CN113945509A - Device and method for performing electrochemical test in high-temperature liquid-phase corrosion environment - Google Patents
Device and method for performing electrochemical test in high-temperature liquid-phase corrosion environment Download PDFInfo
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Abstract
The invention discloses a device for carrying out electrochemical test in a high-temperature liquid-phase corrosion environment, which comprises a glass reaction kettle for containing corrosive liquid, wherein a salt bridge for containing a conductive medium is arranged on the glass reaction kettle, the other end of the salt bridge extends into an open container for containing reference liquid, a reference electrode is arranged in the open container, and an auxiliary electrode and a sample to be tested are arranged in the glass reaction kettle; in addition, the invention also provides a method for carrying out electrochemical test in a high-temperature liquid phase corrosion environment, the obtained current-time curve is smooth, the numerical value is stable, the obtained polarization curve is a standard curve, and key parameters such as self-corrosion potential, self-corrosion current, Vicat current density and the like can be visually measured from the curve.
Description
Technical Field
The invention belongs to the technical field of electrochemical tests, and particularly relates to a device and a method for performing electrochemical tests in a high-temperature liquid-phase corrosion environment.
Background
Failure due to corrosion is one of the most common and most harmful failure modes of metallic materials. The research on the corrosion resistance of the metal material is the basic guarantee for researching and developing the corrosion-resistant metal material. The principle of the method is that a three-electrode system is utilized, and the corrosion resistance of the metal material is evaluated by measuring parameters such as corrosion potential, corrosion current and the like of the metal material to be tested at a specific temperature and in a liquid medium.
At present, the evaluation of the corrosion resistance of the metal material serving under extreme conditions has extremely high difficulty. The reason is that the corrosion experiment condition for simulating the extreme condition is difficult to achieve, and meanwhile, under the extreme condition, the electrochemical test signal, the stability of the electrode material and the like are affected by severe conditions such as high temperature and strong corrosion, so that the accuracy and repeatability of the test result are seriously reduced, and even the condition of incapability of testing is generated. Although the prior art can avoid the direct contact between the reference electrode and the medium to be measured, the prior art cannot simultaneously avoid the measurement error caused by the temperature rise of the reference electrode under the high-temperature condition.
It is highly desirable to have a device and method for electrochemical testing in high temperature liquid phase corrosive environments.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a device for performing electrochemical tests in a high temperature liquid phase corrosive environment, aiming at the above-mentioned deficiencies of the prior art. The device extends glass reation kettle's salt bridge and uncovered container structure through the design on glass reation kettle, switch on corrosive liquids and reference liquid, make reference electrode and auxiliary electrode and the examination sample that awaits measuring be in same return circuit, guaranteed to carry out the electronic exchange smoothly between corrosive liquids and the reference liquid, make the reference electrode need not to put into the corrosive liquids of high temperature, provide stable operational environment for the reference electrode, the temperature of being in service of reference electrode has been reduced, guarantee electrochemical signal's stability, prevent that high temperature and corrosive liquids from leading to the fact the influence to the reference electrode, the going on smoothly of electrochemistry test has been guaranteed.
In order to solve the technical problems, the invention adopts the technical scheme that: the device for carrying out the electrochemical test in the high-temperature liquid-phase corrosion environment is characterized by comprising a sealed glass reaction kettle, wherein corrosive liquid is contained in the glass reaction kettle, a salt bridge with one end extending into the corrosive liquid is arranged on the glass reaction kettle, a dielectric medium is contained in the salt bridge, the other end of the salt bridge extends into an open container filled with reference liquid, a reference electrode extending into the reference liquid is arranged in the open container, an auxiliary electrode and a sample to be tested are also arranged in the corrosive liquid, a condenser pipe communicated with the atmosphere is connected to the upper portion of the glass reaction kettle, a heating table is arranged on the lower side of the glass reaction kettle, and the reference electrode, the auxiliary electrode and the sample to be tested are all connected in an electrochemical workstation.
The device for carrying out electrochemical test in the high-temperature liquid phase corrosion environment is characterized in that the middle part of the salt bridge is immersed in cold water contained in a cooling container.
The device for performing electrochemical test in high-temperature liquid-phase corrosive environment is characterized in that the conductive medium and the corrosive liquid have the same components.
The device for carrying out electrochemical test in high-temperature liquid phase corrosive environment is characterized in that two ends of the salt bridge are sealed by porous glass filters.
The device for performing electrochemical tests in the high-temperature liquid-phase corrosive environment is characterized in that the components of the reference liquid are the same as those of the liquid in the reference electrode.
The device for performing electrochemical test in the high-temperature liquid-phase corrosive environment is characterized in that the heating table is connected with a thermocouple extending into corrosive liquid.
In addition, the invention provides a method for carrying out electrochemical test in a high-temperature liquid phase corrosion environment, which is characterized by comprising the following steps:
pouring corrosive liquid into a glass reaction kettle, then placing the glass reaction kettle on a heating table, and then connecting a thermocouple, a condenser pipe, a salt bridge and an open container to obtain a primary device; the salt bridge is provided with a conductive medium, the open container is provided with a reference liquid, and the middle part of the salt bridge is immersed in cold water contained in the cooling container;
step two, placing a sample to be tested and an auxiliary electrode in a glass reaction kettle in the primary device, and then connecting the reference electrode, the auxiliary electrode and the sample to be tested with an electrochemical workstation to obtain an electrochemical testing device;
and step three, introducing condensed water into a condensation pipe of the electrochemical testing device obtained in the step two, then opening a heating table, opening an electrochemical workstation after corrosive liquid in the glass reaction kettle reaches a specified temperature, and carrying out electrochemical testing in a high-temperature liquid phase corrosion environment.
The method is characterized in that the electrochemical workstation is opened after the specified temperature is reached for 60-240 min in the third step. According to the invention, the time for opening the electrochemical workstation after the specified temperature is reached is controlled, so that the stability of the high-temperature corrosion environment in the glass reaction kettle is ensured, and the stable performance of the electrochemical test is ensured.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the structure of the salt bridge and the open container which extend out of the glass reaction kettle is designed on the glass reaction kettle, and the corrosive liquid and the reference liquid are conducted, so that the reference electrode, the auxiliary electrode and the sample to be tested are in the same loop, thereby ensuring that the corrosive liquid and the reference liquid are smoothly electronically exchanged, avoiding the need of putting the reference electrode into the high-temperature corrosive liquid, providing a stable working environment for the reference electrode, reducing the service temperature of the reference electrode, ensuring the stability of an electrochemical signal, preventing the high-temperature corrosive liquid from influencing the reference electrode, and ensuring the smooth implementation of an electrochemical test.
2. The invention realizes the heating and temperature control of corrosive liquid in the glass kettle through the temperature-controllable heating table, and ensures the repeatability of test conditions; carry out the condensation backward flow through the corrosive steam of condenser pipe to high temperature production, prevent to change because of the liquid medium composition that volatilizees and lead to in the experimentation, reduce the harm of corrosive steam to personnel and environment simultaneously.
3. The invention provides a method for performing electrochemical test in a high-temperature liquid phase corrosion environment, which can realize a method for stably testing electrochemical data in the high-temperature liquid phase environment with the pH value ranging from 3 to 14 at the temperature of between room temperature and 120 ℃, the obtained current-time curve is smooth, the numerical value is stable, the obtained polarization curve is a standard curve, and key parameters such as self-corrosion potential, self-corrosion current, Victoria current density and the like can be visually measured from the curve.
4. The invention is suitable for testing the electrochemical performance of a metal material in a high-temperature liquid phase corrosion environment, and relates to the fields of nuclear power, chemical industry, pharmacy, oceans, weaponry, energy and the like.
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 an apparatus for performing electrochemical tests in a high temperature liquid phase corrosive environment according to the present invention.
FIG. 2 is a graph of current versus time obtained for example 2 of the present invention and comparative example 1.
FIG. 3 is a graph showing polarization curves obtained in example 2 of the present invention and comparative example 1.
Description of reference numerals:
1-a glass reaction kettle; 2-corrosive liquid; 3-salt bridge;
3-1-a conductive medium; 3-2-porous glass filter; 4-an open container;
4-1-reference liquid; 5-a reference electrode; 6-auxiliary electrode;
7-a sample to be tested; 8-a condenser pipe; 9-heating table;
10-an electrochemical workstation; 11-cooling the container; 12-thermocouple.
Detailed Description
An apparatus for performing electrochemical tests in a high temperature liquid phase corrosive environment of the present invention is described in detail in example 1.
Example 1
As shown in fig. 1, the device for electrochemical testing in high temperature liquid phase corrosive environment of this embodiment comprises a sealed glass reaction vessel 1, the glass reaction kettle 1 is filled with corrosive liquid 2, the glass reaction kettle 1 is provided with a salt bridge 3 with one end extending into the corrosive liquid 2, a conductive medium 3-1 is arranged in the salt bridge 3, the other end of the salt bridge 3 extends into an open container 4 filled with a reference liquid 4-1, a reference electrode 5 extending into the reference liquid 4-1 is arranged in the open container 4, an auxiliary electrode 6 and a sample 7 to be tested are also arranged in the corrosive liquid 2, the upper part of the glass reaction kettle 1 is connected with a condensing pipe 8 communicated with the atmosphere, the lower side of the glass reaction kettle 1 is provided with a heating platform 9, the reference electrode 5, the auxiliary electrode 6 and the sample 7 to be tested are all connected with an electrochemical workstation 10.
It should be noted that, through setting up sealed glass reation kettle 1 and holding corrosive liquid 2, provide confined high temperature liquid phase corrosive environment for the electrochemistry test, prevent because the corrosive gas that the heating produced is excessive, increased the security and the reliability of experiment.
It should be noted that, by designing the salt bridge 3 and the open container 4 structure extending out of the glass reaction vessel 1 on the glass reaction vessel 1, on the premise of ensuring that the concentration of the liquid medium of the reference electrode 5 is not changed, the service temperature of the reference electrode 5 is reduced, the stability of the electrochemical signal is ensured, the corrosive liquid 2 and the reference liquid 4-1 are conducted through the salt bridge 3, smooth electronic exchange between the corrosive liquid 2 and the reference liquid 4-1 is ensured, the reference electrode 5, the auxiliary electrode 6 and the sample to be tested 7 are in a loop, the smooth proceeding of the electrochemical test is ensured, a stable working environment is provided for the reference electrode 5 through the open container 4, the influence of the high temperature and the corrosive liquid 2 on the reference electrode 5 is prevented, and the smooth proceeding of the electrochemical test is ensured.
The auxiliary electrode 6 and the sample 7 to be tested are placed in the glass reaction kettle 1, and the reference electrode 5, the auxiliary electrode 6 and the sample 7 to be tested are connected with the electrochemical workstation 10, so that the electrochemical test of the sample 7 to be tested in a high-temperature liquid phase corrosion environment is completed.
It should be noted that, the upper part of the glass reaction kettle 1 is connected with the condensing pipe 8 communicated with the atmosphere, so that the inside of the glass reaction kettle 1 is communicated with the atmosphere, the defect of danger caused by overlarge internal pressure of the glass reaction kettle 1 is avoided, the condensing pipe 8 is used for condensing corrosive steam generated in the heating process, the corrosive steam is prevented from entering the atmosphere, the device has the advantage of environmental friendliness, and the safety and the reliability of the experiment are improved.
The heating table 9 is arranged on the lower side of the glass reaction kettle 1, so that the corrosive liquid 2 in the glass reaction kettle 1 is heated, and a high-temperature liquid phase corrosion environment is provided for an electrochemical test.
In this embodiment, the middle of the salt bridge 3 is immersed in cold water contained in the cooling vessel 11. The middle part of the salt bridge 3 is immersed in cold water contained in a cooling container 11, so that the conductive medium 3-1 in the salt bridge 3 is cooled, heat is prevented from being conducted to an open container 4 and a reference electrode 5 from a glass reaction kettle 1, the service temperature of the reference electrode 5 is reduced, and the stability of an electrochemical signal is ensured; the cooling water in the cooling container 11 is circularly introduced, so that the cooling water contained in the cooling container 11 is always kept at a lower temperature level, and the cooling effect is further ensured.
In this embodiment, the conductive medium 3-1 and the corrosive liquid 2 have the same composition. By making the conductive medium 3-1 and the corrosive liquid 2 have the same composition, the influence of extra ions in the glass reaction kettle 1 on the test result is avoided.
In this embodiment, the salt bridge 3 is sealed at both ends by a porous glass filter 3-2. Through using porous glass filter 3-2 sealed at 3 both ends of salt bridge, guaranteed that conducting medium 3-1 in the salt bridge 3 can not flow out from salt bridge 3, thereby prevent that corrosive liquids 2 from getting into uncovered container 4 and influencing reference electrode 5, under the prerequisite of guaranteeing that the electron switches on, avoid the ion in uncovered container 4 to get into glass reation kettle 1 through salt bridge 3 and influence the test result.
In this embodiment, the composition of the reference liquid 4-1 is the same as the liquid composition in the reference electrode 5. Hold the liquid the same with 5 solution composition of reference electrode in the uncovered container 4, can avoid solution concentration change in the reference electrode 5 and influence the test result, if use corrosive solution, then lead to 5 inefficacy of reference electrode, reference electrode 5 can't use in high temperature, strong corrosive medium.
It should be noted that, the liquid in the open container 4 is the non-corrosive liquid 2 at normal temperature, and does not need to be sealed, so the open container is designed to be open, and can play a role in heat dissipation.
In this embodiment, the heating stage 9 is connected to a thermocouple 12 that extends into the corrosive liquid 2. Through the heating table 9 and the thermocouple 12 stretching into the corrosive liquid 2, the temperature of the corrosive liquid 2 is accurately controlled, and the temperature in the electrochemical test is accurately controlled.
The method of electrochemical testing in a high temperature liquid phase corrosive environment of the present invention is described in detail by examples 2 to 4.
Example 2
The embodiment comprises the following steps:
pouring corrosive liquid 2 into a glass reaction kettle 1, then placing the glass reaction kettle 1 on a heating table 9, and then connecting a thermocouple 12, a condenser pipe 8, a salt bridge 3 and an open container 4 to obtain a primary device; a conductive medium 3-1 is arranged in the salt bridge 3, the conductive medium 3-1 and the corrosive liquid 2 have the same components, a reference liquid 4-1 is arranged in the open container 4, and the middle part of the salt bridge 3 is immersed in cold water contained in the cooling container 11; the corrosive liquid 2 is a nitric acid solution of 8 mol/L; the reference liquid 4-1 is a saturated KCl solution;
step two, placing a sample 7 to be tested and an auxiliary electrode 6 into a glass reaction kettle 1 in the primary device, and then connecting a reference electrode 5, the auxiliary electrode 6 and the sample 7 to be tested with an electrochemical workstation 10 to obtain an electrochemical testing device; sample 7 to be tested was TA 2; the reference electrode 5 is an AgCl/saturated KCl reference electrode;
step three, introducing condensed water into a condensation pipe 8 of the electrochemical testing device obtained in the step two, then opening a heating table 9 until the corrosive liquid 2 in the glass reaction kettle 1 boils, then opening an electrochemical workstation 10, and carrying out electrochemical testing in a high-temperature liquid phase corrosion environment to obtain a current-time curve and a polarization curve; the electrochemical workstation 10 was opened after said boiling for 60 min.
Comparative example 1
The embodiment comprises the following steps:
pouring corrosive liquid 2 into a glass reaction kettle 1, then placing the glass reaction kettle 1 on a heating table 9, and then connecting a thermocouple 12 and a condenser pipe 8 to obtain a primary device; the corrosive liquid 2 is a nitric acid solution of 8 mol/L;
step two, placing a sample 7 to be tested, an auxiliary electrode 6 and a reference electrode 5 into a glass reaction kettle 1 in the primary device, and then connecting the reference electrode 5, the auxiliary electrode 6 and the sample 7 to be tested with an electrochemical workstation 10 to obtain an electrochemical testing device; sample 7 to be tested was TA 2; the reference electrode 5 is an AgCl/saturated KCl reference electrode;
step three, introducing condensed water into a condensation pipe 8 of the electrochemical testing device obtained in the step two, then opening a heating table 9 until the corrosive liquid 2 in the glass reaction kettle 1 boils, then opening an electrochemical workstation 10, and carrying out electrochemical testing in a high-temperature liquid phase corrosion environment to obtain a current-time curve and a polarization curve; the electrochemical workstation 10 was opened after said boiling for 60 min.
Fig. 2 is a graph of current versus time obtained in example 2 of the present invention and comparative example 1, and it can be seen from fig. 2 that the current versus time curve obtained in example 2 is smooth and stable in value, while the current versus time curve obtained in comparative example 1 is greatly fluctuated and unstable in value.
Fig. 3 is a polarization curve diagram obtained in example 2 and comparative example 1 of the present invention, and it can be seen from fig. 3 that the polarization curve measured in example 2 is a standard curve, key parameters such as self-corrosion potential, self-corrosion current, and wiener current density can be visually measured from the standard curve, and the polarization curve measured in comparative example 1 has a plurality of inflection points, so that the key parameters such as self-corrosion potential, self-corrosion current, and wiener current density cannot be accurately determined.
As can be seen from comparison between the comparative example 1 and the example 1, the salt bridge 3 and the open container 4 extending out of the glass reaction kettle 1 are designed, so that the service temperature of the reference electrode 5 is reduced and the stability of electrochemical signals is ensured on the premise that the concentration of a liquid medium in which the reference electrode 5 is located is unchanged.
Example 3
The embodiment comprises the following steps:
pouring corrosive liquid 2 into a glass reaction kettle 1, then placing the glass reaction kettle 1 on a heating table 9, and then connecting a thermocouple 12, a condenser pipe 8, a salt bridge 3 and an open container 4 to obtain a primary device; a conductive medium 3-1 is arranged in the salt bridge 3, the conductive medium 3-1 and the corrosive liquid 2 have the same components, a reference liquid 4-1 is arranged in the open container 4, and the middle part of the salt bridge 3 is immersed in cold water contained in the cooling container 11; the corrosive liquid 2 is a sulfuric acid solution with the mass concentration of 60%; the reference liquid 4-1 is a saturated KCl solution;
step two, placing a sample 7 to be tested and an auxiliary electrode 6 into a glass reaction kettle 1 in the primary device, and then connecting a reference electrode 5, the auxiliary electrode 6 and the sample 7 to be tested with an electrochemical workstation 10 to obtain an electrochemical testing device; the sample to be tested 7 is Zr 702; the reference electrode 5 is an AgCl/saturated KCl reference electrode;
step three, introducing condensed water into a condensation pipe 8 of the electrochemical testing device obtained in the step two, then opening a heating table 9, opening an electrochemical workstation 10 after the corrosive liquid 2 in the glass reaction kettle 1 reaches 80 ℃, and carrying out electrochemical testing in a high-temperature liquid phase corrosion environment to obtain a current-time curve and a polarization curve; the electrochemical workstation 10 was opened 120min after said 80 ℃.
Through detection, the current-time curve obtained by the embodiment is smooth, the numerical value is stable, and key parameters such as self-corrosion potential, self-corrosion current, Victoria current density and the like can be visually measured in the obtained polarization curve.
Example 4
The embodiment comprises the following steps:
pouring corrosive liquid 2 into a glass reaction kettle 1, then placing the glass reaction kettle 1 on a heating table 9, and then connecting a thermocouple 12, a condenser pipe 8, a salt bridge 3 and an open container 4 to obtain a primary device; a conductive medium 3-1 is arranged in the salt bridge 3, the conductive medium 3-1 and the corrosive liquid 2 have the same components, a reference liquid 4-1 is arranged in the open container 4, and the middle part of the salt bridge 3 is immersed in cold water contained in the cooling container 11; the corrosive liquid 2 is 6mol/L NaOH solution; the reference liquid 4-1 is a saturated KCl solution;
step two, placing a sample 7 to be tested and an auxiliary electrode 6 into a glass reaction kettle 1 in the primary device, and then connecting a reference electrode 5, the auxiliary electrode 6 and the sample 7 to be tested with an electrochemical workstation 10 to obtain an electrochemical testing device; the sample to be tested 7 is TC 4; the reference electrode 5 is an AgCl/saturated KCl reference electrode;
step three, introducing condensed water into a condensation pipe 8 of the electrochemical testing device obtained in the step two, then opening a heating table 9 until the corrosive liquid 2 in the glass reaction kettle 1 boils, then opening an electrochemical workstation 10, and carrying out electrochemical testing in a high-temperature liquid phase corrosion environment to obtain a current-time curve and a polarization curve; the electrochemical workstation 10 was opened after said boiling for 240 min.
Through detection, the current-time curve obtained by the embodiment is smooth, the numerical value is stable, and key parameters such as self-corrosion potential, self-corrosion current, Victoria current density and the like can be visually measured in the obtained polarization curve.
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 (8)
1. The device for carrying out the electrochemical test in the high-temperature liquid phase corrosion environment is characterized by comprising a sealed glass reaction kettle (1), corrosive liquid (2) is contained in the glass reaction kettle (1), a salt bridge (3) with one end stretching into the corrosive liquid (2) is arranged on the glass reaction kettle (1), a conductive medium (3-1) is contained in the salt bridge (3), the other end of the salt bridge (3) stretches into an open container (4) containing the reference liquid (4-1), a reference electrode (5) stretching into the reference liquid (4-1) is arranged in the open container (4), an auxiliary electrode (6) and a sample (7) to be tested are also arranged in the corrosive liquid (2), a condensing pipe (8) communicated with the atmosphere is connected to the upper part of the glass reaction kettle (1), a heating table (9) is arranged on the lower side of the glass reaction kettle (1), the reference electrode (5), the auxiliary electrode (6) and the sample (7) to be tested are all connected with an electrochemical workstation (10).
2. An apparatus for electrochemical testing in a hot liquid phase corrosive environment according to claim 1, wherein the middle of said salt bridge (3) is immersed in cold water contained in a cooling vessel (11).
3. The apparatus for electrochemical testing in a high temperature liquid phase corrosive environment according to claim 1, wherein said conductive medium (3-1) is the same composition as the corrosive liquid (2).
4. A device for electrochemical tests in a hot liquid phase corrosive environment according to claim 3, characterized in that said salt bridge (3) is sealed at both ends by a porous glass filter (3-2).
5. An apparatus for electrochemical testing in a high temperature liquid phase corrosive environment according to claim 1, wherein the composition of said reference liquid (4-1) is the same as the composition of the liquid in the reference electrode (5).
6. An apparatus for electrochemical testing in a high temperature liquid phase corrosive environment according to claim 1, characterized in that a thermocouple (12) is connected to the heating stage (9) and extends into the corrosive liquid (2).
7. A method for performing electrochemical testing in a high temperature liquid phase corrosive environment using the apparatus of any one of claims 1 to 6, the method comprising the steps of:
pouring corrosive liquid (2) into a glass reaction kettle (1), then placing the glass reaction kettle (1) on a heating table (9), and then connecting a thermocouple (12), a condenser pipe (8), a salt bridge (3) and an open container (4) to obtain a primary device; a conductive medium (3-1) is arranged in the salt bridge (3), a reference liquid (4-1) is arranged in the open container (4), and the middle part of the salt bridge (3) is immersed in cold water contained in the cooling container (11);
step two, placing a sample (7) to be tested and an auxiliary electrode (6) into a glass reaction kettle (1) in the primary device, and then connecting a reference electrode (5), the auxiliary electrode (6) and the sample (7) to be tested with an electrochemical workstation (10) to obtain an electrochemical testing device;
and step three, introducing condensed water into a condensation pipe (8) of the electrochemical testing device obtained in the step two, then opening a heating table (9), opening an electrochemical workstation (10) after the corrosive liquid (2) in the glass reaction kettle (1) reaches a specified temperature, and carrying out electrochemical testing in a high-temperature liquid phase corrosion environment.
8. The method according to claim 7, characterized in that the electrochemical workstation (10) is opened 60-240 min after the specified temperature is reached in step three.
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