CN107939387A - A kind of microcosmic rock network model production method - Google Patents
A kind of microcosmic rock network model production method Download PDFInfo
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- CN107939387A CN107939387A CN201711123139.5A CN201711123139A CN107939387A CN 107939387 A CN107939387 A CN 107939387A CN 201711123139 A CN201711123139 A CN 201711123139A CN 107939387 A CN107939387 A CN 107939387A
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- E—FIXED CONSTRUCTIONS
- E21—EARTH DRILLING; MINING
- E21B—EARTH DRILLING, e.g. DEEP 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
Abstract
The invention discloses a kind of microcosmic rock network model production method, including：Pore throat passage is extracted, the hole in pore throat passage and venturi are separated, obtains pattern of apertures and venturi pattern, makes hole mask and venturi mask respectively；Substrate is performed etching using the hole mask and venturi mask, forms etching substrate；The etching substrate is bonded with cover plate, forms microcosmic rock network model.The present invention is separated by pore throat, image alignment and repetition photoetching realize the micro-nano oil gas flow channel for being more bonded oil reservoir reality on microscopic glass model; the control in reaction time is accurate in etching technics; the depth-to-width ratio of passage, smoothness and flatness are preferable; bonding process need not provide pressure; nanochannel can preferably be protected; the bonding of the authentic sandstone micromodel of micro-void and nanometer venturi is realized, the change of the Micro dynamics such as the Haynes step that cannot occur in two-dimensional model and non-wetted phase coalescence is presented.
Description
Technical field
The present embodiments relate to oil and gas development field, more particularly to a kind of microcosmic rock network model production method.
Background technology
With deepening continuously for petrol resources exploitation correlation theory research, the hot spot and difficulties of oil-gas field development are gradual
Changed from the exploitation of conventional gas and oil with improving recovery ratio to unconventionaloil pool Efficient Development.
China's microphysics simulated experiment is started late, Chinese Academy of Sciences's seepage flow using the flat academicians of Guo Shang as academic leader
The thought of " microscopic seepage " is proposed earlier, and a series of microscopic seepage emulation and test skill are formd in the nineties in last century
Art, in conventional oil reservoir micro-meter scale passage fluid flowing carried out numerous studies, disclose some important seepage flow mechanisms and
Rule, theory support is provided for routine oil reservoir development.Recently as the expansion of microphysics model use scope, Zhu Wei
The senior scholar in many oil-gas field development fields such as credit, Dai Caili and Yue Xiangan using true sandstone microscopic glass model and
The microscopic glass model of rule has carried out the research of the chemical flooding mechanism of action, and improving recovery ratio research for conventional oil reservoir has provided
Effect support.
But past microscopic glass model exists compared with big limitation when being developed applied to compact oil reservoir, is mainly manifested in four
A aspect：(1) conventional etching sandpack column channel dimension is generally bigger than normal, generally at 20 μm -200 μm, with compact oil reservoir main aperture
Larynx size difference larger (20 μm -80 μm of hole, venturi 100nm-700nm) is difficult to use in stream of the fluid in micro/nano-scale pore throat
Dynamic research；(2) conventional visualization micro-fluidic chip is all two-dimentional chip, whole molded passage depth all, this and true sand
Three dimensional differences have greatest differences between petrosal foramen larynx, and Haynes step that fluid flows between pore throat, grease coalescence etc. are microcosmic dynamic
State is difficult to occur, and there are larger difference with flow regime of the oil gas in compact oil reservoir；(3) using true sandstone section as raw material
The micromodel of making, needs addition adhesive to change core surface property in the production process, and observing effect is poor, up to not
To the flowing of observation channel interior fluid, absorption, the purpose spread.
The content of the invention
The present invention provides a kind of microcosmic rock network model production method, for the micro- of nontraditional reservoir especially compact oil reservoir
The research that fluid flows in metrical scale passage, there is provided be more bonded actual microphysics model.
An embodiment of the present invention provides a kind of microcosmic rock network model production method, including：
Pore throat passage is extracted, the hole in pore throat passage and venturi are separated, obtains pattern of apertures and venturi pattern,
Hole mask and venturi mask are made respectively；
Substrate is performed etching using the hole mask and venturi mask, forms etching substrate；
The etching substrate is bonded with cover plate, forms microcosmic rock network model.
Wherein, the hole in pore throat passage and venturi are separated, obtaining pattern of apertures and venturi pattern includes：
Binary conversion treatment is carried out to the image of rock section, distinguishes rock matrix pattern and pore throat channel pattern；
Determine central axes all in pore throat channel pattern；
Circle is done by the center of circle of each pixel on central axes, the radius of the circle reaches nearest rock matrix for its center of circle
Distance；
Radius being met to, the center of circle of the circle of preset condition is defined as node, corresponding pore throat channel pattern is at each node
Pattern of apertures, the pore throat channel pattern of remainder is venturi pattern.
Wherein, substrate is performed etching using the hole mask and venturi mask, including：
Hole etches, and the substrate is performed etching using the hole mask, and formation etches partially substrate；
Mask alignment, according to corresponding first mark being carved with the hole mask and venturi mask, by described half
Etching substrate is aligned with venturi mask；
Venturi etches, and the substrate that etches partially is performed etching using the venturi mask, obtains the etching substrate；
Model cleans, and the etching substrate is cleaned.
Wherein, the method for the hole etching includes：
Hole mask and substrate are stacked together and are exposed by exposure machine, so that the pattern of hole mask is transferred to
On substrate；
Clean the photoresist and exposed portion on the substrate；
Under ultrasound bath environment, dip the substrate into the first etching liquid and perform etching 30min, formation etches partially base
Piece, first etching liquid are the NH of 0.5mol/L using the HF of 1mol/L as etching agent4F is complexing agent, the HNO of 0.5mol/L3
For the mixing liquid of cosolvent.
Wherein, the line width of first mark sets multiple for the first of the pore throat channel width.
Further, corresponding second mark, second mark are also carved with the hole mask and venturi mask
In the predeterminable area of the described first mark, the line width of second mark is the described first the second setting times for marking line width
Number, the length of the second mark set multiple for the 3rd of the described first mark line width；
Correspondingly, the mask alignment includes：
According to corresponding first mark and the second mark being carved with the hole mask and venturi mask, by described half
Etching substrate is aligned with venturi mask.
Wherein, the venturi etching includes：
By the venturi mask of alignment and substrate is etched partially by exposure machine progress re-expose, so that the pattern of venturi mask
It is transferred to and etches partially on substrate；
The photoresist and exposed portion on substrate are etched partially described in cleaning；
Under ultrasound bath environment, it will etch partially in substrate the second etching liquid of immersion and perform etching 30min, form etching
Substrate, second etching liquid are the NH of 0.0075mol/L using the HF of 0.015mol/L as etching agent4F is complexing agent,
The HNO of 0.0075mol/L3For the mixing liquid of cosolvent.
Wherein, the etching substrate is bonded with cover plate, including：
The etching substrate is pre-processed；
Substrate and cover plate fitting will be etched, forms initial microcosmic rock network model；
The initial microcosmic rock network model is bonded by high-temperature sintering process, forms microcosmic rock network mould
Type.
Wherein, it is described that the initial microcosmic rock network model is bonded by high-temperature sintering process, including：
Initial microcosmic rock network model is put in vacuum high temperature furnace, the vacuum high temperature furnace is carried out to vacuumize place
Reason；
High-temperature vacuum in-furnace temperature is risen to 50 DEG C by room temperature with the speed of 2 DEG C/min, constant temperature 30min after reaching 50 DEG C；
High-temperature vacuum in-furnace temperature is risen to 120 DEG C with the speed of 2 DEG C/min, constant temperature 150min after reaching 120 DEG C；
High-temperature vacuum in-furnace temperature is risen to 700 DEG C with the speed of 1.5 DEG C/min, constant temperature 120min after reaching 700 DEG C；
Naturally cool to room temperature.
Further, further include：
To the initial microcosmic toluene solution of the rock network model inlet injection containing 1% trichloromethyl silane (TCMS)
To constraint water state, to carry out wetting modification to the initial microcosmic rock network model.
The research that the present invention is flowed for fluid in the micro-meter scale passage of nontraditional reservoir especially compact oil reservoir, passes through hole
Larynx separates and repeat photoetching realizes the micro-nano oil gas flow channel for being more bonded oil reservoir reality on microscopic glass model
Portray, there is provided be more bonded actual microphysics model, the extra large grace that cannot occur in two-dimensional model originally can be made
The change of the Micro dynamic such as this step and non-wetted phase coalescence is presented, to promoting fine and close oil gas fundamental research to have very
Benefit greatly.
Brief description of the drawings
Fig. 1 is a kind of flow chart for microcosmic rock network model production method that the embodiment of the present invention one provides；
Fig. 2 is the flow chart for another microcosmic rock network model production method that the embodiment of the present invention one provides；
Fig. 3 is the microcosmic reservoir rocks section picture binaryzation schematic diagram that the embodiment of the present invention one provides；
Fig. 4 is the axis detection schematic diagram that the embodiment of the present invention one provides；
Fig. 5 is the hole node schematic diagram for the pore throat channel interior that the embodiment of the present invention one provides；
Fig. 6 is hole-venturi recognition result schematic diagram that the embodiment of the present invention one provides；
Fig. 7 is the venturi point of intersection hole node schematic diagram that the embodiment of the present invention one provides；
Fig. 8 is the flow chart of the microcosmic rock network model production method of another kind provided by Embodiment 2 of the present invention；
Fig. 9 is hole mask and venturi mask schematic diagram provided by Embodiment 2 of the present invention；
Figure 10 is the flow chart for another microcosmic rock network model production method that the embodiment of the present invention three provides；
Figure 11 is the flow chart for another microcosmic rock network model production method that the embodiment of the present invention four provides.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.It is understood that this place is retouched
The specific embodiment stated is used only for explaining the present invention, rather than limitation of the invention.It also should be noted that in order to just
It illustrate only part related to the present invention rather than entire infrastructure in description, attached drawing.
Embodiment one
A kind of flow chart for microcosmic rock network model production method that Fig. 1 provides for the embodiment of the present invention one, this implementation
Example is applicable to the making of compact oil reservoir micromodel, specifically comprises the following steps：
Step 110, extraction pore throat passage, the hole in pore throat passage and venturi are separated, obtain pattern of apertures and
Venturi pattern, makes hole mask and venturi mask respectively.
Wherein, extracting pore throat passage can use the true sandstone body of casting to realize, the slice-shaped that the true sandstone body of casting is cut into
Cut into slices into rock, binary conversion treatment is carried out by the image that the rock is cut into slices, distinguishes the rock matrix in rock sectioning image
Region and pore throat passage area, realize the extraction of pore throat passage, obtain the pattern that pore region is formed, wherein pore throat channel region
In domain, the region for removing pattern of apertures is venturi pattern, is then carved into pattern of apertures and venturi pattern on mask again respectively,
Hole mask and venturi mask can be obtained, the material of mask can use stainless steel, copper, alloy etc., not be limited herein.
Preferably, the hole in pore throat passage and venturi are separated, obtaining pattern of apertures and venturi pattern includes：
S111, the image to rock section carry out binary conversion treatment, distinguish rock matrix pattern and pore throat channel pattern；
Specifically, Fig. 2 is the flow for another microcosmic rock network model production method that the embodiment of the present invention one provides
Figure, Fig. 3 are the microcosmic reservoir rocks section picture binaryzation schematic diagrames that the embodiment of the present invention one provides.With reference to figure 3, wherein black
Part is the rock matrix obtained after binaryzation, and white portion is the pore throat passage obtained after binaryzation.
S112, determine central axes all in pore throat channel pattern；
Wherein, Fig. 4 is the axis detection schematic diagram that the embodiment of the present invention one provides, and with reference to figure 3 and Fig. 4, utilizes image
Treatment technology carries out hole and venturi to pore throat passage and separates, and black region is rock matrix in original-shape, white picture
Plain region is pore throat passage, by repeatedly rejecting the pixel contacted in pore throat passage with rock matrix, until channel cross-section is only surplus
One pixel, so as to obtain the central axes of pore throat passage.
S113, using each pixel on central axes as the center of circle do circle, and round radius reaches nearest rock matrix for its center of circle
Distance；
Wherein, pore throat channel interior there are hole, and the hole of pore throat channel interior can be by pore throat channel interior
Pixel does circle to judge the size in space residing for the pixel, so that it is determined that the position of pore throat channel interior hole on axis.Specifically
, Fig. 5 is the hole node schematic diagram for the pore throat channel interior that the embodiment of the present invention one provides, with reference to figure 5, on central axes
At each pixel, the circle of a pre-set radius is done using the pixel as the center of circle, which can set as the case may be
A numerical value less than normal is put, then expands round radius, judges whether circumference contacts with rock matrix pixel, if so, then working as first half
Footpath is the distance that the center of circle reaches nearest rock matrix.
Radius, is met that the center of circle of circle of preset condition is defined as node by S114, corresponding pore throat passage at each node
Pattern is pattern of apertures, and the pore throat channel pattern of remainder is venturi pattern.
Wherein, by S113, it can obtain and be placed on pore throat passage and greatest circle of the center of circle on central axes, by all quilts
Comprising ball delete, that is, obtain the circle sequence fitted closely with pore throat passage, check default with the presence or absence of meeting on central axes
The circle of condition, the preset condition for example can be that current pixel point corresponds to whether greatest circle exceedes neighbor pixel on central axes
The preset multiple of corresponding greatest circle, if it does, then the pixel corresponds to greatest circle and then may be defined as node, which can
To be set according to actual hole and venturi size；Can also be whether the corresponding greatest circle of current pixel point is in place
The circle of radius maximum on axis, if so, then the definable pixel is node.Fig. 6 be the embodiment of the present invention one provide hole-
Venturi recognition result schematic diagram, with reference to figure 6, it can be seen that, hole is separated from pore throat passage.Specifically, hole is except presence
Outer inside venturi in pore throat passage, the intersection area of venturi and venturi is generally also bigger, i.e., hole there is likely to be in larynx
The intersection area in road, Fig. 7 are the venturi point of intersection hole node schematic diagrames that the embodiment of the present invention one provides, can be by venturi intersection point
Hole node definition in region is more than 2 hole node for ligancy, wherein, on central axes the ligancy of pixel refer to
The number of the adjacent central axes pixel of the pixel, it is clear that the hole node inside venturi as shown in Figure 5 then may be defined as matching somebody with somebody
Digit is 2 hole node.With reference to figure 7, the picture for determining that 2 can also be more than by searching for ligancy on central axes of hole node
The node of the intersection area of vegetarian refreshments, i.e. venturi, so as to obtain the hole at intersection area.
Obviously, node as described above is hole node, and corresponding pore throat channel pattern can be with each hole node
It is the region that the greatest circle using the node as the center of circle forms, pattern of apertures is then by the corresponding pore throat channel pattern group of hole node
Into venturi pattern is then the region composition that pattern of apertures is removed in pore throat passage, and pattern of apertures and venturi pattern correspond respectively to
Hole and venturi in rock section pore throat passage, it is thus achieved that the separation of rock section mesopore and venturi.
Step 120, using hole mask and venturi mask perform etching substrate, forms etching substrate.
Wherein, the substrate can be glass substrate or glass spin coating chromium plate, according to the hole obtained in last step
Mask and venturi mask respectively carry out same spin coating chromium plate photoetching, including the cleaning of ultraviolet exposure, photoresist, to wash chrome liquor clear
Wash, substrate etching and substrate cleaning etc., portray, restored inside the true sandstone body of casting so as to carry out hole and venturi to substrate
Channel network.
Step 130, will etching substrate be bonded with cover plate, form microcosmic rock network model.
Wherein, etching the pore throat passage portrayed on substrate needs to be closed by cover plate, and leads in order not to change pore throat
For the surface nature of road and substrate, it is necessary to by substrate and cover plate Direct Bonding under certain condition, bonding is then that two panels surface is clear
Clean, atomically flating homogeneity or heterogeneous semiconductor material are through surface clean and activation process, by Van der Waals force, molecular force very
Substrate bonding is integrally formed to atomic force.
The technical solution of the embodiment of the present invention is for fluid in the micro-meter scale passage of nontraditional reservoir especially compact oil reservoir
The research of flowing, photoetching is separated and repeated by pore throat realizes the micro-nano for being more bonded oil reservoir reality on microscopic glass model
Rice bran oil flow of air passage is portrayed, there is provided be more bonded actual microphysics model, make originally in two-dimensional model not
The Micro dynamic change such as the Haynes step and non-wetted phase coalescence that can occur is presented, to promoting fine and close oil gas basis reason
Have by research and benefit greatly very much.
Embodiment two
Fig. 8 is the flow chart of the microcosmic rock network model production method of another kind provided by Embodiment 2 of the present invention, reference
Fig. 8, in production method provided in this embodiment, S120, using hole mask and venturi mask perform etching substrate, specific bag
Include following steps：
S121, hole etching, perform etching substrate using hole mask, formation etches partially substrate；
Wherein, in the step hole etching and step S123 in venturi etching can use wet-etching technology into
OK, can be obtained by hole etching be carved with hole etch partially substrate.
Preferably, the method for hole etching includes：Hole mask and substrate are stacked together and exposed by exposure machine
Light, so that the pattern of hole mask is transferred on substrate；Clean the photoresist and exposed portion on the substrate；In ultrasonic water
Bathe under environment, dip the substrate into the first etching liquid and perform etching 30min, formation etches partially substrate, and first etching liquid is
Using the HF of 1mol/L as etching agent, the NH of 0.5mol/L4F is complexing agent, the HNO of 0.5mol/L3For the mixing liquid of cosolvent.
Wherein, hole mask can be stacked together by hole etching with spin coating chromium plate first is exposed on exposure machine,
The pattern of hole is transferred on spin coating chromium plate；Then cleaned with 5 ‰ NaOH solution, wash away the photoetching on spin coating chromium plate
Glue；Cleaned again with washing chrome liquor, wash away the exposed portion on spin coating chromium plate, by spin coating chromium plate with the corresponding glass of hole
It is exposed；Under ultrasound bath environment, the spin coating chromium plate for exposing hole is immersed in glass etching liquid and is performed etching,
So as to obtain be carved with hole etch partially substrate.Researcher draws the first etching liquid etched for hole by test of many times
Preferably using the HF of 1mol/L as etching agent, the NH of 0.5mol/L4F is complexing agent, the HNO of 0.5mol/L3For the mixing of cosolvent
Liquid, can be etched within the very fast time using the first etching liquid of higher concentration and form hole of the depth at tens microns, its
Etch period is preferably 30min, can at utmost realize the recovery of hole, while HNO is added in etching liquid3And NH4Cl,
Non-uniform corrosions of the HF to glass is suppressed by the principle of ion exchange, ensure that smoothness, flatness and the depth-to-width ratio of hole,
With preferable etching effect.
S122, mask alignment, according to corresponding first mark being carved with hole mask and venturi mask, will etch partially
Substrate is aligned with venturi mask；
Fig. 9 is hole mask and venturi mask schematic diagram provided by Embodiment 2 of the present invention, and hole has been etched in order to realize
The matching for etching partially venturi to be etched on substrate and mask, must carry out the alignment of both before venturi etching, can be in hole
Corresponding mark is portrayed on gap mask and venturi mask, with reference to figure 9, such as can be "+" vernier, etches and completes in hole
Afterwards, venturi mask can be by the first mark 91 thereon with etching partially the first mark 91 etched on substrate completion pair
It is accurate.
Alternatively, the line width of the first mark sets multiple for the first of pore throat channel width.
In order to make hole and venturi reach accurate matching, avoid due to mark it is excessive and caused by hole be aligned with venturi
Failure, can be arranged to the size suitable with pore throat channel width by the line width of the first mark, wherein, pore throat channel width can be with
The average value of pore throat channel width minimum value or all pore throat channel widths is taken, is not limited herein, such as "+" number
The line width of vernier can be 5 times of pore throat passage minimum widith.
Alternatively, corresponding second mark is also carved with hole mask and venturi mask, the second mark is positioned at the first mark
In the predeterminable area of note, the line width of the second mark is the second setting multiple of the first mark line width, and the length of the second mark is the
3rd setting multiple of one mark line width；Correspondingly, mask alignment includes：According to the phase being carved with hole mask and venturi mask
Corresponding first mark and the second mark, will etch partially substrate and are aligned with venturi mask.
Due to the line width of the first mark 91 set it is suitable with pore throat channel width, so when being directed at the first mark 91,
May be because the first mark 91 be too small and is difficult to find, in order to become apparent from and easily search out the first mark 91, can be with
Second mark 92 is set in the predeterminable area of the first mark 91, and the second mark can be arranged on the setting orientation of the first mark 91
Setpoint distance on, such as position as shown in Figure 9 can be placed on.Meanwhile in order to more conveniently by the second mark 92
The first mark 91 is found, the size of the second mark 92 can be the setting multiple of the first mark 91, with reference to figure 9, the second mark 92
Line segment can be used and its width is 6 times of "+" vernier line width, length is 16 times of "+" vernier line width.
S123, venturi etching, are performed etching using venturi mask to etching partially substrate, obtain etching substrate；
Wherein, the venturi etching in the step is identical with the wet-etching technology that the hole etching in step S121 uses,
The substrate that etches partially for being carved with hole can be etched into while have hole and an etching substrate of venturi by venturi etching, so that
The pore throat passage in sandstone section is restored.
Alternatively, the venturi mask of alignment is subjected to re-expose with etching partially substrate by exposure machine, so that venturi is covered
The pattern of film, which is transferred to, to be etched partially on substrate；Cleaning etches partially photoresist and exposed portion on substrate；In ultrasound bath ring
Under border, substrate will be etched partially immerse in the second etching liquid and perform etching 30min, form etching substrate, the second etching liquid be with
The HF of 0.015mol/L is etching agent, the NH of 0.0075mol/L4F is complexing agent, the HNO of 0.0075mol/L3For the mixed of cosolvent
Close liquid.
Likewise, after venturi mask is aligned with the spin coating chromium plate of etched hole, re-expose is carried out, by larynx
Road pattern is transferred on spin coating chromium plate；Then cleaned with 5 ‰ NaOH solution, wash away the photoetching at venturi on spin coating chromium plate
Glue；Cleaned again with washing chrome liquor, wash away the re-expose part on spin coating chromium plate, will be corresponding with venturi on spin coating chromium plate
Glass is exposed；Under ultrasound bath environment, the spin coating chromium plate for exposing hole is immersed in glass etching liquid and is carried out
Etching, thus obtain be carved with hole etch partially substrate.Researcher draws etched for venturi second by test of many times
Etching liquid is the NH of 0.0075mol/L using the HF of 0.015mol/L as etching agent4F is complexing agent, the HNO of 0.0075mol/L3For
The mixing liquid of cosolvent, and when etch period is 30min, can at utmost realize the recovery of hole, have preferable
Etching effect.The second etching liquid of low concentration carries out venturi etching, hundreds of nanometers of venturi etch period can be maintained at tens
Minute, etching depth provides the enough reaction time in order to control.HNO is added in etching liquid at the same time3And NH4Cl, passes through ion exchange
Principle suppress non-uniform corrosions of the HF to glass, ensure smoothness, flatness and the depth-to-width ratio of passage.
S124, model cleaning, clean etching substrate.
In order to ensure the cleaning of model and facilitate follow-up bonding steps, being put into concentration after being cleaned with deionized water is
Photoresist is washed away in 5% NaOH solution, then is put into wash after being cleaned with deionized water and layers of chrome is washed away in chrome liquor.Wash away after layers of chrome again
Chip is rinsed with deionized water.
The technical solution of the embodiment of the present invention, hole present in the pore throat passage by actual sandstone and venturi carry out respectively
Etching, so as to form the hole and venturi for meeting true compact oil reservoir size, efficiently differentiates perforate gap and venturi, and pass through
The substrate that etches partially that mark enables to have etched hole is matched with venturi to be etched on mask and is aligned, and has accurately restored fine and close oil
Hole and venturi in Tibetan, realize the microcosmic rock network model for being more in line with actual compact oil reservoir.
Embodiment three
Figure 10 is the flow chart for another microcosmic rock network model production method that the embodiment of the present invention three provides.With reference to
Figure 10, in production method provided in this embodiment, etching substrate, be bonded by S130 with cover plate, forms microcosmic rock network
Model, specifically comprises the following steps：
S131, pre-process etching substrate；
Wherein, carrying out pretreatment to etching substrate includes boiling processing and rinsing, uses H first2SO4With H2O2By 4:1 ratio
Example configuration solution boils processing etching substrate and cover plate 10-15min, is then used for respectively with petroleum ether and ethanol rinsing 10min
To etching substrate and cover plate cleaning, wherein petroleum ether can wash away the organic matter adhered on etching substrate and cover plate, and ethanol is used for
Wash away the inorganic matter adhered on etching substrate and cover plate.By the pretreatment to etching substrate and cover plate, etching base can be removed
The impurity of piece and coverslip surface, improves the surface hydrophilicity of etching substrate and cover plate, enables etching substrate and cover plate closer
Fitting.
S132, will etch substrate and cover plate fitting, form initial microcosmic rock network model；
Wherein, pretreated etching substrate and cover plate are rinsed into 30min under deionized water, ensure etching substrate with
Pretreatment fluid is no longer remained on cover plate, is then bonded etching substrate and cover plate.
S133, by high-temperature sintering process be bonded initial microcosmic rock network model, forms microcosmic rock network mould
Type.
Wherein, the advantages of having reaction-sintered and hot pressed sintering in high-temperature sintering process concurrently is, it can be achieved that etching substrate and cover plate
Bonding, is made high-compactness, the microcosmic rock network model of the high accuracy of low linear shrinkage ratio.
Preferably, the initial microcosmic rock network model is bonded by high-temperature sintering process, including：Will be initial micro-
See rock network model to be put in vacuum high temperature furnace, vacuumize process is carried out to the vacuum high temperature furnace；With the speed of 2 DEG C/min
High-temperature vacuum in-furnace temperature is risen to 50 DEG C by room temperature, constant temperature 30min after reaching 50 DEG C；It is with the speed of 2 DEG C/min that high temperature is true
Empty in-furnace temperature rises to 120 DEG C, constant temperature 150min after reaching 120 DEG C；With the speed of 1.5 DEG C/min by high-temperature vacuum in-furnace temperature
700 DEG C are risen to, constant temperature 120min after reaching 700 DEG C；Naturally cool to room temperature.
Usual micro-fluidic chip bonding method is mainly using technologies such as adhesive, aux. pressure, stringent super-clean environments come real
Now it is bonded, it operates relatively complicated, it is necessary to special cleaning equipment and super-clean environment.And pass through high-temperature vacuum in this embodiment scheme
Stove carry out chip key and, it is possible to achieve slowly heating and insulating process, precise control of temperature and vacuum, without providing pressure
Power, can preferably protect nanochannel, ensure being bonded naturally for substrate and cover plate, realize the true of micro-void and nanochannel
The recovery of real sandstone micro model.
The technical solution of the embodiment of the present invention, hole present in the pore throat passage by actual sandstone and venturi carry out respectively
Etching, so that the hole and venturi for meeting true compact oil reservoir size are formed, meanwhile, etched hole is realized by high-temperature sintering process
Gap and the etching substrate of venturi and being bonded for cover plate, make etching substrate effective with cover plate and are closely combined as a whole, realize
It is more in line with the microcosmic rock network model of actual compact oil reservoir.
Example IV
Figure 11 is the flow chart for another microcosmic rock network model production method that the embodiment of the present invention four provides.With reference to
Figure 11, in production method provided in this embodiment, after S130, further includes S140, to the initial microcosmic rock network mould
Toluene solution of the type inlet injection containing 1% trichloromethyl silane (TCMS) is to water state is fettered, with to the initial microcosmic rock
Stone network model carries out wetting modification.
Wherein, specific steps further include：Miniature model 60min is fully rinsed with sodium hydroxide, is then cleaned with distilled water
Miniature model；With the microcosmic rock network model of salt water saturation；(TCMS) containing 1% trichloromethyl silane is injected at model inlet
Toluene solution to fettering water state；With toluene and the miniature model of alcohol flushing, then with the miniature model of distilled water flushing；Use
Baking oven dry microcosmic rock network model 60min at 100 DEG C.Microcosmic rock net is rinsed with the toluene solution of trichloromethyl silane
Pore throat passage in network model, the pore throat passage progress of the glass wet to strong water is partially modified, changes microcosmic rock network model
Property for constraint water state so that the mixing wetting model for forming water wet channel and oily wet channel and depositing, it is fine and close to be made more fitting
The microcosmic rock network model of the mixing wetting of oil reservoir hydrocarbon migration channel.
The technical solution of the embodiment of the present invention, completes the recovery of true compact oil reservoir pore throat passage, while overcomes existing
Have wetability control technology be limited only to model integrally soak it is modified be such as changed to the technical problem that pure water is wet or pure oil is wet, realize
The passage that the i.e. oily wet channel of the mixing wetting to be formed coexists with water wet channel coexists with the wet rock of water for the wet rock of oil in compact oil reservoir,
Microcosmic rock network model is realized the mixing wetting characteristics of true compact oil reservoir, make microcosmic rock network model special from structure
More meet truth in point and chemical characteristic, the research to true compact oil reservoir has benefits greatly very much.
Note that it above are only presently preferred embodiments of the present invention and institute's application technology principle.It will be appreciated by those skilled in the art that
The invention is not restricted to specific embodiment described here, can carry out for a person skilled in the art various obvious changes,
Readjust and substitute without departing from protection scope of the present invention.Therefore, although being carried out by above example to the present invention
It is described in further detail, but the present invention is not limited only to above example, without departing from the inventive concept, also
It can include other more equivalent embodiments, and the scope of the present invention is determined by scope of the appended claims.
Claims (10)
- A kind of 1. microcosmic rock network model production method, it is characterised in that including：Pore throat passage is extracted, the hole in pore throat passage and venturi are separated, obtains pattern of apertures and venturi pattern, respectively Make hole mask and venturi mask；Substrate is performed etching using the hole mask and venturi mask, forms etching substrate；The etching substrate is bonded with cover plate, forms microcosmic rock network model.
- 2. production method according to claim 1, it is characterised in that divide the hole in pore throat passage and venturi From obtaining pattern of apertures and venturi pattern includes：Binary conversion treatment is carried out to the image of rock section, distinguishes rock matrix pattern and pore throat channel pattern；Determine central axes all in pore throat channel pattern；Do circle using each pixel on central axes as the center of circle, the radius of the circle for its center of circle reach nearest rock matrix away from From；Radius being met to, the center of circle of the circle of preset condition is defined as node, corresponding pore throat channel pattern is hole at each node Pattern, the pore throat channel pattern of remainder is venturi pattern.
- 3. production method according to claim 1, it is characterised in that using the hole mask and venturi mask to substrate Perform etching, including：Hole etches, and the substrate is performed etching using the hole mask, and formation etches partially substrate；Mask alignment, according to corresponding first mark being carved with the hole mask and venturi mask, etches partially described Substrate is aligned with venturi mask；Venturi etches, and the substrate that etches partially is performed etching using the venturi mask, obtains the etching substrate；Model cleans, and the etching substrate is cleaned.
- 4. production method according to claim 3, it is characterised in that the method for the hole etching includes：Hole mask and substrate are stacked together and are exposed by exposure machine, so that the pattern of hole mask is transferred to substrate On；Clean the photoresist and exposed portion on the substrate；Under ultrasound bath environment, dip the substrate into the first etching liquid and perform etching 30min, formation etches partially substrate, institute It is the NH of 0.5mol/L using the HF of 1mol/L as etching agent to state the first etching liquid4F is complexing agent, the HNO of 0.5mol/L3For hydrotropy The mixing liquid of agent.
- 5. production method according to claim 3, it is characterised in that the line width of first mark is the pore throat passage First setting multiple of width.
- 6. production method according to claim 5, it is characterised in that be also carved with phase on the hole mask and venturi mask Corresponding second mark, in the predeterminable area of the described first mark, the line width of second mark is second mark Second setting multiple of the first mark line width, the length of the second mark is the described first the 3rd setting times for marking line width Number；Correspondingly, the mask alignment includes：According to corresponding first mark and the second mark being carved with the hole mask and venturi mask, etched partially described Substrate is aligned with venturi mask.
- 7. production method according to claim 3, it is characterised in that the venturi etching includes：By the venturi mask of alignment and substrate is etched partially by exposure machine progress re-expose, so that the pattern transfer of venturi mask To etching partially on substrate；The photoresist and exposed portion on substrate are etched partially described in cleaning；Under ultrasound bath environment, it will etch partially in substrate the second etching liquid of immersion and perform etching 30min, form etching base Piece, second etching liquid are the NH of 0.0075mol/L using the HF of 0.015mol/L as etching agent4F is complexing agent, The HNO of 0.0075mol/L3For the mixing liquid of cosolvent.
- 8. production method according to claim 1, it is characterised in that the etching substrate is bonded with cover plate, is wrapped Include：The etching substrate is pre-processed；Substrate and cover plate fitting will be etched, forms initial microcosmic rock network model；The initial microcosmic rock network model is bonded by high-temperature sintering process, forms microcosmic rock network model.
- 9. production method according to claim 8, it is characterised in that it is described by high-temperature sintering process to described initial microcosmic Rock network model is bonded, including：Initial microcosmic rock network model is put in vacuum high temperature furnace, vacuumize process is carried out to the vacuum high temperature furnace；High-temperature vacuum in-furnace temperature is risen to 50 DEG C by room temperature with the speed of 2 DEG C/min, constant temperature 30min after reaching 50 DEG C；High-temperature vacuum in-furnace temperature is risen to 120 DEG C with the speed of 2 DEG C/min, constant temperature 150min after reaching 120 DEG C；High-temperature vacuum in-furnace temperature is risen to 700 DEG C with the speed of 1.5 DEG C/min, constant temperature 120min after reaching 700 DEG C；Naturally cool to room temperature.
- 10. production method according to claim 1, it is characterised in that further include：The toluene solution containing 1% trichloromethyl silane (TCMS) is injected to beam to the initial microcosmic rock network model inlet Water state is tied up, to carry out wetting modification to the initial microcosmic rock network model.
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