CN112342498B - Preparation method and application of silicon nanoparticle-water-soluble polymer film with Raman internal standard - Google Patents
Preparation method and application of silicon nanoparticle-water-soluble polymer film with Raman internal standard Download PDFInfo
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- CN112342498B CN112342498B CN202010944765.6A CN202010944765A CN112342498B CN 112342498 B CN112342498 B CN 112342498B CN 202010944765 A CN202010944765 A CN 202010944765A CN 112342498 B CN112342498 B CN 112342498B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/20—Metallic material, boron or silicon on organic substrates
- C23C14/205—Metallic material, boron or silicon on organic substrates by cathodic sputtering
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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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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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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
Abstract
The invention discloses a preparation method and application of a silicon nanoparticle-water-soluble polymer film with Raman internal standard, which is characterized by comprising the following steps: mixing 1 ml of 5-15 mg per ml of sodium carboxymethyl cellulose aqueous solution and 1 ml of 2-6 mg per ml of silicon nanoparticle aqueous solution by ultrasonic treatment for 10 minutes to fully and uniformly mix the aqueous solution; then dripping the solution on the surface of a clean silicon wafer, placing the silicon wafer at room temperature to naturally dry the silicon wafer into a film, placing the film in a magnetron sputtering machine, sputtering the film for 10 to 40 seconds under the power of 40 watts, and finally uncovering the film from the silicon wafer to obtain the silicon nanoparticle-sodium carboxymethyl cellulose film material.
Description
Technical Field
The invention relates to the field of material engineering and nanotechnology, in particular to a preparation method and application of a silicon nanoparticle-water-soluble polymer film with a Raman internal standard.
Background
Due to the rapid development of surface plasmon resonance technology, surface enhanced raman spectroscopy has become a powerful analytical tool in chemistry, physics, and bioscience and has enabled the detection of trace substances, including pesticide and veterinary drug residues, environmental hormones, heavy metal ions, and the like. On one hand, people introduce a flexible polymer film as a Raman substrate, so that in-situ detection is convenient to realize. However, due to the unstable characteristic of the flexible substrate, the flexible substrate has natural defects in the aspects of realizing quantitative detection and improving detection recovery rate.
On the other hand, the molecules or substances with intrinsic Raman signals are introduced into the Raman substrate, so that the deviation of the molecular signals to be detected can be corrected, and the purpose of quantitative detection is realized, for example, a core-shell structure is designed to wrap the internal standard Raman molecules, and the substrate materials with intrinsic Raman signals, such as graphene, are utilized. However, the core-shell material is difficult to prepare, the Raman signal intensity of the graphene is low, and the graphene is easily covered by a molecular signal to be detected.
In addition, people also often adopt a silicon wafer as a Raman internal standard, but the intensity of the silicon wafer is difficult to adjust, and the silicon wafer is not suitable for different detection molecules and detection environments. Similar to silicon wafers, silicon nanoparticles also have a strong raman signal. Meanwhile, the silicon nanoparticles have good water solubility, are easy to disperse, are stable and cheap, and are easy to prepare the flexible substrate with the Raman internal standard by a spin-coating drying method after being simply mixed in a water solution according to a proportion. At present, silicon nanoparticles are introduced into a flexible substrate to serve as a Raman internal standard, and no relevant report is found in a method for realizing quantitative detection.
Disclosure of Invention
The invention aims to provide a preparation method and application of a silicon nanoparticle-water-soluble polymer film with a Raman internal standard, which can improve the sensitivity and the accuracy of quantitative detection.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a silicon nanoparticle-water-soluble polymer film with a Raman internal standard comprises the following steps:
(1) Mixing 1 ml of 5-15 mg per ml of water-soluble polymer aqueous solution and 1 ml of 2-6 mg per ml of silicon nanoparticle aqueous solution for 10 minutes by ultrasonic treatment, and fully and uniformly mixing to obtain a mixed solution;
(2) And (2) dripping 20 microliters of the mixed solution obtained in the step (1) on the surface of a clean silicon wafer, placing the silicon wafer at room temperature to naturally dry the silicon wafer into a film, placing the silicon wafer coated with the silicon nanoparticles and the water-soluble polymer film in a magnetron sputtering machine as a substrate, installing a silver target in a magnetron radio-frequency sputtering target, controlling the sputtering power to be 40W, sputtering for 10-40 seconds at room temperature, and then uncovering the sputtered sample from the silicon wafer to obtain the silicon nanoparticle-water-soluble polymer film with the Raman internal standard.
The water-soluble polymer is any one of sodium carboxymethylcellulose, methylcellulose, ethyl cellulose, hydroxyethyl cellulose, polyvinylpyrrolidone, polyvinyl alcohol, polymaleic anhydride, polyquaternary ammonium salt and polyethylene glycol.
A quantitative detection method utilizing the silicon nanoparticle-water-soluble polymer film with the Raman internal standard comprises the following steps: attaching the prepared silicon nanoparticle-water-soluble polymer film with the Raman internal standard to the surface of fruits and vegetables adsorbed by molecules to be detected, incubating for 30 minutes, and finally irradiating laser to the surface of the fruits and vegetables through the film to realize in-situ detection of the Raman molecules.
Compared with the prior art, the invention has the advantages that: the preparation method and the application of the silicon nanoparticle-water-soluble polymer film with the Raman internal standard are mainly based on physical mixing and sputtering, the preparation process is simple, the yield is high, and due to the transparency and flexibility of the sodium carboxymethyl cellulose film, the collection and in-situ detection of Raman molecules to be detected can be realized. Meanwhile, the introduced silicon nanoparticles have intrinsic Raman peaks under 520 wave numbers and can be used as internal standards to eliminate the interference of environmental factors in the detection process, particularly, the silicon nanoparticles and the sodium carboxymethyl cellulose have good solubility and dispersibility in an aqueous solution, so that the silicon nanoparticles and the sodium carboxymethyl cellulose can be uniformly mixed, the silicon nanoparticles in the finally obtained sodium carboxymethyl cellulose film are uniformly distributed, the prepared Raman flexible substrate has uniform Raman internal standard signals, and the reliable realization of quantitative detection is facilitated.
Drawings
FIG. 1 is a scanning electron micrograph of silicon nanoparticles according to example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of a silicon nanoparticle-sodium carboxymethylcellulose film with Raman internal standard prepared in example 1 of the present invention;
fig. 3 shows the detection results of the silicon nanoparticle-water-soluble polymer film with the raman internal standard prepared in example 1 of the present invention for raman molecules with different concentrations and the linear fitting results based on the signal of the silicon nanoparticle internal standard;
FIG. 4 is a flow chart of a method for quantitative detection of a silicon nanoparticle-water-soluble polymer film with a Raman internal standard;
fig. 5 shows the detection results of the silicon nanoparticle-water-soluble polymer film with the raman internal standard prepared in example 2 of the present invention for raman molecules with different concentrations and the linear fitting results based on the signal of the silicon nanoparticle internal standard;
fig. 6 shows the detection results of the silicon nanoparticle-water-soluble polymer film with the raman internal standard prepared in example 3 of the present invention for raman molecules with different concentrations and the linear fitting results based on the signal of the silicon nanoparticle internal standard;
FIG. 7 shows the detection results of silicon wafer sputtered silver on Raman molecules of different concentrations and the linear fitting results based on silicon wafer internal standard signals;
FIG. 8 is a Raman spectrum of 50wt%, 60wt%, 70wt%, 80wt% silicon nanoparticles doped in a sodium carboxymethyl cellulose film, respectively.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, and the raw materials used are commercially available products.
Example 1
A preparation method of a silicon nanoparticle-water-soluble polymer film with a Raman internal standard comprises the following steps:
firstly, mixing 1 ml of 5 mg/ml sodium carboxymethylcellulose aqueous solution and 1 ml of 2 mg/ml silicon nanoparticle aqueous solution for 10 minutes by ultrasonic treatment to fully and uniformly mix the two solutions; and secondly, dripping 20 microliters of mixed solution of silicon nanoparticles and sodium carboxymethylcellulose on the surface of a clean silicon wafer, and naturally drying the silicon wafer at room temperature to form a film. Then, the silicon wafer coated with the silicon nanoparticles and the sodium carboxymethylcellulose film was placed in a magnetron sputtering machine as a substrate, and a silver target was mounted in a magnetron rf sputtering target and sputtered at a power of 40 watts for 10 seconds. And finally, uncovering the sputtered sample from the silicon wafer to obtain the silicon nanoparticle-sodium carboxymethyl cellulose film with the Raman internal standard.
Fig. 1 shows a scanning electron microscope photograph of the silicon nanoparticles in the present example. As can be seen from fig. 1, the silicon nanoparticles are better dispersed.
Figure 2 shows a scanning electron micrograph of the silicon nanoparticle-sodium carboxymethylcellulose film with raman internal standard prepared in this example. As can be seen from FIG. 2, the prepared silicon nanoparticle-sodium carboxymethylcellulose thin film has a flat surface, and is uniformly coated with magnetron-sputtered silver particles.
Fig. 3 shows raman detection results obtained by using the silicon nanoparticle-sodium carboxymethyl cellulose film with the raman internal standard prepared in example 1 of the present invention. Dripping 20 microliter of the molecule-ethanol solution to be detected with different concentrations on the surface of fruits and vegetables such as apples. After the film is naturally dried, the silicon nanoparticle-water-soluble polymer film with the raman internal standard prepared in the embodiment 1 is attached to the surface of fruits and vegetables such as apples to be tested, and the fruits and vegetables are adsorbed by molecules to be tested, and the mixture is incubated for 30 minutes. Finally, laser is irradiated to the surface of the apple through the film to realize the in-situ detection of the Raman molecules (the detection process is shown in figure 4). As can be seen from FIG. 3, dividing the Raman intensity of the molecule to be detected by the Raman peak intensity of the silicon nanoparticles at 520 wavenumbers can increase the linear correlation coefficient between the Raman signal intensity and the concentration of the molecule to be detected from 0.957 to 0.996, and the detection limit can reach 10 -9 Millimoles per ml.
Example 2
A preparation method of a silicon nanoparticle-water-soluble polymer film with a Raman internal standard comprises the following steps:
firstly, mixing 1 ml of 10 mg/ml sodium carboxymethylcellulose aqueous solution and 1 ml of 4 mg/ml silicon nanoparticle aqueous solution for 10 minutes by ultrasonic treatment, and fully and uniformly mixing; secondly, dripping 20 microliters of mixed solution of silicon nanoparticles and sodium carboxymethylcellulose on the surface of a clean silicon wafer, and naturally drying the silicon wafer to form a film at room temperature; then, the silicon wafer coated with the silicon nanoparticles and the sodium carboxymethylcellulose film was placed in a magnetron sputtering machine as a substrate, and a silver target was mounted in a magnetron rf sputtering target and sputtered at a power of 40 watts for 20 seconds. And finally, uncovering the sputtered sample from the silicon wafer to obtain the silicon nanoparticle-sodium carboxymethyl cellulose thin film material.
Fig. 5 shows raman detection results obtained by using the silicon nanoparticle-sodium carboxymethyl cellulose film with the raman internal standard prepared in example 1 of the present invention. Dripping 20 microliter of the molecule-ethanol solution to be detected with different concentrations on the surface of fruits and vegetables such as apples. And after the film is naturally dried, attaching the silicon nanoparticle-water-soluble polymer film with the Raman internal standard prepared in the embodiment 2 to the surface of fruits and vegetables such as apples adsorbed by molecules to be detected, and incubating for 30 minutes. And finally, irradiating laser to the surface of the apple through the film to realize the in-situ detection of Raman molecules. As can be seen from FIG. 5, dividing the Raman intensity of the molecule to be detected by the Raman peak intensity of the silicon nanoparticles at 520 wavenumbers can increase the linear correlation coefficient between the Raman signal intensity and the concentration of the molecule to be detected from 0.939 to 0.981, and the detection limit can reach 10 -9 Millimoles per ml.
Example 3
A preparation method of a silicon nanoparticle-water-soluble polymer film with a Raman internal standard comprises the following steps: firstly, mixing 1 ml of 15 mg/ml sodium carboxymethylcellulose aqueous solution and 1 ml of 6 mg/ml silicon nanoparticle aqueous solution for 10 minutes by ultrasonic waves, and fully and uniformly mixing; secondly, dripping 20 microliters of mixed solution of silicon nanoparticles and sodium carboxymethylcellulose on the surface of a clean silicon wafer, and naturally drying the silicon wafer to form a film at room temperature; then, the silicon wafer coated with the silicon nanoparticles and the sodium carboxymethylcellulose film was placed in a magnetron sputtering machine as a substrate, and a silver target was mounted in a magnetron rf sputtering target and sputtered at a power of 40 watts for 40 seconds. And finally, uncovering the sputtered sample from the silicon wafer to obtain the silicon nanoparticle-sodium carboxymethyl cellulose thin film material.
FIG. 6 shows silicon nanoparticles with Raman internal standard prepared in example 1 of the present inventionAnd Raman detection results obtained by the granular-sodium carboxymethylcellulose film. Dripping 20 microliter of the molecule-ethanol solution to be detected with different concentrations on the surface of fruits and vegetables such as apples. After the film is naturally dried, the silicon nanoparticle-water-soluble polymer film with the raman internal standard prepared in the embodiment 1 is attached to the surface of fruits and vegetables such as apples to be tested, and the fruits and vegetables are adsorbed by molecules to be tested, and the mixture is incubated for 30 minutes. And finally, irradiating laser to the surface of the apple through the film to realize the in-situ detection of Raman molecules. As can be seen from FIG. 6, dividing the Raman intensity of the molecule to be detected by the Raman peak intensity of the silicon nanoparticles at 520 wavenumbers increases the linear correlation coefficient between the Raman signal intensity and the concentration of the molecule to be detected from 0.966 to 0.988, and the detection limit can reach 10 -9 Millimoles per ml.
From the above results, if the silicon nanoparticle internal standard is not used, the linear correlation coefficient is only between 0.939 and 0.966, the linearity degree is low, and the quantitative detection is difficult to realize. The linear correlation coefficient after the Raman internal standard is adopted for correction can reach 0.981-0.996, the linearity degree is obviously improved, and the method can be used for actual quantitative detection.
Meanwhile, as shown in fig. 7, the raman signal of the silicon wafer with sputtered silver is used as the internal standard detection result, and the raman intensity of the molecule to be detected is divided by the raman peak intensity of the silicon wafer at the position of 520 wave numbers, so that the linear correlation coefficient between the raman signal intensity and the concentration of the molecule to be detected is only increased from 0.922 to 0.956, and the detection limit is only 10 -5 Millimoles per ml. The comparison result fully reflects the advantages of adding the silicon nanoparticles into the flexible substrate as an internal standard in the aspects of reducing the detection limit and improving the linearity degree. In addition, as is apparent from fig. 8, the silicon nanoparticles are used as a source of the raman internal standard, the raman intensity of the raman internal standard can be controllably adjusted by adjusting the doping ratio of the silicon nanoparticles in the carboxymethyl cellulose, and the intensity of the silicon internal standard can be flexibly changed according to the specific requirements of different specific application fields, which is incomparable with the silicon wafer internal standard signal with fixed intensity.
The above description is not intended to limit the present invention, and the present invention is not limited to the above examples. Those skilled in the art should also realize that changes, modifications, additions and substitutions can be made without departing from the true spirit and scope of the invention.
Claims (3)
1. A preparation method of a silicon nanoparticle-water-soluble polymer film with a Raman internal standard is characterized by comprising the following steps:
(1) Mixing 1 ml of 5-15 mg per ml of water-soluble polymer aqueous solution and 1 ml of 2-6 mg per ml of silicon nanoparticle aqueous solution for 10 minutes by ultrasonic treatment, and fully and uniformly mixing to obtain a mixed solution;
(2) And (2) dripping 20 microliters of the mixed solution obtained in the step (1) on the surface of a clean silicon wafer, placing the silicon wafer at room temperature to naturally dry the silicon wafer into a film, placing the silicon wafer coated with the silicon nanoparticles and the water-soluble polymer film in a magnetron sputtering machine to serve as a substrate, installing a silver target in a magnetron radio frequency sputtering target, controlling the sputtering power to be 40W, sputtering for 10-40 seconds at room temperature, and then uncovering the sputtered sample from the silicon wafer to obtain the silicon nanoparticle-water-soluble polymer film with the Raman internal standard.
2. The method of claim 1, wherein the method comprises the following steps: the water-soluble polymer is any one of sodium carboxymethylcellulose, methylcellulose, ethyl cellulose, hydroxyethyl cellulose, polyvinylpyrrolidone, polyvinyl alcohol, polymaleic anhydride, polyquaternary ammonium salt and polyethylene glycol.
3. A quantitative detection method using the silicon nanoparticle-water-soluble polymer film with raman internal standard according to any one of claims 1-2, characterized by comprising the following steps: attaching the prepared silicon nanoparticle-water-soluble polymer film with the Raman internal standard to the surface of fruits and vegetables adsorbed by molecules to be detected, incubating for 30 minutes, and finally irradiating laser to the surface of the fruits and vegetables through the film to realize in-situ detection of the Raman molecules.
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| CN101221130A (en) * | 2008-01-28 | 2008-07-16 | 郑州大学 | Production method for surface reinforced Raman scattering active substrate based on silicon nano hole column array |
| CN101672786B (en) * | 2009-03-12 | 2011-04-06 | 中国科学院理化技术研究所 | Active substrate with surface provided with enhanced raman scattering effect and production method and application thereof |
| CN101614668B (en) * | 2009-07-22 | 2011-01-12 | 中国科学院理化技术研究所 | Silicon nanowire sensor based on surface enhanced Raman scattering effect and application thereof |
| KR101448111B1 (en) * | 2013-09-17 | 2014-10-13 | 한국기계연구원 | A substrate for surface-enhanced Raman scattering spectroscopy and a preparing method thereof |
| GB201418483D0 (en) * | 2014-10-17 | 2014-12-03 | Johnson Matthey Plc | Analytical method and composition |
| CN104677881B (en) * | 2015-03-26 | 2017-11-10 | 厦门大学 | A kind of core-shell structure nanometer particle and surface-enhanced Raman quantitative detecting method of interior containing the internal standard molecule |
| CN107064107B (en) * | 2017-04-11 | 2019-11-19 | 中山大学 | A kind of super hydrophobic surface enhancing Raman substrate and preparation method thereof using the preparation of silicon nanometer dielectric material |
| US11002682B2 (en) * | 2018-03-12 | 2021-05-11 | Ondavia, Inc. | Aldehyde detection and analysis using surface-enhanced Raman spectroscopy |
| CN109060762B (en) * | 2018-07-27 | 2022-02-08 | 山东师范大学 | Composite flexible surface enhanced Raman substrate based on silver nanoparticles and preparation method thereof |
| CN110658176B (en) * | 2019-09-04 | 2021-10-29 | 宁波工程学院 | Functional sand paper of silicon dioxide nano-star composite material and preparation method thereof |
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