CN112179770A - Shale uniaxial compressive strength evaluation method based on rock debris micro-nano indentation experiment - Google Patents
Shale uniaxial compressive strength evaluation method based on rock debris micro-nano indentation experiment Download PDFInfo
- Publication number
- CN112179770A CN112179770A CN202011046164.XA CN202011046164A CN112179770A CN 112179770 A CN112179770 A CN 112179770A CN 202011046164 A CN202011046164 A CN 202011046164A CN 112179770 A CN112179770 A CN 112179770A
- Authority
- CN
- China
- Prior art keywords
- shale
- rock debris
- loading
- compressive strength
- load
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/40—Investigating hardness or rebound hardness
- G01N3/42—Investigating hardness or rebound hardness by performing impressions under a steady load by indentors, e.g. sphere, pyramid
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
- G01N2001/366—Moulds; Demoulding
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0014—Type of force applied
- G01N2203/0016—Tensile or compressive
- G01N2203/0019—Compressive
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0076—Hardness, compressibility or resistance to crushing
- G01N2203/0078—Hardness, compressibility or resistance to crushing using indentation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/025—Geometry of the test
- G01N2203/0252—Monoaxial, i.e. the forces being applied along a single axis of the specimen
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
Abstract
The invention discloses a shale uniaxial compressive strength evaluation method based on a rock debris micro-nano indentation experiment, which comprises the following steps of: collecting rock debris of a target shale reservoir, and treating the surface of a rock debris sample by using a three-ion beam cutting instrument to change the surface into a flat and smooth high-quality section; carrying out a rock debris micro or nano indentation experiment on the treated rock debris sample to obtain a plurality of groups of indentation experiment load-displacement curve graphs; and calculating the uniaxial shale compressive strength of the shale reservoir. According to the method, a shale debris micro-nano indentation experiment is carried out, indentation load-depth curves under different scales are obtained, the micro-mechanical parameters of shale are obtained through calculation, a relation model between uniaxial compressive strength and the micro-mechanical parameters is established, the macro-mechanical parameter prediction of shale is realized, and therefore the shale mechanical parameters of a shale horizontal well are accurately obtained; the method provides a basic parameter basis for drilling, well completion and hydraulic fracturing of the shale gas horizontal well, and can effectively guide the drilling, well completion and hydraulic fracturing design and construction of the shale gas horizontal well.
Description
Technical Field
The invention relates to a shale uniaxial compressive strength evaluation method based on a rock debris micro-nano indentation experiment, and belongs to the technical field of petroleum exploration and development.
Background
In recent years, the capacity of clean energy in China is continuously expanded, an energy system with clean and low carbon is being rapidly constructed, natural gas is used as the cleanest energy in the traditional petrochemical energy, the demand is continuously increased, and shale gas becomes the core growth point of the natural gas industry in China. In the shale gas exploration and development process, mechanical properties such as uniaxial compressive strength of shale are key factors influencing safe, efficient and economic exploitation of shale oil gas. The mechanical characteristics and the distribution rule of the shale are required to be mastered in the whole exploration and development process: in the drilling process, the mechanical properties of shale strength and the like are closely related to engineering problems of borehole instability, low mechanical drilling speed and the like, and the strength and the like are accurately mastered, so that the drilling method is helpful for preventing underground complexity and accidents and improving the drilling efficiency; in the exploitation process, the mechanical characteristics such as shale strength have obvious influence on well completion segmentation, compressibility evaluation, fracturing design and evaluation, proppant selection and the like, the shale strength mechanical parameters are accurately mastered, the well completion and fracturing scheme is favorably optimized, the fracturing yield-increasing transformation effect is improved, and the shale oil and gas recovery ratio is further improved. Therefore, the shale oil-gas exploration and development overall process has very important functions and statuses on mechanical parameters such as shale strength and the like.
The shale uniaxial compressive strength can be obtained by a plurality of methods, and the methods mainly adopted by the petroleum industry comprise indoor experiments and logging methods:
(1) the indoor experiment mainly adopts single-axis, three-axis and other experimental means; but the indoor experiment has strict requirements on the sample size, the rock mechanical characteristics also have obvious size effect, and due to strong brittleness, bedding and fracture development of the shale, the standard rock sample is difficult to prepare, and the preparation success rate is low; in addition, most indoor experiments cannot adopt underground rock cores to carry out comprehensive tests, so that the experiments have serious randomness and difference; in addition, continuous uniaxial compressive strength parameter profiles (especially for shale reservoir horizontal wells) cannot be obtained through indoor experiments, and the obtained data has great limitation on engineering practicability.
(2) The well logging method comprises the following steps: continuous rock mechanical parameter profiles can be obtained by scaling and explaining logging data through an indoor experiment, but the method is still low in precision, and domestic horizontal well logging is still difficult due to high horizontal well logging difficulty and high risk; for example, the traction force of the underground crawler is limited, and in addition, the horizontal section of the well bore is upwarped, so that the frictional resistance generated by the cable in the three-dimensional horizontal well is difficult to overcome, and the horizontal section of the well can only be generally measured by about 200-400 m; the drilling rod transmission logging process is relatively complex, risks such as drill sticking and drill burying exist, time consumption is long, cost is high, and the drilling rod transmission logging process is rarely adopted; in addition, the over-drill logging technology can take the advantages of cable and transmission logging into account, but is still in the research and development stage at home and is not popularized and applied yet.
Therefore, it is easy to see that the petroleum industry has developed a series of rock mechanical property characterization methods based on uniform continuous medium mechanics, such as indoor experiments, well logging methods, and the like; however, due to the limitations of difficult core acquisition, the detection equipment level and the operation risk, the acquisition of the uniaxial compressive strength parameter of the shale horizontal well is still difficult, and particularly, the horizontal well rock mechanical parameter profile meeting the engineering requirements is difficult to obtain.
Disclosure of Invention
The invention mainly overcomes the defects in the prior art, and aims to provide a shale uniaxial compressive strength evaluation method based on a debris micro-nano indentation experiment.
The technical scheme provided by the invention for solving the technical problems is as follows: the shale uniaxial compressive strength evaluation method based on the rock debris micro-nano indentation experiment comprises the following steps:
s10, collecting rock debris of the target shale reservoir and drying the rock debris;
s20, heating the epoxy resin adhesive and the modified amine hardener to 40 ℃, and then mixing the epoxy resin adhesive and the modified amine hardener in a mass ratio of 3: 1, mixing, fully fusing to form mixed glue, and pouring into a mold;
s30, embedding the dried rock debris into a mold, enabling the rock debris to be in full contact with the mixed glue, standing for more than 24 hours, and obtaining a cemented sample after foams in the mixed glue are eliminated and completely cured;
s40, demolding the cemented rock debris sample, mechanically cutting the cemented rock debris sample, and polishing the cut rock debris sample;
s50, after polishing, processing the surface of the rock debris sample by using a three-ion beam cutting instrument to change the surface into a flat and smooth high-quality section;
s60, carrying out a rock debris micro indentation experiment or a nano indentation experiment on the processed rock debris sample to obtain a plurality of groups of indentation experiment load-displacement curve graphs;
s70, respectively obtaining the maximum indentation load P of each group of indentation experiment load-displacement curve graphsmMaximum penetration depth hmLoading work WtUnloading work WeAnd dissipation energy WirPress-in specific work We/WtNominal hardness Hn；
S80, respectively calculating the uniaxial compressive strength of the shale corresponding to each group of indentation experiment load-displacement curves according to the parameters and the uniaxial compressive strength prediction model of the shale under the micro indentation test condition or the uniaxial compressive strength prediction model of the shale under the nano indentation test condition; finally, calculating the average value of the uniaxial compressive strengths of the plurality of shales, wherein the average value is the uniaxial compressive strength of the shales of the target shale reservoir;
the model for calculating the uniaxial compressive strength of the shale under the micron indentation test condition is as follows:
the shale uniaxial compressive strength calculation model under the nano indentation test condition is as follows:
in the formula: UCS is shale uniaxial strength; h ismMaximum press-in depth; pmThe maximum press-in load; weTo unload work; wtIs the loading work; we/WtThe specific work of pressing in; hnIs the nominal hardness.
The further technical scheme is that in the step S40, the grinding is carried out through a sand disc, and the roughness of the sand disc is gradually refined from 100 meshes to 5000 meshes.
The further technical scheme is that the micron indentation experiment in the step S60 specifically comprises the following steps: loading the surface of the rock debris sample at a constant loading rate of 15N/min, stopping loading and unloading when the surface is loaded to the maximum load of 50N, and obtaining the changes of the load and the loading depth; and performing a gridding lattice experiment on the surface of the rock debris sample to obtain a plurality of groups of indentation experiment load-displacement curve graphs.
The further technical scheme is that the nano indentation experiment in the step S60 specifically comprises the following steps: loading the surface of the rock debris sample at a constant loading rate of 20N/min, stopping loading and unloading when the surface is loaded to the maximum load of 400N, and acquiring the changes of the load and the loading depth; and performing a gridding lattice experiment on the surface of the rock debris sample to obtain a plurality of groups of indentation experiment load-displacement curve graphs.
The further technical scheme is that the specific process of the step S70 is as follows:
directly obtaining the maximum indentation load P from the indentation experiment load-displacement curve chartmMaximum penetration depth hm；
Respectively calculating according to the following formulaLoad work WtUnloading work We；
In the formula: wtIs the loading work; weTo unload work; h ismMaximum press-in depth; p is the loading force at any depth in the loading process; dh is the loading depth step value; h isfTo unload the maximum residual depth;
nominal hardness H is calculated according to the following formulan；
In the formula: hnNominal hardness; a (h)m) As a function of projected area of indenter contact, the function of contact area for a bosch indenter is:
the dissipation energy W is calculated according to the following formulair；
In the formula: wirTo dissipate energy; wtIs the loading work; weTo unload work; h ismMaximum press-in depth; p is the loading force at any depth in the loading process; dh is the loading depth step value; h isfTo unload the maximum residual depth;
the specific power W of the penetration is calculated according to the following formulae/Wt；
In the formula: weW is the press-in specific work; wtIs the loading work; weTo unload work; h ismMaximum press-in depth; p is the loading force at any depth in the loading process; dh is the loading depth step value; h isfTo unload the maximum residual depth.
The further technical scheme is that in the step S60, a rock debris micron indentation experiment is carried out on the processed rock debris sample to obtain a plurality of groups of indentation experiment load-displacement curve graphs; and in the step S80, respectively calculating the uniaxial compressive strength of the shale corresponding to each group of indentation experiment load-displacement curves according to the uniaxial compressive strength prediction model of the shale under the micrometer indentation test condition.
The invention has the following beneficial effects: according to the invention, by developing a shale debris micro-nano indentation experiment, indentation load-depth curves under different scales are obtained, the micro-mechanical parameters of shale are obtained through calculation, a relation model between uniaxial compressive strength and the micro-mechanical parameters is further established, the prediction of the macro-mechanical parameters of the shale is realized, and thus the shale mechanical parameters of a shale horizontal well are accurately obtained; the method can provide basic parameter basis for drilling, well completion and hydraulic fracturing of the shale gas horizontal well, and can effectively guide the drilling, well completion and hydraulic fracturing design and construction of the shale gas horizontal well.
Drawings
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a sample of the collected processed shale cuttings;
FIG. 3 is a sample of shale cuttings after cementing and curing;
FIG. 4 is a sample of surface treated shale cuttings;
FIG. 5 is an electron microscope scanning photograph of a sample of shale debris after surface treatment;
FIG. 6 is a schematic view of a load-displacement curve recorded during loading and unloading;
FIG. 7 is a schematic view of the deformation of the surface of a sample in different loading and unloading states;
FIG. 8 is a load-displacement curve recorded from a micro indentation experiment;
FIG. 9 is a load-displacement curve recorded from a nanoindentation experiment;
FIG. 10 is an energy analysis schematic diagram of a micro-nano indentation load-displacement curve;
FIG. 11 is a statistical histogram of uniaxial compressive strength obtained for the evaluation of micro indentation;
FIG. 12 is a statistical histogram of uniaxial compressive strength obtained from nanoindentation evaluation.
Detailed Description
The present invention will be further described with reference to the following examples and the accompanying drawings.
Example 1
As shown in figure 1, the shale uniaxial compressive strength evaluation method based on the rock debris micro-nano indentation experiment comprises the following steps:
s1, collecting a rock debris sample of the shale reservoir, selecting rock debris which is regular in shape, has a size not less than 2mm and has no obvious cracks, cleaning surface dust, and drying in a vacuum drying box, wherein the processed rock debris sample is shown in figure 2;
s2, heating the epoxy resin adhesive and the modified amine hardener to 40 ℃, and then mixing the epoxy resin adhesive and the modified amine hardener in a mass ratio of 3: 1, mixing, fully fusing to form mixed glue, and pouring into a mold;
s3, embedding the screened rock debris sample, enabling the rock debris sample to be in full contact with the mixed glue, standing for more than 24 hours, and obtaining a cemented rock debris sample after foams in the mixed glue are eliminated and completely cured, wherein the cemented rock debris sample is shown in figure 3;
s4, demolding and mechanically cutting after the rock debris sample is fully cemented, and polishing the cut rock debris sample by using a sand table, wherein the roughness of the sand table is gradually refined from 100 meshes to 5000 meshes;
s5, after the mechanical polishing is finished, processing the surface of the rock debris sample by using a three-ion beam cutting instrument to obtain a flat and smooth high-quality section, as shown in figure 4;
s6, scanning by an electron microscope, as shown in figure 5, after determining that the surface roughness of the rock debris sample meets the requirements of the micro-nano indentation experiment, rapidly packaging the rock debris sample for later use to avoid the contact of the sample to be detected with liquid and dust in the air;
s7, adopting an MFT-4000 type multifunctional material surface property tester, selecting a Bohr pressure head, and keeping the contact position of the pressure head and the rock debris sample to be more than 2mm from the rock debris boundary;
s8, enabling a pressure head to approach the surface of the rock debris sample at a constant speed, loading at a constant loading speed of 15N/min when the pressure head is in contact with the surface of the rock debris sample, stopping loading and unloading when the pressure head is loaded to a maximum load of 50N, and recording changes of the load and the loading depth, wherein fig. 6 shows a load-displacement curve recorded in the loading and unloading process, and fig. 7 shows a sample surface deformation schematic diagram in different loading and unloading states;
s9, performing a gridding lattice experiment on the surface of the rock debris sample to obtain 136 groups of micro indentation experiment load-displacement curves, wherein a part of micro indentation experiment load-displacement curves obtained by the experiment are shown in FIG. 8;
s10, determining the maximum press-in load PmSaid maximum press-in load PmThe maximum indentation load is the maximum indentation load of a micrometer indentation experiment load-displacement curve;
s11, determining the maximum press-in depth hmSaid maximum penetration depth hmThe maximum indentation depth is the maximum indentation depth of a micro indentation experiment load-displacement curve;
s12, determining nominal hardness HnSaid nominal hardness HnCan be driven by the maximum press-in load PmAnd the projected area A (h) of contactm) And calculating to obtain:
in the formula: hnNominal hardness; a (h)m) As a function of projected area of indenter contact, the function of contact area for a bosch indenter is:
s13, determining the loading work WtSaidLoad work WtThe area of OABD in the micrometer indentation test load-displacement curve is shown in fig. 10, i.e.:
in the formula: wtIs the loading work; sOABDIs the area encompassed by curve OABD; h ismMaximum press-in depth; p is the loading force at any depth in the loading process; dh is the loading depth step value;
s14, determining unloading work WeThe unloading work WeThe area of BCD in the micro indentation test load-displacement curve, as shown in fig. 10, is:
in the formula: weTo unload work; sBCDIs the area encompassed by curve BCD; h isfTo unload the maximum residual depth;
s15, determining dissipation energy WirSaid dissipated energy WirThe area of the OABC in the micron indentation test load-displacement curve is shown in fig. 10, i.e.:
in the formula: wirRepresents the difference between the load work and the unload work as dissipated energy; sOABCIs the area encompassed by curve OABC;
s16, determining the press-in ratio work We/WtThe press-in specific work We/WtCan be loaded with work WtAnd the work of unloading WeAnd calculating to obtain:
in the formula: we/WtFor specific work of pressing-in, representing work of unloading WeAnd the loading work WtThe ratio therebetween;
s17, selecting a shale uniaxial compressive strength prediction model under the micron indentation test condition according to the test and analysis requirements, calculating shale uniaxial compressive strength, and performing statistical analysis to obtain a shale uniaxial compressive strength average value;
aiming at the micro indentation test result, the shale uniaxial compressive strength calculation model under the micro indentation test condition is as follows:
in the formula: UCS is shale uniaxial strength; hnNominal hardness; weTo unload work; wtIs the loading work; we/WtThe specific work of pressing in; h ismMaximum press-in depth; pmThe maximum press-in load;
the maximum indentation depth h obtained by 136 groups of micrometer indentation experimentsmMaximum press-in load PmSpecific power We/WtNominal hardness HnThe parameters are substituted into the shale uniaxial compressive strength prediction model under the micron indentation test condition, a statistical histogram of shale uniaxial compressive strength values is obtained through calculation, as shown in fig. 11, the average value of the shale uniaxial compressive strength is 216.19MPa, the test result of the macroscopic uniaxial compressive strength is 248.70MPa, and the deviation between the two values is 13.1%, which shows that the shale uniaxial compressive strength can be accurately evaluated by the method.
Example 2
The shale uniaxial compressive strength evaluation method based on the rock debris micro-nano indentation experiment comprises the following steps:
s10, preparing a rock debris sample of the shale reservoir by adopting the same steps in the example 1;
s20, adopting an Agilent U9820ANano enter G200 nanometer Indenter, selecting a Bow pressure head, and keeping the contact position of the pressure head and the rock debris sample to be more than 2mm from the rock debris boundary;
s30, a control system is utilized to enable a pressure head to approach the surface of the rock debris sample at a constant speed, when the pressure head is in contact with the surface of the rock debris sample, loading is carried out at a constant loading speed of 20mN/min, loading is stopped and unloading is carried out when the maximum load is 400mN, and the system automatically records the changes of the load and the loading depth;
s40, performing a gridding lattice experiment on the surface of the sample to obtain 117 groups of nano indentation experiment load-displacement curves, wherein fig. 9 shows the load-displacement curves of part of the nano indentation experiment obtained by the experiment;
s50, obtaining the maximum indentation load P of each of the 117 sets of nano-indentation experiment load-displacement graphs by respectively adopting the same steps in the example 1mMaximum penetration depth hmLoading work WtUnloading work WeAnd dissipation energy WirPress-in specific work We/WtNominal hardness Hn；
S60, selecting a shale uniaxial compressive strength prediction model under the nano indentation test condition according to the test and analysis requirements, calculating shale uniaxial compressive strength, and performing statistical analysis to obtain a shale uniaxial compressive strength average value;
aiming at the nano indentation test result, the shale uniaxial compressive strength calculation model under the nano indentation test condition is as follows:
in the formula: UCS is shale uniaxial strength; hnNominal hardness; weTo unload work; wtIs the loading work; we/WtThe specific work of pressing in; h ismMaximum press-in depth; pmThe maximum press-in load;
the maximum indentation depth h obtained by 117 groups of micron indentation experimentsmMaximum press-in load PmSpecific power We/WtNominal hardness HnSubstituting the parameters into the shale uniaxial compressive strength prediction model under the micron indentation test condition, calculating to obtain a statistical histogram of shale uniaxial compressive strength values as shown in figure 12, wherein the average value of the shale uniaxial compressive strength is 336.95MPand a, the macroscopic uniaxial compressive strength test result is 248.70MPa, and the deviation between the macroscopic uniaxial compressive strength test result and the macroscopic uniaxial compressive strength test result is 47.50%, which shows that the method can roughly evaluate the uniaxial compressive strength of the shale, and the prediction and evaluation accuracy of the uniaxial compressive strength of the shale still needs to be further improved.
Although the present invention has been described with reference to the above embodiments, it should be understood that the present invention is not limited to the above embodiments, and those skilled in the art can make various changes and modifications without departing from the scope of the present invention.
Claims (6)
1. The shale uniaxial compressive strength evaluation method based on the rock debris micro-nano indentation experiment is characterized by comprising the following steps of:
s10, collecting rock debris of the target shale reservoir and drying the rock debris;
s20, heating the epoxy resin adhesive and the modified amine hardener to 40 ℃, and then mixing the epoxy resin adhesive and the modified amine hardener in a mass ratio of 3: 1, mixing, fully fusing to form mixed glue, and pouring into a mold;
s30, embedding the dried rock debris into a mold, enabling the rock debris to be in full contact with the mixed glue, standing for more than 24 hours, and obtaining a cemented sample after foams in the mixed glue are eliminated and completely cured;
s40, demolding the cemented rock debris sample, mechanically cutting the cemented rock debris sample, and polishing the cut rock debris sample;
s50, after polishing, processing the surface of the rock debris sample by using a three-ion beam cutting instrument to change the surface into a flat and smooth high-quality section;
s60, carrying out a rock debris micro indentation experiment or a nano indentation experiment on the processed rock debris sample to obtain a plurality of groups of indentation experiment load-displacement curve graphs;
s70, respectively acquiring load-displacement of each group of indentation experimentMaximum press-in load P of the graphmMaximum penetration depth hmLoading work WtUnloading work WeAnd dissipation energy WirPress-in specific work We/WtNominal hardness Hn；
S80, respectively calculating the uniaxial compressive strength of the shale corresponding to each group of indentation experiment load-displacement curves according to the parameters and the uniaxial compressive strength prediction model of the shale under the micro indentation test condition or the uniaxial compressive strength prediction model of the shale under the nano indentation test condition; finally, calculating the average value of the uniaxial compressive strengths of the plurality of shales, wherein the average value is the uniaxial compressive strength of the shales of the target shale reservoir;
the model for calculating the uniaxial compressive strength of the shale under the micron indentation test condition is as follows:
the shale uniaxial compressive strength calculation model under the nano indentation test condition is as follows:
in the formula: UCS is shale uniaxial strength; h ismMaximum press-in depth; pmThe maximum press-in load; weTo unload work; wtIs the loading work; we/WtThe specific work of pressing in; hnIs the nominal hardness.
2. The shale uniaxial compressive strength evaluation method based on the detritus micro-nano indentation experiment as claimed in claim 1, wherein the polishing is performed by a sand table in step S40, and the roughness of the sand table is gradually refined from 100 meshes to 5000 meshes.
3. The shale uniaxial compressive strength evaluation method based on the detritus micro-nano indentation experiment as claimed in claim 2, wherein the micro indentation experiment in step S60 comprises the following specific steps: loading the surface of the rock debris sample at a constant loading rate of 15N/min, stopping loading and unloading when the surface is loaded to the maximum load of 50N, and obtaining the changes of the load and the loading depth; and performing a gridding lattice experiment on the surface of the rock debris sample to obtain a plurality of groups of indentation experiment load-displacement curve graphs.
4. The shale uniaxial compressive strength evaluation method based on the detritus micro-nano indentation experiment as claimed in claim 2, wherein the specific steps of the nano indentation experiment in step S60 are as follows: loading the surface of the rock debris sample at a constant loading rate of 20N/min, stopping loading and unloading when the surface is loaded to the maximum load of 400N, and acquiring the changes of the load and the loading depth; and performing a gridding lattice experiment on the surface of the rock debris sample to obtain a plurality of groups of indentation experiment load-displacement curve graphs.
5. The shale uniaxial compressive strength evaluation method based on the detritus micro-nano indentation experiment as claimed in claim 1, wherein the specific process of step S70 is as follows:
directly obtaining the maximum indentation load P from the indentation experiment load-displacement curve chartmMaximum penetration depth hm；
Then, the loading work W is calculated according to the following formulatUnloading work We；
In the formula: wtIs the loading work; weTo unload work; h ismMaximum press-in depth; p is the loading force at any depth in the loading process; dh is the loading depth step value; h isfTo unload the maximum residual depth;
nominal hardness H is calculated according to the following formulan；
In the formula: hnNominal hardness; a (h)m) As a function of projected area of indenter contact, the function of contact area for a bosch indenter is:
the dissipation energy W is calculated according to the following formulair；
In the formula: wirTo dissipate energy; wtIs the loading work; weTo unload work; h ismMaximum press-in depth; p is the loading force at any depth in the loading process; dh is the loading depth step value; h isfTo unload the maximum residual depth;
the specific power W of the penetration is calculated according to the following formulae/Wt；
In the formula: weW is the press-in specific work; wtIs the loading work; weTo unload work; h ismMaximum press-in depth; p is the loading force at any depth in the loading process; dh is the loading depth step value; h isfTo unload the maximum residual depth.
6. The shale uniaxial compressive strength evaluation method based on the rock debris micro-nano indentation experiment as claimed in claim 1, wherein a plurality of sets of indentation experiment load-displacement curves are obtained by performing a rock debris micro-indentation experiment on the processed rock debris sample in step S60; and in the step S80, respectively calculating the uniaxial compressive strength of the shale corresponding to each group of indentation experiment load-displacement curves according to the uniaxial compressive strength prediction model of the shale under the micrometer indentation test condition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011046164.XA CN112179770B (en) | 2020-09-29 | 2020-09-29 | Shale uniaxial compressive strength evaluation method based on rock debris micro-nano indentation experiment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011046164.XA CN112179770B (en) | 2020-09-29 | 2020-09-29 | Shale uniaxial compressive strength evaluation method based on rock debris micro-nano indentation experiment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112179770A true CN112179770A (en) | 2021-01-05 |
| CN112179770B CN112179770B (en) | 2021-05-11 |
Family
ID=73945747
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011046164.XA Active CN112179770B (en) | 2020-09-29 | 2020-09-29 | Shale uniaxial compressive strength evaluation method based on rock debris micro-nano indentation experiment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112179770B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114048640A (en) * | 2022-01-13 | 2022-02-15 | 中国矿业大学(北京) | Method for evaluating shale microcosmic fracture development degree based on nanoindentation experiment |
| CN114091290A (en) * | 2022-01-19 | 2022-02-25 | 中国石油大学(华东) | Rock drillability evaluation method based on rock debris nano indentation |
| CN114486501A (en) * | 2022-02-28 | 2022-05-13 | 西南石油大学 | Rock strength parameter testing method based on rock debris nano-micron indentation experiment |
| CN115046873A (en) * | 2022-05-18 | 2022-09-13 | 中国科学院广州地球化学研究所 | In-situ testing method for mechanical property of shale matrix based on nano indentation technology |
| CN115434699A (en) * | 2022-09-05 | 2022-12-06 | 中国矿业大学(北京) | Logging method and system based on measurement of static mechanical parameters of shale well wall |
Citations (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6349595B1 (en) * | 1999-10-04 | 2002-02-26 | Smith International, Inc. | Method for optimizing drill bit design parameters |
| CN101381836A (en) * | 2008-10-27 | 2009-03-11 | 王铀 | Nano modified WC/Co cemented carbide material and manufacturing method thereof |
| CN101710046A (en) * | 2009-12-02 | 2010-05-19 | 马德军 | Method for testing Young modulus of material through instrumented micron indentation |
| CN101776551A (en) * | 2010-02-09 | 2010-07-14 | 马德军 | Method for testing uniaxial strength mean value of material through instrumented microindentation |
| CN101788420A (en) * | 2010-02-09 | 2010-07-28 | 马德军 | Instrumentation nano press-in method for testing young modulus of material |
| CN102221501A (en) * | 2011-04-22 | 2011-10-19 | 河海大学 | Device and method for measuring mechanical properties of rocks |
| CN102584140A (en) * | 2012-01-19 | 2012-07-18 | 中交上海三航科学研究院有限公司 | Anti-crack concrete for wharf surface layer and preparation method for anti-crack concrete for wharf surface layer |
| CN204027952U (en) * | 2014-06-27 | 2014-12-17 | 尚廷东 | Mortar penetrometer calibrating installation |
| CN105445440A (en) * | 2015-11-19 | 2016-03-30 | 西南石油大学 | Method for evaluating fracturing property of shale based on rock debris microscopic characteristics |
| CN105716976A (en) * | 2016-03-04 | 2016-06-29 | 衢州康平建设工程检测有限公司 | Plastering mortar compressive strength in-situ sphere indentation detector and detection method thereof |
| CN108106938A (en) * | 2017-12-21 | 2018-06-01 | 西南石油大学 | It is a kind of to test the method for determining that acid solution influences dense carbonate Young's modulus |
| CN109506996A (en) * | 2018-10-12 | 2019-03-22 | 西南石油大学 | A kind of shale chip sample preparation method for micron indentation test |
| CN110579400A (en) * | 2019-09-25 | 2019-12-17 | 西南石油大学 | Measuring and calculating method for micro-scale strength and residual strength of brittle rock |
| WO2020021202A1 (en) * | 2018-07-26 | 2020-01-30 | Vicat | Novel cement composition for 3d printing and method of use |
| CN107290219B (en) * | 2017-07-20 | 2020-04-07 | 长江大学 | Comprehensive brittleness evaluation method for gas storage cap rock |
| CN111257536A (en) * | 2020-01-20 | 2020-06-09 | 中国科学院武汉岩土力学研究所 | Rock mechanics and reservoir engineering parameter evaluation method |
| CN112179769A (en) * | 2020-09-29 | 2021-01-05 | 西南石油大学 | Shale elastic modulus evaluation method based on rock debris micro-nano indentation experiment |
-
2020
- 2020-09-29 CN CN202011046164.XA patent/CN112179770B/en active Active
Patent Citations (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6349595B1 (en) * | 1999-10-04 | 2002-02-26 | Smith International, Inc. | Method for optimizing drill bit design parameters |
| CN101381836A (en) * | 2008-10-27 | 2009-03-11 | 王铀 | Nano modified WC/Co cemented carbide material and manufacturing method thereof |
| CN101710046A (en) * | 2009-12-02 | 2010-05-19 | 马德军 | Method for testing Young modulus of material through instrumented micron indentation |
| CN101776551A (en) * | 2010-02-09 | 2010-07-14 | 马德军 | Method for testing uniaxial strength mean value of material through instrumented microindentation |
| CN101788420A (en) * | 2010-02-09 | 2010-07-28 | 马德军 | Instrumentation nano press-in method for testing young modulus of material |
| CN102221501A (en) * | 2011-04-22 | 2011-10-19 | 河海大学 | Device and method for measuring mechanical properties of rocks |
| CN102584140A (en) * | 2012-01-19 | 2012-07-18 | 中交上海三航科学研究院有限公司 | Anti-crack concrete for wharf surface layer and preparation method for anti-crack concrete for wharf surface layer |
| CN204027952U (en) * | 2014-06-27 | 2014-12-17 | 尚廷东 | Mortar penetrometer calibrating installation |
| CN105445440A (en) * | 2015-11-19 | 2016-03-30 | 西南石油大学 | Method for evaluating fracturing property of shale based on rock debris microscopic characteristics |
| CN105716976A (en) * | 2016-03-04 | 2016-06-29 | 衢州康平建设工程检测有限公司 | Plastering mortar compressive strength in-situ sphere indentation detector and detection method thereof |
| CN107290219B (en) * | 2017-07-20 | 2020-04-07 | 长江大学 | Comprehensive brittleness evaluation method for gas storage cap rock |
| CN108106938A (en) * | 2017-12-21 | 2018-06-01 | 西南石油大学 | It is a kind of to test the method for determining that acid solution influences dense carbonate Young's modulus |
| WO2020021202A1 (en) * | 2018-07-26 | 2020-01-30 | Vicat | Novel cement composition for 3d printing and method of use |
| CN109506996A (en) * | 2018-10-12 | 2019-03-22 | 西南石油大学 | A kind of shale chip sample preparation method for micron indentation test |
| CN110579400A (en) * | 2019-09-25 | 2019-12-17 | 西南石油大学 | Measuring and calculating method for micro-scale strength and residual strength of brittle rock |
| CN111257536A (en) * | 2020-01-20 | 2020-06-09 | 中国科学院武汉岩土力学研究所 | Rock mechanics and reservoir engineering parameter evaluation method |
| CN112179769A (en) * | 2020-09-29 | 2021-01-05 | 西南石油大学 | Shale elastic modulus evaluation method based on rock debris micro-nano indentation experiment |
Non-Patent Citations (2)
| Title |
|---|
| RICARDO-ANDRÉS GARCÍA1 等: "DEVELOPMENT OF EXPERIMENTAL CORRELATIONS BETWEEN INDENTATION PARAMETERS AND UNCONFINED COMPRESSIVE", 《CIENCIA, TECNOLOGÍA Y FUTURO》 * |
| 林东: "页岩微米压痕实验研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114048640A (en) * | 2022-01-13 | 2022-02-15 | 中国矿业大学(北京) | Method for evaluating shale microcosmic fracture development degree based on nanoindentation experiment |
| CN114048640B (en) * | 2022-01-13 | 2022-03-18 | 中国矿业大学(北京) | Method for evaluating shale microcosmic fracture development degree based on nanoindentation experiment |
| CN114091290A (en) * | 2022-01-19 | 2022-02-25 | 中国石油大学(华东) | Rock drillability evaluation method based on rock debris nano indentation |
| CN114091290B (en) * | 2022-01-19 | 2022-04-12 | 中国石油大学(华东) | Rock drillability evaluation method based on rock debris nano indentation |
| CN114486501A (en) * | 2022-02-28 | 2022-05-13 | 西南石油大学 | Rock strength parameter testing method based on rock debris nano-micron indentation experiment |
| CN114486501B (en) * | 2022-02-28 | 2023-08-29 | 西南石油大学 | Rock strength parameter testing method based on rock debris nano-micron indentation experiment |
| CN115046873A (en) * | 2022-05-18 | 2022-09-13 | 中国科学院广州地球化学研究所 | In-situ testing method for mechanical property of shale matrix based on nano indentation technology |
| CN115434699A (en) * | 2022-09-05 | 2022-12-06 | 中国矿业大学(北京) | Logging method and system based on measurement of static mechanical parameters of shale well wall |
| CN115434699B (en) * | 2022-09-05 | 2023-08-29 | 中国矿业大学(北京) | Logging method and system based on measurement of shale well wall static mechanical parameters |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112179770B (en) | 2021-05-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112179770B (en) | Shale uniaxial compressive strength evaluation method based on rock debris micro-nano indentation experiment | |
| CN112179769A (en) | Shale elastic modulus evaluation method based on rock debris micro-nano indentation experiment | |
| CN109506996B (en) | Preparation method of shale rock debris sample for micron indentation experiment | |
| CN108590601B (en) | Experimental method for optimizing water injection expansion construction parameters | |
| Zhou et al. | Fatigue damage mechanism and deformation behaviour of granite under ultrahigh-frequency cyclic loading conditions | |
| Jeong et al. | Performance assessment of hard rock TBM and rock boreability using punch penetration test | |
| Perras et al. | Compressive and tensile behavior of 3D-printed and natural sandstones | |
| CN110288233B (en) | Deep shale gas compressibility evaluation method based on fuzzy gray correlation method | |
| CN110637223A (en) | Real-time in-situ mechanical characterization of wellbore cuttings | |
| CN1818608A (en) | Method for computing rock II-type fracture toughness | |
| US20230228189A1 (en) | Method for evaluating rock drillability by nano-indentation test on rock cutting | |
| CN110687253B (en) | Rock sample internal crack manufacturing and grouting effect quantitative evaluation method | |
| CN108318351B (en) | Test method for testing rock shearing mechanical property under normal unloading condition | |
| CN107063791B (en) | Test method and test sample for bonding characteristics of disintegrated soft rock and concrete | |
| Morgan | An experimental and numerical study on the fracturing processes in Opalinus shale | |
| CN103852379A (en) | Method for measuring mechanical properties of rocks through replacing standard-sized rock cores with non-standard-sized rock cores | |
| CN110399699B (en) | Single-tooth rock breaking efficiency evaluation method based on micro-nano indentation | |
| WO2017030838A1 (en) | Mechanisms-based fracture model for geomaterials | |
| CN112730101B (en) | Test method for researching loess landslide mechanism under different working conditions | |
| Qiu et al. | Optimization and experimental research on process parameters of the softness consolidation abrasive particles | |
| CN112213179B (en) | Method and device for measuring surface rigidity of underground shale layer | |
| CN114486501B (en) | Rock strength parameter testing method based on rock debris nano-micron indentation experiment | |
| CN117057083A (en) | Rock drillability determination method based on nanoindentation energy | |
| CN202882768U (en) | Rigid body polycrystalline diamond compact (PDC) centerless drill for micro-drilling experiment | |
| Ding et al. | Mechanical Analyses and ROP Equation Study of Coiled Tubing Bridge Plugs |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |