CN107939387B - A method for making microscopic rock network model - Google Patents
A method for making microscopic rock network model Download PDFInfo
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- CN107939387B CN107939387B CN201711123139.5A CN201711123139A CN107939387B CN 107939387 B CN107939387 B CN 107939387B CN 201711123139 A CN201711123139 A CN 201711123139A CN 107939387 B CN107939387 B CN 107939387B
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- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B49/00—Testing the nature of borehole walls; Formation testing; Methods or apparatus for obtaining samples of soil or well fluids, specially adapted to earth drilling or wells
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Abstract
本发明公开了一种微观岩石网络模型制作方法，其中包括：提取孔喉通道，对孔喉通道中的孔隙和喉道进行分离，获得孔隙图案和喉道图案，分别制作孔隙掩膜和喉道掩膜；利用所述孔隙掩膜和喉道掩膜对基片进行刻蚀，形成刻蚀基片；将所述刻蚀基片与盖片进行键合，形成微观岩石网络模型。本发明通过孔喉分离、图像对准和重复光刻在微观玻璃模型上实现了更加贴合油藏实际的微纳米油气流动通道，刻蚀工艺中反应时间的控制精确，通道的深宽比、光滑度和平整度较好，键合过程无需提供压力，能够更好地保护纳米通道，实现了微米孔隙和纳米喉道的真实砂岩微观模型的键合，使二维平面模型上不能发生的海恩斯阶跃以及非润湿相聚并等微观动态变化得以呈现。
The invention discloses a method for making a microscopic rock network model. mask; using the pore mask and the throat mask to etch the substrate to form an etched substrate; to bond the etched substrate and the cover sheet to form a microscopic rock network model. The invention realizes a micro-nano oil and gas flow channel that is more suitable for the actual oil reservoir through pore-throat separation, image alignment and repeated photolithography on the micro-glass model, the reaction time in the etching process is precisely controlled, the aspect ratio of the channel, The smoothness and flatness are good, and the bonding process does not need to provide pressure, which can better protect the nano-channels, and realize the bonding of the real sandstone microscopic models of micro-pores and nano-throat, so that the sea can not occur on the two-dimensional plane model. Microscopic dynamic changes such as Enns step and non-wetting phase coalescence are presented.
Description
Technical Field
The embodiment of the invention relates to the field of oil and gas development, in particular to a method for manufacturing a microscopic rock network model.
Background
With the continuous and deep research of the theory related to the development of oil and gas resources, the hot and difficult problems of oil and gas field development gradually change from the development and the increase of the recovery ratio of conventional oil and gas to the efficient development of unconventional oil and gas.
The micro physical simulation experiment of China starts late, the concept of 'micro seepage' is put forward earlier by seepage of Chinese academy of sciences taking Guoshengping academy as a subject, a series of micro seepage simulation and test technologies are formed in the last 90 th century, a large amount of research is carried out on fluid flow in a micron-scale channel of a conventional oil reservoir, some important seepage mechanisms and rules are disclosed, and theoretical support is provided for conventional oil reservoir development. In recent years, with the expansion of the application range of microscopic physical models, deep-seated scholars in many oil and gas field development fields such as Zhu Wei, Dai Lily and Yue Xiang' an and the like use the microscopic glass models of real sandstone and the regular microscopic glass models to research the chemical flooding action mechanism, and provide effective support for the conventional oil reservoir recovery rate improvement research.
However, the past microscopic glass model has great limitation when being applied to the development of tight oil reservoirs, and is mainly represented in four aspects: (1) the channel dimension of a conventional etching sand filling model is generally larger, generally ranges from 20 micrometers to 200 micrometers, and is difficult to be used for flow research of fluid in micro-nano-scale pore throats due to the fact that the size difference with the main pore throats of a compact oil reservoir is larger (the pore size ranges from 20 micrometers to 80 micrometers, and the throat size ranges from 100nm to 700 nm); (2) the conventional visual microfluidic chips are two-dimensional chips, the depth of the whole model channel is the same, the three-dimensional difference is huge compared with the three-dimensional difference between the pore throats of real sandstone, the micro-dynamics such as Hayns step, oil-water coalescence and the like of fluid flowing between the pore throats are difficult to appear, and the micro-dynamics is greatly different from the flowing state of oil gas in a compact oil reservoir; (3) the microscopic model made of the real sandstone slice as the raw material needs to be added with the adhesive in the making process to change the surface property of the core, and has poor observation effect, so that the purposes of observing the flow, adsorption and diffusion of the fluid in the channel cannot be achieved.
Disclosure of Invention
The invention provides a method for manufacturing a microscopic rock network model, and provides a microscopic physical model which is more practical for the research of fluid flow in a micron-scale channel of an unconventional oil reservoir, particularly a compact oil reservoir.
The embodiment of the invention provides a method for manufacturing a microscopic rock network model, which comprises the following steps:
extracting a pore throat channel, separating pores and a throat in the pore throat channel to obtain a pore pattern and a throat pattern, and respectively manufacturing a pore mask and a throat mask;
etching the substrate by using the pore mask and the throat mask to form an etched substrate;
and bonding the etching substrate and the cover plate to form a microscopic rock network model.
Wherein separating the pores and the throat in the throat passage to obtain a pore pattern and a throat pattern comprises:
carrying out binarization processing on the image of the rock slice, and distinguishing a rock skeleton pattern and a pore throat channel pattern;
determining all central axes in the pore-throat channel pattern;
making a circle by taking each pixel point on the central axis as the center of the circle, wherein the radius of the circle is the distance from the center of the circle to the nearest rock skeleton;
and defining the circle center of a circle with the radius meeting the preset condition as a node, wherein the corresponding pore throat channel pattern at each node is a pore pattern, and the remaining pore throat channel patterns are throat patterns.
Wherein, utilizing the aperture mask and the throat mask to etch the substrate comprises:
etching a pore, namely etching the substrate by using the pore mask to form a semi-etched substrate;
aligning the mask, and aligning the semi-etching substrate with the throat mask according to the corresponding first marks engraved on the aperture mask and the throat mask;
etching the throat, namely etching the semi-etched substrate by using the throat mask to obtain the etched substrate;
and cleaning the model, namely cleaning the etched substrate.
The pore etching method comprises the following steps:
stacking the aperture mask and the substrate together and exposing the substrate through an exposure machine so that the pattern of the aperture mask is transferred to the substrate;
cleaning the photoresist and the exposed part on the substrate;
immersing the substrate into the first etching solution for etching for 30min under the environment of ultrasonic water bath to formThe first etching solution is HF of 1mol/L as an etchant and NH of 0.5mol/L4F is a complexing agent and 0.5mol/L of HNO3Is a mixed liquid of cosolvent.
Wherein the line width of the first mark is a first set multiple of the throat channel width.
Further, corresponding second marks are further engraved on the aperture mask and the throat mask, the second marks are located in a preset area of the first marks, the line width of the second marks is a second set multiple of the line width of the first marks, and the length of the second marks is a third set multiple of the line width of the first marks;
accordingly, the mask alignment comprises:
and aligning the semi-etching substrate with the throat mask according to the corresponding first mark and the second mark engraved on the aperture mask and the throat mask.
Wherein the throat etch comprises:
carrying out secondary exposure on the aligned throat mask and the semi-etching substrate through an exposure machine so as to transfer the pattern of the throat mask to the semi-etching substrate;
cleaning the photoresist and the exposed part on the semi-etching substrate;
immersing the semi-etching substrate into a second etching solution for etching for 30min under the environment of ultrasonic water bath to form the etching substrate, wherein the second etching solution takes 0.015mol/L HF as an etching agent and 0.0075mol/L NH4F is a complexing agent, 0.0075mol/L of HNO3Is a mixed liquid of cosolvent.
Wherein, bonding the etching substrate and the cover plate comprises:
preprocessing the etched substrate;
attaching the etching substrate and the cover plate to form an initial microscopic rock network model;
and bonding the initial microscopic rock network model by a high-temperature sintering method to form the microscopic rock network model.
Bonding the initial microscopic rock network model by a high-temperature sintering method, wherein the bonding of the initial microscopic rock network model by the high-temperature sintering method comprises the following steps:
placing the initial micro rock network model in a high-temperature vacuum furnace, and vacuumizing the high-temperature vacuum furnace;
raising the temperature in the high-temperature vacuum furnace from normal temperature to 50 ℃ at the speed of 2 ℃/min, and keeping the temperature for 30min after the temperature reaches 50 ℃;
heating the high-temperature vacuum furnace to 120 ℃ at the speed of 2 ℃/min, and keeping the temperature for 150min after the temperature reaches 120 ℃;
heating the high-temperature vacuum furnace to 700 ℃ at the speed of 1.5 ℃/min, and keeping the temperature for 120min after the temperature reaches 700 ℃;
naturally cooling to normal temperature.
Further, still include:
and injecting a toluene solution containing 1% Trichloromethylsilane (TCMS) into the initial micro rock network model injection port to a bound water state so as to perform wetting modification on the initial micro rock network model.
Aiming at the research of fluid flow in a micron-scale channel of an unconventional oil reservoir, particularly a compact oil reservoir, the invention realizes the depiction of a micro-nano oil-gas flow channel which is more fit with the actual oil reservoir on a microscopic glass model through pore-throat separation and repeated photoetching, provides a microscopic physical model which is more fit with the actual oil reservoir, can present the micro dynamic changes such as Haynes step and non-wetting phase coalescence which cannot occur on a two-dimensional plane model originally, and is greatly beneficial to promoting the basic theoretical research of compact oil gas.
Drawings
FIG. 1 is a flow chart of a method for making a micro rock network model according to an embodiment of the present invention;
FIG. 2 is a flow chart of another method for modeling a micro rock network according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of image binarization of a microscopic reservoir rock slice according to an embodiment of the present invention;
FIG. 4 is a schematic illustration of a central axis extraction according to an embodiment of the present invention;
FIG. 5 is a schematic view of the pore nodes inside the pore throat channel provided in accordance with one embodiment of the present invention;
FIG. 6 is a schematic diagram of the pore-throat identification result provided by the embodiment of the invention;
FIG. 7 is a schematic diagram of a pore node at the intersection of the throat according to an embodiment of the present invention;
FIG. 8 is a flow chart of another method for modeling a micro rock network according to a second embodiment of the present invention;
FIG. 9 is a schematic view of an aperture mask and a throat mask provided in accordance with a second embodiment of the present invention;
FIG. 10 is a flow chart of another method for modeling a micro rock network according to a third embodiment of the present invention;
fig. 11 is a flowchart of another method for modeling a micro rock network according to a fourth embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention. It should be further noted that, for the convenience of description, only some of the structures related to the present invention are shown in the drawings, not all of the structures.
Example one
Fig. 1 is a flowchart of a method for making a microscopic rock network model according to an embodiment of the present invention, which is applicable to making a compact reservoir microscopic model, and specifically includes the following steps:
and 110, extracting the pore-throat channel, separating pores and throats in the pore-throat channel to obtain a pore pattern and a throat pattern, and respectively manufacturing a pore mask and a throat mask.
The extraction of the pore throat channel can be realized by adopting a real sandstone casting body, a rock slice is formed by slicing the real sandstone casting body, the image of the rock slice is subjected to binarization processing, a rock skeleton area and a pore throat channel area in the rock slice image are distinguished, the extraction of the pore throat channel is realized, a pattern formed by a pore area is obtained, wherein the area without the pore pattern in the pore throat channel area is the throat pattern, then the pore pattern and the throat pattern are respectively and repeatedly engraved on a mask, so that a pore mask and a throat mask can be obtained, and the mask can be made of stainless steel, copper, alloy and the like without limitation.
Preferably, separating the apertures and the throat in the throat passage to obtain the aperture pattern and the throat pattern comprises:
s111, carrying out binarization processing on the image of the rock slice, and distinguishing a rock skeleton pattern and a pore throat channel pattern;
specifically, fig. 2 is a flowchart of another method for making a microscopic rock network model according to the first embodiment of the present invention, and fig. 3 is a diagram illustrating binarization of a microscopic reservoir rock slice image according to the first embodiment of the present invention. Referring to fig. 3, the black part is the rock skeleton obtained after binarization, and the white part is the pore throat channel obtained after binarization.
S112, determining all central axes in the pore-throat channel pattern;
fig. 4 is a schematic diagram of extracting a central axis according to an embodiment of the present invention, and referring to fig. 3 and 4, a pore and a throat of a throat channel are separated by using an image processing technique, a black region in an original shape is a rock skeleton, a white pixel region is the throat channel, and pixels in the throat channel, which are in contact with the rock skeleton, are removed for multiple times until only one pixel point remains in a channel section, so as to obtain the central axis of the throat channel.
S113, making a circle by taking each pixel point on the central axis as the center of the circle, wherein the radius of the circle is the distance from the center of the circle to the nearest rock skeleton;
the pore inside the pore throat channel is provided with a pore, and the pore inside the pore throat channel can judge the size of a space where a pixel is located by rounding the pixel on a central axis inside the pore throat channel, so that the position of the pore inside the pore throat channel is determined. Specifically, fig. 5 is a schematic diagram of a pore node inside a pore throat channel according to an embodiment of the present invention, referring to fig. 5, a circle with a preset radius is made at each pixel point on a central axis with the pixel point as a center, the preset radius may be set to a smaller value according to specific situations, then the radius of the circle is enlarged, whether the circumference is in contact with a rock skeleton pixel is determined, and if so, the current radius is the distance from the center to the nearest rock skeleton.
S114, defining the circle center of a circle with the radius meeting the preset condition as a node, wherein the corresponding pore throat channel pattern at each node is a pore pattern, and the pore throat channel patterns at the rest part are throat channel patterns.
Through S113, a maximum circle which is placed on the pore throat channel and has the center on the central axis can be obtained, all contained spheres are deleted, a circle sequence which is tightly attached to the pore throat channel is obtained, whether a circle meeting a preset condition exists on the central axis is checked, the preset condition can be, for example, whether the maximum circle corresponding to the current pixel point on the central axis exceeds a preset multiple of the maximum circle corresponding to the adjacent pixel point, if the maximum circle corresponding to the pixel point on the central axis exceeds the preset multiple, the pixel point corresponding to the maximum circle can be defined as a node, and the set multiple can be set according to the actual pore and throat size; or, whether the maximum circle corresponding to the current pixel point is the circle with the largest radius on the central axis, if so, the pixel point may be defined as the node. Fig. 6 is a schematic diagram of the pore-throat identification result provided by one embodiment of the present invention, and it can be seen with reference to fig. 6 that the pores are separated from the pore-throat channels. Specifically, the pore exists inside the throat of the throat channel, and the intersection area of the throat and the throat is also generally larger, that is, the pore may also exist in the intersection area of the throat, fig. 7 is a schematic diagram of a pore node at the intersection of the throat provided in the first embodiment of the present invention, and the pore node in the intersection area of the throat may be defined as a pore node with a coordination number greater than 2, where the coordination number of a pixel on the central axis refers to the number of pixels on the central axis adjacent to the pixel, and obviously, the pore node inside the throat shown in fig. 5 may be defined as a pore node with a coordination number of 2. Referring to fig. 7, the determination of the pore node can also be performed by searching for a pixel point with a coordination number greater than 2 on the axis, i.e., a node of the intersection region of the throat, so as to obtain a pore at the intersection region.
Obviously, the nodes are pore nodes, the pore throat channel pattern corresponding to each pore node may be an area formed by a maximum circle with the node as a center, the pore pattern is formed by the pore throat channel pattern corresponding to the pore node, the throat pattern is formed by an area in the pore throat channel from which the pore pattern is removed, and the pore pattern and the throat pattern respectively correspond to the pore and the throat in the pore throat channel of the rock slice, so that the separation of the pore and the throat in the rock slice is realized.
And 120, etching the substrate by using the pore mask and the throat mask to form an etched substrate.
The substrate can be a glass substrate or a glass uniform glue chromium plate, and the same uniform glue chromium plate is respectively subjected to photoetching, including ultraviolet exposure, photoresist cleaning, chromium washing liquid cleaning, substrate etching, substrate cleaning and the like, according to the pore mask and the throat mask obtained in the last step, so that pores and throats of the substrate are carved, and a channel network in the real sandstone casting is recovered.
And 130, bonding the etched substrate and the cover plate to form a micro rock network model.
The etching substrate is provided with a pore throat channel, a substrate and a cover plate, wherein the pore throat channel etched on the etching substrate needs to be sealed through the cover plate, the substrate and the cover plate need to be directly bonded under certain conditions in order to not change the surface properties of the pore throat channel and the substrate, the bonding is to carry out surface cleaning and activation treatment on two homogeneous or heterogeneous semiconductor materials with clean surfaces and flat atomic levels, and the substrate is bonded into a whole through Van der Waals force, molecular force and even atomic force.
Aiming at the research of fluid flow in a micron-scale channel of an unconventional oil reservoir, particularly a compact oil reservoir, the technical scheme of the embodiment of the invention realizes the depiction of the micro-nano oil-gas flow channel which is more fit with the actual oil reservoir on a microscopic glass model through pore-throat separation and repeated photoetching, provides a microscopic physical model which is more fit with the actual oil reservoir, presents the micro dynamic changes such as Haynes step and non-wetting phase coalescence which cannot occur on a two-dimensional plane model originally, and is greatly beneficial to promoting the research of the compact oil-gas basic theory.
Example two
Fig. 8 is a flowchart of another method for manufacturing a microscopic rock network model according to a second embodiment of the present invention, and referring to fig. 8, in the manufacturing method provided in this embodiment, S120 etching a substrate by using a pore mask and a throat mask specifically includes the following steps:
s121, etching a pore, and etching the substrate by using a pore mask to form a semi-etched substrate;
both the pore etching in the step and the throat etching in the step S123 may be performed by using a wet etching process, and a half-etched substrate with pores may be obtained by the pore etching.
Preferably, the method of pore etching comprises: stacking the aperture mask and the substrate together and exposing the substrate through an exposure machine so that the pattern of the aperture mask is transferred to the substrate; cleaning the photoresist and the exposed part on the substrate; immersing a substrate into a first etching solution for etching for 30min under the environment of ultrasonic water bath to form a semi-etched substrate, wherein the first etching solution takes 1mol/L HF as an etching agent and 0.5mol/L NH4F is a complexing agent and 0.5mol/L of HNO3Is a mixed liquid of cosolvent.
The pore etching method comprises the following steps of firstly, stacking a pore mask and a uniform glue chromium plate together, exposing the stacked pore mask and the uniform glue chromium plate on an exposure machine, and transferring a pore pattern to the uniform glue chromium plate; then, washing the photoresist by using 5 per mill of NaOH solution to wash away the photoresist on the photoresist homogenizing chromium plate; washing with a chromium washing liquid to wash off the exposed part on the uniform glue chromium plate and expose the glass corresponding to the pores on the uniform glue chromium plate; and under the ultrasonic water bath environment, immersing the even glue chromium plate with the exposed pores into glass etching liquid for etching, thereby obtaining the semi-etched substrate with the etched pores. Through multiple experiments, researchers find that the first etching solution for etching the pores is preferably 1mol/L HF and 0.5mol/L NH4F is a complexing agent and 0.5mol/L of HNO3The first etching liquid with higher concentration is used as the mixed liquid of the cosolvent, the pores with the depth of dozens of microns can be etched and formed in a shorter time, the etching time is preferably 30min, the pores can be recovered to the maximum extent, and HNO is added into the etching liquid3And NH4Cl, inhibits the uneven corrosion of HF to glass by the principle of ion exchange, and ensures the smoothness of poresThe degree, the flatness and the depth-to-width ratio have better etching effect.
S122, aligning the mask, and aligning the semi-etched substrate with the throat mask according to the corresponding first marks engraved on the aperture mask and the throat mask;
fig. 9 is a schematic diagram of an aperture mask and a throat mask according to a second embodiment of the present invention, in order to match a half-etched substrate with an etched aperture with a throat to be etched on the mask, the two must be aligned before the throat is etched, corresponding marks may be marked on the aperture mask and the throat mask, for example, a "+" vernier is shown in fig. 9, and after the aperture is etched, the throat mask may be aligned with a first mark 91 etched on the half-etched substrate through a first mark 91 thereon.
Optionally, the line width of the first mark is a first set multiple of the throat channel width.
In order to achieve precise matching between the aperture and the throat and avoid alignment failure between the aperture and the throat due to the overlarge mark, the line width of the first mark may be set to a size equivalent to the width of the throat channel, wherein the width of the throat channel may be the minimum value of the width of the throat channel or an average value of the widths of all the throat channels, which is not limited herein, for example, the line width of the "+" cursor may be 5 times the minimum width of the throat channel.
Optionally, corresponding second marks are further engraved on the aperture mask and the throat mask, the second marks are located in a preset area of the first marks, the line width of the second marks is a second set multiple of the line width of the first marks, and the length of the second marks is a third set multiple of the line width of the first marks; accordingly, the mask alignment includes: and aligning the semi-etched substrate with the throat mask according to the corresponding first mark and the second mark engraved on the aperture mask and the throat mask.
Since the line width of the first mark 91 is set to be equivalent to the throat passage width, when aligning the first mark 91, it may be difficult to find the first mark 91 because the first mark 91 is too small, and in order to find the first mark 91 more clearly and conveniently, the second mark 92 may be provided in a predetermined area of the first mark 91, and the second mark may be set at a set distance of the set orientation of the first mark 91, for example, at a position as shown in fig. 9. Meanwhile, in order to more conveniently search for the first mark 91 through the second mark 92, the size of the second mark 92 may be a set multiple of that of the first mark 91, and referring to fig. 9, the second mark 92 may be a line segment and have a width 6 times the line width of the "+" cursor and a length 16 times the line width of the "+" cursor.
S123, etching the throat, and etching the half-etched substrate by using a throat mask to obtain an etched substrate;
the throat etching in the step is the same as the wet etching process used for the pore etching in the step S121, and the half-etched substrate with the pores can be etched into an etched substrate with the pores and the throat simultaneously through the throat etching, so that the pore throat channel in the sandstone slice is recovered.
Optionally, carrying out secondary exposure on the aligned throat mask and the semi-etching substrate through an exposure machine so as to transfer the pattern of the throat mask onto the semi-etching substrate; cleaning the photoresist and the exposed part on the semi-etched substrate; immersing the semi-etching substrate into a second etching solution for etching for 30min under the environment of ultrasonic water bath to form the etching substrate, wherein the second etching solution takes 0.015mol/L HF as an etching agent and 0.0075mol/L NH4F is a complexing agent, 0.0075mol/L of HNO3Is a mixed liquid of cosolvent.
Similarly, after the throat mask is aligned with the even glue chromium plate etched with the pores, carrying out secondary exposure, and transferring the throat pattern to the even glue chromium plate; then, washing the photoresist by using 5 per mill of NaOH solution to wash away the photoresist on the throat on the photoresist homogenizing chromium plate; washing with a chromium washing liquid to wash off the secondary exposure part on the uniform glue chromium plate and expose the glass corresponding to the throat on the uniform glue chromium plate; and under the ultrasonic water bath environment, immersing the even glue chromium plate with the exposed pores into glass etching liquid for etching, thereby obtaining the semi-etched substrate with the etched pores. Through multiple experiments, researchers find that the second etching solution for etching the throat is 0.015mol/L HF serving as an etching agent and 0.0075mol/L NH4F is a complexing agent, 0.0075moL/L HNO3Is a mixed liquid of a cosolvent, and can realize the restoration of pores to the maximum extent when the etching time is 30min, thereby having better etching effect. The low-concentration second etching liquid is used for throat etching, the throat etching time of hundreds of nanometers can be kept for dozens of minutes, and sufficient reaction time is provided for controlling the etching depth. Simultaneously adding HNO into the etching solution3And NH4And Cl, the uneven corrosion of HF to the glass is inhibited through the principle of ion exchange, and the smoothness, the flatness and the depth-to-width ratio of the channel are ensured.
And S124, cleaning the model, and cleaning the etched substrate.
In order to ensure the cleanness of the model and facilitate the subsequent bonding step, the model can be washed by deionized water and then put into a NaOH solution with the concentration of 5 percent to wash away the photoresist, and then the model is washed by deionized water and then put into a chromium washing liquid to wash away the chromium layer. And rinsing the chip by using deionized water after the chromium layer is removed.
According to the technical scheme of the embodiment of the invention, the holes and the throats existing in the pore-throat channel of the actual sandstone are respectively etched, so that the holes and the throats conforming to the size of the real compact reservoir are formed, the holes and the throats are effectively distinguished, the half-etched substrate with the etched holes and the throats to be etched on the mask can be matched and aligned through the marks, the holes and the throats in the compact reservoir are accurately recovered, and the microscopic rock network model more conforming to the actual compact reservoir is realized.
EXAMPLE III
FIG. 10 is a flow chart of another method for modeling a micro rock network according to a third embodiment of the present invention. Referring to fig. 10, in the manufacturing method provided in this embodiment, S130, bonding the etched substrate and the cover plate to form a micro rock network model specifically includes the following steps:
s131, preprocessing an etched substrate;
wherein the pretreatment of the etched substrate comprises boiling and rinsing, first with H2SO4And H2O2Preparing solution according to the ratio of 4:1, boiling for etching the substrate and the cover plate for 10-15min, respectively rinsing with petroleum ether and ethanol for 10min,the cleaning agent is used for cleaning the etched substrate and the cover plate, wherein petroleum ether can wash off organic matters adhered to the etched substrate and the cover plate, and ethanol is used for washing off inorganic matters adhered to the etched substrate and the cover plate. Through the pretreatment of the etching substrate and the cover plate, impurities on the surfaces of the etching substrate and the cover plate can be removed, the surface hydrophilicity of the etching substrate and the cover plate is improved, and the etching substrate and the cover plate can be attached more closely.
S132, attaching the etched substrate and the cover plate to form an initial microscopic rock network model;
and washing the pretreated etching substrate and the pretreated cover plate under deionized water for 30min to ensure that no pretreatment liquid is left on the etching substrate and the cover plate, and then attaching the etching substrate and the cover plate.
And S133, bonding the initial microscopic rock network model by a high-temperature sintering method to form the microscopic rock network model.
The high-temperature sintering method has the advantages of both reactive sintering and hot-pressing sintering, can realize bonding of the etched substrate and the cover plate, and can prepare the high-precision micro rock network model with high density and low linear shrinkage.
Preferably, the bonding of the initial micro rock network model is performed by a high temperature sintering method, comprising: placing the initial micro rock network model in a high-temperature vacuum furnace, and vacuumizing the high-temperature vacuum furnace; raising the temperature in the high-temperature vacuum furnace from normal temperature to 50 ℃ at the speed of 2 ℃/min, and keeping the temperature for 30min after the temperature reaches 50 ℃; heating the high-temperature vacuum furnace to 120 ℃ at the speed of 2 ℃/min, and keeping the temperature for 150min after the temperature reaches 120 ℃; heating the high-temperature vacuum furnace to 700 ℃ at the speed of 1.5 ℃/min, and keeping the temperature for 120min after the temperature reaches 700 ℃; naturally cooling to normal temperature.
Generally, the bonding method of the microfluidic chip mainly adopts the technologies of adhesive, auxiliary pressure, strict ultra-clean environment and the like to realize bonding, the operation is complicated, and special cleaning equipment and the ultra-clean environment are needed. In the scheme of the embodiment, the chip is bonded through the high-temperature vacuum furnace, so that the slow temperature rise and heat preservation process can be realized, the temperature and the vacuum degree can be accurately controlled, the pressure is not required to be provided, the nano channel can be better protected, the natural bonding of the substrate and the cover plate is ensured, and the restoration of the real sandstone microscopic model of the micro-pore and the nano channel is realized.
According to the technical scheme of the embodiment of the invention, the holes and the throats existing in the hole-throat channel of the actual sandstone are respectively etched, so that the holes and the throats conforming to the size of the real compact reservoir are formed, and meanwhile, the bonding of the etched substrate and the cover plate of the etched holes and throats is realized through a high-temperature sintering method, so that the etched substrate and the cover plate are effectively and tightly combined into a whole, and the microscopic rock network model more conforming to the actual compact reservoir is realized.
Example four
Fig. 11 is a flowchart of another method for modeling a micro rock network according to a fourth embodiment of the present invention. Referring to fig. 11, in the manufacturing method provided in this embodiment, after S130, the method further includes S140, injecting a toluene solution containing 1% Trichloromethylsilane (TCMS) into the injection port of the initial micro rock network model until the toluene solution is in a bound water state, so as to wet-modify the initial micro rock network model.
Wherein, the concrete step still includes: rinsing the miniature model with sodium hydroxide for 60min, and cleaning the miniature model with distilled water; saturating the microscopic rock network model with saline water; injecting a toluene solution containing 1% Trichloromethylsilane (TCMS) from a model injection port to a bound water state; washing the miniature model with toluene and ethanol, and then washing the miniature model with distilled water; the microscopic rock network model was dried using an oven at 100 ℃ for 60 min. And (3) flushing the pore throat channel in the microscopic rock network model by using a toluene solution of trichloromethylsilane, and partially modifying the pore throat channel of the glass with strong water wetting to modify the microscopic rock network model into a bound water state, so that a mixed wetting model with the water wetting channel and the oil wetting channel coexisting is formed, and the micro rock network model which is more attached to the oil and gas migration channel of the compact reservoir and is mixed wetting is manufactured.
The technical scheme of the embodiment of the invention completes the restoration of the pore-throat channel of the real compact oil reservoir, simultaneously overcomes the technical problem that the existing wettability control technology is only limited to the whole wetting modification of the model, such as changing the whole wetting modification into pure water wetting or pure oil wetting, realizes the mixed wetting formed by the coexistence of the oil-wet rock and the water-wet rock in the compact oil reservoir, namely the channel of the coexistence of the oil-wet channel and the water-wet channel, ensures that the micro rock network model realizes the mixed wetting characteristic of the real compact oil reservoir, ensures that the micro rock network model is more consistent with the real situation from the structural characteristics and the chemical characteristics, and is greatly beneficial to the research of the real compact oil reservoir.
It is to be noted that the foregoing is only illustrative of the preferred embodiments of the present invention and the technical principles employed. It will be understood by those skilled in the art that the present invention is not limited to the particular embodiments described herein, but is capable of various obvious changes, rearrangements and substitutions as will now become apparent to those skilled in the art without departing from the scope of the invention. Therefore, although the present invention has been described in greater detail by the above embodiments, the present invention is not limited to the above embodiments, and may include other equivalent embodiments without departing from the spirit of the present invention, and the scope of the present invention is determined by the scope of the appended claims.
Claims (9)
1. A method for making a microscopic rock network model is characterized by comprising the following steps:
extracting a pore throat channel, separating pores and a throat in the pore throat channel to obtain a pore pattern and a throat pattern, and respectively manufacturing a pore mask and a throat mask;
etching the substrate by using the pore mask and the throat mask to form an etched substrate;
bonding the etching substrate and the cover plate to form a microscopic rock network model;
separating the pores and throat in the throat passage to obtain a pore pattern and a throat pattern comprising:
carrying out binarization processing on the image of the rock slice, and distinguishing a rock skeleton pattern and a pore throat channel pattern;
determining all central axes in the pore-throat channel pattern;
making a circle by taking each pixel point on the central axis as the center of the circle, wherein the radius of the circle is the distance from the center of the circle to the nearest rock skeleton;
and defining the circle center of a circle with the radius meeting the preset condition as a node, wherein the corresponding pore throat channel pattern at each node is a pore pattern, and the remaining pore throat channel patterns are throat patterns.
2. The method of claim 1, wherein etching the substrate using the aperture mask and the throat mask comprises:
etching a pore, namely etching the substrate by using the pore mask to form a semi-etched substrate;
aligning the mask, and aligning the semi-etching substrate with the throat mask according to the corresponding first marks engraved on the aperture mask and the throat mask;
etching the throat, namely etching the semi-etched substrate by using the throat mask to obtain the etched substrate;
and cleaning the model, namely cleaning the etched substrate.
3. The method of claim 2, wherein the pore etching method comprises:
stacking the aperture mask and the substrate together and exposing the substrate through an exposure machine so that the pattern of the aperture mask is transferred to the substrate;
cleaning the photoresist and the exposed part on the substrate;
immersing a substrate into a first etching solution for etching for 30min under the environment of ultrasonic water bath to form a semi-etched substrate, wherein the first etching solution takes 1mol/L HF as an etching agent and 0.5mol/L NH4F is a complexing agent and 0.5mol/L of HNO3Is a mixed liquid of cosolvent.
4. The method of claim 2, wherein the first mark has a line width that is a first set multiple of the throat channel width.
5. The method according to claim 4, wherein the aperture mask and the throat mask are further engraved with corresponding second marks, the second marks are located in a predetermined region of the first marks, a line width of the second marks is a second predetermined multiple of a line width of the first marks, and a length of the second marks is a third predetermined multiple of the line width of the first marks;
accordingly, the mask alignment comprises:
and aligning the semi-etching substrate with the throat mask according to the corresponding first mark and the second mark engraved on the aperture mask and the throat mask.
6. The method of manufacturing of claim 2, wherein the throat etch comprises:
carrying out secondary exposure on the aligned throat mask and the semi-etching substrate through an exposure machine so as to transfer the pattern of the throat mask to the semi-etching substrate;
cleaning the photoresist and the exposed part on the semi-etching substrate;
immersing the semi-etching substrate into a second etching solution for etching for 30min under the environment of ultrasonic water bath to form the etching substrate, wherein the second etching solution takes 0.015mol/L HF as an etching agent and 0.0075mol/L NH4F is a complexing agent, 0.0075mol/L of HNO3Is a mixed liquid of cosolvent.
7. The method of claim 1, wherein bonding the etched substrate to the cover sheet comprises:
preprocessing the etched substrate;
attaching the etching substrate and the cover plate to form an initial microscopic rock network model;
and bonding the initial microscopic rock network model by a high-temperature sintering method to form the microscopic rock network model.
8. The method of claim 7, wherein bonding the initial micro rock network model by a high temperature sintering process comprises:
placing the initial micro rock network model in a high-temperature vacuum furnace, and vacuumizing the high-temperature vacuum furnace;
raising the temperature in the high-temperature vacuum furnace from normal temperature to 50 ℃ at the speed of 2 ℃/min, and keeping the temperature for 30min after the temperature reaches 50 ℃;
heating the high-temperature vacuum furnace to 120 ℃ at the speed of 2 ℃/min, and keeping the temperature for 150min after the temperature reaches 120 ℃;
heating the high-temperature vacuum furnace to 700 ℃ at the speed of 1.5 ℃/min, and keeping the temperature for 120min after the temperature reaches 700 ℃;
naturally cooling to normal temperature.
9. The method of manufacturing according to claim 7, further comprising:
and injecting a toluene solution containing 1% Trichloromethylsilane (TCMS) into the initial micro rock network model injection port to a bound water state so as to perform wetting modification on the initial micro rock network model.
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| CN114594230B (en) * | 2022-02-22 | 2023-10-13 | 山东科技大学 | Preparation device and preparation method of mixed wettability sandstone microscopic model |
| CN114575799A (en) * | 2022-03-08 | 2022-06-03 | 西南石油大学 | An experimental device based on the displacement process of nano-micro-nano pore structure |
| CN116920971A (en) * | 2023-07-20 | 2023-10-24 | 常州大学 | Microfluidic chip for researching oil-water seepage mechanism of carbonate reservoir and manufacturing method thereof |
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