CN108372314B - Preparation method of hollow gold-silver alloy nanoparticles with high SERS activity - Google Patents
Preparation method of hollow gold-silver alloy nanoparticles with high SERS activity Download PDFInfo
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- CN108372314B CN108372314B CN201810268295.9A CN201810268295A CN108372314B CN 108372314 B CN108372314 B CN 108372314B CN 201810268295 A CN201810268295 A CN 201810268295A CN 108372314 B CN108372314 B CN 108372314B
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- 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 preparation method of a hollow gold-silver alloy nano particle with high SERS activity. The cubic gold-silver alloy nano particles with complete outer walls and hollow interiors are obtained through the current replacement reaction between the silver simple substance and the chloroauric acid solution and the double effects of reducing and depositing silver ions and chloroauric acid by ascorbic acid; the preparation process of the hollow gold-silver alloy nano particle is simple and convenient, and the process is controllable; the gold-silver alloy characteristics ensure that the nano particles have high stability and can resist strong oxidizing agents (such as H)2O2) The application range of the etching is wider; the cubic structure with sharp corners and edges ensures that the nanoparticles have high SERS activity and high detection sensitivity, can carry out Raman detection on trace harmful food additives, and therefore has good application prospect.
Description
Technical Field
The invention belongs to the technical field of food safety detection, and particularly relates to a preparation method of a hollow gold-silver alloy nanoparticle with high SERS activity.
Background
The silver nano material has unique optical property, electrical property, catalytic property, excellent sensing capability and biological detection capability, so that the silver nano materials with various shapes are widely researched. Compared with the shapes such as sphere, rice grain, rod, belt and line, the cubic silver nanoparticles are most concerned. The silver nanocube has sharp edges and uniform appearance, and can be used as a high-sensitivity local plasma sensing and surface enhanced Raman substrate. But Ag is unstable and is easy to be substituted by H2O2、O2And oxidants such as halogen are oxidized into silver ions, so that the crystal structure is damaged, particularly the sharp edge angle of the silver nanocube is etched, and the SERS activity of the silver nanocube is greatly reduced. And silver ions generated by the oxidation of the Ag simple substance have toxic and side effects, so that the application of the silver ions in the biological field is limited.
As is well known, Au nanocrystals have excellent chemical stability, good biocompatibility and no toxic or side effects, and have wide application in the biological field. It is found that after silver and gold form a gold-silver alloy, the stability of silver element is greatly enhanced, and the silver in the gold-silver alloy is extremely difficult to be oxidized. Therefore, the prepared gold-silver alloy structure can obtain a high-stability SERS substrate, and the SERS application range of the silver nano material is widened. As a SERS substrate, the sharp corners of the nanoparticle surface are the sites that generate strong electromagnetic enhancement, i.e., active sites that enhance raman signals. The silver nanocubes are used as templates, hollow gold-silver alloy nanoparticles with strong electromagnetic enhancement sharp edges and corners can be obtained, the cubic structures of the hollow gold-silver alloy nanoparticles are reserved, and the hollow gold-silver alloy nanoparticles have high stability and high SERS activity and are important to be applied to the field of food detection.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a hollow gold-silver alloy nanoparticle with high SERS activity, which is simple in process, good in repeatability, controllable in particle size and high in stability.
In order to solve the technical problems, the technical scheme of the invention is as follows: a preparation method of hollow gold-silver alloy nanoparticles with high SERS activity is characterized by comprising the following specific steps:
the method comprises the following steps: preparing a silver nanocube by adopting a polyol process, and dispersing the silver nanocube into water to prepare a dispersion liquid with the mass concentration of 7.4 g/L;
step two: measuring 10-100 uL of the silver nano cubic dispersion liquid prepared in the step one, and magnetically stirring and uniformly mixing the silver nano cubic dispersion liquid with a stabilizer PVP and a reducing agent ascorbic acid at room temperature;
step three: continuously and uniformly stirring the solution obtained in the step two by magnetic force, and slowly dropwise adding a chloroauric acid aqueous solution into the solution to obtain a hollow cubic gold-silver alloy nano particle sol with the side length of 45-80 nm;
step four: and (4) repeatedly washing the gold-silver alloy nanoparticle sol obtained in the step three with ethanol and water for multiple times to obtain hollow gold-silver alloy nanoparticles, and dispersing the hollow gold-silver alloy nanoparticles in water for storage.
And in the second step, the molecular weight of the stabilizer PVP is one of 15000, 30000 and 55000.
In the second stepThe volume of the stabilizer PVP is 1-20 mL, and the concentration is 0.05-1 x 10-2mol/L, the volume of the reducing agent ascorbic acid is 0.1-5 mL, and the concentration is 0.01-1 mol/L.
The volume of the chloroauric acid aqueous solution in the third step is 0.5-10 mL, and the concentration is 0.1-2 mmol/L.
The dropping speed of the chloroauric acid aqueous solution in the third step is 0.01-0.2 mL/min.
The hollow gold-silver alloy nano particles obtained in the fourth step can be used for detecting trace harmful additives in food.
The first step of preparing the silver nanocubes comprises the following steps: adding 12mL of anhydrous Ethylene Glycol (EG) into a three-neck round-bottom flask, heating for 50 min under the condition of oil bath at 160 ℃, and then quickly adding 140 uL of Na with the concentration of 3mmol/L into the flask2S ethylene glycol solution, after 2min, 3 mL PVP ethylene glycol solution with the concentration of 180 mmol/L and the molecular weight of 40000 and 1mL AgNO with the concentration of 265 mmol/L are continuously added3The ethylene glycol solution, the whole process was carried out under magnetic stirring, the degree of progress of the reaction was monitored by ultraviolet-visible absorption spectroscopy, and when continuous characteristic ultraviolet absorption peaks appeared near 350 nm and 435nm, the flask was taken out and immersed in an ice-water bath to terminate the reaction, and then silver nanocubes having a particle size of about 43 nm were centrifugally separated.
The hollow gold-silver alloy nano particle prepared by the method has the following characteristics: (1) the structure is controllable, and the particle size is uniform; (2) the internal hollow structure reduces the consumption of metal elements and reduces the material cost; (3) the chemical stability is high, and the method can be used for monitoring systems with harsh conditions; (4) has sharp edges and corners, high SRES activity, and high concentration of p-aminophenol (4-ABT) of 10- 11When mol/L is reached, the characteristic peak can be still detected, and the detection sensitivity of the kit to additive melamine in food is 10-8mol/L; (5) as the SERS substrate, the universality is strong, and the SERS substrate can be used for detecting various analysis substances.
According to the invention, the hollow gold-silver alloy nanoparticles are obtained through the current displacement reaction between the chloroauric acid aqueous solution and the silver nanocubes, the speed of the electrostatic displacement reaction is reduced by adopting a titration mode in the reaction, so that the added gold ions and the silver ions subjected to electrostatic displacement are simultaneously reduced and deposited on the surface of the template to form a uniform and cavity-free wall, and meanwhile, the outer wall of the hollow structure is made of the gold-silver alloy component, so that the hollow gold-silver alloy nanoparticles have a high SERS effect and are used for detecting trace poisons. The method has the advantages of mild reaction conditions, simple operation, low equipment requirement and high reaction efficiency, thereby having good application prospect.
Drawings
FIG. 1 is a graph of the UV-VIS absorption spectrum of sample 1 prepared in example 1;
FIG. 2 is a graph of the UV-VIS absorption spectrum of sample 2 prepared in example 2;
FIG. 3 is a graph of the UV-VIS absorption spectrum of sample 3 prepared in example 3;
FIG. 4 is a transmission electron micrograph of sample 1 prepared in example 1;
FIG. 5 is a transmission electron micrograph of sample 2 prepared in example 2;
FIG. 6 is a transmission electron micrograph of sample 3 prepared in example 2;
FIG. 7 is an elemental distribution plot of sample 1 prepared in example 1;
FIG. 8 is a Raman spectrum of sample 1 prepared in example 1 for detection of p-aminophenol.
Detailed Description
To further illustrate the technical means and effects of the present invention for achieving the predetermined objects, the following detailed description of the specific implementation, method, steps, features and effects of the method for preparing hollow gold-silver alloy nanoparticles with high SERS activity according to the present invention with reference to the preferred embodiments is as follows:
example 1:
the method comprises the following steps: preparing silver nanocubes: adding 12m L anhydrous Ethylene Glycol (EG) into a three-neck round-bottom flask, heating at 160 deg.C in oil bath for 50 min, and rapidly adding 140 uL Na with concentration of 3mmol/L into the flask2S ethylene glycol solution, after 2min, 3 mL PVP (molecular weight 40000) ethylene glycol solution with concentration of 180 mmol/L and 1mL AgNO with concentration of 265 mmol/L are added continuously3Ethylene glycol solution, the whole process is carried out under magnetic stirring. Monitoring the reaction progress degree by using an ultraviolet visible absorption spectrum, taking out the flask and immersing the flask into an ice water bath to terminate the reaction when two characteristic ultraviolet absorption peaks appear near 350 nm and 435nm, then centrifugally separating a silver nanocube with the particle size of about 43 nm, repeatedly washing the silver nanocube with acetone, and dispersing the silver nanocube in water to prepare the silver nanocube with the mass concentration of 7.4 g/L;
step two: preparing hollow gold-silver alloy nanoparticles: and (2) at room temperature, adding 20 mu L of silver nanocube aqueous solution prepared in the step one and 5 mL of PVP aqueous solution with the concentration of 0.1mmol/L and the molecular weight of 30000 into a 50 mL reagent bottle, uniformly stirring by magnetic force, adding 0.5 mL of ascorbic acid aqueous solution with the concentration of 0.1mol/L, slowly dropwise adding 1mL of chloroauric acid aqueous solution with the concentration of 1mmol/L by using a syringe pump at the dropwise adding speed of 0.05 mL/min to obtain cubic gold-silver alloy nanoparticle sol with a hollow interior and a side length of 50 nm, repeatedly washing the hollow gold-silver alloy nanoparticles by using ethanol and water for multiple times, and dispersing in water for storage.
Example 2:
at room temperature, 40. mu.L of the silver nanocube aqueous solution prepared in the first step of example 1 and 10mL of PVP aqueous solution with a concentration of 0.3mmol/L and a molecular weight of 15000 were added to a 50 mL reagent bottle, after stirring uniformly by magnetic force, 2mL of ascorbic acid aqueous solution with a concentration of 0.05 mol/L was added, and then 6 mL of chloroauric acid aqueous solution with a concentration of 1.6m mol/L was slowly dropped using a syringe pump at a dropping speed of 0.1 mL/min. Obtaining cubic gold-silver alloy nano particle sol with hollow interior, wherein the side length is 60 nm. Then the hollow gold-silver alloy nano particles are repeatedly washed by ethanol and water for a plurality of times and then dispersed in water for storage.
Example 3:
at room temperature, 80. mu.L of the silver nanocube aqueous solution prepared in the first step of example 1 and 15 mL of PVP aqueous solution with a concentration of 0.8m mol/L and a molecular weight of 55000 are added into a 50 mL reagent bottle, after magnetic stirring is carried out uniformly, 4 mL of ascorbic acid aqueous solution with a concentration of 0.6 mol/L is added, and then 10mL of chloroauric acid aqueous solution with a concentration of 0.2mmol/L is slowly dripped by using a syringe pump, wherein the dripping speed is 0.17 mL/min. Obtaining cubic gold-silver alloy nano particle sol with hollow interior, wherein the side length is 72 nm. Then the hollow gold-silver alloy nano particles are repeatedly washed by ethanol and water for a plurality of times and then dispersed in water for storage.
The performance characterization of the hollow gold-silver alloy nanoparticles of sample 1 prepared in example 1, sample 2 prepared in example 2, and sample 3 prepared in example 3:
1. detecting an ultraviolet visible absorption spectrum:
the aqueous solutions of the sample 1, the sample 2 and the sample 3 are respectively detected by an ultraviolet-visible absorption spectrometer to obtain an ultraviolet-visible absorption spectrum, which is specifically shown in fig. 1, fig. 2 and fig. 3. It can be seen from the figure that 3 samples all have strong absorption in the visible light range, and the maximum absorption wavelengths thereof are 565 nm, 580 nm and 600 nm, respectively, which shows that the surface plasmon resonance absorption of the prepared hollow gold-silver alloy nanoparticles has adjustability, and the surface plasmon resonance absorption thereof gradually generates red shift as the wall thickness of the hollow gold-silver alloy nanoparticles increases.
2. Transmission electron microscope inspection and model schematic
Taking transmission electron microscope pictures of the sample 1, the sample 2 and the sample 3, as shown in fig. 4, fig. 5 and fig. 6, it can be known that the three samples are all in a cubic structure, and the surfaces of the three samples have sharp edges and corners and are active sites for enhancing the SERS effect; the interior is hollow, the wall thickness at the periphery is uniform and complete, the particle size is uniform, the side length of a cube is about 50 nm, 60nm and 73 nm, and the wall thickness is about 5nm, 10nm and 14 nm.
3. Elemental profile of sample 1
The elemental distribution of sample 1 was measured using an X-ray spectrometer, as shown in fig. 7, which indicates that sample 1 contains both gold and silver elements, and that both elements are uniformly distributed.
4. Surface enhanced Raman Scattering Activity of sample 1
To characterize the SERS activity of the nanoparticles, sample 1 was mixed with various concentrations of para-aminophenol (4-ABT) in a centrifuge tube and after standing at room temperature for 1h, the functionalized nanoparticles were washed free of excess 4-ABT with ethanol and water. Finally, the 4-ABT functional nano particles are divided intoDispersed in water, Raman signal was monitored, as shown in FIG. 8, when the concentration of 4-ABT was 10-11 When the concentration is mol/L, the characteristic peak can be still detected, which shows that the hollow gold-silver alloy nano particles in the sample 1 are used as an SERS substrate, have high SERS activity and can be applied to high-sensitivity detection.
5. Sample 1 as SERS substrate for detecting melamine
Sample 1 was mixed with different concentrations of melamine in a centrifuge tube and after standing at room temperature for 3 h, the unadsorbed melamine was washed off with water. Dispersing the melamine adsorbed nanoparticles in water, detecting Raman signals, and determining the concentration of melamine to be 10-8 When the concentration is mol/L, the characteristic peak can be detected, the hollow gold-silver alloy nano particles in the sample 1 are used as an SERS substrate, and the detection sensitivity of the hollow gold-silver alloy nano particles to melamine is 10-8 mol/L, can be applied to highly sensitive detection of toxic additives in food.
Claims (4)
1. A preparation method of hollow gold-silver alloy nanoparticles with high SERS activity is characterized by comprising the following specific steps:
the method comprises the following steps: preparing a silver nanocube by adopting a polyol process, and dispersing the silver nanocube into water to prepare a dispersion liquid with the mass concentration of 7.4 g/L;
step two: measuring 10-100 muL of silver nano cube dispersion liquid prepared in the first step, and magnetically stirring and uniformly mixing the silver nano cube dispersion liquid with a stabilizer PVP and a reducing agent ascorbic acid at room temperature;
step three: continuously and uniformly stirring the solution obtained in the step two by magnetic force, and slowly dropwise adding a chloroauric acid aqueous solution into the solution to obtain a hollow cubic gold-silver alloy nano particle sol with the side length of 45-80 nm;
step four: repeatedly washing the gold-silver alloy nanoparticle sol obtained in the step three with ethanol and water for multiple times to obtain hollow gold-silver alloy nanoparticles, and dispersing the hollow gold-silver alloy nanoparticles in water for storage;
in the second step, the volume of the stabilizer PVP is 1-20 mL, and the concentration is 0.05-1 multiplied by 10-2mol/L, the volume of the reducing agent ascorbic acid is 0.1-5 mL, and the concentration is 0.01-1 mol/L;
in the third step, the volume of the chloroauric acid aqueous solution is 0.5-10 mL, and the concentration is 0.1-2 mmol/L;
the dropping speed of the chloroauric acid aqueous solution in the third step is 0.01-0.2 mL/min.
2. The method of claim 1, wherein: and in the second step, the molecular weight of the stabilizer PVP is one of 15000, 30000 and 55000.
3. The method of claim 1, wherein: the hollow gold-silver alloy nano particles obtained in the fourth step can be used for detecting trace harmful additives in food.
4. The method of claim 1, wherein: the first step of preparing the silver nanocubes comprises the following steps: adding 12mL of anhydrous ethylene glycol into a three-neck round-bottom flask, heating for 50 min at 160 ℃ in an oil bath, and quickly adding 140 uL of Na with the concentration of 3mmol/L into the flask2S ethylene glycol solution, after 2min, 3 mL PVP ethylene glycol solution with the concentration of 180 mmol/L and the molecular weight of 40000 and 1mL AgNO with the concentration of 265 mmol/L are continuously added3The reaction was terminated by taking out the flask and immersing it in an ice-water bath when two characteristic uv absorption peaks appeared around 350 nm and 435nm, and then centrifuging the silver nanocubes having a particle size of about 43 nm.
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