CN113552114A - Preparation method and detection method of surface-enhanced Raman scattering substrate - Google Patents
Preparation method and detection method of surface-enhanced Raman scattering substrate Download PDFInfo
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- CN113552114A CN113552114A CN202110907272.XA CN202110907272A CN113552114A CN 113552114 A CN113552114 A CN 113552114A CN 202110907272 A CN202110907272 A CN 202110907272A CN 113552114 A CN113552114 A CN 113552114A
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- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 title claims abstract description 62
- 239000000758 substrate Substances 0.000 title claims abstract description 32
- 238000001514 detection method Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 73
- 239000000243 solution Substances 0.000 claims abstract description 54
- 239000000843 powder Substances 0.000 claims abstract description 42
- 239000002245 particle Substances 0.000 claims abstract description 25
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 229910052709 silver Inorganic materials 0.000 claims abstract description 16
- 239000004332 silver Substances 0.000 claims abstract description 16
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002105 nanoparticle Substances 0.000 claims abstract description 15
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 15
- 239000001509 sodium citrate Substances 0.000 claims abstract description 15
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 12
- 238000009835 boiling Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000011521 glass Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 239000011148 porous material Substances 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000001704 evaporation Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 28
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 13
- 238000001228 spectrum Methods 0.000 claims description 12
- 230000000694 effects Effects 0.000 claims description 11
- 239000005909 Kieselgur Substances 0.000 claims description 5
- 238000001069 Raman spectroscopy Methods 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 238000004621 scanning probe microscopy Methods 0.000 description 1
- -1 silver nanoparticle-modified diatomaceous earth Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
- 238000000479 surface-enhanced Raman spectrum Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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- Health & Medical Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The embodiment of the invention discloses a preparation method and a detection method of a surface-enhanced Raman scattering substrate, wherein the preparation method comprises the following steps: grinding diatomite to obtain diatomite particles, wherein the diatomite particles comprise sheet structures which fall off from the three-dimensional pore structures of the diatomite powder after grinding; adding the diatomite particles into a beaker filled with deionized water, and stirring and ultrasonically treating to obtain a diatomite aqueous solution; transferring the diatomite aqueous solution into a flask, adding a silver nitrate solution into the flask, and heating and stirring until the mixture is boiled; adding a sodium citrate solution into the boiling solution and continuously heating the solution for a preset time; cooling the remainder in the flask to room temperature, pouring the remainder into a centrifuge tube, and centrifugally cleaning the remainder with deionized water to obtain a precipitate at the lower end of the centrifuge tube; and dropping the precipitate onto a glass slide, and naturally evaporating the liquid to obtain the silver nanoparticle modified diatomite powder serving as the surface-enhanced Raman scattering substrate.
Description
Technical Field
The invention relates to the technical field of Raman spectrum detection, in particular to a preparation method and a detection method of a surface enhanced Raman scattering substrate.
Background
Surface-Enhanced Raman Scattering (SERS) is a Surface-Enhanced effect spectrum of local field enhancement caused by Surface plasmons, and is widely used in the fields of analytical chemistry, Surface science, electrochemistry, material research, and the like due to its simple and rapid analysis capability. The high enhancement effect of SERS mainly results from the enhancement of a local electromagnetic field, when incident light irradiates the surface of a metal nanostructure, the metal nanostructure generates surface plasmon resonance, and generates a huge local electric field near the metal nanostructure, which greatly enhances the raman scattering signal of a detected molecule in the local electric field, and the metal nanostructure is called a "hot spot".
However, the SERS substrate of the prior art has low stability and sensitivity, which is difficult to meet the requirements of special applications such as trace detection.
Disclosure of Invention
The present invention is directed to a method for preparing a surface-enhanced raman scattering substrate and a method for detecting the same, which solve at least one of the above problems of the prior art.
In order to achieve the above object, the present invention provides a method for preparing a surface-enhanced raman scattering substrate, comprising:
grinding the diatomite to obtain diatomite particles with the particle size of 5-20 microns, wherein the diatomite particles comprise sheet structures which fall off from a three-dimensional pore structure of the diatomite after grinding;
adding the diatomite particles into a beaker filled with deionized water, and respectively stirring and ultrasonically treating the mixture by a magnetic stirrer and an ultrasonic cleaner to obtain a diatomite aqueous solution;
transferring the diatomite aqueous solution into a flask, adding a silver nitrate solution into the flask, and heating and stirring until the mixture is boiled;
adding a sodium citrate solution into the boiled solution and continuously heating the solution for a preset time;
cooling the remainder in the flask to room temperature, pouring the remainder into a centrifuge tube, and centrifugally cleaning the remainder with deionized water to obtain a precipitate at the lower end of the centrifuge tube;
and dropping the precipitate onto a glass slide, and naturally evaporating the liquid to obtain the silver nanoparticle modified diatomite powder serving as the surface-enhanced Raman scattering substrate.
Preferably, the silver nanoparticle modified diatomite powder used as the surface enhanced raman scattering substrate is used for generating the concentration of 10-16And (3) surface enhanced Raman scattering spectrum of the object to be detected in mol/L.
Preferably, the silver nanoparticle-modified diatomaceous earth powder has similar surface raman enhancement effects at various positions.
Preferably, the particle size of the diatomite powder is 10 μm.
Preferably, the adding of the diatomite powder into the beaker with the deionized water comprises: and adding 1-2mg of the diatomite powder into the centrifugal tube containing the deionized water according to the proportion of adding 1mL of the deionized water into the deionized water.
Preferably, the adding of the silver nitrate solution to the flask comprises: 1mL of silver nitrate solution with a concentration of 0.005-0.01mol/L was added to the flask.
Preferably, the adding the sodium citrate solution into the boiled solution comprises: 1mL of a sodium citrate solution with a concentration of 0.03-0.05mol/L was added to the boiled solution.
Preferably, after the sodium citrate solution is added into the boiled solution and is continuously heated for a preset time, before the residue in the three-neck flask is cooled to room temperature and poured into a centrifuge tube, the method further comprises the following steps: the solution was stopped from boiling for 1-2 minutes by discontinuing heating, and then continued to boil for 3-4 minutes by continuing heating.
The invention provides a method for carrying out surface enhanced Raman scattering detection, which comprises the following steps: detecting a sample by using the diatomite powder modified by the silver nanoparticles prepared by the method as a surface-enhanced Raman scattering substrate to obtain a surface-enhanced Raman scattering spectrum of the sample at a preset concentration; the preset concentration comprises 10-16mol/L; performing surface enhanced Raman scattering detection on the object to be detected, comparing the detected object with the surface enhanced Raman scattering spectrum of the sample, and determining the object to be detectedAnd (3) components.
Compared with the prior art, the invention has at least the following advantages:
the method comprises the following steps of grinding diatomite to obtain diatomite particles with the particle size of 5-20 micrometers, wherein the diatomite particles comprise sheet structures falling off from three-dimensional pore structures of the diatomite powder, the diatomite powder modified by silver nanoparticles serving as a surface-enhanced Raman scattering substrate is obtained based on the diatomite particles, the silver nanoparticles can be uniformly loaded by utilizing the stable three-dimensional and porous structure advantages of the diatomite to obtain a large number of uniform 'hot spots', the different positions have similar SERS detection effects, and the high sensitivity and low-concentration trace detection of SERS detection can be realized.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing a surface-enhanced raman scattering substrate according to an embodiment of the present invention.
Fig. 2 is a schematic flow chart of a method for preparing a surface-enhanced raman scattering substrate according to an embodiment of the present invention.
Fig. 3(a) -3(d) are scanning electron microscope views of SERS substrates prepared according to embodiments of the present invention.
Fig. 3(e) and 3(f) are spectra obtained by SERS enhancement of the SERS substrate prepared according to the embodiment of the present invention.
Fig. 4 is a schematic flow chart of a method for performing surface enhanced raman scattering detection according to an embodiment of the present invention.
Detailed Description
In the drawings, the same or similar reference numerals are used to denote the same or similar elements or elements having the same or similar functions. Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
In the description of the present invention, the terms "central", "longitudinal", "lateral", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and therefore, should not be construed as limiting the scope of the present invention.
In the present invention, the technical features of the embodiments and implementations may be combined with each other without conflict, and the present invention is not limited to the embodiments or implementations in which the technical features are located.
The embodiment of the invention provides a preparation method of a surface-enhanced Raman scattering substrate, as shown in FIG. 1, comprising the following steps:
102, adding the diatomite particles into a beaker filled with deionized water, and respectively stirring and ultrasonically treating the mixture through a magnetic stirrer and an ultrasonic cleaner to obtain a diatomite aqueous solution.
And 104, adding the sodium citrate solution into the boiled solution and continuously heating the solution for a preset time.
And 105, cooling the remainder in the flask to room temperature, pouring the remainder into a centrifuge tube, and centrifugally cleaning the remainder with deionized water to obtain a precipitate at the lower end of the centrifuge tube.
And 106, dripping the precipitate onto a glass slide, and naturally evaporating the liquid to obtain the silver nanoparticle modified diatomite powder serving as the surface-enhanced Raman scattering substrate.
Wherein the silver nanoparticle modified diatomaceous earth powder is used to produce a concentration of 10-16And (3) surface enhanced Raman scattering spectrum of the object to be detected in mol/L.
Wherein each position of the silver nanoparticle modified diatomite powder has similar surface Raman enhancement effect.
In one embodiment, the particle size of the diatomaceous earth powder is optimally 10 μm.
In one embodiment, adding the diatomaceous earth powder to a beaker of deionized water comprises: adding 1-2mg of the diatomite powder into 1mL of deionized water in a proportion of adding the diatomite powder into the beaker containing the deionized water. For example, 10-20mg of diatomaceous earth powder is added to a beaker containing 10mL of deionized water.
In one embodiment, the flask is a three-neck flask, and the adding of the silver nitrate solution to the flask comprises: 10mL of silver nitrate solution with a concentration of 0.03-0.05mol/L was added to the flask. Among them, a silver nitrate solution of 0.035mol/L is preferable.
In one embodiment, the adding the sodium citrate solution to the boiling solution comprises: 10mL of a sodium citrate solution with a concentration of 0.005-0.01mol/L are added to the boiling solution. Among them, a 0.007mol/L sodium citrate solution is most preferable.
In one embodiment, after the sodium citrate solution is added to the boiling solution and heated for a preset time, the method further comprises the following steps before the residue in the flask is cooled to room temperature and poured into a centrifuge tube: the solution was stopped from boiling for 1-2 minutes by discontinuing heating, and then continued to boil for 3-4 minutes by continuing heating.
A specific example is provided below. It is to be understood that this example is provided only for better illustration of the method of preparing the surface enhanced raman scattering substrate of the present invention and is not intended to particularly limit the scope of the present invention.
As shown in fig. 2, the method for preparing a surface enhanced raman scattering substrate provided in this example includes:
Wherein the rotating speed of the magnetic stirrer is 900 revolutions per minute, and the frequency of the ultrasonic cleaner is 28 KHz.
And step 204, cooling the residue in the three-neck flask to room temperature, pouring the residue into a centrifuge tube, and washing the centrifuge tube with deionized water to obtain a precipitate at the lower end of the centrifuge tube.
And step 205, dripping the precipitate on a glass slide, and obtaining the silver nanoparticle modified diatomite powder used as the surface-enhanced Raman scattering substrate after the liquid is naturally evaporated and dried.
In order to illustrate the SERS detection effect of the SERS substrate prepared according to the embodiment of the present invention, that is, the silver nanoparticle modified diatomite powder, electron scanning microscopy (SEM) images of the silver nanoparticle modified diatomite powders prepared according to the method provided in the above example with different degrees of grinding are shown in fig. 3(a) - (d), and SERS detection spectra of rhodamine (R6G) molecules are shown in fig. 3(e) and 3(f), respectively. It will be readily appreciated that other molecules of interest may be substituted for the R6G molecule, and that the R6G molecule is illustrated herein by way of example only.
When SERS detection is carried out, firstly, solution of an object to be detected is prepared, for example, a certain amount of diatomite powder modified by silver nanoparticles prepared according to the method in the embodiment and different in grinding degree is poured into the solution of the object to be detected for full mixing, a small amount of mixed solution is dripped onto a glass slide, and SERS spectrum detection is carried out after the mixed solution is dried.
In FIGS. 3(e) and (f), the concentration of R6G was 10-12M、10-13M、10-14M、10-15M、10-16M(mol/L)。
As can be seen from fig. 3(a) -3(b), a large amount of silver nanoparticles are uniformly loaded on the diatomite powder, and the silver nanoparticles on the surface of the diatomite powder form a large amount of "hot spot" areas, which is very beneficial to the enhancement effect of SERS.
As can be seen from fig. 3(e) and 3(f), the silver nanoparticle modified diatomaceous earth powders with different degrees of attrition have very good SERS enhancement effect for different concentrations of R6G molecules, even when the concentration of R6G is as low as 10-16When M is used, SERS signals with relatively high relative intensity can be detected, and in addition, a sample with silver nanoparticles attached to the ground diatomite has a better enhancement effect and repeatability. The abscissa in FIGS. 3(e) and 3(f) is Raman Shift in cm-1The ordinate is Intensity in a.u (ArbitraryUnit).
An embodiment of the present invention further provides a method for performing surface enhanced raman scattering detection, as shown in fig. 4, including:
The diatomite powder modified by the silver nanoparticles is the diatomite powder modified by the silver nanoparticles and used as a surface-enhanced Raman scattering substrate, which is prepared by the method shown in figure 1 or 2.
And 402, performing surface enhanced Raman scattering detection on the object to be detected, comparing the detected object with the surface enhanced Raman scattering spectrum of the sample, and determining the components of the object to be detected.
As shown in fig. 3(e) and 3(f) above, the silver nanoparticle modified diatomite powder provided by the embodiment of the invention is used as the surface enhanced raman scattering substrate when the concentration of R6G is as low as 10-16And when M is adopted, SERS signals with relatively high relative intensity can be detected, so that the silver nanoparticle modified diatomite powder can be used as an SERS substrate for trace detection.
In addition, the diatomite powder modified by the silver nanoparticles provided by the embodiment of the invention is used as the surface-enhanced Raman scattering substrate, the repeatability is strong, the SERS detection at different positions of the substrate has similar effect, or the intensity change of the detected Raman spectrum is small, for example, in the range of 1/10 of the intensity value, so that the efficiency and the reliability of the SERS detection can be greatly improved by using the diatomite powder modified by the silver nanoparticles as the surface-enhanced Raman scattering substrate.
Finally, it should be pointed out that: the above examples are only for illustrating the technical solutions of the present invention, and are not limited thereto. Those of ordinary skill in the art will understand that: modifications can be made to the technical solutions described in the foregoing embodiments, or some technical features may be equivalently replaced; such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. A method for preparing a surface-enhanced Raman scattering substrate, comprising:
grinding the diatomite to obtain diatomite particles with the particle size of 5-20 microns, wherein the diatomite particles comprise sheet structures which are separated from the three-dimensional pore structures of the diatomite powder after grinding;
adding the diatomite particles into a beaker filled with deionized water, and respectively stirring and ultrasonically treating the mixture by a magnetic stirrer and an ultrasonic cleaner to obtain a diatomite aqueous solution;
transferring the diatomite aqueous solution into a flask, adding a silver nitrate solution into the flask, and heating and stirring until the mixture is boiled;
adding a sodium citrate solution into the boiled solution and continuously heating the solution for a preset time;
cooling the remainder in the flask to room temperature, pouring the remainder into a centrifuge tube, and centrifugally cleaning the remainder with deionized water to obtain a precipitate at the lower end of the centrifuge tube;
and dropping the precipitate onto a glass slide, and naturally evaporating the liquid to obtain the silver nanoparticle modified diatomite powder serving as the surface-enhanced Raman scattering substrate.
2. The method of claim 1, wherein the silver nanoparticles are modifiedDiatomaceous earth powder was used to produce a concentration of 10-16And (3) surface enhanced Raman scattering spectrum of the object to be detected in mol/L.
3. The method of claim 1, wherein the silver nanoparticle modified diatomaceous earth powder has similar surface raman enhancement effects at each site.
4. The method of claim 1, wherein the diatomaceous earth powder has a particle size of 10 μ ι η.
5. The method of claim 4, wherein adding the diatomaceous earth particles in a beaker of deionized water comprises:
adding the diatomite powder into the beaker with the deionized water according to the proportion of adding 1-2mg of the diatomite particles into 1mL of the deionized water.
6. The method of claim 1, wherein adding the silver nitrate solution to the flask comprises:
1mL of silver nitrate solution with a concentration of 0.005-0.01mol/L was added to the flask.
7. The method of claim 6, wherein adding the sodium citrate solution to the boiled solution comprises:
1mL of a sodium citrate solution with a concentration of 0.03-0.05mol/L was added to the boiled solution.
8. The method of claim 1, wherein after the adding the sodium citrate solution into the boiled solution and heating for a predetermined time, the method further comprises the following steps:
stopping heating to stop boiling for 5-10 min, and continuing heating to keep boiling for 30-40 min.
9. A method of performing surface enhanced raman scattering detection, comprising:
detecting a sample by using the silver nanoparticle modified diatomite powder prepared by the method according to any one of claims 1-8 as a surface-enhanced Raman scattering substrate to obtain a surface-enhanced Raman scattering spectrum of the sample at a preset concentration; the preset concentration comprises 10-16mol/L；
And performing surface enhanced Raman scattering detection on the object to be detected, and comparing the detected object with the surface enhanced Raman scattering spectrum of the sample to determine the components of the object to be detected.
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