated after Raman substrate be completely submerged in the 4- aminothiophenol solution of 10-7mol/L, impregnated under room temperature 10h is three times washed out the 4- aminothiophenol molecule being not connected in Raman substrate with deionized water continuous flushing after taking-up, 10s is rinsed every time, then at room temperature to dry;
S5, the synthesis of Nano silver grain: being that the 9mg/ml silver nitrate solution of 10ml is added in the deionized water of 490ml first, It is boiled in the case where magneton revolving speed is the rate of 550r/min, the sodium citrate that the mass fraction that 10ml is then slowly added dropwise is 1% is molten Liquid, solution continue to keep fluidized state 1h after becoming taupe;
The surface modification of Nano silver grain: S6 takes the 4- aminothiophenol solution of the 10-4mol/L of 100ul to be added to the silver of 900ul In glue, one hour is vibrated in an oscillator to achieve the effect that sufficiently adsorbing for 4- aminothiophenol molecule and Nano silver grain, 4- aminothiophenol molecule and Nano silver grain form the S-Ag key of strong interaction;
The connection of S7, TNT molecule: the Raman substrate in the 4- aminothiophenol solution for being immersed in 10-7mol/L is immersed in not With 10h in the TNT ethanol solution of concentration, take out at room temperature to dry;
S8, Raman detection.
Preferably, in the step S8 Raman detection the following steps are included:
S81, substrate compliance test result: being configured to mother liquor for R6G molecular melting in ethanol, is then diluted to by ethyl alcohol different dense The prepare liquid of degree, it is gold-plated after Raman substrate be immersed in the R6G solution of various concentration its surface made to connect upper determinand molecule R6G verifies the Raman effect of prepared substrate by the Raman spectrum that Raman Measurement obtains;
The verifying of S82, TNT effect: three kinds of samples are detected respectively, first is that being immersed in 10-7mol/L4- aminothiophenol solution The Raman substrate of 10h is taken out second is that being immersed in the Raman substrate of 10h in 10-7mol/L 4- aminothiophenol solution and rinses 3 It is secondary, then it is immersed in 10h in the elargol of 4- aminothiophenol modification, it takes out and rinses, drying at room temperature is to be measured, third is that being immersed in 10- The Raman substrate of 10h in 7mol/L 4- aminothiophenol solution is taken out and is rinsed 3 times, then is immersed in the TNT solution of 10-5mol/L Middle 10h takes out wait do, is finally immersed in 10h in the elargol of 4- aminothiophenol modification, takes out and rinse 3 times, drying at room temperature waits for It surveys;
S83, TNT gradient concentration: being immersed in 10h in 10-7mol/L 4- aminothiophenol solution for Raman substrate, take out and rinse, It is separately immersed in 10h in the TNT solution of 10-8 ~ 10-13mol/L again, takes out wait do, is finally immersed in the modification of 4- aminothiophenol Elargol in 10h, take out rinse 3 times, remove free molecule, drying at room temperature is to be measured;
Compliance test result: S84 verifies substrate and the effect of TNT using the raman spectrum of Raman spectrometer control sample.
Preferably, PET film hydrophilic treated includes that PET film is cut into the pros of 2.0 × 2.0 cm in the step S1 Then shape is successively cleaned by ultrasonic surface with ethyl alcohol and deionized water, after 15 minutes, take out then with being dried with nitrogen, then put Enter to clean 3 minutes in plasma cleaner and make PET film surface hydrophilic, carries out plasma after waiting PET films to be dried at room temperature for Body cleans 3 minutes.
Preferably, the Raman spectrometer is the burnt drawing of Confocal laser-scanning microscopy instrument LabRAM HR Evolution type copolymerization Graceful spectrometer, it is 633nm that the parameter of spectrometer, which is set as excitation light source, and laser power is in 2.5 ~ 5mW, time of integration 10s, product Gradation number is 3 times.
Preferably, the model ME-3A of the reactive ion etching machine.
The invention has the benefit that
1. the present invention realizes quick, efficient, lossless decomposition, and operates without professional person, detection operating process is simple.
2. can achieve lower detection limit by the way of detecting indirectly.
Detailed description of the invention
Fig. 1 is TNT molecule connection schematic diagram.
Fig. 2 is that the SEM of flexible substrates schemes.
Fig. 3 is the raman spectrum for the R6G that flexible substrates measure.
Fig. 4 is the homogeneity and repeatability detection of flexible substrates.
Fig. 5 is TNT concentration gradient raman spectrum and its corresponding linear regression curves figure.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
Referring to Fig.1-5, the SERS substrate preparation based on nanosphere etching and its application in explosive TNT detection, packet Include following steps:
S1, the spin coating of single layer polystyrene microsphere in PET film: first to PET film hydrophilic treated, then by PS ball mother solution It is centrifuged and moves in the mixed solution containing ethyl alcohol and methanol that volume ratio is 2:1, and PS solution concentration is finally adjusted to 2.5 Surfactant TX-100 is added in final mixture by w/v% with 0.5 volume %, is then about 8 μ l by a drop volume PS solution be spin-coated on pure PET film, rotated 15 seconds at 650 rpm, then 1000 rpm spin coating 1 second, excessive to remove Film is kept for a few minutes in the heater so that solvent seasoning, obtains the PET film with single layer PS ball in this way by liquid;
Reactive ion etching: S2 the PET film with single layer PS ball is placed in the etch chamber of reactive ion etching machine and is carried out Etching, adjusting etch period are 5min, finally obtain the cyclic array containing nanocone on PET film surface, obtain the period Property nano-cone array film substrate;
S3, electron beam deposition gold nano grain: by the periodic nanometer cone array film substrate of acquisition in electron beam deposition system In gold-plated, the Raman substrate with a thickness of 30nm of finally obtained gold nanoparticle carried out with the rate of 0.02 ~ 0.03nm/s;
The modification of PET film substrate: S4 4- aminothiophenol is dissolved in ethanol solution for 10-5mol/L as 4- using concentration Then 4- aminothiophenol original solution is taken and a certain amount of ethyl alcohol is used to be diluted to 10- as solvent by aminothiophenol original solution 7mol/L, then will be gold-plated after Raman substrate be completely submerged in the 4- aminothiophenol solution of 10-7mol/L, impregnated under room temperature 10h is three times washed out the 4- aminothiophenol molecule being not connected in Raman substrate with deionized water continuous flushing after taking-up, 10s is rinsed every time, then at room temperature to dry;
S5, the synthesis of Nano silver grain: being that the 9mg/ml silver nitrate solution of 10ml is added in the deionized water of 490ml first, It is boiled in the case where magneton revolving speed is the rate of 550r/min, the sodium citrate that the mass fraction that 10ml is then slowly added dropwise is 1% is molten Liquid, solution continue to keep fluidized state 1h after becoming taupe;
The surface modification of Nano silver grain: S6 takes the 4- aminothiophenol solution of the 10-4mol/L of 100ul to be added to the silver of 900ul In glue, one hour is vibrated in an oscillator to achieve the effect that sufficiently adsorbing for 4- aminothiophenol molecule and Nano silver grain, 4- aminothiophenol molecule and Nano silver grain form the S-Ag key of strong interaction;
The connection of S7, TNT molecule: the Raman substrate in the 4- aminothiophenol solution for being immersed in 10-7mol/L is immersed in not With 10h in the TNT ethanol solution of concentration, take out at room temperature to dry;
S8, Raman detection.
In present embodiment, Raman detection in step S8 the following steps are included:
S81, substrate compliance test result: being configured to mother liquor for R6G molecular melting in ethanol, is then diluted to by ethyl alcohol different dense The prepare liquid of degree, it is gold-plated after Raman substrate be immersed in the R6G solution of various concentration its surface made to connect upper determinand molecule R6G verifies the Raman effect of prepared substrate by the Raman spectrum that Raman Measurement obtains;
The verifying of S82, TNT effect: three kinds of samples are detected respectively, first is that being immersed in 10-7mol/L4- aminothiophenol solution The Raman substrate of 10h is taken out second is that being immersed in the Raman substrate of 10h in 10-7mol/L 4- aminothiophenol solution and rinses 3 It is secondary, then it is immersed in 10h in the elargol of 4- aminothiophenol modification, it takes out and rinses, drying at room temperature is to be measured, third is that being immersed in 10- The Raman substrate of 10h in 7mol/L 4- aminothiophenol solution is taken out and is rinsed 3 times, then is immersed in the TNT solution of 10-5mol/L Middle 10h takes out wait do, is finally immersed in 10h in the elargol of 4- aminothiophenol modification, takes out and rinse 3 times, drying at room temperature waits for It surveys;
S83, TNT gradient concentration: being immersed in 10h in 10-7mol/L 4- aminothiophenol solution for Raman substrate, take out and rinse, It is separately immersed in 10h in the TNT solution of 10-8 ~ 10-13mol/L again, takes out wait do, is finally immersed in the modification of 4- aminothiophenol Elargol in 10h, take out rinse 3 times, remove free molecule, drying at room temperature is to be measured;
Compliance test result: S84 verifies substrate and the effect of TNT using the raman spectrum of Raman spectrometer control sample.
In present embodiment, PET film hydrophilic treated includes that PET film is being cut into 2.0 × 2.0 cm just in step S1 It is rectangular, then successively it is cleaned by ultrasonic surface with ethyl alcohol and deionized water, after 15 minutes, takes out then with being dried with nitrogen, then Be put into clean 3 minutes in plasma cleaner and make PET film surface hydrophilic, carried out after waiting PET films to be dried at room temperature for etc. from Daughter is cleaned 3 minutes.
In present embodiment, Raman spectrometer is that the copolymerization of Confocal laser-scanning microscopy instrument LabRAM HR Evolution type is burnt Raman spectrometer, it is 633nm that the parameter of spectrometer, which is set as excitation light source, laser power in 2.5 ~ 5mW, time of integration 10s, Integral number of times is 3 times.
In present embodiment, the model ME-3A of reactive ion etching machine.
In the present invention, the modification principle of Raman substrate are as follows: Jenner's grain of rice on 4- aminothiophenol molecule and Raman substrate Son forms the S-Au key of strong interaction, and the Raman spectrum of the Raman substrate of the 4- aminothiophenol modification of 10-7mol/L It is the characteristic peak that not can be measured 4- aminothiophenol, this is influential on not having when subsequent detection.The catenation principle of TNT molecule Are as follows: stronger π-π, which is formed, using TNT molecule and 4- aminothiophenol molecule is interacted namely the 4- ammonia of supplied for electronic by donor There is interaction as between ligand and the TNT phenyl ring of missing electronics in the amino of base benzenethiol molecule, this is also subsequent connection The basis of the Nano silver grain of 4- aminothiophenol molecular modification.
In the description of the present invention, it is to be understood that, term " center ", " longitudinal direction ", " transverse direction ", " length ", " width ", It is " thickness ", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outside", " suitable The orientation or positional relationship of the instructions such as hour hands ", " counterclockwise " is to be based on the orientation or positional relationship shown in the drawings, merely to just In description the present invention and simplify description, rather than the equipment of indication or suggestion meaning or element must have a particular orientation, with Specific orientation construction and operation, therefore be not considered as limiting the invention.
In addition, term " first ", " second " are used for description purposes only, it is not understood to indicate or imply relatively important Property or implicitly indicate the quantity of indicated technical characteristic.Define " first " as a result, the feature of " second " can be expressed or Person implicitly includes one or more of the features.In the description of the present invention, the meaning of " plurality " is two or two with On, unless otherwise specifically defined.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (5)

1. the SERS substrate preparation based on nanosphere etching and its application in explosive TNT detection, which is characterized in that including Following steps:
S1, the spin coating of single layer polystyrene microsphere in PET film: first to PET film hydrophilic treated, then by PS ball mother solution It is centrifuged and moves in the mixed solution containing ethyl alcohol and methanol that volume ratio is 2:1, and PS solution concentration is finally adjusted to 2.5 Surfactant TX-100 is added in final mixture by w/v% with 0.5 volume %, is then about 8 μ l by a drop volume PS solution be spin-coated on pure PET film, rotated 15 seconds at 650 rpm, then 1000 rpm spin coating 1 second, excessive to remove Film is kept for a few minutes in the heater so that solvent seasoning, obtains the PET film with single layer PS ball in this way by liquid;
Reactive ion etching: S2 the PET film with single layer PS ball is placed in the etch chamber of reactive ion etching machine and is carried out Etching, adjusting etch period are 5min, finally obtain the cyclic array containing nanocone on PET film surface, obtain the period Property nano-cone array film substrate;
S3, electron beam deposition gold nano grain: by the periodic nanometer cone array film substrate of acquisition in electron beam deposition system In gold-plated, the Raman substrate with a thickness of 30nm of finally obtained gold nanoparticle carried out with the rate of 0.02 ~ 0.03nm/s;
The modification of PET film substrate: S4 4- aminothiophenol is dissolved in ethanol solution for 10-5mol/L as 4- using concentration Then 4- aminothiophenol original solution is taken and a certain amount of ethyl alcohol is used to be diluted to 10- as solvent by aminothiophenol original solution 7mol/L, then will be gold-plated after Raman substrate be completely submerged in the 4- aminothiophenol solution of 10-7mol/L, impregnated under room temperature 10h is three times washed out the 4- aminothiophenol molecule being not connected in Raman substrate with deionized water continuous flushing after taking-up, 10s is rinsed every time, then at room temperature to dry;
S5, the synthesis of Nano silver grain: being that the 9mg/ml silver nitrate solution of 10ml is added in the deionized water of 490ml first, It is boiled in the case where magneton revolving speed is the rate of 550r/min, the sodium citrate that the mass fraction that 10ml is then slowly added dropwise is 1% is molten Liquid, solution continue to keep fluidized state 1h after becoming taupe;
The surface modification of Nano silver grain: S6 takes the 4- aminothiophenol solution of the 10-4mol/L of 100ul to be added to the silver of 900ul In glue, one hour is vibrated in an oscillator to achieve the effect that sufficiently adsorbing for 4- aminothiophenol molecule and Nano silver grain, 4- aminothiophenol molecule and Nano silver grain form the S-Ag key of strong interaction;
The connection of S7, TNT molecule: the Raman substrate in the 4- aminothiophenol solution for being immersed in 10-7mol/L is immersed in not With 10h in the TNT ethanol solution of concentration, take out at room temperature to dry;
S8, Raman detection.
2. the SERS substrate according to claim 1 based on nanosphere etching prepares and its in explosive TNT detection Using, which is characterized in that Raman detection in the step S8 the following steps are included:
S81, substrate compliance test result: being configured to mother liquor for R6G molecular melting in ethanol, is then diluted to by ethyl alcohol different dense The prepare liquid of degree, it is gold-plated after Raman substrate be immersed in the R6G solution of various concentration its surface made to connect upper determinand molecule R6G verifies the Raman effect of prepared substrate by the Raman spectrum that Raman Measurement obtains;
The verifying of S82, TNT effect: three kinds of samples are detected respectively, first is that being immersed in 10-7mol/L4- aminothiophenol solution The Raman substrate of 10h is taken out second is that being immersed in the Raman substrate of 10h in 10-7mol/L 4- aminothiophenol solution and rinses 3 It is secondary, then it is immersed in 10h in the elargol of 4- aminothiophenol modification, it takes out and rinses, drying at room temperature is to be measured, third is that being immersed in 10- The Raman substrate of 10h in 7mol/L 4- aminothiophenol solution is taken out and is rinsed 3 times, then is immersed in the TNT solution of 10-5mol/L Middle 10h takes out wait do, is finally immersed in 10h in the elargol of 4- aminothiophenol modification, takes out and rinse 3 times, drying at room temperature waits for It surveys;
S83, TNT gradient concentration: being immersed in 10h in 10-7mol/L 4- aminothiophenol solution for Raman substrate, take out and rinse, It is separately immersed in 10h in the TNT solution of 10-8 ~ 10-13mol/L again, takes out wait do, is finally immersed in the modification of 4- aminothiophenol Elargol in 10h, take out rinse 3 times, remove free molecule, drying at room temperature is to be measured;
Compliance test result: S84 verifies substrate and the effect of TNT using the raman spectrum of Raman spectrometer control sample.
3. the SERS substrate according to claim 2 based on nanosphere etching prepares and its in explosive TNT detection Using, which is characterized in that PET film hydrophilic treated includes that PET film is cut into the pros of 2.0 × 2.0 cm in the step S1 Then shape is successively cleaned by ultrasonic surface with ethyl alcohol and deionized water, after 15 minutes, take out then with being dried with nitrogen, then put Enter to clean 3 minutes in plasma cleaner and make PET film surface hydrophilic, carries out plasma after waiting PET films to be dried at room temperature for Body cleans 3 minutes.
4. the SERS substrate according to claim 2 or 3 based on nanosphere etching prepares and its in explosive TNT detection Application, which is characterized in that the Raman spectrometer is that the copolymerization of Confocal laser-scanning microscopy instrument LabRAM HR Evolution type is burnt Raman spectrometer, it is 633nm that the parameter of spectrometer, which is set as excitation light source, laser power in 2.5 ~ 5mW, time of integration 10s, Integral number of times is 3 times.
5. the SERS substrate according to any one of claims 1 to 3 based on nanosphere etching is prepared and its in explosive TNT Application in detection, which is characterized in that the model ME-3A of the reactive ion etching machine.
CN201910465736.9A 2019-05-30 2019-05-30 Preparation of SERS substrate based on nanosphere etching and application of SERS substrate in explosive TNT detection Expired - Fee Related CN110082341B (en)

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CN110726711A (en) * 2019-10-29 2020-01-24 江南大学 SERS substrate of metal-modified semiconductor-based bionic compound eye bowl structure and construction method
CN113295670A (en) * 2021-05-21 2021-08-24 合肥工业大学 Preparation method of micro-fluidic chip detection device based on SERS substrate
CN113702354A (en) * 2021-09-02 2021-11-26 电子科技大学 Flexible SERS substrate based on array type microstructure and preparation method thereof
CN114199854A (en) * 2021-12-15 2022-03-18 曲阜师范大学 Preparation method of SERS substrate constructed by flexible transparent cone ordered array
CN114354568A (en) * 2021-12-06 2022-04-15 西北大学 Surface-enhanced Raman spectrum substrate, preparation method and application

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