CN111504801A - Device and method for performing stress corrosion experiment in high-temperature liquid phase corrosion environment - Google Patents
Device and method for performing stress corrosion experiment in high-temperature liquid phase corrosion environment Download PDFInfo
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- 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
- G01N3/18—Performing tests at high or low temperatures
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G—PHYSICS
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- G01N2203/0001—Type of application of the stress
- G01N2203/0003—Steady
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- 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
- G01N2203/0017—Tensile
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- 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
- G01N2203/022—Environment of the test
- G01N2203/0222—Temperature
- G01N2203/0226—High temperature; Heating means
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- 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
- G01N2203/022—Environment of the test
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Abstract
The invention discloses a device for carrying out a stress corrosion experiment in a high-temperature liquid phase corrosion environment, which comprises a universal testing machine and a stress corrosion experiment box clamped by a clamp holder with the universal testing machine, wherein the stress corrosion experiment box comprises a double-layer glass cylinder and an upper plug head and a lower plug head which are hermetically connected with the double-layer glass cylinder; in addition, the invention also discloses a stress corrosion experiment method, which is to load a stress corrosion experiment sample and corrosive liquid into a stress corrosion experiment box by using a universal testing machine to obtain the loaded experiment sample and data. The invention avoids the contact of the universal testing machine and corrosive liquid, realizes the stress corrosion experiment in a high-temperature liquid phase corrosion environment, and can realize accurate loading and real-time observation.
Description
Technical Field
The invention belongs to the technical field of stress corrosion performance testing, and particularly relates to a device and a method for performing a stress corrosion experiment in a high-temperature liquid phase corrosion environment.
Background
Metal corrosion caused by the simultaneous action of corrosive environment and static tensile stress often leads to the formation of cracks, resulting in a significant reduction in the load-bearing properties of the metal structure.
The methods used for assessing the stress corrosion properties of metals are diverse and in some cases each method has its own particular advantages, and prior to planning the stress corrosion experiments, it is necessary to determine which method of experiment is appropriate, depending on the purpose of the experiment and the information required, some experiments are merely valuable to plant engineers and attempt to repeat the conditions of the service as much as possible, simpler experimental methods such as U-bend experiments, C-ring experiments may be selected, and conversely, when it is necessary to carry out an in-depth analysis of the stress corrosion cracking mechanism, such as critical stress analysis, crack propagation rate analysis, relatively complicated experimental procedures must be used, the usual method being constant stress tension and constant strain rate 1 × 10-4s-1～1×10-6s-1Slow strain rate tensile experiments.
At present, for the stress corrosion experiment method of the metal material in the high temperature liquid phase environment, mainly relatively simple U-shaped bending experiment and C-shaped ring experiment, refer to GB/T105-6-1788 "experimental method of stress corrosion of iron-chromium-nickel alloy in high temperature water", but such method only provides a rough evaluation scheme of stress corrosion performance, which cannot realize precise control of stress, and further cannot obtain critical performance indexes of the metal material such as critical stress, crack propagation rate and the like under the stress corrosion condition, and the reference of the experiment result is far inferior to the slow strain rate tensile experiment, in addition, for the stress corrosion experiment method in the high temperature liquid phase environment, the liquid phase environment is mostly water and salt solution, and for the stress corrosion experiment test of the metal material in the corrosive liquid phase (such as strong acid and strong base), there is no mature test method at present, in addition, although the prior art has used a method and an apparatus for performing a stress corrosion test using a universal tester, the apparatus and the method used in the prior art are not suitable for testing the stress corrosion performance in a high-temperature liquid phase corrosive environment.
People hope to obtain a device and a method for realizing the stress corrosion experiment of the metal material in the high-temperature liquid phase corrosion environment.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a device for performing a stress corrosion experiment in a high-temperature liquid phase corrosion environment, aiming at the defects of the prior art, the device avoids a universal testing machine from contacting with corrosive liquid, and realizes the stress corrosion experiment in the high-temperature liquid phase corrosion environment; the invention also provides a method for carrying out stress corrosion experiments in the high-temperature liquid phase corrosion environment, which can provide various loading modes, realize accurate control on loading, realize real-time observation and output key data such as stress-strain curves and the like.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a device for carrying out stress corrosion experiments in a high-temperature liquid phase corrosion environment is characterized by comprising a universal testing machine and a stress corrosion experiment box connected with the universal testing machine through a clamp holder in a clamping manner, wherein the universal testing machine comprises a workbench and two stand columns respectively arranged at two ends of a table top of the workbench, the top ends of the two stand columns are respectively connected with two ends of a fixed cross beam, a movable cross beam used for loading a stress corrosion experiment sample is arranged between the two stand columns, an upper clamp head connected with the upper end of the stress corrosion experiment sample is arranged on the movable cross beam, a lower clamp head connected with the lower end of the stress corrosion experiment sample is arranged on the workbench, the clamp holder comprises a first clamp holder and a second clamp holder which are symmetrically arranged on the two stand columns, and the clamping ends of the first clamp holder and the second clamp holder are symmetrically clamped on the stress corrosion experiment box, the stress corrosion experiment box comprises a double-layer glass cylinder for containing corrosive liquid, an upper plug head connected with the upper end of the double-layer glass cylinder in a sealing manner, and a lower plug head connected with the lower end of the double-layer glass cylinder in a sealing manner, the side wall of the double-layer glass cylinder is of a hollow structure, a heating medium outlet communicated with the hollow structure is formed in the outer wall of the upper end of the double-layer glass cylinder, a heating medium inlet communicated with the hollow structure is formed in the outer wall of the lower end of the double-layer glass cylinder, the center of the upper plug head and the center of the lower plug head respectively correspond to an upper plug head sample through hole and a lower plug head sample through hole which are used for supplying power corrosion experiment samples to pass and are connected with the stress corrosion experiment samples in a sealing manner, a condensing device through hole is formed in the upper plug head, and the condensing.
The device for carrying out the stress corrosion experiment in the high-temperature liquid phase corrosion environment is characterized in that the length of the stress corrosion experiment sample is 50-100 mm longer than the height of the stress corrosion experiment box. In the invention, if the length of the stress corrosion test sample is too short, the stress corrosion test sample cannot be assembled with the upper chuck and the lower chuck of the universal testing machine, and if the length of the stress corrosion test sample is too long, the sample is inconvenient to assemble and disassemble and material waste is caused.
The device for carrying out the stress corrosion experiment in the high-temperature liquid phase corrosion environment is characterized in that a thermocouple is arranged on the inner wall of the double-layer glass cylinder, and a display instrument connected with the thermocouple is arranged on the outer wall of the double-layer glass cylinder. The invention monitors the temperature in the stress corrosion experiment box in real time, so that the experiment process is more accurate, and the experiment precision is increased.
In addition, the invention also provides a method for carrying out stress corrosion experiments in a high-temperature liquid phase corrosion environment, which is characterized by comprising the following steps:
step one, processing a metal material to be tested to obtain a stress corrosion experiment sample;
step two, loading the stress corrosion experiment sample and corrosive liquid obtained in the step one into a stress corrosion experiment box, and then respectively clamping and fixing the stress corrosion experiment sample extending out of two ends of the stress corrosion experiment box in an upper chuck and a lower chuck of a universal testing machine;
and step three, introducing a heating medium into the side wall of the double-layer glass cylinder of the stress corrosion experiment box, heating the corrosive liquid, loading the stress corrosion experiment sample when the temperature and the corrosion condition borne by the stress corrosion experiment sample meet the experiment requirements, and stopping the experiment until the stress corrosion experiment sample is broken or the loading time of the experiment requirements is reached to obtain the loaded experiment sample and the experiment data.
The method is characterized in that the stress corrosion test sample in the step one is a test rod or a test plate. The experimental bar or the experimental plate is a sample form which is most widely applied to metal materials, and can be used for testing the mechanical properties of metal materials in different states such as cast ingots, forgings and the like and in different specifications and sizes; in addition, the experiment board compares in the experiment stick, can be used for the sample of the sheet metal material that specific direction size is less than 5mm to cut out, has compensatied the not enough that the experiment stick can't take a sample to the sheet metal material.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, through the universal testing machine and the stress corrosion experiment box, the chuck of the universal testing machine is prevented from being corroded, the experiment device is protected, the stress corrosion experiment is realized in a high-temperature liquid phase corrosion environment, the accurately controllable stress corrosion experiment such as constant stress stretching, slow strain rate stretching and the like can be realized, the stress corrosion experiment sample can be loaded and fractured, the timing loading can be realized, the key data such as a stress-strain curve, critical stress, a critical stress intensity factor, a crack propagation rate, crack initiation time, failure time and the like can be output, and the defect that the stress corrosion experiment is not carried out in the high-temperature liquid phase corrosion environment in the prior art is solved.
2. The stress corrosion experiment box adopts the double-layer glass cylinder, meets the requirements of the stress corrosion experiment box on high temperature and corrosion environment, an experimenter can observe the state of a sample in test in real time during an experiment, and key data such as the surface appearance of the sample to be tested, a crack propagation path, a crack propagation rate and the like can be acquired in real time by the aid of a camera.
3. According to the invention, the heating medium is introduced between the side walls of the double-layer glass cylinder through the circulating pump, and the type of corrosive liquid is adjusted, so that the temperature and corrosion conditions borne by a stress corrosion experimental sample meet experimental requirements, a required high-temperature and corrosion environment is provided for the experiment, and the stress corrosion experiment in a high-temperature liquid phase corrosion environment is realized; the area where the stress corrosion experiment sample is tested is completely immersed in the corrosive solution, so that the whole area where the stress corrosion experiment sample is tested is in the same high-temperature liquid phase corrosion environment, and the accuracy of the experiment is improved.
4. According to the invention, the metal material to be tested is processed into the stress corrosion experiment sample, so that two ends of the stress corrosion experiment sample can extend out of the corrosion experiment box, the connection between the stress corrosion experiment sample and the upper chuck and the lower chuck is satisfied, the connection between the stress corrosion experiment sample and the universal testing machine is stable by processing the threads and the through holes on the stress corrosion experiment sample, the metal material to be tested is processed into the experiment plate, the defect that the experiment rod cannot sample a sheet material is overcome, the stress corrosion experiment can be carried out on materials in various shapes, and the applicability of the stress corrosion experiment is widened.
5. The upper plug head is provided with the condensing device for condensing corrosive steam generated in the heating process, so that the corrosive steam is prevented from entering the atmosphere, the advantage of environmental friendliness is achieved, and the safety of an experiment is improved; the invention is provided with the thermocouple and the display instrument connected with the thermocouple, and monitors the temperature in the stress corrosion experiment box in real time, so that the experiment process is more accurate, and the experiment precision is increased.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic diagram of the structure of the apparatus of the present invention.
FIG. 2 is a schematic view showing the connection relationship between the clamper of the present invention and a stress corrosion test chamber.
Fig. 3 is a schematic structural view of the upper plug head of the present invention.
Fig. 4 is a schematic structural view of the lower plug head of the present invention.
FIG. 5 is a schematic structural diagram of a test bar before corrosion test in example 2 of the present invention.
FIG. 6 is an SEM image of a test rod obtained after loading in example 2 of the present invention.
FIG. 7 is an SEM image of the fracture surface of the experimental rod obtained after loading in example 2 of the present invention.
FIG. 8 is a stress-strain diagram obtained in example 2 of the present invention.
FIG. 9 is a top view of the test plate before corrosion experiments in examples 3 and 4 of the present invention.
FIG. 10 is a front view of a test plate before corrosion tests in examples 3 and 4 of the present invention.
Description of reference numerals:
1-stress corrosion experiment box; 1-double glass cylinder; 1-1-1-heating medium outlet;
1-1-2-heating medium inlet; 1-2-upper plug head; 1-2-1-upper plug sample through hole;
1-2-through holes of the condensing unit; 1-3-lower plug; 1-3-1-lower plug sample through hole;
1-4-a condensing unit; 2-universal testing machine; 2-1-moving the beam;
2-a workbench; 2-3-upright column; 2-4, an upper chuck;
2-5-lower chuck; 2-6-fixed beam; 3-stress corrosion test sample;
3-1-lower clamping section; 3-2-short connecting segment; 3-bar gauge length section;
3-4-long connecting section; 3-5-upper clamping section; 3-6-short clamping section;
3-7-plate gauge length section; 3-8-long clamping section; 4-1 — a first gripper;
4-2 — a second gripper; 5-corrosive liquid.
Detailed Description
An apparatus for performing a stress corrosion test in a high temperature liquid phase corrosive environment according to the present invention is described in detail in example 1.
Example 1
As shown in fig. 1, fig. 2, fig. 3 and fig. 4, the device for performing stress corrosion experiments in a high temperature liquid phase corrosion environment of the present embodiment includes a universal testing machine 2 and a stress corrosion experiment box 1 connected to the universal testing machine 2 by being clamped by a clamp, the universal testing machine 2 includes a workbench 2-2 and two columns 2-3 respectively disposed at two ends of a table top of the workbench 2-2, top ends of the two columns 2-3 are respectively connected to two ends of a fixed beam 2-6, a movable beam 2-1 for loading a stress corrosion experiment sample 3 is disposed between the two columns 2-3, an upper chuck 2-4 connected to an upper end of the stress corrosion experiment sample 3 is disposed on the movable beam 2-1, a lower chuck 2-5 connected to a lower end of the stress corrosion experiment sample 3 is disposed on the workbench 2-2, the clamp comprises a first clamp 4-1 and a second clamp 4-2 which are symmetrically arranged on two upright posts 2-3, the clamping ends of the first clamp 4-1 and the second clamp 4-2 are symmetrically clamped on a stress corrosion experiment box 1, the stress corrosion experiment box 1 comprises a double-layer glass cylinder 1-1 for containing corrosive liquid 5, an upper plug head 1-2 which is hermetically connected with the upper end of the double-layer glass cylinder 1-1 and a lower plug head 1-3 which is hermetically connected with the lower end of the double-layer glass cylinder 1-1, the side wall of the double-layer glass cylinder 1-1 is of a hollow structure, a heating medium outlet 1-1-1 which is communicated with the hollow structure is arranged on the outer wall of the upper end of the double-layer glass cylinder 1-1, and a heating medium inlet which is communicated with the hollow structure is arranged on the outer wall of the lower end of the double-layer glass cylinder 1-1 The device comprises a port 1-1-2, the centers of an upper plug head 1-2 and a lower plug head 1-3 are respectively and correspondingly provided with an upper plug head sample through hole 1-2-1 and a lower plug head sample through hole 1-3-1 which are used for supplying a force corrosion experiment sample 3 to penetrate and are in sealing connection with the stress corrosion experiment sample 3, the upper plug head 1-2 is provided with a condensing device through hole 1-2-2, and a condensing device 1-4 penetrates through the condensing device through hole 1-2-2 and is in sealing connection with the upper plug head 1-2.
In the embodiment, by arranging the universal testing machine 2, the clamp and the stress corrosion experiment box 1, during actual use, firstly, the clamp is used for clamping the stress corrosion experiment box 1, secondly, the stress corrosion experiment sample 3 is connected with the stress corrosion experiment box 1, corrosive liquid 5 is introduced into the stress corrosion experiment box 1, afterwards, the stress corrosion experiment sample 3 is connected with the universal testing machine 2, then, the corrosive liquid 5 is heated, then the universal testing machine 2 is used for loading the stress corrosion experiment sample 3, the upper clamp 2-4 and the lower clamp 2-5 of the universal testing machine 2 are prevented from extending into the stress corrosion experiment box 1, the upper clamp 2-4 and the lower clamp 2-5 of the universal testing machine 2 are prevented from being corroded, the stress corrosion experiment sample 3 and the upper clamp 2-4 and the lower clamp 2-5 of the universal testing machine 2 form electrochemical corrosion in the corrosive liquid 5, the experimental device is protected, the stress corrosion experiment in the high-temperature liquid phase corrosion environment is realized, the accurate controllable stress corrosion experiment such as constant stress stretching, slow strain rate stretching and the like can be realized, the stress corrosion experiment sample 3 can be loaded and broken, the timing loading can also be realized, the critical data such as a stress strain curve, critical stress, a critical stress intensity factor, a crack propagation rate, crack leading time, failure time and the like are output, and the defect that the stress corrosion experiment is not carried out in the high-temperature liquid phase corrosion environment in the prior art is overcome.
In the embodiment, the universal testing machine 2 is provided with a movable beam 2-1, a workbench 2-2, two upright posts 2-3 and a beam 2-6, the movable beam 2-1 is provided with an upper chuck 2-4 connected with the upper end of a stress corrosion experimental sample 3, the workbench 2-2 is provided with a lower chuck 2-5 connected with the lower end of the stress corrosion experimental sample 3, when in actual use, the upper chuck 2-4 and the lower chuck 2-5 can be fixedly connected with the stress corrosion experimental sample 3, so that the stress corrosion experimental sample 3 is connected with the universal testing machine 2, the stress corrosion experimental sample 3 is stably fixed on the universal testing machine 2, the connection is reliable, the stress corrosion experimental sample 3 can be loaded in various modes by adopting the universal testing machine 2, and the experiment applicability is improved.
In the embodiment, the clamp holder comprises a first clamp holder 4-1 and a second clamp holder 4-2 which are symmetrically arranged on two upright posts 2-3, and when the clamp holder is actually used, the stress corrosion experiment box 1 is fixedly connected through the clamp holder, so that the stress corrosion experiment box 1 is stably fixed on the universal testing machine 2, and the connection is reliable.
In the embodiment, the stress corrosion experiment box 1 comprises a double-layer glass cylinder 1-1 for containing corrosive liquid 5, an upper plug head 1-2 connected with the upper end of the double-layer glass cylinder 1-1 in a sealing way and a lower plug head 1-3 connected with the lower end of the double-layer glass cylinder 1-1 in a sealing way, when in actual use, glass is used as a material, the stress corrosion experiment box has the advantages of high temperature resistance, corrosion resistance and good heat conduction effect, meets the requirements of the stress corrosion experiment box on high temperature and corrosion environment, is colorless and transparent, can be used for an experimenter to observe the state of a stress corrosion experiment sample 3 in a test in real time during an experiment, can also realize the real-time acquisition of key data such as the surface appearance, a crack propagation path, a crack propagation rate and the like of the stress corrosion experiment sample 3 in the test by means of a camera, and avoids the corrosive liquid 5 from flowing out of the stress corrosion experiment box 1, the safety and the reliability of the experiment are improved.
In this embodiment, the side wall of the double-layer glass cylinder 1-1 is of a hollow structure, the outer wall of the upper end of the double-layer glass cylinder 1-1 is provided with a heating medium outlet 1-1-1 communicated with the hollow structure, and the outer wall of the lower end of the double-layer glass cylinder 1-1 is provided with a heating medium inlet 1-1-2 communicated with the hollow structure, so that in practical use, a heating medium can be continuously introduced into the double-layer glass cylinder 1-1 through the heating medium inlet 1-1-2 and the heating medium outlet 1-1-1, and the corrosive liquid 5 contained in the double-layer glass cylinder 1-1 can be heated, thereby uniformly heating the corrosive liquid 5 in the stress corrosion experiment box 1, and providing a required high-temperature environment for the experiment.
In the embodiment, the middle positions of the upper plug head 1-2 and the lower plug head 1-3 are respectively provided with an upper plug head sample through hole 1-2-1 and a lower plug head sample through hole 1-3-1 which are used for a force corrosion experiment sample 3 to penetrate and are hermetically connected with a stress corrosion experiment sample 3, can lead the stress corrosion experiment sample 3 to pass through the stress corrosion experiment box 1, prevents the upper chuck 2-4 and the lower chuck 2-5 of the universal tester 2 from being corroded, prevents the stress corrosion experiment sample 3 and the upper chuck 2-4 and the lower chuck 2-5 of the universal tester 2 from forming electrochemical corrosion in corrosive liquid 5, improves the accuracy of the experiment, the corrosive liquid 5 is prevented from flowing out of the stress corrosion experiment box 1 through sealing connection, and the safety and the reliability of the experiment are improved.
In the embodiment, the upper plug head 1-2 is provided with the condensing device through hole 1-2-2, the condensing device 1-4 penetrates through the condensing device through hole 1-2-2 to be hermetically connected with the upper plug head 1-2, when in actual use, the upper plug head 1-2 is provided with the condensing device through hole 1-2-2, so that the interior of the stress corrosion experiment box 1 is communicated with the atmosphere, the defect of danger caused by overlarge internal pressure of the stress corrosion experiment box 1 is avoided, the condensing device 1-4 is used for condensing corrosive steam generated in the heating process, the corrosive steam is prevented from entering the atmosphere, the environment-friendly advantage is achieved, the safety of the experiment is improved, the leakage of corrosive steam from the stress corrosion experiment box 1 is avoided through the sealing connection, and the safety and the reliability of the experiment are improved.
In this embodiment, the length of the stress corrosion test sample 3 is 50mm to 100mm longer than the height of the stress corrosion test box 1, and preferably 50mm, 65mm, or 100 mm.
The inner wall of the double-layer glass cylinder 1-1 is provided with a K-type thermocouple, and the outer wall of the double-layer glass cylinder 1-1 is provided with an HD 830-type digital temperature display connected with the K-type thermocouple.
The method of performing a stress corrosion test in a high temperature liquid phase corrosive environment according to the present invention is described in detail in examples 2 to 4.
Example 2
The embodiment comprises the following steps:
step one, processing a zirconium alloy metal rod to obtain an experimental rod, wherein the structure and the size of the experimental rod are shown in figure 5;
step two, clamping and connecting a first clamp 4-1 and a second clamp 4-2 arranged on an upright post 2-3 of a universal testing machine 2 with the middle part of a double-layer glass cylinder 1-1, hermetically connecting the lower end of the double-layer glass cylinder 1-1 with a lower plug 1-3, inserting a short connecting section 3-2 of the experimental rod obtained in the step one into a lower plug sample through hole 1-3-1 of the lower plug 1-3 and keeping sealing, injecting a nitric acid solution with the mass concentration of 6 mol/L into the double-layer glass cylinder 1-1, keeping a rod gauge length section 3-3 of the experimental rod completely immersed in the nitric acid solution, hermetically connecting the upper end of the double-layer glass cylinder 1-1 and an upper plug 1-2, hermetically connecting a long connecting section 3-4 of the experimental rod with an upper plug sample through hole 1-2-1 of the upper plug 1-2, inserting a chuck into a through hole 1-2-2 of a condensing device through hole 1-2, and fixing the long connecting section 3-4 of the experimental rod with the upper plug sample through hole 1-2, and fixing the lower plug of the experimental rod in a clamping tube, wherein the lower plug 3-2 clamping tube of the experimental rod extends out of the universal testing machine through a clamping device through hole 5;
step three, continuously enabling methyl silicone oil heated to 120 ℃ by the constant temperature bath to enter the side wall of the double-layer glass cylinder 1-1 through the heating medium inlet 1-1-2 and flow out of the heating medium outlet 1-1-1 by adopting a circulating pump so as to perform constant temperature heating on the nitric acid solution contained in the double-layer glass cylinder 1-1, starting the universal testing machine 2 to perform slow strain rate stretching on the experimental rod after the nitric acid solution in the stress corrosion experimental box 1 is boiled, wherein the strain rate is 1 × 10-4s-1And stopping the experiment after the experimental rod subjected to slow strain rate stretching breaks to obtain the loaded experimental rod and experimental data.
FIG. 5 is a schematic structural diagram of an experimental rod before corrosion test in this embodiment, as can be seen from FIG. 5, the experimental rod before corrosion test has a length of 180mm, and the experimental rod before corrosion test sequentially comprises, from left to right, a lower clamping section 3-1 with a thread having a length of 20mm and a diameter of 6mm, a short connecting section 3-2 with a length of 45mm and a diameter of 8mm, a rod gauge section 3-3 with a length of 20mm and a diameter of 3mm, a long connecting section 3-4 with a length of 75mm and a diameter of 8mm, an upper clamping section 3-5 with a thread having a length of 20mm and a diameter of 6mm, wherein a junction between the short connecting section 3-2 and the lower clamping section 3-1 is chamfered at an angle of 1 × 45 °, a junction between the long connecting section 3-4 and the upper clamping section 3-5 is chamfered at an angle of 1 × 45 °, a junction between the short connecting section 3-2 and the rod gauge section 3-3 is chamfered at an angle of R5, and a junction between the long connecting section 3-4 and the rod gauge section 5.
Fig. 6 is an SEM image of the test rod obtained after loading in the present example, and it can be seen from fig. 6 that the test rod used in the present example was fractured in the stress corrosion test performed in the high temperature liquid phase corrosion environment.
FIG. 7 is an SEM image of the fracture surface of the experimental rod obtained after loading in this example, and it can be seen from FIG. 7 that the experimental rod used in this example is stress corrosion cracked in a high temperature liquid phase corrosion environment in a brittle intergranular fracture mode.
Fig. 8 is a stress-strain graph obtained in this example, and it can be seen from fig. 8 that the experimental bar used in this example did not yield, i.e., fracture, significantly in the high temperature liquid phase corrosive environment, consistent with the brittle fracture conclusion drawn in fig. 7.
Example 3
The embodiment comprises the following steps:
step one, processing a 304L stainless steel metal plate to obtain an experimental plate;
step two, clamping and connecting a first clamp 4-1 and a second clamp 4-2 arranged on an upright post 2-3 of a universal testing machine 2 with the middle part of a double-layer glass cylinder 1-1, hermetically connecting the lower end of the double-layer glass cylinder 1-1 with a lower plug head 1-3, inserting a short clamping section 3-6 of the experimental plate obtained in the step one into a lower plug head sample through hole 1-3-1 of the lower plug head 1-3 and keeping sealing, injecting a nitric acid solution with the mass concentration of 8 mol/L into the double-layer glass cylinder 1-1, keeping a plate gauge length section 3-7 of the experimental plate completely immersed in the nitric acid solution, hermetically connecting the upper end of the double-layer glass cylinder 1-1 and an upper plug head 1-2, hermetically connecting a long clamping section 3-8 of the experimental plate with an upper plug head sample through hole 1-2-1 of the upper plug head 1-2, inserting a chuck into a through hole 1-2-2 through hole of a condensing device 1, and fixing the long clamping section 3-2 of the condensing device, which extends out of the condensing device, fixing the long clamping section 3-2 through the short clamping section 3-2 of the universal testing machine, and fixing the short clamping device through hole 3-2 through the short clamping section 3-6 of the lower plug head 3-1-3 of the lower plug head 2;
and step three, continuously enabling the methyl silicone oil heated to 120 ℃ by the constant temperature bath to enter the side wall of the double-layer glass cylinder 1-1 through the heating medium inlet 1-1-2 by adopting a circulating pump and flow out of the heating medium outlet 1-1-1 so as to heat the nitric acid solution in the double-layer glass cylinder 1-1 at constant temperature, starting the universal testing machine 2 to perform constant stress stretching on the experimental plate after the nitric acid solution in the stress corrosion experimental box 1 boils, wherein the constant stress is 150MPa, and stopping the experiment after the experimental plate subjected to constant stress stretching is broken so as to obtain the loaded experimental plate and experimental data.
Fig. 9 is a top view of the experimental plate before corrosion test in this embodiment, and as can be seen from fig. 9, the length of the experimental plate before corrosion test is 195mm, and the experimental plate before corrosion test sequentially comprises from left to right: a short clamping section 3-6 with the length of 68.7mm and the width of 20mm, a long clamping section 3-8 with the length of 40mm and the width of 6mm, a board gauge distance section 3-7 with the length of 86.3mm and the width of 20mm, wherein a through hole with the diameter of 8.1mm is arranged on one surface with the larger area of the short clamping section 3-6, the distance from the axis of the through hole to the end surface of the short clamping section 3-6 is 16mm, the distance from the axis of the through hole to the two surfaces with the smaller area connected with the end surface of the short clamping section 3-6 is 10mm, a through hole with the diameter of 8.1mm is arranged on one surface with the larger area of the long clamping section 3-8, the distance from the axis of the through hole to the end surface of the long clamping section 3-8 is 16mm, the distance from the axis of the through hole to the two surfaces with the smaller area connected with the end surface of the long clamping section 3-8 is 10mm, R5 chamfer is arranged at the connection part of the, r5 chamfer is carried out at the connection part of the long clamping section 3-8 and the plate gauge length section 3-7.
FIG. 10 is a front view of the experimental plate before the corrosion test of this embodiment, and it can be seen from FIG. 10 that the thickness of the experimental plate before the corrosion test of this embodiment is 3 mm.
Example 4
The embodiment comprises the following steps:
step one, processing a 310L stainless steel metal plate to obtain an experimental plate, wherein the structure and the size of the experimental plate are shown in figures 9 and 10;
step two, a first clamp 4-1 and a second clamp 4-2 arranged on an upright post 2-3 of a universal testing machine 2 are connected with the middle part of a double-layer glass cylinder 1-1 in a clamping manner, the lower end of the double-layer glass cylinder 1-1 is connected with a lower plug 1-3 in a sealing manner, a short clamping section 3-6 of the experimental plate obtained in the step one is inserted into a lower plug sample through hole 1-3-1 of the lower plug 1-3 and kept sealed, a sulfuric acid solution with the mass concentration of 8 mol/L is injected into the double-layer glass cylinder 1-1, a plate gauge length section 3-7 of the experimental plate is kept completely immersed in the sulfuric acid solution, the upper end of the double-layer glass cylinder 1-1 and an upper plug 1-2 are connected in a sealing manner, a long clamping section 3-8 of the experimental plate is connected with an upper plug sample through hole 1-2-1 of the upper plug 1-2 in a sealing manner, a through hole 1-2-2 of the condensation device of the upper plug 1-2 is inserted into a through hole 1-2, the condensation device through the short clamping section 3-2, the lower plug 3-2 is fixed in the experimental plate through a cold water clamping section of the experimental plate, and the short clamping section 3-2 of the universal testing machine, and the universal testing machine, the long clamping section extends out of the short clamping device through hole 1-2 through the short clamping section 3-2;
and step three, continuously enabling the methyl silicone oil heated to 107 ℃ by the constant temperature bath to enter the side wall of the double-layer glass cylinder 1-1 through the heating medium inlet 1-1-2 by adopting a circulating pump and flow out of the heating medium outlet 1-1-1 so as to heat the nitric acid solution in the double-layer glass cylinder 1-1 at constant temperature, starting the universal testing machine 2 to perform constant stress stretching on the experimental plate after the temperature of the sulfuric acid solution in the stress corrosion experimental box 1 is 105 ℃, wherein the constant stress is 200MPa, stopping the experiment when the loading time of the experimental plate subjected to constant stress stretching reaches 50 hours, and obtaining the loaded experimental plate and experimental data.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (5)
1. A device for carrying out stress corrosion experiments in a high-temperature liquid phase corrosion environment is characterized by comprising a universal testing machine (2) and a stress corrosion experiment box (1) connected with the universal testing machine (2) in a clamping manner through a clamping device, wherein the universal testing machine (2) comprises a workbench (2-2) and two stand columns (2-3) respectively arranged at two ends of the table top of the workbench (2-2), the top ends of the two stand columns (2-3) are respectively connected with two ends of a fixed cross beam (2-6), a movable cross beam (2-1) used for loading a stress corrosion experiment sample (3) is arranged between the two stand columns (2-3), an upper clamping head (2-4) connected with the upper end of the stress corrosion experiment sample (3) is arranged on the movable cross beam (2-1), the stress corrosion testing device is characterized in that a lower chuck (2-5) connected with the lower end of a stress corrosion test sample (3) is arranged on the workbench (2-2), the clamps comprise a first clamp (4-1) and a second clamp (4-2) which are symmetrically arranged on two upright columns (2-3), the clamping ends of the first clamp (4-1) and the second clamp (4-2) are symmetrically clamped on a stress corrosion testing box (1), the stress corrosion testing box (1) comprises a double-layer glass cylinder (1-1) used for containing corrosive liquid (5), an upper plug head (1-2) hermetically connected with the upper end of the double-layer glass cylinder (1-1) and a lower plug head (1-3) hermetically connected with the lower end of the double-layer glass cylinder (1-1), the side wall of the double-layer glass cylinder (1-1) is of a hollow structure, the outer wall of the upper end of the double-layer glass cylinder (1-1) is provided with a heating medium outlet (1-1-1) communicated with the hollow structure, the outer wall of the lower end of the double-layer glass cylinder (1-1) is provided with a heating medium inlet (1-1-2) communicated with the hollow structure, the centers of the upper plug head (1-2) and the lower plug head (1-3) are respectively and correspondingly provided with an upper plug head sample through hole (1-2-1) and a lower plug head sample through hole (1-3-1) which are used for a stress corrosion experiment sample (3) to pass through and are hermetically connected with the stress corrosion experiment sample (3), the upper plug head (1-2) is provided with a condensing device through hole (1-2-2), and the condensing device (1-4) penetrates through the condensing device through hole (1-2-2) to be hermetically connected with the upper plug head (1-2).
2. The device for carrying out the stress corrosion experiment in the high-temperature liquid phase corrosion environment according to claim 1, wherein the length of the stress corrosion experiment sample (3) is 50mm to 100mm longer than the height of the stress corrosion experiment box (1).
3. The device for carrying out the stress corrosion experiment in the high-temperature liquid phase corrosion environment according to claim 1, wherein a thermocouple is arranged on the inner wall of the double-layer glass cylinder (1-1), and a display instrument connected with the thermocouple is arranged on the outer wall of the double-layer glass cylinder (1-1).
4. A method for performing stress corrosion experiments in a high temperature liquid phase corrosive environment using the apparatus of any one of claims 1-3, the method comprising the steps of:
step one, processing a metal material to be tested to obtain a stress corrosion experiment sample (3);
step two, loading the stress corrosion experiment sample (3) and the corrosive liquid (5) obtained in the step one into a stress corrosion experiment box (1), and then respectively clamping and fixing the stress corrosion experiment sample (3) extending out of two ends of the stress corrosion experiment box (1) in an upper chuck (2-4) and a lower chuck (2-5) of a universal testing machine (2);
and step three, introducing a heating medium into the side wall of the double-layer glass cylinder (1-1) of the stress corrosion experiment box (1), heating the corrosive liquid (5), loading the stress corrosion experiment sample (3) when the temperature and corrosion conditions borne by the stress corrosion experiment sample (3) meet the experiment requirements, and stopping the experiment until the stress corrosion experiment sample (3) is broken or the loading time meeting the experiment requirements is reached, so as to obtain the loaded experiment sample and the experiment data.
5. The method according to claim 4, wherein the stress corrosion test specimen (3) in the first step is a test bar or a test plate.
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