阅读说明：本技术 一种同时用于电化学实验和慢应变速率拉伸测试的可控温电解池装置及其使用方法 (Temperature-controllable electrolytic cell device simultaneously used for electrochemical experiment and slow strain rate tensile test and use method thereof ) 是由 高志明 刘英杰 王利钦 夏大海 胡文彬 刘永长 于 2018-06-15 设计创作，主要内容包括：本发明公开了一种同时用于电化学实验和慢应变速率拉伸测试的可控温电解池装置及其使用方法,本装置通过在反应池内部形成电解池,沿电解池外圈形成有循环水槽,达到了在进行拉伸测试的同时完成对电解池内的实验环境进行控温,密封塞、密封垫和旋盖组合完成了拉伸试样的固定与及密封,本装置可以对不同温度下,不同受力情况下的样品进行电化学测试,比如极化曲线测量、电化学交流阻抗谱、电化学噪声测试、M-S曲线测量等,来分析材料的腐蚀情况。(The invention discloses a temperature-controllable electrolytic cell device for electrochemical experiments and slow strain rate tensile tests and a using method thereof.)

1. A temperature-controllable electrolytic cell device simultaneously used for electrochemical experiments and slow strain rate tensile tests is characterized in that: the cover is placed to reaction tank, electrode, sealing plug, sealed pad and spiral cover, the inside electrolytic cell that is formed with of reaction tank, is formed with the circulating water tank along the electrolytic cell outer lane, is provided with water inlet and delivery port on the circulating water tank outer wall, is provided with the electrode on the electrolytic cell and places the lid, the electrode is placed and is covered center department and be provided with the sample hole that supplies tensile sample to pass through, the electrode is placed and is covered still to be provided with first electrode hole and the second electrode hole that is used for placing reference electrode and counter electrode, is formed with the through-hole in electrolytic cell bottom surface center department, is provided with the sealing plug in the through-hole, is formed with the seal receptacle in the electrolytic cell lower part, is provided with annular sealed pad in the seal receptacle, is provided with the spiral cover.

2. The controllable temperature electrolytic cell device for electrochemical experiments and slow strain rate tensile tests simultaneously according to claim 1, wherein: and the electrode placing cover and the upper edge of the electrolytic cell are fastened and sealed through nuts.

3. The controllable temperature electrolytic cell device for electrochemical experiments and slow strain rate tensile tests simultaneously according to claim 1, wherein: the electrode placing cover is provided with a through vertical pipe towards one side of the electrolytic cell, the electrode placing cover is provided with an air hole, the vertical pipe and the air hole are used for being connected with an air bottle to control the atmosphere in the electrolytic cell, the vertical pipe is an air inlet, the air hole is an air outlet, and internal threads used for being connected with an air pipe of the air bottle are arranged on the inner ring of the air hole and the upper edge of the vertical pipe.

4. The controllable temperature electrolytic cell device for electrochemical experiments and slow strain rate tensile tests simultaneously according to claim 1, wherein: an annular outer cover used for sealing, insulating and preventing circulating water from splashing is arranged above the circulating water tank.

5. The controllable temperature electrolytic cell device for electrochemical experiments and slow strain rate tensile tests simultaneously according to claim 1, wherein: the water inlet and the water outlet are connected with the constant-temperature water tank through water pipes, the water inlet and the water outlet are oppositely arranged on the outer wall of the reaction tank, and the position of the water outlet is higher than the position of the water inlet which is arranged externally.

6. The controllable temperature electrolytic cell device for electrochemical experiments and slow strain rate tensile tests simultaneously according to claim 1, wherein: the whole sealing plug is wedge-shaped and is formed by combining a left plug body and a right plug body which are symmetrical to each other, and a sample square hole for a tensile sample to pass through is formed in the middle of the sealing plug.

7. The controllable temperature electrolytic cell device for electrochemical experiments and slow strain rate tensile tests simultaneously according to claim 1, wherein: the reaction tank, the electrode placing cover, the annular outer cover, the sealing gasket and the screw cover are all made of PVC materials.

8. A method for using a temperature-controllable electrolytic cell device for electrochemical experiments and slow strain rate tensile tests simultaneously is characterized in that: the method comprises the following steps:

fixing the middle part of a tensile sample through a sealing plug, vertically placing the tensile sample in an electrolytic cell, covering an electrode placing cover to enable the upper end of the tensile sample to extend out of a sample hole, placing an annular sealing gasket in a sealing seat below the sealing plug, screwing a screw cover, and enabling the lower end of the tensile sample to extend out of a screw cover hole of the screw cover;

step two: fixing the upper end and the lower end of a tensile sample through an upper clamp and a lower clamp of a stress corrosion testing machine, and fixing the tensile sample together with the position of an electrolytic cell device;

step three: connecting a water inlet and a water outlet with a constant-temperature water tank through water pipes, communicating a circulating water tank with the constant-temperature water tank, and controlling the temperature of an experiment in an electrolytic cell by adjusting the temperature of the constant-temperature water tank;

step four: and putting a corrosion medium of the simulated working condition into the electrolytic cell, fixing a reference electrode and a counter electrode in the first electrode hole and the second electrode hole respectively, connecting the three electrodes through a test testing device, starting a stress corrosion testing machine to stretch the tensile sample, and simultaneously performing an electrochemical experiment and a slow strain rate tensile test.

9. The use method of the controllable temperature electrolytic cell device for electrochemical experiments and slow strain rate tensile tests simultaneously according to claim 8 is characterized in that: and in the fourth step, before the stress corrosion testing machine is started to stretch the tensile sample, filling inert gas into the corrosion medium through a vertical pipe extending into the corrosion medium, wherein the inert gas is nitrogen.

10. Use of a temperature-controlled electrolyzer device for simultaneous electrochemical experiments and slow strain rate tensile tests according to one of claims 1 to 7 or of a method of use of a temperature-controlled electrolyzer device for simultaneous electrochemical experiments and slow strain rate tensile tests according to one of claims 8 to 9 for polarization curve measurements under controlled temperature, atmospheric conditions, electrochemical impedance spectroscopy measurements, electrochemical noise measurements and Mott-Schottky curve measurements.

Technical Field

The invention relates to an electrochemical test device, in particular to a temperature-controllable electrolytic cell device simultaneously used for an electrochemical experiment and a slow strain rate tensile test and a using method thereof.

Background

Corrosion of metals refers to the deterioration and destruction of metals in the natural environment or under operating conditions due to chemical or electrochemical interaction with the surrounding medium. With the gradual development of the industry, various industrial environments where metals are located tend to be complicated, such as water-hydrogen sulfide corrosion environments of petroleum transportation pipelines, high-pressure chloride ion environments of deep-sea pipelines, high-temperature and high-pressure environments of boiler pipelines, and the like.

Currently, common corrosion rate-reducing means for metals include sacrificial anodic protection and impressed current cathodic protection. Particularly, for petroleum pipelines and sea-crossing bridges, due to the fact that the stress of the structure is large, if metal materials are not well protected, due to the fact that the stress sectional area of the structure is reduced, the structure can be rapidly failed, and service life is affected. Therefore, the use of cathodic protection to protect metal materials has become a popular protection method. However, if the cathode protection selection potential is not proper, the problem of metal hydrogen embrittlement can be caused, the accumulation of hydrogen atoms increases the internal defects of the material, the mechanical property is obviously reduced, and the phenomenon of bubbling and falling off of the external coating of the pipeline steel due to the action of hydrogen bubbles can be caused, so that local corrosion is caused. In addition, the temperature change range in the petroleum pipeline is large, and the corrosion condition of the pipeline under various conditions can be judged by researching the difference of mechanical properties under different hydrogen charging conditions and different temperature conditions. Meanwhile, the corrosion condition of the material can be analyzed by performing electrochemical tests on samples under different stress conditions at different temperatures, such as polarization curve measurement, electrochemical alternating current impedance spectroscopy, electrochemical noise test, M-S curve measurement and the like.

Disclosure of Invention

The invention aims to overcome the defects of the prior art, solve the problem that the traditional electrolytic cell cannot control the temperature while stretching at a slow strain rate, and provide a temperature-controllable electrolytic cell device which is simultaneously used for an electrochemical experiment and a slow strain rate stretching test.

The invention is realized by the following technical scheme:

the utility model provides a controllable temperature electrolytic cell device that is used for electrochemistry experiment and slow strain rate tensile test simultaneously, lid, sealing plug, sealed pad and spiral cover are placed to reaction tank, electrode, the inside electrolytic cell that is formed with of reaction tank is formed with the circulating water tank along the electrolytic cell outer lane, is provided with water inlet and delivery port on the circulating water tank outer wall, is provided with the electrode in the electrolytic cell upper end and places the lid, the electrode is placed lid center department and is provided with the sample hole that supplies tensile sample to pass through, the electrode is placed and is covered still to be provided with first electrode hole and the second electrode hole that is used for placing reference electrode and counter electrode, is formed with the through-hole in electrolytic cell bottom surface center department, is provided with the sealing plug in the through-hole, is formed with the seal receptacle in the electrolytic cell lower part, is provided with annular sealed pad in the seal receptacle, is provided with the spiral.

In the technical scheme, the electrode placing cover and the upper edge of the electrolytic cell are fastened and sealed through the nut.

In the technical scheme, the electrode placing cover is provided with the through vertical pipe towards one side of the electrolytic cell, the electrode placing cover is provided with the air hole, the vertical pipe and the air hole are used for being connected with an air bottle to control the atmosphere in the electrolytic cell, the vertical pipe is an air inlet, and the air hole is an air outlet.

In the technical scheme, the inner ring of the air hole and the upper edge of the vertical pipe are both provided with internal threads used for being connected with an air pipe of the air bottle.

In the technical scheme, an annular outer cover used for sealing, insulating and preventing the circulating water from splashing is arranged above the circulating water tank.

In the technical scheme, the water inlet and the water outlet are connected with the constant-temperature water tank through water pipes.

In the technical scheme, the water inlet and the water outlet are oppositely arranged on the outer wall of the reaction tank, and the position of the water outlet is higher than the position of the water inlet which is arranged outside.

In the above technical scheme, the whole sealing plug is wedge-shaped, is made of rubber, and is formed by combining the left plug body and the right plug body which are symmetrical to each other, and the middle part of the sealing plug is provided with a sample square hole for a tensile sample to pass through.

In the above technical solution, the tensile test specimen is a dumbbell-shaped tensile standard with a slow strain rate.

In the technical scheme, the reaction tank, the electrode placing cover, the annular outer cover, the sealing gasket and the screw cover are all made of PVC materials.

A method for using a temperature-controlled electrolytic cell device for electrochemical experiments and slow strain rate tensile tests simultaneously comprises the following steps:

fixing the middle part of a tensile sample through a sealing plug, vertically placing the tensile sample in an electrolytic cell, covering an electrode placing cover to enable the upper end of the tensile sample to extend out of a sample hole, placing an annular sealing gasket in a sealing seat below the sealing plug, screwing a screw cover, and enabling the lower end of the tensile sample to extend out of a screw cover hole of the screw cover;

step two: fixing the upper end and the lower end of a tensile sample through an upper clamp and a lower clamp of a stress corrosion testing machine, and fixing the tensile sample together with the position of an electrolytic cell device;

step three: connecting a water inlet and a water outlet with a constant-temperature water tank through water pipes, communicating a circulating water tank with the constant-temperature water tank, and controlling the temperature of an experiment in an electrolytic cell by adjusting the temperature of the constant-temperature water tank;

step four: and putting a corrosion medium of the simulated working condition into the electrolytic cell, fixing a reference electrode and a counter electrode in the first electrode hole and the second electrode hole respectively, connecting the three electrodes through a test testing device, starting a stress corrosion testing machine to stretch the tensile sample, and simultaneously performing an electrochemical experiment and a slow strain rate tensile test.

In the technical scheme, in the fourth step, the reference electrode and the counter electrode are fixed through plasticine.

In the above technical scheme, in the fourth step, before the stress corrosion testing machine is started to stretch the tensile sample, inert gas is filled into the corrosive medium through the vertical tube extending into the corrosive medium, and the inert gas is nitrogen.

The temperature-controllable electrolytic cell device simultaneously used for the electrochemical experiment and the slow strain rate tensile test and the use method thereof can be applied to the electrochemical experiment, and the electrochemical experiment comprises polarization curve measurement under the conditions of controlled temperature and controlled atmosphere, electrochemical impedance spectrum measurement, electrochemical noise measurement and Mott-Schottky curve measurement.

The invention has the advantages and beneficial effects that:

this device is through forming the electrolytic bath in the reaction tank inside, be formed with circulating water tank along the electrolytic bath outer lane, has reached and has accomplished the experimental environment in to the electrolytic bath and control the temperature when carrying out tensile test, and sealing plug, sealed pad and spiral cover combination have accomplished tensile sample' S fixed and sealed, and this device can be to different temperatures down, and the sample under the different atress circumstances carries out the electrochemistry test, for example polarization curve measurement, electrochemistry alternating-current impedance spectrum, electrochemistry noise test, M-S curve measurement etc. comes the corruption condition of analysis material.

Drawings

FIG. 1 is a plan exploded view of the present invention.

Fig. 2 is a three-dimensional exploded structure view of the present invention.

Fig. 3 is a schematic view of the electrode placement cover structure.

FIG. 4 is a schematic diagram of the reaction cell structure.

Fig. 5 is a schematic view of a gasket structure.

Fig. 6 is a schematic view of a screw cap structure.

Fig. 7 is a schematic view of a tensile specimen configuration.

FIG. 8 is a graph of the stress-strain curves for a charged and uncharged tensile member of X65 steel, where 1 is charged and 2 is uncharged.

Wherein, 1 is an electrode placing cover, 1-1 is a cover body, 1-2 is a vertical pipe, 1-3 is an air hole, 1-4 is a first electrode hole, 1-5 is a sample hole, 1-6 is a second electrode hole, 2 is a reaction tank, 2-1 is an electrolytic tank, 2-2 is a circulating water tank, 2-3 is a water inlet, 2-4 is a water outlet, 2-5 is a through hole, 2-6 is a sealing seat, 2-7 is a sealing plug groove, 3 is a sealing plug, 3-1 is a left plug body, 3-2 is a right plug body, 3-3 is a sample square hole, 4 is a sealing pad, 5 is a rotary cover, and 5-1 is a rotary cover hole.

For a person skilled in the art, other relevant figures can be obtained from the above figures without inventive effort.

Detailed Description

In order to make the technical solution of the present invention better understood, the technical solution of the present invention is further described below with reference to specific examples.