CN111830005A - Detection method of chip Raman signal - Google Patents
Detection method of chip Raman signal Download PDFInfo
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- CN111830005A CN111830005A CN201910314129.2A CN201910314129A CN111830005A CN 111830005 A CN111830005 A CN 111830005A CN 201910314129 A CN201910314129 A CN 201910314129A CN 111830005 A CN111830005 A CN 111830005A
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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 relates to the technical field of laser Raman detection, in particular to a detection method of a chip Raman signal, which comprises the steps of forming a hydrophobic layer comprising a hydrophobic solution on the surface of a chip to be detected, dripping the solution to be detected on the hydrophobic layer, detecting the chip to be detected with the dripped solution to be detected through a Raman detector, and obtaining the Raman signal of the chip to be detected.
Description
Technical Field
The invention relates to the technical field of laser Raman detection, in particular to a detection method of a chip Raman signal
Background
In 1974, Fleischmann et al obtain Raman spectra of high-quality pyridine molecules on the surface of a rough silver electrode, and in 1977, Van Duyne et al experimentally and theoretically calculate that the Raman scattering signals of the pyridine molecules adsorbed on the rough silver surface are about 6 orders of magnitude stronger than those in a solution, which is called a surface-enhanced Raman scattering effect. The surface enhanced raman Scattering Effect (SERS) is like a magnifying glass, which amplifies weak raman signals to be detected by us.
Therefore, SERS becomes an important analysis means, and has a great application prospect in the fields of material science, surface catalysis, environmental detection, food safety, biomedicine and the like.
Surface-enhanced Raman scattering (SERS) is mainly an abnormal optical enhancement phenomenon on a nanoscale rough metal Surface or a particle system, and can amplify a Raman signal of a molecule adsorbed on the Surface of a substrate structure by about 106-1014And some can even realize single-molecule detection.
In recent years, in SERS research, researchers have focused on preparing controllable, repeatable, hot spot concentrated, mass producible SERS substrates. In the three-dimensional nanostructure, the liquid to be measured has uneven concentration distribution on the surface of the three-dimensional nanostructure, and when the raman signal is detected, the detection sensitivity is reduced due to the uneven concentration distribution on the surface of the three-dimensional nanostructure, so that the enhanced raman signal is obtained by measuring sometimes, and the raman signal cannot be measured sometimes, thereby causing measurement errors.
Therefore, how to avoid the measurement error caused by the non-uniform solubility of the solution to be measured on the surface of the chip is an urgent technical problem to be solved at present.
Disclosure of Invention
In view of the above, the present invention has been made to provide a method for detecting a chip raman signal that overcomes or at least partially solves the above problems.
The embodiment of the invention provides a detection method of a chip Raman signal, which comprises the following steps:
forming a hydrophobic layer comprising a hydrophobic solution on the surface of a chip to be detected;
dropwise adding a solution to be detected on the hydrophobic layer;
and detecting the chip to be detected dropwise with the solution to be detected by using a Raman detector to obtain a Raman signal of the chip to be detected.
Further, the hydrophobic solution is specifically any one of the following solutions:
n-dodecyl mercaptan, ethyl orthosilicate, methyl orthosilicate, and polysilazane.
Further, the concentration of the hydrophobic solution is specifically 0.01 mol/L-0.1 mol/L.
Further, the forming of the hydrophobic layer including the hydrophobic solution on the surface of the chip to be detected specifically includes:
and soaking the chip to be detected in the hydrophobic solution for 24-48 h, and taking out the chip to be detected to form a hydrophobic layer comprising the hydrophobic solution on the surface of the chip to be detected.
Further, the substrate of the chip to be detected specifically adopts any one of the following materials:
silicon, silicon dioxide, black silicon, a porous alumina template, titanium dioxide, graphene, non-woven fabric, polymethyl methacrylate and adhesive tape.
Further, metal nano particles and/or metal nano wires are deposited on the substrate of the chip to be detected.
Further, the metal nanoparticles are specifically single metal nanoparticles and/or alloy nanoparticles;
the single metal nano-particle is specifically a gold nano-particle, a silver nano-particle or a copper nano-particle;
the alloy nanoparticles comprise at least two metals of gold, silver and copper;
the metal nanowire is specifically a gold nanowire, a copper nanowire or a silver nanowire.
Further, the shape of the metal nanoparticles is specifically any one of the following:
star, hexagon, and circle.
Further, the solution to be detected is specifically any one of the following solutions:
R6G solution, malachite green solution, and methylene blue solution.
Further, after the solution to be tested is dripped on the hydrophobic layer, the method further comprises the following steps: and drying the chip to be detected after waiting for 10-30 min.
One or more technical solutions in the embodiments of the present invention have at least the following technical effects or advantages:
the invention provides a detection method of a chip Raman signal, which comprises the steps of forming a hydrophobic layer comprising a hydrophobic solution on the surface of a chip to be detected, dripping the solution to be detected on the hydrophobic layer, detecting the chip to be detected on which the solution to be detected is dripped by a Raman detector to obtain the Raman signal of the chip to be detected.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a schematic diagram showing a prior art process of dropping a solution to be tested on a surface of a chip to be tested;
FIG. 2 is a schematic diagram showing the concentration of a solution to be measured after the solution to be measured is dripped on the surface of a chip to be measured in the prior art;
FIG. 3 is a schematic diagram showing the detection of Raman signals after a solution to be detected is dropped on the surface of a chip to be detected in the prior art;
FIG. 4 is a flow chart illustrating steps of a method for detecting a chip Raman signal according to an embodiment of the present invention;
FIG. 5 is a schematic diagram showing the chip surface to be tested formed after dropping the solution to be tested in the embodiment of the present invention.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
The raman scattering effect is a very weak process, typically with an intensity of only about 10 of the incident intensity-10Therefore, the raman signal is weak and cannot be directly detected by the raman detector.
In the prior art, a raman signal is enhanced by dripping a solution to be detected on the surface of a chip to be detected, specifically, an R6G solution is dripped on the surface of the chip to be detected, and molecules of the solution are gathered on the surface of the chip, so that the raman signal is improved. However, due to the tension effect of water in the R6G solution, a structure as shown in fig. 1 is formed, as can be seen from fig. 1, a contact angle smaller than 90 degrees is formed between the solution to be detected and the surface of the chip to be detected, as shown in fig. 2 and fig. 3, the solution concentrations at the edge 201 and the central position 202 of the solution to be detected are different, the solubility at the edge 201 of the solution to be detected is higher, and the concentration at the central position 202 is lower, when a raman signal of the chip to be detected is detected by using a raman detector, because the solution concentration directly affects the intensity of the raman signal, the detected raman signal has a plurality of measurement results, as shown in fig. 3, the intensity of the raman signal at the edge 201 of the solution to be detected is strong, and the intensity of the raman signal at the central position 202 of the solution to.
In order to solve the above technical problem, an embodiment of the present invention provides a method for detecting a chip raman signal, as shown in fig. 4, including: s401, forming a hydrophobic layer comprising a hydrophobic solution on the surface of a chip to be detected; s402, dropwise adding the solution to be detected on the hydrophobic layer; and S403, detecting the chip to be detected, to which the solution to be detected is dripped, by using a Raman detector to obtain a Raman signal of the chip to be detected.
In S401, specifically, the chip to be detected is soaked in the hydrophobic solution and then taken out, and a hydrophobic layer including the hydrophobic solution is formed on the surface of the chip to be detected.
In an alternative embodiment, the hydrophobic solution is specifically any one of the following: n-dodecyl mercaptan, ethyl orthosilicate, methyl orthosilicate, and polysilazane.
Specifically, the hydrophobic solution may be used to directly soak the chip to be detected, or may be used to dilute the hydrophobic solution and then soak the chip to be detected, and the diluted hydrophobic solution may be selected in consideration of effective utilization of resources. When the hydrophobic solution is diluted, the hydrophobic solution can be diluted by any one of the following solutions, including: methanol, ethanol, acetone, benzene and ethyl acetate, although not limited to these solutions.
The concentration of the diluted hydrophobic solution is specifically 0.01mol/L to 0.1mol/L, and specifically may be 0.01mol/L, 0.05mol/L or 0.1 mol/L.
Taking out the chip to be detected after soaking the chip in the hydrophobic solution, and the method specifically comprises the following steps: soaking the chip to be detected in hydrophobic solution for 24-48 h. The formation of the hydrophobic layer on the surface of the chip to be detected is facilitated by the long-time soaking.
After the hydrophobic layer is formed on the surface of the chip to be detected, the tension of the solution to be detected can be improved, as shown in fig. 5. Comparing the contact angle theta of the solution to be tested and the surface of the chip to be tested (here, the hydrophobic layer) in fig. 5 with the contact angle theta in fig. 1, it can be seen that the contact angle increases after the hydrophobic layer is formed on the surface of the chip to be tested. The tension of the liquid dropped on the hydrophobic layer is improved, so that the uniformity of the concentration of the solution to be measured dropped on the hydrophobic layer can be improved.
Next, S402 is performed, and the solution to be tested is dropped on the hydrophobic layer.
The solution to be detected is specifically any one of the following solutions: R6G solution, malachite green solution, and methylene blue solution. The concentration of the solution to be detected is 10-5M, the concentration is not particularly limited.
After the solution to be detected is dripped on the hydrophobic layer, the method further comprises the following steps: and after waiting for 10-30 min, drying the chip to be detected, wherein natural air drying or nitrogen blow drying can be specifically adopted.
And finally, S403 is executed, the chip to be detected, to which the solution to be detected is dripped, is detected through a Raman detector, and a Raman signal of the chip to be detected is obtained.
When the Raman detector detects a Raman signal, laser with the incident wavelength of 532nm is adopted to irradiate the surface of the chip to be detected, a scattered Raman spectrum is detected, and an enhanced Raman signal is obtained.
Besides the above-mentioned improvement of the tension of the solution to be detected by forming the hydrophobic layer on the surface of the chip to be detected after soaking the chip to be detected in the hydrophobic solution, the tension of the solution to be detected can also be improved by changing the chip to be detected with the three-dimensional nanostructure.
Specifically, the substrate of the chip to be detected specifically adopts any one of the following materials: silicon, silicon dioxide, black silicon, a porous alumina template, titanium dioxide, graphene, non-woven fabric, polymethyl methacrylate and adhesive tape. The present invention is not limited to the above materials.
And depositing metal nano particles and/or metal nano wires on the substrate of the chip to be detected to form a three-dimensional nano structure. The three-dimensional nanostructures may also improve the tonicity of the solution.
The metal nanoparticles are specifically single metal nanoparticles and/or alloy nanoparticles. The single metal nanoparticle is specifically a gold nanoparticle, a silver nanoparticle, or a copper nanoparticle. The alloy nanoparticles comprise at least two metals of gold, silver and copper. The metal nanowire is specifically a gold nanowire, a copper nanowire or a silver nanowire. Of course, it is not limited to the three-dimensional nanostructures described above.
Wherein the shape of the metal nano-particle is specifically any one of the following: star, hexagon, and circle. Of course, the shape is not limited to the above, and patterns and the like may be used.
Therefore, the chip to be detected with the three-dimensional nanostructure is taken out after being soaked in the hydrophobic solution, so that the tension of the solution to be detected can be improved, and the solution uniformity of the solution to be detected after the chip to be detected is dripped can be improved.
One or more technical solutions in the embodiments of the present invention have at least the following technical effects or advantages:
the invention provides a detection method of a chip Raman signal, which comprises the steps of forming a hydrophobic layer comprising a hydrophobic solution on the surface of a chip to be detected, dripping the solution to be detected on the hydrophobic layer, detecting the chip to be detected on which the solution to be detected is dripped by a Raman detector to obtain the Raman signal of the chip to be detected.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A method for detecting a chip Raman signal, comprising:
forming a hydrophobic layer comprising a hydrophobic solution on the surface of a chip to be detected;
dropwise adding a solution to be detected on the hydrophobic layer;
and detecting the chip to be detected dropwise with the solution to be detected by using a Raman detector to obtain a Raman signal of the chip to be detected.
2. The method of claim 1, wherein the hydrophobic solution is specifically any one of:
n-dodecyl mercaptan, ethyl orthosilicate, methyl orthosilicate, and polysilazane.
3. The method according to claim 1, wherein the concentration of the hydrophobic solution is in particular between 0.01mol/L and 0.1 mol/L.
4. The method according to claim 1, wherein forming a hydrophobic layer comprising a hydrophobic solution on the surface of the chip to be detected comprises:
and soaking the chip to be detected in the hydrophobic solution for 24-48 h, and taking out the chip to be detected to form a hydrophobic layer comprising the hydrophobic solution on the surface of the chip to be detected.
5. The method according to claim 1, characterized in that the substrate of the chip to be tested is made of any one of the following materials:
silicon, silicon dioxide, black silicon, a porous alumina template, titanium dioxide, graphene, non-woven fabric, polymethyl methacrylate and adhesive tape.
6. The method according to claim 5, wherein the substrate of the chip to be tested has metal nanoparticles and/or metal nanowires deposited thereon.
7. The method of claim 6,
the metal nanoparticles are specifically single metal nanoparticles and/or alloy nanoparticles;
the single metal nano-particle is specifically a gold nano-particle, a silver nano-particle or a copper nano-particle;
the alloy nanoparticles comprise at least two metals of gold, silver and copper;
the metal nanowire is specifically a gold nanowire, a copper nanowire or a silver nanowire.
8. The method of claim 1, wherein the metal nanoparticles are shaped specifically as any one of:
star, hexagon, and circle.
9. The method of claim 1, wherein the solution to be tested is specifically any one of the following solutions:
R6G solution, malachite green solution, and methylene blue solution.
10. The method of claim 1, further comprising, after dropping the solution to be tested on the hydrophobic layer: and drying the chip to be detected after waiting for 10-30 min.
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| CN201910314129.2A CN111830005A (en) | 2019-04-18 | 2019-04-18 | Detection method of chip Raman signal |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113702348A (en) * | 2021-04-30 | 2021-11-26 | 中国农业科学院茶叶研究所 | Surface-enhanced Raman substrate with three-dimensional hot spots and preparation method thereof |
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