CN107589106A - A kind of method for preparing surface enhanced Raman scattering substrate - Google Patents
A kind of method for preparing surface enhanced Raman scattering substrate Download PDFInfo
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Abstract
The embodiment of the invention discloses a kind of method for preparing surface enhanced Raman scattering substrate, including：Silica aerogel powder is added in the beaker for fill deionized water, and the aerosil aqueous solution is obtained by magnetic stirrer；The aerosil aqueous solution is transferred in single-necked flask, and silver nitrate solution is added in the single-necked flask, boiling is stirred and heated to by magnetic force warm table；Sodium citrate solution is added in the solution after boiling simultaneously continuous heating preset time；Centrifuge tube is poured into after residue in the single-necked flask is cooled into room temperature, with deionized water eccentric cleaning, obtains the sediment of centrifuge tube lower floor；The sediment is added drop-wise on wave carrier piece, after liquid natural evaporation, obtains the silica aerogel powder of the modified by silver nanoparticles as surface enhanced Raman scattering substrate.Using the silica aerogel powder of the modified by silver nanoparticles, realizing the high of SERS detections strengthens and repeatability.
Description
Technical field
The present invention relates to Raman spectrum detection technique field, and surface enhanced Raman scattering substrate is prepared more particularly to one kind
Method.
Background technology
Raman scattering phenomenon is experimentally observed by India physicist Raman (Raman) earliest, is light irradiation
The inelastic scattering phenomenon occurred when on to atom or molecule, that is, scatter and occur the light different from incident light frequency in light.Raman
Spectrum carries " fingerprint " information of material, and the internal structure for research crystal and molecule provides an effective means, because
This Raman spectroscopy is widely used in material detection.
However, generally the raman scattering cross section very little of molecule, only substantial amounts of molecule could contribute measurable Raman signal,
This causes it to have significant limitation as a kind of spectrum detection technique.In the 1970s, SERS
The discovery of (Surface-Enhanced Raman Scattering, SERS) causes the extensive concern and interest of people.SERS
Intensity can be scattered relative to normal Raman and produce several or even more than ten of order of magnitude enhancings, have higher detection sensitive
Degree.Therefore, SERS is widely used to the fields such as material science, surface chemistry, biomedicine.
SERS high enhancement effect mostlys come from local Electromagnetic enhancement.Metal Nano structure is under the exciting of incident light
Surface plasma body resonant vibration behavior can be produced, huge local electric field is produced near metal Nano structure, so that
The Raman scattering of molecule in the electric field is enhanced, and this metal Nano structure is referred to as " focus ".
Hotspot density that existing SERS substrates provide is low, stability is poor, it is difficult to obtains highly sensitive with repeated SERS
Detection.
The content of the invention
The method of surface enhanced Raman scattering substrate is prepared it is an object of the invention to provide a kind of, while realizes that surface increases
The high enhancing of strong Raman scattering detection and repeatability.
To achieve the above object, the present invention provides a kind of method for preparing surface enhanced Raman scattering substrate, including：
Silica aerogel powder is added in the beaker for fill deionized water, and is obtained by magnetic stirrer
The aerosil aqueous solution；
The aerosil aqueous solution is transferred in single-necked flask, and nitric acid is added in the single-necked flask
Silver-colored solution, boiling is stirred and heated to by magnetic force warm table；
Sodium citrate solution is added in the solution after boiling simultaneously continuous heating preset time；
Centrifuge tube is poured into after residue in the single-necked flask is cooled into room temperature, with deionized water eccentric cleaning, is obtained
To the sediment of centrifuge tube lower floor；
The sediment is added drop-wise on wave carrier piece, after liquid natural evaporation, acquisition is used as SERS
The silica aerogel powder of the modified by silver nanoparticles of substrate.
Preferably, the particle diameter of the silica aerogel powder is 5-20 μm.
Preferably, silica aerogel powder is added in the beaker for fill deionized water includes：According to 1ml deionizations
The ratio that silica aerogel powder described in 1-2mg is added in water adds described two in the beaker for filling deionized water
Silica aerogel powder.
Preferably, the silver nitrate solution that added in the single-necked flask includes：Added in the single-necked flask
10mL concentration is 0.0294-0.0412mol/L silver nitrate solution.
Preferably, the solution that sodium citrate solution is added to after boiling includes：It is 0.0051- by 10ml concentration
0.0085mol/L sodium citrate solution is added in the solution after boiling.
It is preferably, described that sodium citrate solution is added in the solution after boiling and after continuous heating preset time,
Residue in the single-necked flask is cooled to before pouring into centrifuge tube after room temperature, in addition to：Stopping heating stops solution
Seethe with excitement 5-10 minutes, then continuing heating makes solution constantly boiling 20-30 minutes.
Compared with prior art, the present invention at least tool has the advantage that：
The silica aerogel powder for obtaining modified by silver nanoparticles is used as surface enhanced Raman scattering substrate, passes through
Using aerosil as carrier, more silver nano-grain is loaded using its special structural advantage, is produced highly dense
Degree, stability high " focus ", so as to realize the highly sensitive and repeated detection of SERS detections.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of the method provided in an embodiment of the present invention for preparing surface enhanced Raman scattering substrate.
Fig. 2 is that the flow of the method for preparing surface enhanced Raman scattering substrate provided according to an example of the invention is illustrated
Figure.
Fig. 3 (a) and Fig. 3 (b) is that the electronic scanner microscope for the SERS substrates being prepared according to embodiments of the present invention regards
Figure.
Fig. 3 (c) and Fig. 3 (d) is that the SERS substrates progress SERS being prepared according to embodiments of the present invention strengthens what is obtained
SERS spectra view.
Embodiment
In the accompanying drawings, represent same or similar element using same or similar label or there is same or like function
Element.Embodiments of the invention are described in detail below in conjunction with the accompanying drawings.
In the description of the invention, term " " center ", " longitudinal direction ", " transverse direction ", "front", "rear", "left", "right", " vertical ",
The orientation or position relationship of the instruction such as " level ", " top ", " bottom " " interior ", " outer " are to be closed based on orientation shown in the drawings or position
System, it is for only for ease of and describes the present invention and simplify description, rather than indicates or imply that signified device or element must have
Specific orientation, with specific azimuth configuration and operation, therefore it is not intended that limiting the scope of the invention.
In the case where not conflicting, the technical characteristic in various embodiments of the present invention and each embodiment can be mutually combined,
It is not limited in the embodiment or embodiment where the technical characteristic.
The embodiment of the present invention provides a kind of method for preparing surface enhanced Raman scattering substrate, as shown in figure 1, including：
Step 101, silica aerogel powder is added in the beaker for fill deionized water, and passes through magnetic stirring apparatus
Stirring obtains the aerosil aqueous solution.
Step 102, the aerosil aqueous solution is transferred in single-necked flask, and in the single-necked flask
Silver nitrate solution is added, boiling is stirred and heated to by magnetic force warm table.
Step 103, sodium citrate solution is added in the solution after boiling simultaneously continuous heating preset time.
Step 104, centrifuge tube is poured into after the residue in the single-necked flask being cooled into room temperature, is centrifuged with deionized water
Cleaning, obtains the sediment of centrifuge tube lower floor.
Step 105, the sediment is added drop-wise on wave carrier piece, after liquid natural evaporation, acquisition is used as surface enhanced
The silica aerogel powder of the modified by silver nanoparticles of Raman scattering substrate.
In one embodiment, the particle diameter of the silica aerogel powder is 5-20 μm, is optimal with 15 μm.
In one embodiment, silica aerogel powder is added in the beaker for fill deionized water includes：Press
According in 1ml deionized waters add 1-2mg described in silica aerogel powder ratio in the beaker for filling deionized water
It is middle to add the silica aerogel powder.10ml is filled for example, 10-20 ㎎ silica aerogel powders are added to
In the beaker of ionized water.
In one embodiment, silver nitrate solution is added in the single-necked flask includes：In the single-necked flask
Add the silver nitrate solution that 10mL concentration is 0.0294-0.0412mol/L.
In one embodiment, the solution that sodium citrate solution is added to after boiling includes：10ml is dense
The sodium citrate solution spent for 0.0051-0.0085mol/L is added in the solution after boiling.Wherein, with 0.0353mol/l's
Sodium citrate solution is optimal.
In one embodiment, it is described by sodium citrate solution be added to boiling after solution in and continuous heating preset
After time, the residue in the single-necked flask is cooled to before pouring into centrifuge tube after room temperature, in addition to：Stopping heating makes
Solution stops boiling 5-10 minutes, and then continuing heating makes solution constantly boiling 20-30 minutes.
An instantiation is provided below.It is readily appreciated that, the example is merely to be better described preparation provided by the invention
The method of surface enhanced Raman scattering substrate, it is not used to be particularly limited to the scope of the present invention.
As shown in Fig. 2 the method for preparing surface enhanced Raman scattering substrate that the example provides includes：
Step 201, the silica aerogel powder of about 5-20 μm of 10-20 ㎎ particle diameters is added to and fills 10ml deionizations
In the beaker of water, after magnetic stirrer about 10-20 minutes.
Wherein, the rotating speed of magnetic stirring apparatus is 900 revs/min.
Step 202, the solution after stirring is transferred in single-necked flask, is 0.0294-0.0412mol/l by 10ml concentration
Silver nitrate solution is added in the aerosil aqueous solution, and boiling is stirred and heated to by magnetic force warm table.During boiling
Temperature be maintained at 100-120 DEG C, be optimal with 110 DEG C.
Step 203, by sodium citrate solution that 10ml concentration is 0.0051-0.0085mol/l, to be added to above-mentioned boiling molten
In liquid, continuous heating about 20-30 minutes, 100-120 DEG C is maintained the temperature at, be optimal with 110 DEG C.
Step 204, reactant remaining after heating is cooled to room temperature and pours into centrifuge tube, centrifuged with deionized water clear
Wash, the sediment of centrifuge tube lower floor is added drop-wise on sheet glass, after liquid natural evaporation, obtain the two of modified by silver nanoparticles
Silica aerogel powder, i.e. SERS substrates.
In order to illustrate the silica airsetting of SERS substrates, i.e. modified by silver nanoparticles that the embodiment of the present invention is prepared
The SERS Detection results at rubber powder end, the modified by silver nanoparticles that the method provided examples detailed above is prepared is provided separately below
Silica aerogel powder electronic scanner microscope (SEM) Fig. 3 (a) and Fig. 3 (b), to rhodamine (R6G) molecule
SERS detection spectrograms 3 (c) and the SERS detection spectrograms 3 (d) to 5 FU 5 fluorouracil.Wherein, Fig. 3 (b) is empty in Fig. 3 (a)
View after the amplification of inframe sample.
When carrying out SERS detections, the solution of thing to be detected is configured first, by what is for example prepared according to examples detailed above method
The silica aerogel powder of modified by silver nanoparticles is poured into the solution of thing to be detected and is sufficiently mixed, by a small amount of mixed solution
Drip to for example on slide, after solution to be mixed is dried, carry out SERS spectra detection.
R6G concentration is respectively 10 in Fig. 3 (c)-10、10-13The concentration of 5 FU 5 fluorouracil is respectively 10 in M, Fig. 3 (d)-10、
10-13M。
As can be seen that dense distribution a large amount of silver nanoparticles on silica aerogel powder from Fig. 3 (a) and 3 (b)
Grain, its shape meet the condition to form focus.Fig. 3 (c) is Raman shift with abscissa X in 3 (d), and unit is cm-1, ordinate Y
Intensity is represented, unit is a.u. (Arbitrary Unit).
As can be seen that the silica aerogel powder of modified by silver nanoparticles is dense for two kinds from Fig. 3 (c) and 3 (d)
Two kinds of molecules of degree have extraordinary enhancing effect.
It is last it is to be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations.This
The those of ordinary skill in field should be understood：Technical scheme described in foregoing embodiments can be modified, or it is right
Which part technical characteristic carries out equivalent substitution；These modifications are replaced, and the essence of appropriate technical solution is departed from this
Invent the spirit and scope of each embodiment technical scheme.
Claims (6)
- A kind of 1. method for preparing surface enhanced Raman scattering substrate, it is characterised in that including：Silica aerogel powder is added in the beaker for fill deionized water, and dioxy is obtained by magnetic stirrer SiClx airsetting glue solution；The aerosil aqueous solution is transferred in single-necked flask, and addition silver nitrate is molten in the single-necked flask Liquid, boiling is stirred and heated to by magnetic force warm table；Sodium citrate solution is added in the solution after boiling simultaneously continuous heating preset time；Pour into centrifuge tube after residue in the single-necked flask is cooled into room temperature, with deionized water eccentric cleaning, obtain from The sediment of Xin Guan lower floors；The sediment is added drop-wise on wave carrier piece, after liquid natural evaporation, acquisition is used as surface enhanced Raman scattering substrate Modified by silver nanoparticles silica aerogel powder.
- 2. the method as described in claim 1, it is characterised in that the particle diameter of the silica aerogel powder is 5-20 μm.
- 3. method as claimed in claim 2, it is characterised in that silica airsetting is added in the beaker for fill deionized water Rubber powder end includes：Ratio according to silica aerogel powder described in 1-2mg is added in 1ml deionized waters fills deionized water described Beaker in add the silica aerogel powder.
- 4. the method as described in claim 1, it is characterised in that described that silver nitrate solution bag is added in the single-necked flask Include：The silver nitrate solution that 10mL concentration is 0.0294-0.0412mol/L is added in the single-necked flask.
- 5. method as claimed in claim 4, it is characterised in that described that sodium citrate solution is added in the solution after boiling Including：The sodium citrate solution that 10ml concentration is 0.0051-0.0085mol/L is added in the solution after boiling.
- 6. the method as described in claim 1, it is characterised in that described that sodium citrate solution is added in the solution after boiling And after continuous heating preset time, the residue in the single-necked flask is cooled to before pouring into centrifuge tube after room temperature, also Including：Stopping heating makes solution stop boiling 5-10 minutes, and then continuing heating makes solution constantly boiling 20-30 minutes.
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| CN113552114A (en) * | 2021-08-09 | 2021-10-26 | 首都师范大学 | Preparation method and detection method of surface-enhanced Raman scattering substrate |
| CN114280029A (en) * | 2022-01-04 | 2022-04-05 | 朱媛媛 | Method for detecting western medicine components in Chinese patent medicine |
| CN116297389A (en) * | 2023-02-15 | 2023-06-23 | 中国人民解放军空军特色医学中心 | Drug detection method capable of causing driving operation disability in biological sample at accident site |
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