CN111141654A - Preparation method of metal standard substance - Google Patents

Preparation method of metal standard substance Download PDF

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Publication number
CN111141654A
CN111141654A CN201911404163.5A CN201911404163A CN111141654A CN 111141654 A CN111141654 A CN 111141654A CN 201911404163 A CN201911404163 A CN 201911404163A CN 111141654 A CN111141654 A CN 111141654A
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standard
metal
sign board
permeability
nickel
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秦婧
杨佳佳
沈斌
徐学敏
许智超
汪双清
孙玮琳
栗敏
张小涛
黄春华
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NATIONAL Research CENTER OF GEOANALYSIS
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • 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
    • G01N15/0806—Details, e.g. sample holders, mounting samples for testing
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • 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
    • G01N15/0893—Investigating volume, surface area, size or distribution of pores; Porosimetry by measuring weight or volume of sorbed fluid, e.g. B.E.T. method

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Abstract

The invention provides a preparation method of a metal standard substance, which is used for permeability test and comprises the following steps: determining a first weight of the metal powder according to the compaction rate, the size and the metal density of the standard substance to be prepared, wherein the first weight is the weight of the standard substance to be prepared; placing the metal powder with the first weight in a prefabricated mould, and carrying out mould pressing to obtain a mould pressing semi-finished product; and sintering the mould pressing semi-finished product at a first temperature for a first time to obtain the metal standard product. The preparation method of the metal standard substance is simple and convenient, and the prepared metal standard substance can be used for calibrating a permeability testing instrument, can be repeatedly used, and has long service life and low cost.

Description

Preparation method of metal standard substance
Technical Field
The invention relates to a standard product of a testing instrument, in particular to a preparation method of a metal standard product.
Background
At present, permeability testing methods are various and mainly include a normal-pressure steady-state measuring method, a non-steady-state measuring method under overpressure and the like. In the testing process, a universal standard substance is lacked to check and verify the instrument before testing, and the state of the instrument and the validity of testing data are monitored in the testing process.
Among the existing standards in the market at present, the permeability values are 0.40md, 1.0md, 0.60md, 100md, 200md, 300md, 500md and 2000md-3000md, but most of the standards are artificial rock cores formed by pressing purple sand mud, quartz sand, talcum powder and the like after proportioning, the permeability test is to forcibly fill liquid or gas into a sample, when the mercury pressing method is used for filling liquid, the standard is greatly damaged and has high use cost, when the covering hole nitriding gas adsorption method is used, the mineral is subjected to microcrack by additional pressure, the service life of the standard is limited, the use of the standard is limited, and most of the porosity permeability tests in the industry at present are in a state that the standard is not used for instrument calibration and test quality monitoring.
Disclosure of Invention
In view of the above, there is a need for a method for preparing a metal standard, which is simple and convenient, and the prepared metal standard can be used for calibrating a permeability test instrument, and is reusable, long in service life and low in cost.
A method of making a metal standard for use in permeability testing, comprising:
determining a first weight of the metal powder according to the compaction rate, the size and the metal density of the standard substance to be prepared, wherein the first weight is the weight of the standard substance to be prepared;
placing the metal powder with the first weight in a prefabricated mould, and carrying out mould pressing to obtain a mould pressing semi-finished product;
and sintering the mould pressing semi-finished product at a first temperature for a first time to obtain the metal standard product.
Wherein the metal standard is a stainless steel standard or a nickel standard.
Wherein the metal powder is stainless steel powder, and the particle size of the stainless steel powder is 25-120 μm.
Wherein the first temperature is 950 ℃ -1300 ℃.
Wherein the metal powder is nickel powder, and the particle size of the nickel powder is 1-48 mu m.
Wherein the first temperature is 800 ℃ to 950 ℃.
Wherein the standard is cylindrical, and the first weight is calculated by the following formula:
Mmetal＝π(dSign board/2)2hSign boardΦSign boardρSign board
Wherein M isMetalIs a first weight, phiSign boardThe compaction rate of the standard product is obtained; dSign boardIs the diameter of the standard, hSign boardIs a predetermined size; rhoSign boardIs the density of the metal.
Wherein, the standard substance is a cuboid, and the first weight is calculated by the following formula:
Mmetal＝lSign boardwSign boardhSign boardΦSign boardρSign board
Wherein M isMetalIs a first weight, phiSign boardThe compaction rate of the standard to be prepared; lSign boardLength of standard to be prepared, wSign boardIs the width of the standard, hSign boardIs the height of the standard to be prepared; rhoSign boardIs the density of the metal.
Wherein the first time is 0.5h-4 h.
Wherein the sintering is performed in a vacuum state.
Therefore, the preparation method of the metal standard substance is simple and convenient, and the prepared metal standard substance can be used for calibrating a permeability testing instrument, can be repeatedly used, and has long service life and low cost.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The technical solution of the present invention will be clearly and completely described below with reference to specific embodiments. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, shall fall within the scope of protection of the present invention.
Permeability refers to the ability of a rock to allow the passage of fluids (liquids or gases) under a certain pressure differential. The permeability is a parameter that characterizes the ability of the soil or rock itself to conduct fluids. The magnitude of the permeability is related to factors such as porosity, pore geometry in the direction of fluid penetration, particle size, and orientation, and is independent of the nature of the fluid moving through the medium. Permeability is used to indicate the magnitude of permeability.
The grades of permeability can be divided into: ultra-low permeability (permeability)<10md), low permeability (10 md)<Permeability rate of penetration<100md), conventional permeability (100 md)<Permeability rate of penetration<500md), high permeability (500 md)<Permeability rate of penetration<2000md) and ultra high permeability (permeability)>2000 md). The metal standard substance for the permeability testing instrument can be used for testing ultra-low permeability, and the Ke's permeability can be as low as 2 x 10-4md。
The permeability standard substance is an article used for comparison in permeability test analysis of rocks or other substances, has known permeability value and good reproducibility, and can be used for evaluating an analysis method or examining the technical operation level of an analyst and the like.
The "permeability" of the present invention means a permeability in terms of Kjeldahl unless otherwise specified. "parts" means parts by weight unless otherwise specified.
The metal standard substance for low and ultra-low permeability test of the preferred embodiment of the invention is prepared by molding and sintering metal powder.
In some embodiments, the metal standard of the present invention is a nickel standard having a 2 x 10 k permeability as measured at a measured confining pressure of 1000psi to 5000psi-4md-20md, porosity 0.3%-45％。
"porosity" refers to the ratio of the sum of all the volumes of pore space in a rock sample to the volume of the rock sample, referred to as the total porosity of the rock, expressed as a percentage.
In some embodiments, the nickel standard has a compaction ratio of 53% to 92%. When the compaction rate is higher than 92%, the permeability of the nickel standard substance is very low and exceeds the detection lower limit of an instrument; when the compaction rate is lower than 53%, the porosity of the prepared standard product is higher, and the stability of the standard product is reduced.
"compaction" refers to the ratio of the calculated density of the metal standard produced to the theoretical density of the metal.
In other embodiments, the metal standard of the present invention is a stainless steel standard having a permeability in grams per centimeter of 2.5-63 md and a porosity of 9% -35% when measured at a measured confining pressure of 1000-5000 psi.
In some embodiments, the stainless steel standard has a compaction ratio of 61% to 85%. When the compaction rate is higher than 85%, the permeability of the stainless steel standard substance is very low and exceeds the detection lower limit of an instrument; when the compaction rate is lower than 61%, the porosity of the prepared standard product is higher, and the stability of the standard product is reduced.
According to the requirements of a pore penetration testing instrument, a common metal standard product is cylindrical, and the diameter of the standard product is 2.35cm-2.66cm or 3.68cm-3.94 cm; the height is 1.9cm-7.62 cm. In other embodiments, the metal standard may also be a rectangular parallelepiped.
The preparation method of the metal standard substance provided by the embodiment of the invention comprises the following steps:
s1, determining a first weight of the metal powder according to the compaction rate of the standard to be prepared, the size of the standard to be prepared (such as the shape, radius, height, etc. of the standard), and the metal density, wherein the first weight is the weight of the standard to be prepared;
in some embodiments, when the metal powder is nickel powder, the nickel powder has a particle size of 1 μm to 48 μm.
In some embodiments, when the metal powder is stainless steel powder, the stainless steel powder has a particle size of 25 μm to 120 μm.
The larger the particle size of the metal powder, the higher the permeability of the prepared standard.
The shape of the standard includes but is not limited to solid cylindrical shape or solid shape such as rectangular parallelepiped.
In one embodiment, the standard is cylindrical, and a first weight M of the standard to be prepared is calculated by the following formula (1);
formula (1): m ═ pi (d)Sign board/2)2hSign boardΦSign boardρSign board
Wherein phiSign boardThe compaction rate of the standard to be prepared; dSign boardDiameter of the standard to be prepared, hSign boardIs the height of the standard to be prepared; rhoSign boardIs the density of the metal.
In another embodiment, if the standard is a rectangular parallelepiped, a first weight M of the standard to be prepared in a predetermined size is calculated by formula (2);
formula (2): m ═ lSign boardwSign boardhSign boardΦSign boardρSign board
Wherein phiSign boardThe compaction rate of the standard product is obtained; lSign boardIs the length of the standard, wSign boardIs the width of the standard, hSign boardIs the height of the standard; rhoSign boardIs the density of the metal.
And S2, placing the metal powder with the first weight in a prefabricated mould, and carrying out mould pressing to obtain a mould pressing semi-finished product.
Specifically, metal powder with the required weight is weighed and placed in a prefabricated mold, the prefabricated mold is placed in a press machine for mold pressing, the pressure of the metal powder is relieved when the metal powder is slowly pressed to the preset size, and a formed product is taken out of the mold, namely a mold pressing semi-finished product. In the process of molding, the molding time should be controlled to be not less than 30 seconds so as to prevent the standard product to be prepared from being in time to conduct at the contact surface, and the distribution of internal pores is extremely uneven.
Wherein the predetermined size is a size of a standard to be prepared. In one embodiment, the predetermined dimension is determined if the standard is cylindricalIs the diameter d of the standard to be preparedSign boardOr radius dSign boardA/2, and a height hSign board. In another embodiment, if the standard is a cuboid, the predetermined dimensions are the length, width, height of the standard to be prepared.
And S3, sintering the mould pressing semi-finished product at a first temperature to obtain the metal standard product.
Wherein the first temperature is 800-950 ℃, and when the sintering temperature is lower than 950 ℃, the nickel powder can not be well condensed, thereby forming a stable standard product. When the temperature is higher than 950 ℃, the formed standard product has very high compaction rate and small porosity, the permeability of the standard product cannot be measured, and the standard product cannot be used as a standard product for permeability test.
Wherein the first time is 0.5h-4 h. The first time is too short, the stability of the standard is not good, the first time is too long, part of the metal in the standard may melt, so that the porosity is reduced or unbalanced, and the like.
The higher the first temperature, the shorter the first time.
Specifically, the semi-finished product of the mould pressing is placed in a vacuum sintering furnace, sintered for 0.5 to 4 hours at the temperature of 800 to 950 ℃ in a vacuum state, cooled and taken out to prepare the standard product. The vacuum can prevent the metal from being oxidized and influencing the porosity and permeability of the prepared metal standard product.
In some embodiments, the method of preparing the metal standard further comprises: and polishing the side surface of the prepared standard product. The shape of the prepared standard product is more regular by grinding, so that the measurement accuracy is further improved. It should be understood that the top and bottom surfaces of the prepared standard were not ground. If the top surface and the bottom surface of the prepared standard product are polished, the pores of the top surface and the bottom surface are easily blocked, and the permeability is influenced. In one embodiment, the gas permeability is measured by measuring the permeability of the gas in the vertical direction of the cylinder under the overpressure, and the pressure is closed all around, so that the side processing does not affect the value.
The metal standard substance of the invention adopts a CMS-300 type overburden pore permeability tester of American rock core company to measure the permeability and the porosity. Through a large number of experiments and test metersIt is clear that porosity and compaction have the following relationship: compaction ratio (. PHI.)Sign board) 0.0122 Xporosity20.371 × porosity +92.353, correlation coefficient R20.9963. Thus, the higher the porosity of the metal standard, the lower the compaction rate during preparation.
Repeated test experiments show that the metal standard substance prepared by the invention can be repeatedly used for more than 50 times, and can be repeatedly used all the time as long as the metal standard substance is not oxidized.
The metal prepared by the method has firm standard quality, can bear large confining pressure, can meet the measurement of porosity and permeability under different pressure covering conditions, and has stable numerical value. The permeability tester can be repeatedly used, greatly prolongs the service life of the standard substance of the permeability tester, and can be used for calibrating the instrument and monitoring the test quality.
The technical solutions of the present invention are described in more detail below with reference to specific examples, which are provided only for better understanding of the present invention and are not intended to limit the present invention.
Example 1
Nickel powder with the average particle size of 2 microns is used as a raw material to manufacture a cylindrical standard product with the diameter of 2.5cm, the height of 4.7cm and the compaction rate of 91.5%, and a porosity and permeability repeatability test is carried out by utilizing a CMS-300 type overburden pore infiltration tester of American rock core company.
The manufacturing process of the metal standard product is as follows:
1) calculating the weight M of the required nickel powder according to the formula (1)Nickel (II)178 g;
2) adding 178g of nickel powder into a mould, placing the mould on a press, releasing pressure when the nickel powder in the mould is pressed to the standard substance with the height of 4.7cm, and taking out the mould to obtain a mould pressing semi-finished product;
3) and (3) putting the mould pressing semi-finished product into a vacuum sintering furnace, sintering for 1 hour at 900 ℃, cooling and taking out to obtain the nickel standard product.
Testing of nickel standards: the porosity and the krcker permeability of the nickel standard prepared in the embodiment are repeatedly measured by adopting a porosity calibration standard of a CMS-300 type overburden pore permeability tester of American rock core company.
The specific test procedures and conditions were as follows:
a) measuring the diameter and the height of the porosity calibration standard nickel standard by using a vernier caliper, and measuring the average value for 5 times respectively;
b) after the instrument was debugged, the porosity and the kreb permeability of the nickel standard were measured at confining pressures of 1000psi and 3000psi, respectively. The porosity calibration standard is a porosity calibration standard of an instrument of American rock core company and is used for inspecting a porosity test value so as to judge whether the instrument is in a good state or not.
The test shows that the nickel standard substance prepared by the embodiment has good repeatability, and can be repeatedly measured for at least more than 30 times. The data of 12 replicates of the nickel standard prepared in this example were randomly extracted as shown in table 1 below.
Table 1 test results for nickel standards made in example 1
Figure BDA0002348183190000071
Example 2
Nickel powder with the average particle size of 2 microns is used as a raw material to manufacture a cylindrical standard product with the diameter of 2.5cm, the height of 4.7cm and the compaction rate of 92%, and a CMS-300 type overburden pore infiltration tester of American rock core company is used for testing the porosity and the permeability.
The manufacturing process of the metal standard product is as follows:
1) calculating the weight M of the required nickel powder according to the formula (1)Nickel (II)Is 180 g;
2) adding 180g of nickel powder into a mold, placing the mold on a press, releasing pressure when the nickel powder in the mold is pressed to the standard product with the height of 4.7cm, and taking out to obtain a semi-finished product for mold pressing;
3) and (3) putting the mould pressing semi-finished product into a vacuum sintering furnace, sintering for 1 hour at 900 ℃, cooling and taking out to obtain the nickel standard product.
Testing of nickel standards: the porosity and the krcker permeability of the nickel standard prepared in the embodiment are repeatedly measured by adopting a porosity calibration standard of a CMS-300 type overburden pore permeability tester of American rock core company.
The specific test procedures and conditions were as follows:
a) measuring the diameter and the height of the porosity calibration standard nickel standard by using a vernier caliper, and measuring the average value for 5 times respectively;
b) after the instrument debugging is completed, the porosity and the Kjeldahl permeability of the nickel standard are measured under the confining pressure of 1000psi, 3000psi and 5000psi respectively.
The porosity and permeability test data of the nickel standard are shown in table 2.
Table 2 test results for nickel standards made in example 2
Figure BDA0002348183190000081
Example 3
Nickel powder with the average particle size of 2 microns is used as a raw material to manufacture a cylindrical standard product with the diameter of 2.5cm, the height of 4.25cm and the compaction rate of 53 percent, and a CMS-300 type overburden pore infiltration tester of American rock core company is used for testing the porosity and the permeability.
The manufacturing process of the metal standard product is as follows:
1) calculating the weight M of the required nickel powder according to the formula (1)Nickel (II)Is 100 g;
2) adding 100g of nickel powder into a mold, placing the mold on a press, releasing pressure when the nickel powder in the mold is pressed to the standard product with the height of 4.25cm, and taking out to obtain a semi-finished product for mold pressing;
3) and (3) putting the mould pressing semi-finished product into a vacuum sintering furnace, sintering for 1 hour at 900 ℃, cooling and taking out to obtain the nickel standard product.
Testing of nickel standards: the porosity and the krcker permeability of the nickel standard prepared in the embodiment are repeatedly measured by adopting a porosity calibration standard of a CMS-300 type overburden pore permeability tester of American rock core company.
The specific test procedures and conditions were as follows:
a) measuring the diameter and the height of the porosity calibration standard nickel standard by using a vernier caliper, and measuring the average value for 5 times respectively;
b) after the instrument was debugged, the porosity and the kreb's permeability of the nickel standard were measured 2 times at a confining pressure of 1000 psi.
The porosity and permeability test data of the nickel standard are shown in table 3.
Table 3 test results for nickel standards made in example 3
Figure BDA0002348183190000091
Example 4
Nickel powder with the average particle size of 48 microns and nickel powder with the average particle size of 2 microns are used as raw materials, cylindrical standard products with the compaction rate of 86.5% are respectively manufactured, and porosity and permeability tests are carried out by utilizing a CMS-300 type overburden pore infiltration tester of American rock core company.
The manufacturing process of the metal standard product is as follows:
1) calculating the weight M of the required nickel powder according to the formula (1)Nickel (II)Is 164 g;
2) adding 164g of nickel powder into a mold, placing the mold on a press, releasing pressure when the nickel powder in the mold is pressed to the standard product with the height of 4.3cm, and taking out to obtain a semi-finished product for mold pressing;
3) and (3) putting the mould pressing semi-finished product into a vacuum sintering furnace, sintering for 1 hour at 900 ℃, cooling and taking out to obtain the nickel standard product.
Testing of nickel standards: the porosity and the krcker permeability of the nickel standard prepared in the embodiment are repeatedly measured by adopting a porosity calibration standard of a CMS-300 type overburden pore permeability tester of American rock core company.
The specific test procedures and conditions were as follows:
a) measuring the diameter and the height of the porosity calibration standard nickel standard by using a vernier caliper, and measuring the average value for 5 times respectively;
b) after the instrument was debugged, the porosity and the kreb's permeability of the nickel standard were measured 2 times at a confining pressure of 1000 psi.
The porosity and permeability test data of the nickel standard are shown in table 4.
Table 4 test results for nickel standards made in example 4
Figure BDA0002348183190000101
Example 5
Nickel powder with the average particle size of 2 microns is used as a raw material to manufacture a cylindrical standard product with the diameter of 2.4cm, the height of 4.5cm and the compaction rate of 90%, and a CMS-300 type overburden pore infiltration tester of American rock core company is used for testing the porosity and the permeability.
The manufacturing process of the metal standard product is as follows:
1) calculating the weight M of the required nickel powder according to the formula (1)Nickel (II)169 g;
2) adding 169g of nickel powder into a mold, placing the mold on a press, releasing pressure when the nickel powder in the mold is pressed to the standard product with the height of 4.5cm, and taking out to obtain a semi-finished product for mold pressing;
3) and (3) putting the mould pressing semi-finished product into a vacuum sintering furnace, sintering for 1 hour at 900 ℃, cooling and taking out to obtain the nickel standard product.
Testing of nickel standards: the porosity and the krcker permeability of the nickel standard prepared in the embodiment are repeatedly measured by adopting a porosity calibration standard of a CMS-300 type overburden pore permeability tester of American rock core company.
The specific test procedures and conditions were as follows:
a) measuring the diameter and the height of the porosity calibration standard nickel standard by using a vernier caliper, and measuring the average value for 5 times respectively;
b) after the instrument was debugged, the porosity and the kreb's permeability of the nickel standard were measured 2 times at a confining pressure of 1000 psi.
The porosity and permeability test data of the nickel standard are shown in table 5.
Table 5 test results for nickel standards made in example 5
Figure BDA0002348183190000111
Example 6
Nickel powder with the average particle size of 2 microns is used as a raw material to manufacture a cylindrical standard product with the diameter of 2.5cm, the height of 4.3cm and the compaction rate of 87.5%, and a CMS-300 type overburden pore infiltration tester of American rock core company is used for testing the porosity and the permeability.
The manufacturing process of the metal standard product is as follows:
1) calculating the weight M of the required nickel powder according to the formula (1)Nickel (II)166 g;
2) adding 166g of nickel powder into a mold, placing the mold on a press, releasing pressure when the nickel powder in the mold is pressed to the standard product with the height of 4.3cm, and taking out the nickel powder to obtain a semi-finished product for mold pressing;
3) and (3) putting the mould pressing semi-finished product into a vacuum sintering furnace, sintering for 1 hour at 900 ℃, cooling and taking out to obtain the nickel standard product.
Testing of nickel standards: the porosity and the krcker permeability of the nickel standard prepared in the embodiment are repeatedly measured by adopting a porosity calibration standard of a CMS-300 type overburden pore permeability tester of American rock core company.
The specific test procedures and conditions were as follows:
a) measuring the diameter and the height of the porosity calibration standard nickel standard by using a vernier caliper, and measuring the average value for 5 times respectively;
b) after the instrument was debugged, the porosity and the kreb's permeability of the nickel standard were measured 2 times at a confining pressure of 1000 psi.
The porosity and permeability test data of the nickel standard are shown in table 6.
Table 6 test results for nickel standards made in example 6
Figure BDA0002348183190000121
Example 7
Nickel powder with the average particle size of 2 microns is used as a raw material to manufacture a cylindrical standard product with the diameter of 2.5cm, the height of 4cm and the compaction rate of 75.8%, and a CMS-300 type overburden pore infiltration tester of American rock core company is used for testing the porosity and the permeability.
The manufacturing process of the metal standard product is as follows:
1) calculating the weight M of the required nickel powder according to the formula (1)Nickel (II)135.5 g;
2) adding 135.5g of nickel powder into a mould, placing the mould on a press, releasing pressure when the nickel powder in the mould is pressed to the standard substance height of 4cm, and taking out to obtain a mould pressing semi-finished product;
3) and (3) putting the mould pressing semi-finished product into a vacuum sintering furnace, sintering for 1 hour at 900 ℃, cooling and taking out to obtain the nickel standard product.
Testing of nickel standards: the porosity and the krcker permeability of the nickel standard prepared in the embodiment are repeatedly measured by adopting a porosity calibration standard of a CMS-300 type overburden pore permeability tester of American rock core company.
The specific test procedures and conditions were as follows:
a) measuring the diameter and the height of the porosity calibration standard nickel standard by using a vernier caliper, and measuring the average value for 5 times respectively;
b) after the instrument was debugged, the porosity and the kreb's permeability of the nickel standard were measured 2 times at a confining pressure of 1000 psi.
The porosity and permeability test data of the nickel standard are shown in table 7.
Table 7 test results for nickel standards made in example 7
Figure BDA0002348183190000131
Example 8
Nickel powder with the average particle size of 2 micrometers is used as a raw material to manufacture a cylindrical standard product with the diameter of 2.5cm, the height of 4.25cm and the compaction rate of 61.2%, and porosity and permeability tests are carried out by utilizing a CMS-300 type overburden pore infiltration tester of American rock core company.
The manufacturing process of the metal standard product is as follows:
1) calculating the weight M of the required nickel powder according to the formula (1)Nickel (II)115 g;
2) adding 115g of nickel powder into a mould, placing the mould on a press, releasing pressure when the nickel powder in the mould is pressed to the standard product with the height of 4.25cm, and taking out to obtain a mould pressing semi-finished product;
3) and (3) putting the mould pressing semi-finished product into a vacuum sintering furnace, sintering for 1 hour at 900 ℃, cooling and taking out to obtain the nickel standard product.
Testing of nickel standards: the porosity and the krcker permeability of the nickel standard prepared in the embodiment are repeatedly measured by adopting a porosity calibration standard of a CMS-300 type overburden pore permeability tester of American rock core company.
The specific test procedures and conditions were as follows:
a) measuring the diameter and the height of the porosity calibration standard nickel standard by using a vernier caliper, and measuring the average value for 5 times respectively;
b) after the instrument was debugged, the porosity and the kreb's permeability of the nickel standard were measured 2 times at a confining pressure of 1000 psi.
The porosity and permeability test data of the nickel standard are shown in the table 8.
Table 8 test results for nickel standards made in example 8
Figure BDA0002348183190000132
Figure BDA0002348183190000141
Example 9
306 stainless steel powder with the grain diameter of 48 mu m is used as a raw material to manufacture a cylindrical standard product with the diameter of 2.47cm, the height of 4.40cm and the compaction rate of 76 percent, and a CMS-300 type overburden porosity tester of American rock core company is utilized to carry out porosity and permeability repeatability tests.
The manufacturing process of the metal standard product is as follows:
1) calculating the required weight M of the stainless steel powder according to the above formula (1)Stainless steelIs 128 g;
2) adding 130g of stainless steel powder into a mold, placing on a press, releasing pressure when the stainless steel powder in the mold is pressed to a standard substance height of 4.4cm, and taking out to obtain a semi-finished product for mold pressing;
3) and (3) putting the mould pressing semi-finished product into a vacuum sintering furnace, sintering for 1 hour at 1100 ℃, cooling and taking out to obtain the stainless steel standard product.
Testing of stainless steel standards: the porosity and permeability of the stainless steel standard prepared in this example were repeatedly measured using a porosity calibration standard of a model CMS-300 overburden pore permeability tester from american core corporation. The specific test procedures and conditions were as follows:
c) measuring the diameter and the height of a porosity calibration standard stainless steel standard by using a vernier caliper, and respectively measuring for 5 times to obtain an average value;
d) opening nitrogen and hydrogen gas cylinders, instruments and control software in a computer to detect the gas leakage of the instruments;
e) and inputting the diameters and the heights of the porosity calibration standard and the stainless steel standard, sequentially putting the porosity calibration standard and the stainless steel standard into a sample cell, and measuring the porosity and the permeability of the stainless steel standard under the confining pressure of 1000 psi. The porosity calibration standard is a porosity calibration standard carried by an instrument of American core company, and can only be used for inspecting a porosity test value so as to judge whether the instrument is in a good state or not.
The stainless steel standard product prepared by the embodiment has good repeatability and can be repeatedly measured for at least more than 50 times. The data from 6 replicates of the stainless steel standards made in this example were randomly sampled as shown in table 9 below.
Table 9 test results for stainless steel standards made in example 9
Figure BDA0002348183190000151
Example 10
306 stainless steel powder with the average grain diameter of 48 mu m is used as a raw material to prepare a cylindrical standard product with the diameter of 2.5cm, the height of 4.0cm and the compaction rate of 80 percent, and a CMS-300 type overburden permeability tester of American rock core company is used for carrying out porosity and permeability tests.
The manufacturing process of the metal standard product is as follows:
1) calculating the required weight M of the stainless steel powder according to the above formula (1)Stainless steel127 g;
2) adding 127.8g of stainless steel powder into a mold, placing on a press, releasing pressure when the stainless steel powder in the mold is pressed to the standard substance height of 4.0cm, and taking out to obtain a semi-finished product for mold pressing;
3) and (3) putting the mould pressing semi-finished product into a vacuum sintering furnace, sintering for 1 hour at 1100 ℃, cooling and taking out to obtain the stainless steel standard product.
Testing of stainless steel standards: the porosity and permeability of the stainless steel standard prepared in this example were repeatedly measured using a porosity calibration standard of a model CMS-300 overburden pore permeability tester from american core corporation. The specific test procedures and conditions were as follows:
a) measuring the diameter and the height of a porosity calibration standard stainless steel standard by using a vernier caliper, and respectively measuring for 5 times to obtain an average value;
b) opening nitrogen and hydrogen gas cylinders, instruments and control software in a computer to detect the gas leakage of the instruments;
c) and inputting the diameters and the heights of the porosity calibration standard and the stainless steel standard, sequentially putting the porosity calibration standard and the stainless steel standard into a sample cell, and measuring the porosity and the permeability of the stainless steel standard under the confining pressure of 1000 psi. The porosity calibration standard is a porosity calibration standard carried by an instrument of American core company, and can only be used for inspecting a porosity test value so as to judge whether the instrument is in a good state or not.
The stainless steel standard product prepared by the embodiment has good repeatability and can be repeatedly measured for at least more than 50 times. The following table 10 randomly extracts 3 replicates of the stainless steel standards made in this example.
Table 10 test results for stainless steel standards made in example 10
Serial number Height (cm) Diameter (cm) Porosity (%) Permeability (md)
1 4.0364 2.5082 18.14 4.11
2 4.0364 2.5082 17.86 4.13
3 4.0364 2.5082 17.72 3.95
Example 11
306 stainless steel powder with the particle size of 60-120 mu m is used as a raw material, the raw material is sintered for 1 hour at 1300 ℃, a cylindrical standard product with the diameter of 2.5cm, the height of 4.5cm and the compaction rate of 85 percent is manufactured, and a porosity and permeability test is carried out by utilizing a CMS-300 type overburden porosity tester of the American rock core company.
The manufacturing process of the metal standard product is as follows:
1) calculating the required weight M of the stainless steel powder according to the above formula (1)Stainless steel152 g;
2) adding 152g of stainless steel powder into a mold, placing on a press, releasing pressure when the stainless steel powder in the mold is pressed to a standard substance height of 4.5cm, and taking out to obtain a semi-finished product for mold pressing;
3) and (3) placing the die pressing semi-finished product into a vacuum sintering furnace, sintering for 1 hour at 1300 ℃, cooling and taking out to obtain the stainless steel standard product.
Testing of stainless steel standards: the porosity and permeability of the stainless steel standard prepared in this example were measured using a model CMS-300 overburden pore permeability tester from core americas. The specific test procedures and conditions were as follows:
a) measuring the diameter and the height of a porosity calibration standard stainless steel standard by using a vernier caliper, and respectively measuring for 5 times to obtain an average value;
b) after the instrument was debugged, the stainless steel standards were measured for porosity and kruse permeability 2 times at a confining pressure of 1000 psi.
The experimental data of the stainless steel standard prepared in this example are shown in table 11 below.
Table 11 test results for stainless steel standards made in example 11
Serial number Height (cm) Diameter (cm) Porosity (%) Permeability (md)
1 4.515 2.507 9.45 2.54
2 4.515 2.507 9.43 2.49
Example 12
A306 stainless steel powder with the particle size of 25 mu m is used as a raw material to prepare a cylindrical standard product with the diameter of 2.5cm, the height of 4.0cm and the compaction rate of 85 percent, the cylindrical standard product is sintered for 1 hour at 1100 ℃, and a CMS-300 type overburden pressure pore infiltration tester of American rock core company is used for testing the porosity and the permeability.
The manufacturing process of the metal standard product is as follows:
1) calculating the required weight M of the stainless steel powder according to the above formula (1)Stainless steel133 g;
2) adding 133g of stainless steel powder into a mold, placing on a press, releasing pressure when the stainless steel powder in the mold is pressed to a standard substance height of 4.0cm, and taking out to obtain a mold pressing semi-finished product;
3) and (3) putting the mould pressing semi-finished product into a vacuum sintering furnace, sintering for 1 hour at 1100 ℃, cooling and taking out to obtain the stainless steel standard product.
Testing of stainless steel standards: the porosity and permeability of the stainless steel standard prepared in this example were measured using a model CMS-300 overburden pore permeability tester from core americas. The specific test procedures and conditions were as follows:
c) measuring the diameter and the height of a porosity calibration standard stainless steel standard by using a vernier caliper, and respectively measuring for 5 times to obtain an average value;
d) after the instrument was debugged, the stainless steel standards were measured for porosity and kruse permeability 2 times at a confining pressure of 1000 psi.
The experimental data of the stainless steel standard prepared in this example are shown in table 12 below.
Table 12 test results for stainless steel standards made in example 12
Serial number Height (cm) Diameter (cm) Porosity (%) Permeability (md)
1 4.098 2.505 9.67 2.75
2 4.098 2.505 9.65 2.72
Example 13
A306 stainless steel powder with the particle size of 25 mu m is used as a raw material to prepare a cylindrical standard product with the diameter of 2.5cm, the height of 4.5cm and the compaction rate of 61 percent, and a CMS-300 type overburden pore infiltration tester of American rock core company is utilized to carry out porosity and permeability tests.
The manufacturing process of the metal standard product is as follows:
1) calculating the required weight m of the stainless steel powder according to the above formula (1)Stainless steelIs 110 g;
2) adding 108g of stainless steel powder into a mold, placing on a press, releasing pressure when the stainless steel powder in the mold is pressed to a standard substance height of 4.0cm, and taking out to obtain a mold pressing semi-finished product;
3) and (3) putting the mould pressing semi-finished product into a vacuum sintering furnace, sintering for 1 hour at 1100 ℃, cooling and taking out to obtain the stainless steel standard product.
Testing of stainless steel standards: the porosity and permeability of the stainless steel standard prepared in this example were measured using a model CMS-300 overburden pore permeability tester from core americas. The specific test procedures and conditions were as follows:
e) measuring the diameter and the height of a porosity calibration standard stainless steel standard by using a vernier caliper, and respectively measuring for 5 times to obtain an average value;
f) after the instrument was debugged, the stainless steel standards were measured for porosity and kruse permeability 2 times at a confining pressure of 1000 psi.
The experimental data of the stainless steel standard prepared in this example are shown in table 13 below.
Table 13 test results for stainless steel standards made in example 13
Serial number Height (cm) Diameter (cm) Porosity (%) Permeability (md)
1 4.512 2.507 35.05 62.33
2 4.512 2.507 35.07 62.15
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive various equivalent modifications or substitutions within the technical scope of the present invention, and these modifications or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (10)

1. A method of preparing a metal standard for use in permeability testing, comprising:
determining a first weight of the metal powder according to the compaction rate, the size and the metal density of the standard substance to be prepared, wherein the first weight is the weight of the standard substance to be prepared;
placing the metal powder with the first weight in a prefabricated mould, and carrying out mould pressing to obtain a mould pressing semi-finished product;
and sintering the mould pressing semi-finished product at a first temperature for a first time to obtain the metal standard product.
2. The method of claim 1, wherein the metal standard is a stainless steel standard or a nickel standard.
3. The method of claim 1, wherein the metal powder is stainless steel powder, and the stainless steel powder has a particle size of 25 μm to 120 μm.
4. The method of claim 3, wherein the first temperature is 950 ℃ to 1300 ℃.
5. The method according to claim 1, wherein the metal powder is nickel powder, and a particle diameter of the nickel powder is 1 μm to 48 μm.
6. The method of claim 4, wherein the first temperature is in a range of 800 ℃ to 950 ℃.
7. The method of preparing a metal standard according to claim 1, wherein the standard is cylindrical, and the first weight is calculated by the following formula:
Mmetal＝π(dSign board/2)2hSign boardΦSign boardρSign board
Wherein M isMetalIs a first weight, phiSign boardThe compaction rate of the standard product is obtained; dSign boardIs the diameter of the standard, hSign boardIs a predetermined size; rhoSign boardIs the density of the metal.
8. The method of manufacturing a metal standard according to claim 1, wherein the standard is a rectangular parallelepiped, and the first weight is calculated by the following formula:
Mmetal＝lSign boardwSign boardhSign boardΦSign boardρSign board
Wherein M isMetalIs a first weight, phiSign boardThe compaction rate of the standard to be prepared; lSign boardLength of standard to be prepared, wSign boardIs the width of the standard, hSign boardIs the height of the standard to be prepared; rhoSign boardIs the density of the metal.
9. The method of claim 1, wherein the first time period is 0.5h to 4 h.
10. The method of claim 1, wherein the sintering is performed under vacuum.
CN201911404163.5A 2019-12-31 2019-12-31 Preparation method of metal standard substance Pending CN111141654A (en)

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