CN117420167B - Method for measuring years of deep land shale natural crack calcite filling - Google Patents
Method for measuring years of deep land shale natural crack calcite filling Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000000608 laser ablation Methods 0.000 claims abstract description 49
- 238000002679 ablation Methods 0.000 claims abstract description 44
- 239000000945 filler Substances 0.000 claims abstract description 44
- 238000009826 distribution Methods 0.000 claims abstract description 40
- 238000001514 detection method Methods 0.000 claims abstract description 28
- 238000005136 cathodoluminescence Methods 0.000 claims abstract description 11
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- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 238000009616 inductively coupled plasma Methods 0.000 claims description 4
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
- G01N23/2254—Measuring cathodoluminescence
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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
- G01N21/84—Systems specially adapted for particular applications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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Abstract
The invention relates to the technical field of oil and gas geology, and provides a method for measuring years of a deep land phase shale natural fracture calcite filler, which comprises the following steps: obtaining a core sample to be tested containing calcite filler; respectively manufacturing a cathode luminescent sheet and a laser sheet aiming at the same area of the core sample to be measured; observing the cathode luminescent sheet under the cathode luminescent condition to obtain a cathode luminescent image, and identifying and obtaining calcite distribution areas on the cathode luminescent image; mapping calcite distribution areas on the cathodoluminescence image onto a laser sheet to obtain a laser ablation area to be detected of the laser sheet, and calibrating a plurality of ablation points to be detected on the laser ablation area to be detected; and carrying out laser ablation on the ablation to-be-detected point, carrying out isotope detection on the obtained ablation product, and carrying out calcite filling material year detection based on an isotope detection result. The method can accurately calibrate the distribution ranges of the secondary calcite in different periods in different types of fillers of the deep land shale natural cracks.
Description
Technical Field
The invention relates to the technical field of oil and gas geology, in particular to a method for measuring years of a deep land shale natural fracture calcite filler.
Background
The land sedimentary basin in China develops a plurality of sets of organic shale, and mainly comprises 5 shale layers such as Songliao basin chalky system, quasi-Songli basin, three-pond lake basin two-fold system, erdos basin three-fold system, sichuan basin dwarf system, bohai bay, jiang Han and the like, east subsidence basin ancient system and the like. The Chinese land stratum generally undergoes stronger and more complex late-stage structural movement, the content of the brittle minerals of the shale rich in organic matters can reach more than 40%, and a foundation condition is laid for the extensive development and distribution of natural cracks of the shale oil system. The deep land shale has extremely poor physical properties, and the average porosity and permeability are respectively less than 5 percent and 0.1mD. Natural fractures are used as effective reservoir empty and main seepage channels of deep shale, and are important for the enrichment and high yield of shale oil.
The study of the formation time of cracks has important guiding significance for understanding the space-time matching relationship of shale oil generation, migration and aggregation. Current studies on crack formation time mainly include: (1) Determining the sequence of crack formation based on the cutting restriction relation of cracks in the core and outcrop hand information; (2) The formation time of the fracture is determined indirectly by the homogenization temperature of the fluid inclusions trapped in the fracture charge. However, the intersection of the multi-stage cracks in the core and the outcrop cannot be observed sometimes, the fluid inclusion cannot be always captured in the crack filling, and the research on the crack formation time is limited by practical data and samples.
In recent years, calcite laser in-situ U-Pb isotope dating has been developed into a mature dating technology, so that the absolute age of calcite filling in cracks can be determined, and the method has important oil-gas geology significance for analyzing the formation evolution of the cracks.
The related art has the following two defects in the aspect of annual measurement of crack calcite filling: (1) The annual testing procedure is complex in the current stage, firstly, standard targets with the diameters of 25mm and the thicknesses of 5mm are manufactured for crack filler samples by using epoxy resin, then, the surfaces of the targets are polished, and the annual testing targets are put into ultrapure water to be cleaned and dried by ultrasonic waves before formal testing; (2) Deep land shale undergoes complex diagenetic effects in long geological history, fluid sources are complex, natural cracks are mostly filled by multiple types of mineral cements except calcite, and standard targets can only be observed under the condition of reflected light of an optical microscope, so that the distribution range of calcite cannot be accurately identified, and the annual survey accuracy is affected.
Disclosure of Invention
The invention provides a method for measuring years of a calcite filling material for natural cracks of deep land shale, which is used for solving the defect that the distribution range of calcite cannot be accurately identified in the prior art, so that the accuracy of measuring years is affected.
The invention provides a method for measuring years of a deep land shale natural fracture calcite filler, which comprises the following steps:
obtaining a core sample to be tested containing calcite filler;
respectively manufacturing a cathode luminescent sheet and a laser sheet aiming at the same area of the core sample to be measured;
observing the cathode luminescent sheet under a cathode luminescent condition to obtain a cathode luminescent image, and identifying and obtaining a calcite distribution area on the cathode luminescent image;
mapping calcite distribution areas on the cathodoluminescence image onto the laser sheet to obtain a laser ablation area to be detected of the laser sheet, and calibrating a plurality of ablation points to be detected on the laser ablation area to be detected;
and carrying out laser ablation on the ablation to-be-detected point, carrying out isotope detection on the obtained ablation product, and carrying out calcite filling year detection based on an isotope detection result.
According to the method provided by the invention, the calcite distribution area on the cathode luminescence image is mapped onto the laser sheet to obtain a laser ablation area to be detected of the laser sheet, and a plurality of ablation points to be detected are calibrated on the laser ablation area to be detected, and the method comprises the following steps:
respectively carrying out single polarization and orthogonal light observation on the cathode luminescent sheet under a polarization microscope to obtain a single polarization image and an orthogonal light image;
and observing the laser sheet under transmitted light, combining the single polarized light image, the orthogonal light image and the cathode luminescence image, mapping the calcite distribution area onto the laser sheet to obtain a laser ablation area to be detected of the laser sheet, and calibrating a plurality of ablation points to be detected on the laser ablation area to be detected.
According to the method provided by the invention, before the laser ablation is carried out on the ablation to-be-detected point, the method further comprises the following steps:
and pre-ablating the to-be-ablated point by using a laser beam spot.
According to the method provided by the invention, the laser ablation is carried out on the ablation to-be-detected point, and isotope detection is carried out on the obtained ablation product, and the method comprises the following steps:
carrying out laser ablation on the point to be ablated by using a laser ablation system, and sending the obtained ablation product out of a sample cell by using helium;
and mixing the obtained degraded product with argon, and sending the mixture into an inductively coupled plasma mass spectrometer for isotope detection.
According to the method provided by the invention, the method for carrying out calcite filling yearly detection based on the isotope detection result comprises the following steps:
for the isotope detection results, NIST614 is adopted as an internal standard for correction, and 238 U/ 206 pb data is on the horizontal axis, 207 Pb/ 206 pb data is taken as a vertical axis, isoplot software is utilized to fit an isochrone, and the isochrone is matched withThe age of the lower intersection of the harmonic lines is the age of the calcite filling.
According to the method provided by the invention, the radius of the to-be-degraded measured points is 50-100 mu m, and the number of the to-be-degraded measured points is 40-60.
According to the method provided by the invention, the cathode luminescent sheet and the laser sheet are respectively manufactured for the same area of the core sample to be measured, and the method comprises the following steps:
cutting the core sample to be tested into a cuboid by using a cutting machine, and enabling a crack filler to be positioned at the center of the cuboid;
and sticking the cuboid onto a glass plate to respectively manufacture a cathode luminescent sheet and a laser sheet, wherein the thickness of the cathode luminescent sheet is 0.04mm, and the thickness of the laser sheet is 0.08-0.2mm.
According to the method provided by the invention, the length of the cuboid is 30-40mm, the width is 20-25mm, and the thickness is 10-20mm.
The method provided by the invention further comprises the following steps:
and identifying and obtaining different periods of the calcite filling based on the color shade of the calcite filling on the cathodoluminescent image.
According to the method for measuring years of the deep land shale natural fracture calcite filling material, cathode luminescent sheets and laser sheets are respectively manufactured aiming at the same region of a core sample to be measured; observing the cathode luminescent sheet under the cathode luminescent condition to obtain a cathode luminescent image, and identifying and obtaining calcite distribution areas on the cathode luminescent image; the calcite distribution area on the cathode luminous image is mapped onto the laser sheet to obtain a laser ablation area to be detected of the laser sheet, and a plurality of ablation points to be detected are calibrated on the laser ablation area to be detected, so that the calcite distribution range and the annual measurement points can be accurately identified, and the annual measurement accuracy is improved.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the following description will briefly explain the drawings used in the embodiments or the description of the prior art, and it is obvious that the drawings in the following description are some embodiments of the invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of a method for testing a deep land shale natural fracture calcite filler according to the present invention;
FIG. 2 is a microscopic image of a natural fracture calcite filler provided by the present invention;
FIG. 3 is a schematic diagram of annual results of calcite filler provided by the invention;
FIG. 4 is a microscopic image of a natural fracture multi-phase calcite filler provided by the present invention;
FIG. 5 is an SEM-CL image of a multi-stage calcite filler provided by the present invention;
FIG. 6 is a second schematic flow chart of the method for testing the natural fracture calcite filler of deep land shale.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The related art has the following two defects in the aspect of annual measurement of crack calcite filling: (1) The annual testing procedure is complex in the current stage, firstly, standard targets with the diameters of 25mm and the thicknesses of 5mm are manufactured for crack filler samples by using epoxy resin, then, the surfaces of the targets are polished, and the annual testing targets are put into ultrapure water to be cleaned and dried by ultrasonic waves before formal testing; (2) Deep land shale undergoes complex diagenetic effects in long geological history, fluid sources are complex, natural cracks are mostly filled by multiple types of mineral cements except calcite, and standard targets can only be observed under the condition of reflected light of an optical microscope, so that the distribution range of calcite cannot be accurately identified, and the annual survey accuracy is affected.
Aiming at the problems that the procedures of target making, polishing, cleaning and the like are complex, the distribution range of calcite in the multi-period filling material of the crack cannot be accurately selected, and the annual measurement point location cannot be accurately identified, so that the annual measurement accuracy is affected, the invention has the following conception in order to improve the annual measurement accuracy: respectively manufacturing a cathode luminescent sheet and a laser sheet aiming at the same area of the core sample to be measured; observing the cathode luminescent sheet under the cathode luminescent condition to obtain a cathode luminescent image, and identifying and obtaining calcite distribution areas on the cathode luminescent image; the calcite distribution area on the cathode luminous image is mapped onto the laser sheet to obtain a laser ablation area to be detected of the laser sheet, and a plurality of ablation points to be detected are calibrated on the laser ablation area to be detected, so that the calcite distribution range and the annual measurement points can be accurately identified, and the annual measurement accuracy is improved.
Based on the inventive concept, the invention provides a method for measuring years of a deep land shale natural fracture calcite filling material, which can be applied to an age measurement scene of the deep land shale natural fracture calcite filling material so as to improve the year measurement accuracy and has important oil-gas geological significance for analyzing the formation evolution of cracks.
The technical scheme of the present invention will be described in detail with reference to the accompanying drawings. Fig. 1 is a schematic flow chart of a method for testing years of a deep land shale natural fracture calcite filling, as shown in fig. 1, which comprises the following steps:
step 110, obtaining a core sample to be tested containing calcite filler;
step 120, respectively manufacturing a cathode luminescent sheet and a laser sheet aiming at the same area of the core sample to be tested;
step 130, observing the cathode luminescent sheet under the cathode luminescent condition to obtain a cathode luminescent image, and identifying and obtaining calcite distribution areas on the cathode luminescent image;
step 140, mapping calcite distribution areas on the cathodoluminescence image onto a laser sheet to obtain a laser ablation area to be detected of the laser sheet, and calibrating a plurality of ablation points to be detected on the laser ablation area to be detected;
and 150, performing laser ablation on the ablation to-be-detected point, performing isotope detection on the obtained ablation product, and performing calcite filling year detection on the basis of an isotope detection result.
Specifically, the core sample to be measured is a core sample which needs to measure the absolute age of the fracture calcite filler in the core sample, for example, the core sample to be measured can be a core fracture filler sample typical of a deep land-phase shale oil well in a block of China.
The natural fractures of the core sample to be tested are typically filled with various types of mineral bonds other than calcite, such as small particle quartz, large particle quartz, and the like. In the related art, the standard target can only be observed under the light emitted by an optical microscope, and the light-transmitting information of the filled minerals cannot be observed by using the transmitted light, so that the distribution range of calcite cannot be accurately identified, and the year measurement accuracy is affected.
In step 120 of the embodiment of the present invention, a cathode luminescent sheet and a laser sheet are respectively manufactured for the same region of the core sample to be measured. The cathode luminescent sheet and the laser sheet belong to the same area of the core sample to be measured, and can reflect the mineral characteristics of crack fillers in the area, for example, after a certain area is selected, the cathode luminescent sheet is firstly manufactured, and then the laser sheet is manufactured in the area.
In some embodiments, step 120 separately prepares a cathode luminescent sheet and a laser sheet for the same region of the core sample to be measured, and specifically includes:
cutting the core sample to be measured into a cuboid by using a cutting machine, and positioning a crack filler in the center of the cuboid;
and sticking the cuboid onto a glass plate to respectively prepare a cathode luminescent sheet and a laser sheet, wherein the thickness of the cathode luminescent sheet is 0.04mm, and the thickness of the laser sheet is 0.08-0.2mm.
Specifically, a cutting machine can be used for cutting a shale sample of the developing natural fracture filler, namely a core sample to be measured into cuboid small blocks, and the size of the cuboid small blocks can be flexibly selected according to actual test conditions, and for example, the shale sample can be cuboid small blocks with the length of 30-40mm, the width of 20-25mm and the thickness of 10-20mm. While the crack-filler is located substantially in the center of the cuboid.
Then, the cuboid small pieces are stuck on a glass plate by using an adhesive, such as 502 glue, and the cathode luminescent sheet with the thickness of 0.04mm is manufactured. And then manufacturing a laser sheet with the thickness of 0.08-0.2mm in the same area of the same cuboid small block, and simultaneously polishing the laser sheet on two sides to ensure that the surface of a sample is smooth so as to meet the subsequent laser ablation test.
After the cathodoluminescent sheet and the laser sheet are fabricated, step 130 is performed, and the cathodoluminescent sheet is observed under cathodoluminescent conditions to obtain a cathodoluminescent image, and the calcite distribution area on the cathodoluminescent image is identified.
Here, a nikon LV100N polarizing microscope with a CLF-2 cathodoluminescence apparatus may be used, and the cathodoluminescence system is activated to make the vacuum degree less than 0.003mbar, and the cathodoluminescence sheet is observed and photographed under cathodoluminescence to obtain a cathodoluminescence image. Due to the different colors of the various minerals, calcite distribution areas on the cathodoluminescent image can be identified by color. The orange-red area can be defined as calcite distribution area.
After the calcite distribution area on the cathodoluminescent image is obtained, step 140 is performed. Because the cathode luminescent sheet and the laser sheet are sampled in the same area of the core sample to be measured, the distribution range of calcite is the same on the cathode luminescent sheet and the laser sheet, so that the position mapping can be carried out according to the calcite distribution area on the cathode luminescent sheet, the calcite can be used as a laser ablation area to be measured at the same position of the laser sheet, and a plurality of ablation points to be measured are calibrated on the laser ablation area to be measured.
Here, in order to further improve the accuracy of the laser ablation test area and the positioning of the ablation test point, step 140 maps the calcite distribution area on the cathodoluminescence image onto the laser sheet to obtain the laser ablation test area of the laser sheet, and marks a plurality of ablation test points on the laser ablation test area, which specifically includes:
respectively carrying out single polarization and orthogonal light observation on a cathode luminescent sheet under a polarization microscope to obtain a single polarization image and an orthogonal light image;
observing the laser sheet under the transmitted light, combining the single polarized light image, the orthogonal light image and the cathode luminescent image, mapping the calcite distribution area onto the laser sheet to obtain a laser ablation area to be detected of the laser sheet, and calibrating a plurality of ablation points to be detected on the laser ablation area to be detected.
First, a single polarization image and an orthogonal light image are obtained by observing the cathode luminescence sheet under a polarization microscope. The single polarization image can reflect the texture characteristics of the natural crack filler under the microscope, the orthogonal light image can reflect the color characteristics of the natural crack filler under the microscope, and the single polarization image and the orthogonal light image can identify mineral substances such as calcite or quartz stone and the like of the crack filler.
On the basis, combining a calcite distribution area on a cathode luminescence image, observing a laser sheet under transmitted light, mapping the calcite distribution area onto the laser sheet to obtain a laser ablation area to be detected of the laser sheet, and calibrating a plurality of ablation points to be detected on the laser ablation area to be detected.
FIG. 2 is a microscopic image of the natural fissured calcite filler provided by the present invention, as shown in FIG. 2, where (a) in FIG. 2 is a single polarized image; (b) is an orthogonal light image; (c) Is a cathodoluminescent image from which calcite distribution areas can be identified; (d) The small circles in the test strip are a plurality of ablation test points marked on the laser sheet.
Preferably, the radius of the ablation to-be-detected points can be set to be 50-100 mu m, and 40-60 ablation to-be-detected points can be calibrated in the area with larger calcite distribution area as far as possible.
After the laser sheet is calibrated to degrade the point to be measured, step 150 may be performed. And carrying out laser ablation on the ablation to-be-detected point, carrying out isotope detection on the obtained ablation product, and carrying out calcite filling material year detection based on an isotope detection result.
The point to be ablated may be pre-ablated using the laser beam spot before performing step 150, the purpose of the pre-ablation being to eliminate potential contamination of the mineral surface on the laser sheet for more accurate age measurement.
A formal test of calcite filler age may then begin. Step 150 specifically includes:
carrying out laser ablation on the point to be ablated by using a laser ablation system, and sending the obtained ablation product out of a sample cell by using helium;
and mixing the obtained degraded product with argon, and sending the mixture into an inductive coupling plasma mass spectrometer for isotope detection.
The laser ablation system here may be, for example, a ASI RESOlution SE-S155 laser ablation system. The inductively coupled plasma mass spectrometer may be a Thermo Fisher iCAP-RQ inductively coupled plasma mass spectrometer.
After the isotope detection results are obtained, calcite filling years can be measured based on the isotope detection results. The method specifically comprises the following steps:
for isotope detection results, NIST614 is used as an internal standard for correction, and the acquired data is processed offline by using Iolite software, including selection of samples and blank signals and calculation of element content. FIG. 3 is a schematic diagram showing the annual results of calcite filler according to the present invention, as shown in FIG. 3, for 238 U/ 206 Pb data is on the horizontal axis, 207 Pb/ 206 pb data is taken as a vertical axis, isoplot software is used for fitting out an isochrone, and the isochrone and the isoplotteThe age of the lower intersection of the harmonic lines is the age of calcite filler.
Based on the above embodiment, considering that natural cracks in some areas develop multi-stage calcite filling, different stages of calcite filling can be identified based on the color shade of calcite filling above the cathodoluminescent image by the cathodoluminescent image obtained in step 130. Years can be measured for calcite of different periods separately.
The shade of color herein refers to the comparison between colors of different periods of calcite filling for the same cathodoluminescent image that contains multiple periods of calcite filling. And meanwhile, different periods of calcite filling are identified by combining the growth characteristics and the interpenetration relation of calcite crystals.
The method for measuring the years can be used for measuring the years of the filling of the calcite in different periods respectively. Pre-scan results for early calcite 238 U/ 206 The Pb ratio is less than 1, and the annual measurement requirement cannot be met; and the annual measurement result of the advanced calcite is 191+/-26 Ma. Further, calcite with different shades is verified as crack filler for two periods.
FIG. 4 is a microscopic image of a natural fracture multi-stage calcite filler provided by the present invention, as shown in FIG. 4, where (a) in FIG. 4 is a single polarization image of the multi-stage calcite filler; (b) an orthogonal light image of a multi-stage calcite filler; (c) A cathodoluminescent image of a multi-stage calcite charge from which it can be identified as multi-stage, wherein the dashed line is the parting line of the multi-stage calcite charge; (d) The small circles in the test strip are a plurality of ablation test points respectively calibrated on the laser sheet aiming at calcite filling in each period.
Fig. 5 is an SEM-CL image of the multi-stage calcite filler provided by the present invention. The SEM-CL image refers to a Scanning Electron Microscope (SEM) cathode fluorescence (CL) image, and the samples used in fig. 5 and 4 are the same sample, and as can also be seen in fig. 5, the calcite filling of the sample is multi-stage.
Fig. 6 is a second flow chart of a method for testing years of natural cracking calcite filling of deep land shale provided by the invention, as shown in fig. 6, the method for testing years of natural cracking calcite filling of deep land shale comprises the following steps:
s1, acquiring a shale natural fracture filler sample, namely a core sample to be measured.
S2, cutting the core sample to be detected into cuboid small blocks with the length of 30mm, the width of 25mm and the thickness of 10mm by using a cutting machine, and enabling crack fillers to be located at the center of the cuboid small blocks.
S3, sticking the cuboid onto a glass plate to respectively manufacture a cathode luminescent sheet and a laser sheet, wherein the thickness of the cathode luminescent sheet is 0.04mm, and the thickness of the laser sheet is 0.1mm.
And S4, observing the cathode luminescent sheet under the cathode luminescent condition to obtain a cathode luminescent image, and identifying and obtaining a calcite range, namely a calcite distribution area, on the cathode luminescent image.
And S5, mapping the calcite distribution area on the cathode luminescent image onto a laser sheet to obtain a laser ablation area to be detected of the laser sheet, and calibrating a plurality of ablation points to be detected on the laser ablation area to be detected.
S6, performing pre-ablation on the ablation to-be-detected point by using the laser beam spot.
S7, performing laser ablation on the ablation point to be detected by using a laser ablation system, and sending the obtained ablation product out of a sample cell by using helium; and mixing the obtained degraded product with argon, and sending the mixture into an inductive coupling plasma mass spectrometer for isotope detection.
S8, aiming at the isotope detection result, NIST614 is adopted as an internal standard for correction, and 238 U/ 206 pb data is on the horizontal axis, 207 Pb/ 206 pb data is taken as a vertical axis, isoplot software is used for fitting out an isochrone, and the isochrone and the isoplotteThe age of the lower intersection of the harmonic lines is the age of calcite filler.
The method provided by the embodiment of the invention can accurately calibrate the distribution ranges of the calcite in different periods in different types of fillers of deep land shale natural cracks, and overcomes the defect that the annual survey target cannot accurately identify the calcite. Natural cracks in deep land shale are important reservoir spaces and migration channels, and the research of the formation time of the cracks has important guiding significance for understanding space-time matching relations of shale oil generation, migration and aggregation.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. A method for yearly testing a deep land shale natural fracture calcite filler, comprising:
obtaining a core sample to be tested containing calcite filler;
respectively manufacturing a cathode luminescent sheet and a laser sheet aiming at the same area of the core sample to be measured;
observing the cathode luminescent sheet under a cathode luminescent condition to obtain a cathode luminescent image, and identifying and obtaining a calcite distribution area on the cathode luminescent image;
mapping calcite distribution areas on the cathodoluminescence image onto the laser sheet to obtain a laser ablation area to be detected of the laser sheet, and calibrating a plurality of ablation points to be detected on the laser ablation area to be detected;
performing laser ablation on the ablation to-be-detected point, performing isotope detection on the obtained ablation product, and performing calcite filling year measurement based on an isotope detection result;
mapping the calcite distribution area on the cathodoluminescence image onto the laser sheet to obtain a laser ablation area to be detected of the laser sheet, and calibrating a plurality of ablation points to be detected on the laser ablation area to be detected, wherein the method comprises the following steps:
respectively carrying out single polarization and orthogonal light observation on the cathode luminescent sheet under a polarization microscope to obtain a single polarization image and an orthogonal light image; the single polarization image is used for reflecting the texture characteristics of the natural crack filler under a microscope, the orthogonal light image is used for reflecting the color characteristics of the natural crack filler under the microscope, and the type of the natural crack filler is identified through the single polarization image and the orthogonal light image;
and observing the laser sheet under transmitted light, combining the single polarized light image, the orthogonal light image and the cathode luminescence image, mapping the calcite distribution area onto the laser sheet to obtain a laser ablation area to be detected of the laser sheet, and calibrating a plurality of ablation points to be detected on the laser ablation area to be detected.
2. The method of claim 1, wherein prior to laser ablating the ablation site, further comprising:
and pre-ablating the to-be-ablated point by using a laser beam spot.
3. The method of claim 1, wherein the laser ablating the site to be ablated and isotope detecting the resulting ablated product comprises:
carrying out laser ablation on the point to be ablated by using a laser ablation system, and sending the obtained ablation product out of a sample cell by using helium;
and mixing the obtained degraded product with argon, and sending the mixture into an inductively coupled plasma mass spectrometer for isotope detection.
4. The method of claim 1, wherein performing calcite filling yearly based on isotope detection results comprises:
for the isotope detection results, NIST614 is adopted as an internal standard for correction, and 238 U/ 206 pb data is on the horizontal axis, 207 Pb/ 206 pb data is taken as a vertical axis, isoplot software is utilized to fit an isochrone, and the isochrone is matched withThe age of the lower intersection of the harmonic lines is the age of the calcite filling.
5. The method according to any one of claims 1 to 4, wherein the radius of the ablation to-be-measured point is 50 to 100 μm, and the number of the ablation to-be-measured points is 40 to 60.
6. The method according to any one of claims 1-4, wherein the preparing a cathodoluminescent sheet and a laser sheet, respectively, for the same region of the core sample to be measured, comprises:
cutting the core sample to be tested into a cuboid by using a cutting machine, and enabling a crack filler to be positioned at the center of the cuboid;
and sticking the cuboid onto a glass plate to respectively manufacture a cathode luminescent sheet and a laser sheet, wherein the thickness of the cathode luminescent sheet is 0.04mm, and the thickness of the laser sheet is 0.08-0.2mm.
7. The method of claim 6, wherein the cuboid has a length of 30-40mm, a width of 20-25mm, and a thickness of 10-20mm.
8. The method of any one of claims 1-4, further comprising:
and identifying and obtaining different periods of the calcite filling based on the color shade of the calcite filling on the cathodoluminescent image.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017031056A (en) * | 2016-11-10 | 2017-02-09 | 住友電気工業株式会社 | Single crystal diamond |
| CN107655914A (en) * | 2017-09-11 | 2018-02-02 | 中国地质大学（武汉） | Method of discrimination based on the BIFhosted gold deposit oxidation-reduction quality of scheelite cathodoluminescence feature in Skarn Deposit |
| CN110376273A (en) * | 2019-07-15 | 2019-10-25 | 中国石油天然气股份有限公司 | A kind of laser in-situ uranium lead isotope dating methods for ancient Marine Carbonate Rocks |
| CN111007141A (en) * | 2019-12-04 | 2020-04-14 | 中国石油天然气股份有限公司 | Calcite mineral laser uranium-lead isotope dating process |
| CN111398571A (en) * | 2020-05-19 | 2020-07-10 | 中南大学 | Mineral exploration method for rapidly judging mineral potential of skarn deposit by using zircon |
| CN112113990A (en) * | 2019-06-20 | 2020-12-22 | 中国石油化工股份有限公司 | Method and system for identifying diagenetic fluid source based on micro-area in-situ element distribution |
| CN112485239A (en) * | 2020-10-26 | 2021-03-12 | 中国地质大学（武汉） | Ancient fluid comprehensive analysis method related to oil and gas reservoir |
| CN112946780A (en) * | 2021-02-07 | 2021-06-11 | 中国石油天然气股份有限公司 | Method and device for determining sliding fracture active period |
| CN113624830A (en) * | 2021-08-04 | 2021-11-09 | 中国科学院地质与地球物理研究所 | In-situ micro-area calcite U-Pb dating method |
| CN114705830A (en) * | 2022-03-22 | 2022-07-05 | 中南大学 | Tracing method for concealed granite mass in thick-layer limestone coverage area |
| CN115855597A (en) * | 2022-11-26 | 2023-03-28 | 中南大学 | Method for distinguishing mining specificity of granite mass by using apatite |
-
2023
- 2023-12-14 CN CN202311718080.XA patent/CN117420167B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017031056A (en) * | 2016-11-10 | 2017-02-09 | 住友電気工業株式会社 | Single crystal diamond |
| CN107655914A (en) * | 2017-09-11 | 2018-02-02 | 中国地质大学（武汉） | Method of discrimination based on the BIFhosted gold deposit oxidation-reduction quality of scheelite cathodoluminescence feature in Skarn Deposit |
| CN112113990A (en) * | 2019-06-20 | 2020-12-22 | 中国石油化工股份有限公司 | Method and system for identifying diagenetic fluid source based on micro-area in-situ element distribution |
| CN110376273A (en) * | 2019-07-15 | 2019-10-25 | 中国石油天然气股份有限公司 | A kind of laser in-situ uranium lead isotope dating methods for ancient Marine Carbonate Rocks |
| CN111007141A (en) * | 2019-12-04 | 2020-04-14 | 中国石油天然气股份有限公司 | Calcite mineral laser uranium-lead isotope dating process |
| CN111398571A (en) * | 2020-05-19 | 2020-07-10 | 中南大学 | Mineral exploration method for rapidly judging mineral potential of skarn deposit by using zircon |
| CN112485239A (en) * | 2020-10-26 | 2021-03-12 | 中国地质大学（武汉） | Ancient fluid comprehensive analysis method related to oil and gas reservoir |
| CN112946780A (en) * | 2021-02-07 | 2021-06-11 | 中国石油天然气股份有限公司 | Method and device for determining sliding fracture active period |
| CN113624830A (en) * | 2021-08-04 | 2021-11-09 | 中国科学院地质与地球物理研究所 | In-situ micro-area calcite U-Pb dating method |
| CN114705830A (en) * | 2022-03-22 | 2022-07-05 | 中南大学 | Tracing method for concealed granite mass in thick-layer limestone coverage area |
| CN115855597A (en) * | 2022-11-26 | 2023-03-28 | 中南大学 | Method for distinguishing mining specificity of granite mass by using apatite |
Non-Patent Citations (2)
| Title |
|---|
| Norma Betania Palacios-García等.U–Pb calcite dating of brittle deformation in Permian carbonates within the Chicomuselo fold and thrust belt, SE Mexico.Journal of Structural Geology.2023,第171卷104863. * |
| 陈家旭等.应用方解石激光原位U-Pb同位素定年确定多旋回叠合盆地油气成藏绝对时间——以塔里木盆地塔河油田为例.石油与天然气地质.2021,第42卷(第6期),1365-1375. * |
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