CN108982350B - Electrochemical testing device for high-temperature stress corrosion environment under slow strain rate stretching condition - Google Patents

Electrochemical testing device for high-temperature stress corrosion environment under slow strain rate stretching condition Download PDF

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CN108982350B
CN108982350B CN201811123257.0A CN201811123257A CN108982350B CN 108982350 B CN108982350 B CN 108982350B CN 201811123257 A CN201811123257 A CN 201811123257A CN 108982350 B CN108982350 B CN 108982350B
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temperature
electrolytic cell
temperature resistant
resistant electrolytic
electrochemical
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CN108982350A (en
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杜娟
刘青茂
魏子明
尹元博
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Civil Aviation University of China
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    • G01N17/00Investigating resistance of materials to the weather, to corrosion, or to light
    • G01N17/02Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement

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Abstract

An electrochemical testing device for high-temperature stress corrosion environment under a slow strain rate stretching condition. The device comprises an electronic universal material testing machine, a high-temperature furnace and a high-temperature electrochemical testing system; the high-temperature furnace is arranged in the inner space of the electronic universal material testing machine; the high-temperature electrochemical test system comprises a reference electrode, an auxiliary electrode, a working electrode, a high-temperature resistant electrolytic cell, an intelligent temperature control system and an electrochemical workstation; in the invention, the auxiliary electrode and the reference electrode are sealed in the inner wall of the high-temperature resistant electrolytic cell, so that the electrodes are uniformly heated in the high-temperature test process, and the stable operation is ensured; the working electrode is connected with the electrochemical workstation in a manner of embedding a lead wire, so that the connection is firmer. The device is stable and reliable, is suitable for electrochemical test of a high-temperature stress corrosion environment within the range of 100-300 ℃ under a slow strain rate stretching condition, and can realize electrochemical stability test and analysis in the high-temperature stress corrosion process.

Description

Electrochemical testing device for high-temperature stress corrosion environment under slow strain rate stretching condition
Technical Field
The invention belongs to the technical field of corrosion electrochemical measuring devices, and particularly relates to a high-temperature stress corrosion environment electrochemical testing device under a slow strain rate stretching condition.
Background
The electrochemical testing device for the high-temperature stress corrosion environment under the slow strain rate stretching condition mainly comprises a high-temperature furnace, a high-temperature electrochemical system and an electronic universal material testing machine; the high-temperature furnace provides heat to generate a high-temperature environment and can realize program temperature control; the high-temperature electrochemical system is used for placing a high-temperature electrode and plasma liquid and is connected with the electrochemical workstation, and the electronic universal material testing machine is used for fixing the working electrode, namely a tensile sample, and performing tensile test.
Electrochemical behavior of metallic materials in high temperature aqueous solutions has been of great interest. The high temperature causes the physical and chemical properties of the aqueous solution to change greatly compared with the room temperature, and the aqueous solution cannot be kept in a liquid state in a normal pressure environment. In addition, how to effectively apply the electrochemical test to the dynamic stretching system is also a big difficulty. At present, researches mainly focus on in-situ static electrochemical tests in high-temperature and high-pressure environments, high-temperature steam static electrochemical tests and high-temperature molten salt static electrochemical system tests, and the researches on the electrochemical tests in a dynamic stretching system under normal pressure are not deep yet. The technical problems of the electrochemical testing device for high-temperature and dynamic stretching systems mainly focus on the stability of the liquid electrolyte and dynamic system testing. At high temperature, the electrolyte based on the aqueous solution can generate boiling phenomenon, thereby interfering the transmission of electric signals, and consequently, the current loop monitored in the electrochemical test process is unstable, thereby influencing the accuracy of the electrochemical test result; in the process of the tensile test, the deformation of the metal can drive the liquid electrolyte to generate physical disturbance, so that the current conducted through the electrolyte changes, errors are increased, the reliability of data in a high-temperature electrochemical test is seriously influenced, and scientific analysis and evaluation can not be performed on a research system. Therefore, basic performance experimental researches such as electrochemical test technology of material mechanical behavior in a high-temperature and dynamic stretching system are urgently needed to be carried out so as to solve the problems of instability, numerical fluctuation and the like of corresponding electrochemical tests in the high-temperature stretching process in the prior art.
Disclosure of Invention
In order to solve the above problems, the present invention provides an electrochemical testing device under a high temperature stress corrosion environment under a slow strain rate tensile condition.
In order to achieve the aim, the electrochemical testing device for the high-temperature stress corrosion environment under the slow strain rate tensile condition comprises an electronic universal material testing machine, a high-temperature furnace and a high-temperature electrochemical testing system; wherein the high-temperature furnace is arranged in the inner space of the electronic universal material testing machine; the high-temperature electrochemical test system comprises a reference electrode, an auxiliary electrode, a working electrode, a high-temperature resistant electrolytic cell, an intelligent temperature control system and an electrochemical workstation; the inside of the high-temperature resistant electrolytic cell is filled with plasma liquid serving as electrolyte; the high-temperature resistant electrolytic cell is arranged inside the high-temperature furnace; the tensile sample as the working electrode main body is arranged in the middle of the high-temperature resistant electrolytic cell, and the upper end and the lower end of the tensile sample extend out of the high-temperature resistant electrolytic cell and are connected with the electronic universal material testing machine through clamps; the reference electrode and the auxiliary electrode are arranged on the high-temperature resistant electrolytic cell, and the reference electrode, the auxiliary electrode and the working electrode are respectively connected with an electrochemical workstation arranged outside the electronic universal material testing machine through leads; the intelligent temperature control system is connected with the high-temperature furnace.
The high-temperature resistant electrolytic cell is made of high-temperature glass and is in a cuboid shape, a hole is formed in the center of the top end, the hole is in a conical inner buckle shape, and a screw hole is formed in the center of the bottom end; the tensile sample is of a dumbbell-shaped structure, external threads are respectively arranged on the circumferential surfaces of the upper part and the lower part, the upper end of the tensile sample protrudes out of an opening at the top end of the high-temperature resistant electrolytic cell, the lower part of the tensile sample is in threaded connection with a screw hole of the high-temperature resistant electrolytic cell, a copper wire is wound at the screw hole, the middle part of the copper wire is embedded in the wall of the high-temperature resistant electrolytic cell, the upper end of the copper wire is led out from the top end of the high-temperature resistant electrolytic cell, and; the reference electrode is inserted into the high-temperature resistant electrolytic cell from the top end of the high-temperature resistant electrolytic cell, the inlet is of a double-sleeve design and can rotate for 360 degrees, the tail end of the reference electrode extends outwards to form a thin glass tube, and the tube opening of the reference electrode is close to a tensile sample; the auxiliary electrode is made of a platinum sheet and is directly embedded in the middle section wall of the high-temperature resistant electrolytic cell, one side surface of the auxiliary electrode is kept in a parallel state with the tensile sample, one side surface of the auxiliary electrode is connected with a lead embedded in the wall of the high-temperature resistant electrolytic cell, and the lead is led out from the top end of the high-temperature resistant electrolytic cell.
And the upper end and the lower end of the tensile sample are in threaded connection with a clamp on the electronic universal material testing machine.
A gasket is arranged between the clamp on the electronic universal material testing machine and the high-temperature resistant electrolytic cell; and gaps among the high-temperature furnace, the high-temperature resistant electrolytic cell and the tensile sample are sealed by asbestos.
The auxiliary electrode and the reference electrode in the electrochemical testing device under the high-temperature stress corrosion environment under the slow strain rate stretching condition are sealed in the inner wall of the high-temperature resistant electrolytic cell, so that the electrodes are uniformly heated in the high-temperature testing process, and the stable operation is ensured; the working electrode is connected with the electrochemical workstation in a manner of embedding a lead wire, so that the connection is firmer. The device is stable and reliable, is suitable for electrochemical test in a high-temperature stress corrosion environment within the range of 100-300 ℃ under a slow strain rate stretching condition, can realize electrochemical stability test and analysis in a high-temperature stress corrosion process, and can solve the problem that other materials need high-temperature electrochemical test.
Drawings
FIG. 1 is a schematic diagram of a high temperature resistant electrolytic cell in an electrochemical testing device under a high temperature stress corrosion environment under a slow strain rate tensile condition.
FIG. 2 is a schematic structural diagram of an electrochemical testing apparatus for high temperature stress corrosion environment under a slow strain rate tensile condition according to the present invention.
FIG. 3 is a schematic diagram of a tensile sample in an electrochemical testing device for high temperature stress corrosion environment under a slow strain rate tensile condition according to the present invention.
Detailed Description
The electrochemical testing device under the high-temperature stress corrosion environment under the tensile condition with the slow strain rate provided by the invention is described in detail below with reference to the accompanying drawings and specific examples.
As shown in fig. 1-3, the electrochemical testing device for high-temperature stress corrosion environment under the slow strain rate tensile condition provided by the invention comprises an electronic universal material testing machine 5, a high-temperature furnace 6 and a high-temperature electrochemical testing system; wherein the high temperature furnace 6 is arranged in the inner space of the electronic universal material testing machine 5; the high-temperature electrochemical test system comprises a reference electrode 1, an auxiliary electrode 2, a working electrode 3, a high-temperature resistant electrolytic cell 4, an intelligent temperature control system 7 and an electrochemical workstation 8; the plasma liquid as electrolyte is contained in the high-temperature resistant electrolytic cell 4, so that the electrolytic cell can be effectively prevented from bursting due to uneven heating, and the electrolyte is prevented from bumping in the high-temperature test process; the high-temperature resistant electrolytic cell 4 is arranged inside the high-temperature furnace 6; a tensile sample 9 as a main body of the working electrode 3 is arranged in the middle of the high-temperature resistant electrolytic cell 4, and the upper end and the lower end of the tensile sample extend out of the high-temperature resistant electrolytic cell 4 and are connected with the electronic universal material testing machine 5 through a clamp; the reference electrode 1 and the auxiliary electrode 2 are both arranged on the high-temperature resistant electrolytic cell 4, and the reference electrode 1, the auxiliary electrode 2 and the working electrode 3 are respectively connected with an electrochemical workstation 8 arranged outside the electronic universal material testing machine 5 through leads; the intelligent temperature control system 7 is connected with the high-temperature furnace 6 and is used for carrying out program temperature control on the high-temperature furnace 6.
The high-temperature resistant electrolytic cell 4 is made of high-temperature glass and is in a cuboid shape, a hole is formed in the center of the top end, the hole is in a conical inner buckle shape, and a screw hole is formed in the center of the bottom end; the tensile sample 9 is of a dumbbell-shaped structure, external threads are respectively arranged on the circumferential surfaces of the upper part and the lower part, the upper end of the tensile sample protrudes out of an opening at the top end of the high-temperature resistant electrolytic cell 4, the lower part of the tensile sample is in threaded connection with a screw hole of the high-temperature resistant electrolytic cell 4, a copper wire is wound at the screw hole, the middle part of the copper wire is embedded in the wall of the high-temperature resistant electrolytic cell 4, the upper end of the copper wire is led out from the top end of the high-temperature resistant electrolytic cell 4, and the tensile; the reference electrode 1 is inserted into the high-temperature resistant electrolytic cell 4 from the top end thereof, the inlet is of a double-sleeve design and can rotate by 360 degrees, the tail end extends outwards to form a thin glass tube, and the tube opening is close to the tensile sample 9; the auxiliary electrode 2 is made of platinum sheet and is directly embedded in the middle section wall of the high-temperature resistant electrolytic cell 4, one side surface of the auxiliary electrode is kept in a parallel state with the tensile sample 9, one side surface of the auxiliary electrode is connected with a lead embedded in the wall of the high-temperature resistant electrolytic cell 4, and the lead is led out from the top end of the high-temperature resistant electrolytic cell 4.
The upper end and the lower end of the tensile sample 9 are in threaded connection with a clamp on the electronic universal material testing machine 5.
A gasket is arranged between the clamp on the electronic universal material testing machine 5 and the high-temperature resistant electrolytic cell 4; the gaps between the high-temperature furnace 6, the high-temperature resistant electrolytic cell 4 and the tensile sample 9 are sealed by asbestos.
The working principle of the electrochemical testing device under the condition of slow strain rate and stretching and high-temperature stress corrosion environment provided by the invention is explained as follows:
firstly, a tester puts a high-temperature resistant electrolytic cell 4 which is provided with a reference electrode 1, an auxiliary electrode 2 and a working electrode 3 and is injected with plasma liquid into a high-temperature furnace 6, then the upper end and the lower end of a tensile sample 9 which is taken as the main body of the working electrode 3 are connected with an electronic universal material testing machine 5 through clamps so as to prevent the device from excessively vibrating in the tensile process, and gaps among the high-temperature furnace 6, the high-temperature resistant electrolytic cell 4 and the tensile sample 9 are sealed by asbestos, so that the uniform heating and no overflow of heat can be ensured; the high-temperature furnace 6 is then closed and the leads connected to the reference electrode 1, the auxiliary electrode 2 and the working electrode 3 are connected to an electrochemical workstation 8. The conical inner-buckled opening in the center of the top end of the high-temperature resistant electrolytic cell 4 can generate gas backflow, so that the outward permeation rate of the plasma liquid belonging to a corrosive medium can be slowed down; and then a gasket is added between the high-temperature resistant electrolytic cell 4 and a clamp on the electronic universal material testing machine 5 so as to prevent the pollution and the damage of experimental instruments caused by the leakage of the plasma liquid. And then, the intelligent temperature control system 7 is used for controlling the high-temperature furnace 6 to be started for heating, and when the display on the intelligent temperature control system 7 displays that the temperature in the high-temperature furnace 6 is stable, the electrochemical test of high-temperature stress corrosion can be started. The electronic universal material testing machine 5 adopts a slow strain rate stretching method to enable the whole of the tensile sample 9 and the high-temperature resistant electrolytic cell 4 to be in a quasi-static process, so that reliable potential testing can be realized.

Claims (2)

1. The utility model provides a high temperature stress corrosion environment electrochemistry testing arrangement under tensile condition of slow strain rate which characterized in that: the device comprises an electronic universal material testing machine (5), a high-temperature furnace (6) and a high-temperature electrochemical testing system; wherein the high-temperature furnace (6) is arranged in the space inside the electronic universal material testing machine (5); the high-temperature electrochemical test system comprises a reference electrode (1), an auxiliary electrode (2), a working electrode (3), a high-temperature resistant electrolytic cell (4), an intelligent temperature control system (7) and an electrochemical workstation (8); the high-temperature resistant electrolytic cell (4) is internally provided with plasma liquid serving as electrolyte; the high-temperature resistant electrolytic cell (4) is arranged inside the high-temperature furnace (6); a tensile sample (9) serving as a main body of the working electrode (3) is arranged in the middle of the high-temperature resistant electrolytic cell (4), and the upper end and the lower end of the tensile sample extend out of the high-temperature resistant electrolytic cell (4) and are connected with the electronic universal material testing machine (5) through clamps; the reference electrode (1) and the auxiliary electrode (2) are arranged on the high-temperature resistant electrolytic cell (4), and the reference electrode (1), the auxiliary electrode (2) and the working electrode (3) are respectively connected with an electrochemical workstation (8) arranged outside the electronic universal material testing machine (5) through leads; the intelligent temperature control system (7) is connected with the high-temperature furnace (6);
the method is characterized in that: the high-temperature resistant electrolytic cell (4) is made of high-temperature glass and is in a cuboid shape, a hole is formed in the center of the top end, the hole is in a conical inner buckle shape, and a screw hole is formed in the center of the bottom end; the tensile sample (9) is of a dumbbell-shaped structure, external threads are respectively arranged on the circumferential surfaces of the upper part and the lower part, the upper end of the tensile sample protrudes out of an opening at the top end of the high-temperature resistant electrolytic cell (4), the lower part of the tensile sample is connected in a screw hole of the high-temperature resistant electrolytic cell (4) in a threaded manner, a copper wire is wound at the screw hole, the middle part of the copper wire is embedded in the wall of the high-temperature resistant electrolytic cell (4), the upper end of the copper wire is led out from the top end of the high-temperature resistant electrolytic cell (4), and the tensile sample (9); the reference electrode (1) is inserted into the high-temperature resistant electrolytic cell (4) from the top end thereof, the inlet is of a double-sleeve design and can rotate for 360 degrees, the tail end extends outwards to form a thin glass tube, and the tube opening is close to the tensile sample (9); the auxiliary electrode (2) is made of a platinum sheet and is directly embedded into the middle section wall of the high-temperature resistant electrolytic cell (4), one side surface of the auxiliary electrode is kept in a parallel state with the tensile sample (9), one side surface of the auxiliary electrode is connected with a lead embedded into the wall of the high-temperature resistant electrolytic cell (4), and the lead is led out from the top end of the high-temperature resistant electrolytic cell (4);
a gasket is arranged between the clamp on the electronic universal material testing machine (5) and the high-temperature resistant electrolytic cell (4); gaps among the high-temperature furnace (6), the high-temperature resistant electrolytic cell (4) and the tensile sample (9) are sealed by asbestos.
2. The device for electrochemical testing under a slow strain rate tensile condition in a high-temperature stress corrosion environment according to claim 1, wherein: the upper end and the lower end of the tensile test sample (9) are in threaded connection with a clamp on the electronic universal material testing machine (5).
CN201811123257.0A 2018-09-26 2018-09-26 Electrochemical testing device for high-temperature stress corrosion environment under slow strain rate stretching condition Active CN108982350B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101498648A (en) * 2009-01-14 2009-08-05 北京科技大学 Multifunctional in-situ electro-chemical measuring apparatus for tensile test
CN201867358U (en) * 2010-08-04 2011-06-15 南京工业大学 Vapor-liquid two-phase flow accelerated corrosion test device
CN202814850U (en) * 2012-08-28 2013-03-20 中国科学院金属研究所 Portable variable-load digital stress corrosion measuring device
CN104458559A (en) * 2014-11-24 2015-03-25 辽宁石油化工大学 Device capable of testing stress-electrochemical corrosion
CN105300874A (en) * 2015-09-11 2016-02-03 中国民航大学 Stress corrosion and hydrogen measuring electrochemical in-situ measurement device under slow strain speed condition
CN106468650A (en) * 2015-08-21 2017-03-01 中国石油天然气股份有限公司 Reactor and corrosion test system

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101498648A (en) * 2009-01-14 2009-08-05 北京科技大学 Multifunctional in-situ electro-chemical measuring apparatus for tensile test
CN201867358U (en) * 2010-08-04 2011-06-15 南京工业大学 Vapor-liquid two-phase flow accelerated corrosion test device
CN202814850U (en) * 2012-08-28 2013-03-20 中国科学院金属研究所 Portable variable-load digital stress corrosion measuring device
CN104458559A (en) * 2014-11-24 2015-03-25 辽宁石油化工大学 Device capable of testing stress-electrochemical corrosion
CN106468650A (en) * 2015-08-21 2017-03-01 中国石油天然气股份有限公司 Reactor and corrosion test system
CN105300874A (en) * 2015-09-11 2016-02-03 中国民航大学 Stress corrosion and hydrogen measuring electrochemical in-situ measurement device under slow strain speed condition

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