CN110907426B - Method for enhancing SERS activity of silver decahedral nanoparticles by chloroauric acid - Google Patents

Method for enhancing SERS activity of silver decahedral nanoparticles by chloroauric acid Download PDF

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CN110907426B
CN110907426B CN201911273921.4A CN201911273921A CN110907426B CN 110907426 B CN110907426 B CN 110907426B CN 201911273921 A CN201911273921 A CN 201911273921A CN 110907426 B CN110907426 B CN 110907426B
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silver
nanoparticles
decahedral
chloroauric acid
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CN110907426A (en
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郑先亮
李宁
杨开宇
王欣
刘洋
于显利
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Jilin University
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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
    • 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

Abstract

The invention relates to a method for enhancing the SERS activity of silver decahedral nanoparticles by chloroauric acid. In general terms, silver decahedral nanoparticles (DeAgNPs) are used to exchange with trivalent gold ionsThe obtained silver-core gold-shell decahedral nanoparticles with different etching degrees are transferred to a silica gel substrate to form a two-dimensional film, so that the surface Raman enhancement of the 4-mercaptobenzoic acid (4-MBA) probe molecules is realized, and the results prove that the silver decahedral nanoparticles etched by chloroauric acid with different concentrations correspond to the Raman enhancement with different degrees. The method has the advantages of simple raw materials, low cost and safe and simple operation, and compared with pure silver decahedral nanoparticles, the chloroauric acid (HAuCl) prepared by the method of the invention4) The etched silver decahedron nanoparticles have special structure and good stability, the SERS activity is greatly improved, the method for detecting the object to be detected of 4-mercaptobenzoic acid is simple and effective, the operation process is safe and pollution-free, and the method can be applied to water quality detection, biological detection and other aspects and has wide application prospect.

Description

Method for enhancing SERS activity of silver decahedral nanoparticles by chloroauric acid
The technical field is as follows:
the invention relates to a surface enhanced Raman spectroscopy detection technology, in particular to chloroauric acid (HAuCl)4) A method for enhancing SERS activity of silver decahedral nanoparticles (DeAgNPs). In summary, bimetallic nanoparticles with different etching degrees, which are obtained by the replacement reaction of the silver decahedral nanoparticles and a chloroauric acid solution with a specific concentration, are used as SERS substrates, so that the optimal SERS effect on the 4-mercaptobenzoic acid molecular probe is realized. The Raman signal of the substance to be detected with low concentration is enhanced, and the accurate detection of the toxic and harmful substances is realized.
Background art:
SERS (surface Enhanced Raman scattering) is a surface spectroscopy technique, and in short, SERS amplifies the Raman signal of a molecule by several orders of magnitude, wherein the signal amplification is mainly achieved by the electromagnetic interaction of light and metal, commonly referred to as plasmon resonance, which can greatly amplify the laser field. To benefit from this, the molecules must usually be adsorbed on the metal surface, or at least very close to the metal surface (usually ≈ 10nm maximum), in order to exploit this amplification field to enhance the raman signal of the molecules.
Metal colloids in water or deposited on planar substrates, which are mostly composed of silver (Ag) or gold (Au), are commonly used as SERS substrates, and are among the simplest and easiest ways to reach SERS. Compared with other nanoparticles, the silver nanoparticles can generate stronger and clearer plasma resonance, have excellent electromagnetic enhancement performance and have wider application prospect in theory, so that the silver nanoparticles are earlier and widely applied to the SERS field. At present, many reports of using gold or silver nanoparticles with different shapes and sizes as surface-enhanced raman scattering substrates are reported, such as those in the patent publication No. CN107235471B, and the like, and using an orderly etched silver nanowire film as an SERS substrate for detecting rhodamine B; further, as in Jinmingliang et al (published patent No.: CN10987487A), a silver nanocluster SERS substrate was prepared, which was detectable by a minimum of 10-16The single molecule detection is realized by the mol/L rhodamine, and the SERS effect can be realized by the visible nano silver/particles. In 2008, Vladimir Kitaev et al prepared silver decahedral nanoparticles (chem. mater.2008,20, 5186-.
However, the enhancement effect of the single silver nanoparticle serving as the SERS substrate is limited, silver is very easy to oxidize and difficult to store, and the gold nanoparticle is much more stable than silver under the same environmental condition, is difficult to oxidize and is widely applied to biology for many years, so that abundant synthesis and property knowledge is accumulated. Therefore, researchers have developed SERS research on bimetallic nanoparticles, such as Zhang super et al (published patent No. CN106442460A), and prepared a three-dimensional Raman-enhanced substrate combining gold @ silver nanoparticles and pyramidal silicon, which can give full play to the advantages of two metals and can be applied to various fields.
In order to solve the problems that the single silver nanoparticle is limited in Raman enhancement effect and difficult to store and poor in stability, and no report related to the SERS activity of the silver decahedral nanoparticles deposited with gold is found at present, chloroauric acid is introduced on the basis of the decahedral nanoparticles, the SERS activity of the silver decahedral nanoparticles is enhanced by a method of depositing part of gold through displacement reaction, and the SERS technology is expected to be applied to the fields of molecular quantitative detection, chemical and biological sensing, disease diagnosis and treatment, catalysis and the like.
The invention content is as follows:
the invention provides a method for enhancing the SERS activity of silver decahedral nanoparticles by chloroauric acid. The silver decahedral nanoparticles prepared by the photochemical reaction method have uniform size and higher SERS activity (Langmuir 2009,25, 3802-3807). According to the surface enhanced Raman scattering principle, the silver nanoparticles which are deposited with gold after the silver nanoparticles are subjected to the displacement reaction with the chloroauric acid solution with a specific concentration range can enhance the Raman spectrum of the 4-mercaptobenzoic acid molecular probe to different degrees and are used for the surface enhanced Raman detection technology.
The invention provides a method for enhancing SERS activity of silver decahedral nanoparticles by chloroauric acid, which comprises the following steps:
1) preparing the silver decahedral nanoparticles by a photochemical reaction method;
2) under high-speed stirring, quickly injecting quantitative deionized water or sodium chloride aqueous solution (contrast) into the silver decahedral nanoparticles prepared by the photoinduction method, and mixing and stirring for a certain time;
3) injecting chloroauric acid aqueous solutions with the same volume and different concentrations into the system in the step 2) at the same speed under medium-speed stirring in a time-volume mode of an injection pump;
4) adding a 4-mercaptobenzoic acid (4-MBA) molecular probe into the reaction system finished in the step 3), standing for a certain time, centrifuging, removing supernatant liquid, dropwise adding onto a clean silica gel substrate, and naturally drying.
In the invention, after the preparation of the silver decahedron in the step 1) is finished, sodium hydroxide is added for preservation, the concentration of the added sodium hydroxide is 0.01-0.2mol/L, and the dosage is 100-500 uL.
In the invention, the stirring speed of the step 2) is 3000r/min, the concentration of the sodium chloride aqueous solution is 0.1-0.01mol/L, the volume ratio of the silver decahedron to the sodium chloride solution is 100:1, and the mixing and stirring time is 1-3 min.
In the invention, the stirring speed in the step 3) is 1000--4-10-11mol/L, the speed of the injection pump is 0.1-0.3mL/h, and the time is 2 h.
In the invention, the concentration of the 4-mercaptobenzoic acid in the step 4) is 10-3-10-4mol/L; the volume ratio of the silver decahedron in the step 1) is 1:1-1: 2; centrifuging at 12000r/min for 10-15 min; the volume dropped on the silica gel substrate was 20-40 uL.
The method for enhancing the SERS activity of the silver decahedron nanoparticles by the aid of the chloroauric acid is characterized in that the growth process of the silver decahedron nanoparticles is monitored by combining ultraviolet-visible light spectroscopy (UV-Vis), the size and appearance of the nanoparticles are observed by a Transmission Electron Microscope (TEM), and the Raman spectroscopy (Raman) detects the enhancement degree of the Raman spectrum of the gold-silver bimetal decahedron nanoparticles on a 4-mercaptobenzoic acid probe.
Description of the drawings:
fig. 1 is a graph of ultraviolet-visible light spectrum (UV-Vis) of the growth process of the silver decahedral nanoparticles of example 1.
FIG. 2(a) (b) is a Transmission Electron Microscope (TEM) image of the silver decahedral nanoparticles prepared in example 1; (c) (d) is the chlorine-rich chloroauric acid (10) of example 6-9mol/L) Transmission Electron Microscopy (TEM) images of etched silver decahedral nanoparticles; (e) (f) (g) is the chlorine-rich chloroauric acid (10) of example 6-9mol/L) etched silver decahedral nanoparticle energy spectrum (EDS) diagram.
FIG. 3 is a schematic representation of the use of 4-mercaptobenzoic acid in ethanol aqueous solution with the silver decahedral nanoparticles of example 2 and 10, respectively-10mol/LHAuCl4Reaction product of solution, silver decahedral nanoparticles of example 3 and 10-9mol/L HAuCl4Reaction product of solution, silver decahedral nanoparticles of example 4 and 10-2The reaction product of the mol/L NaCl solution (control) and the mixed product of the silver decahedral nanoparticles and deionized water in example 5 (control) are SERS spectra of the Raman substrate.
The specific implementation mode is as follows:
example 1 preparation of silver decahedral nanoparticles
The experimental conditions and parameters were as follows:
1) 1.4705g of sodium citrate (Na) are weighed out3C6H5O7) Dissolving in 100mL deionized water to obtain 0.05mol/L sodium citrate aqueous solution. 0.1699g of silver nitrate (AgNO) were weighed out3) Dissolving in 100mL of deionized water to obtain 0.01mol/L silver nitrate solution. 0.076g of sodium borohydride (NaBH) is weighed out4) 50mL of cold water is measured in a small glass bottle and is quickly dissolved to prepare 0.02mol/L sodium borohydride solution, and the solution is stored at low temperature. (ii) a
2) Respectively taking 1mL of the sodium citrate solution and the silver nitrate solution, mixing the sodium citrate solution and the silver nitrate solution in a 150mL conical flask, adding 98mL of deionized water into the conical flask, and electromagnetically stirring the mixture at 1500r/min for 10min to uniformly mix the mixture. To the above mixed solution was slowly added dropwise 50uL of a sodium borohydride solution with vigorous electromagnetic stirring (3000 r/min). The mixed solution is rapidly changed into yellow from a colorless state, namely Ag + in the solution is changed into Ag and is aggregated to form nano-crystal, and the silver seed sol is formed. After the dropwise addition of the sodium borohydride solution, the mixed solution was continuously stirred for 3 min.
3) And transferring the 100mL of silver seed sol into a 200mL double-wall cooling reactor, cooling the reactor by circulating water at 10 ℃ along with slow electromagnetic stirring, carrying out photoinduction reaction on the system by using a self-made 465nm blue Light Emitting Diode (LED) lamp ring, monitoring a solution ultraviolet-visible light spectrogram 30 minutes/time, and judging the reaction process.
4) After the reaction, 300uL of NaOH solution was added to the reaction system, stirred for 3 minutes, and then stored in a sealed and dark place. After the final reaction product is subjected to centrifugal treatment, the morphology and the size of the silver decahedral nanoparticles are observed by a Transmission Electron Microscope (TEM).
Example 2 Chloroauric acid (10)-10mol/L) preparation of etched silver decahedral nanoparticles and SERS substrate
The experimental conditions and parameters were as follows:
1) formulation 10-10Chloroauric acid (HAuCl) in mol/L concentration gradient4) An aqueous solution. Formulation 10-4mol/L of ethyl 4-mercaptobenzoateThe alcohol-water solution is ready for use.
2) A liquid-transferring gun is used for transferring 4mL of the silver nanoparticles prepared in the example 1 into a small glass bottle, the whole process is carried out under the electromagnetic stirring of 3000r/min, after 30s, 40uL of deionized water is transferred and rapidly injected into the glass bottle, and the stirring is continuously carried out for 30 min; then the rotating speed is adjusted to 1000r/min, and 400uL of HAuCl is slowly pumped into the mixture at a constant speed of 2mL/h by using an injection pump4Periodically measuring the ultraviolet and visible light spectrum of each group of samples in the solution; finally, the supernatant is removed after 12000r/min and 10min of centrifugal treatment. When preparing a Raman test sample, adding 2mL of 4-mercaptobenzoic acid solution into the centrifugal product, fully stirring for 20s, standing for 30min, taking 30uL, slowly dripping on a cleaned silica gel substrate, and airing in a dark room.
Example 3 Chloroauric acid (10)-9mol/L) preparation of etched silver decahedral nanoparticles and SERS substrate
The experimental conditions and parameters were as follows:
1) formulation 10-9Chloroauric acid (HAuCl) in mol/L concentration gradient4) An aqueous solution. Formulation 10-4The 4-mercaptobenzoic acid ethanol water solution with mol/L is reserved.
2) A liquid-transfering gun transfers 4ml of the silver nano-particles prepared in the example 1 into a small glass bottle, the whole process is operated under the electromagnetic stirring of 3000r/min, after 30s, 40uL of deionized water is transferred and quickly injected into the glass bottle, and the stirring is continued for 30 min; then the rotating speed is adjusted to 1000r/min, and 400uL of HAuCl is slowly pumped into the mixture at a constant speed of 2mL/h by using an injection pump4Periodically measuring the ultraviolet and visible light spectrum of each group of samples in the solution; finally, the supernatant is removed after 12000r/min and 10min of centrifugal treatment. When preparing a Raman test sample, adding 2mL of 4-mercaptobenzoic acid solution into the product, fully stirring for 20s, standing for 30min, taking 30uL, slowly dripping the solution on a silica gel substrate which is cleaned, and airing the silica gel substrate in a dark room.
Example 4 sodium chloride (10)-2mol/L) preparation of etched silver decahedral nanoparticles and SERS substrate
The experimental conditions and parameters were as follows:
1) 0.0234g of NaCl is weighed out and dissolved in 40ml of deionized water to obtain 0.01mol/L of sodium chloride solution. Formulation 10-4The 4-mercaptobenzoic acid ethanol water solution with mol/L is reserved.
2) A liquid-transferring gun transfers 4mL of the silver nanoparticles prepared in the example 1 into a small glass bottle, the whole process is operated under the electromagnetic stirring of 3000r/min, after 30s, 40uL of sodium chloride solution is transferred and rapidly injected into the glass bottle, and the stirring is continued for 30 min; then, the rotation speed is adjusted to 1000r/min, 400uL deionized water is slowly pumped into the sample by an injection pump at a constant speed of 2mL/h, and the ultraviolet visible light spectrum of each group of samples is periodically measured; finally, the supernatant is removed after 12000r/min and 10min of centrifugal treatment. When preparing a Raman test sample, adding 2mL of 4-mercaptobenzoic acid solution into the product, fully stirring for 20s, standing for 30min, taking 30uL, slowly dripping the solution on a silica gel substrate which is cleaned, and airing the silica gel substrate in a dark room.
Example 5 preparation of pure silver decahedral nanoparticle SERS substrate
The experimental conditions and parameters were as follows:
1) formulation 10-4The 4-mercaptobenzoic acid ethanol water solution with mol/L is reserved.
2) A liquid-transferring gun is used for transferring 4mL of the silver nanoparticles prepared in the example 1 into a small glass bottle, the whole process is carried out under the electromagnetic stirring of 3000r/min, after 30s, 40uL of deionized water is transferred and rapidly injected into the glass bottle, and the stirring is continuously carried out for 30 min; then, the rotation speed is adjusted to 1000r/min, 400uL of deionized water is slowly pumped into the sample by an injection pump at a constant speed of 2ml/h, and the ultraviolet visible light spectrum of each group of samples is periodically measured; finally, the supernatant is removed after 12000r/min and 10min of centrifugal treatment. When preparing a Raman test sample, adding 2mL of 4-mercaptobenzoic acid solution into the product, fully stirring for 20s, standing for 30min, taking 30uL, slowly dripping the solution on a silica gel substrate which is cleaned, and airing the silica gel substrate in a dark room.
Example 6 chlorine-rich chloroauric acid (10)-9mol/L) preparation of etched silver decahedral nanoparticles and SERS substrate
The experimental conditions and parameters were as follows:
1) formulation 10-9Chloroauric acid (HAuCl) in mol/L concentration gradient4) An aqueous solution. 0.0234g of NaCl is weighed out and dissolved in 40mL of deionized water to obtain 0.01mol/L of sodium chloride solution. Formulation 10-4molThe solution of the alcohol water solution of the 4-mercaptobenzoic acid is L for standby.
2) A liquid-transferring gun transfers 4mL of the silver nanoparticles prepared in the example 1 into a small glass bottle, the whole process is operated under the electromagnetic stirring of 3000r/min, after 30s, 40uL of sodium chloride solution is transferred and rapidly injected into the glass bottle, and the stirring is continued for 30 min; then the rotating speed is adjusted to 1000r/min, and 400uL of HAuCl is slowly pumped into the mixture at a constant speed of 2ml/h by using an injection pump4Periodically measuring the ultraviolet and visible light spectrum of each group of samples in the solution; finally, the supernatant is removed after 12000r/min and 10min of centrifugal treatment. When preparing a Raman test sample, adding 2mL of 4-mercaptobenzoic acid solution into the product, fully stirring for 20s, standing for 30min, taking 30uL, slowly dripping the solution on a silica gel substrate which is cleaned, and airing the silica gel substrate in a dark room.
According to the method provided by the invention, the method for enhancing the SERS activity of the silver decahedral nanoparticles by the chloroauric acid can be provided, and is characterized in that:
1) ultraviolet-visible spectrum (UV-vis) characterization was performed on the decahedral silver nanoparticles synthesized by light induction in example 1. The results show that the silver decahedral nanoparticles with uniform size are successfully prepared. As shown in fig. 1, the initial silver nano-seed sol has a broad absorption peak around 400nm, representing the exciton characteristics of the small-sized spherical AgNPs. According to the ultraviolet-visible light absorption spectrum, under the surrounding radiation of a 465nm blue LED light source, a characteristic plasma peak absorption band appears at the 485nm position, the peak at the 485nm position gradually rises and has a red shift trend along with the extension of the photoinduction reaction time, and the half-height width is narrow, which represents the formation of uniform large-size AgNPs; and the seed peak at 400nm shows a descending trend, which shows the reduction of the small-size AgNPs, the whole dynamic change shows the aggregation and orientation growth process of the small-size nanoparticles under the light induction, and when the reaction stops, the absorption peak at 500nm keeps unchanged for a period of time.
2) Transmission Electron Microscope (TEM) observation and energy spectrum analysis were performed for examples 1 and 6. As shown in FIGS. 2(a) and (b), it can be seen that DeAgNPs having a relatively uniform size were successfully prepared, and the average particle diameter (expressed as side length) was about 32 nm. FIG. 2(c) (d) is a high-resolution TEM image of Ag nanoparticles with Au deposited after adding 1nM chloroauric acid in example 6, in which the sharp corners of the decahedron of Ag are passivated by the displacement reaction of Ag and trivalent Au ions at the high-activity sites, and Au is deposited on the decahedron. Fig. 2(e) (f) (g) is an Energy Dispersive Spectroscopy (EDS) of elemental analysis of the nanoparticles of fig. 2(c), and it can be seen from fig. 2(e) (f) that gold is deposited on the silver nanoparticles.
3) FIG. 3 is a graph of 4-MBA SERS spectra adsorbed on the surface of nanoparticles prepared in examples 2-5. From the figure we can see the distinct characteristic vibrational band attributed to 4-MBA. For example, the graph shows the 4-MBA SERS spectrum (DeAgNPs) adsorbed on the surface of the pure silver nanoparticles prepared in example 4: the peak at 1586cm-1 is due to C-C symmetric stretching vibration; the spectral peak at 1482cm-1 is caused by C-C asymmetric stretching vibration and C-H in-plane bending vibration; the broad spectrum peak at 1422cm-1 is due to COO-stretching vibrations; the spectral peak at 1182cm-1 is attributed to the planar bending vibration of C-H; the peak at 1140cm-1 is due to the in-plane bending vibration of CCC, stretching vibration of C-S and C-COOH; the spectral peak at 1079cm < -1 > belongs to the in-plane respiratory vibration of a benzene ring and the C-S telescopic vibration; the spectral peak at 844cm-1 is attributed to the deformation vibration of COO-; the spectral peak at 717cm-1 is attributed to the out-of-plane bending vibration of CCC. Compared with the SERS spectrum of the 4-MBA enhanced by the pure silver decahedron, the SERS signal intensity (based on 1586cm < -1 >) of the silver nanoparticle substrate added with the sodium chloride, the 1n M chloroauric acid and the 0.1n M chloroauric acid is respectively improved by 1.5 percent, 22.3 percent and 51.3 percent compared with the pure DeAgNPs. The improvement of the performance is more beneficial to the application of the decahedral silver nanoparticle in spectral detection, and is expected to effectively detect molecules in a lower concentration range.

Claims (4)

1. A method for enhancing SERS activity of silver decahedral nanoparticles by chloroauric acid is characterized by comprising
The method comprises the following steps:
1) preparing silver decahedron nanoparticles by a photochemical reaction method, wherein firstly, the prepared silver seed sol finishes a photoinduction reaction in a low-temperature water bath environment at 10 ℃ and a slow electromagnetic stirring process, a 465nm blue Light Emitting Diode (LED) array is adopted as a light source in the photoinduction reaction process, after the reaction is finished, a sodium hydroxide solution is dripped into the silver decahedron nanoparticle sol, the mixture is stirred for 3min and then sealed and kept away from light, wherein the concentration of the sodium hydroxide is 0.01-0.2mol/L, and the volume is 100 and 500 uL;
2) under the high-speed stirring of 3000r/min, deionized water or 0.1-0.01mol/L sodium chloride aqueous solution in a specific proportion is quickly injected into the stable silver decahedral nano particles to serve as a control group, and the mixture is mixed and stirred for a certain time;
3) injecting chloroauric acid solutions with the same volume and different concentrations into the system of the step 2) at the speed of 0.1-0.3mL/h under the stirring of 1000--4-10-11mol/L；
4) Adding 10 concentration into the reaction system of the step 2) and the step 3)-3-10-4Standing a 4-mercaptobenzoic acid (4-MBA) molecular probe of mol/L for a certain time, centrifuging at 12000r/min for 10-15min, removing supernatant, dripping on a clean silica gel substrate, and naturally drying.
2. The method of claim 1, wherein: and 2) the volume ratio of the decahedron silver to the sodium chloride or deionized water solution is 100:1, and the mixing and stirring time is 1-3 min.
3. The method of claim 1, wherein: and 3) the injection time of the injection pump in the step 3) is 2 h.
4. The method of claim 1, wherein: the volume ratio of the probe molecule 4-mercaptobenzoic acid used in the step 4) to the silver decahedron used in the step 1) is 1:1-1: 2; the carrier for depositing the nano particles is a silica gel substrate, and the volume of the carrier dropped on the silica gel substrate is 20-40 uL.
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