CN110961620A - Nano material for SERS detection and preparation method and application thereof - Google Patents
Nano material for SERS detection and preparation method and application thereof Download PDFInfo
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
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- 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
Abstract
The invention relates to a nano material for SERS detection and a preparation method and application thereof. The nano material for SERS detection has the advantages of high SERS activity, high stability, simple preparation operation and good repeatability.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a nano material for SERS detection and a preparation method and application thereof.
Background
The Surface Enhanced Raman Scattering (SERS) effect refers to the phenomenon that Raman scattering signals of adsorbed molecules are enhanced compared with common Raman scattering signals on the surfaces of some specially prepared good metal conductors or in sol, and the Surface Enhanced Raman Scattering (SERS) has the characteristics of fingerprint property, ultrahigh detection sensitivity, nondestructive detection, no interference of solvent water and the like, and has important application value in the field of analysis. The SERS enhancement mechanism includes chemical enhancement and electromagnetic enhancement, wherein the signal enhancement in SERS mainly comes from the electromagnetic enhancement between light and metal, and the electromagnetic enhancement can greatly enhance the laser field through the excitation of plasma resonance. The strongest electromagnetic enhancement generally occurs at sharp edges, corners or voids formed between metal particles of the metal structure. For example, silver nanocubes and nanopyramids with sharp corners, silver or gold nanostars with many sharp points, and the like are excellent SERS materials, but the preparation of the nanoparticles with controllable morphology is generally difficult and complex in process.
Disclosure of Invention
The technical problem solved by the invention is as follows: the nano material for SERS detection has the advantages of high SERS activity, high stability, simple preparation operation and good repeatability.
The specific solution provided by the invention comprises the following steps:
the invention provides a nano material for SERS detection, which consists of an inner core, an intermediate layer coated on the surface of the inner core and a shell coated on the surface of the intermediate layer, wherein the inner core is a silver nanosphere, the intermediate layer is a titanium dioxide layer, and the shell is formed by aggregating silver nanoparticles.
The scheme based on the invention has the following beneficial effects:
(1) the silver nanospheres with larger particle sizes as the inner cores have higher SERS activity, and gaps formed among the silver nanoparticles with small particle sizes at the outer layers can also generate high electromagnetic enhancement, so that the composite material has high SERS activity.
(2) Titanium dioxide is a material with high physical and chemical stability, has excellent biocompatibility, and has been widely used in the fields of catalysis, environmental protection, biosensing, and the like. The composite material prepared by coating a layer of titanium dioxide on the surface of the silver nanosphere as an intermediate layer and then depositing silver nanoparticles on the surface in situ has high stability in various solvents due to a large amount of hydroxyl on the surface of the titanium dioxide.
Further, the particle size of the inner core is 20-40 nm, the thickness of the middle layer is 10-40nm, the thickness of the outer shell is 5-20nm, and the particle size of the silver nanoparticles is 5-20 nm.
The signal enhancement in SERS mainly comes from the electromagnetic action between light and silver nano particles and silver nanospheres and enables the laser field to be greatly enhanced through plasma resonance excitation, and to generate the phenomenon, molecules must be adsorbed on or very close to the metal surface, and the silver @ titanium dioxide @ nano silver structure under the structural condition can generate high electromagnetic enhancement and has high SERS activity.
The invention also provides a preparation method of the nano material for SERS detection, which is characterized by comprising the following steps:
1) dispersing silver nanospheres in a mixed solution of 120-200 mL of ethanol, acetonitrile and ammonia water to obtain a silver nanosphere dispersion liquid, wherein the concentration of the nanosphere dispersion liquid is 0.05-0.25mg/mL, and the volume ratio of the ethanol to the acetonitrile to the ammonia water in the mixed solution is (200-300) to (60-100): 1;
2) under the stirring condition, 0.1-10ml of titanate is dripped into the silver nanosphere dispersion liquid, and stirring is continued for 0.5-6 h to obtain a core-shell structure composite material silver @ titanium dioxide nanosphere which takes the silver nanosphere as an inner core and takes titanium dioxide as a shell;
3) the composite material silver @ titanium dioxide with the core-shell structure is washed and then dispersed in a mixed solution B of ethanol and n-butylamine, silver nitrate is added and dissolved to obtain a silver @ titanium dioxide dispersion solution, the dispersion solution is stirred and reacts in a water bath at the temperature of 50-80 ℃ for 0.5-4h to obtain a product silver @ titanium dioxide @ nano silver, wherein the product silver @ titanium dioxide @ nano silver takes silver nanospheres as an inner core, titanium dioxide as an intermediate layer and silver nanoparticles as a shell.
The preparation method based on the invention has the following beneficial effects:
(1) the preparation method has the advantages of simplicity, good repeatability, high efficiency and the like, the outer layer is a gap formed between the silver nano particles with small particle size, high electromagnetic enhancement can be generated, and compared with silver nano cubes, nano triangular plates and a plurality of sharp-angled silver or gold nano stars, the method for preparing the high SERS active material with simple operation and good repeatability is used for forming the nano gap by aggregating the metal nano particles.
(2) The prepared composite material has high SERS activity and catalytic activity and high stability in various solvents.
Further, the concentration of silver @ titanium dioxide in the silver @ titanium dioxide dispersion liquid in the step 3) is 1-2 mg/ml, the concentration of silver nitrate is 0.5-3.5 mg/ml, and the concentration of n-butylamine is 1-2 mg/ml.
Under the condition, the silver nanoparticles on the outer shell have uniform and dense particle sizes to form nanogap, the silver nanospheres with larger particle sizes on the inner core and the silver nanoparticle gaps with small particle sizes on the outer layer can generate high electromagnetic enhancement, so that the composite material has high SERS activity.
Specifically, the silver nanospheres are purchased from commercial products or prepared, and the diameter of the silver nanospheres is 20-40 nm.
Preferably, the silver nanospheres are prepared by methods disclosed in the prior art.
See in particular the publications L.Rainville, M.C.Dorais, D.Boudreau, Controlledsynthesis of low polydispersivity Ag @ SiO2 core-shell nanoparticles for use in electrochemical applications, RSC adv.3(2013) 13953-.
Silver is easy to oxidize, and the silver nanosphere with high SERS activity can be obtained by the existing method.
Further, the titanate is selected from any one of tetrabutyl titanate, tetraisopropyl titanate or tetraethyl titanate.
Further, the step 3) comprises the steps of repeatedly washing the product silver @ titanium dioxide @ nano silver with ethanol and water for multiple times, and dispersing in water for storage.
The invention takes silver nanospheres with large particle size as cores, coats a titanium dioxide shell layer at room temperature by a gel sol method, and then in-situ deposits silver nanoparticles on the surface of titanium dioxide by taking n-butylamine as a reducing agent to obtain the silver @ titanium dioxide @ silver nanoparticle composite material. The silver nanospheres with larger particle sizes as the inner cores can generate high electromagnetic enhancement in gaps formed among the silver nanoparticles with small particle sizes on the outer layers, so that the composite material has high SERS activity; in addition, the titanium dioxide intermediate layer enables the composite material to have high stability in various solvents, and the composite material is simple in preparation method, mild in reaction conditions, controllable in reaction process, high in efficiency and good in repeatability.
The application of the nano material for SERS detection as described above is used for detecting the concentration of organic pollutants or monitoring the catalytic degradation process of organic pollutants.
Further, the nano material is used for catalyzing sodium borohydride to reduce and degrade organic pollutants, and meanwhile, the degradation process of the organic pollutants is monitored.
The material shows stronger SERS activity and higher enhancement factor, and meanwhile, the silver nanoparticles with small particle size on the outer layer have intrinsic catalytic activity, so that the composite material has both SERS and catalytic functions and can be applied to SERS detection of organic dyes or SERS in-situ monitoring of degradation processes of the organic dyes. The composite material can effectively catalyze the sodium borohydride to reduce and degrade the organic pollutants and monitor the degradation process of the organic pollutants.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a TEM, SEM and elemental profile of a material prepared according to example 1 of the present invention, wherein (A) is a TEM image of silver @ titanium dioxide; (B) the graph is the distribution of silver in silver @ titanium dioxide, (C) the distribution of titanium in silver @ titanium dioxide, (D) the distribution of oxygen in silver @ titanium dioxide, (E) the SEM image of silver @ titanium dioxide, and (F) the SEM image of silver @ titanium dioxide @ nanosilver.
FIG. 2 is a graph showing the UV spectra of the silver @ titanium dioxide @ nano-silver composite material prepared in example 2 dispersed in different solvents as a function of time, wherein (A) is water, (B) is ethanol, (C) is a 0.1M phosphoric acid buffer solution, and (D) is a 0.4mM sodium chloride solution;
FIG. 3 is a graph of the silver @ titanium dioxide @ nano-silver composite prepared in example 2 versus the concentration of 10-6～10-10SERS spectrogram of mol/L4-mercaptobenzoic acid;
FIG. 4 is a graph of (A) SERS spectra and (B) Raman peak intensity versus time of the silver @ titanium dioxide @ nano-silver composite material prepared in example 3 in the process of catalyzing degradation of crystal violet by sodium borohydride.
Detailed Description
The following detailed description of embodiments of the invention is intended to be illustrative, and is not to be construed as limiting the invention.
Example 1
A preparation method of a nano material for SERS detection comprises the following steps:
(1) preparing silver nanospheres: 90mg of AgNO3Dissolving in 400mL of water to prepare a homogeneous solution, further dissolving 250mg of tannic acid and 360mg of trisodium citrate in 100mL of water, heating the two solutions to 60 ℃ in water baths, respectively, then mixing the two solutions under vigorous stirring, maintaining the reaction solution at 60 ℃ for 5 minutes, and then boiling the reaction solution for 20 minutes. After the reaction is finished, cooling the reaction liquid to room temperature, then centrifugally separating to obtain silver nanospheres with the particle size of about 35nm, repeatedly washing the silver nanospheres with ethanol and water for many times, and dispersing the silver nanospheres in the ethanol to prepare silver nanosphere dispersion liquid with the mass concentration of 6.5 mg/mL.
(2) Preparation of silver @ titanium dioxide: adding 120mL of ethanol, 40mL of acetonitrile and 0.5mL of ammonia water into a beaker, uniformly stirring by magnetic force, adding 2mL of prepared silver nanosphere dispersion liquid, continuously stirring for 30 minutes, slowly dropwise adding 3mL of tetrabutyl titanate by using a liquid transfer gun, continuously stirring for reacting for 3 hours, then carrying out centrifugal separation, repeatedly washing with ethanol and water by ultrasound repeatedly for multiple times to obtain 20mg of silver @ titanium dioxide, and dispersing the silver @ titanium dioxide in 2mL of ethanol for storage.
(3) Preparation of silver @ titanium dioxide @ nano silver: 1.0mL of the prepared silver @ titanium dioxide ethanol dispersion is centrifuged to remove the supernatant, and then the silver @ dioxide is oxidizedTitanium with 10mL ethanol and 2X 10-4Ultrasonic mixing of n-butylamine solution, adding 1.1 × 10-4And (3) completely dissolving the silver nitrate solid by ultrasonic treatment, magnetically stirring the reaction solution in a water bath at 60 ℃ for reaction for 1.5h, after the reaction is finished, performing centrifugal separation, repeatedly washing ethanol and water for multiple times to obtain the silver @ titanium dioxide @ nano silver composite material, and finally dispersing the silver nitrate solid in water for storage.
The silver @ titanium dioxide and the silver @ titanium dioxide @ nano silver prepared in the example 1 are subjected to morphology analysis, and the silver @ titanium dioxide is subjected to element analysis, and the result is shown in the attached drawing 1, wherein a Transmission Electron Microscope (TEM) image of the silver @ titanium dioxide prepared in the example 1 is shown in the drawing 1, and the silver @ titanium dioxide is of a complete core-shell structure and is uniform in shell thickness; FIGS. 1B, 1C and 1D are the silver, titanium and oxygen profiles, respectively, of the silver @ titanium dioxide prepared in example 1, showing that the titanium and oxygen elements are coated on the surface of the silver spheres; FIG. 1E is a TEM image of the silver @ titanium dioxide prepared in example 1, from which it can be seen that the silver @ titanium dioxide has a smooth surface and a uniform particle size; FIG. 1F is a TEM image of the silver @ titanium dioxide @ nanosilver prepared in the example, from which it can be seen that the silver @ titanium dioxide @ nanosilver has dense, uniform silver nanoparticles deposited on the surface.
Example 2
A preparation method of a nano material for SERS detection comprises the following steps:
(1) preparing silver nanospheres: meanwhile, example 1 is different in that after repeatedly washing with ethanol and water for many times, the silver nanospheres are dispersed in ethanol to prepare a silver nanosphere dispersion liquid with a mass concentration of 7.2 mg/mL.
(2) Preparation of silver @ titanium dioxide: adding 120mL of ethanol, 40mL of acetonitrile and 0.5mL of ammonia water into a beaker, uniformly stirring by magnetic force, adding 3mL of prepared silver nanospheres, continuously stirring for 30 minutes, slowly dropwise adding 6mL of tetrabutyl titanate by using a liquid transfer gun, continuously stirring for reacting for 4 hours, then carrying out centrifugal separation, repeatedly washing with ethanol and water by ultrasound for multiple times to obtain 35mg of silver @ titanium dioxide, and dispersing the silver @ titanium dioxide in 3mL of ethanol for storage.
(3) Preparation of silver @ titanium dioxide @ nano silver:1.0mL of the prepared silver @ titanium dioxide ethanol dispersion was centrifuged to remove the supernatant, and then the silver @ titanium dioxide was mixed with 10mL of ethanol and 2X 10-4Ultrasonic mixing of n-butylamine in mol, adding 1.7X 10-4And (3) performing ultrasonic treatment on mol silver nitrate solid, performing magnetic stirring reaction on the reaction solution in a water bath at 50 ℃ for 3 hours after the reaction is finished, performing centrifugal separation, repeatedly washing ethanol and water for multiple times to obtain the silver @ titanium dioxide @ nano silver composite material, and finally dispersing the silver nitrate solid in water for storage.
Example 3
A preparation method of a nano material for SERS detection comprises the following steps:
(1) preparing silver nanospheres: the same as in example 1.
(2) Preparation of silver @ titanium dioxide: adding 120mL of ethanol, 40mL of acetonitrile and 0.5mL of ammonia water into a beaker, uniformly stirring by magnetic force, adding 2mL of prepared silver nanospheres, continuously stirring for 30 minutes, slowly dropwise adding 1.6mL of tetraisopropyl titanate by using a liquid transfer gun, continuously stirring for reacting for 6 hours, then carrying out centrifugal separation, repeatedly washing with ethanol and water by ultrasound for multiple times to obtain 24mg of silver @ titanium dioxide, and finally dispersing the silver @ titanium dioxide in 2mL of ethanol for storage.
(3) Preparation of silver @ titanium dioxide @ nano silver: 1.5mL of the prepared silver @ titanium dioxide was centrifuged to remove the supernatant, and the silver @ titanium dioxide was mixed with 10mL of ethanol and 2X 10-4Ultrasonic mixing of n-butylamine in mol, adding 1.8X 10-4And (3) carrying out ultrasonic treatment on mol silver nitrate solid to completely dissolve the silver nitrate solid, and then carrying out magnetic stirring reaction on the reaction liquid in a water bath at the temperature of 70 ℃ for 2 hours. After the reaction is finished, centrifugally separating, repeatedly washing ethanol and water for many times to obtain the silver @ titanium dioxide @ nano silver composite material, and finally dispersing the silver @ titanium dioxide @ nano silver composite material in water for storage.
And (3) detecting the stability of the silver @ titanium dioxide @ nano silver composite material:
the silver @ titanium dioxide @ nano-silver composite material prepared in the same amount in example 2 is uniformly mixed with solvent water, ethanol, 0.1M phosphoric acid buffer solution and 0.4mM sodium chloride solution respectively, standing is carried out, then visible-ultraviolet absorption spectrogram tests are carried out in different time periods, the test results are shown in figures 2A-D, and the ultraviolet absorption spectral intensity of the nano-particles is basically not reduced within 3h, so that the silver @ titanium dioxide @ nano-silver composite material prepared in the invention is proved to have high dispersion stability in the solutions.
Detection of SERS activity of silver @ titanium dioxide @ nano silver composite material:
the silver @ titanium dioxide @ nano-silver composite material prepared in the example 2 is added into the solution with the concentration of 10-6～10-10SERS spectrogram test is carried out in mol/L4-mercaptobenzoic acid, the test result is shown in figure 3, the Raman enhancement effect is very strong, the sensitivity is high, and the detection concentration of 4-mercaptobenzoic acid can reach 10-9mol/L。
Example of an application of SERS in situ monitoring of crystal violet reductive degradation:
taking 0.2mL of silver @ titanium dioxide @ nano-silver aqueous dispersion prepared in example 3 and 3mL of aqueous dispersion with the concentration of 10-4mixing mol/L crystal violet water solution in a centrifugal test tube, standing for 12h at room temperature, washing redundant crystal violet from functionalized nano particles by water, dispersing the crystal violet functionalized nano particles in 0.25mL of water, uniformly mixing the crystal violet functionalized nano particles with 0.25mL of 5mg/mL sodium borohydride water solution, transferring the mixture into a quartz cuvette, placing the quartz cuvette in a detection tank of a portable Raman spectrometer, and collecting Raman signals at certain time points, wherein the used laser wavelength is 785nm, and the signal collection time is 20 s. As shown in FIGS. 4A-B, it can be seen from FIG. 4A that the crystal violet is present at 912cm with the lapse of time-1，1170cm-1And 1619cm-1The characteristic Raman shift peak intensity of the Raman spectrum is rapidly weakened and completely disappears at 6 min. FIG. 4B is a 912cm diagram from FIG. 4A-1Ln (I) calculated from Raman peak intensityt/I0) Fitting a first-order straight line relative to a time relation graph to obtain a reaction rate constant of 0.3473min-1. The result shows that the crystal violet can be rapidly degraded into small molecules, and the silver @ titanium dioxide @ nano-silver composite material prepared by the method can be applied to SERS in-situ monitoring of the catalytic degradation process of organic dyes.
Although embodiments of the present invention have been described in detail above, those of ordinary skill in the art will understand that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (8)
1. The nanometer material for SERS detection is characterized by comprising an inner core, an intermediate layer and a shell, wherein the intermediate layer is coated on the surface of the inner core, the shell is coated on the surface of the intermediate layer, the inner core is a silver nanosphere, the intermediate layer is a titanium dioxide layer, and the shell is formed by gathering silver nanoparticles.
2. The nanomaterial for SERS detection according to claim 1, wherein the particle size of the core is 20-40 nm, the thickness of the intermediate layer is 10-40nm, the thickness of the shell is 5-20nm, and the particle size of the silver nanoparticle is 5-20 nm.
3. A method for preparing a nano-material for SERS detection according to claim 1 or 2, comprising the steps of:
1) dispersing silver nanospheres in a mixed solution of 120-200 mL of ethanol, acetonitrile and ammonia water to obtain a silver nanosphere dispersion solution, wherein the concentration of the nanosphere dispersion solution is 0.05-0.25mg/mL, and the volume ratio of the ethanol to the acetonitrile to the ammonia water in the mixed solution is (200-300) to (60-100): 1;
2) under the stirring condition, 0.1-10ml of titanate is dripped into the silver nanosphere dispersion liquid, and the stirring is continued for 0.5-6 h to obtain the composite material with the core-shell structure, wherein the silver nanospheres are used as the inner core, and the titanium dioxide is used as the shell;
3) and (2) washing the composite material with the core-shell structure, dispersing the washed composite material into a mixed solution B of ethanol and n-butylamine, adding silver nitrate, dissolving to obtain a composite material dispersion liquid with the core-shell structure, and stirring and reacting in a water bath at 50-80 ℃ for 0.5-4h to obtain a product with silver nanospheres as an inner core, titanium dioxide as an intermediate layer and silver nanoparticles as an outer shell.
4. The preparation method of the nanomaterial for SERS detection according to claim 3, wherein the concentration of the composite material with the core-shell structure in the composite material dispersion with the core-shell structure is 1-2 mg/ml, the concentration of silver nitrate is 0.5-3.5 mg/ml, and the concentration of n-butylamine is 1-2 mg/ml.
5. The method for preparing a nano material for SERS detection as recited in claim 3, wherein the titanate is selected from any one of tetrabutyl titanate, tetraisopropyl titanate or tetraethyl titanate.
6. The method for preparing a nano material for SERS detection according to any one of claims 3 to 5, wherein the step 3) further comprises repeatedly washing the product with ethanol and water for multiple times, and dispersing the product in water for storage.
7. Use of a nanomaterial for SERS detection according to claim 1 or 2, wherein the nanomaterial is used for concentration detection of organic contaminants or for catalytic degradation process monitoring of organic contaminants.
8. The use of the nanomaterial for SERS detection according to claim 7, wherein the nanomaterial is used to catalyze the reductive degradation of organic contaminants by sodium borohydride while monitoring the degradation process of organic contaminants.
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| CN114397286B (en) * | 2022-01-04 | 2024-04-23 | 武汉工程大学 | Self-cleaning SERS active material and preparation method and application thereof |
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