CN112782227B - Method and system for measuring oil-containing distribution of rock - Google Patents
Method and system for measuring oil-containing distribution of rock Download PDFInfo
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- CN112782227B CN112782227B CN201911085631.7A CN201911085631A CN112782227B CN 112782227 B CN112782227 B CN 112782227B CN 201911085631 A CN201911085631 A CN 201911085631A CN 112782227 B CN112782227 B CN 112782227B
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Abstract
The invention provides a method and a system for measuring oil-containing distribution of rock. The method comprises the following steps: fixing an oil-bearing rock sample on a sample table; adjusting the sample stage to enable the upper surface of the oil-bearing rock sample to be positioned on a focal plane of the focused scanning electron beam; continuously moving the sample stage to make the focused scanning electron beam spot on the oil-bearing rock sample to form a dot matrix, and acquiring oil-bearing current data of each point in the dot matrix; generating an oil-containing current two-dimensional distribution image according to the oil-containing current data of each point; removing crude oil in the oil-containing rock sample to obtain a deoiled rock sample; continuously moving the sample stage to make a focused scanning electron beam dot on the deoiled rock sample to form a dot matrix, and acquiring deoiling current data of each point in the dot matrix; generating a two-dimensional distribution image of the oil removing current according to the oil removing current data of each point; the oil-containing two-dimensional distribution image of the rock is obtained according to the oil-containing current two-dimensional distribution image and the deoiling current two-dimensional distribution image, and the oil-containing distribution characteristics of the rock can be accurately and quickly obtained.
Description
Technical Field
The invention relates to the field of oil-containing rock determination, in particular to a method and a system for determining oil-containing distribution of rock.
Background
Shale oil resources in China have great potential and are likely to become key resources for increasing the production of main petroleum in storage for decades. The traditional methods for evaluating the oil content of shale oil rock are pyrolysis, chloroform asphalt extraction and the like, the rock is often crushed into powder, the oil content in a sample can be obtained, but the analysis result is a number, and the characteristics of oil content distribution and the like cannot be obtained. Rock often has very strong heterogeneity, and the difference of heterogeneity has been destroyed to the powder with a rock core, and a figure often is difficult to represent the oiliness condition of a rock that the heterogeneity is stronger.
Disclosure of Invention
The embodiment of the invention mainly aims to provide a method and a system for measuring oil-containing distribution of rocks so as to obtain accurate and rapid oil-containing distribution characteristics of the rocks.
In order to achieve the above object, an embodiment of the present invention provides a method for determining oil content distribution of a rock, including:
fixing an oil-bearing rock sample on a sample table;
adjusting the sample stage to enable the upper surface of the oil-bearing rock sample to be positioned on a focal plane of the focused scanning electron beam;
continuously moving the sample stage to make the focused scanning electron beam spot on the oil-bearing rock sample to form a dot matrix, and acquiring oil-bearing current data of each point in the dot matrix;
generating an oil-containing current two-dimensional distribution image according to the oil-containing current data of each point;
removing crude oil in the oil-containing rock sample to obtain a deoiled rock sample;
continuously moving the sample stage to make the focused scanning electron beam dot on the deoiled rock sample to form a dot matrix, and acquiring deoiling current data of each point in the dot matrix;
generating a deoiling current two-dimensional distribution image according to the deoiling current data of each point;
obtaining a two-dimensional distribution initial image of the current according to the two-dimensional distribution image of the oil-containing current and the two-dimensional distribution image of the deoiling current;
and converting the current two-dimensional distribution initial image into a rock oil-containing two-dimensional distribution image.
The embodiment of the invention also provides a system for measuring the oil-containing distribution of the rock, which comprises:
the device comprises a sample table, a scanning electron gun, an ammeter, a fixing device, a sample table adjusting device, a crude oil removing device and a processor, wherein the ammeter is connected with the sample table;
the fixing device is used for fixing the oil-bearing rock sample on the sample table;
the crude oil removing device is used for removing crude oil in the oil-containing rock sample to obtain a deoiled rock sample;
scanning electron guns are used for: emitting a focused scanning electron beam to form a dot matrix on the petroliferous sample; emitting a focused scanning electron beam to dot on the deoiled rock sample to form a dot matrix;
sample platform adjusting device is used for: adjusting the sample stage to enable the upper surface of the oil-bearing rock sample to be positioned on a focal plane of the focused scanning electron beam; continuously moving the sample stage to make the focused scanning electron beam spot on the petroliferous sample to form a dot matrix; continuously moving the sample stage to make the focused scanning electron beam dot on the deoiled rock sample to form a dot matrix;
the current meter is used for: acquiring oil-containing current data of each point in the dot matrix; acquiring deoiling current data of each point in the dot matrix;
the processor is configured to: generating an oil-containing current two-dimensional distribution image according to the oil-containing current data of each point; generating a deoiling current two-dimensional distribution image according to the deoiling current data of each point; obtaining a two-dimensional distribution initial image of the current according to the two-dimensional distribution image of the oil-containing current and the two-dimensional distribution image of the deoiling current; and converting the current two-dimensional distribution initial image into a rock oil-containing two-dimensional distribution image.
The method and the system for measuring the oil-containing distribution of the rock firstly adjust a sample stage, enable the upper surface of an oil-containing rock sample fixed on the sample stage to be positioned on a focal plane of a focusing scanning electron beam, then continuously move the sample stage to enable the focusing scanning electron beam to form a dot matrix on the oil-containing rock sample, obtain oil-containing current data of each point in the dot matrix, and then generate an oil-containing current two-dimensional distribution image according to the oil-containing current data of each point; continuously moving the sample stage to make the focused scanning electron beam spot on the deoiling rock sample without crude oil to form a dot matrix, and generating a deoiling current two-dimensional distribution image according to the deoiling current data of each point in the dot matrix; and finally, obtaining a rock oil-containing two-dimensional distribution image according to the oil-containing current two-dimensional distribution image and the deoiling current two-dimensional distribution image, so that the accurate and quick rock oil-containing distribution characteristics can be obtained.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a flow chart of a method for determining oil content distribution in rock according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a system for determining oil content distribution of rocks in an embodiment of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As will be appreciated by one skilled in the art, embodiments of the present invention may be embodied as a system, apparatus, device, method, or computer program product. Accordingly, the present disclosure may be embodied in the form of: entirely hardware, entirely software (including firmware, resident software, micro-code, etc.), or a combination of hardware and software.
In view of the fact that the prior art is difficult to obtain the oil-bearing condition of a rock with strong heterogeneity, the embodiment of the invention provides a method for measuring the oil-bearing distribution of the rock so as to obtain the accurate and rapid oil-bearing distribution characteristics of the rock. The present invention will be described in detail below with reference to the accompanying drawings.
FIG. 1 is a flow chart of a method for determining oil content distribution in rock according to an embodiment of the invention. As shown in figure 1, the method for measuring the oil-containing distribution of the rock comprises the following steps:
s101: and fixing the oil-bearing rock sample on a sample table.
The oil-bearing rock sample can be a shale sample, a hydrocarbon source rock sample, a mudstone sample, a tight sandstone sample, a tight carbonate rock sample and the like. The rock sample is mainly characterized in that micro-nano pores are formed in the rock sample in a large quantity, a certain amount of crude oil is filled in the pores, or kerogen is contained in the pores, and crude oil is adsorbed in the kerogen.
In specific implementation, the oil-bearing rock sample can be fixed on the sample table through fixing glue, and the surface of the fixing glue is coated with conductive glue. The fixing glue can adopt epoxy resin.
S102: and adjusting the sample stage to enable the upper surface of the oil-bearing rock sample to be positioned on a focal plane of the focused scanning electron beam.
Before executing S102, the method may further include: the oil-bearing rock samples were mechanically and ion polished to obtain smooth surfaces. The mechanical polishing may allow the upper and lower surfaces of the oil-bearing rock sample to be parallel to ensure that the upper surface of the oil-bearing rock sample, which is ultimately placed on the sample stage, is parallel to the ground. The ion polishing can adopt argon ion polishing to obtain a micro-nano level flat surface, and a high-resolution rock oil-containing two-dimensional distribution image can be obtained in the later period.
S103: and continuously moving the sample stage to make the focused scanning electron beam point on the oil-bearing rock sample to form a dot matrix, and acquiring oil-bearing current data of each point in the dot matrix.
Before executing S103, the method may further include: adjusting the parameter setting of the focusing scanning electron beam, and testing and calibrating the current of the focusing scanning electron beam by using a Faraday cup until the current of the focusing scanning electron beam reaches a preset current value; setting the scanning range and the testing lattice of the focused scanning electron beam on the samples (oil-bearing rock samples and deoiled rock samples). The Faraday cup is positioned on the sample table, so that the test and calibration are convenient.
When S103 is executed, the dwell time of the focused scanning electron beam at each point may be set to ensure that electrons are accumulated at a certain point; and setting a time interval for dotting the focusing scanning electron beam, wherein the time interval is matched with the residence time of the electron beam at each point and the moving time of the sample stage, so that a test period is formed.
S104: and generating an oil-containing current two-dimensional distribution image according to the oil-containing current data of each point.
S105: and removing the crude oil in the oil-containing rock sample to obtain a deoiled rock sample.
In one embodiment, removing crude oil from an oil-bearing rock sample comprises: and carrying out heating drying treatment or polar solvent extraction treatment on the petroliferous rock sample to remove the crude oil.
The heating and drying treatment can be carried out by adopting various modes such as a muffle furnace, microwaves, lasers, an oven and the like; the polar solvent extraction treatment of the oil-bearing rock sample comprises the following steps: reversely immersing the upper surface of the petroliferous rock sample in a polar solvent for crude oil cleaning; and drying the oil-bearing rock sample subjected to crude oil cleaning. The polar solvent may include one or any combination of chloroform, dichloromethane, methanol, benzene, and petroleum ether.
S106: and continuously moving the sample stage to make the focused scanning electron beam dot on the deoiled rock sample to form a dot matrix, and acquiring deoiling current data of each point in the dot matrix.
Wherein, the lattice position in S106 is the same as the lattice position in S103; the scanning range of the focused scanning electron beam on the deoiled rock sample is the same as that of the focused scanning electron beam on the deoiled rock sample. For the same position point, the resistivity before and after oil washing obviously changes, and the current data also obviously changes, so that the oil-containing condition can be calculated according to the two changes.
S107: and generating a two-dimensional distribution image of the oil removing current according to the oil removing current data of each point.
S108: and obtaining a current two-dimensional distribution initial image according to the oil-containing current two-dimensional distribution image and the deoiling current two-dimensional distribution image.
S109: and converting the current two-dimensional distribution initial image into a rock oil-containing two-dimensional distribution image.
And the staff can subsequently acquire a series of data such as surface average value, oil-containing area connectivity and the like through the oil-containing two-dimensional distribution image of the rock. Where the area average is the ratio of the oil-containing region to the total region.
As can be seen from the process shown in fig. 1, in the method for determining the oil-containing distribution of the rock according to the embodiment of the present invention, the sample stage is adjusted, the upper surface of the oil-containing rock sample fixed on the sample stage is located on the focal plane of the focused scanning electron beam, the sample stage is continuously moved to make the focused scanning electron beam spot on the oil-containing rock sample to form a dot matrix, oil-containing current data of each point in the dot matrix is obtained, and then an oil-containing current two-dimensional distribution image is generated according to the oil-containing current data of each point; continuously moving the sample stage to make the focused scanning electron beam dot on the deoiling rock sample without crude oil to form a dot matrix, and generating a deoiling current two-dimensional distribution image according to the deoiling current data of each point in the dot matrix; and finally, obtaining a rock oil-containing two-dimensional distribution image according to the oil-containing current two-dimensional distribution image and the deoiling current two-dimensional distribution image, so that the accurate and quick rock oil-containing distribution characteristics can be obtained.
The specific process of the embodiment of the invention is as follows:
1. a black mudstone sample in an Ordos basin is taken, the kerogen maturity Ro is about 0.75 percent, and the interior of the sample contains certain free hydrocarbon.
FIG. 2 is a schematic diagram of a system for determining oil content distribution of rocks in an embodiment of the invention. As shown in fig. 2, a portion of a scanning electron gun 1, a focused scanning electron beam 3, a petroliferous sample 4, a fixing glue 5, a conductive glue 6, a faraday cup 7, a metal sample stage 8 and an aluminum sample stage 9 are all located in a vacuum chamber 2.
2. The black mudstone sample is processed by cutting the sample into 1cm x 0.5cm oily rock samples 4, and the oily rock samples 4 are adhered to an aluminum sample table 9 by a fixing device with a fixing glue 5 (such as AB glue). After the fixing glue 5 is cured, coating conductive glue 6 (such as conductive silver glue powder) on the surface of the fixing glue 5, performing surface mechanical polishing by using a Leica TXP lapping all-in-one machine, and performing surface argon ion polishing by using RES 102 equipment to obtain a polished sample.
3. And (3) current calibration of the focusing scanning electron beam 3 is carried out, and the Faraday cup 7 positioned on the metal sample table 8 is utilized to carry out electron beam current calibration and test, so that the beam stability of the electron beam is adjusted. The accelerating voltage of the scanning electron gun 1 is 10kV, and the beam current is 0.8nA.
4. The sample stage adjusting device vertically adjusts the aluminum sample stage 9 so that the upper surface of the oil-bearing rock sample 4 is positioned on the focal plane of the focused scanning electron beam 3. In the present embodiment, when the working distance of the upper surface of the oil-bearing rock sample 4 from the electron tube of the scanning electron gun 1 is 4mm, the upper surface of the oil-bearing rock sample 4 is located on the focal plane of the focused scanning electron beam 3.
5. The sample stage adjusting device continuously moves the metal sample stage 8 to make the focused scanning electron beam point on the petroliferous sample to form a dot matrix, and the galvanometer acquires oil-containing current data of each point in the dot matrix.
The lattice area is about 10 μm × 10 μm, and dots are formed at intervals of 100nm in the horizontal direction to form a 100 × 100 lattice. Setting the dwell time of the focusing scanning electron beam to be 30 mus, automatically moving to the next point after each point is printed, and testing point by point.
6. And the processor generates an oil-containing current two-dimensional distribution image according to the oil-containing current data of each point.
7. And removing the crude oil in the oil-bearing rock sample by using the crude oil removing device to obtain the deoiled rock sample.
During specific implementation, the sample is still adhered to the aluminum sample table 9, the upper surface of the sample is reversely immersed into the mixed liquid of hot chloroform and methanol with a reflux device for crude oil cleaning and soaking for 12 hours, and the magnetic stirring is used for continuously stirring the bottom of the liquid, so that the continuous washing of the fresh extract is ensured. The ratio of chloroform to methanol in the mixed solution is 9:1. and removing crude oil on the surface and then drying.
8. The sample stage adjusting device continuously moves the sample stage to make the focused scanning electron beam point on the deoiled rock sample to form a dot matrix, and the galvanometer acquires the deoiled current data of each point in the dot matrix.
9. The processor generates a two-dimensional distribution image of the deoiling current according to the deoiling current data of each point, and obtains a two-dimensional distribution initial image of the current according to the two-dimensional distribution image of the oil-containing current and the two-dimensional distribution image of the deoiling current.
To sum up, the method for determining the oil-containing distribution of the rock according to the embodiment of the invention comprises the steps of firstly adjusting a sample stage, positioning the upper surface of an oil-containing rock sample fixed on the sample stage on a focal plane of a focused scanning electron beam, then continuously moving the sample stage to make the focused scanning electron beam spot on the oil-containing rock sample to form a dot matrix, obtaining oil-containing current data of each point in the dot matrix, and then generating an oil-containing current two-dimensional distribution image according to the oil-containing current data of each point; continuously moving the sample stage to make the focused scanning electron beam dot on the deoiling rock sample without crude oil to form a dot matrix, and generating a deoiling current two-dimensional distribution image according to the deoiling current data of each point in the dot matrix; and finally, obtaining a rock oil-containing two-dimensional distribution image according to the oil-containing current two-dimensional distribution image and the deoiling current two-dimensional distribution image, so that the accurate and quick rock oil-containing distribution characteristics can be obtained.
Based on the same inventive concept, the embodiment of the invention also provides a system for measuring the oil-containing distribution of the rock, and as the principle of solving the problems of the system is similar to the method for measuring the oil-containing distribution of the rock, the implementation of the system can be referred to the implementation of the method, and repeated parts are not repeated.
As shown in fig. 2, the system for determining oil distribution in rock comprises:
the device comprises a sample table, a scanning electron gun, an ammeter, a fixing device, a sample table adjusting device, a crude oil removing device and a processor, wherein the ammeter is connected with the sample table;
the fixing device is used for fixing the oil-bearing rock sample on the sample table;
the crude oil removing device is used for removing crude oil in the oil-containing rock sample to obtain a deoiled rock sample;
scanning electron guns are used for: emitting a focused scanning electron beam to form a dot matrix on the petroliferous sample; emitting a focused scanning electron beam to dot on the deoiled rock sample to form a dot matrix;
sample platform adjusting device is used for: adjusting the sample stage to enable the upper surface of the oil-bearing rock sample to be positioned on a focal plane of the focused scanning electron beam; continuously moving the sample stage to make the focused scanning electron beam dot on the oil-bearing rock sample to form a dot matrix; continuously moving the sample stage to make the focused scanning electron beam dot on the deoiled rock sample to form a dot matrix;
the current meter is used for: acquiring oil-containing current data of each point in the dot matrix; acquiring deoiling current data of each point in the dot matrix;
the processor is configured to: generating an oil-containing current two-dimensional distribution image according to the oil-containing current data of each point; generating a two-dimensional distribution image of the oil removing current according to the oil removing current data of each point; obtaining a two-dimensional distribution initial image of the current according to the two-dimensional distribution image of the oil-containing current and the two-dimensional distribution image of the deoiling current; and converting the current two-dimensional distribution initial image into a rock oil-containing two-dimensional distribution image.
In one embodiment, the method further comprises the following steps:
and the polishing device is used for carrying out mechanical polishing and ion polishing on the oil-containing rock sample.
In one embodiment, the fixing device is specifically configured to:
fixing the oil-bearing rock sample on a sample table by using fixing glue;
and coating the conductive glue on the surface of the fixing glue.
In one embodiment, the crude removal unit is specifically configured to:
reversely immersing the upper surface of the petroliferous rock sample in a polar solvent for crude oil cleaning;
and drying the oil-bearing rock sample subjected to crude oil cleaning.
In one embodiment, the polar solvent comprises one or any combination of chloroform, dichloromethane, methanol, benzene, and petroleum ether.
To sum up, the system for measuring the oil-containing distribution of the rock in the embodiment of the invention firstly adjusts the sample stage, so that the upper surface of the oil-containing rock sample fixed on the sample stage is positioned on the focal plane of the focused scanning electron beam, then continuously moves the sample stage to make the focused scanning electron beam spot on the oil-containing rock sample to form a dot matrix, obtains oil-containing current data of each point in the dot matrix, and then generates an oil-containing current two-dimensional distribution image according to the oil-containing current data of each point; continuously moving the sample stage to make the focused scanning electron beam dot on the deoiling rock sample without crude oil to form a dot matrix, and generating a deoiling current two-dimensional distribution image according to the deoiling current data of each point in the dot matrix; and finally, obtaining a rock oil-containing two-dimensional distribution image according to the oil-containing current two-dimensional distribution image and the deoiling current two-dimensional distribution image, so that the accurate and quick rock oil-containing distribution characteristics can be obtained.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A method for determining oil-bearing distribution of rock, which is characterized by comprising the following steps:
fixing an oil-bearing rock sample on a sample table;
adjusting a sample stage to enable the upper surface of the oil-bearing rock sample to be positioned on a focal plane of a focusing scanning electron beam;
continuously moving the sample stage to make the focused scanning electron beam point on the petroliferous sample to form a dot matrix, and acquiring oil-bearing current data of each point in the dot matrix;
generating an oil-containing current two-dimensional distribution image according to the oil-containing current data of each point;
removing crude oil in the oil-bearing rock sample to obtain a deoiled rock sample;
continuously moving the sample stage to make the focused scanning electron beam dot on the deoiled rock sample to form a dot matrix, and acquiring deoiling current data of each point in the dot matrix;
generating a deoiling current two-dimensional distribution image according to the deoiling current data of each point;
obtaining a two-dimensional distribution initial image of the current according to the two-dimensional distribution image of the oil-containing current and the two-dimensional distribution image of the deoiling current;
converting the current two-dimensional distribution initial image into a rock oil-containing two-dimensional distribution image;
fixing the oil-bearing rock sample on the sample stage comprises:
fixing the oil-bearing rock sample on a sample table through fixing glue;
and coating conductive glue on the surface of the fixing glue.
2. The method for determining oil-containing distribution in rock according to claim 1, wherein before adjusting the sample stage, the method further comprises:
and carrying out mechanical polishing and ion polishing on the oil-containing rock sample.
3. The method for determining oil-bearing distribution of rock as claimed in claim 1, wherein removing crude oil from the oil-bearing rock sample comprises:
reversely immersing the upper surface of the petroliferous rock sample in a polar solvent for crude oil cleaning;
and drying the oil-bearing rock sample subjected to crude oil cleaning.
4. The method of determining oil content distribution in rock according to claim 3,
the polar solvent comprises one or any combination of chloroform, dichloromethane, methanol, benzene and petroleum ether.
5. A system for determining oil distribution in rock, comprising: the device comprises a sample table, a scanning electron gun, an ammeter, a fixing device, a sample table adjusting device, a crude oil removing device and a processor, wherein the ammeter is connected with the sample table;
the fixing device is used for fixing the oil-bearing rock sample on the sample table;
the crude oil removing device is used for removing crude oil in the oil-bearing rock sample to obtain a deoiled rock sample;
the scanning electron gun is configured to: emitting a focused scanning electron beam to dot on the oil-bearing rock sample to form a dot matrix; emitting a focused scanning electron beam to dot on the deoiled rock sample to form a dot matrix;
the sample stage adjusting device is used for: adjusting a sample stage to enable the upper surface of the oil-bearing rock sample to be positioned on a focal plane of a focusing scanning electron beam; continuously moving the sample stage to make the focused scanning electron beam point on the petroliferous sample to form a dot matrix; continuously moving the sample stage to make the focused scanning electron beam dot on the deoiled rock sample to form a dot matrix;
the current meter is used for: acquiring oil-containing current data of each point in the dot matrix; acquiring deoiling current data of each point in the dot matrix;
the processor is configured to: generating an oil-containing current two-dimensional distribution image according to the oil-containing current data of each point; generating a deoiling current two-dimensional distribution image according to the deoiling current data of each point; obtaining a two-dimensional distribution initial image of the current according to the two-dimensional distribution image of the oil-containing current and the two-dimensional distribution image of the deoiling current; converting the current two-dimensional distribution initial image into a rock oil-containing two-dimensional distribution image;
the fixing device is specifically used for:
fixing the oil-bearing rock sample on a sample table through fixing glue;
and coating conductive glue on the surface of the fixing glue.
6. The system for determining oil-bearing distribution of rock of claim 5, further comprising:
and the polishing device is used for carrying out mechanical polishing and ion polishing on the oil-containing rock sample.
7. The system for determining oil-bearing distribution of rock of claim 5, wherein the crude oil removal unit is specifically configured to:
reversely immersing the upper surface of the petroliferous rock sample in a polar solvent for crude oil cleaning;
and drying the oil-bearing rock sample subjected to crude oil cleaning.
8. The system for determining oil-containing distribution in rock according to claim 7,
the polar solvent comprises one or any combination of chloroform, dichloromethane, methanol, benzene and petroleum ether.
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