CN111610212B - Scanning electron microscope sample positioning device and method for oil and gas reservoir transformation experiment - Google Patents
Scanning electron microscope sample positioning device and method for oil and gas reservoir transformation experiment Download PDFInfo
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- 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
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- 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]
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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
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- H—ELECTRICITY
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- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/02—Details
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- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
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Abstract
The invention relates to a scanning electron microscope sample positioning device and a method for an oil and gas reservoir transformation experiment, wherein the sample positioning device comprises a sample stage base, a connecting bolt and a positioning sample stage, the sample stage base is used for being directly connected with a scanning electron microscope, and the positioning sample stage is used for bearing a tested rock sample; the top of the cylindrical positioning sample table is provided with a plurality of positioning reference points, observation points before and after an oil and gas reservoir transformation experiment can be accurately and quickly positioned through the plurality of reference points, the experiment operation steps are optimized, the micro-morphology analysis and comparison before and after the sample reservoir transformation experiment are quickly carried out, and the effectiveness of reservoir transformation is conveniently and accurately evaluated.
Description
Technical Field
The invention relates to the technical field of oil and gas reservoir transformation experiments, in particular to a scanning electron microscope sample positioning device and method in the oil and gas reservoir transformation experiments.
Background
The analysis technology of a scanning electron microscope (scanning electron microscope for short) is a test analysis technology for researching the characteristics of micro-morphology, components and the like in a micro-nano scale, and is widely applied to the fields of materials science, biology, medicine, geology and the like. The reservoir transformation technology is used for transforming and treating petroleum and natural gas reservoirs by adopting processes of acidification, water injection, fracturing and the like, and is an important method and means for improving oil and gas recovery efficiency and productivity in the development process of oil and gas fields. In the process of reservoir transformation evaluation, in order to clarify the sensitivity of different minerals (quartz, feldspar, clay minerals and the like) to different working fluids (acidizing fluid, water, fracturing fluid and the like), a scanning electron microscope is required to be used for positioning and observing the same mineral or the same point in the same sample before and after a reservoir transformation experiment, so that the change of the mineral characteristics and the difference of the mineral characteristics before and after the experiment are subjected to microscopic representation, and the effectiveness of the reservoir transformation is evaluated.
However, because the scanning electron microscope is usually used to study features of micro-morphology, components and the like in micro-nano scale, and mineral particles in a rock sample are small and need to be amplified several hundred to several thousand times or even several ten thousand times under the scanning electron microscope, the positioning and searching technology of the sample in the existing scanning electron microscope is usually to judge the position of the sample according to the observed micro-features in the field of view in a single experimental process. In addition, more importantly, when the microscopic morphology features of the minerals change before and after the reservoir transformation experiment, whether the observation points before and after the experiment are the same cannot be judged, so that the effectiveness of the reservoir transformation cannot be evaluated.
In addition, in research processes such as feldspar corrosion simulation experiments related to the formation mechanism of oil and gas sandstone reservoirs, calcite and dolomite corrosion simulation experiments related to the formation mechanism of carbonate reservoirs and the like, in order to evaluate the experimental effect more accurately, the same mineral (feldspar, calcite, dolomite and the like) in the sample needs to be subjected to comparative observation and analysis before and after the experiment. Therefore, a device and a method which can be used for accurately and rapidly positioning and comparing the same mineral or the same point in the same sample before and after a scanning electron microscope research oil and gas reservoir transformation experiment are needed to be solved.
Disclosure of Invention
The invention aims to provide a scanning electron microscope sample positioning device and method for an oil and gas reservoir transformation experiment aiming at the defects of the prior art, and the scanning electron microscope sample positioning device and method can be used for accurately and quickly positioning the same mineral or the same point in the same sample before and after the reservoir transformation experiment.
The technical scheme adopted by the invention for realizing the purpose is as follows: the invention discloses a scanning electron microscope sample positioning device for an oil and gas reservoir transformation experiment, which comprises: the device comprises a sample table base, a positioning sample table and a connecting bolt connected with the sample table base and the positioning sample table;
the base of the sample stage is used as a base for positioning the sample stage, the lower part of the base is connected with a scanning electron microscope, the upper part of the base is connected with the positioning sample stage by using bolts, a radial base alignment marking and a circumferential base alignment marking are arranged from the center to the edge of the top surface of the base, and a screw hole is formed in the center of the top surface, wherein the radial base alignment marking is arranged along the radial direction from the screw hole in the center of the top surface, and the radial base alignment marking is vertical to the circumferential base alignment marking;
the sample table base is fixedly connected with the positioning sample table through a connecting bolt, the positioning sample table is fixed on the sample table base, and the positioning sample table can be connected with and separated from the sample table base through rotation;
the positioning sample table is cylindrical, the top surface of the positioning sample table is provided with three positioning reference point marks (A, B, C) distributed on the top surface of the cylinder wall, the side surfaces of the positioning sample table are eight hollow columns uniformly distributed, a bolt for fixing a sample is distributed above and below each hollow column respectively, a sample table positioning mark line is arranged at the bottom of each hollow column, the bottom surface of each hollow column is eight uniformly distributed fan-shaped hollows, and the center of each hollow column is a screw hole;
the positioning sample table is in a hollow cylindrical shape, so that a rock sample can be fixed and protected, the influence (such as microcracks and the like) on a rock reservoir in the manual operation process is prevented, particularly, after the rock sample is subjected to a reservoir transformation experiment, the sample is looser than before, the positioning sample table can play a role in fixing and protecting, the original state of the transformation experiment is really preserved, and the objectivity and the effectiveness of reservoir evaluation are improved;
the arrangement position of the circumferential base alignment mark line on the radial base alignment mark line is the outer radius of the cylindrical positioning sample table, when the positioning sample table is tightly attached to the sample table frame, the side edge of the cylindrical positioning sample table is just aligned with the circumferential base alignment mark line, and when the cylindrical positioning sample table is not aligned with the circumferential base alignment mark line, the connection between the positioning sample table and the sample table frame is deviated, so that a worker is reminded to check the connection mode and correct the installation relation;
the three positioning reference points (A, B, C) are uniformly distributed on the top surface of the cylinder wall, in the other embodiment, the number of the positioning reference points can be increased, the positioning accuracy can be increased, the reference point closest to the observation point P can be preferentially selected as the looking direction of the scanning electron microscope, and the observation points before and after the oil and gas reservoir transformation experiment are positioned more accurately and quickly;
the invention discloses a scanning electron microscope sample positioning method for an oil and gas reservoir transformation experiment, which comprises the following steps:
step (1): putting a standard plunger rock sample for reservoir transformation experiments into the positioning sample table from the upper port of the positioning sample table, enabling the top surface of the sample to be approximately parallel to the top surface of the positioning sample table, and fixing the sample by using a sample fixing bolt so that the sample and the positioning sample table do not have relative displacement;
step (2): connecting the positioning sample stage and the sample stage base by using a connecting bolt; loading a sample before a reservoir transformation experiment is completed, and putting the sample into a scanning electron microscope to perform microstructure analysis on the sample before the reservoir transformation experiment;
and (3): reading and recording the coordinate of a positioning reference point (A, B, C) on the top surface of the positioning sample platform under a scanning electron microscope as ((x) A ，y A )、(x B ，y B )、(x C ，y C ) Reading and recording the coordinates (x) of the observation point (P) P ，y P ) (ii) a Analyzing the microscopic morphology of the sample before the reservoir transformation experiment by using a scanning electron microscope, and sequentially reading and recording the coordinates of each analysis point;
and (4): screwing down the positioning sample table to separate the positioning sample table from the sample table base and the connecting bolt; putting the rock sample and the positioning sample table into a reservoir stratum transformation experimental device together, keeping the rock sample and the positioning sample table from relative displacement, and performing a reservoir stratum transformation experiment;
and (5): taking out the sample after the reservoir transformation experiment and the positioning sample table, and repeating the step (2); loading the sample after the reservoir transformation experiment is completed, and putting the sample into a scanning electron microscope to perform microscopic analysis work of reservoir transformation evaluation;
and (6): reading and recording the coordinates of a top surface positioning reference point (A, B, C) of the positioning sample table under a scanning electron microscope as ((x' A ，y’ A )，(x’ B ，y’ B )，(x’ C ，y’ C ) Coordinates ((x) of a positioning reference point (A, B, C)) read and recorded before a reservoir reformation experiment are utilized A ，y A )、(x B ，y B )、(x C ，y C ) And P coordinate (x) of point to be observed P ，y P ) And new coordinates ((x ') of a locating reference point (A, B, C) of the top surface of the locating sample platform after the reservoir reconstruction experiment' A ，y’ A )，(x’ B ，y’ B )，(x’ C ，y’ C ) Calculating a coordinate (x ') of a point to be observed P after a reservoir transformation experiment' P ，y’ P ) Comprises the following steps:
and (7): inputting P coordinate (x ') of point to be observed' P ，y’ P ) Finding a point P to be observed after the reservoir transformation experiment, correcting the point P by combining with stable minerals (such as quartz and the like), and completing the sample micro-morphology analysis after the reservoir transformation experiment by utilizing a scanning electron microscope;
the step (2) further comprises reading an initial included angle alpha between the positioning sample stage and the sample stage base through a base alignment marking on the sample stage base and/or a sample stage positioning marking of the positioning sample stage;
the step (5) further comprises reading an included angle alpha 'between the positioning sample stage and the base of the sample stage again, and comparing the included angle alpha' with the included angle alpha to preliminarily judge the approximate position of the observation point and improve the positioning efficiency of the observation point;
certainly, for convenience, in another embodiment, four quadrant regions can be divided on the base of the sample stage, and the quadrant region where the observation is to be performed is judged according to the included angle relationship;
in another embodiment, the top periphery of the sample stage and/or the bottom periphery of the side surface of the positioning sample stage are/is further provided with angle measurement scales, and the relative position of the sample stage and the positioning sample stage during rotary connection can be accurately positioned by reading the angle value of the alignment marking of the radial base on the positioning sample stage and/or the angle value of the positioning marking of the sample stage on the positioning sample stage before and after an experiment, so that the observation area before and after the experiment can be quickly determined, the same point position can be accurately positioned, and the working efficiency is greatly improved;
in another embodiment, the connecting bolt is further provided with a limiting block, the limiting block can divide the bolt into two sections, the upper section is connected with the positioning sample stage, the lower section is connected with the sample stage base, the limiting block respectively limits the connecting length of the connecting bolt, the positioning sample stage and the sample stage base, the position relation between the alignment marking of the radial base and the positioning marking of the sample stage before and after an experiment is ensured, and the efficiency of determining an observation area is further improved;
the length of the connecting bolt is preferably 1/2-4/5 of the depth of the threaded hole for respectively embedding the sample rack and positioning the sample platform;
the sample stage base and the positioning sample stage can be fixedly connected in a connecting mode of clamping, nesting, clamping and the like besides the connecting bolt;
the beneficial effects of the invention are: the invention has simple structure and convenient operation, adopts the structure of the sample table base, the connecting bolt and the positioning sample table, is convenient for holding and connecting the core sample, and arranges angle scale values on the periphery of the top surface of the sample table base and/or the periphery of the bottom of the side surface of the positioning sample table; the angle value is read through the base of the sample table and the marked lines arranged on the positioning sample table, and the observation point can be preliminarily positioned according to the relation between the front angle and the rear angle;
the connecting bolt is limited by the limiting block, so that the connecting length of the connecting bolt, the positioning sample stage and the sample stage is limited, the position relation between the alignment mark line of the radial base and the positioning mark line of the sample stage before and after the experiment is ensured, the operation steps of the experiment are further optimized, and the efficiency of determining the observation area is improved;
the positioning sample table disclosed by the invention adopts a hollow structure, a plurality of sample fixing bolts are arranged on hollow columns on the side surfaces, and a core sample is fixed through the sample fixing bolts, so that the sample and the positioning sample table are prevented from moving; the top surface of the cylindrical positioning sample table is provided with a plurality of reference points, the coordinates of the reference points before and after reservoir transformation are read and recorded, and the coordinates of the observation points after reservoir transformation are calculated through coordinate parameters, so that the accurate and rapid positioning and comparative observation of the same mineral or the same point in the same sample before and after an oil and gas reservoir transformation experiment is researched by utilizing a scanning electron microscope, and the effectiveness of reservoir transformation is evaluated;
the invention also combines stable minerals (such as quartz and the like) to carry out correction, further improves the positioning accuracy, and utilizes a scanning electron microscope to complete the sample micro-morphology analysis after the reservoir transformation experiment; in the operation process, the rock sample and the positioning sample table are placed into the reservoir stratum transformation experiment device together, no relative displacement between the rock sample and the positioning sample table is kept, and a reservoir stratum transformation experiment is carried out; the rock core sample is protected, the rock core is prevented from being influenced by human activities, particularly after the reservoir transformation, the rock sample is relatively loose, the sample is protected, the accuracy of the reservoir transformation experiment is improved, and the reservoir transformation effectiveness can be objectively evaluated;
the method can be used for, but not limited to, carrying out accurate and rapid positioning and comparative observation on the same mineral or the same point in the same sample before and after the oil and gas reservoir transformation experiment by utilizing a scanning electron microscope, and can be used for similar experiments needing the scanning electron microscope to carry out positioning and comparative observation on the same point before and after the experiment, such as feldspar corrosion simulation experiment in the oil and gas sandstone reservoir formation mechanism research, positioning and comparative experiment before and after corrosion of metals such as steel and the like.
Drawings
FIG. 1 is an overall configuration diagram of the apparatus of the present invention;
FIG. 2 is a table diagram of a positioning sample for loading a sample to be tested;
FIG. 3 is a view of the positioning sample stage and the sample stage base;
FIG. 4 is a diagram of a finished product after a sample to be tested is loaded;
FIG. 5 is a schematic view of a top surface of a positioning stage and a schematic view of a positioning reference point;
FIG. 6 is an overall configuration diagram of another embodiment of the apparatus of the present invention;
fig. 7 is a schematic structural view of the coupling bolt.
Reference numerals: 1. a sample stage base; 1.1. aligning the radial base with the marked line; 1.2. a screw hole; 1.3 aligning the circumferential base with the marked line; 2. a connecting bolt; 2.1 a limiting block; 3. positioning a sample stage; 3.1 positioning a marking line of the sample table; 3.2. a bolt for fixing the sample; 3.3. the top surface locates the reference point.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. 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 shown in fig. 1, the scanning electron microscope sample positioning device for hydrocarbon reservoir reformation experiments of the present invention includes: the device comprises a sample table base 1, a positioning sample table 3 and a connecting bolt 2 connected with the sample table base 1 and the positioning sample table 3;
the sample stage base 1 is used as a base for positioning the sample stage 3, the lower part of the sample stage base is connected with a scanning electron microscope, the upper part of the sample stage base is connected with the positioning sample stage 3 by using a bolt 2, a radial base alignment mark line 1.1 and a circumferential base alignment mark line 1.3 are arranged from the center to the edge of the top surface of the sample stage base, a screw hole 1.2 is arranged in the center of the top surface, the radial base alignment mark line 1.1 is arranged along the radial direction from the screw hole 1.2 in the center of the top surface, and the radial base alignment mark line 1.1 is vertical to the circumferential base alignment mark line 1.3;
the sample table base 1 is fixedly connected with the positioning sample table 3 through a connecting bolt 2, the positioning sample table 3 is fixed on the sample table base 1, and the positioning sample table 3 can be connected with and separated from the sample table base 1 through rotation;
the positioning sample table 3 is cylindrical, the top surface of the positioning sample table is three top surface positioning reference points 3.3 (A, B, C) distributed on the top surface of the cylinder wall, the side surface of the positioning sample table is eight hollow columns which are uniformly distributed, a bolt 3.2 for fixing a sample is respectively distributed above and below each hollow column, a sample table positioning mark line 3.1 is arranged at the bottom of each hollow column, the bottom surface of each hollow column is eight fan-shaped hollow sections which are uniformly distributed, and the center of each hollow column is a screw hole;
the positioning sample table 3 is in a hollow cylindrical shape, so that a rock sample can be fixed and protected, the influence (such as microcracks and the like) on a rock reservoir in the manual operation process is prevented, particularly, after the rock sample is subjected to a reservoir transformation experiment, the sample is looser than before, the positioning sample table 3 can play a role in fixing and protecting, the original state of the transformation experiment is really preserved, and the objectivity and the effectiveness of reservoir evaluation are improved;
the setting position of the circumferential base alignment mark line 1.3 on the radial base alignment mark line 1.1 is the outer radius of the cylindrical positioning sample stage 3, when the positioning sample stage 3 is tightly attached to the sample stage frame 1, the side edge of the cylindrical positioning sample stage 3 is just aligned with the circumferential base alignment mark line 1.3, and when the cylindrical positioning sample stage 3 is not aligned with the circumferential base alignment mark line 1.3, the connection between the positioning sample stage 3 and the sample stage frame 1 is deviated, so that a worker is reminded to check the connection mode and correct the installation relationship;
the three top surface positioning reference points 3.3 (A, B, C) are uniformly distributed on the top surface of the cylinder wall, in another embodiment, the number of the top surface positioning reference points 3.3 can be increased, so that the positioning accuracy can be increased, the top surface positioning reference point 3.3 closest to the observation point P can be preferentially selected as the looking direction of the scanning electron microscope, and the observation points before and after the oil and gas reservoir transformation experiment are positioned more accurately and quickly;
as shown in fig. 2, 3, 4 and 5, the scanning electron microscope sample positioning method for the oil and gas reservoir transformation experiment comprises the following steps:
step (1): putting a standard plunger rock sample for reservoir transformation experiments into the positioning sample table 3 from an upper port, enabling the top surface of the sample to be approximately parallel to the top surface of the positioning sample table 3, fixing the sample by using a sample fixing bolt 3.2, and enabling the sample and the positioning sample table 3 not to have relative displacement;
step (2): connecting the positioning sample stage 3 with the sample stage base 1 by using a connecting bolt 2; loading a sample before a reservoir transformation experiment is completed, and putting the sample into a scanning electron microscope to perform microstructure analysis on the sample before the reservoir transformation experiment;
and (3): reading and recording the coordinate of a positioning reference point 3.3 (A, B, C) on the top surface of the positioning sample platform under a scanning electron microscope as ((x) x A ，y A )、(x B ，y B )、(x C ，y C ) Reading and recording the coordinates (x) of the observation point (P) P ，y P ) (ii) a Analyzing the microscopic morphology of the sample before the reservoir transformation experiment by using a scanning electron microscope, and sequentially reading and recording the coordinates of each analysis point;
and (4): screwing off the positioning sample stage 3 to separate the positioning sample stage 3 from the sample stage base 1 and the connecting bolt 2; putting the rock sample and the positioning sample table 3 into a reservoir stratum transformation experimental device together, keeping the rock sample and the positioning sample table 3 from relative displacement, and performing a reservoir stratum transformation experiment;
and (5): taking out the sample after the reservoir transformation experiment and the positioning sample table, and repeating the step (2); loading the sample after the reservoir transformation experiment is completed, and putting the sample into a scanning electron microscope to perform microscopic analysis work of reservoir transformation evaluation;
and (6): the coordinates of the top surface positioning reference point 3.3 (A, B, C) of the positioning sample stage 3 were read and recorded under a scanning electron microscope as ((x' A ，y’ A )，(x’ B ，y’ B )，(x’ C ，y’ C ) Coordinates ((x) of the locating reference point 3.3 (A, B, C)) read and recorded before reservoir reformation experiment were used A ，y A )、(x B ，y B )、(x C ，y C ) And P coordinate (x) of point to be observed P ，y P ) And new coordinates ((x ') of a locating sample table top surface locating reference point 3.3 (A, B, C) after reservoir reconstruction experiment' A ，y’ A )，(x’ B ，y’ B )，(x’ C ，y’ C ) Obtaining P coordinate (x ') of point to be observed after reservoir transformation experiment' P ，y’ P ) Comprises the following steps:
and (7): inputting P coordinate (x ') of point to be observed' P ，y’ P ) Finding a point P to be observed after the reservoir transformation experiment, correcting the point P by combining with stable minerals (such as quartz and the like), and completing the sample micro-morphology analysis after the reservoir transformation experiment by utilizing a scanning electron microscope;
the step (2) further comprises reading an initial included angle alpha of the relative relation between the positioning sample stage 3 and the sample stage base 1 through a base alignment mark line 1.1 on the sample stage base 1 and/or a sample stage positioning mark line 3.1 of the positioning sample stage 3;
the step (5) further comprises reading the included angle α ' between the positioning sample stage 3 and the sample stage base 1 again, and comparing the included angle α ' with the included angle α to preliminarily determine the approximate position of the observation point, so as to improve the positioning efficiency of the observation point, for example, in a certain experiment, if the initial included angle α is 10 °, the included angle α ' after the reservoir reforming experiment is 170 °, the worker can determine the opposite direction of the point P to be observed after the reservoir reforming experiment at the initial position; certainly, for convenience, in another embodiment, four quadrant regions can be divided on the sample stage base 1, and the quadrant region where the observation is to be performed is determined according to the included angle relationship;
as shown in fig. 6, in another embodiment, the top periphery of the sample stage base 1 and/or the bottom periphery of the side surface of the positioning sample stage 3 are further provided with angle measurement scales, and by reading the angle value of the radial base alignment mark line 1.1 on the positioning sample stage 3 before and after the experiment and/or the angle value of the sample stage positioning mark line 3.1 on the positioning sample stage 3 on the sample stage base 1, the relative position of the sample stage base 1 and the positioning sample stage 3 during the rotational connection can be accurately positioned, so that the observation area before and after the experiment can be quickly determined, the same point position can be accurately positioned, and the working efficiency can be greatly improved;
as shown in fig. 7, in another embodiment, a limiting block 2.1 is further disposed on the connecting bolt 2, the limiting block 2.1 can divide the bolt 2 into two sections, an upper section is connected with the positioning sample stage 3, a lower section is connected with the sample stage base 1, the limiting block 2.1 respectively limits the length of the connecting bolt 2 connected with the positioning sample stage 3 and the sample stage base 1, so as to ensure the positional relationship between the radial base alignment mark 1.1 and the sample stage positioning mark 3.1 before and after an experiment, and further improve the efficiency of determining an observation area;
the length of the connecting bolt 2 is preferably 1/2-4/5 of the depth of the threaded hole respectively embedded into the sample table base 1 and the positioning sample table 3;
the sample stage base 1 and the positioning sample stage 3 can be fixedly connected in a connecting mode of clamping, nesting, clamping and the like besides the connecting bolt 2;
the device and the method can be used for similar experiments which need a scanning electron microscope to position and observe the same point before and after the experiment, such as feldspar corrosion simulation experiment in the formation mechanism research of oil and gas sandstone reservoir, positioning comparison experiment before and after corrosion of metals such as steel and the like, and the like.
The above embodiments are only for illustrating the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention accordingly, and not to limit the protection scope of the present invention accordingly. All equivalent changes and modifications made according to the spirit of the present disclosure should be covered within the scope of the present disclosure.
Claims (7)
1. The utility model provides a scanning electron microscope sample positioner for oil and gas reservoir reforms transform experiment which characterized in that: the sample positioning device comprises a sample stage base (1), a connecting bolt (2) and a positioning sample stage (3), wherein the bottom of the sample stage base (1) is directly connected with a scanning electron microscope, and the top of the sample stage base is fixedly connected with the positioning sample stage (3) through the connecting bolt (2); the positioning sample table (3) is cylindrical, a sample table positioning mark line (3.1) is arranged at the bottom edge of the side wall of the positioning sample table (3), a radial base aligning mark line (1.1) is arranged on the top surface of the sample table base (1), the position of a test point can be preliminarily judged through the relative position of the radial base aligning mark line (1.1) and the sample table positioning mark line (3.1) of the positioning sample table (3), a plurality of sample fixing bolts (3.2) are arranged on the side wall of the positioning sample table (3), a rock test sample can be fixed in the positioning sample table by adjusting the tightness of the sample fixing bolts (3.2), a plurality of top surface positioning reference points (3.3) are arranged at the top of the cylindrical positioning sample table (3), observation points before and after oil and gas reservoir transformation can be accurately positioned through the plurality of top surface positioning reference points (3.3), and sample microscopic morphology analysis and comparison are carried out; the top surface of the sample table base (1) is also provided with a circumferential base alignment marking (1.3), and the circumferential base alignment marking (1.3) is vertical to the radial base alignment marking (1.1); an angle scale value is further arranged in the circumferential direction of the top of the sample table base (1) and the circumferential direction of the bottom of the side wall of the positioning sample table (3), and the rotating included angle between the positioning sample table (3) and the sample table base (1) is read through a radial base alignment marking (1.1) on the sample table base (1) and a sample table positioning marking (3.1) of the positioning sample table (3), so that the position of the observation point can be preliminarily judged conveniently; the side surface of the positioning sample table (3) is provided with eight hollow columns which are uniformly distributed, and a sample fixing bolt (3.2) is distributed above and below each hollow column respectively; the bottom surface of the positioning sample table (3) is eight uniformly distributed fan-shaped hollows, and the center position of the positioning sample table is a threaded hole (1.2) used for being connected with the connecting bolt (2).
2. The scanning electron microscope sample positioning device for oil and gas reservoir transformation experiments according to claim 1, characterized in that: the connecting bolt (2) both ends all are provided with the external screw thread, the top center of sample platform base (1) with the bottom center of location sample platform (3) all is provided with screw hole (1.2), can realize through the rotation location sample platform (3) with the connection and the separation of sample platform base (1).
3. The scanning electron microscope sample positioning device for oil and gas reservoir transformation experiments according to claim 1, characterized in that: and carrying out primary positioning on the observation point by recording the angle values of the front and the back times.
4. A positioning method of a scanning electron microscope sample positioning device for oil and gas reservoir transformation experiments, which is used for any one of claims 1 to 3, is characterized in that: the positioning method comprises the following steps: step (1): putting a standard plunger rock sample for reservoir transformation experiments into the positioning sample table (3) from an upper port of the positioning sample table (3), enabling the top surface of the sample to be approximately parallel to the top surface of the positioning sample table (3), and fixing the sample by using a sample fixing bolt (3.2) so that the sample and the positioning sample table (3) do not have relative displacement;
step (2): the positioning sample stage (3) and the sample stage base (1) are connected by a connecting bolt (2)Loading a sample before a reservoir transformation experiment is completed, and putting the sample into a scanning electron microscope to perform microstructure analysis on the sample before the reservoir transformation experiment; and (3): reading and recording the coordinate (x) of the positioning reference point A, B, C of the top surface of the positioning sample platform under the scanning electron microscope A ，y A )、(x B ，y B )、(x C ，y C ) Reading and recording the coordinate of the point P to be observed as (x) P ，y P ) Analyzing the microscopic morphology of the sample before the reservoir transformation experiment by using a scanning electron microscope, and sequentially reading and recording the coordinates of each analysis point;
and (4): screwing off a positioning sample table (3), separating the positioning sample table (3) from a sample table base (1) and a connecting bolt (2), putting a rock sample and the positioning sample table (3) into a reservoir stratum reconstruction experiment device, keeping the rock sample and the positioning sample table from relative displacement, and performing a reservoir stratum reconstruction experiment;
and (5): taking out the sample after the reservoir transformation experiment and the positioning sample table, repeating the step (2), completing the loading of the sample after the reservoir transformation experiment, and putting the sample into a scanning electron microscope for microscopic analysis work of the reservoir transformation evaluation;
and (6): reading and recording the coordinate of the positioning reference point A, B, C of the top surface of the positioning sample table (3) to be (x ') under a scanning electron microscope' A ，y’ A )，(x’ B ，y’ B )，(x’ C ，y’ C ) Using the coordinates (x) of the positioning reference point A, B, C read and recorded before the reservoir reconstruction experiment A ，y A )、(x B ，y B )、(x C ，y C ) And the coordinates (x) of the point P to be observed P ，y P ) And new coordinates (x ') of the locating sample platform top surface locating reference point A, B, C after reservoir reconstruction experiment' A ，y’ A )，(x’ B ，y’ B )，(x’ C ，y’ C ) Obtaining the coordinate (x ') of the point P to be observed after the reservoir transformation experiment' P ，y’ P ) Comprises the following steps:
x p '＝[(y C '-y A ')(x' B 2 -x B 2 +x A 2 -x' A 2 +2x P (x B -x A )+y' B 2 -y B 2 +y A 2 -y' A 2 +2y P (y B -y A ))
-(y B '-y A ')(x' C 2 -x C 2 +x A 2 -x' A 2 +2x P (x C -x A )+y' C 2 -y C 2 +y A 2 -y' A 2 +2y P (y C -y A ))]/2((x' B -x' A )(y' C -y' A )-(x' C -x' A )(y' B -y' A ))，
y p '＝[(x C '-x A ')(x' B 2 -x B 2 +x A 2 -x' A 2 +2x P (x B -x A )+y' B 2 -y B 2 +y A 2 -y' A 2 +2y P (y B -y A ))-(x B '-x A ')(x' C 2 -x C 2 +x A 2 -x' A 2 +2x P (x C -x A )+y' C 2 -y C 2 +y A 2 -y' A 2 +2y P (y C -y A ))]/2((y' B -y' A )(x' C -x' A )-(y' C -y' A )(x' B -x' A ))；
and (7): inputting the coordinate (x ') of the point P to be observed' P ，y’ P ) Namely, the point P to be observed after the reservoir reforming experiment can be accurately positioned, and the microscopic morphology analysis of the sample after the reservoir reforming experiment is completed by utilizing a scanning electron microscope.
5. The positioning method according to claim 4, characterized in that: the step (2) also comprises the step of reading an initial included angle alpha between the positioning sample stage (3) and the sample stage base (1) through a radial base alignment marking (1.1) on the sample stage base (1) and a sample stage positioning marking (3.1) of the positioning sample stage (3); and the step (5) further comprises reading the included angle alpha ' between the positioning sample stage (3) and the sample stage base (1) again, and preliminarily judging the approximate position of the observation point by comparing the included angle alpha ' with the included angle alpha '.
6. The positioning method according to claim 4, characterized in that: the sample stage base (1) can be further divided into four quadrant areas, and the quadrant area where the point to be observed is located is judged according to the included angle relation.
7. The positioning method according to claim 4, characterized in that: the step (7) further comprises correcting in combination with a stable mineral, wherein the stable mineral comprises quartz.
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