CN110749530B - Method for measuring porosity of irregular rock sample by liquid metal one-time sample loading - Google Patents
Method for measuring porosity of irregular rock sample by liquid metal one-time sample loading Download PDFInfo
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- 229910001338 liquidmetal Inorganic materials 0.000 title claims abstract description 91
- 238000000034 method Methods 0.000 title claims abstract description 66
- 239000011435 rock Substances 0.000 title claims abstract description 30
- 230000001788 irregular Effects 0.000 title claims abstract description 16
- 239000007789 gas Substances 0.000 claims description 56
- 239000007769 metal material Substances 0.000 claims description 17
- 238000004891 communication Methods 0.000 claims description 9
- 230000006641 stabilisation Effects 0.000 claims description 6
- 238000011105 stabilization Methods 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical group [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052792 caesium Inorganic materials 0.000 claims description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 2
- 238000012937 correction Methods 0.000 claims description 2
- 229910052730 francium Inorganic materials 0.000 claims description 2
- KLMCZVJOEAUDNE-UHFFFAOYSA-N francium atom Chemical compound [Fr] KLMCZVJOEAUDNE-UHFFFAOYSA-N 0.000 claims description 2
- 230000000087 stabilizing effect Effects 0.000 claims description 2
- 238000005259 measurement Methods 0.000 abstract description 19
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052753 mercury Inorganic materials 0.000 abstract description 5
- 238000000691 measurement method Methods 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 description 14
- 239000007788 liquid Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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Abstract
The invention relates to a method for measuring the porosity of an irregular rock sample by utilizing one-time sample loading of liquid metal, relates to the technical field of oil and gas exploration, and is used for providing a porosity analysis method which has low sample preparation requirements and is applicable to all rock samples. In the invention, as the liquid metal is adopted for the measurement of the sample, the sample has almost no volatility in a molten state, so the method has obvious superiority compared with the traditional mercury pump method; in addition, the method has no requirement on the shape of the sample during liquid metal measurement, so that the limitation of the traditional measurement method is broken, and the method brings convenience for full-automatic measurement of the porosity of the rock sample with any irregular shape.
Description
Technical Field
The invention relates to the technical field of oil and gas exploration, in particular to a method for measuring the porosity of an irregular rock sample by utilizing one-time loading of liquid metal.
Background
The porosity (effective porosity) of a rock sample refers to the percentage of the interconnected pore volume of the rock to the total volume of the rock sample. In general, if any two of the three parameters of total volume of rock, communication pore volume and rock skeleton volume can be determined, the porosity can be calculated, whereby the prior art measurement technique measures for these three parameters. The current method for obtaining the three parameters mainly comprises the following steps: the measurement method, the liquid method and the gas method.
The measuring method is mainly aimed at cylindrical rock samples with regular sizes, but in the actual testing process, especially shale samples, more samples are difficult to drill regular plunger samples, so that the measuring method has larger limitation. The liquid method is to obtain the total volume and the pore volume by using the Archimedes buoyancy law, and the dry weight, the total weight after saturation and the weight in the liquid, thereby obtaining the porosity. The liquid used in the liquid method mainly comprises mercury, kerosene, water and alcohol, but the liquid has outstanding problems, wherein the mercury is a toxic and harmful substance, has great harm to human bodies and is almost eliminated, but the total volume can be obtained by mainly using a mercury porosimeter. In addition, kerosene, water, or then alcohol may all introduce greater uncertainty in the test results for different types of samples. For example, in shale, micro-nano pores are dominant, and the above three media are difficult to enter nano-scale pores, so that the measured pore volume is smaller. Meanwhile, due to the existence of the swelling clay mineral, water or alcohol can cause the sample volume to swell and crack, thereby affecting the total volume measurement.
In addition, the total volume of the rock is measured by a liquid method or a measuring method, and the pore volume or the skeleton volume of the rock is required to be measured by other methods after the measurement, so that two steps are required, and the measurement efficiency is low. Therefore, currently, aiming at a compact rock core, a skeleton volume is mainly obtained by adopting a gas method, and Chinese patent discloses a measuring device (application number: 200910230023.0) capable of measuring the porosity of the rock core by once sample loading, wherein the porosity can be obtained by once sample loading based on a gas expansion law. However, the method has the greatest defects that the test sample must have a plane so as to be convenient for the sample to be tightly attached to the base of the cup bottom, the requirement not only increases the processing steps of the sample, but also can make the processing and the acquisition of some loose samples difficult; meanwhile, the method is based on the wrapping of the rubber sleeve on the rock sample, so that the method is not applicable to helium, and the rubber sleeve cannot be completely attached to the sample, so that errors caused by the fact that the rubber sleeve is relatively large can be avoided.
Disclosure of Invention
The invention provides a method for measuring the porosity of an irregular rock sample by utilizing one-time loading of liquid metal, which is used for providing a porosity analysis method with low sample preparation requirements and suitable for all rock samples.
The invention provides a method for measuring the porosity of an irregular rock sample by utilizing one-time sample loading of liquid metal, which comprises the following steps:
step S10: according to the law of Boseki-Ma Lvete, a relation curve between the volume of an object in a first container and the gas pressure in a second container is obtained by calibrating the object with a known volume in the first container;
step S20: adding liquid metal and a sample to be measured into the first container, and respectively obtaining the pressure P of the gas in the second container when the sample to be measured floats on the surface of the liquid metal and when the sample to be measured is immersed into the liquid metal 1 And P 2 ；
Step S30: according to the relation in step S10, the pressure of the gas in the second container is obtained as P 1 And P 2 At the time, the volumes V1 and V2 of the liquid metal and the sample to be measured in the first container are obtained, and the skeleton volume V of the sample to be measured is obtained Skeleton frame And total volume V Total (S) ；
Framework volume V of sample to be measured Skeleton frame And total volume V Total (S) The following definitions are satisfied:
V 1 ＝V metal material +V Skeleton frame
V 2 ＝V Metal material +V Total (S)
Wherein V is Metal material Is the volume of liquid metal in the first vessel;
step S40: obtaining a porosity Φ of the sample, wherein the porosity Φ of the sample satisfies the following definition:
in one embodiment, step S20 includes the sub-steps of:
s21: setting the pressure of the gas in the second container to a predetermined pressure P 0 ；
S22: adding liquid metal and a sample to be tested into the first container, floating the sample to be tested on the surface of the liquid metal, keeping the first container at normal pressure and isolating the first container from the outside, communicating the first container with the second container, and obtaining the pressure P of the gas in the second container after stabilizing 1 ；
S23: the first container and the second container are not communicated, the pressure in the first container is restored to normal pressure, and the pressure of the gas in the second container is restored to a preset pressure P 0 ；
S24: sinking the sample to be tested into the liquid metal, communicating the first container with the second container, and obtaining the pressure P of the gas in the second container after stabilization 2 。
In one embodiment, the liquid metal added to the first vessel is volumetric calibrated prior to the beginning of step S20.
In one embodiment, in step S20, the liquid metal in the first container is not solidified by heating the first container.
In one embodiment, the liquid metal has a melting point below 100 ℃.
In one embodiment, step S10 includes the sub-steps of:
s11: applying a predetermined pressure P to the gas in the second container 0 ；
S12: placing an object with a known volume into the first container, isolating the first container from the outside, keeping normal pressure, communicating the first container with the second container, and obtaining the pressure of the gas in the second container after the object is stabilized;
s13: and repeating the step S12 to obtain gas pressure values corresponding to objects with different volumes, and obtaining a relation curve between the volumes and the gas pressure values.
In one embodiment, in step S30, the pressure of the gas in the second container is obtained as P by linear interpolation or curve fitting according to the relationship in step S10 1 And P 2 Volume V of sample to be measured 1 And V 2 。
In one embodiment, a sample cap for immersing the sample to be tested in the liquid metal is provided in the first container, and a via hole for flowing the liquid metal is provided in the sample cap.
In one embodiment, a communication pipeline is arranged between the first container and the second container, and a control valve is arranged on the communication pipeline.
In one embodiment, the gas in the second container is air or helium.
Compared with the prior art, the invention has the advantages that: the method has the advantages that the porosity of the irregular rock sample can be measured by utilizing the characteristics of liquid metal, and the sample is measured by adopting the liquid metal, so that the liquid metal has almost no volatility in a molten state, and the method has obvious superiority compared with the traditional mercury pump method; in addition, the method has no requirement on the shape of the sample during liquid metal measurement, so that the limitation of the traditional measurement method is broken, and the method brings convenience for full-automatic measurement of the porosity of the rock sample with any irregular shape.
Drawings
The invention will be described in more detail hereinafter on the basis of embodiments and with reference to the accompanying drawings.
FIG. 1 is a flow chart of a method for determining porosity of an irregular rock sample using liquid metal one-shot loading in an embodiment of the invention;
FIG. 2 is a schematic illustration of calibrating an object of known volume in an embodiment of the invention;
FIG. 3 is a first state diagram of a measurement process in an embodiment of the invention;
FIG. 4 is a second state diagram of a measurement process in an embodiment of the invention;
fig. 5 is a graph of volume versus pressure in an embodiment of the invention.
Reference numerals:
1-a first container; 2-a second container; 3-an object of known volume;
4-sample; 5-liquid metal; 6-sample cover;
7-connecting pipelines; 8-valve; 61-via.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
As shown in FIG. 1, the core of the method is that the characteristic that liquid metal can be melted from solid state to liquid state (such as gallium metal with a melting point of only about 30 ℃) at a certain temperature (such as lower than 100 ℃) is utilized to obtain the skeleton volume and the total volume of a sample to be measured, and the measurement principle is based on the glass-Mary law, namely the principle of measuring the rock skeleton volume by a gas method.
In one embodiment of the invention, the method comprises the steps of:
in a first step, an object 3 of known volume is calibrated, obtaining a volume-pressure relationship or a volume-pressure data set.
In a second step, the pressure of the gas in the corresponding second container 2 is measured, with the sample 4 to be measured respectively floating on the surface of the liquid metal 5 and sinking into the liquid metal 5.
Thirdly, according to the relation curve of volume-pressure, obtaining the skeleton volume and total volume of the sample 4 to be measured corresponding to the pressure of the gas in the second container 2, wherein the pore volume of the sample 4 to be measured is the difference between the total volume and the skeleton volume.
Fourth, the porosity phi of the sample is obtained.
Each step of the present invention is specifically described below.
In a first step, the relationship between the volume of the object 3 in the first container 1 and the gas pressure in the second container 2 is obtained by calibrating the object 3 of known volume in the first container 1 according to the law of Boseki-Ma Lvete.
Specifically, the method for obtaining the relationship (or data set) in the first step is as follows:
first, a predetermined pressure P is applied to the gas in the second container 0 . At this time, the first container and the second container are not in communication.
Next, as shown in fig. 2, after placing an object 3 of a known volume in the first container 1, the first container 1 is isolated from the outside and kept at normal pressure (i.e., one standard atmospheric pressure), and the first container 1 and the second container 2 are communicated, and the pressure of the gas in the second container 2 is obtained after stabilization;
finally: the operation of the previous step is repeated to obtain the gas pressure values corresponding to the objects 3 with different volumes, and a relation curve between the volumes and the gas pressure values is obtained.
Wherein the object 3 of known volume is a standard block, which is of cylindrical configuration, and which can be made of stainless steel or the like.
The first standard block has a volume of V Label 1 The corresponding pressure of the gas in the second container 2 is P Label 1 Similarly, the volume of the ith standard block is V Sign i The corresponding pressure of the gas in the second container 2 is P Sign i Then the relationship between the volume of the object and the gas pressure can be obtained with the volume as the ordinate and the pressure as the abscissa.
Before starting the second step of operation, the liquid metal 5 introduced into the first vessel 1 is calibrated in volume. The method of specific calibration is similar to that in the first step.
That is, the gas pressure in the second container is set to a predetermined pressure P 0 The method comprises the steps of carrying out a first treatment on the surface of the And the first container 1 and the second container 2 are communicated, and the pressure P of the gas in the second container 2 is obtained after the stabilization Metal material . According to the above-mentioned relation, the volume V of the liquid metal in the first container 1 is obtained Metal material 。
Alternatively, the liquid metal in the first container 1 may be cooled, and then the mark may be placed in the first container 1A calibration block for calibrating the residual space in the first container 1 and obtaining the volume V of the residual space The remainder is The volume of the first container 1 is subtracted by the volume V of the remaining space The remainder is The volume V of liquid metal in the first vessel 1 is obtained Metal material 。
The volume calibration of the liquid metal 5 is to obtain a more accurate volume of the liquid metal 5, and since the volume of the liquid metal 5 needs to be used in each measurement, the volume is calibrated to an accurate value, which is beneficial to improving the accuracy of the measurement result.
Of course, other methods, such as a direct reading method, may be used to obtain the volume of the liquid metal 5, so long as the volume of the liquid metal 5 is ensured to be a known parameter, and will not be described herein.
After the calibration is completed, the second step can be performed.
In a second step, as shown in fig. 3 and 4, the liquid metal 5 and the sample 4 to be measured are added to the first container 1, and the pressure P of the gas in the second container 2 is obtained when the sample 4 to be measured floats on the surface of the liquid metal 5 (i.e., the first state) and when the sample 4 to be measured sinks into the liquid metal 5 (i.e., the second state) 1 And P 2 。
Specifically, in the second step, P is obtained 1 And P 2 The method of (2) is as follows:
first, the pressure of the gas in the second container 2 is set to a predetermined pressure P 0 。
Next, the liquid metal 5 and the sample 4 to be measured are added to the first container 1, and the sample 4 to be measured floats on the surface of the liquid metal 5, and at this time, although a part of the sample 4 to be measured is immersed in the liquid metal 5, since the porosity is measured as the porosity of the communicating pores, the result of the measurement is not affected as long as the sample 4 to be measured has a part of the surface exposed to the liquid metal.
After the first container 1 is kept at normal pressure (i.e., a standard atmospheric pressure) and isolated from the outside, the first container 1 and the second container are connected 2, and the pressure P of the gas in the second container 2 is obtained after stabilization 1 。
Wherein the first container 1 is provided with a sealing partThe sealing valve is communicated with the outside, and the first container 1 is communicated and isolated with the outside through the opening and closing of the valve. Again, the first container 1 and the second container 2 are disconnected, the pressure in the first container 1 is restored to normal pressure, and the pressure of the gas in the second container 2 is restored to a predetermined pressure P 0 。
Finally, the sample 4 to be measured is immersed in the liquid metal 5, the first container 1 and the second container 2 are communicated, and the pressure P of the gas in the second container 2 is obtained after the stabilization 2 . Although the liquid metal 5 has a certain pressure for a part of the sample 4 to be measured when the sample 4 to be measured floats on the liquid metal 5, the liquid metal 5 has a higher surface tension, so that the pressure of the liquid metal 5 on the sample 4 to be measured is insufficient to enable the liquid metal 5 to enter the pores of the sample 4 to be measured, thereby affecting the accuracy of the measurement result.
It should be noted that the liquid metal should be kept from solidifying during the second measurement step. The liquid metal 5 in the first container 1 is not solidified by heating the first container 1.
In addition, the melting point of the liquid metal 5 is lower than 100 ℃ for convenience of operation.
The liquid metal 5 may be gallium, francium, cesium, or other metals or alloys thereof (alloys with melting point lower than 100 ℃).
Third, according to the relationship between the volume and the pressure obtained in the first step, the pressure of the gas in the second container 2 is obtained to be P 1 And P 2 At this time, the volumes V1 and V2 of the liquid metal and the sample to be measured in the first container are obtained, and the skeleton volume V of the sample to be measured 4 is obtained Skeleton frame And total volume V Total (S) 。
First, the pressure of the gas in the second container 2 is obtained as P 1 And P 2 At this time, the volume V of the object in the first container 1 1 And V 2 (II), (III), (V), (; next, according to V 1 And V 2 Obtaining the skeleton volume V of the sample 4 to be detected Skeleton frame And total volume V Total (S) 。
Specifically, the pressure of the gas in the second container 2 is P 1 When in the first state, the corresponding object in the first container 1 is obtainedVolume V of body 1 Wherein V is 1 The following relationship is satisfied:
V 1 ＝V metal material +V Skeleton frame ；
Since the sample 4 to be measured floats above the liquid metal 5 in the first state, when the first container 1 is communicated with the second container 2, the pressurizing of the first container 1 is equivalent, and in the process, the gas in the first container 1 can enter the pores of the sample 4 to be measured, thus the obtained volume V 1 Is the sum of the volume of the liquid metal 4 and the skeleton volume of the sample 4 to be measured.
The pressure of the gas in the second container 2 is P 2 In the second state, the corresponding volume V of the object in the first container 1 is obtained 2 ，
Wherein V is 2 The following relationship is satisfied:
V 2 ＝V metal material +V Total (S) 。
Since the sample 4 to be measured is immersed in the liquid metal 5 in the second state, the liquid metal 5 is fluctuant to seal the pores of the sample 4 to be measured by the liquid metal 5, and the first container 1 is pressurized after the first container 1 is communicated with the second container 2, and the gas in the first container 1 cannot enter the pores of the sample 4 to be measured in the process, the volume V is obtained after the sample 4 to be measured is immersed in the liquid metal 5 2 Is the sum of the volume of the liquid metal 4 and the total volume of the sample 4 to be measured. By the above relation, the skeleton volume V of the sample 4 can be obtained Skeleton frame And total volume V Total (S) I.e.
V Skeleton frame ＝V 1 -V Metal material ；
V Total (S) ＝V 2 -V Metal material 。
As shown in FIG. 5, according to the relation S between volume and pressure, a linear interpolation method or a curve fitting method can be adopted to obtain the pressure P of the gas in the second container 1 And P 2 At this time, the volume V of the object in the first container 1 1 And V 2 。
When calculating by adopting a straight line interpolation method, the method is adoptedThe volume difference between the two end points used (e.g. points a and B) must be small enough to meet the accuracy requirements of the measurement, i.e. the standard blocks used in the first step must be sufficiently large to meet the accuracy requirements. As shown in FIG. 5, the pressure obtained by the linear interpolation method is P 1 Corresponding volume is V 1 。
When the calculation is performed by adopting a curve fitting method, V is calculated according to the law of Boseki-Ma Lvete 1 And V 2 The following definitions are satisfied:
wherein a, b, c and d are all coefficients, and in the process of calibrating the standard block in the first step, since the four coefficients whose volume and pressure are known parameters are unknown parameters, any two points A (P Sign i ，V Sign i ) And B (P) Mark i+1 ，V Mark i+1 ) The four coefficients can be obtained, so that the equation of the curve AB segment can be obtained. In the third step, the four coefficients are known parameters, and the obtained pressure is P 1 Obtaining volume V 1 ；V 2 Is similar to the method of obtaining the same.
As can be seen from FIG. 5, V is calculated by curve fitting 1 Can fall on the relation curve S more accurately, so the measurement accuracy is higher.
Fourth, obtaining the porosity Φ of the sample, wherein the porosity Φ of the sample satisfies the following definition formula:
in the above measurement, the first container 1 is provided with a sample cap 6 for immersing the sample 4 to be measured in the liquid metal 5, and the sample cap 6 is provided with a via hole 61 for passing the liquid metal 5. When the sample 4 to be measured is pressed down by the sample cap 6, the liquid metal 5 flows through the through hole 61, and the liquid level of the liquid metal 5 rises, so that the remaining space in the first container 1 becomes small.
In one embodiment, the sample hood 6 is configured as a link structure.
It should be noted that, in order to press the sample 4 to be tested down into the liquid metal 5, a portion of the connecting rod enters the first container 1, which corresponds to a portion of the volume V added to the first container 1 Rod Thus, the volume V obtained is required 2 Performing correction, wherein the corrected volume V 2 ' satisfy the following definition:
V 2 ’＝V metal material +V Total (S) ’+V Rod 。
Volume V of the connecting rod Rod Can be obtained by calculation according to the descending height of the connecting rod and the diameter of the connecting rod, thereby obtaining the total volume V of the corrected sample 4 to be measured Total (S) ' wherein the corrected volume V Total (S) ' satisfy the following definition:
V total (S) ’＝V 2 ’-V Metal material -V Rod 。
A communication line 7 is provided between the first container 1 and the second container 2, and a control valve 8 is provided in the communication line 7. The on-off of the communication pipeline 7 can be controlled by controlling the opening and closing of the valve 8, so that the on-off between the first container 1 and the second container 2 is realized.
In one embodiment, the gas in the second container 2 is air or helium. Specifically, for the sample to be tested with larger pores, air may be filled in the second container 2, and for the sample to be tested 4 with higher density, helium may be filled in the second container 2.
In summary, the data set of the volume corresponding to each pressure value is obtained through a series of standard blocks; therefore, when the volume of the sample to be measured is unknown, the volume corresponding to the corresponding pressure can be obtained by adopting an interpolation method or a curve method through the data set of the pressure and the volume, so that the porosity of the sample to be measured is obtained, and in the whole process, the measuring process can be completed by only one sample loading, so that the measuring efficiency and the measuring accuracy are improved.
While the invention has been described with reference to a preferred embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the technical features mentioned in the respective embodiments may be combined in any manner as long as there is no structural conflict. The present invention is not limited to the specific embodiments disclosed herein, but encompasses all technical solutions falling within the scope of the claims.
Claims (6)
1. A method for measuring the porosity of an irregular rock sample by using one-time loading of liquid metal, which is characterized by comprising the following steps:
step S10: according to the law of Boseki-Ma Lvete, a relation curve between the volume of an object in a first container and the gas pressure in a second container is obtained by calibrating the object with a known volume in the first container; the gas in the second container is helium;
step S20: adding liquid metal and a sample to be measured into the first container, and respectively obtaining the pressure P of the gas in the second container when the sample to be measured floats on the surface of the liquid metal and when the sample to be measured is immersed into the liquid metal 1 And P 2 The method comprises the steps of carrying out a first treatment on the surface of the Before step S20 begins, calibrating the volume of the liquid metal added into the first container, after the liquid metal in the first container is cooled, calibrating the residual space in the first container by putting a standard block into the first container, and obtaining the volume V of the residual space The remainder is Subtracting the volume V of the remaining space from the volume of the first container The remainder is The volume V of the liquid metal in the first container can be obtained Metal material The method comprises the steps of carrying out a first treatment on the surface of the The liquid metal is gallium, francium, cesium or alloys thereof;
step S30: according to the relation in step S10, the pressure of the gas in the second container is obtained as P 1 And P 2 When the liquid metal in the first container and the volume V of the sample to be tested 1 And V 2 And obtaining the skeleton volume V of the sample to be tested Skeleton frame And total volume V Total (S) ；
Framework volume V of sample to be measured Skeleton frame And total volume V Total (S) The following definitions are satisfied:
V 1 ＝V metal material +V Skeleton frame
V 2 ＝V Metal material +V Total (S)
Wherein V is Metal material Is the volume of liquid metal in the first vessel;
step S40: obtaining a porosity Φ of the sample, wherein the porosity Φ of the sample satisfies the following definition:
step S20 comprises the following sub-steps:
s21: setting the pressure of the gas in the second container to a predetermined pressure P 0 ；
S22: adding liquid metal and a sample to be tested into the first container, floating the sample to be tested on the surface of the liquid metal, keeping the first container at normal pressure and isolating the first container from the outside, communicating the first container with the second container, and obtaining the pressure P of the gas in the second container after stabilizing 1 ；
S23: the first container and the second container are not communicated, the pressure in the first container is restored to normal pressure, and the pressure of the gas in the second container is restored to a preset pressure P 0 ；
S24: sinking the sample to be tested into the liquid metal, communicating the first container with the second container, and obtaining the pressure P of the gas in the second container after stabilization 2 ；
A sample cover for sinking the sample to be tested into the liquid metal is arranged in the first container, a through hole for allowing the liquid metal to flow through is formed in the sample cover, and the sample cover is in a connecting rod structure;
also comprises the step of obtaining the volume V 2 A step of performing correction, wherein the corrected volume V 2 ' satisfy the following definition:
V 2 ’＝V metal material +V Total (S) ’+V The rod is provided with a plurality of holes,
volume V of the connecting rod Rod The diameter of the connecting rod is obtained according to the descending height of the connecting rod;
according to the corrected volume V 2 ' obtaining the total volume V of the corrected sample to be tested Total (S) ' wherein the corrected volume V Total (S) ' satisfy the following definition:
V total (S) ’＝V 2 ’-V Metal material -V Rod 。
2. The method for measuring porosity of irregular rock samples by one-time loading of liquid metal according to claim 1, wherein in step S20, the liquid metal in the first container is not solidified by heating the first container.
3. The method for determining the porosity of an irregular rock sample using one-time loading of liquid metal according to claim 2, wherein the melting point of the liquid metal is lower than 100 ℃.
4. The method for measuring the porosity of an irregular rock sample by means of one-time loading of liquid metal according to claim 1, wherein the step S10 comprises the following sub-steps:
s11: applying a predetermined pressure P to the gas in the second container 0 ；
S12: placing an object with a known volume into the first container, isolating the first container from the outside, keeping normal pressure, communicating the first container with the second container, and obtaining the pressure of the gas in the second container after the object is stabilized;
s13: and repeating the step S12 to obtain gas pressure values corresponding to objects with different volumes, and obtaining a relation curve between the volumes and the gas pressure values.
5. The method for measuring the porosity of an irregular rock sample by one-time loading of liquid metal according to claim 1, wherein in step S30, according to the relation curve in step S10, a linear interpolation method or a curve fitting method is adopted to obtain the pressure of the gas in the second container as P 1 And P 2 Volume V of sample to be measured 1 And V 2 。
6. The method for measuring the porosity of an irregular rock sample by utilizing one-time loading of liquid metal according to claim 1, wherein a communication pipeline is arranged between the first container and the second container, and a control valve is arranged on the communication pipeline.
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