CN114563341A - Device and method for measuring hydrogen diffusion coefficient of welding joint microcell and application of device and method - Google Patents

Device and method for measuring hydrogen diffusion coefficient of welding joint microcell and application of device and method Download PDF

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CN114563341A
CN114563341A CN202110145219.0A CN202110145219A CN114563341A CN 114563341 A CN114563341 A CN 114563341A CN 202110145219 A CN202110145219 A CN 202110145219A CN 114563341 A CN114563341 A CN 114563341A
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姜圆博
邸新杰
利成宁
王东坡
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Tianjin University
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    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
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Abstract

The invention provides a device for measuring the hydrogen diffusion coefficient of a welding joint microcell and a measuring method and application thereof.A cathode electrolyte is filled in a cathode pool, and an auxiliary electrode of the cathode pool is connected with the anode of a direct current constant current power supply through a lead; the anode pool is filled with anolyte, an anode pool auxiliary electrode and an anode pool reference electrode both extend into the anolyte and are respectively connected with an electrochemical workstation through leads, and the electrochemical workstation is connected with a computer; the side walls of the cathode pool and the anode pool are respectively and oppositely provided with a circular truncated cone-shaped through hole, a sample to be tested is arranged between the cathode pool through hole and the anode pool through hole, and the sample to be tested is respectively connected with the negative pole and the electricity of the direct current constant current power supply through leadsThe chemical workstation is connected. Testing the hydrogen diffusion coefficient of a micro-area in the welded joint by adjusting the cone angle range of the circular truncated cone-shaped through hole and the diameter of the bottom surface of the circular truncated cone, wherein the area range of the micro-area exposed to the electrolyte is 0.20-1.13cm2The cone angle range of the circular truncated cone-shaped through hole which is contacted with the sample to be tested is 30-70 degrees.

Description

Device and method for measuring hydrogen diffusion coefficient of welding joint microcell and application of device and method
Technical Field
The invention relates to the technical field of metal corrosion electrochemical tests, in particular to a device for measuring a hydrogen diffusion coefficient of a welding joint microcell, and a measuring method and application thereof.
Background
The corrosion problem of metal materials is spread in various fields of national economy and society, direct or indirect economic loss caused by corrosion failure is often immeasurable, and the production and the life of people are seriously damaged. Hydrogen embrittlement is one of the most common forms of corrosion failure due to the unavoidable presence of hydrogen in the ambient medium. Hydrogen embrittlement is a brittle fracture that is not easily detectable, with no obvious signs prior to fracture, typically a catastrophic failure. The number of sudden accident cases caused by hydrogen induced fracture in local areas is particularly significant in the corrosion damage of metal welded joints. This is because, under the action of welding heat cycle, each micro-region of the weld joint, the heat affected zone, the base metal, etc. has different chemical compositions and microstructures, and the mechanical properties of each region are also obviously different. This microstructural and mechanical property inhomogeneity often results in differences in the adsorption and diffusion behavior of hydrogen in the micro-zones of the weld joint. Therefore, more attention is paid to hydrogen permeation and cracking mechanisms of all micro-areas of the welding joint, and researchers can be helped to prevent local hydrogen embrittlement of the welding joint by adopting a more appropriate welding process or a more effective protection means.
The hydrogen diffusion coefficient is the main parameter characterizing the hydrogen permeation process. Generally, methods for measuring the hydrogen diffusion coefficient mainly include two methods, i.e., a gas phase method and an electrochemical method. Compared with the former, the hydrogen permeation technology needs to provide a high vacuum environment and is equipped with expensive equipment, and the latter is a hydrogen permeation technology which is more widely applied and simpler and more convenient to operate at present. Electrochemical hydrogen permeation methods for measuring the diffusion coefficient of hydrogen were first proposed by devanaathan and Stachurski in 1962, and the materials were charged and tested using a dual cell. With the advancement of science and technology, most electrochemical hydrogen permeation devices are improved on the basis of a Devanathan-Stachurski double-electrolytic cell method. The improved double electrolytic cell technology principle is as follows: the test material is used as a working electrode and clamped between two electrolytic cells with round holes, and the two sides of the working electrode are respectively exposed in the electrolyte solution through the round holes; the cathode electrolytic cell is used as a hydrogen charging cell, and hydrogen atoms are generated in the electrolyte by applying constant current between a working electrode and a corresponding auxiliary electrode (generally a platinum electrode), adsorbed on the surface of the working electrode and diffused into the material; the anode electrolytic cell is used as a detection cell, hydrogen atoms diffused from the hydrogen charging cell are electrolyzed by applying constant potential between the working electrode and the auxiliary electrode, and the corresponding generated current can be recorded in real time, so that a hydrogen diffusion curve is drawn. By analyzing the time-current curve of the diffusion characteristic of the hydrogen in the material, relevant diffusion kinetic parameters, particularly the hydrogen diffusion coefficient, can be obtained.
In many studies on hydrogen diffusion characteristics by using a Devanathan-Stachyrski double-electrolytic cell method, the hydrogen diffusion behavior of a welded joint and each micro-area thereof has not been analyzed specially, and particularly for a flat plate or steel pipe welded joint with small thickness, each micro-area, particularly a heat affected area, is affected by the size, and the extracted hydrogen permeation sample is small. However, most of the current double electrolytic cell devices are designed for uniform materials having large sizes, and the diameter of the circular hole between the double electrolytic cells is generally large. The heat affected zone of the welded joint is small in size, and such a double electrolytic cell with a large aperture cannot be used. The diameter of the circular hole of the electrolytic cell is reduced, and the hydrogen bubbles generated on the surface of the working electrode cannot be discharged out of the circular hole in time to block a current path between the electrolyte and the working electrode, so that data cannot be stably acquired.
Patent CN 104950024 a discloses a modified Devanathan-Stachurski two-cell device for measuring hydrogen diffusion coefficient, but it cannot be applied to a small size of weld heat affected zone due to its large diameter of the circular hole (about 2.3 cm).
Patent CN 109883942 a discloses a test method for micro-area electrochemical test of a welding joint based on a microscope, but the method can only test the open circuit potential and polarization curve of the micro-area, and cannot obtain the hydrogen diffusion coefficient of each micro-area.
Disclosure of Invention
The invention overcomes the defects in the prior art, the existing hydrogen diffusion coefficient measuring method cannot be suitable for a welding heat affected zone with a small size, and the hydrogen diffusion coefficient of each micro zone cannot be obtained, and provides a measuring device for the hydrogen diffusion coefficient of the micro zone of a welding joint, a measuring method and application thereof2So as to obtain the hydrogen diffusion coefficient of the metal material, and specify the hydrogen diffusion behavior and hydrogen embrittlement mechanism of the micro-area of the welding joint of the metal material.
The purpose of the invention is realized by the following technical scheme.
A device for measuring the hydrogen diffusion coefficient of a welding joint microcell comprises a cathode electrolytic cell hydrogen charging system, an anode electrolytic cell hydrogen measuring system, a sample to be measured and a computer,
the cathode electrolytic cell hydrogen charging system comprises a direct current constant current power supply, a cathode cell and a cathode cell auxiliary electrode, wherein cathode electrolyte is filled in the cathode cell, the cathode cell auxiliary electrode extends into the cathode electrolyte, the cathode cell auxiliary electrode is connected with the positive electrode of the direct current constant current power supply through a lead, and a cathode cell through hole is formed in the side wall of the cathode cell;
the anode electrolytic cell hydrogen measurement system comprises an electrochemical workstation, an anode cell auxiliary electrode and an anode cell reference electrode, wherein an anode electrolyte is filled in the anode cell, the anode cell auxiliary electrode and the anode cell reference electrode both extend into the anode electrolyte, the anode cell auxiliary electrode and the anode cell reference electrode are connected with the electrochemical workstation, the electrochemical workstation is connected with the computer, an anode cell through hole is formed in the side wall of the anode cell, and the cathode cell through hole and the anode cell through hole are oppositely arranged;
the sample to be tested is arranged between the cathode pool through hole and the anode pool through hole, one side surface of the sample to be tested, which is provided with the nickel coating, faces the anode pool, one side surface of the sample to be tested, which is not provided with the nickel coating, faces the cathode pool, and the sample to be tested is respectively connected with the cathode of the direct current constant current power supply and the electrochemical workstation through leads.
The exposed surface area of the sample to be tested, which is in contact with the catholyte and the anolyte, is 0.20-1.13cm2。
And a first communicating sealing ring is also arranged between the sample to be tested and the cathode pool through hole, and a second communicating sealing ring is also arranged between the sample to be tested and the anode pool through hole.
The current output range of the direct current constant current power supply is 0-3A, and the current output precision is controlled to be 1 mA.
The current measuring range of the electrochemical workstation is 0-3A, the current measuring precision is 10pA, the voltage output range is 0-30V, and the control voltage output precision is 0.01 mV.
The cathode pool through hole and the anode pool through hole are both in a circular truncated cone type through hole structure, and the taper angle range of the cathode pool through hole and the taper angle range of the anode pool through hole are 30-70 degrees.
The catholyte adopts 0.5mol/L H2SO4With 3g/L NH4And the anode electrolyte adopts 0.1mol/L NaOH solution.
The cathode pool and the anode pool both adopt an acrylic organic glass structure.
The cathode pool auxiliary anode and the anode pool auxiliary electrode both adopt platinum mesh electrodes, and the first communicating sealing ring and the second communicating sealing ring both adopt silica gel gaskets.
A method for measuring the hydrogen diffusion coefficient of a micro-area of a welded joint comprises the following steps:
step 1, manufacturing a micro heat affected zone extracted from a welded joint into a welded joint with an area of 1.0cm2And a sheet sample with the thickness of 1.2mm is gradually polished to 1000# by using abrasive paper, then ultrasonic cleaning is respectively carried out in acetone and alcohol solution, then the surface of the sample is electroplated with a nickel coating, one surface of the nickel-plated sheet sample is polished to 1000# abrasive paper, the nickel coating on the surface is removed, and the other surface retains the nickelCoating, namely finally putting the sample in acetone for ultrasonic cleaning, and washing the sample by using deionized water to prepare a flaky sample to be detected;
step 2, placing the sheet-shaped sample to be measured prepared in the step 1 between a first communicating sealing ring and a second communicating sealing ring, enabling the surface of one side of the sample to be measured, which is provided with a nickel coating, to face an anode pool, fixing a measuring device on the premise of ensuring good sealing and no liquid leakage, then installing an anode pool auxiliary electrode and an anode pool reference electrode in the anode pool, connecting the anode pool auxiliary electrode and the anode pool reference electrode with the sample to be measured and an electrochemical workstation to form an anode electrolytic cell hydrogen measuring system, and simultaneously connecting the anode electrolytic cell hydrogen measuring system with a computer;
step 3, injecting 0.1mol/L NaOH anolyte into the anode pool, and adjusting the reference potential of the electrochemical workstation to 300mV to enable the whole anode electrolytic cell hydrogen measuring system to start working;
step 4, when the hydrogen permeation current value displayed by the computer is reduced to below 1.0 muA, the recording is suspended and the data recorded by the computer is cleared, then a cathode auxiliary electrode is arranged in the cathode pool, the anode and the cathode of the direct current constant current power supply are respectively connected with the cathode auxiliary electrode and the sample to be tested, and simultaneously 0.5mol/L H is injected into the cathode pool2SO4With 3g/L NH4The mixed solution of SCN is used as cathode electrolyte, a direct current constant current power supply is switched on, and the output current density is controlled to be 5mA/cm2Simultaneously, restarting to record the test data;
and 5, after the hydrogen permeation current data recorded by the computer in the step 4 does not rise any more along with the time and keeps in a stable state for a period of time, ending the hydrogen permeation experiment, closing the direct-current constant-current power supply and the electrochemical workstation, storing the experiment data on the computer, finally respectively emptying the catholyte and the anolyte in the cathode pool and the anode pool, taking out the test sample clamped between the two electrodes, processing the obtained data to obtain a hydrogen diffusion curve, and calculating by using a known formula to obtain the hydrogen diffusion coefficient of the welding joint micro-area.
The beneficial effects of the invention are as follows: compared with the prior art, the invention has the following obvious and substantial advantages:
a. the invention designs a circular truncated cone-shaped through hole on the wall of the double electrolytic cell, which enlarges the escape space of hydrogen bubbles as much as possible while reducing the area of the sample to be tested exposed in the solution, reduces the influence of the hydrogen bubbles on the test result, and greatly improves the precision and the reliability of the test result of the welding joint microcell;
b. the device has the advantages of simple equipment, easy processing, convenient assembly and low cost;
c. the device can simultaneously adjust the cone angle of the circular truncated cone-shaped through hole and the diameter of the bottom surface of the circular truncated cone so as to achieve the purpose of testing the hydrogen diffusion characteristic of the material under different exposure areas.
Drawings
Fig. 1 is a schematic structural diagram of the apparatus of the present invention, in which 1 is a dc constant current power supply, 2 is a cathode cell, 3 is a cathode cell auxiliary electrode, 4 is a cathode electrolyte, 5 is a cathode cell through hole, 6 is a first communicating seal ring, 7 is an electrochemical workstation, 8 is a computer, 9 is an anode cell, 10 is an anode cell auxiliary electrode, 11 is an anode cell reference electrode, 12 is an anode electrolyte, 13 is a second communicating seal ring, and 14 is a sample to be measured;
FIG. 2 is a schematic view of the sampling pattern of different micro-regions of the weld joint of the present invention;
FIG. 3 is a graph of hydrogen diffusion profiles obtained using the present invention to determine weld joint micro-zones.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
Example one
A device for measuring the hydrogen diffusion coefficient of a welding joint microcell comprises a cathode electrolytic cell hydrogen charging system, an anode electrolytic cell hydrogen measuring system, a sample to be measured 14 and a computer 8,
the cathode electrolytic cell hydrogen charging system comprises a direct current constant current power supply 1, a cathode cell 2 and a cathode cell auxiliary electrode 3, wherein a cathode electrolyte 4 is filled in the cathode cell 2, the cathode cell auxiliary electrode 3 extends into the cathode electrolyte 4, the cathode cell auxiliary electrode 3 is connected with the anode of the direct current constant current power supply 1 through a lead, and a cathode cell through hole 5 is formed in the side wall of the cathode cell 2;
the anode electrolytic cell hydrogen measuring system comprises an electrochemical workstation 7, an anode cell 9, an anode cell auxiliary electrode 10 and an anode cell reference electrode 11, wherein the anode cell 9 is filled with an anode electrolyte 12, the anode cell auxiliary electrode 10 and the anode cell reference electrode 11 both extend into the anode electrolyte 12, the anode cell auxiliary electrode 10 and the anode cell reference electrode 11 are connected with the electrochemical workstation 7, the electrochemical workstation 7 is connected with a computer 8, an anode cell through hole is formed in the side wall of the anode cell 9, and a cathode cell through hole 5 and the anode cell through hole are oppositely arranged;
the sample 14 to be tested is arranged between the cathode pool through hole 5 and the anode pool through hole, one side surface of the sample 14 to be tested, which is provided with the nickel coating, faces the anode pool 9, one side surface of the sample 14 to be tested, which does not contain the nickel coating, faces the cathode pool 2, and the sample 14 to be tested is respectively connected with the cathode of the direct current constant current power supply 1 and the electrochemical workstation 7 through leads.
Example two
On the basis of example one, the exposed surface area of the sample 14 to be tested in contact with the catholyte 4 and the anolyte 12 is 0.20-1.13cm2。
A first communicating sealing ring 6 is arranged between the sample to be tested 14 and the cathode pool through hole 5, and a second communicating sealing ring 13 is arranged between the sample to be tested 14 and the anode pool through hole.
The current output range of the direct current constant current power supply 1 is 0-3A, and the current output precision is controlled to be 1 mA.
The current measuring range of the electrochemical workstation 7 is 0-3A, the current measuring precision is 10pA, the voltage output range is 0-30V, and the voltage output precision is controlled to be 0.01 mV.
EXAMPLE III
On the basis of the second embodiment, the cathode cell through hole 5 and the anode cell through hole both adopt a structure of a circular truncated cone-shaped through hole, and the cone angle range of the cathode cell through hole 5 and the cone angle range of the anode cell through hole are 30-70 degrees.
The catholyte 4 adopts 0.5mol/L of H2SO4With 3g/L NH4The mixed solution of SCN and the anolyte 12 adopts 0.1mol/L NaAnd (4) OH solution.
The cathode pool 2 and the anode pool 9 both adopt the structure of acrylic organic glass.
The cathode pool auxiliary anode 3 and the anode pool auxiliary electrode 10 both adopt platinum mesh electrodes, and the first communicating sealing ring 6 and the second communicating sealing ring 13 both adopt silica gel gaskets.
Example four
A method for measuring the hydrogen diffusion coefficient of a micro-area of a welded joint comprises the following steps:
step 1, according to the sampling mode of figure 2, the micro heat affected zone extracted from the welding joint is made into an area of 1.0cm2Polishing a sheet sample with the thickness of 1.2mm to 1000# step by using abrasive paper, then respectively carrying out ultrasonic cleaning in acetone and alcohol solution, then electroplating a nickel coating on the surface of the sample, polishing one surface of the nickel-plated sheet sample to 1000# abrasive paper, removing the nickel coating on the surface, reserving the nickel coating on the other surface, finally placing the sample in acetone for ultrasonic cleaning, and washing the sample by using deionized water to prepare a sheet-shaped sample to be detected;
step 2, placing the sheet-shaped sample to be measured prepared in the step 1 between a first communicating sealing ring and a second communicating sealing ring, enabling the surface of one side of the sample to be measured, which is provided with a nickel coating, to face an anode pool, fixing a measuring device on the premise of ensuring good sealing and no liquid leakage, then installing an anode pool auxiliary electrode and an anode pool reference electrode in the anode pool, connecting the anode pool auxiliary electrode and the anode pool reference electrode with the sample to be measured and an electrochemical workstation to form an anode electrolytic cell hydrogen measuring system, and simultaneously connecting the anode electrolytic cell hydrogen measuring system with a computer;
step 3, injecting 0.1mol/L NaOH anolyte into the anode pool, and adjusting the reference potential of the electrochemical workstation to 300mV to enable the whole anode electrolytic cell hydrogen measurement system to start working;
step 4, when the hydrogen permeation current value displayed by the computer is reduced to below 1.0 muA, the recording is suspended and the data recorded by the computer is cleared, then a cathode auxiliary electrode is arranged in the cathode pool, so that the anode and the cathode of the direct current constant current power supply are respectively connected with the cathode auxiliary electrode and the sample to be tested, and simultaneouslyInjecting 0.5mol/L H into the cathode pool2SO4With 3g/L NH4The mixed solution of SCN is used as cathode electrolyte, a direct current constant current power supply is switched on, and the output current density is controlled to be 5mA/cm2Simultaneously, restarting to record the test data;
and 5, after the hydrogen permeation current data recorded by the computer in the step 4 does not rise any more along with the time and keeps in a stable state for a period of time, ending the hydrogen permeation experiment, closing the direct-current constant-current power supply and the electrochemical workstation, storing the experiment data on the computer, finally respectively emptying the catholyte and the anolyte in the cathode pool and the anode pool, taking out the test sample clamped between the two electrodes, and processing the obtained data to obtain a hydrogen diffusion curve, wherein the hydrogen diffusion coefficient of the welding joint micro-area can be obtained by utilizing a known formula for calculation, as shown in figure 3.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.

Claims (10)

1. A measuring device for the hydrogen diffusion coefficient of a welding joint microcell is characterized in that: comprises a cathode electrolytic cell hydrogen charging system, an anode electrolytic cell hydrogen measuring system, a sample to be measured and a computer,
the cathode electrolytic cell hydrogen charging system comprises a direct current constant current power supply, a cathode cell and a cathode cell auxiliary electrode, wherein cathode electrolyte is filled in the cathode cell, the cathode cell auxiliary electrode extends into the cathode electrolyte, the cathode cell auxiliary electrode is connected with the positive electrode of the direct current constant current power supply through a lead, and a cathode cell through hole is formed in the side wall of the cathode cell;
the anode electrolytic cell hydrogen measurement system comprises an electrochemical workstation, an anode cell auxiliary electrode and an anode cell reference electrode, wherein an anode electrolyte is filled in the anode cell, the anode cell auxiliary electrode and the anode cell reference electrode both extend into the anode electrolyte, the anode cell auxiliary electrode and the anode cell reference electrode are connected with the electrochemical workstation, the electrochemical workstation is connected with the computer, an anode cell through hole is formed in the side wall of the anode cell, and the cathode cell through hole and the anode cell through hole are oppositely arranged;
the sample to be tested is arranged between the cathode pool through hole and the anode pool through hole, one side surface of the sample to be tested, which is provided with the nickel coating, faces the anode pool, one side surface of the sample to be tested, which is not provided with the nickel coating, faces the cathode pool, and the sample to be tested is respectively connected with the cathode of the direct current constant current power supply and the electrochemical workstation through leads.
2. The apparatus for determining the hydrogen diffusion coefficient of the micro-area of the weld joint according to claim 1, wherein: the exposed surface area of the sample to be tested in contact with the catholyte and the anolyte is 0.20-1.13cm2。
3. The apparatus for determining the hydrogen diffusion coefficient of the micro-area of the weld joint according to claim 1, wherein: and a first communicating sealing ring is also arranged between the sample to be tested and the through hole of the cathode pool, and a second communicating sealing ring is also arranged between the sample to be tested and the through hole of the anode pool.
4. The apparatus for determining the hydrogen diffusion coefficient of the micro-area of the weld joint according to claim 1, wherein: the current output range of the direct current constant current power supply is 0-3A, and the current output precision is controlled to be 1 mA; the current measuring range of the electrochemical workstation is 0-3A, the current measuring precision is 10pA, the voltage output range is 0-30V, and the control voltage output precision is 0.01 mV.
5. The apparatus for determining the hydrogen diffusion coefficient of the micro-area of the weld joint according to claim 1, wherein: the cathode pool through hole and the anode pool through hole are both in a circular truncated cone type through hole structure, and the taper angle range of the cathode pool through hole and the taper angle range of the anode pool through hole are 30-70 degrees.
6. The apparatus for determining the hydrogen diffusion coefficient of the micro-area of the weld joint according to claim 1, wherein: the catholyte adopts 0.5mol/L H2SO4With 3g/L NH4And the anode electrolyte adopts 0.1mol/L NaOH solution.
7. The apparatus for determining the hydrogen diffusion coefficient of the micro-area of the weld joint according to claim 1, wherein: the cathode pool and the anode pool both adopt an acrylic organic glass structure.
8. The apparatus for determining the hydrogen diffusion coefficient of the micro-area of the weld joint according to claim 1, wherein: the cathode pool auxiliary electrode and the anode pool auxiliary electrode both adopt platinum mesh electrodes, and the first communicating sealing ring and the second communicating sealing ring both adopt silica gel gaskets.
9. A method for measuring the hydrogen diffusion coefficient of a welding joint microcell is characterized by comprising the following steps: the method comprises the following steps:
step 1, manufacturing a micro heat affected zone extracted from a welded joint into a welded joint with an area of 1.0cm2Polishing a sheet sample with the thickness of 1.2mm to 1000# by using abrasive paper, then respectively carrying out ultrasonic cleaning in acetone and alcohol solution, then electroplating a nickel coating on the surface of the sample, polishing one surface of the nickel-plated sheet sample to 1000# abrasive paper, removing the nickel coating on the surface, reserving the nickel coating on the other surface, finally placing the sample in acetone for ultrasonic cleaning, and washing the sample by using deionized water to prepare a sheet-shaped sample to be detected;
step 2, placing the sheet-shaped sample to be measured prepared in the step 1 between a first communicating sealing ring and a second communicating sealing ring, enabling the surface of one side of the sample to be measured, which is provided with a nickel coating, to face an anode pool, fixing a measuring device on the premise of ensuring good sealing and no liquid leakage, then installing an anode pool auxiliary electrode and an anode pool reference electrode in the anode pool, connecting the anode pool auxiliary electrode and the anode pool reference electrode with the sample to be measured and an electrochemical workstation to form an anode electrolytic cell hydrogen measuring system, and simultaneously connecting the anode electrolytic cell hydrogen measuring system with a computer;
step 3, injecting 0.1mol/L NaOH anolyte into the anode pool, and adjusting the reference potential of the electrochemical workstation to 300mV to enable the whole anode electrolytic cell hydrogen measurement system to start working;
step 4, when the hydrogen permeation current value displayed by the computer is reduced to below 1.0 muA, the recording is suspended and the data recorded by the computer is cleared, then a cathode auxiliary electrode is arranged in the cathode pool, the anode and the cathode of the direct current constant current power supply are respectively connected with the cathode auxiliary electrode and the sample to be tested, and simultaneously 0.5mol/L H is injected into the cathode pool2SO4With 3g/L NH4The mixed solution of SCN is used as the cathode electrolyte, a direct current constant current power supply is turned on, and the output current density is controlled to be 5mA/cm2Simultaneously restarting to record test data;
and 5, after the hydrogen permeation current data recorded by the computer in the step 4 does not rise along with the time and keeps a stable state for a period of time, ending the hydrogen permeation experiment, closing the direct current constant current power supply and the electrochemical workstation, storing the experiment data on the computer, finally respectively emptying the catholyte and the anolyte in the cathode pool and the anode pool, taking out the test sample clamped between the two electrodes, processing the obtained data to obtain a hydrogen diffusion curve, and calculating by using a known formula to obtain the hydrogen diffusion coefficient of the welding joint microcell.
10. The device for measuring the hydrogen diffusion coefficient of the micro-area of the welding joint as claimed in any one of claims 1 to 8, which belongs to the technical field of metal corrosion electrochemical test.
CN202110145219.0A 2021-02-02 2021-02-02 Device and method for measuring hydrogen diffusion coefficient of welding joint microcell and application of device and method Pending CN114563341A (en)

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