CN114839180A - Preparation method of spray type bi-component composite Raman substrate - Google Patents
Preparation method of spray type bi-component composite Raman substrate Download PDFInfo
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- CN114839180A CN114839180A CN202210462445.6A CN202210462445A CN114839180A CN 114839180 A CN114839180 A CN 114839180A CN 202210462445 A CN202210462445 A CN 202210462445A CN 114839180 A CN114839180 A CN 114839180A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
- B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
- B05B7/02—Spray pistols; Apparatus for discharge
- B05B7/04—Spray pistols; Apparatus for discharge with arrangements for mixing liquids or other fluent materials before discharge
- B05B7/0408—Spray pistols; Apparatus for discharge with arrangements for mixing liquids or other fluent materials before discharge with arrangements for mixing two or more liquids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0218—Pretreatment, e.g. heating the substrate
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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
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention aims to provide a preparation method of a spray type bi-component composite surface enhanced Raman substrate, belonging to the technical field of Raman substrate preparation. The method comprises the steps of respectively placing a gold nanorod solution and a silicon dioxide dielectric microsphere solution in two centrifuge tubes, controlling the spraying speed of the two substances by controlling the caliber of a spray gun, and distributing the mixture of the two substances on a substrate to be heated and dried to be used as an SERS substrate. The substrate manufacturing method is convenient and rapid, the storage method is simple, the detection limit is low, and the substrate can be produced in a large scale.
Description
Technical Field
The invention belongs to the technical field of Raman substrate preparation, and particularly relates to a preparation method of a spray type bi-component composite surface enhanced Raman substrate.
Background
According to the traditional SERS technology, a nano array composed of gold, silver and other noble metals is used as a detection substrate, when incident light is incident to the surface of gold, silver and other noble metal nano particles at a certain frequency, Local Surface Plasmon Resonance (LSPR) can occur, an electromagnetic field can be greatly enhanced at the position, and the main effect on the SERS effect is achieved. The SERS technology has great potential in various fields as a high-sensitivity vibration spectrum detection technology and an analysis method. However, when the SERS technology is developed to a higher detection limit, the stability and the detection limit of the SERS substrate manufactured by using only the noble metal nano-array are not high enough, so that the actual scene requirements cannot be well met in the actual detection.
In recent years, composite raman substrates composed of metal nanoparticles and dielectric particles have been proved to improve SERS capability, such as Cga, B et al (Preparation of a monolayer array of silicon @ gold core-shell nanoparticles as a SERS substrate-scientific direct. optik 221(2020).) by coating a monolayer structure of gold nanoparticles on the surface of silica microspheres by chemical synthesis method as SERS substrate, and the detection limit of crystal violet is 10 -8 mol/L; chenlizhen et al (one)Preparation method and application of silicon oxide/gold microspheres with surface-enhanced Raman scattering effect) and high-temperature tube furnace are used for preparing silicon oxide/gold microsphere surface-enhanced Raman substrate by spray pyrolysis method, and detection limit of detection object mercaptobenzoic acid is 10 -7 mol/L, but the temperature of the high-temperature tube furnace in the method is higher, the use is dangerous, and the occupied area of the instrument is large; in patent CN202010226998.2, a surface-enhanced raman substrate and a preparation method thereof are disclosed, in the method, a substrate with a surface having noble metal nanoparticles needs to be tilted, and then a dielectric microsphere particle solution is dropped, so as to prepare the raman substrate. However, these methods have disadvantages of complicated operation and low production efficiency, and are not suitable for mass production.
Therefore, how to simply and rapidly prepare the composite raman substrate with high sensitivity is extremely important.
Disclosure of Invention
Aiming at the problems in the background art, the invention aims to provide a preparation method of a spray type bi-component composite surface enhanced Raman substrate. The method comprises the steps of respectively placing a gold nanorod solution and a silicon dioxide dielectric microsphere solution in two centrifuge tubes, controlling the spraying speed of the two substances by controlling the caliber of a spray gun, and distributing the mixture of the two substances on a substrate to be heated and dried to be used as an SERS substrate. The substrate manufacturing method is convenient and rapid, the storage method is simple, the detection limit is low, and the substrate can be produced in a large scale.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a spray type bi-component composite surface enhanced Raman substrate comprises the following steps:
and 3, heating the substrate to 80-110 ℃, uniformly mixing the solution A and the solution B, uniformly spraying the mixture on the surface of the heated substrate, wherein the spraying caliber is 0.3-0.5 mm, the spraying time is 10-30 min, stopping heating the substrate after spraying is finished, and naturally cooling to obtain the enhanced Raman substrate on the surface of the substrate.
Further, the gold nanorods in the step 1 are prepared by adopting a seed growth method.
Further, the substrate is a silicon wafer, quartz, glass or the like.
Further, the volume ratio of ethanol to ethylene glycol in step 2 is 1:1.
The invention also provides a spray gun suitable for the preparation method, which comprises a nozzle, a spray gun body, a feeding pipe and two storage pipes; the device comprises a spray gun body, a nozzle, a feeding pipe and two storage pipes, wherein the nozzle is arranged at the front end of the spray gun body and used for spraying a Raman substrate mixed solution to a substrate to form spray; gold nanorod solution and silicon dioxide dielectric microsphere solution are respectively arranged in the two storage tubes; the gold nanorod solution and the silicon dioxide dielectric microsphere solution are mixed in the feeding pipe and then sprayed by the nozzle to form spray.
Further, the diameter of the nozzle is 0.3 mm-0.5 mm.
The mechanism of the invention is as follows: mixing the gold nanorods with the silicon dioxide dielectric microsphere solution, wherein the solvent is a mixture of water, ethanol and ethylene glycol, and adjusting the surface tension of the solvent so as to regulate the spreading degree of the gold nanorods on the surface of the silicon dioxide, thereby spontaneously forming a single-layer gold nanorod on the surface of the silicon dioxide microsphere; meanwhile, the caliber of the spray gun is controlled, so that the surface of the substrate is deposited in a spray mode, different from a conventional dripping method for preparing the Raman substrate, large liquid drops on the surface of the substrate cannot be dried quickly, and the coffee ring effect can generate agglomerated gold nanorods, so that the final effect of the Raman substrate is directly influenced. In addition, the performance of the finally obtained substrate is regulated and controlled by adjusting the spraying time, and the gold nanorods cannot be uniformly distributed on the substrate due to insufficient spraying time, so that the enhancement effect is weak; if the spraying time is too long, the gold nanorods are easy to form a multilayer structure on the substrate, and a region with uneven thickness is generated, so that the enhancement effect of the SERS substrate is not obvious, and the cost for manufacturing the substrate is increased.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. the preparation method of the invention is not complicated by chemical assembly, template self-assembly and other methods, can simply and quickly form the enhanced Raman substrate on the surface of the substrate, and has the detection sensitivity of 10 -8 mol/L, and meanwhile, the method has high production efficiency and is suitable for large-scale production.
2. The gold nanorod precursor solution and the dielectric microsphere precursor solution in the preparation process can be respectively placed in two storage tubes for storage, so that the gold nanorods are not easy to agglomerate, the interference of other chemical substances is avoided, and the storage time is longer and more stable compared with methods such as chemical self-assembly and the like.
Drawings
FIG. 1 is a pictorial view of a spray gun apparatus of the present invention.
FIG. 2 is an SEM image of gold nanorods with aspect ratio of 3 synthesized by the invention.
FIG. 3 is an SEM image of a gold nanorod-silica microsphere composite structure of the invention.
Fig. 4 is a surface scanning raman detection result chart of embodiment 1 of the present invention.
FIG. 5 is a SERS plot of different concentrations of MDMA detected by the two-component composite structured substrate of the present invention.
FIG. 6 illustrates a SERS substrate 10 with different injection times according to the present invention -3 A Raman diagram of a solution of p-mercaptoaniline in mol/L.
Figure 7 is an SEM image of a two component composite raman substrate prepared using a 0.8mm diameter nozzle of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following embodiments and accompanying drawings.
A preparation method of a spray type bi-component composite surface enhanced Raman substrate comprises the following steps:
and 3, heating the substrate to 80-110 ℃, uniformly mixing the solution A and the solution B, uniformly spraying the mixture on the surface of the heated substrate, wherein the spraying caliber is 0.3-0.5 mm, the spraying time is 10-30 min, stopping heating the substrate after spraying is finished, and naturally cooling to obtain the enhanced Raman substrate on the surface of the substrate.
Example 1
A preparation method of a spray type bi-component composite surface enhanced Raman substrate comprises the following steps:
step 1.1, preparing a gold nanorod seed solution: 0.5mL of chloroauric acid solution with the concentration of 0.5mmol/L is added into 7.5mL of 0.1mol/L CTAB solution at 25 ℃, and the solution is changed from transparent color to light yellow; then 0.8mL of 0.01M sodium borohydride solution in ice bath is added, and the solution turns brown; storing for two hours at 25 ℃ to obtain a seed solution of the gold nanorods;
step 1.2, preparing a gold nanorod growth solution: at 25 ℃, adding 0.8mL of chloroauric acid solution with the concentration of 0.5mmol/L into 9.5mL of 0.1mol/L CTAB solution, and changing the solution from transparent color to light yellow; then, 60 mu L of silver nitrate solution with the concentration of 0.01mol/L and 64 mu L of ascorbic acid solution with the concentration of 0.1mol/L are sequentially added, and the mixture is uniformly stirred until the solution turns colorless; finally, 40 mu L of the seed solution obtained in the step 1.1 is added, and the mixture is kept stand for 2 hours to obtain a growth solution of the gold nanorods with the length-diameter ratio of 3;
step 1.3, taking 2mL of the gold nanorod growth solution obtained in the step 1.2, centrifuging at the rotating speed of 12000r/min for 10min, removing supernatant, adding 2mL of deionized water, and repeating the step twice to remove particles with small particle size and excessive surfactant CTAB; placing the centrifuged gold nanorod solution into a centrifugal tube;
the SEM image of the synthesized gold nanorods is shown in FIG. 2; the gold nanorods have uniform appearance and good dispersibility;
step 3, installing a spray gun, wherein the spray gun is shown in a real object diagram in fig. 1 and comprises a spray nozzle, a spray gun body, a feeding pipe and two storage pipes, wherein the two storage pipes are centrifugal pipes, the two centrifugal pipes are fixedly connected with the feeding pipe through a three-way pipe, and the spray nozzle is aligned to clean glass soaked by using a piranha solution (concentrated sulfuric acid: hydrogen peroxide: 7: 3); the diameter of the nozzle is 0.3mm, the spraying speed is small, the spraying time is 30 minutes, and the SERS substrate can be obtained on the glass until the color of the substrate is light yellow.
An SEM image of the gold nanorod-silica microsphere composite raman substrate obtained on the glass substrate in this example is shown in fig. 3. As can be seen from the figure, the coverage rate of the gold nanorods on the surface of the silicon dioxide dielectric microsphere is high, the gold nanorods which are hardly agglomerated are on the surface of the silicon dioxide dielectric microsphere, and the coverage rates of the surfaces of different silicon dioxide dielectric microspheres are approximately the same.
Soaking the obtained SERS substrate in 10 -3 And (3) in the p-mercaptoaniline to be detected in mol/L, after half an hour, washing off the redundant p-mercaptoaniline solution on the substrate by using ethanol, and detecting the substrate under the excitation wavelength of 785 nm.
The substrate was scanned area-by-area using confocal raman spectroscopy, with the accumulation time of 0.5s and the spacing between each spot taken being 2 μm, as shown in the inset of fig. 4. The resulting SERS spectrum is shown in FIG. 4, and it was determined by Lorentzian fitting that p-mercaptoaniline was 1077cm -1 The peak height is higher, the SERS intensity is from strong to weak according to the depth of gray level,the white area has the strongest signal and the black area has the weakest signal. According to the signal intensity and the actual scanning area, the SERS signal of the mixed area containing silicon dioxide is far higher than that of the area of the pure gold nanorod.
Example 2
To explore the utility of the device, the detection of 3, 4-methylenedioxymethamphetamine (MDMA) using the hybrid substrate was chosen. MDMA solutions were prepared at concentrations of 10nM, 100nM, 1. mu.M, 10. mu.M and 100. mu.M, respectively, with ethanol as the solvent. And (3) after the substrate is manufactured, soaking the substrate in a corresponding solvent, washing the soaked substrate with ethanol after half an hour, and performing an SERS test after natural drying. In order to achieve accuracy of results, 5 different places are selected for corresponding regions of the SERS substrate to collect signals, and Raman spectrums of the SERS substrate are average levels of Raman spectrums of the SERS substrates in different regions.
The SERS spectrum obtained from the test of this example is shown in fig. 5. As can be seen from the figure, the detection limit of MDMA of the Raman enhanced substrate of the invention can reach 10 nM.
Comparative example 1
The gold nanorod-silica microsphere composite raman substrate was prepared according to the procedure of example 1, with the spraying time adjusted to 5min and 40min only, and the rest was unchanged. The prepared raman substrate was also used for detection 10 -3 The SERS spectrum of the solution to be detected for mol/L p-mercaptoaniline is shown in FIG. 6.
As can be seen from fig. 6, the raman substrates obtained by spraying for 30min in example 1 and 40min in comparative example 1 have the same peak intensity after the background is subtracted, so that the longer the spraying time exceeds 30min, the less the enhancement effect of the SERS substrate is, and the cost for manufacturing the substrate is increased; and if the time is too short, the enhancement effect of the Raman substrate is weaker, and the purpose of application cannot be achieved.
Comparative example 2
The gold nanorod-silica microsphere composite raman substrate was prepared according to the procedure of example 1, with only the nozzle diameter adjusted to 0.8mm, and the rest unchanged. The SEM of the prepared raman substrate is shown in fig. 7. When the diameter of the nozzle is 0.8mm, the gold nanorods on the surface of the silicon dioxide can be blown away due to overlarge area of the sprayed liquid drop and overlarge nozzle, so that the gold nanorods cannot be dried and deposited on the silicon dioxide microspheres quickly; when a nozzle with the diameter of 0.3mm is used, as shown in fig. 3, the quantity of the gold nanorods on the surface of the silicon dioxide is far higher than that of the nozzle with the diameter of 0.8mm, and the SERS enhancement effect of the substrate is better.
Experiments prove that when the aperture exceeds 0.5mm, a large liquid drop area can be generated on the substrate, so that the large liquid drop cannot be dried quickly, and the coffee ring effect can generate agglomerated gold nanorods, thereby affecting the detection capability of the Raman substrate.
While the invention has been described with reference to specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise; all of the disclosed features, or all of the method or process steps, may be combined in any combination, except mutually exclusive features and/or steps.
Claims (7)
1. A preparation method of a spray type bi-component composite surface enhanced Raman substrate is characterized by comprising the following steps:
step 1, dispersing the centrifuged gold nanorods in deionized water to obtain a solution A, wherein the concentration of the gold nanorods in the solution A is 0.3-0.5 g/mL;
step 2, dispersing the silicon dioxide dielectric microspheres in a mixed solution of ethanol and ethylene glycol to obtain a solution B, wherein the concentration of the silicon dioxide dielectric microspheres in the solution B is 0.025-0.05 g/mL;
and 3, heating the substrate to 80-110 ℃, uniformly mixing the solution A and the solution B, uniformly spraying the mixture on the surface of the heated substrate, wherein the spraying caliber is 0.3-0.5 mm, the spraying time is 10-30 min, stopping heating the substrate after spraying is finished, and naturally cooling to obtain the enhanced Raman substrate on the surface of the substrate.
2. The method for preparing the spray-type two-component composite surface-enhanced Raman substrate according to claim 1, wherein the gold nanorods in step 1 are prepared by a seed growth method.
3. The method for preparing the spray-type two-component composite surface-enhanced Raman substrate according to claim 1, wherein the substrate is a silicon wafer, quartz or glass.
4. The method for preparing the spray-type two-component composite surface enhanced Raman substrate according to claim 1, wherein the volume ratio of ethanol to ethylene glycol in step 2 is 1:1.
5. A spray gun suitable for use in the method of any one of claims 1 to 4, comprising a nozzle, a spray gun body, a feed pipe and two stock pipes; the spray gun comprises a spray gun body, a spray nozzle, a feed pipe and two storage pipes, wherein the spray nozzle is arranged at the front end of the spray gun body and used for spraying a Raman substrate mixed solution to a substrate to form spray; gold nanorod solution and silicon dioxide dielectric microsphere solution are respectively arranged in the two storage tubes.
6. The spray gun of claim 5, wherein the gold nanorod solution and the silicon dioxide dielectric microsphere solution are mixed in the feeding pipe and then sprayed from the nozzle to form a spray to be deposited on the surface of the substrate.
7. A lance as claimed in claim 5, in which the nozzle diameter is in the range 0.3mm to 0.5 mm.
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