WO2018039038A1 - Mesure d'angles de contact entre une paire solide-fluide au moyen d'une imagerie par rayons x de l'interface solide-fluide-fluide à l'intérieur d'un capillaire - Google Patents

Mesure d'angles de contact entre une paire solide-fluide au moyen d'une imagerie par rayons x de l'interface solide-fluide-fluide à l'intérieur d'un capillaire Download PDF

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WO2018039038A1
WO2018039038A1 PCT/US2017/047379 US2017047379W WO2018039038A1 WO 2018039038 A1 WO2018039038 A1 WO 2018039038A1 US 2017047379 W US2017047379 W US 2017047379W WO 2018039038 A1 WO2018039038 A1 WO 2018039038A1
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fluid
solid
interface
capillary
recited
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PCT/US2017/047379
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English (en)
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Meinhard Bayani R. CARDENAS
Philip C. BENNETT
Kuldeep CHAUDHARY
Eric J. GUILTINAN
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Board Of Regents, The University Of Texas System
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Publication of WO2018039038A1 publication Critical patent/WO2018039038A1/fr

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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
    • E21B47/00—Survey of boreholes or wells
    • E21B47/002—Survey of boreholes or wells by visual inspection
    • E21B47/0025—Survey of boreholes or wells by visual inspection generating an image of the borehole wall using down-hole measurements, e.g. acoustic or electric
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N13/02—Investigating surface tension of liquids
    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/24—Earth materials
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N13/02—Investigating surface tension of liquids
    • G01N2013/0208—Investigating surface tension of liquids by measuring contact angle
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material

Definitions

  • the present invention relates generally to measuring contact angles between minerals/materials and two fluids, and more particularly to measuring contact angles between a solid-fluid pair, such as at reservoir pressure-temperature conditions, using X-ray images of a specific solid-fluid-fluid configuration.
  • Measuring contact angles between minerals/materials and two fluids is important for characterizing, predicting and modeling multiphase flow in a solid-multi-fluid system, such as in geologic porous media, which includes petroleum reservoirs and aquifers.
  • a solid-multi-fluid system such as in geologic porous media, which includes petroleum reservoirs and aquifers.
  • high temperatures and high pressures may be present.
  • measurements of contact angles under ambient conditions are potentially not applicable to measurements of contact angles in such underground environments.
  • Subsurface multiphase fluid flow and transport is largely controlled by the wettability of the aquifer or reservoir matrix. Wettability is the measure of one fluid's affinity relative to another competing fluid to spread or contract on a solid surface.
  • Wettability is the measure of one fluid's affinity relative to another competing fluid to spread or contract on a solid surface.
  • An increasingly relevant example of multiphase flow phenomena is that which occurs during the injection and storage of C0 2 in deep brine-saturated geologic reservoirs which is seen as a viable strategy for curbing anthropogenic C0 2 emissions to the atmosphere.
  • the mechanisms for the permanent storage of C0 2 in subsurface brine reservoirs are: (a) structural or stratigraphic trapping, (b) residual or capillary trapping of CO?., (c) solubility trapping, and (d) mineral trapping.
  • Pc is the capillary pressure
  • ju is interfacial tension between fluid 1 and fluid 2
  • r is the cylinder radius
  • ⁇ ⁇ is the equilibrium contact angle, i.e., the measure of wettability.
  • the contact angle or the contact line of the two fluids' intersection with the solid surface is the macroscopic manifestation of the microscopic force balance between interfacial tension (or surface free energies) of the fluids and the solid (denoted by y) given by the Young equation:
  • Wettability is one of the most significant factors controlling all four mechanisms for C0 2 storage outlined above. For example, a ⁇ ⁇ >90° for seal or cap rocks will lead to negative capillar ⁇ ' pressure and could potentially result in ineffective structural or stratigraphic trapping, C0 2 -wet or C0 2 -mixed-wet media is known to critically limit the C0 2 capillary trapping potential. Furthermore, the efficiency of mechanisms (c) and (d) is dependent on the success of mechanisms (a) and (b).
  • the fluid volume injected controls the drop size, and a similar injected volume may result in different drop sizes depending on pressure-temperature (P-T) conditions.
  • P-T pressure-temperature
  • different contact lengths/drop sizes can lead to differences in measured 6 e .
  • Reproducibility of experimental results, i.e., recovering a drop with precisely the same volume and contact length, can be a challenge in the sessile drop method.
  • Wettability measurements can be fraught with uncertainty leading to a wide range of values and typically poor agreement between different studies.
  • the sessile drop method is subject to the effects of buoyancy and gravitational forces leading to inaccurate results.
  • improvement of existing approaches or perhaps new robust techniques for measuring contact angles between minerals/materials and two fluids are welcome particularly for high P-T conditions representative of reservoirs.
  • a method for measuring contact angles comprises forming a column out of a mineral or a rock.
  • the method further comprises placing a core holder with a drilled capillary or a slot vertically inside the column.
  • the method additionally comprises injecting a first fluid within the capillary or the slot.
  • the method comprises injecting a second fluid within the capillary or the slot.
  • the method comprises performing an X-ray scan of a solid-fluid-fluid interface in the capillary or the slot to generate image data, where the solid-fluid-fluid-interface corresponds to an interface of a material of the core holder, the first fluid and the second fluid.
  • the method comprises calculating a contact angle at the solid-fluid-fluid interface using the generated image data.
  • Figure 1 illustrates a system for measuring the contact angles between minerals/materials and two fluids, such as at reservoir pressure-temperature conditions, in accordance with an embodiment of the present invention
  • Figure 2 is a flowchart of a method for measuring the contact angle defined by the solid- fluid pair interface using the system of Figure 1 in accordance with an embodiment of the present invention
  • Figure 3A is a diagrammatic sketch of the setup for imaging the solid-fluid-fluid interface inside a column in accordance with an embodiment of the present invention
  • Figure 3B is an image of a quartz core holder with a capillary in accordance with an embodiment of the present invention.
  • Figure 3C is an X-ray computed tomography (CT) image showing the magnified view of a quartz -brine-C0 2 interface inside the quartz capillary in accordance with an embodiment of the present invention
  • Figure 3D is an image illustrating the definition and calculation of the contact angle, ⁇ ⁇ , in accordance with an embodiment of the present invention.
  • Figures 4A-4E are X-ray images of fluid-fluid- sol id interfaces at room conditions (25°C and 0.1 MPa) for quartz-air-brine, borosilicate glass-air-brine, shale-air-brine, PTFE-air- deionized (DI) water and PTFE-air-brine, respectively, in accordance with an embodiment of the present invention.
  • Figures 5A-5F are X-ray images of solid-fluid-fluid interfaces at reservoir conditions (60-71° C and 12.4-22.8 MPa) for quartz-C0 2 -brine, muscovite plates-C0 2 -brine, borosilicate glass-C0 2 -brine, shale-C0 2 -brine, PTFE-C0 2 -brine and PEEK-C0 2 -brine, respectively.
  • the principles of the present invention provide a means for measuring contact angles between minerals/materials and two fluids, such as at reservoir pressure-temperature conditions, using X-ray images of a specific solid-fluid-fluid configuration.
  • the present invention ensures that capillary forces, whose balance controls the contact angle, dominate which makes the measurements using the present invention more accurate.
  • the present invention is particularly suitable for situations where one fluid is "supercritical" (low density and high viscosity).
  • Figure 1 illustrates a system 100 for measuring the contact angles between minerals/materials and two fluids, such as at reservoir pressure- temperature conditions, in accordance with an embodiment of the present invention.
  • System 100 includes an X-ray imaging system 101, such as a three-dimensional X-ray imaging system (e.g., computed tomography scanner, such as Xradia® MicroXCT-400 scanner) whose image data is sent to a computing system 102.
  • X-ray imaging system 101 such as a three-dimensional X-ray imaging system (e.g., computed tomography scanner, such as Xradia® MicroXCT-400 scanner) whose image data is sent to a computing system 102.
  • X-ray imaging system 101 such as a three-dimensional X-ray imaging system (e.g., computed tomography scanner, such as Xradia® MicroXCT-400 scanner) whose image data is sent to a computing system 102.
  • X-ray imaging system 101 such as a three-dimensional X-ray imaging system (e.g., computed tomography scanner, such as Xradia® MicroXCT-400 scanner) whose image data is sent to a computing system 102
  • Computing system 102 may be any type of computing device (e.g., portable computing unit, Personal Digital Assistant (PDA), smartphone, laptop computer, mobile phone, navigation device, game console, desktop computer system, workstation, Internet appliance and the like) configured with the capability of computing the contact angle of a specific solid-fluid-fluid configuration using the X-ray image data provided by X-ray imaging system 101.
  • PDA Personal Digital Assistant
  • Figure 1 further illustrates forming a column 103 out of a mineral or rock 104, where a core holder 105 with a drilled capillary 106 is inserted within column 103. A discussion regarding such aspects is provided further below.
  • Figure 1 additionally illustrates the injection of a first fluid 107 and a second fluid 108 in capillary 106, where an X-ray scan of the solid-fluid-fluid interface (105/107/108), where the "solid” refers to the material of core holder 105, is performed to generate an image (image data), which is sent to computing system 102 to calculate the contact angle defined by the solid-fluid pair interface as discussed further below.
  • Figure 2 is a flowchart of a method 200 for measuring the contact angle defined by the solid-fluid pair interface using system 100 of Figure 1 in accordance with an embodiment of the present invention.
  • FIG. 3 A is a diagrammatic sketch of the setup for imaging the solid-fluid-fluid interface inside column 103 in accordance with an embodiment of the present invention.
  • a core holder 105 e.g., quartz core holder
  • a drilled capillary 106 e.g., 1 to 1.5 mm inner diameter (ID)
  • ID inner diameter
  • Figure 3B is an image of a quartz core holder 105 with capillary 106 in accordance with an embodiment of the present invention.
  • core holder 105 is pervious to X- rays.
  • the material of core holder 105 consists of polyether ether ketone (PEEK), which is capable of handling potentially corrosive fluids, such as supercritical C0 2 .
  • the material of core holder 105 consists of one of the following: quartz, muscovite, shale, silica glass, borosilicate glass or polytetrafluoroethylene (PTFE).
  • capillary 106 is produced either entirely hollow or with one end plugged or solid, such that the capillary force that the fluids are subject to are dominant over gravitational or buoyancy forces, i.e., the Eotvos number or Bond number is small (e.g., ⁇ 1).
  • the Eotvos number or Bond number is small (e.g., ⁇ 1).
  • two parallel planar surfaces can be used with a small slot between the planar surfaces so that the Bond number is ⁇ 1.
  • the precision spacing of the slot or the capillary diameter allows for controlling the Bond number.
  • the Bond number ⁇ 1 the influence of body forces (e.g., buoyancy and gravity) is removed thereby allowing for more accurate contact angle measurements.
  • a first fluid 107 e.g., brine, deionized water, sodium chloride brine
  • a first fluid 107 e.g., brine, deionized water, sodium chloride brine
  • a second fluid 108 (e.g., air, carbon dioxide) is injected within capillary 106 or the slot at a desired pressure to pressurize the system in core holder 105 so as to be able to withstand high pressure and temperature as shown in Figure 3C.
  • Figure 3C is an X-ray computed tomography (CT) image showing the magnified view of a quartz-brine-air interface (105/107/108) inside the quartz capillary 106 in accordance with an embodiment of the present invention.
  • first fluid 107 corresponds to brine
  • second fluid 108 corresponds to air.
  • the "solid" corresponds to quartz, which is the material of core holder 105.
  • step 205 core holder 105 is heated at a desired temperature, such as by using a heating sleeve with precise temperature control.
  • step 206 an X-ray scan of the solid-fluid-fluid interface (105/107/108) in capillary 106 or the slot is performed by X-ray imaging system 101 to generate an image (image data).
  • step 207 the image data is sent to computing system 102 by X-ray imaging system 101.
  • step 208 surfaces on the image (e.g., surfaces of an image of the solid-fluid-fluid interface (105/107/108)) are selected by a user of a computing system 101.
  • surfaces on the image e.g., surfaces of an image of the solid-fluid-fluid interface (105/107/108)
  • step 209 computing system 102 calculates the contact angle between the selected surfaces. That is, computing system 102 calculates the contact angle at the solid-fluid-fluid interface (105/107/108) using the generated image data.
  • An image illustrating the definition and calculation of the contact angle 301, 6 e is shown in Figure 3D in accordance with an embodiment of the present invention.
  • X-ray computed tomography CT
  • radiography is much faster, as imagery can be obtained in seconds, but at a cost in clarity, as the interface is viewed through intervening material.
  • Computed tomography provides clearer data, but may require several minutes to a few hours of imaging. Radiography requires that the interface be exactly orthogonal to the source- detector path to allow accurate measurement.
  • the fluid-fluid-solid interface (108/107/105) is expected to have axial symmetry, and a radiograph may be sufficient for accurate contact angle measurements.
  • X-ray CT scanning may be required.
  • the energy and power of the X- ray source along with the concentration of the contrasting agent in brine were optimized to obtain images with unique isolation of grayscale peaks for the various materials including silica glass, borosilicate glass, PEEK, polytetrafluoroethylene (PTFE), quartz, muscovite, C0 2 , air, water, and brine.
  • Radiography was conducted typically at 1-2 ⁇ resolution and X-ray CT scanning at ⁇ 10 ⁇ resolution.
  • the window is placed a few column pixels away from the fluid-fluid-solid interface (107/108/105) since the denoising partly blurs this zone.
  • each column within the window can be scanned for the greatest pixel value change across some interval, usually 10 pixels (the average value of 5 pixels compared to the next 5 pixels). The length of this interval depends upon the resolution of the image, where "noisy" images may require larger intervals.
  • a point is placed in the middle of the relatively narrow interval to mark the fluid- fluid interface (107/108). In this manner, a point along the interface is found for each column within the search window.
  • the fluid interface When the surface tension forces are dominant, i.e., the Bond number Bo ⁇ ⁇ , the fluid interface successfully minimizes energy and takes the form of a spherical cap in three dimensions or an arc of a circle in two dimensions.
  • a circle is fit to the selected points using the MATLAB® function circfit.
  • the intersection of the wall of capillary 106 and the circle is then calculated and a tangent line to the circle at this point is plotted. Finally, the angle formed by the tangent line and the wall defines f) e .
  • This approach which is illustrated in Figures 4A-4E, thus takes into account the shape of the entire interface which is also a check for the robustness of the experimental design, i.e., if the Bo condition is met.
  • Figures 4A-4E are X- ray images of fluid-fluid-solid interfaces at room conditions (25°C and 0.1 MPa) for quartz-air- brine, borosilicate glass-air-brine, shale-air-brine, PTFE-air-deionized (DI) water and PTFE-air- brine, respectively, in accordance with an embodiment of the present invention.
  • a cylindrical core (6 mm x 20 mm) was obtained by mechanically drilling in the direction perpendicular to the c axis of a quartz crystal.
  • a high-precision diamond-bit drill press was later used to form a capillary 106 ( ⁇ 1 mm) in the quartz 105 or shale core as shown in Figure 3B.
  • the high-precision drill press created a smooth- surface capillary at the ⁇ -scale that was cleaned by an air pump.
  • Monoclinic muscovite crystals have a well -developed platy cleavage along the [001] plane and posed a challenge to obtain a core or drill capillary 106.
  • two rectangular muscovite flakes (7 mm x 20 mm) cleaved parallel to the [001] plane were obtained and arranged them to be parallel with each other with ⁇ 1 mm spacer along their long edges, i.e., a narrow slot form.
  • the cleaved muscovite flakes were smooth and the flat surfaces had a vitreous luster.
  • the slot between the parallel plates was used the same way as capillary 106 in core holder 105.
  • Other laboratory materials, i.e., PTFE, PEEK, and glass were available in a capillary form ( ⁇ 1 mm ID) and used for experiments similar to the description above.
  • the column used to house the capillaries is made of PEEK, a material that is pervious to X-rays and can withstand pressures of up to 27.6 MPa.
  • the exterior of the column consists of a carbon fiber heating sleeve powered by a DC voltage modulator, which helps optimize the voltage to maintain a constant temperature of 60°C ⁇ 2°C in the column.
  • Brine is injected from the bottom of the column using a manual syringe and C0 2 is injected from the top of the column using a supercritical C0 2 pump until a constant pressure of 13.8 ⁇ 0.1 MPa is attained.
  • the column is then set aside for about 4 hours for C0 2 dissolution equilibration in the brine.
  • the brine volume injected was on the order of 2 mL and was optimized to position the interface of fluids in capillaries or the slit of muscovite flakes.
  • Figures 5A- 5F are X-ray images of solid-fluid-fluid interfaces at reservoir conditions (60-71° C and 12.4- 22.8 MPa) for quartz-C0 2 -brine, muscovite plates-C0 2 -brine, borosilicate glass-CC -brine, shale-C0 2 -brine, PTFE-C0 2 -brine and PEEK-CC -brine, respectively.
  • the high-precision drill press created a smooth surface and thus a smooth capillary, showing that this method can be readily adopted for most minerals in geologic porous media.
  • Figures 4A-4E also display the difference between imaging modes.
  • Figure 4B is a radiograph image
  • Figure 4A is a vertical reslicing through a CT volume.
  • the radiograph is a proj ection through the entire experimental setup, and thus incorporates spurious material leading to a noisier image, while the CT reslice image isolates the region of interest.
  • the borosilicate-air-brine system at ambient room condition is brine or water-wetting with a convex liquid interface and a G e of 9° ( Figure 4B).
  • borosilicate-CC ⁇ -brine system at 13.8 MPa and 60° C shows decreased brine or water-wetting characteristics, yet with a convex fluid interface and a Q e of 54° ( Figure 5C).
  • the PTFE-C0 2 -brine system is C0 2 wetting, with a concave brine interface and a G e of 140° ( Figure 5E).
  • the PEEK-C0 2 -brine system is also CO 2 wetting, with a concave brine interface and a G e of 127° (Figure 5F).
  • Figure 5F The examples above demonstrate the utility of the method of the present invention for quantifying wettability of minerals and materials that can be configured in a capillary form or parallel planes.
  • the method of the present invention is fast to setup, uses little fluid volume, and can provide rapid measurements for changing thermodynamics conditions. For example, X-ray imaging can be done with stepwise change in P-T conditions of the column.
  • Another advantage of the method of the present invention is the fixed spacing between fluid and solid surfaces which allows a constant external or body force on the interface of fluids.
  • the method of the present invention can be adapted for advancing and receding contact angle measurements. X-ray radiographs can be obtained at a frequency of 1 image per 2 seconds, thus allowing transient scanning of the advancing or receding interface. Furthermore, because the column setup consists of PEEK, the method of the present invention can also be applied to contact angle measurement of corrosive fluids with low pH and various salinities. Such a column can also be left saturated with such fluids for aging purposes.
  • the present invention measures wettability of reservoir and seal/cap rock minerals and laboratory materials at elevated P-T conditions.
  • the present invention is based on constructing reservoir material (rocks or minerals) into a capillary (1 mm ID) or slot form (1-1.5 mm ID) and placing this vertically inside a high P-T column. Two fluids are then injected such that their interface is within the solid's interspace.
  • the solid-fluid-fluid interfaces are imaged by X-ray radiography and/or CT scanning, and the images are later processed for the contact angle measurement.
  • the wettability of reservoir rocks and minerals is conventionally measured using the sessile drop method, in which recovering the same volume for the drop with the same contact length can be a challenge.
  • the spacing for the fluid-solid interface remains constant and can be easily optimized for precluding gravitational effects, i.e., precise control of the Bond number.

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Abstract

La présente invention concerne un procédé de mesure d'angles de contact entre une paire solide-fluide, par exemple dans des conditions de pression-température de réservoir, au moyen d'images à rayons X d'une configuration solide-fluide-fluide spécifique. Une colonne est formée à partir d'un minéral ou d'une roche. Un support de carotte avec un capillaire percé ou une fente est placé verticalement à l'intérieur de la colonne. Un premier et un deuxième fluide sont ensuite injectés à l'intérieur du capillaire ou de la fente. Un balayage à rayons X d'une interface solide-fluide-fluide dans le capillaire ou la fente est effectué pour générer des données d'image, l'interface solide-fluide-fluide correspondant à une interface d'un matériau du support de carotte, du premier fluide et du deuxième fluide. Un angle de contact au niveau de l'interface solide-fluide-fluide est ensuite calculé au moyen des données d'image générées. En conséquence, des angles de contact définis par une interface de paire solide-fluide dans des conditions typiques d'environnements géologique profonds peuvent être mesurés de façon rapide et économique.
PCT/US2017/047379 2016-08-26 2017-08-17 Mesure d'angles de contact entre une paire solide-fluide au moyen d'une imagerie par rayons x de l'interface solide-fluide-fluide à l'intérieur d'un capillaire WO2018039038A1 (fr)

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CN114414437A (zh) * 2022-01-18 2022-04-29 中国石油大学(北京) 界面张力和接触角的测量装置
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