CN109001175A - A kind of preparation method of SERS substrate, SERS substrate and its application - Google Patents
A kind of preparation method of SERS substrate, SERS substrate and its application Download PDFInfo
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- CN109001175A CN109001175A CN201810574153.5A CN201810574153A CN109001175A CN 109001175 A CN109001175 A CN 109001175A CN 201810574153 A CN201810574153 A CN 201810574153A CN 109001175 A CN109001175 A CN 109001175A
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract
The invention discloses a kind of preparation methods of SERS substrate, comprising the following steps: (1) using the golden shell layer nanoparticle sol of method of fractional steps preparation package silica；(2) the golden shell layer nanoparticle sol that step (1) obtains is added drop-wise on miillpore filter, naturally dry obtains SERS substrate；Wherein the diameter of the golden shell layer nanoparticle is greater than the aperture of micropore in miillpore filter.The invention also discloses the application of the SERS substrate prepared by the above method and the substrate in the organic solution of Polychlorinated biphenyls and the trace detection of aqueous topical antibiotics.It is an advantage of the current invention that the preparation method of SERS substrate is simple, quick, stability is good, can increase substantially the signal strength of SERS detection.
Description
Technical field
The invention belongs to spectrum analysis detection fields, and in particular to a kind of preparation method of SERS substrate, SERS substrate and
It is applied.
Background technique
Polychlorinated biphenyls (PCB:Polychlorinated biphenyls) is a kind of persistent organic pollutants.On biphenyl
Hydrogen atom replaced by multiple chlorine atoms to get to Polychlorinated biphenyls, theoretically it shares 209 kinds of homologues, in actual production,
Typically result in the mixture of Polychlorinated biphenyls.Due to the unique physicochemical properties of Polychlorinated biphenyls, it can be used for multiple fields, such as
For the insulating oil in capacitor and transformer, the conduction oil in industrial production, lubricating oil in air compressor machine etc..Polychlorinated biphenyls by
It is artificial synthesized, after being widely used, enter empty gas and water by all means, in soil, and assemble in water body and soil.
However, extremely difficult be degraded of Polychlorinated biphenyls and it is long-term in the environment retain, there is long-distance migration, fat-soluble, bioconcentration, it is right
Organism generates toxic action, has carcinogenicity to human body, causes to nerve system of human body, endocrine system, cardiovascular system etc.
Negative effect.
Abuse of the antibiotic in medical treatment and livestock culture industry not only results in chemical contamination, it is also possible in meeting induced environment
The generation of resistant organisms and resistant gene, and accelerate the propagation and diffusion of antibiotic resistance.These resistant microorganisms can be by straight
It connects or the approach such as mediate contact enters human body, increase the drug resistance of human body, threaten to human health.The property of antibiotic is steady
It is fixed, there is certain persistence.Currently, detecting the presence of antibiotic in soil, surface water and underground water.
For the angle of environmental protection, Polychlorinated biphenyls, the antibiotic in environmental sample are carried out rapidly, conveniently, specifically
Property detection, have certain necessity and urgency.
Surface enhanced Raman spectroscopy (SERS:surface enhanced Raman spectroscopy) quick, nothing with it
The ability of damage and trace detection has received widespread attention.Substance is detected using SERS, needs to prepare suitable metal
Particle or its sol surface are as substrate, but Polychlorinated biphenyls and antibiotic are not easy to be adsorbed on metal surface, and detection effect is not
It is good；And existing substrate is modified, although can be improved the adsorption capacity of Polychlorinated biphenyls and antibiotic, its is complicated for operation,
It is with high costs, it is not suitable for being widely popularized；And existing substrate uses solvent to clean upon completion of the assays, the discharge of solvent again can be right
Environment generates pollution.
Summary of the invention
Technical problem to be solved by the present invention lies in: the existing side using SERS detection Polychlorinated biphenyls and antibiotic
Method, it is complicated for operation, with high costs, be unsuitable for being widely popularized and be suitable for.
The present invention solves above-mentioned technical problem using following technical scheme:
A kind of preparation method of SERS substrate, comprising the following steps:
(1) using the golden shell layer nanoparticle sol of method of fractional steps preparation package silica；
(2) the golden shell layer nanoparticle sol that step (1) obtains is added drop-wise on miillpore filter, naturally dry obtains SERS
Substrate；Wherein the diameter of the golden shell layer nanoparticle is greater than the aperture of micropore in miillpore filter.
Preferably, the preparation method of a kind of SERS substrate of the present invention, the middle preparation package titanium dioxide of the step (1)
The method of the golden shell layer Nano sol of silicon are as follows:
A, Nano particles of silicon dioxide suspension and gold nanoparticle colloidal sol are prepared；
B, to Nano particles of silicon dioxide surface modification coupling agent；
C, a certain amount of gold nanoparticle colloidal sol is taken, it is made to have the silicon dioxde reaction of coupling agent with surface modification, by Jenner
Rice corpuscles is connected to silica surface, obtains seed solution；
D, a certain amount of gold nanoparticle colloidal sol is taken, seed solution and reducing agent are added thereto, reaction is stood, in titanium dioxide
Silicon face grows golden shell layer, obtains the golden shell layer Nano sol of package silica.
Preferably, the preparation method of a kind of SERS substrate of the present invention, Nano particles of silicon dioxide described in A useMethod preparation.
Preferably, the preparation method of a kind of SERS substrate of the present invention, gold nanoparticle colloidal sol described in A it is specific
The preparation method is as follows:
A, aqueous solution of chloraurate is configured, 4 DEG C of preservations are protected from light, it is spare；
B, it takes ultrapure water to be placed in reactor, lye is added, reducing agent solution is added while stirring, add obtained
Aqueous solution of chloraurate, after mixing evenly, sealing are still aging；
C, carbonate solution is configured, carbonate solution is added in the aqueous solution of chloraurate being aged, it is stirring while adding, until molten
After liquid becomes colorless, sealing is kept in dark place, and makes its solation.
Preferably, the preparation method of a kind of SERS substrate of the present invention, coupling agent described in B are selected from 3- aminopropyl
Triethoxysilane, octadecyl siloxanes, aminoethylaminopropyl dimethyl silicone polymer.
Preferably, the preparation method of a kind of SERS substrate of the present invention, reducing agent described in D are formaldehyde or an oxidation
Carbon.
Preferably, the preparation method of a kind of SERS substrate of the present invention, reducing agent described in b be selected from sodium citrate,
Tetramethylol chloride or sodium borohydride.
The present invention provides a kind of SERS substrates, and the above method is used to be prepared.
The present invention also provides a kind of above-mentioned SERS substrates in Polychlorinated biphenyls organic solution or the trace of aqueous topical antibiotics
Application in amount detection, Polychlorinated biphenyls organic solution or aqueous topical antibiotics are added drop-wise in the SERS substrate, then used
Raman spectrometer carries out SERS detection.
Preferably, a kind of SERS substrate of the present invention is in Polychlorinated biphenyls organic solution or the trace of aqueous topical antibiotics
Application in detection, the Polychlorinated biphenyls organic solution include the hexane solution of Polychlorinated biphenyls or the dimethyl sulfoxide of Polychlorinated biphenyls
Solution；The antibiotic is tetracycline, Ciprofloxacin or Norfloxacin.
The technology of the present invention the utility model has the advantages that
The golden shell layer nanoparticle of technical solution of the present invention preparation package silica is core-shell structure, and size can basis
It needs to adjust within the scope of 200-500nm；There is spongiform porous structure, so that it is with biggish ratio inside miillpore filter
Surface area provides adsorption site abundant, is conducive to nanoparticle and testing molecule uniformly, in large quantities adsorbs, utilization is infrared
Wave band 785nm laser detects organic molecule, can increase substantially the signal-to-noise ratio of SERS spectra, reduces sample and measured
Fluorescence interference in journey；SERS substrate preparation process in the present invention is simple, quickly, and the substrate stability of acquisition is good, be not easy by
Oxidation, can save for a long time, and be able to maintain certain SERS enhancing ability, and when detection, substrate can be prepared at any time, convenient fast
It is prompt；
Since this substrate is prepared using organic miillpore filter, detection can directly concentrate destruction without using after completing
Solvent cleaning, avoids further polluting.
Detailed description of the invention
Fig. 1 is the TEM figure of the golden shell nanoparticle of the single package silica prepared in the embodiment of the present invention one；
The SERS spectra figure of the PCB-77 of various concentration is detected in Fig. 2 embodiment one；
Fig. 3 is 1595cm-1Place, the SERS intensity of the PCB-77 of various concentration with concentration variation relation figure；
Fig. 4 is the SERS spectra figure that the PCB-3 of various concentration is detected in embodiment two；
Fig. 5 is in 1446cm-1Place, the SERS intensity of the PCB-3 of various concentration with concentration variation relation figure；
Fig. 6 is the SERS spectra figure that the tetracycline of various concentration is detected in embodiment three；
Fig. 7 is in 1535cm-1Place, the SERS intensity of the tetracycline of various concentration with concentration variation relation figure.
Specific embodiment
For convenient for those skilled in the art understand that technical solution of the present invention, now in conjunction with Figure of description to the technology of the present invention side
Case is described further.
Embodiment one
Present embodiment discloses the preparation methods for preparing SERS substrate, the specific steps of which are as follows:
(1) nano SiO 2 particle and gold nanoparticle are prepared
The nano SiO 2 particle usesMethod synthesis, synthetic method reference literature Stober W, Fink
A,Bohn E.Controlled growth of monodisperse silica spheres in the micron size
range[J].Journal of colloid and interface science,1968,26(1):62-69.In the present embodiment
By adjusting synthesis condition, the Nano particles of silicon dioxide having a size of 180nm is obtained.
The preparation process of the gold nanoparticle is as follows: gold chloride powder a, being dissolved in ultrapure water to obtain gold chloride water-soluble
The aqueous solution, is protected from light standing at least 10 days by liquid under the conditions of 4 DEG C；B, it takes ultrapure water to be placed in conical flask, is added thereto
NaOH solution, then tetramethylol chloride is added under conditions of being vigorously stirred, step a is then added into conical flask again and is made
Aqueous solution of chloraurate, after mixing evenly, sealing, still aging one month；C, solution of potassium carbonate is configured, by the chlorine being aged gold
Aqueous acid is added in solution of potassium carbonate, stirring while adding, until being kept in dark place after solution becomes colorless, makes its solation i.e.
It can.
In the preparation process of gold nanoparticle, the NaOH solution in the step b can also use other alkaline solutions
Instead of, such as KOH；The tetramethylol chloride plays the role of reducing agent, can also use sodium citrate, sodium borohydride
Equal reducing substances replace；Other carbonate solutions also can be used in solution of potassium carbonate in step c.In addition, in step b
The still aging time is at least two weeks, and generally within four months, the effect of ageing one month is best.
(2) in Nano particles of silicon dioxide surface modification coupling agent
The Nano particles of silicon dioxide for taking step (1) to obtain is dissolved in dehydrated alcohol, and ultrasonic disperse obtains suspension；It takes
Coupling agent is added thereto, at the uniform velocity stirs in reactor for the suspension, stays overnight, then heating water bath, this is continuous in the process
Ethyl alcohol is added to maintain volume stability.After reaction, it is washed with dehydrated alcohol, finally product is dissolved in dehydrated alcohol, it is standby
With.
Purpose of heating water bath is to improve coupling agent in the joint efficiency of silica surface during this.
There are many selections for the coupling agent, such as 3- aminopropyl triethoxysilane, octadecyl siloxanes, aminoethyl ammonia
Propyl dimethyl silicone polymer, the present embodiment select 3- aminopropyl triethoxysilane.
(3) gold nanoparticle is connected to silica surface, obtains seed solution
The gold nanoparticle colloidal sol for taking step (1) to obtain, under ultrasonic state, NaCl and surface modification are added thereto to be had
The silicon dioxde solution of coupling agent, at the uniform velocity fully reacting under stirring condition after centrifuge washing, then use milli-Q water, finally
Product is dissolved in ultrapure water and obtains seed solution.
(4) seed solution and reducing agent is added in the gold nanoparticle colloidal sol for taking a certain amount of step (1) to obtain thereto, quiet
Set reaction.First centrifuge washing after reaction, then with milli-Q water to get to the golden shell layer nanometer for wrapping up silica
Grain, having a size of 200nm.Fig. 1 gives the TEM figure of single golden shell nanoparticle.
Formalin or CO gas can be used in reducing agent described in step (4).
(5) the golden shell nanoparticle that step (4) obtains is dispersed in the golden shell that package silica is obtained in ultrapure water
Layer nanoparticle sol；The colloidal sol is added drop-wise on the miillpore filter that aperture is 0.2um again, naturally dry obtains SERS substrate.
Miillpore filter described in step (5) can by nylon material, mixed cellulose ester, polytetrafluoroethylene (PTFE), gather inclined fluorine
The various materials such as ethylene or polypropylene are made, as long as it guarantees that the micropore size in miillpore filter is less than the golden shell layer nanoparticle
The diameter of son.
According to actual needs, when preparing SERS substrate, miillpore filter is cut in square sheets of uniform size, size
For 0.5cm × 0.5cm.
By the SERS substrate of above-mentioned preparation applied in the detection of PCB-77.
Compound concentration is 10-3The hexane solution of the PCB-77 of M takes a SERS substrate prepared, will be prepared molten
Drop is added in the substrate, then carries out SERS detection using Raman spectrometer.
It similarly, is respectively respectively 5 × 10 to concentration-4M、10-4M、5×10-5M、10-5The PCB-77 hexane solution of M, point
SERS detection is not carried out using Raman spectrometer.
The SERS spectra figure of the PCB-77 of various concentration as shown in Figure 2；By analyzing its Characteristic Raman peak 1595cm-1's
Peak intensity, obtains PCB-77 Raman signal with the response signal of concentration, as shown in Figure 3 in 1595cm-1Place, the PCB- of various concentration
77 SERS intensity with concentration variation relation figure.It follows that the concentration of PCB-77 is bigger, in 1595cm-1The SERS at place
Intensity is bigger, to realize the trace detection analysis to PCB-77.
Miillpore filter inside spongy porous structure abundant provides largely for nanoparticle and PCB-77 to be measured
Adsorption site, and the aperture of micropore is less than the diameter of golden shell nanoparticle, so that golden shell nanoparticle is trapped in filter by it
Film surface, after PCB-77 drop is added dropwise, drop is spread rapidly, is equably adsorbed on substrate surface, at this point, metal surface and to
It surveys particle and is distributed in substrate surface, be conducive to significantly enhance SERS signal.This method preparation process is simple, quick, steady
It is qualitative good.When being detected, substrate can be prepared at any time, it is only necessary to be got out sample, can be carried out by simple step
It tests and analyzes.
Embodiment two
The preparation method of SERS substrate is basically the same as the first embodiment in the present embodiment, only by control experiment condition, is obtained
The size of the golden shell nanoparticle of the package silica obtained is 520nm, and wherein the size of Nano particles of silicon dioxide is
500nm。
The SERS substrate that the present embodiment obtains is used for the detection of the dimethyl sulfoxide solution of PCB-3, operating procedure and implementation
It is identical in example one.The experimental result of the present embodiment is as shown in Figures 4 and 5, and wherein Fig. 4 is the PCB- of various concentration in the present embodiment
3 SERS spectra figure；Fig. 5 is in 1446cm-1Place, the SERS intensity of the PCB-3 of various concentration with concentration variation relation figure.
It is detected, is detected it should be noted that other homologues of Polychlorinated biphenyls also can use the SERS substrate
As a result close with embodiment one, embodiment two, due to length, details are not described herein again.
Embodiment three
The preparation method of SERS substrate is basically the same as the first embodiment in the present embodiment, only by control experiment condition, is obtained
The size of the golden shell nanoparticle of the package silica obtained is 310nm, and wherein the size of Nano particles of silicon dioxide is
300nm。
SERS substrate made from the present embodiment is used for the SERS detection of tetracycline aqueous solution, operating procedure and embodiment
One is identical, and experimental result is shown in Fig. 6 and Fig. 7, and wherein Fig. 6 is the SERS spectra that the tetracycline of various concentration is detected in the present embodiment
Figure；Fig. 7 is in 1535cm-1Place, the SERS intensity of the tetracycline of various concentration with concentration variation relation figure.
It should be noted which progress can also be used in the aqueous solution of other antibiotic such as Ciprofloxacin, Norfloxacin
SERS detection, testing result are close with the testing result of tetracycline.
Except the detection of PCB-77, PCB-3 and tetracycline for being itemized in above-described embodiment, for different Polychlorinated biphenyls
Homologue and other antibiotic, required golden shell layer nano-particles size select as needed, wherein the thickness of golden shell layer
It is selected within the scope of 5-20nm as needed, and obtained by regulating and controlling specific preparation condition.
In addition, above-described embodiment one, into three kinds of SERS substrate preparation process of embodiment, required reagent, reaction condition etc. have
Body parameter is regulated and controled as needed, has no direct relation with improvement of the present invention, thus not narration in detail.
Technical solution of the present invention is exemplarily described invention above in conjunction with attached drawing, it is clear that present invention specific implementation
It is not subject to the restrictions described above, changes as long as using the various unsubstantialities that the inventive concept and technical scheme of the present invention carry out
Into, or it is not improved the conception and technical scheme of invention are directly applied into other occasions, in protection scope of the present invention
Within.
Claims (10)
1. a kind of preparation method of SERS substrate, which comprises the following steps:
(1) using the golden shell layer nanoparticle sol of method of fractional steps preparation package silica；
(2) the golden shell layer nanoparticle sol that step (1) obtains is added drop-wise on miillpore filter, naturally dry obtains SERS base
Bottom；Wherein the diameter of the golden shell layer nanoparticle is greater than the aperture of micropore in miillpore filter.
2. a kind of preparation method of SERS substrate according to claim 1, which is characterized in that preparation in the step (1)
The method for wrapping up the golden shell layer Nano sol of silica is as follows:
A, Nano particles of silicon dioxide suspension and gold nanoparticle colloidal sol are prepared；
B, in Nano particles of silicon dioxide surface modification coupling agent；
C, a certain amount of gold nanoparticle colloidal sol is taken, it is made to have the silica of coupling agent anti-with surface modification under ultrasonic state
It answers, gold nanoparticle is connected to silica surface, obtains seed solution；
D, a certain amount of gold nanoparticle colloidal sol is taken, seed solution and reducing agent are added thereto, reaction is stood, in silicon dioxide meter
It looks unfamiliar and grows golden shell layer, obtain the golden shell layer Nano sol of package silica.
3. a kind of preparation method of SERS substrate according to claim 2, which is characterized in that silica described in A is received
Rice corpuscles usesMethod preparation.
4. a kind of preparation method of SERS substrate according to claim 2, which is characterized in that gold nanoparticle described in A
Colloidal sol specific the preparation method is as follows:
A, aqueous solution of chloraurate is configured, 4 DEG C of preservations are protected from light, it is spare；
B, it takes ultrapure water to be placed in reactor, lye is added, reducing agent solution is added while stirring, add chlorine gold obtained
Aqueous acid, after mixing evenly, sealing are still aging；
C, carbonate solution is configured, carbonate solution is added in the aqueous solution of chloraurate being aged, it is stirring while adding, until solution becomes
After colourless, sealing is kept in dark place, and makes its solation.
5. a kind of preparation method of SERS substrate according to claim 2, which is characterized in that the choosing of coupling agent described in B
From 3- aminopropyl triethoxysilane, octadecyl siloxanes, aminoethylaminopropyl dimethyl silicone polymer.
6. a kind of preparation method of SERS substrate according to claim 2, which is characterized in that reducing agent described in D is first
Aldehyde or carbon monoxide.
7. a kind of preparation method of SERS substrate according to claim 4, which is characterized in that reducing agent described in b is selected from
Sodium citrate, tetramethylol chloride or sodium borohydride.
8. a kind of SERS substrate uses claim 1-7 the method to be such as prepared.
9. a kind of SERS substrate as claimed in claim 8 is in Polychlorinated biphenyls organic solution or the trace detection of aqueous topical antibiotics
In application, which is characterized in that Polychlorinated biphenyls organic solution or aqueous topical antibiotics are added drop-wise in the SERS substrate, then
SERS detection is carried out using Raman spectrometer.
10. a kind of SERS substrate according to claim 9 is in Polychlorinated biphenyls organic solution or the trace of aqueous topical antibiotics
Application in detection, which is characterized in that the Polychlorinated biphenyls organic solution includes the hexane solution or more chlorine connection of Polychlorinated biphenyls
The dimethyl sulfoxide solution of benzene；The antibiotic is tetracycline, Ciprofloxacin or Norfloxacin.
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| CN111380857A (en) * | 2018-12-29 | 2020-07-07 | 同方威视技术股份有限公司 | Method for detecting ciprofloxacin in milk |
| CN112540072A (en) * | 2020-11-20 | 2021-03-23 | 江苏大学 | Preparation method of surface-enhanced Raman spectrum substrate material for detecting xanthoxylin in hotpot condiment |
| CN113834804A (en) * | 2021-09-23 | 2021-12-24 | 中国农业大学 | Construction method and application of flexible surface enhanced Raman substrate |
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| CN113834804A (en) * | 2021-09-23 | 2021-12-24 | 中国农业大学 | Construction method and application of flexible surface enhanced Raman substrate |
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