CN117920364A - Three-dimensional microfluidic chip, preparation method thereof and three-dimensional microfluidic system - Google Patents
Three-dimensional microfluidic chip, preparation method thereof and three-dimensional microfluidic system Download PDFInfo
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Abstract
The embodiment of the invention provides a three-dimensional microfluidic chip, a preparation method thereof and a three-dimensional microfluidic system, and belongs to the technical field of petroleum exploitation. The three-dimensional microfluidic chip includes: the visual shell and the seepage fluid are sintered in the visual shell, the seepage fluid is formed by sintering a plurality of visual microbeads, and the seepage morphology of the fluid to be observed is observed through the seepage fluid. The three-dimensional microfluidic chip has a simple structure, is convenient to manufacture, can accurately simulate the form of a porous medium, and shows a more accurate seepage process.
Description
Technical Field
The invention relates to the technical field of petroleum exploitation, in particular to a three-dimensional micro-fluidic chip, a three-dimensional micro-fluidic system and a preparation method of the three-dimensional micro-fluidic chip.
Background
Tertiary oil recovery is an important means for increasing and stabilizing the yield of the domestic oil field at present, and mainly comprises chemical oil displacement, gas displacement, thermal oil displacement and other modes. In chemical flooding, the flowing process of fluid including displacement fluid and crude oil in an underground reservoir is a typical seepage process, and visual research is carried out on the process, so that the method has great significance in revealing the mechanism of flooding and improving the displacement formula. The development of the micro-fluidic technology provides a new idea for the visual research of the seepage process.
The existing microfluidic technology adopts a soft etching technology, and a rapid prototyping method of model replication is applied to manufacture the microfluidic chip. However, in the oil displacement process research in tertiary oil recovery, a transparent porous medium is needed to realize visualization in the displacement process, and the porous medium is needed to be simulated by a three-dimensional microfluidic chip. However, the traditional soft etching technology is used for manufacturing the three-dimensional micro-fluidic chip, the processing technology is complex, the requirements on instruments and equipment are high, and the three-dimensional micro-fluidic chip is not easy to manufacture.
The invention provides a three-dimensional microfluidic chip, which has a simple preparation method, can accurately simulate the form of a porous medium, and shows a more accurate seepage process.
Disclosure of Invention
The embodiment of the invention aims to provide a three-dimensional microfluidic chip, a preparation method of the three-dimensional microfluidic chip and a three-dimensional microfluidic system, wherein the three-dimensional microfluidic chip is simple in structure, convenient to manufacture, capable of accurately simulating the form of a porous medium and showing a more accurate seepage process.
In order to achieve the above object, in a first aspect, an embodiment of the present invention provides a three-dimensional microfluidic chip, including a visualization shell and a seepage body, where the seepage body is sintered in the visualization shell, and the seepage body is formed by sintering a plurality of visualization microbeads, and the seepage morphology of a fluid to be observed is observed through the seepage body.
Preferably, the three-dimensional microfluidic chip further comprises a fluid inlet and a fluid outlet, wherein the fluid inlet and the fluid outlet are respectively arranged on a first side wall and a second side wall of the visual shell, and the first side wall is opposite to the second side wall.
Preferably, the visual shell is made of quartz glass, and the visual beads are made of spherical borosilicate glass.
Preferably, the permeability of the three-dimensional microfluidic chip is determined by the visualized bead size, sintering temperature and sintering time.
In a second aspect, an embodiment of the present invention provides a three-dimensional microfluidic system, including a fluid input assembly, an observation platform, a fluid form sampling assembly, and a three-dimensional microfluidic chip as described above, where the three-dimensional microfluidic chip is disposed on the observation platform, an output end of the fluid input assembly is connected to the three-dimensional microfluidic chip and is used for injecting fluid into the three-dimensional microfluidic chip, and the fluid form sampling assembly is erected above the three-dimensional microfluidic chip and is used for collecting seepage forms of the fluid in the three-dimensional microfluidic chip.
Preferably, the fluid input assembly comprises a micro sample injection pump and a syringe, wherein the syringe is arranged above the micro sample injection pump and connected with the micro sample injection pump, and the micro sample injection pump controls the volume of the injected fluid.
Preferably, the observation table is a constant temperature heating table, and a temperature sensor is further arranged on the constant temperature heating table and used for monitoring the temperature on the constant temperature heating table.
Preferably, the fluid body sampling assembly comprises an image acquisition device, a laser confocal microscope and a computer, wherein the laser confocal microscope is arranged above the three-dimensional microfluidic chip, the image acquisition device is used for acquiring an imaging result of the laser confocal microscope, and the computer is used for processing and displaying the acquisition result of the image acquisition device.
Preferably, the three-dimensional microfluidic system further comprises pressure sensors, and the pressure sensors are respectively arranged on the fluid inlet side and the fluid outlet side of the three-dimensional microfluidic chip.
Preferably, the three-dimensional microfluidic system further comprises a fluid collection device, wherein the fluid collection device is a standard nuclear magnetic tube, and scale marks are arranged on the standard nuclear magnetic tube.
In a third aspect, an embodiment of the present invention provides a method for manufacturing a three-dimensional microfluidic chip, which is used for manufacturing the three-dimensional microfluidic chip described above, including the following steps:
and (3) packaging: filling the visual shell with visual microbeads, and sealing a fluid outlet and a fluid inlet on the visual shell;
and (3) sintering: placing the packaged three-dimensional microfluidic chip into a muffle furnace for sintering, wherein the sintering temperature is not lower than 821 ℃, and the sintering time is less than 10 minutes;
The installation step comprises the following steps: and fixing the three-dimensional microfluidic chip after sintering on an observation table, and installing pipelines at the positions of the fluid inlet and the fluid outlet to realize fluid circulation.
The visual microbeads are sintered to form the seepage fluid, so that the porous medium form in the tertiary oil recovery process can be accurately simulated, and the simulated seepage form result is more accurate.
The three-dimensional microfluidic chip is prepared by adopting a sintering method, and the method is simple in process and easy to prepare.
Additional features and advantages of embodiments of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings are included to provide a further understanding of embodiments of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain, without limitation, the embodiments of the invention. In the drawings:
Fig. 1 is a schematic structural diagram of a three-dimensional microfluidic chip provided in embodiment 1 of the present invention;
fig. 2 is a schematic structural diagram of a three-dimensional microfluidic system provided in embodiment 1 of the present invention;
FIG. 3 is a three-dimensional imaging chart provided in embodiment 1 of the present invention;
FIG. 4 is a three-dimensional imaging chart according to embodiment 2 of the present invention;
FIG. 5 is a three-dimensional imaging chart according to embodiment 3 of the present invention;
FIG. 6 is a three-dimensional imaging chart provided in embodiment 4 of the present invention;
FIG. 7 is a three-dimensional imaging chart according to embodiment 5 of the present invention;
FIG. 8 is a three-dimensional imaging chart provided in example 6 of the present invention;
Fig. 9 is a three-dimensional imaging chart provided in embodiment 7 of the present invention.
Description of the reference numerals
The three-dimensional micro-fluidic chip comprises a 1-three-dimensional micro-fluidic chip, a 11-visual shell, 12-seepage fluid, a 13-fluid inlet, a 14-fluid outlet, a 2-micro sample injection pump, a 3-syringe, a 4-constant temperature heating table, a 5-image acquisition device, a 6-laser confocal microscope, a 7-computer, an 8-pressure sensor and a 9-standard nuclear magnetic tube.
Detailed Description
The following describes the detailed implementation of the embodiments of the present invention with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
In the embodiments of the present invention, unless otherwise indicated, terms such as "upper, lower, left, and right" and "upper, lower, left, and right" are used generally referring to directions or positional relationships based on those shown in the drawings, or those conventionally used in the use of the inventive products. The terms "first," "second," "third," and the like are used merely to distinguish between descriptions and are not to be construed as indicating or implying relative importance.
The terms "parallel", "perpendicular", and the like do not denote that the components are required to be absolutely parallel or perpendicular, but may be slightly inclined. For example, "parallel" merely means that the directions are more parallel than "perpendicular" and does not mean that the structures must be perfectly parallel, but may be slightly tilted.
The terms "horizontal," "vertical," "overhang," and the like do not denote that the component is required to be absolutely horizontal, vertical, or overhang, but may be slightly inclined. As "horizontal" merely means that its direction is more horizontal than "vertical", and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
Furthermore, the terms "substantially," "essentially," and the like, are intended to be limited to the precise form disclosed herein and are not necessarily intended to be limiting. For example: the term "substantially equal" does not merely mean absolute equal, but is difficult to achieve absolute equal during actual production and operation, and generally has a certain deviation. Thus, in addition to absolute equality, "approximately equal to" includes the above-described case where there is a certain deviation. In other cases, the terms "substantially", "essentially" and the like are used in a similar manner to those described above unless otherwise indicated.
In the description of the present invention, it should also be noted that, unless explicitly specified and limited otherwise, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
Example 1
Referring to fig. 1, in a first aspect, the present embodiment provides a three-dimensional microfluidic chip 1, which includes a visual housing 11 and a seepage body 12, wherein the seepage body 12 is sintered in the visual housing 11, the seepage body 12 is formed by sintering a plurality of visual microbeads, and the seepage morphology of the fluid to be observed is observed through the seepage body 12.
Specifically, the multiple visualized positions are sintered to form a three-dimensional seepage body 12, and the three-dimensional seepage body 12 is more like a porous medium shape in the tertiary oil recovery process compared with a two-dimensional seepage hole of a microfluidic chip in the prior art. The seepage body 12 formed by sintering the plurality of visual microbeads can more accurately simulate the form of the porous medium, and can accurately acquire the fluid seepage form in the chemical flooding process.
The invention adopts the visual microbeads to form the porous medium, the porous medium has single structure and the permeability is accurate and controllable.
The seepage body 12 is sintered by adopting visual microbeads, so that visual observation is facilitated.
The three-dimensional micro-fluidic chip 1 is prepared by adopting a sintering method, and the preparation process is simple and easy to prepare.
In this embodiment, the three-dimensional microfluidic chip 1 further includes a fluid inlet 13 and a fluid outlet 14, where the fluid inlet 13 and the fluid outlet 14 are respectively disposed on a first sidewall and a second sidewall of the visual housing 11, and the first sidewall is opposite to the second sidewall. Fluid enters the interior of the visual housing 11 from the fluid inlet, flows through the osmotic fluid 12, and exits through the fluid outlet 14. The morphology of the seepage flowing within the seepage 12 is collected to simulate the morphology of the seepage within the porous medium.
The seepage body 12 is arranged in the visual shell 11 by adopting a sintering process, so that the manufacturing process is simple and easy to manufacture. And moreover, by adopting a sintering process, the seepage body 12 and the visual shell 11 are firmly connected, the structure is more compact, the three-dimensional microfluidic chip 1 is more temperature and pressure resistant, and the environment condition in the oil extraction process can be accurately simulated.
Further, in this embodiment, the fluid inlet 13 and the fluid outlet 14 are both protruded from the visual housing 11, so as to facilitate adhesion of the pipes through which the working fluid flows.
In this embodiment, the material of the visual housing 11 is quartz glass, and the material of the visual beads is spherical borosilicate glass. The quartz glass can resist the high temperature of 1200 ℃ and 1400 ℃ in a short time, and the melting of the outer shell in the sintering process can be avoided. Borosilicate glass has a melting temperature of 821 ℃ lower than the high temperature resistance of quartz glass, and is easy to sinter and mold.
Further, in the present embodiment, the visual housing 11 is a rectangular parallelepiped, and the visual beads are spheres.
In this embodiment, the permeability of the three-dimensional microfluidic chip 1 is determined by the visualized bead size, sintering temperature and sintering time.
Specifically, the sintering temperature should be greater than the melting temperature (821 ℃) of borosilicate glass, and the sintering time should be less than 10 minutes to avoid hardening of the visual glass beads.
Preparing a three-dimensional microfluidic chip 1 with low permeability, adopting small-sized visual microbeads, increasing sintering temperature and prolonging sintering time; when the high-permeability three-dimensional microfluidic chip 1 is prepared, large-size visual microbeads are adopted, so that the sintering temperature is reduced and the sintering time is shortened. Increasing the sintering temperature and increasing the sintering time can facilitate the melting of borosilicate glass. Notably, in the preparation of the three-dimensional microfluidic chip 1 with high permeability, the sintering temperature should be ensured to be not lower than 821 ℃ and the sintering time should be less than 10 minutes.
In this embodiment, the permeability of the three-dimensional microfluidic chip 1 is also related to the visual shell, and the corresponding formula is:
Wherein k is permeability and the unit is D; q is the volume flow in [ mu ] L min -1, L is the length of the visual housing in cm, A is the cross-sectional area of the visual housing in cm 2, and ΔP is the pressure differential of the visual housing in KPa.
The example shows that the size of the visualized beads is 19.+ -.2. Mu.m, 38.+ -.3. Mu.m, 45.+ -.3. Mu.m, or 75.+ -.5. Mu.m. Specifically, the size of the visualized micro-beads used in the preparation of the k >5D three-dimensional microfluidic chip 1 is 75+/-5 μm, the size of the visualized micro-beads used in the preparation of the 5D > k >1D three-dimensional microfluidic chip 1 is 38+/-3 μm or 45+/-3 μm, and the size of the visualized micro-beads used in the preparation of the k <1D three-dimensional microfluidic chip 1 is 19+/-2 μm.
The present example also provides a functional relationship of permeability with sintering temperature, sintering time, and visualized bead size, as follows:
wherein T is the sintering temperature, T is the sintering time, s is the size of the visual microbead, and k is the permeability.
In a second aspect, the present embodiment provides a three-dimensional microfluidic system, including a fluid input assembly, an observation platform, a fluid form sampling assembly, and a three-dimensional microfluidic chip 1 as described above, where the three-dimensional microfluidic chip 1 is disposed on the observation platform, an output end of the fluid input assembly is connected to the three-dimensional microfluidic chip 1, and is used for injecting fluid into the three-dimensional microfluidic chip 1, and the fluid form sampling assembly is set up above the three-dimensional microfluidic chip 1, and collects a seepage form of the fluid in the three-dimensional microfluidic chip 1.
Specifically, the fluid input assembly inputs fluid to the three-dimensional microfluidic chip 1, and the fluid form sampling assembly is used for collecting seepage forms of the fluid in the seepage process of the seepage 12.
In this embodiment, the fluid input assembly includes a micro-sampling pump 2 and an injector 3, wherein the injector 3 is disposed above the micro-sampling pump 2 and connected to the micro-sampling pump 2, and the micro-sampling pump 2 controls the volume of the injected fluid.
In this embodiment, the observation stand is a constant temperature heating stand 4, and a temperature sensor is further disposed on the constant temperature heating stand 4, and the temperature sensor is used for monitoring the temperature on the constant temperature heating stand 4. To ensure real-time recording of temperature parameters during the percolation process.
In this embodiment, the fluid body sampling assembly includes an image acquisition device 5, a confocal laser microscope 6, and a computer 7, where the confocal laser microscope 6 is disposed above the three-dimensional microfluidic chip 1, the image acquisition device 5 is used to acquire an imaging result of the confocal laser microscope 6, and the computer 7 is used to process and display an acquisition result of the image acquisition device 5.
Specifically, the objective lens of the laser confocal microscope 6 is aligned to the three-dimensional microfluidic chip 1, the image acquisition device 5 is aligned to the light-emitting light path of the laser confocal microscope 6, the image acquisition device 5 is used for acquiring a seepage picture displayed by the laser confocal microscope 6, and sending the seepage form to the computer 7, and the computer 7 processes and displays the seepage picture.
Specifically, the image pickup device 5 is a high-speed camera in this embodiment.
In this embodiment, the three-dimensional microfluidic system further includes a pressure sensor 8, and the pressure sensor 8 is disposed on the fluid inlet 13 side and the fluid outlet 14 side of the three-dimensional microfluidic chip 1, respectively. The pressure sensor 8 is used to measure the pressure of the input fluid and the pressure of the output fluid, facilitating the analysis of the subsequent permeability.
In this embodiment, the three-dimensional microfluidic system further includes a fluid collecting device, where the fluid collecting device is a standard nuclear magnetic tube 9, and scale marks are disposed on the standard nuclear magnetic tube 9.
The difference between the volume of the outgoing fluid and the volume of the incoming fluid can be compared by collecting the outgoing fluid.
In a third aspect, the present embodiment provides a method for manufacturing a three-dimensional microfluidic chip 1, for manufacturing the three-dimensional microfluidic chip 1 as described above, including the steps of:
Packaging the three-dimensional microfluidic chip 1: filling the visual microbeads into the visual square tube, and sealing the fluid outlet 14 and the fluid inlet 13; specifically, the wall of the visual shell 11 should be tapped after the visual beads are assembled, so that the visual beads are filled in the visual shell 11 to the maximum extent; the visual housing 11 should be filled with the visual beads as much as possible and the fluid inlet 13 and the fluid outlet 14 should be sealed with tape to avoid collapse of the visual beads during transfer.
Sintering the three-dimensional microfluidic chip 1: and placing the packaged three-dimensional microfluidic chip 1 into a muffle furnace for sintering, wherein the sintering temperature is not lower than 821 ℃, and the sintering time is less than 10 minutes. .
Three-dimensional microfluidic chip 1 mounting: and fixing the three-dimensional microfluidic chip 1 after sintering on the observation table, and installing pipelines at the positions of the fluid inlet 13 and the fluid outlet 14 to realize fluid circulation. Specifically, the three-dimensional micro-flow control chip after sintering is adhered and fixed on a thin glass sheet on the constant temperature heating table 4, and the adhesive material is modified acrylate adhesive. The pipes installed at the fluid inlet 13 and the fluid outlet 14 are made of polyethylene, and sealing of the fluid inlet 13 and the fluid outlet 14 is completed.
After the preparation of the three-dimensional microfluidic chip 1 is completed, a three-dimensional microfluidic system is formed, and an oil phase is pumped into the three-dimensional microfluidic chip 1 at a high injection rate to ensure that the channel is saturated with the oil. After the oil saturation process is finished, water phase is injected into the channel at a certain speed for displacement, real-time pressure is recorded, and meanwhile, the temperature and the injection flow are monitored to ensure the consistency of different experimental groups. The displacement process is performed using a gas tight syringe 3. To distinguish between the oil and water phases, the aqueous phase was labeled with fluorescein and the oil phase was labeled with nile red. And (3) microscopic imaging is carried out on the displacement process by using a confocal microscope, and a Z-axis scanning mode is adopted in the three-dimensional imaging process.
The fluorescein marked water phase and the nile red marked oil phase are adopted, so that the oil-water two phases can be clearly distinguished under the excitation light, and the seepage situation in the displacement process can be more clearly observed.
Specifically, the embodiment provides a three-dimensional microfluidic chip 1, wherein the cross-sectional area of a visual shell 11 is 3×3mm 2, the length of the visual shell is 55mm, a thin-wall square glass tube is filled with hydrophilic glass beads with the radius of 38±3μm, and the hydrophilic glass beads are sintered for 10min at 850 ℃ to prepare the rigid three-dimensional microfluidic chip 1. The overall volume of the porous media was about 495mm 3, the effective porosity was about 40% as measured by image analysis, and the absolute permeability was about 3.9Darcy as measured by water injection.
After the pipeline connection is finished, the three-dimensional microfluidic chip 1 is horizontally fixed on a 40C heat table, and alkane separated from crude oil is pumped into the three-dimensional microfluidic chip 1 at a high injection rate (100 mu l min -1) to serve as an oil phase so as to ensure that the channel is saturated by the oil. After the oil saturation process is finished, pure water is injected into the channel at a certain speed for displacement, real-time pressure is recorded, and meanwhile, the temperature and the injection flow are monitored, so that the consistency of different experimental groups is ensured. The displacement process was carried out using a 2.5ml airtight syringe 3 at an injection rate of 10 μl·min -1.
To distinguish between the oil and water phases, 1×10 -4mol·L-1 fluorescein was used to label the water and 3×10 -5mol·L-1 nile red was used to label the oil phase. The displacement process was three-dimensionally imaged with confocal laser microscope 6, fluorescent images were captured using excitation filters in the wavelength range 420-485nm and emission filters in the wavelength 515nm, and the photographs were further three-dimensionally reconstructed by ZEN software. Three-dimensional imaging after 1 hour of displacement is shown in fig. 3.
Example 2
The embodiment provides a three-dimensional microfluidic chip 1, wherein the cross-sectional area of a visual shell 11 is 3 x 3mm 2, the length of the visual shell is 55mm of a thin-wall square glass tube, hydrophilic glass beads with the radius of 38+/-3 μm are filled, and the visual shell is sintered for 5min at 850 ℃ to prepare the rigid three-dimensional microfluidic chip 1. The overall volume of the porous media was about 495mm 3, the effective porosity was about 40% as measured by image analysis, and the absolute permeability was about 3.9Darcy as measured by water injection.
After the pipeline connection is finished, the three-dimensional microfluidic chip 1 is horizontally fixed on a 40C heat table, and alkane separated from crude oil is pumped into the three-dimensional microfluidic chip 1 at a high injection rate (100 mu l min -1) to serve as an oil phase so as to ensure that the channel is saturated by the oil. After the oil saturation process is finished, a cycloalkyl aryl sulfonate solution is injected into the channel at a certain speed for displacement, the real-time pressure is recorded, and the temperature and the injection flow are monitored at the same time, so that the consistency of different experimental groups is ensured. The displacement process was carried out using a 2.5ml airtight syringe 3 at an injection rate of 10 μl·min -1.
To distinguish between the oil and water phases, 1×10 -4mol·L-1 fluorescein was used to label the water and 3×10 -5mol·L-1 nile red was used to label the oil phase. The displacement process was three-dimensionally imaged with confocal laser microscope 6, fluorescent images were captured using excitation filters in the wavelength range 420-485nm and emission filters in the wavelength 515nm, and the photographs were further three-dimensionally reconstructed by ZEN software. Three-dimensional imaging after 1 hour of displacement is shown in fig. 4.
Example 3
The embodiment provides a three-dimensional microfluidic chip 1, wherein the cross-sectional area of a visual shell 11 is 3 x 3mm 2, the length of the visual shell is 55mm of a thin-wall square glass tube, hydrophilic glass beads with the radius of 38+/-3 μm are filled, and the visual shell is sintered for 5min at 850 ℃ to prepare the rigid three-dimensional microfluidic chip 1. The overall volume of the porous media was about 495mm 3, the effective porosity was about 40% as measured by image analysis, and the absolute permeability was about 3.9Darcy as measured by water injection.
After the pipeline connection is finished, the three-dimensional microfluidic chip 1 is horizontally fixed on a 40C heat table, and aromatic hydrocarbon separated from crude oil is pumped into the three-dimensional microfluidic chip 1 at a high injection rate (100 mu l min -1) to serve as an oil phase so as to ensure that the channel is saturated by the oil. After the oil saturation process is finished, pure water is injected into the channel at a certain speed for displacement, real-time pressure is recorded, and meanwhile, the temperature and the injection flow are monitored, so that the consistency of different experimental groups is ensured. The displacement process was carried out using a 2.5ml airtight syringe 3 at an injection rate of 10 μl·min -1.
To distinguish between the oil and water phases, 1×10 -4mol·L-1 fluorescein was used to label the water and 3×10 -5mol·L-1 nile red was used to label the oil phase. The displacement process was three-dimensionally imaged with confocal laser microscope 6, fluorescent images were captured using excitation filters in the wavelength range 420-485nm and emission filters in the wavelength 515nm, and the photographs were further three-dimensionally reconstructed by ZEN software. Three-dimensional imaging after 1 hour of displacement is shown in fig. 5.
Example 4
The embodiment provides a three-dimensional microfluidic chip 1, wherein the cross-sectional area of a visual shell 11 is 3 x 3mm 2, the length of the visual shell is 55mm, a thin-wall square glass tube is filled with hydrophilic glass beads with the radius of 38+/-3 mu m, and the visual shell is sintered for 8min at 850 ℃ to prepare the rigid three-dimensional microfluidic chip 1. The overall volume of the porous media was about 495mm 3, the effective porosity was about 40% as measured by image analysis, and the absolute permeability was about 3.9Darcy as measured by water injection.
After the pipeline connection is finished, the three-dimensional microfluidic chip 1 is horizontally fixed on a 40C heat table, and aromatic hydrocarbon separated from crude oil is pumped into the three-dimensional microfluidic chip 1 at a high injection rate (100 mu l min -1) to serve as an oil phase so as to ensure that the channel is saturated by the oil. After the oil saturation process is finished, a cycloalkyl aryl sulfonate solution is injected into the channel at a certain speed for displacement, the real-time pressure is recorded, and the temperature and the injection flow are monitored at the same time, so that the consistency of different experimental groups is ensured. The displacement process was carried out using a 2.5ml airtight syringe 3 at an injection rate of 10 μl·min -1.
To distinguish between the oil and water phases, 1×10 -4mol·L-1 fluorescein was used to label the water and 3×10 -5mol·L-1 nile red was used to label the oil phase. The displacement process was three-dimensionally imaged with confocal laser microscope 6, fluorescent images were captured using excitation filters in the wavelength range 420-485nm and emission filters in the wavelength 515nm, and the photographs were further three-dimensionally reconstructed by ZEN software. Three-dimensional imaging after 1 hour of displacement is shown in fig. 6.
Example 5
The embodiment provides a three-dimensional microfluidic chip 1, wherein the cross-sectional area of a visual shell 11 is 3 x 3mm 2, the length of the visual shell is 55mm, a thin-wall square glass tube is filled with hydrophilic glass beads with the radius of 19+/-2 mu m, and the hydrophilic glass beads are sintered for 7min at 900 ℃ to prepare the rigid three-dimensional microfluidic chip 1. The overall volume of the porous media was about 495mm 3, the effective porosity was about 34% as measured by image analysis, and the absolute permeability was about 190mD as measured by water injection.
After the pipeline connection is completed, the three-dimensional microfluidic chip 1 is horizontally fixed on a heat table at 40 ℃, and alkane separated from crude oil is pumped into the three-dimensional microfluidic chip 1 at a high injection rate (30 mu l min -1) as an oil phase to ensure that the channel is saturated with oil. After the oil saturation process is finished, pure water is injected into the channel at a certain speed for displacement, real-time pressure is recorded, and meanwhile, the temperature and the injection flow are monitored, so that the consistency of different experimental groups is ensured. The displacement process was carried out using a 2.5ml airtight syringe 3 at an injection rate of 1 μl·min -1.
To distinguish between the oil and water phases, 1×10 -4mol·L-1 fluorescein was used to label the water and 3×10 -5mol·L-1 nile red was used to label the oil phase. The displacement process was three-dimensionally imaged with confocal laser microscope 6, fluorescent images were captured using excitation filters in the wavelength range 420-485nm and emission filters in the wavelength 515nm, and the photographs were further three-dimensionally reconstructed by ZEN software. Three-dimensional imaging after 1 hour of displacement is shown in fig. 7.
Example 6
The embodiment provides a three-dimensional microfluidic chip 1, wherein the cross-sectional area of a visual shell 11 is 3 x 3mm 2, the length of the visual shell is 55mm, a thin-wall square glass tube is filled with hydrophilic glass beads with the radius of 75+/-5 mu m, and the visual shell is sintered for 6min at 950 ℃ to prepare the rigid three-dimensional microfluidic chip 1. The overall volume of the porous media was about 495mm 3, the effective porosity was about 41% as measured by image analysis, and the absolute permeability was about 8.7Darcy as measured by water injection.
After the pipeline connection is completed, the three-dimensional microfluidic chip 1 is horizontally fixed on a heat table at 40 ℃, and alkane separated from crude oil is pumped into the three-dimensional microfluidic chip 1 at a high injection rate (20 mu l min -1) to serve as an oil phase so as to ensure that the channel is saturated by the oil. After the oil saturation process is finished, pure water is injected into the channel at a certain speed for displacement, real-time pressure is recorded, and meanwhile, the temperature and the injection flow are monitored, so that the consistency of different experimental groups is ensured. The displacement process was carried out using a 2.5ml airtight syringe 3 at an injection rate of 1 μl·min -1.
To distinguish between the oil and water phases, 1×10 -4mol·L-1 fluorescein was used to label the water and 3×10 -5mol·L-1 nile red was used to label the oil phase. The displacement process was three-dimensionally imaged with confocal laser microscope 6, fluorescent images were captured using excitation filters in the wavelength range 420-485nm and emission filters in the wavelength 515nm, and the photographs were further three-dimensionally reconstructed by ZEN software. Three-dimensional imaging after 1 hour of displacement is shown in fig. 8.
Example 7
The embodiment provides a three-dimensional microfluidic chip 1, wherein the cross-sectional area of a visual shell 11 is 3 x 3mm 2, the length of the visual shell is 55mm, a thin-wall square glass tube is filled with hydrophilic glass beads with the radius of 45+/-3 mu m, and the visual shell is sintered for 6min at 900 ℃ to prepare the rigid three-dimensional microfluidic chip 1. The overall volume of the porous media was about 495mm 3, the effective porosity was about 40% as measured by image analysis, and the absolute permeability was about 4.1Darcy as measured by water injection.
After the pipeline connection is completed, the three-dimensional microfluidic chip 1 is horizontally fixed on a heat table at 40 ℃, and alkane separated from crude oil is pumped into the three-dimensional microfluidic chip 1 at a high injection rate (100 mu l min -1) to serve as an oil phase so as to ensure that the channel is saturated by the oil. After the oil saturation process is finished, a cycloalkyl aryl sulfonate solution is injected into the channel at a certain speed for displacement, the real-time pressure is recorded, and the temperature and the injection flow are monitored at the same time, so that the consistency of different experimental groups is ensured. The displacement process was carried out using a 2.5ml airtight syringe 3 at an injection rate of 10 μl·min -1.
To distinguish between the oil and water phases, 1×10 -4mol·L-1 fluorescein was used to label the water and 3×10 -5mol·L-1 nile red was used to label the oil phase. The displacement process was three-dimensionally imaged with confocal laser microscope 6, fluorescent images were captured using excitation filters in the wavelength range 420-485nm and emission filters in the wavelength 515nm, and the photographs were further three-dimensionally reconstructed by ZEN software. Three-dimensional imaging after 1 hour of displacement is shown in fig. 9.
The foregoing details of the optional implementation of the embodiment of the present invention have been described in conjunction with the accompanying drawings, but the embodiment of the present invention is not limited to the specific details of the foregoing implementation, and various simple modifications may be made to the technical solution of the embodiment of the present invention within the scope of the technical concept of the embodiment of the present invention, where all the simple modifications belong to the protection scope of the embodiment of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, various possible combinations of embodiments of the present invention are not described in detail.
Those skilled in the art will appreciate that all or part of the steps in implementing the methods of the embodiments described above may be implemented by a program stored in a storage medium, including instructions for causing a single-chip microcomputer, chip or processor (processor) to perform all or part of the steps of the methods of the embodiments described herein. And the aforementioned storage medium includes: a usb disk, a removable hard disk, a Read-Only Memory (ROM), a random access Memory (RAM, random Access Memory), a magnetic disk, or an optical disk, or other various media capable of storing program codes.
In addition, any combination of various embodiments of the present invention may be performed, so long as the concept of the embodiments of the present invention is not violated, and the disclosure of the embodiments of the present invention should also be considered.
Claims (9)
1. The three-dimensional microfluidic chip is characterized by comprising a visual shell (11) and a seepage body (12), wherein the seepage body (12) is sintered in the visual shell (11), the seepage body (12) is formed by sintering a plurality of visual microbeads, and the seepage morphology of a fluid to be observed is observed through the seepage body (12); the visual shell (11) is made of quartz glass, and the visual microbeads are made of spherical borosilicate glass; the permeability of the three-dimensional microfluidic chip (1) is determined by the size of the visual microbeads, the sintering temperature and the sintering time.
2. The three-dimensional microfluidic chip according to claim 1, wherein the three-dimensional microfluidic chip (1) further comprises a fluid inlet (13) and a fluid outlet (14), the fluid inlet (13) and the fluid outlet (14) being provided at a first side wall and a second side wall of the visualization housing (11), respectively, the first side wall being opposite to the second side wall.
3. A three-dimensional microfluidic system, characterized by comprising a fluid input assembly, an observation stage, a fluid morphology sampling assembly, and a three-dimensional microfluidic chip (1) according to any one of claims 1-2; the three-dimensional microfluidic chip (1) is arranged on the observation table, and the output end of the fluid input assembly is connected with the three-dimensional microfluidic chip and is used for injecting fluid into the three-dimensional microfluidic chip (1); the fluid form sampling assembly is erected above the three-dimensional microfluidic chip (1) and is used for collecting seepage forms of fluid in the three-dimensional microfluidic chip (1).
4. The three-dimensional microfluidic system according to claim 3, wherein the fluid input assembly comprises a micro-sampling pump (2) and an injector (3), the injector (3) being arranged above the micro-sampling pump (2) and connected to the micro-sampling pump (2), the volume of fluid injected being controlled by the micro-sampling pump (2).
5. A three-dimensional microfluidic system according to claim 3, wherein the observation stage is a constant temperature heating stage (4), and a temperature sensor is further provided on the constant temperature heating stage (4), and the temperature sensor is used for monitoring the temperature on the constant temperature heating stage (4).
6. A three-dimensional microfluidic system according to claim 3, wherein the fluid body sampling assembly comprises an image acquisition device (5), a laser confocal microscope (6) and a computer (7), the laser confocal microscope (6) is arranged above the three-dimensional microfluidic chip (1), the image acquisition device (5) is used for acquiring imaging results of the laser confocal microscope (6), and the computer (7) is used for processing and displaying acquisition results of the image acquisition device (5).
7. A three-dimensional microfluidic system according to claim 3, further comprising a pressure sensor (8), the pressure sensor (8) being arranged on the fluid inlet (13) side and the fluid outlet (14) side of the three-dimensional microfluidic chip (1), respectively.
8. A three-dimensional microfluidic system according to claim 3, further comprising a fluid collection device, said fluid collection device being a standard nuclear magnetic tube (9), said standard nuclear magnetic tube (9) being provided with graduation marks.
9. A method for preparing a three-dimensional microfluidic chip for manufacturing the three-dimensional microfluidic chip according to claim 2, comprising the steps of:
And (3) packaging: filling the visual shell (11) with visual microbeads, and sealing a fluid outlet (14) and a fluid inlet (13) on the visual shell (11);
And (3) sintering: placing the packaged three-dimensional microfluidic chip (1) into a muffle furnace for sintering, wherein the sintering temperature is not lower than 821 ℃, and the sintering time is less than 10 minutes;
The installation step comprises the following steps: and fixing the three-dimensional microfluidic chip (1) after sintering on an observation table, and installing pipelines at the positions of the fluid inlet (13) and the fluid outlet (14) to realize fluid circulation.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211318808.5A CN117920364A (en) | 2022-10-26 | 2022-10-26 | Three-dimensional microfluidic chip, preparation method thereof and three-dimensional microfluidic system |
| PCT/CN2023/112517 WO2024087802A1 (en) | 2022-10-26 | 2023-08-11 | Three-dimensional microfluidic chip and preparation method therefor, and three-dimensional microfluidic system |
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| CN202211318808.5A CN117920364A (en) | 2022-10-26 | 2022-10-26 | Three-dimensional microfluidic chip, preparation method thereof and three-dimensional microfluidic system |
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| CN112730196B (en) * | 2020-12-25 | 2022-03-11 | 西南石油大学 | High-temperature high-pressure microscopic visual flowing device and experimental method |
| WO2022147565A1 (en) * | 2021-01-04 | 2022-07-07 | Saudi Arabian Oil Company | Microfluidic chip with multiple porosity regions for reservoir modeling |
| US11534759B2 (en) * | 2021-01-22 | 2022-12-27 | Saudi Arabian Oil Company | Microfluidic chip with mixed porosities for reservoir modeling |
| CN114011478B (en) * | 2021-02-20 | 2023-06-02 | 中国海洋石油集团有限公司 | Multifunctional microfluidic chip and manufacturing method thereof |
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