CN110596075B - Method for enhancing Raman signal on surface of graphdiyne - Google Patents
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Abstract
The invention relates to the technical field of laser Raman and material structure identification, and provides a method for enhancing a graphene surface Raman signal, which comprises the following steps: s1, transferring the graphite alkyne film to a target substrate by a wet transfer method; s2, transferring the molybdenum disulfide which grows through mechanical stripping or chemical vapor deposition to the surface of the graphite alkyne film on the target substrate obtained in the step S1 to obtain a substrate-graphite alkyne-molybdenum disulfide structure; s3, carrying out Raman spectrum detection on the overlapping area of the molybdenum disulfide and the graphite alkyne in the structure, and obviously enhancing Raman signals. The invention has the beneficial effects that: aiming at the problem that the alkyne Raman peak with the thickness of 2-10nm is weak, the Raman enhanced scattering of molybdenum disulfide is utilized, so that the Raman peak intensity can be obviously improved; the method has obvious effect and high sensitivity, and the peak position area on the graphite alkyne is far away from the peak position areas of the molybdenum disulfide, so that the peak position areas cannot influence each other.
Description
Technical Field
The invention relates to the technical field of laser Raman and material structure identification, in particular to a method for enhancing a Raman signal on a graphite alkyne surface.
Background
The excellent properties and wide application of carbon materials benefit from the abundant hybridization of carbon atoms and the structure of carbon materials. Since the discovery of graphdiynes and fullerenes, research has been conducted to develop new carbon allotropes. The graphyne is a novel carbon allotrope, and is formed by connecting acetylene bonds with benzene rings, so that the graphyne has three hybridization states of sp, sp2 and sp 3. Theoretically, the composite material has adjustable band gap, large elastic modulus and excellent conductivity.
Since 2010, graphite alkyne is synthesized for the first time, and further synthesis of single-layer graphite alkyne with high crystal type is attempted. However, in the characterization and detection of the thin-layer graphyne structure, the acetylene bond peak is strong and weak, and accurate qualitative, observation and analysis cannot be performed.
Therefore, if the method for enhancing the surface Raman signal of the graphyne film is provided, newly synthesized graphyne can be more accurately characterized and analyzed, a foundation is laid for synthesizing high-quality single-layer graphyne, and obstacles are swept away.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for enhancing the Raman signal of the surface of the graphdine, which has the advantages of obvious enhancement of the Raman signal of the graphdine, high repeatability and simple and controllable method and solves the technical problem of weak Raman signal of the thin-layer graphdine.
The invention adopts the following technical scheme:
a method for enhancing Raman signals of a graphite alkyne surface is characterized in that a graphite alkyne film and molybdenum disulfide are sequentially transferred on a target substrate to obtain a substrate-graphite alkyne-molybdenum disulfide structure, wherein a molybdenum disulfide and graphite alkyne overlapping region of the structure is a Raman signal enhancement region (Raman spectrum detection is carried out on the molybdenum disulfide and graphite alkyne overlapping region of the structure, and Raman signals are obviously enhanced).
The method for surface raman signal enhancement of graphdiyne according to claim 1, specifically comprising the steps of:
s1, transferring the graphite alkyne film to a target substrate by a wet transfer method;
s2, preparing molybdenum disulfide, and transferring the molybdenum disulfide to the surface of the graphite alkyne film on the target substrate obtained in the step S1 to obtain a substrate-graphite alkyne-molybdenum disulfide structure;
s3, carrying out Raman spectrum detection on the overlapping area of the molybdenum disulfide and the graphdine of the structure, wherein the overlapping area is a Raman signal enhancement area.
Further, the target substrate is a silicon substrate, quartz, ceramic, or flexible substrate.
Further, step S1 is specifically: uniformly coating the copper foil with the graphyne with polymethyl methacrylate, removing the copper foil by etching with a ferric chloride solution, then fishing up the polymethyl methacrylate with the graphyne with the target substrate, and cleaning to obtain a clean graphyne film on the target substrate.
Further, the thickness of the graphite alkyne film is 2-10 nm.
Further, in step S2, the method for preparing molybdenum disulfide is mechanical stripping or chemical vapor deposition.
Further, step S2 specifically includes:
s2.1, uniformly coating polymethyl methacrylate on the substrate attached with the molybdenum disulfide, and etching and separating the molybdenum disulfide and a silicon growth substrate by using a hydrofluoric acid solution;
s2.2, transferring the molybdenum disulfide to a target substrate containing the graphite alkyne film by using accurate transfer, removing polymethyl methacrylate by using acetone, cleaning by using isopropanol, and drying by using nitrogen to obtain a substrate-graphite alkyne-molybdenum disulfide structure.
Further, the silicon growth substrate is a p-type doped silicon substrate, wherein the thickness of the silicon dioxide layer of the upper layer is 300 nm.
Further, in step S3, the graphyne target substrate attached with molybdenum disulfide is irradiated with 532nm laser and detected by raman spectroscopy, resulting in an enhanced graphyne raman peak.
The invention has the beneficial effects that: aiming at the problem that the alkyne Raman peak with the thickness of 2-10nm is weak, the Raman enhanced scattering of molybdenum disulfide is utilized, so that the Raman peak intensity can be obviously improved; the method has obvious effect and high sensitivity, and the peak position area on the graphite alkyne is far away from the peak position areas of the molybdenum disulfide, so that the peak position areas cannot influence each other.
Drawings
FIG. 1 shows SiO2(iii) electron microscopy images of graphdines on a/Si target substrate.
FIG. 2 is a graph showing a comparison of intrinsic Raman spectra of graphyne and enhanced Raman spectra of graphyne enhanced with molybdenum disulfide in examples.
FIG. 3 is an electron micrograph of a graphdine Raman-enhanced structure and a Raman intensity map of a region corresponding to the location in accordance with an embodiment of the present invention; wherein (a) is a region raman spectrometer test region; (b) is a regional raman intensity map.
Detailed Description
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be noted that technical features or combinations of technical features described in the following embodiments should not be considered as being isolated, and they may be combined with each other to achieve better technical effects. In the drawings of the embodiments described below, the same reference numerals appearing in the respective drawings denote the same features or components, and may be applied to different embodiments.
Example 1
The embodiment of the invention provides a method for enhancing a Raman signal on a graphite alkyne surface, which comprises the following steps:
1. a Si substrate having a 300nm thick oxide layer was cut into a size of 1cm × 1cm as a target substrate, and a silicon growth substrate (for growing molybdenum disulfide).
2. Multilayer graphite alkyne is prepared on a copper foil by a cross coupling method, and an ultrathin graphite alkyne film is obtained by oxygen plasma etching, as shown in figure 1. Uniformly coating polymethyl methacrylate on a copper foil attached with grapargyne, removing the copper foil by etching with a ferric chloride solution, taking out the polymethyl methacrylate attached with the grapargyne from a substrate, heating the polymethyl methacrylate on a hot plate for 10 minutes, cleaning the polymethyl methacrylate with acetone at the temperature of 85-95 ℃ for ten minutes, taking out the polymethyl methacrylate, immediately putting the polymethyl methacrylate into isopropanol, and drying the isopropanol with nitrogen to obtain clean grapargyne on a target substrate
3. And preparing the monolayer molybdenum disulfide by using a chemical vapor deposition method. Putting 10mg of molybdenum trioxide powder into a tubular furnace, reacting the molybdenum trioxide powder with sulfur steam for 25 minutes at 850 ℃, introducing oxygen to assist the reaction to generate, and preparing a monolayer molybdenum disulfide layer on a silicon growth substrate.
4. After polymethyl methacrylate is evenly coated on the single-layer molybdenum disulfide on the silicon growth substrate, the molybdenum disulfide and the silicon growth substrate are etched and separated by hydrofluoric acid solution. By utilizing accurate transfer, after molybdenum disulfide is transferred to a target substrate containing graphite alkyne, acetone at 85-95 ℃ is used for cleaning for ten minutes and then taken out, then the molybdenum disulfide is immediately put into isopropanol and is dried by nitrogen gas, and a substrate-graphite alkyne-molybdenum disulfide structure is obtained and used for detecting the Raman of the graphite alkyne structure.
5. And (3) performing Raman spectrometer test on the sample obtained in the step (3) by using laser with a wavelength of 532, and analyzing and testing Raman spectrums of the graphite alkyne and the intrinsic graphite alkyne (only the graphite alkyne film is attached with the molybdenum disulfide layer) covered by the molybdenum disulfide.
6. As shown in FIG. 2, comparative analysis shows that the Raman spectrum of the graphite alkyne covered by molybdenum disulfide is 1580cm-1、1367cm-1、1929cm-1、2202cm-1The Raman signal of the graphdine is obviously enhanced with the help of the molybdenum disulfide.
Example 2
The embodiment of the invention provides a method for enhancing a Raman signal on a graphite alkyne surface, which comprises the following steps:
1. a Si substrate having a 300nm thick oxide layer was cut into a size of 1cm × 1cm as a target substrate, and a silicon growth substrate (for growing molybdenum disulfide).
2. Multilayer graphite alkyne is prepared on a copper foil by a cross coupling method, and an ultrathin graphite alkyne film is obtained by oxygen plasma etching, as shown in figure 1. Uniformly coating polymethyl methacrylate on a copper foil attached with grapargyne, removing the copper foil by etching with a ferric chloride solution, taking out the polymethyl methacrylate attached with the grapargyne from a substrate, heating the polymethyl methacrylate on a hot plate for 10 minutes, cleaning the polymethyl methacrylate with acetone at the temperature of 85-95 ℃ for ten minutes, taking out the polymethyl methacrylate, immediately putting the polymethyl methacrylate into isopropanol, and drying the isopropanol with nitrogen to obtain clean grapargyne on a target substrate
3. And preparing the monolayer molybdenum disulfide by using a chemical vapor deposition method. Putting 10mg of molybdenum trioxide powder into a tubular furnace, reacting the molybdenum trioxide powder with sulfur steam for 25 minutes at 850 ℃, introducing oxygen to assist the reaction to generate, and preparing a monolayer molybdenum disulfide layer on a silicon growth substrate.
4. After polymethyl methacrylate is evenly coated on the single-layer molybdenum disulfide on the silicon growth substrate, the molybdenum disulfide and the silicon growth substrate are etched and separated by hydrofluoric acid solution. By utilizing accurate transfer, after molybdenum disulfide is transferred to a target substrate containing graphite alkyne, acetone at 85-95 ℃ is used for cleaning for ten minutes and then taken out, then the molybdenum disulfide is immediately put into isopropanol and is dried by nitrogen gas, and a substrate-graphite alkyne-molybdenum disulfide structure is obtained and used for detecting the Raman of the graphite alkyne structure.
5. And (3) performing a regional Raman spectrometer test on the sample obtained in the step (3) by using laser with a wavelength of 532, and analyzing and testing the regional Raman intensity graphs of the graphite alkyne and the intrinsic graphite alkyne (only the graphite alkyne film is attached with the molybdenum disulfide layer) covered by the molybdenum disulfide. The test area is shown in the electron micrograph of fig. 3(a), wherein half of the graphdine is covered with molybdenum disulfide and half is attached with a molybdenum disulfide layer.
6. After the area of the electron micrograph in fig. 3(a) is subjected to a raman spectroscopy test, a raman intensity map in the area in fig. 3(b) is obtained. As can be seen from the figure, the areas of the graphite alkyne covered with molybdenum disulphide show a dark colour, while the areas of the graphite alkyne without molybdenum disulphide covering show a light colour. The color depth indicates the strength of the graphyne peak in the region, and the graph indicates that the graphyne Raman signal is obviously enhanced with the help of molybdenum disulfide.
While several embodiments of the present invention have been presented herein, it will be appreciated by those skilled in the art that changes may be made to the embodiments herein without departing from the spirit of the invention. The above examples are merely illustrative and should not be taken as limiting the scope of the invention.
Claims (8)
1. A method for enhancing Raman signals on the surface of graphyne is characterized in that a graphyne film and molybdenum disulfide are sequentially transferred on a target substrate to obtain a substrate-graphyne-molybdenum disulfide structure, wherein the overlapping area of the molybdenum disulfide and the graphyne in the structure is a Raman signal enhancement area;
the method specifically comprises the following steps:
s1, transferring the graphite alkyne film to a target substrate by a wet transfer method;
s2, preparing molybdenum disulfide, and transferring the molybdenum disulfide to the surface of the graphite alkyne film on the target substrate obtained in the step S1 to obtain a substrate-graphite alkyne-molybdenum disulfide structure;
s3, carrying out Raman spectrum detection on the overlapping area of the molybdenum disulfide and the graphdine of the structure, wherein the overlapping area is a Raman signal enhancement area.
2. The method of graphoyne surface raman signal enhancement of claim 1, wherein the target substrate is a silicon substrate, quartz, ceramic, or a flexible substrate.
3. The method for enhancing the surface raman signal of the graphdine according to claim 1, wherein the step S1 specifically comprises: uniformly coating the copper foil with the graphyne with polymethyl methacrylate, removing the copper foil by etching with a ferric chloride solution, then fishing up the polymethyl methacrylate with the graphyne with the target substrate, and cleaning to obtain a clean graphyne film on the target substrate.
4. The method for surface raman signal enhancement of a graphdiyne of claim 1 or 3 wherein the graphdiyne film has a thickness of 2 to 10 nm.
5. The method for preparing molybdenum disulfide according to claim 1, wherein in step S2, the method for preparing molybdenum disulfide is mechanical stripping or chemical vapor deposition.
6. The method for enhancing the surface raman signal of a graphdine according to claim 1, wherein the step S2 specifically includes:
s2.1, uniformly coating polymethyl methacrylate on the substrate attached with the molybdenum disulfide, and etching and separating the molybdenum disulfide and a silicon growth substrate by using a hydrofluoric acid solution;
s2.2, transferring the molybdenum disulfide to a target substrate containing the graphite alkyne film by using accurate transfer, removing polymethyl methacrylate by using acetone, cleaning by using isopropanol, and drying by using nitrogen to obtain a substrate-graphite alkyne-molybdenum disulfide structure.
7. The method for graphone surface raman signal enhancement according to claim 6, wherein the silicon growth substrate is a p-type doped silicon substrate, wherein the thickness of the silicon dioxide layer of the upper layer is 300 nm.
8. The method for enhancing the surface raman signal of the graphdine according to claim 1, wherein in step S3, the graphdine target substrate attached with molybdenum disulfide is irradiated by 532nm laser and detected by raman spectroscopy, so as to obtain the enhanced graphdine raman peak.
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