CN113624743B - Method for dividing microscopic components by applying Raman spectrum parameters - Google Patents
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- 238000001237 Raman spectrum Methods 0.000 title claims abstract description 66
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- 238000001069 Raman spectroscopy Methods 0.000 claims description 21
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Abstract
The invention discloses a method for dividing microscopic components by applying Raman spectrum parameters. The method realizes the description of different microscopic components by using organic laser Raman spectrum data and the parameters, and can effectively reflect the basic principle of the first-order vibration condition of carbon molecules based on the difference of the first-order vibration of the carbon molecules of different microscopic components. The method solves the problems of time and labor waste in distinguishing the microscopic components of the vitrinite and the inert substance; the laser Raman spectrum analysis has the advantages of less consumption, short analysis time and the like. The invention has good reliability, economy and universality, and has good application and popularization prospects.
Description
Technical Field
The invention relates to application of a laser Raman spectrum technology in the field of petroleum geology, in particular to a method for dividing microscopic components by applying Raman spectrum parameters.
Background
The micro-component classification has important significance for distinguishing the organic matter type of the hydrocarbon source rock and researching the pore space of the shale gas reservoir. In recent years, research means is developed from an optical microscope to a scanning electron microscope with higher resolution, organic microscopic component analysis is mainly determined by traditional manual identification, and influence caused by human factors such as polished quality of polished sections and capability difference of researchers is larger. In recent years, ancient marine shale is a research hotspot, most organic matters of the ancient marine shale are in a high-over mature stage, optical properties of microscopic components gradually converge, and errors are easier to identify by using a traditional manual analysis method.
The Raman spectroscopy is a microstructure analysis technology, and can reflect the ordered degree and the structural defects of the structure in the thermal evolution process of the graphitized carbon substance, so that the Raman spectroscopy is widely used in oil-gas geological research in recent years. The chemical structures of different microscopic components in the coal have difference, and the carbon structure of the coal gradually becomes ordered along with the continuous deepening of the coalification effect. Therefore, the coal micro-components can be researched from the microstructure by using the Raman spectroscopy, the analysis errors caused by human factors are effectively reduced, and a reference is provided for the difference research of the shale micro-components.
Disclosure of Invention
The invention aims to provide a method for dividing microscopic components by using Raman spectrum parameters, which can make up the defects of the existing method.
The method for dividing the microscopic components by applying the Raman spectrum parameters comprises the following steps:
s1, taking n hydrocarbon source rock samples as standard samples, and sequentially marking the samples as a standard sample 1, a standard sample 2, a standard sample 8230, a standard sample n and a standard sample 8230; n can be a natural number between 5 and 10;
s2, taking a standard sample 1, and selecting a microscopic component A1 on the standard sample 1; performing laser Raman scanning on one scanning point A1-1 of the microscopic component A1 to obtain a laser Raman spectrum of the scanning point A1-1 of the microscopic component A1 in the standard sample 1, deducting the background to obtain a laser Raman spectrum of the scanning point A1-1 with the background subtracted, wherein the abscissa of the spectrum represents Raman shift and the unit is cm -1 The ordinate represents the raman intensity, dimensionless; the spectrogram has two original peaks, wherein the peak with small displacement is a D peak, and the peak with large displacement is a G peak;
the laser raman scan can be performed under the following conditions:
determining the laser wavelength and the laser power according to the adopted laser Raman spectrometer, wherein the laser wavelength and the laser power are required to be kept consistent in the whole experimental process, for example, the laser wavelength is 532nm, the laser power is 10mW, the exposure time is 10-20 s, and the scanning range is 100-3500 cm -1 。
The microscopic components can be selected by a microscope carried by a laser Raman spectrometer;
s3, performing 5-peak fitting on the laser Raman spectrum of the scanning point A1-1 with the background subtracted by adopting a Mixed fitting mode of Lorentzian and Gaussian to obtain 5 fitting function peak curves of a D peak and a G peak in the laser Raman spectrum of the scanning point A1-1 with the background subtracted, wherein the fitting function peak curve shifts from small to large sequentially to form a D4 peak fitting function curve, a D1 peak fitting function curve, a D3 peak fitting function curve, a G peak fitting function curve and a D2 peak fitting function curve;
the peak intensities represented by the maximum ordinate values of the D1 peak fitting function curve and the G peak fitting function curve are respectively recorded as I Bisection 1-A1-1D1 And I Label 1-A1-1G The peak displacement represented by the abscissa value corresponding to the maximum ordinate value is respectively recorded as W Label 1-A1-1D1 And W Label 1-A1-1G The full width at half maximum indicated by the peak width corresponding to one half of the maximum vertical coordinate is denoted as FWHM-D1 Label 1-A1-1 And FWHM-G Label 1-A1-1 ；
The spectral peak area of the D1 peak fitting function curve and the spectral peak area of the G peak fitting function curve are respectively marked as A Bisection 1-A1-1D1 And A Label 1-A1-1G ；
Said I Label 1-A1-1D1 The said I Label 1-A1-1G W is as described Label 1-A1-1D1 W is as described Label 1-A1-1G The FWHM-D1 Label 1-A1-1 The FWHM-G Label 1-A1-1 The above-mentioned A Label 1-A1-1D1 And said A Label 1-A1-1G As a base parameter for the D1 peak fitting function curve and the G peak fitting function curve;
peak intensity ratio I Label 1-A1-1D1 /I Label 1-A1-1G Peak displacement ratio W Label 1-A1-1D1 /W Label 1-A1-1G Sum peak area ratio A Label 1-A1-1D1 /A Label 1-A1-1G As derived parameters of said D1 peak fitting function curve and said G peak fitting function curve;
s4, determining a plurality of scanning points of the microscopic component A1, and obtaining basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum of the microscopic component A1 after background subtraction of different scanning points according to the steps S2-S3; preferably, 5 to 10 scanning points are determined;
s5, selecting other microscopic components on the standard sample 1, marking as microscopic components A2, A3, \8230, and Ai, \8230, respectively determining a plurality of scanning points of each microscopic component, and obtaining basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum after background subtraction is carried out on the different scanning points of the different microscopic components according to the steps S2-S3; preferably, 5 to 10 scanning points are determined;
s6, measuring vitrinite reflectivity R of the standard sample 1 o Is denoted as R o mark 1 ；
S7, repeating the steps S2-S5 to obtain basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum spectrogram after background subtraction is carried out on different scanning points of different microscopic components on the rest standard samples;
s8, repeating the step S6 to obtain vitrinite reflectivities of different standard samples, and recording the vitrinite reflectivities as R o mark 2 、R o mark 3 、……R o denotes n ；
S9, respectively mapping basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in a laser Raman spectrum spectrogram after the vitrinite reflectivity of different standard samples and the background subtraction of different scanning points of different microscopic components on different standard samples to obtain Raman spectrum parameters with good correlation with the vitrinite reflectivity on the D1 peak fitting function curve and the G peak fitting function curve in the laser Raman spectrum spectrogram;
s10, respectively drawing the reflectivity of the vitrinite of different standard samples and Raman spectrum parameters with good correlation with the reflectivity of the vitrinite on a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum spectrogram obtained in the step S9 to obtain Raman spectrum parameters and R o Whether the combined cross plot can partition the microscopic components and correlate with thermal maturity R o % of combined cross plots of every two Raman spectrum parameters with good correlation can be used for dividing organic microscopic components;
s11, taking the intersection image of the parameter combinations which can divide the microscopic components and are obtained in the step S11 as a template, wherein the data point concentration area is the distribution range of the microscopic components of the vitrinite and the inert material.
In the method, the type III hydrocarbon source rock sample can be a coal sample or shale in a continental phase stratum, a marine phase stratum or a sea-land transition phase stratum.
The method mainly utilizes organic laser Raman spectrum data and the parameters to realize the description of different microscopic components, and is based on the basic principle that the first-order vibration of carbon molecules of different microscopic components is different, and the laser Raman spectrum can effectively reflect the first-order vibration condition of the carbon molecules. The method solves the problems of time and labor waste in distinguishing the microscopic components of the vitrinite and the inert substance; the laser Raman spectrum analysis has the advantages of less consumption, short analysis time and the like. The invention has good reliability, economy and universality, and has good application and popularization prospects.
Drawings
FIG. 1 shows the peak fitting results of Raman spectra.
Fig. 2 shows raman spectra of different organic micro-components (fig. 2a shows the original raman spectrum, and fig. 2b shows the raman spectrum after pretreatment).
FIG. 3 is a combination of Raman spectral parameters for sectioning microscopic components.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The experimental apparatus used in the following examples is an in Via type laser microscopy confocal Raman spectrometer with a laser wavelength of 532nm, a laser power of 10mW, an exposure time of 10s, and a scanning range of 100-3500 cm -1 The number of analysis spots per micro-component in each sample was 10.
The method for dividing the microscopic components by using the Raman spectrum parameters comprises the following steps:
step one, taking 10 coal samples with different maturity at east edges of an Ordos basin as standard samples, numbering the 10 standard samples, and sequentially marking 1 standard sample, 2 standard sample, 8230, 9 standard sample and 10 standard sample;
secondly, a standard sample 1 is taken, one scanning point of one micro component is selected on the standard sample 1 for laser Raman scanning, and a laser Raman spectrum of the scanning point of the micro component in the standard sample 1 is obtained, wherein the abscissa of the spectrum represents Raman displacement and the unit is cm -1 The ordinate represents the raman intensity, dimensionless; the spectrogram has two original peaks, wherein the peak with small displacement is a D peak, and the peak with large displacement is a G peak;
deducting the background of the original Raman spectrum of the scanning points of the microscopic components in the standard sample 1 to obtain a laser Raman spectrum of the scanning points of the microscopic components in the standard sample 1 after deducting the background;
step four, adopting a Mixed fitting mode of Lorentzian and Gaussian functions to perform 5-peak fitting on the laser Raman spectrum spectrogram of the standard sample 1 with the background subtracted from the scanning points of the microscopic components to obtain 5 fitting function peak curves of the D peak and the G peak in the laser Raman spectrum spectrogram of the standard sample 1 with the background subtracted from the scanning points of the microscopic components, wherein the displacement is 1240cm from small to large -1 Nearby 1350cm -1 Nearby 1540cm -1 About 1600cm -1 Near, 1610cm -1 Near, the displacement of the fitting function peak curve is sequentially a D4 peak fitting function curve, a D1 peak fitting function curve, a D3 peak fitting function curve, a G peak fitting function curve and a D2 peak fitting function curve (figure 1) from small to large;
the peak intensities represented by the maximum ordinate of the D1 peak fitting function curve and the G peak fitting function curve in the laser Raman spectrum spectrogram after background subtraction of the microscopic component scanning points in the standard sample 1 are respectively marked as I Label 1-1D1 、I Label 1-1G (ii) a The peak displacement represented by the abscissa value corresponding to the maximum ordinate value is respectively recorded as W Label 1-1D1 、W Label 1-1G (ii) a The full widths at half maximum indicated by the peak widths corresponding to one half of the maximum vertical coordinate are respectively denoted as FWHM-D1 Label 1-1 、FWHM-G Tab 1-1 ；
The spectral peak area of the D1 peak fitting function curve and the G peak fitting function curve in the laser Raman spectrum spectrogram after background subtraction of the scanning points of the microscopic components in the standard sample 1 are respectively marked as A Label 1-1D1 、A Label 1-1G ；
I in laser Raman spectrum spectrogram fitting curve of standard sample 1 with background subtracted from scanning point of micro-component Label 1-1D1 、I Label 1-1G 、W Bisection 1-1D1 、W Label 1-1G 、FWHM-D1 Label 1-1 、FWHM-G Label 1-1 、A Bisection 1-1D1 、A Label 1-1G Fitting the basic parameters of the function curve for the D1 peak and the G peak; the derivative parameters of the D1 peak fitting function curve and the G peak fitting function curve have a peak intensity ratio I Label 1-1D1 /I Label 1-1G Peak displacement ratio W Label 1-1D1 /W Label 1-1G Peak area ratio A Bisection 1-1D1 /A Label 1-1G ；
Fifthly, re-determining 10 scanning points of the microscopic component on the standard sample 1 obtained in the second step, and operating each scanning point according to the second step to the fourth step to obtain basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum after background subtraction of different scanning points of the microscopic component;
sixthly, re-determining other microscopic components on the standard sample obtained in the second step, and classifying the microscopic components by taking a microscopic component and an inert component as classification standards; respectively determining 10 scanning points for different microscopic components, and performing operations from the second step to the fifth step on each scanning point; obtaining laser Raman spectrum spectrograms (figure 2) of different scanning points of different microscopic components and basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrograms after background subtraction, wherein the Raman spectrograms of the different microscopic components are different before and after treatment according to figure 2;
step seven, taking the standard sample 1 which completes the 6 steps as a measuring object, and measuring the reflectivity R of the vitrinite o Is denoted as R o mark 1 ；
Eighthly, repeating the second step to the sixth step to obtain basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum spectrogram after background subtraction is carried out on different scanning points of different microscopic components on different standard samples;
step nine, repeating the step seven to obtain the vitrinite reflectivity R on different standard samples o mark 2 、R o mark 3 、……R o denotes n ；
Step ten, obtaining vitrinite reflectivity R of different standard samples in step seven and step nine o mark 1 、R o mark 2 、……R o denotes n And basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum spectrogram obtained in the first step, the sixth step and the ninth step after background subtraction is carried out on different scanning points of different microscopic components on different standard samplesRespectively mapping to obtain Raman spectrum parameters with good correlation with vitrinite reflectance on a D1 peak fitting function curve and a G peak fitting function curve in a laser Raman spectrum spectrogram;
step eleven, obtaining vitrinite reflectivity R of different standard samples in step seven and step nine o mark 1 、R o mark 2 、……R o denotes n And respectively mapping the Raman spectrum parameters with good correlation with the vitrinite reflectance of the D1 peak fitting function curve and the G peak fitting function curve in the laser Raman spectrum spectrogram obtained in the step ten to obtain the Raman spectrum parameters and the R o Whether the combined cross plot can partition the microscopic components and correlate with thermal maturity R o % Raman spectral parameters with good correlation whether a two-by-two merged plot can partition organic microscopic components.
Specific results are shown in table 1. Wherein the displacement difference RBS = W G -W D1 Peak intensity ratio R1= I D1 /I G
Table 1 shows the Raman spectrum parameter combinations of the microscopic components (Ro% = 0.55-1.88%)
Step twelve, taking the intersection image of the parameter combinations which can be used for dividing the microscopic components and is obtained in the step eleven as a template, and taking a part of the distribution image of the data point concentrated region, namely the distribution range of the microscopic components, the inert components and other large-class microscopic components as shown in the figure 3, so that the laser Raman spectrum parameters can well distinguish different microscopic components.
The above embodiments are only for illustrating the technical idea and features of the present invention, and the purpose of the present invention is to enable those skilled in the art to understand the content of the present invention and implement the present invention, and not to limit the protection scope of the present invention by this means. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (1)
1. A method for dividing microscopic components by using Raman spectrum parameters comprises the following steps:
s1, taking n hydrocarbon source rock samples as standard samples, and sequentially marking the samples as a standard sample 1, a standard sample 2, a standard sample 8230, a standard sample n, n is a natural number between 5 and 10;
the hydrocarbon source rock sample is a coal sample or shale in a continental facies stratum, a marine facies stratum or a sea-land transition facies stratum;
s2, taking a standard sample 1, and selecting a microscopic component A1 on the standard sample 1; performing laser Raman scanning on one scanning point A1-1 of the microscopic component A1 to obtain a laser Raman spectrum of the scanning point A1-1 of the microscopic component A1 in the standard sample 1, and subtracting the background to obtain a laser Raman spectrum of the scanning point A1-1 with the background subtracted;
the laser raman scanning conditions were as follows:
determining laser wavelength and laser power according to the adopted laser Raman spectrometer, keeping consistent in the whole experimental process, wherein the exposure time is 10-20s, and the scanning range is 100-3500cm -1 ；
Selecting the microscopic components by using a microscope carried by a laser Raman spectrometer;
s3, performing 5-peak fitting on the laser Raman spectrum of the scanning point A1-1 with the background subtracted by adopting a Mixed fitting mode of Lorentzian and Gaussian to obtain 5 fitting function peak curves of a D peak and a G peak in the laser Raman spectrum of the scanning point A1-1 with the background subtracted, wherein the fitting function peak curves are a D4 peak fitting function curve, a D1 peak fitting function curve, a D3 peak fitting function curve, a G peak fitting function curve and a D2 peak fitting function curve in sequence from small to large according to the displacement;
the peak intensities represented by the maximum ordinate values of the D1 peak fitting function curve and the G peak fitting function curve are respectively recorded as I Label 1-A1-1D1 And I Label 1-A1-1G The peak displacement represented by the abscissa value corresponding to the maximum ordinate value is respectively recorded as W Label 1-A1-1D1 And W Label 1-A1-1G The full width at half maximum represented by the peak width at half maximum of the ordinate values is denoted as FWHM-D1 Label 1-A1-1 And FWHM-G Label 1-A1-1 ；
The spectral peak area of the D1 peak fitting function curve and the G peak fitting function curve are respectively marked as A Bisection 1-A1-1D1 And A Label 1-A1-1G ；
Said I Label 1-A1-1D1 The said I Label 1-A1-1G W is as described Label 1-A1-1D1 W is as described Label 1-A1-1G The FWHM-D1 Bisection 1-A1-1 The FWHM-G Label 1-A1-1 The above-mentioned A Label 1-A1-1D1 And said A Label 1-A1-1G As basic parameters of the D1 peak fitting function curve and the G peak fitting function curve;
peak intensity ratio I Bisection 1-A1-1D1 /I Label 1-A1-1G Peak displacement ratio W Bisection 1-A1-1D1 /W Label 1-A1-1G Sum peak area ratio A Label 1-A1-1D1 /A Label 1-A1-1G As derived parameters of said D1 peak fitting function curve and said G peak fitting function curve;
s4, re-determining 5-10 scanning points of the microscopic component A1, and obtaining basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in a laser Raman spectrum of the microscopic component A1 after background subtraction of different scanning points of the microscopic component A1 according to the steps S2-S3;
s5, selecting other microscopic components on the standard sample 1, marking as microscopic components A2, A3, \ 8230 \ 8230and Ai, respectively determining 5 to 10 scanning points of each microscopic component, and obtaining basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in a laser Raman spectrum of different microscopic components after background subtraction of different scanning points of different microscopic components according to the steps S2 to S3;
s6, measuring the vitrinite reflectivity of the standard sample 1R o Is marked asR oLabel 1 ；
S7, repeating the steps S2-S5 to obtain basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum spectrogram after background subtraction is carried out on different scanning points of different microscopic components on the rest standard samples;
s8, repeating the step S6 to obtain vitrinite reflectivities of different standard samples, and recording the vitrinite reflectivities asR oLabel 2 、R oLabel 3 、……R oSymbol n ；
S9, respectively mapping basic parameters and derivative parameters of a D1 peak fitting function curve and a G peak fitting function curve in a laser Raman spectrum spectrogram after the vitrinite reflectivity of different standard samples and the background subtraction of different scanning points of different microscopic components on different standard samples to obtain Raman spectrum parameters with good correlation with the vitrinite reflectivity on the D1 peak fitting function curve and the G peak fitting function curve in the laser Raman spectrum spectrogram;
s10, respectively drawing the reflectivity of the vitrinite of different standard samples and Raman spectrum parameters with good correlation with the reflectivity of the vitrinite on a D1 peak fitting function curve and a G peak fitting function curve in the laser Raman spectrum spectrogram obtained in the step S9 to obtain Raman spectrum parameters and Raman spectrum parametersR o Whether the combined cross plot can partition and thermally mature the microscopic componentsR o % of combined intersection graph of every two Raman spectrum parameters with good correlation can divide the organic microscopic component;
and S11, taking the intersection image of the parameter combinations which can divide the microscopic components and are obtained in the step S10 as a template, wherein the data point concentration area is the distribution range of the microscopic components of the vitrinite and the inert material.
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