CN109839369B - Method for determining graphite order degree based on laser Raman Mapping - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 89
- 239000010439 graphite Substances 0.000 title claims abstract description 89
- 238000000034 method Methods 0.000 title claims abstract description 38
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- 238000004458 analytical method Methods 0.000 claims abstract description 29
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
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- 239000011435 rock Substances 0.000 claims description 3
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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
Abstract
The invention discloses a method for determining the degree of order of graphite based on laser Raman Mapping, which comprises the following steps: s1, preparing a sample; s2, observing and analyzing graphite; s3, setting equipment parameters; s4, calibrating and correcting the instrument; s5, data processing and imaging: and (3) placing the sample prepared in the step S1 in a corresponding detection area, collecting the Raman spectrum of the marked site in the step S2 by the system according to set conditions, storing the measured graphite Mapping original data, performing fitting analysis on the data of the D peak and the G peak on the original data, selecting the area ratio of the D peak to the G peak, setting different color representation ranges, and reflecting the order degree of the graphite by different colors. The method has the advantages of simple sample preparation and low sample requirement, and can directly test common sheets, and meanwhile, the method adopts high-precision in-situ micro-area analysis, the precision can reach 2 mu m, and the problem that the in-situ micro-area analysis is difficult to determine the order degree of the graphite by using the traditional experimental method is actually solved.
Description
Technical Field
The invention belongs to the technical field of mineral detection, and particularly relates to a method for determining the degree of order of graphite based on laser Raman Mapping.
Background
Graphite (graphite) is a crystalline carbon, hexagonal, black to dark gray in color, 2.25 g/cm 3 in density, 1.5 in hardness, 3652 ℃ in melting point and 4827 ℃ in boiling point. The graphite crystal is characterized by a typical layered structure, carbon atoms are arranged in layers, each carbon is connected with adjacent carbons at equal intervals, the carbons in each layer are arranged according to a hexagonal ring shape, the carbon hexagonal rings of the upper adjacent layer and the lower adjacent layer are mutually displaced in the direction of a parallel net surface and then are superposed to form the layered structure, and different polytype structures are caused by different displacement directions and distances. The disordered and loose accumulation of the same carbon atoms means that the disorder degree is poor, only black and soft graphite can be formed, and the well-ordered carbon atoms are combined into a cuboctahedral structure to form a hard and unmatched diamond.
Laser Raman spectroscopy is a microscopic analysis technique for non-destructive determination of molecular components of a substance, and is a molecular scattering spectrum based on the change of the original incident frequency after inelastic collision of laser photons with the molecules of the substance. In recent years, with the development of raman spectroscopy, not only molecular structure information is directly reflected, but also changes in crystallinity and order in geological samples are reflected in the form, half-width value, and area ratio, and thus the raman spectroscopy has been attracting attention.
The technology is realized by a novel inVia series Raman spectrum system provided with a Stream L inviHR imaging accessory, and an imaging area can be freely selected, so that Raman data inside a sample, such as the intensity of a Raman spectrum band or other more complex parameters, can be collected and displayed in a large range and in a three-dimensional manner, and a test mode is improved from conventional point scanning to surface scanning.
At present, an XDR method is used as a conventional method for acquiring the order degree of graphite, but an XDR test method can only represent the existence of a magnetic substance, and does not have any corresponding peak of carbon, so that the condition of the carbon is determined, and a Raman spectrum is a good choice, but the method has the defects of excessive measuring points and low efficiency.
Disclosure of Invention
The invention aims to solve the problems and provides a method for determining the graphite order degree based on laser Raman Mapping.
In order to solve the technical problems, the technical scheme of the invention is as follows: a method for determining the degree of order of graphite based on laser Raman Mapping comprises the following steps:
s1, sample preparation: preparing a rock sample, grinding a two-side polishing sheet to obtain a conventional graphite sheet;
s2, observation and analysis of graphite: confirming the position and the shape of the graphite, and marking;
s3, setting parameters: setting conventional parameters of a Raman instrument, wherein the exposure time is 1S-1.5S, the microscope selects an objective lens of 100X or 50X, the spectrum acquisition time is 1S-1.5S, and the step length is 1-3 mu m;
s4, calibrating and correcting the instrument: calibrating the optical path and the peak position of the instrument;
s5, data processing and imaging: and (3) placing the sample prepared in the step S1 in a corresponding detection area, collecting the Raman spectrum of the marked site in the step S2 by the system according to set conditions, storing the measured graphite Mapping original data, performing fitting analysis on the data of the D peak and the G peak on the original data, selecting the area ratio of the D peak to the G peak, setting different color representation ranges, and reflecting the order degree of the graphite by different colors.
In the above technical solution, in the step S1, too thick flakes affect the testing and identification of the sample, and too thin flakes are not suitable for some minerals. The thickness of the sheet is preferably 0.1 to 0.3 mm. The flake size is preferably 50mm 25mm, and the shape and length and width are not particularly limited for raman. Further, it is preferable to prepare a sample at room temperature, clean and polish surface impurities after the preparation of the sheet. If the surface of the sample is oxidized or has other impurities after being placed for a long time before the test, the thin sheet needs to be cleaned and polished again.
Still further, in the present invention, it is preferable that the sample is not covered with a cover slip. The laser can penetrate the slide and the placement of the sample under a transparent glass cover slip is generally unaffected. However, the possibility of glue contamination can be reduced by not covering the glass slide, and when the glass slide is covered, the Raman focusing position is not aligned, and the Raman focusing position is gathered on the glass slide, and the measured result is the spectrum of the glass. The reason for the influence of the glue is as follows: fluorescence is generated. Raman measurement is the reflection light of molecules after being excited, so that for some substances such as amorphous substance glass and the like, strong fluorescence interference is generated in measurement, and a Raman signal is covered. At present, the light source is generally replaced for eliminating fluorescence, fluorescence is prevented from appearing in a measured wave number range by changing the excitation wavelength, sometimes, the fluorescence background is strong when Raman is performed, the excitation wavelength needs to be changed to eliminate the influence of the fluorescence, and therefore the complexity of the test is increased.
In the above technical solution, in the step S2, the purpose of confirming the position and the shape of the graphite is to find a test target for preparation for the next step, because the sample may include a plurality of graphites, and a mapping test is performed by selecting a range first. The range size is not particularly limited, and the range can be determined according to actual conditions, but the range is not suitable to be too large, because the size determines the number of points, and the total time efficiency of the test is influenced. The specific operation steps are that graphite is found under an optical microscope, a marker pen is used for marking circles of the graphite, Arabic numbers are used for marking all the positions in sequence, then the positions are marked by lines and connected in sequence, and the shape of the positions and a reference object near the graphite are photographed and recorded. The form includes the shape, size, luster, surface crack and surface grain of graphite mineral.
In the above technical solution, in step S3, the exposure time, the microscope objective lens selection multiple, the spectrum acquisition time, and the step size may affect the test accuracy. The exposure time is 1S, the microscope selects an objective lens 100X, the spectrum acquisition time is 1S, and the step length is 1 mu m. For other conventional parameters of the raman instrument, the settings of the laser, the grating, the confocal pinhole and the slit can be set according to the conventional setting parameters in the field, and in the invention, a 514 nm/30-50 mW laser, a 1800-line grating, a 200-400 μm confocal pinhole size and a 100 μm slit are preferred. 514 nanometer (green light) laser, the performance is very stable, in addition 532 nanometer solid diode pump laser, 632.8 nanometer (red light), 780 nanometer and other visible light laser, and 785 nanometer diode, 830 nanometer near-infrared laser can all be used for this invention.
Theoretically, the raman spectrum is independent of the wavelength of the excitation light. However, some samples can generate strong fluorescence under the excitation of laser with one wavelength, and the interference is generated on the Raman spectrum. In this case, the excitation light is changed to avoid interference of fluorescence. If the sample does not fluoresce under different laser excitations, any laser may be used.
In the above technical solution, the step S4 further includes the following steps:
s41, laser path spot correction: the light spot is positioned in the center of the cross, and the light spot has uniformity and even breathing;
s42, calibrating a signal light path: the signal light path comprises an optical sheet, a focusing mirror, a slit, a prism, a grating W and a detector CCD signal detection system, and the size and the position of the slit and a signal receiving area of the detector CCD are adjusted;
s43, matching the XY automatic platform with manual control, and calibrating the focus plane of the white light state and the laser state to be consistent;
s44, wave number calibration and correction of the Raman instrument: firstly using 520.7cm-1Calibrating the wave number of a silicon chip as a Raman Instrument, selecting a 514nm laser when calibrating a standard sample, collecting a spectrum of the silicon chip in real time, obtaining the peak position of the spectrum by removing the back bottom and calibrating the peak position, and then adjusting the peak position of the silicon chip to the standard 520.7cm through Instrument calibration in a setup menu-1。
It is worth noting that calibration of the instrument peak position and optical path is a routine practice in the art. For laser light path light spots, the sizes of Raman light spots of different devices are different under different focusing conditions of the same device, and the Raman light spots need to be set and corrected, so that the Raman reproducibility and the Raman accuracy are guaranteed. For a signal light path, if a light source is not changed, calibration is generally not needed, only the light path and the intensity need to be corrected, and when a laser needs to be changed to measure a sample, the calibration needs to be performed again. The XY automatic platform tests according to the point locations of the program, and manually tests the interested point locations, so that the effect is the same, and the manual flexibility is high. The calibration of the white light state and the laser state is to make the result more reliable, complement each other, and the information detected by the two is more reliable.
In the above technical solution, the step S5 further includes the following steps:
s51, moving the sample to a Mapping area, confirming that the laser spot is in the center of the sample, and then turning off the laser;
s52, sequentially selecting four points along the upper left, lower right, upper right and lower left by using a Point Mapping mode of a system, then checking X and Y in Mapping properties, selecting a single window mode, setting the spectrum acquisition time to be 1-10 seconds, clicking Mapping acquisition after all parameters are set to enable an automatic platform to scan a circle along the upper left, lower right, upper right and lower left points sequentially, selecting a Mapping range by using a square frame, setting the step length in the X-axis direction and the Y-axis direction, setting the step length to be 1um in the embodiment, changing the spectrum acquisition range to be a multi-window mode, clicking Mapping acquisition after the parameters are set to perform spectrum acquisition test analysis, obtaining four windows of a spark, a Point, a Map and a Video after the test is finished, and simultaneously storing the spark and the Video windows to store the measured original graphite parameter data, wherein the peak of the measured graphite spectrum is reflected on a three-dimensional original space;
s53, processing the data of the D and G peaks by using Wire software on the basis of Mapping spectral data acquisition, wherein the specific operation method comprises the following steps: performing baseline removal and peak fitting on all spectra in a Spim window, when a sample is influenced by fluorescence or thermal background, the Raman spectrum has an angle inclination, and a signal source is contained on an inclined substrate, a spectrum with a flat baseline needs to be obtained by a baseline removal method, and the spectrum can be directly operated by a Processing sub baseline function of a software window; the peak position comprises peak intensity, half peak width and peak area, fitting analysis is carried out on the peak position, under the general condition, deviation can exist in the required peak position or superposition of two or more peak positions, the peak position fitting can obtain not only the accurate parameters of a simple single peak, but also the accurate parameters of a complex spectral band overlapped by a plurality of peaks, and the specific method comprises the following steps: selecting an Analysis curve fit function to open a curve fitting window, amplifying G and D peaks needing fitting, moving a mouse to the position of a spectral band needing fitting, clicking the added peak position, continuously clicking, clicking Add in when no peak position continues to appear, then defining two component spectrums of D and G through a Model function, thereby obtaining the distribution of the two components on the two-dimensional plane, constructing a graphite three-dimensional space D and G peak distribution on the basis of the Analysis, reading the distribution conditions of related parameters of the graphite D peak and the graphite G peak through a Raman spectrometer, obtaining the graphite D/G area ratio, finally selecting the area ratio of the D peak and the G peak, setting different color expression ranges, and reflecting the order degree of the graphite with different colors.
Basic principle involved in step S53: after subtracting the substrate, the D peak corresponds to 1360cm, according to the standard D, G peak position-1Left and right, G peak is 1580cm-1There may be a deviation of about plus or minus 10 to determine the peak area of the corresponding position of the sample spectral line, and the analysis is performed by using the symmetrical peak principle. The fitting of the partial peaks is carried out when necessary (there is an overlap of the two peaks), which is generally not required for graphite samples. The D peak is a disordering peak (disorder), and both the D and G peaks are caused by sp 2. 1585cm-1The raman peaks on the left and right are typical of bulk crystalline graphite and are referred to as the G-band. This peak is the fundamental vibration mode of the graphite crystal, the intensity of which is related to the size of the crystal. 1360cm-1The raman peak at (a) originates from the oscillation of the graphitic carbon crystalline edge, called the D-band. These two raman peaks are typical of graphite-like carbons (e.g., graphite, carbon black, activated carbon, etc.).
Other methods, such as curve fitting using the mathematical software MAP L E, are also possible.
The method for determining the graphite order degree based on laser Raman Mapping provided by the invention has the following beneficial effects:
(1) the traditional XDR method for obtaining the graphite order degree is tested on the basis of points, but in fact, graphite minerals in a slice are possibly influenced by various factors and are not uniform, and especially in manual point-by-point testing, partial important points can be omitted in analysis, especially the measuring time is long, and the human-computer interaction time is long; the method is simple in sample preparation and low in sample requirement, a common sheet can be directly tested, and meanwhile, the method adopts high-precision in-situ micro-area analysis, so that the precision can reach 2 mu m;
(2) the laser Raman analysis technology based on the measurement of the layered mineral structure has stronger visualization and simplified operation, is non-destructive and quick, provides a new technical means for obtaining the order degree of the graphite, actually solves the problem that the in-situ micro-area analysis is difficult to measure the order degree of the graphite by using the traditional experimental method, and provides reliable technical support for researches such as the cause mechanism, the structural analysis and the like of the graphite.
Drawings
FIG. 1 is a flow chart of the present invention for determining the degree of order of graphite based on laser Raman mapping.
FIG. 2 shows Mapping measuring points and Raman peak spectra of the present invention.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments:
as shown in fig. 1, the method for determining the graphite order degree based on laser raman Mapping of the present invention comprises the following steps:
s1, sample preparation: preparing a rock sample, grinding a two-side polished sheet, wherein the thickness of the sheet is 0.1-0.3 mm, obtaining a conventional graphite sheet, and covering no glass slide;
s2, observation and analysis of graphite: the position and form of the graphite are confirmed and marked, specifically,
firstly, finding graphite under an optical microscope, marking circles of the graphite by using a marking pen, marking each point by using Arabic numerals in sequence, then marking the points, connecting the points in sequence, and photographing and recording the form of the points and a reference object near the graphite;
s3, setting parameters: selecting a 514 nm/30-50 mW laser, a grating 1800 line, a confocal pinhole with the size of 200-400 mu m, a slit with the size of 100 mu m, exposure time of 1S, a microscope selecting objective lens with the size of 100X, a spectrum acquisition time of 1S and a step size of 1 um;
s4, calibrating and correcting the instrument: the peak position is calibrated by adopting a standard sample, and the specific steps are as follows
S41, laser path spot correction: the light spot is positioned in the center of the cross, and the light spot has uniformity and even breathing;
s42, calibrating a signal light path: the signal light path comprises an optical sheet, a focusing mirror, a slit, a prism, a grating W and a detector CCD signal detection system, and the size and the position of the slit and a signal receiving area of the detector CCD are adjusted;
s43, matching the XY automatic platform with manual control, and calibrating the focus plane of the white light state and the laser state to be consistent;
s44, wave number calibration and correction of the Raman instrument: firstly using 520.7cm-1Calibrating the wave number of a silicon chip as a Raman Instrument, selecting a 514nm laser when calibrating a standard sample, collecting a spectrum of the silicon chip in real time, obtaining the peak position of the spectrum by removing the back bottom and calibrating the peak position, and then adjusting the peak position of the silicon chip to the standard 520.7cm through Instrument calibration in a setup menu-1；
S5, data processing and imaging: placing the sample prepared in the step S1 in a corresponding detection area, collecting the Raman spectrum of the marked site in the step S2 by the system according to set conditions, storing the measured graphite Mapping original data, performing fitting analysis on the data of the D and G peaks on the original data, selecting the area ratio of the D and G peaks, setting different color representation ranges, reflecting the order degree of the graphite by different colors,
s51, moving the sample to a Mapping area, confirming that the laser spot is in the center of the sample, and then turning off the laser;
s52, sequentially selecting four points along the upper left, lower right, upper right and lower left by using a Point Mapping mode of a system, then checking X and Y in Mapping properties, selecting a single window mode, setting the spectrum acquisition time to be 1-10 seconds, clicking Mapping acquisition after all parameters are set to enable an automatic platform to scan a circle along the upper left, lower right, upper right and lower left points sequentially, selecting a Mapping range by using a square frame, setting the step length in the X-axis direction and the Y-axis direction, setting the step length to be 1um in the embodiment, changing the spectrum acquisition range to be a multi-window mode, clicking Mapping acquisition after the parameters are set to perform spectrum acquisition test analysis, obtaining four windows of a spark, a Point, a Map and a Video after the test is finished, and simultaneously storing the spark and the Video windows to store the measured original graphite parameter data, wherein the peak of the measured graphite spectrum is reflected on a three-dimensional original space;
s53, processing the data of the D and G peaks by using Wire software on the basis of Mapping spectral data acquisition, wherein the specific operation method comprises the following steps: performing baseline removal and peak fitting on all spectra in a Spim window, when a sample is influenced by fluorescence or thermal background, the Raman spectrum has an angle inclination, and a signal source is contained on an inclined substrate, a spectrum with a flat baseline needs to be obtained by a baseline removal method, and the spectrum can be directly operated by a Processing sub baseline function of a software window; the peak position comprises peak intensity, half peak width and peak area, fitting analysis is carried out on the peak position, under the general condition, deviation can exist in the required peak position or superposition of two or more peak positions, the peak position fitting can obtain not only the accurate parameters of a simple single peak, but also the accurate parameters of a complex spectral band overlapped by a plurality of peaks, and the specific method comprises the following steps: selecting an Analysis curve fit function to open a curve fitting window, amplifying G and D peaks needing fitting, moving a mouse to the position of a spectral band needing fitting, clicking the added peak position, continuously clicking, clicking Add in when no peak position continues to appear, then defining two component spectrums of D and G through a Model function, thereby obtaining the distribution of the two components on the two-dimensional plane, constructing a graphite three-dimensional space D and G peak distribution on the basis of the Analysis, reading the distribution conditions of related parameters of the graphite D peak and the graphite G peak through a Raman spectrometer, obtaining the graphite D/G area ratio, finally selecting the area ratio of the D peak and the G peak, setting different color expression ranges, and reflecting the order degree of the graphite with different colors.
In this embodiment, the graphite sample of the geological sample is analyzed by mapping to obtain a parameter value of G, D peak and finally the change condition of the graphite order degree is analyzed, and different color end member ranges and color levels are selected and expressed on the two-dimensional plane by different colors.
As shown in FIG. 2, the Raman shift was 1370cm-1(peak D) and 1583cm-1Two spectral peaks near the (G peak) are obvious, and the area ratio of the two spectral peaks is one of methods for representing the graphite order degree, so that the two Raman shifted spectral peaks are selected as main analysis objects. According to the results of Raman spectrum analysis of a large number of samples, as the area of the D peak becomes larger, the area ratio of D/G increases, the number of aromatic rings increases, defects of the carbon atom skeleton increase, and the degree of graphite ordering becomes worse. Therefore, as the degree of order of the graphite becomes higher, the Raman peak Raman shift is 1370cm-1The area decreases from side to side, and the ratio of the D/G peak area decreases, and the phenomenon of the decrease of the D peak area is also observed in the geological sample analyzed.
In summary, the method for determining the graphite order degree by laser raman Mapping is represented as a gridding operation, Mapping is a new imaging technology of a laser raman instrument, and is characterized in that an automatic sample platform (in two directions of X and Y) is controlled by software to move, a sample is recorded point by point, each point can be imaged on a detector, and therefore, more precise imaging test analysis on space can be achieved. And the parameter change of each point can be visually displayed in a two-dimensional or three-dimensional space, so that the method is more accurate and efficient compared with the prior art.
It will be appreciated by those of ordinary skill in the art that the embodiments described herein are intended to assist the reader in understanding the principles of the invention and are to be construed as being without limitation to such specifically recited embodiments and examples. Those skilled in the art can make various other specific changes and combinations based on the teachings of the present invention without departing from the spirit of the invention, and these changes and combinations are within the scope of the invention.
Claims (7)
1. A method for determining the degree of order of graphite based on laser Raman Mapping is characterized in that: the method comprises the following steps:
s1, sample preparation: preparing a rock sample, grinding a two-side polishing sheet to obtain a conventional graphite sheet;
s2, observation and analysis of graphite: confirming the position and the shape of the graphite, and marking;
s3, setting parameters: setting conventional parameters of a Raman instrument, wherein the exposure time is 1S-1.5S, the microscope selects an objective lens of 100X or 50X, the spectrum acquisition time is 1S-1.5S, and the step length is 1-3 mu m;
s4, calibrating and correcting the instrument: calibrating the optical path and the peak position of the instrument;
s5, data processing and imaging: placing the sample prepared in the step S1 in a corresponding detection area, collecting the Raman spectrum of the marked site in the step S2 by the system according to set conditions, storing the measured graphite Mapping original data, performing fitting analysis on the data of the D peak and the G peak on the original data, selecting the area ratio of the D peak and the G peak, setting different color representation ranges, and reflecting the order degree of the graphite by different colors;
in step S5, the method further includes the following steps:
s51, moving the sample to a Mapping area, confirming that the laser spot is in the center of the sample, and then turning off the laser;
s52, sequentially selecting four points along the upper left, the lower right, the upper right and the lower left by using a pointing mode of a system, then checking X and Y in pointing properties, performing spectrum acquisition test analysis, obtaining four windows of a spider, a Point, a Map and a Video after the test is finished, and simultaneously storing the Spim window and the Video window to store the measured graphite Mapping original parameter data, wherein the peak spectrum of the measured graphite Mapping original data is reflected on a three-dimensional space;
s53, processing the data of the D and G peaks by using Wire software on the basis of Mapping spectral data acquisition, wherein the specific operation method comprises the following steps: dividing baseline and peak fitting are carried out on all the spectra in a Spim window; the peak position comprises peak intensity, half peak width and peak area for fitting analysis, and the specific method comprises the following steps: selecting an Analysiscurvefit function to open a curve fitting window, amplifying G and D peaks to be fitted, moving a mouse to the position of a spectral band to be fitted, clicking to add a peak position, continuously clicking to add, then defining spectra of two components D and G through a Model function, obtaining a parameter value of G, D peak according to Mapping analysis, selecting different color end member ranges and color levels, expressing the ranges on a two-dimensional plane by using different colors, thus obtaining the distribution of the two components on the two-dimensional plane, constructing a graphite three-dimensional space D and G peak distribution on the basis of the analysis, reading the distribution conditions of related parameters of the graphite D peak and the graphite G peak through a Raman spectrometer, obtaining the D/G area ratio of the graphite, finally selecting the area ratio of the D peak and the G peak, setting different color expression ranges, and reflecting the order degree of the graphite by using different colors.
2. The method for determining the degree of order of graphite based on laser Raman Mapping according to claim 1, wherein: in the step S1, the thickness of the sheet is 0.1-0.3 mm.
3. The method for determining the degree of order of graphite based on laser Raman Mapping according to claim 1, wherein: in step S1, after the conventional graphite flakes are obtained, the graphite flakes are not covered with a glass slide.
4. The method for determining the degree of order of graphite based on laser Raman Mapping according to claim 1, wherein: in step S2, the specific operation steps include finding graphite under an optical microscope, circling the graphite with a marker pen, sequentially marking the respective dots with arabic numerals, drawing a line to connect the respective dots in sequence, and photographing and recording the shape of the reference object and the reference object near the graphite.
5. The method for determining the degree of order of graphite based on laser Raman Mapping according to claim 1, wherein: in step S3, the exposure time is 1S, the microscope selects the objective lens 100X, the sampling time is 1S, and the step size is 1 μm.
6. The method for determining the degree of order of graphite based on laser Raman Mapping according to claim 1, wherein: in the step S3, a 514 nm/30-50 mW laser, a grating 1800 line, a confocal pinhole size of 200-400 μm and a slit of 100 μm are selected.
7. The method for determining the degree of order of graphite based on laser Raman Mapping according to claim 1, wherein: in step S4, the method further includes the following steps:
s41, laser path spot correction: the light spot is positioned in the center of the cross, and the light spot has uniformity and even breathing;
s42, calibrating a signal light path: the signal light path comprises an optical sheet, a focusing mirror, a slit, a prism, a grating W and a detector CCD signal detection system, and the size and the position of the slit and a signal receiving area of the detector CCD are adjusted;
s43, matching the XY automatic platform with manual control, and calibrating the focus plane of the white light state and the laser state to be consistent;
s44, wave number calibration and correction of the Raman instrument: firstly using 520.7cm-1Calibrating the wave number of a silicon chip as a Raman Instrument, selecting a 514nm laser when calibrating a standard sample, collecting a spectrum of the silicon chip in real time, obtaining the peak position of the spectrum by removing the back bottom and calibrating the peak position, and then adjusting the peak position of the silicon chip to the standard 520.7cm through Instrument calibration in a setup menu-1。
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