CN111208162B - Quantitative characterization method for rapidly determining organic matter pores based on scanning electron microscope and application - Google Patents
Quantitative characterization method for rapidly determining organic matter pores based on scanning electron microscope and application Download PDFInfo
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Abstract
The invention belongs to the technical field of organic matter pore identification, and discloses a quantitative characterization method for rapidly determining organic matter pores based on a scanning electron microscope and application thereof, wherein the distribution position of organic matter is determined by using the scanning electron microscope; determining the types of the microscopic components by using an energy spectrometer and the form of organic matters; determining organic pores by using organic matter microscopic components; determining the distribution position of organic matters, determining the types of microscopic components and determining the development condition of organic pores. The method adopts the scanning electron microscope to identify the organic matter micro-components, can effectively solve the problems that the observation visual field is small, the organic hole is difficult to find and does not grow, the observation time is long, and the experiment and scientific research efficiency is reduced when the scanning electron microscope is used for observing the organic matter pores. The scanning electron microscope has the advantages of high magnification, strong stereoscopic impression of images and simple sample preparation method; the organic matter pores and the microscopic components are related, the self enrichment mode, morphological characteristics and the contact relationship with minerals of each microscopic component can be directly observed, and the organic matter pores are identified.
Description
Technical Field
The invention belongs to the technical field of organic matter pore identification, and particularly relates to a quantitative characterization method for rapidly determining organic matter pores based on a scanning electron microscope and application thereof.
Background
Currently, the closest prior art: at the present stage, the exploration and development of shale gas have important significance for changing the resource structure of China and improving the problems of energy shortage and the like. A large number of micro-nano pores develop in the shale gas reservoir, and the structural characteristics of the micro-nano pores are important indexes for measuring and evaluating the shale gas reservoir. The organic matter pores have close relation with the physical properties of the shale reservoir, the physical properties of the shale reservoir can be preliminarily judged by judging the organic matter pores, and the method has guiding significance for the exploration and development of shale gas.
Currently, for the field of organic matter pore observation, the closest prior art is: the prepared shale sample is placed under a field emission scanning electron microscope to directly search organic matter pores for observation, but the shale has a compact structure, and the pore sizes of the shale are widely distributed from micron-scale to nanometer-scale. The aperture of organic pores is mainly nano-scale, and is difficult to find under a scanning electron microscope, generally the organic pores need to be amplified by ten thousand times, and the organic pores with the size of 100nm need to be amplified to 60000 times for observation. At the present stage, the following is frequently observed for organic matter:
case 1: the organic matter is directly amplified and searched, and because organic matter pores cannot be observed under the visual field of 800 times, the red area in the figure is amplified, and the organic matter pores are not found after amplification, and the visual field needs to be selected again for amplification observation. Generally, the nano-scale organic hole can be effectively observed only under the vision field of ten thousand times, and the problems of long time consumption, time waste and the like exist in repeatedly selecting the vision field.
Case 2: the organic matter is amplified, when the organic matter exists in 6000-time vision field, the organic matter is amplified, but the organic hole does not develop in 120000-time vision field, the morphological characteristics of the organic matter are not easy to observe effectively, the organic matter needs to be reselected, and the problems of repeated vision field selection, long time consumption and the like exist.
At present, the research on the organic matter pore of the shale reservoir by using a field emission scanning electron microscope is widely accepted, but the technical method is not mature enough, has the vision field selection randomness and organic pore development limitation, and is not convenient enough in the observation mode. Firstly, the observation image based on the field emission scanning electron microscope has random view selection. Due to the fact that the imaging multiple is high, the observation visual field is small, the probability of repeatedly selecting the visual field to search for organic matter pores is increased for the problems that the selection of the position of an observation image is random and the like. In a fixed observation visual field, if the magnification is larger, the quantity of the observed substances is smaller, the probability of observing organic pores is smaller, and the visual field needs to be selected again to search for the organic pores. Secondly, organic pores develop on organic matter, and the types of different types of organic matter micro-components determine whether the organic pores develop or not. The organic matter on the visual field is enlarged, the condition that the machine hole does not develop can occur, and the form and the structural characteristics of the hole are difficult to be described finely. The field of view still needs to be reselected to search for organic matter.
Although the traditional scanning electron microscope imaging analysis technology for shale reservoir micropores is widely applied and has a good effect, the problems of view selection randomness and organic pore development limitation still exist at present. The method mainly comprises the steps that when the organic pore is observed by using a scanning electron microscope, the organic pore needs to be observed under a high-magnification vision field, the problems that the observation vision field is small, the organic pore is difficult to find and does not grow, the observation time is long and the like exist, the experiment and scientific research efficiency is reduced, and a method for quickly positioning the organic pore growth position is lacked.
In summary, the problems of the prior art are as follows: the traditional imaging analysis technology of the scanning electron microscope for the shale reservoir micropores has the problems that when the organic matter pores are observed by using the scanning electron microscope, the observation field is small, the difficulty in discovering the organic pores is high, the organic pores are not developed, the observation time is long and the like due to the fact that the organic matter pores need to be observed under the high-magnification field of view, and the experiment and scientific research efficiency is reduced.
The difficulty of solving the technical problems is as follows: at the current stage, the organic pore is observed by using a field emission scanning electron microscope under the condition of amplifying the vision field by tens of thousands of times, and the problem that the existing method for finding the organic pore by amplifying the vision field is difficult to solve, such as difficulty in finding the organic pore, long time consumption and the like.
The significance of solving the technical problems is as follows: the observation process is simplified, the experiment efficiency is effectively improved, and the purpose of saving time is achieved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a quantitative characterization method for rapidly determining organic matter pores based on a scanning electron microscope and application thereof.
The invention is realized in such a way that a quantitative characterization method for rapidly determining organic matter pores based on a scanning electron microscope comprises the following steps:
firstly, determining the distribution position of organic matters by using a scanning electron microscope;
secondly, determining the types of the microscopic components by using an energy spectrometer and the form of an organic matter;
thirdly, determining organic pores by using organic matter microscopic components;
and step four, determining the distribution position of the organic matters, determining the types of the microscopic components and determining the development condition of the organic pores.
Further, the sample selection of the quantitative characterization method for rapidly determining the organic matter pore based on the scanning electron microscope adopts a natural section sample preparation method to prepare a fresh section in the vertical layer.
Further, the sample preparation of the quantitative characterization method for rapidly determining organic matter pores based on the scanning electron microscope is as follows: after the sample is fixed, the sample is plated with gold at 20mA for 150 s.
Further, when the organic micro-components are detected under the scanning electron microscope based on the quantitative characterization method for rapidly determining organic pore space based on the scanning electron microscope, firstly, the organic matters are identified; then, according to the morphological characteristics of the organic matters, the state is presented; and determining the microscopic components by combining geological age.
In summary, the advantages and positive effects of the invention are: the method adopts a scanning electron microscope to identify the organic matter micro-components, and can effectively solve the problems that the existing fluorescence microscope is complex in manufacturing when used for observing organic matters, the eyes can be damaged in the using process, the structural details of the micro-components can not be observed when the organic matters are observed, and the like.
The method is used for rapidly positioning the development position of the shale reservoir organic matter pore, and qualitatively and quantitatively describing and evaluating the form and structural characteristics of the shale organic matter pore. The scanning electron microscope has the advantages of high magnification, strong stereoscopic impression of images and the like, and the sample preparation method is simple, and the enrichment mode, morphological characteristics and contact relation with minerals of each microscopic component can be directly observed.
Drawings
Fig. 1 is a flowchart of a quantitative characterization method for rapidly determining organic matter pores based on a scanning electron microscope according to an embodiment of the present invention.
Fig. 2 is a schematic view of a scanning electron microscope image of the sapropel group provided by the embodiment of the invention.
FIG. 3 is a spectrum of the sapropel group provided by the embodiment of the present invention.
FIG. 4 is a graph showing the effect of the organic pore development dominance micro-component provided by the embodiment of the invention.
Fig. 5 is a diagram of the effect provided by the embodiment of the invention and enlarged to 80000 times.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Aiming at the problems in the prior art, the invention provides a quantitative characterization method for rapidly determining organic matter pores based on a scanning electron microscope and application thereof, and the invention is described in detail below with reference to the accompanying drawings.
As shown in fig. 1, the method for rapidly determining the organic matter pore based on the scanning electron microscope according to the embodiment of the present invention includes the following steps:
s101: determining the distribution position of the organic matters by using a scanning electron microscope;
s102: determining the types of the microscopic components by using an energy spectrometer and the form of organic matters;
s103: determining organic pores by using organic matter microscopic components;
s104: determining the distribution position of organic matters, determining the types of microscopic components and determining the development condition of organic pores.
The quantitative characterization method for rapidly determining organic matter pores based on the scanning electron microscope specifically comprises the following steps:
(1) selecting a sample: and preparing a fresh section in the vertical layer by adopting a natural section sample preparation method, wherein the fresh section has good representativeness as possible.
(2) Sample preparation: after the sample was fixed, the sample was subjected to a plating process at an operating current of 20mA for a plating time of 150s in order to increase the conductivity.
(3) And (3) operating the machine for observation: when organic micro-components are researched under a scanning electron microscope, organic matters are firstly identified, then states are presented according to morphological characteristics of the organic matters, and then the micro-components are determined by combining geological ages.
(5) And (4) detecting energy spectrums.
(6) Statistics and analysis results, experimental equipment and working conditions: experimental equipment and working conditions: the FEIQuanta200F type field emission scanning electron microscope has the working voltage of 20kV and the working distance of 10 mm; the LeicaSCD500 type coating instrument has the working current of 20mA and the coating time of 150 s.
The technical solution of the present invention is further described below with reference to the accompanying drawings.
The quantitative characterization method for rapidly determining organic matter pores based on the scanning electron microscope specifically comprises the following steps:
firstly, determining the distribution position of organic matters by using a scanning electron microscope; and putting the prepared shale sample into an instrument, determining a rectangular observation area required by the research under a scanning electron microscope at low times, observing whether organic matters exist, and moving the visual field until the organic matters are found if the organic matters do not exist. Under the condition of a scanning electron microscope, the organic matters are dark and have obvious color difference with surrounding minerals.
Secondly, determining the types of the microscopic components by using an energy spectrometer and morphological characteristics of organic matters; under the premise of finding organic matters, organic microscopic components are determined by using a scanning electron microscope, and the microscopic components are determined by combining an energy spectrometer according to morphological characteristics of the organic matters and occurrence states. Identifying organic matters under an electron microscope:
set of sapropel: the image brightness is darkest, the image is mainly amorphous, has no fixed shape, is usually in the shape of strips, blocks and gaps, and can see air holes, asphalt pellet holes and casting mould holes; and the second is algal thallus, which has obvious biological characteristic appearance and various shapes, and is seen in biological pores. According to the analysis result of an energy spectrometer, the main chemical components of the sapropel group are C, SI and O (figure 3 and table 1).
Second, vitrinite: the image is darker in brightness, has the characteristics of compactness, uniformity, flatness, smoothness, strip shape or block shape with different widths, and the like, and is seen in a shell-shaped fracture (figure 2). The development of pores, the development of endogenous cracks, the visible contraction joints and the common casting holes. The components are simple, mainly C and O, wherein the content of C is higher and can reach 80-90%.
Third, chitin group: the imaging picture is dark, and the resin body is in a circular, oval or irregular shape with different sizes; the horniness bodies are distributed in the shale in a bent or strip shape; the sporophyte can be divided into megaspore and microspore, and under the scanning electron microscope, the sporophyte is mostly microspore, and is in the shape of flat sphere, thin and short thready, worm and the like. The energy spectrometer shows that the carbon and hydrogen content is high.
Fourthly, inert matter group: the image is brighter, mainly the filamentous body retains more plant tissue structures, is arranged in parallel layers, has a screen structure with a clear and tidy cross section, and is often filled with mineral substances to different degrees. The energy spectrum analysis is carried out on the sericin, and the content of C is between 80 and 90 percent.
As shown in fig. 3 and 4, spectrogram processing:
peaks not to be ignored
And (4) processing options: all analyzed elements (normalized)
Number of repetitions of 5
Standard samples:
TABLE 1 humic substances composition
Thirdly, determining organic pores by using organic matter microscopic components;
the saprolite group is found to be the most favorable microscopic component for organic pore development through research, the microscopic component is the second, and the chitin group and the inert component are not favorable for organic pore development. The fast positioning of organic matter pores can be realized by judging the sapropel group and the vitrinite group under the low-multiple vision field.
And step four, determining the distribution position of the organic matters, determining the types of the microscopic components and determining the development condition of the organic pores.
In a preferred embodiment of the present invention, when the organic pore is observed under a scanning electron microscope based on the method for determining the development position of the organic pore by the scanning electron microscope, the organic pore can be described finely according to the morphological characteristics of the organic pore, as shown in table 2.
TABLE 2
The technical effects of the present invention will be described in detail with reference to experiments.
The experimental case of the invention selects 7 sections of shale in south region of Ordos basin, which has good regional geological basic data, basic geochemical test data and the like, the organic matter content and maturity of the shale are moderate, the pore types are various and complex, including inter-granular (inner) pores, erosion pores, inter-granular pores, microcracks, organic matter pores and the like, and the invention is adopted to rapidly position and observe the organic matter pores of the shale reservoir.
Aiming at the example of fast identifying organic holes of long 7-section shale FY2-24 rock samples in south areas of Ordos basin, the specific implementation steps of the technical scheme adopted by the invention are as follows:
performing argon ion polishing treatment on the FY2-24 rock sample, then placing the sample under a scanning electron microscope instrument to observe the characteristics of the polished surface of the sample, and determining a rectangular observation area required by research under the low multiple of the scanning electron microscope
According to the requirement of observing the shale organic matter, after a rectangular observation area is determined, a proper scanning electron microscope image magnification factor is selected, wherein the magnification factor is required to ensure that the organic matter can be observed, and 2500 times is selected in the experiment in order to accurately identify the organic matter.
As shown in fig. 4, according to the morphological characteristics of the organic matter, the occurrence state and the geological age are presented; and determining the type of the organic matter micro-component in the field as a saprolite group by combining an energy spectrometer, wherein the organic matter micro-component is an organic pore development dominant micro-component.
As shown in fig. 5, it was observed that when the organic pore was enlarged to 80000 times, the development of the organic pore in the visual field was advantageous to describe the morphological characteristics and pore size of the organic pore precisely, and the pore size was quantitatively calculated.
According to the method, the shale reservoir organic hole scanning electron microscope image is analyzed, the position of the shale reservoir organic hole is determined by a new method and thought, the experimental time is effectively saved, the scientific research efficiency is improved, the technical problem that the observation difficulty of the shale reservoir organic hole is high in the prior art is solved by establishing the relation between organic matter micro-components and the organic hole, and a new organic hole research thought is provided.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. The method for rapidly determining the quantitative characterization of the organic matter pore based on the scanning electron microscope is characterized by comprising the following steps of:
firstly, determining the distribution position of organic matters by using a scanning electron microscope; selecting a sample of the quantitative characterization method for rapidly determining the organic matter pore based on the scanning electron microscope, and preparing a fresh section in a vertical layer by adopting a natural section sample preparation method;
the method specifically comprises the following steps: putting the prepared shale sample into an instrument, determining a required rectangular observation area under a low multiple of a scanning electron microscope, observing whether organic matters exist or not, and moving a visual field until the organic matters are found if the organic matters do not exist; under the condition of a scanning electron microscope, the organic matters are dark and have obvious color difference with surrounding minerals;
secondly, determining the types of the microscopic components by using an energy spectrometer and the form of an organic matter;
the method specifically comprises the following steps: determining organic microscopic components under a scanning electron microscope, presenting states according to morphological characteristics of organic matters, and determining the microscopic components by combining an energy spectrometer;
the organic matter recognition standard is as follows:
a sapropel group: the brightness of an imaging picture is dark, the organic matter form is in a strip shape, and the chemical components of the sapropel group are C, SI and O;
vitrinite group: the imaging graph has the characteristics of relatively low brightness, uniform, flat and smooth organic matter surface, strip or block shape with different widths and the like, and the content of C reaches 80-90 percent when seen in a shell-shaped fracture;
chitin group: the resin body is in a round shape, an oval shape and an irregular shape with different sizes; the horniness bodies are distributed in the shale in a bent or strip shape; the sporophyte can be divided into megaspore and microspore, and the microspore is mostly microspore under a scanning electron microscope, and is oblate spheroid, thin and short threadlike and vermicular;
inertinite group: the imaging picture is bright, the plant tissue structure is easy to see, and the C content is 80-90 percent;
thirdly, determining organic pores by using organic matter microscopic components;
fast positioning of organic matter pores is realized by judging and identifying sapropel groups and vitrinite groups under low-multiple vision field;
and step four, determining the distribution position of the organic matters, determining the types of the microscopic components and determining the development condition of the organic pores.
2. The method for rapidly determining the quantitative characterization of organic matter pore based on scanning electron microscope according to claim 1, wherein the sample preparation of the method for rapidly determining the quantitative characterization of organic matter pore based on scanning electron microscope is as follows: after the sample is fixed, the sample is plated with gold at 20mA for 150 s.
3. The quantitative characterization method for rapidly determining organic matter pores based on scanning electron microscope according to claim 1, wherein when organic micro-components are detected under a scanning electron microscope, the organic matter is firstly identified; then, according to the morphological characteristics of the organic matters, the state is presented; and determining the microscopic components by combining geological age.
4. The application of the scanning electron microscope-based quantitative characterization method for rapidly determining organic pores according to any one of claims 1 to 3 in organic pore identification.
5. Application of the scanning electron microscope-based quantitative characterization method for rapidly determining organic matter pores in shale gas exploration and development as claimed in any one of claims 1 to 3.
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