CN113484348A - Method for representing water absorption expansibility of shale microstructure by using small-angle neutron scattering experiment - Google Patents
Method for representing water absorption expansibility of shale microstructure by using small-angle neutron scattering experiment Download PDFInfo
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Abstract
The invention provides a method for representing water absorption expansibility of a shale microstructure by using a small-angle neutron scattering experiment, which is used for performing the small-angle neutron scattering experiment on a shale particle sample to be detected to obtain original data; preparing a fluid with a scattering length density of zero, and fully soaking the shale particle sample to be detected in the fluid; performing a small-angle neutron scattering experiment on the fully-infiltrated shale particle sample to be detected to obtain original data; calculating the processed data through an Irena macro plug-in IGOR Pro software to obtain the pore structure information of the shale particle sample to be detected before and after infiltration; and obtaining the water absorption expansibility of the shale in a microscopic state by comparing the pore structure information of the shale particle sample to be detected before and after infiltration. The technical scheme provided by the invention has the beneficial effects that: the method provides a brand-new experimental technology for representing the micro-expansibility of the shale, enriches the theory of understanding the micro-expansibility of the shale by the action of the water and rock, and has the advantages of no damage, high efficiency, short time consumption and the like in small-angle neutron scattering.
Description
Technical Field
The invention relates to the technical field of unconventional natural gas experiments, in particular to a method for representing water absorption expansibility of a shale microstructure by using a small-angle neutron scattering experiment.
Background
The influence of the water-rock action on the microstructure of the shale exists many problems to be solved, for example, the exploitation of shale gas requires injecting a large amount of pressure fluid containing proppant under high pressure to generate cracks. Taking the example of U.S. shale gas recovery, on average only 6% to 10% of the fracturing fluid is flowback, and the unremoved fracturing fluid is believed to be retained in the shale matrix, fractures, and other types of pore spaces by various mechanisms. However, the retention mechanism, distribution and water-rock interaction of a large amount of fracturing fluid in the pore space of the shale reservoir are not clear. The water rock effect is an important cause of stress sensitivity damage of shale reservoirs and is one of the influencing factors causing the shale expansion cracking to cause borehole wall instability. Therefore, the research on the shale water-rock action on the microscopic scale is particularly important.
Disclosure of Invention
In view of the above, to solve the above problems, embodiments of the present invention provide a method for characterizing water-absorption expansibility of a shale microstructure by using a small-angle neutron scattering experiment.
The embodiment of the invention provides a method for representing water absorption expansibility of a shale microstructure by using a small-angle neutron scattering experiment, which comprises the following steps of:
s1, preparing a shale particle sample to be detected;
s2, carrying out a small-angle neutron scattering experiment on the shale particle sample to be detected to obtain original data;
s3, preparing a fluid with a scattering length density of zero, and sufficiently soaking the shale particle sample to be detected in the fluid to fill the pores of the shale particle sample to be detected with the fluid;
s4, performing a small-angle neutron scattering experiment on the shale particle sample to be detected which is fully soaked in the step S3 to obtain original data;
s5 pre-processes the raw data in steps S2 and S4;
s6, calculating the processed data through an Irena macro plug in IGOR Pro software, so as to obtain the pore structure information of the shale particle sample to be detected before and after infiltration;
s7, comparing the pore structure information of the shale particle sample to be tested before and after infiltration to obtain the water-absorbing expansibility of the shale in a microscopic state.
Further, in step S3, the fluid and the shale particle sample to be tested are loaded into a quartz sample cell, and the shale particle sample to be tested is sufficiently soaked in the fluid.
Further, the inner diameter of the quartz sample cell is 1 mm.
Further, step S5 is specifically to import the original data in step S2 and step S4 into an IRENA plugin based on IGOR, perform one-dimensional processing on the two-dimensional scattering image obtained by the small-angle neutron scattering experiment by using Guinier and Porod fitting to obtain a one-dimensional scattering intensity curve, and perform background subtraction and normalization processing on the one-dimensional scattering intensity curve.
Further, a fluid with a scattering length density of zero was loaded into a quartz sample cell as a background for background subtraction treatment.
Further, in step S7, the pore structure information includes porosity, pore size distribution, and pore volume.
Further, in step S3, the fluid is prepared by mixing water and heavy water.
Further, step S1 is to select a shale sample to be tested, grind the shale sample into shale particles by a grinder, and dry the shale particles.
Further, the particle size of the shale particles is 177-500 mu m.
Further, the temperature for sample drying was 60 ℃ and drying was carried out until the mass did not change any more.
The technical scheme provided by the embodiment of the invention has the following beneficial effects: the fluid with the scattering length density of zero is injected into the pores of the shale sample, the pore space of the shale sample can expand after encountering water, the fluid with the scattering length density same as that of the pore space can not bring extra scattering signals, the expansion of the shale microstructure in contact with fracturing fluid can be researched on a nanoscale, the pore size distribution of the shale sample before and after absorbing water is represented by comparing and matching small-angle neutron scattering experiments, and the expansion of the shale under the microscale can be quantitatively represented by comparing the difference of the pore size distribution of the shale sample and the pore size distribution of the shale sample. The small-angle neutron scattering experiment does not damage the shale sample, so the experiment has repeatability.
The invention provides a brand-new experimental technology for representing the micro-expansibility of shale based on a small-angle neutron scattering experiment, enriches the theory of understanding the micro-expansibility of shale by the action of water and rock, and has the advantages of no damage, high efficiency, short time consumption and the like.
Drawings
FIG. 1 is a schematic flow chart diagram illustrating an embodiment of a method for characterizing water swelling capacity of a shale microstructure by a small-angle neutron scattering experiment according to the present invention;
FIG. 2 is a schematic representation of pores in a shale sample before and after water absorption;
FIG. 3 is a graph showing pore size distribution and pore volume distribution before and after the swelling and water absorption of the Longmaxi group shale;
FIG. 4 is a graph showing pore size distribution and pore volume distribution before and after swelling and water absorption of illite mineral.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
As shown in fig. 1, an embodiment of the present invention provides a method for characterizing water swelling capacity of a shale microstructure by using a small-angle neutron scattering experiment, including the following steps:
s1, preparing a shale particle sample to be detected, wherein the specific operation steps comprise selecting the shale sample to be detected, grinding the shale sample into shale particles by a grinder, and drying the shale particles.
It should be noted that the obtained shale particles are obtained from the same core pillar at a similar position, so as to eliminate the influence of the heterogeneity of the shale. Specifically, the shale particles have the particle size of 177-500 microns and are dried in an oven at the drying temperature of 60 ℃ until the mass of the shale particles is not changed any more, so that free water and bound water in a shale sample are removed, and the accuracy of an experiment is improved.
S2, carrying out a small-angle neutron scattering experiment on the shale particle sample to be detected, and acquiring original data. In this example, the small-angle neutron scattering experiments were performed using a Quokka small-angle scattering spectrometer in the Australian institute of Nuclear science and technology (ANSTO) laboratory. Before a small-angle neutron scattering experiment is carried out, workers need to complete detector efficiency correction, wavelength correction, background correction, transmittance measurement and other works, and the thickness and the test time of a sample and the wavelength of an adopted neutron beam current need to be recorded in the sample test process for subsequent data processing work.
In the experiment, the granular shale sample is selected to obtain the pore structure information of average orientation, so that the small-angle neutron scattering experiment after water absorption can be conveniently carried out. The particles are screened to 177-500 mu m, a quartz sample cell with the inner diameter of 1mm is used for loading, the particle sample is molded under pressure, and the particle sample is compacted as much as possible to carry out a small-angle neutron scattering experiment. The neutron wavelength adopted in the experiment is
By varying the location of the detector signal reception, a range of scatter vectors (q) can be covered
For polydisperse porous media, the relationship between pore radius (r) and scattering vector (q) is r ≈ 2.5/q, and experimentally detectable sample pore diameters ranging from 1 to 128nm can be calculated.
S3, preparing a fluid with a scattering length density of zero, and sufficiently soaking the shale particle sample to be detected in the fluid so as to fill the pores of the shale particle sample to be detected with the fluid. In the present embodiment, the fluid is water (H)2O) and heavy water (D)2O) and the SLD value of water (-0.56X 10)10cm-2) And SLD value of heavy Water (+ 6.39X 10)10cm-2) With the difference and the same fluid chemistry, a mixture of water and heavy water injected into the shale pores can obtain scatterers with average contrast close to zero. In other embodiments, deuteration may also be usedThe fluid produces a solution with a scattering length density of zero. Specifically, the fluid and the shale particle sample to be detected are filled into a quartz sample cell, and the shale particle sample to be detected is fully soaked in the fluid for at least 24 hours.
S4, performing a small-angle neutron scattering experiment on the shale particle sample to be detected which is fully soaked in the step S3, repeating the step S2, and obtaining original data.
S5 preprocessing the original data in the step S2 and the step S4, wherein the original data are two-dimensional scattering images of scattering vectors and scattering intensity, specifically, the original data in the step S2 and the step S4 are led into an IRENA plug-in based on IGOR, Guinier and Porod fitting is utilized, one-dimensional processing is carried out on the two-dimensional scattering images obtained by the small-angle neutron scattering experiment to obtain a one-dimensional scattering intensity curve, and background subtraction and normalization processing are carried out on the one-dimensional scattering intensity curve. A fluid with a scattering length density of zero was loaded into a quartz sample cell as background for background subtraction treatment.
S6, calculating the processed data through an Irena macro plug-in IGOR Pro software, thereby obtaining the pore structure information of the shale particle sample to be detected before and after infiltration, wherein the pore structure information comprises porosity, pore size distribution, pore volume and the like.
In the embodiment, two different types of samples of rock shale and illite minerals of the Longmaxi group are respectively selected for comparison experiments, the size of a particle sample of each experiment is 177-500 mu m, and drying treatment is carried out in a vacuum oven at the temperature of 60 ℃ for more than 48 hours until the mass is not changed any more. And performing a small-angle neutron scattering experiment on the shale sample and the illite mineral sample, preparing mixed fluid with zero SLD (saturated gradient D) by using water and heavy water, and fully infiltrating the mixed fluid with the shale sample and the illite mineral in quartz sample pools with neutron transmission lengths of 1mm respectively, wherein the infiltration time is 24 h. And performing a small-angle neutron scattering experiment on the shale sample and the illite sample containing the mixed fluid to obtain original data, and preprocessing the original data. And calculating the processed data through an Irena macro plug in IGOR Pro software to obtain the pore structure information of the shale sample/illite sample before and after infiltration, and comparing the pore structure information of the shale sample/illite sample before and after infiltration to obtain the water swelling property of the shale sample/illite sample in a microscopic state.
The experimental results are as follows:
as shown in fig. 2a-2c, the pores 2 in the shale matrix 1, after being filled with the fluid 3, have a swelling phenomenon of the pores 2, and 4 in fig. 2c is the increased pore space after the shale swells by absorbing water. As shown in fig. 3 and 4, fig. 3 is the experimental results before and after water absorption of the rock shale of the ramstream group, fig. 4 is the experimental results before and after water absorption of the illite mineral, the gray curve represents the pore size distribution curve before water absorption, and the black color represents the pore size distribution curve after water absorption expansion. For the shale sample, the porosity of the shale before water absorption was 2.99%, and the porosity after water absorption expansion was 5.21%, which changed by 74.25% due to water absorption expansion. It can be observed that the water swelling of the shale mainly occurs in
The aperture section of (a). For the illite mineral sample, the porosity of the illite prior to water absorption was 2.68%, the porosity after water absorption swelling was 5.62%, and the porosity changed 109.70% due to water absorption swelling. Unlike shale samples, illite minerals are in the full pore size section
The swelling phenomenon occurs.
The basic principle of the small-angle neutron scattering technology is as follows: the difference in scattering length density between the pore space and the shale matrix will result in the generation of a scattering signal, so the spatial distribution of pores in the shale matrix can be deduced by interpreting the scattering pattern. Many important parameters, such as porosity, pore size distribution, fractal dimension, etc., can be obtained by small-angle neutron scattering techniques. Besides the application in the characterization of the shale pore structure, the contrast matching small-angle neutron scattering technology has good application prospect in the research of the water-rock action.
According to the technical scheme provided by the invention, a fluid with the scattering length density of zero is injected into the pores of the shale sample, the pore space of the shale sample can expand after the shale sample meets water (figure 1), the fluid with the scattering length density same as that of the pore space can not bring extra scattering signals, the expansion of the shale microstructure and the fracturing fluid when the shale microstructure contacts can be researched on a nanometer scale, the pore size distribution of the shale sample before and after water absorption can be represented by comparing and matching a small-angle neutron scattering experiment, and the expansion of the shale under the micro scale can be quantitatively represented by comparing the difference of the pore size distribution of the shale sample and the pore size distribution of the shale sample. The small-angle neutron scattering experiment does not damage the shale sample, so the experiment has repeatability.
The invention provides a brand-new experimental technology for representing the micro-expansibility of shale based on a small-angle neutron scattering experiment, enriches the theory of understanding the micro-expansibility of shale by the action of water and rock, and has the advantages of no damage, high efficiency, short time consumption and the like.
In this document, the terms front, back, upper and lower are used to define the components in the drawings and the positions of the components relative to each other, and are used for clarity and convenience of the technical solution. It is to be understood that the use of the directional terms should not be taken to limit the scope of the claims.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A method for representing water-absorbing expansibility of a shale microstructure by using a small-angle neutron scattering experiment is characterized by comprising the following steps of:
s1, preparing a shale particle sample to be detected;
s2, carrying out a small-angle neutron scattering experiment on the shale particle sample to be detected to obtain original data;
s3, preparing a fluid with a scattering length density of zero, and sufficiently soaking the shale particle sample to be detected in the fluid to fill the pores of the shale particle sample to be detected with the fluid;
s4, performing a small-angle neutron scattering experiment on the shale particle sample to be detected which is fully soaked in the step S3 to obtain original data;
s5 pre-processes the raw data in steps S2 and S4;
s6, calculating the processed data through an Irena macro plug in IGOR Pro software, so as to obtain the pore structure information of the shale particle sample to be detected before and after infiltration;
s7, comparing the pore structure information of the shale particle sample to be tested before and after infiltration to obtain the water-absorbing expansibility of the shale in a microscopic state.
2. The method for characterizing the water-swelling property of the shale microstructure through the small-angle neutron scattering experiment according to claim 1, wherein in step S3, the fluid and the shale particle sample to be tested are loaded into a quartz sample cell, and the shale particle sample to be tested is sufficiently soaked in the fluid.
3. The method for characterizing the water-swelling capacity of a shale microstructure using small-angle neutron scattering experiments according to claim 2, wherein the quartz sample cell has an inner diameter of 1 mm.
4. The method for characterizing water-swelling capacity of a shale microstructure through a small-angle neutron scattering experiment according to claim 2, wherein step S5 is specifically that the original data in step S2 and step S4 are imported into an IRENA plug-in based on IGOR, Guinier and Porod fitting is utilized, a one-dimensional scattering intensity curve is obtained by performing one-dimensional processing on a two-dimensional scattering image obtained through the small-angle neutron scattering experiment, and background subtraction and normalization processing are performed on the one-dimensional scattering intensity curve.
5. The method for characterizing the water-swelling property of the shale microstructure by using the small-angle neutron scattering experiment as claimed in claim 4, wherein the fluid with the scattering length density of zero is filled in a quartz sample cell as a background for background subtraction treatment.
6. The method for characterizing the water-swellable property of the shale microstructure by using a small-angle neutron scattering experiment of claim 1, wherein in the step S7, the pore structure information comprises porosity, pore size distribution and pore volume.
7. The method for characterizing the water-swelling capacity of a shale microstructure using small-angle neutron scattering experiments according to claim 1, wherein the fluid is prepared by mixing water and heavy water in step S3.
8. The method for characterizing the water-swelling property of the microstructure of shale according to claim 1, wherein step S1 specifically comprises selecting a shale sample to be tested, grinding the shale sample into shale particles with a grinder, and drying the shale particles.
9. The method for characterizing the water-swelling property of the microstructure of shale according to claim 8, wherein the shale particles have a particle size of 177-500 μm.
10. The method for characterizing the water-swelling capacity of a shale microstructure by using a small-angle neutron scattering experiment of claim 1, wherein the sample is dried at a temperature of 60 ℃ until the mass does not change any more.
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