[go: up one dir, main page]

CN113945509A - A device and method for electrochemical testing in a high temperature liquid phase corrosion environment - Google Patents

A device and method for electrochemical testing in a high temperature liquid phase corrosion environment Download PDF

Info

Publication number
CN113945509A
CN113945509A CN202111281652.3A CN202111281652A CN113945509A CN 113945509 A CN113945509 A CN 113945509A CN 202111281652 A CN202111281652 A CN 202111281652A CN 113945509 A CN113945509 A CN 113945509A
Authority
CN
China
Prior art keywords
liquid
electrochemical
corrosive
salt bridge
liquid phase
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202111281652.3A
Other languages
Chinese (zh)
Inventor
刘承泽
吴金平
赵恒章
徐建平
杨帆
宰伟
余中狄
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xian Rare Metal Materials Research Institute Co Ltd
Original Assignee
Xian Rare Metal Materials Research Institute Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xian Rare Metal Materials Research Institute Co Ltd filed Critical Xian Rare Metal Materials Research Institute Co Ltd
Priority to CN202111281652.3A priority Critical patent/CN113945509A/en
Publication of CN113945509A publication Critical patent/CN113945509A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00Investigating resistance of materials to the weather, to corrosion, or to light
    • G01N17/02Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00Investigating resistance of materials to the weather, to corrosion, or to light
    • G01N17/006Investigating resistance of materials to the weather, to corrosion, or to light of metals

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Biodiversity & Conservation Biology (AREA)
  • Ecology (AREA)
  • Environmental & Geological Engineering (AREA)
  • Environmental Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)

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

Device and method for performing electrochemical test in high-temperature liquid-phase corrosion environment
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)

1.一种高温液相腐蚀环境中进行电化学测试的装置,其特征在于,包括密封的玻璃反应釜(1),所述玻璃反应釜(1)中盛放有腐蚀性液体(2),所述玻璃反应釜(1)上设置有一端伸入腐蚀性液体(2)的盐桥(3),所述盐桥(3)中装有导电介质(3-1),所述盐桥(3)的另一端伸入装有参比液体(4-1)的敞口容器(4),所述敞口容器(4)中设置有伸入参比液体(4-1)的参比电极(5),所述腐蚀性液体(2)中还设置有辅助电极(6)和待测试样品(7),所述玻璃反应釜(1)上部连接有与大气相通的冷凝管(8),所述玻璃反应釜(1)下侧设置有加热台(9),所述参比电极(5)、辅助电极(6)和待测试样品(7)均于电化学工作站(10)连接。1. a device for carrying out electrochemical testing in a high-temperature liquid phase corrosive environment, is characterized in that, comprises a sealed glass reaction still (1), and described glass reaction still (1) contains corrosive liquid (2), The glass reactor (1) is provided with a salt bridge (3) with one end extending into the corrosive liquid (2), the salt bridge (3) is provided with a conductive medium (3-1), and the salt bridge ( 3) The other end extends into the open container (4) containing the reference liquid (4-1), and the open container (4) is provided with a reference electrode extending into the reference liquid (4-1) (5), an auxiliary electrode (6) and a sample to be tested (7) are also provided in the corrosive liquid (2), and the upper part of the glass reactor (1) is connected with a condenser tube (8) communicating with the atmosphere, A heating table (9) is arranged on the lower side of the glass reaction kettle (1), and the reference electrode (5), the auxiliary electrode (6) and the sample to be tested (7) are all connected to the electrochemical workstation (10). 2.根据权利要求1所述的一种高温液相腐蚀环境中进行电化学测试的装置,其特征在于,所述盐桥(3)的中部浸入在冷却容器(11)盛放的冷水中。2 . The device for electrochemical testing in a high temperature liquid phase corrosion environment according to claim 1 , wherein the middle part of the salt bridge ( 3 ) is immersed in the cold water contained in the cooling container ( 11 ). 3 . 3.根据权利要求1所述的一种高温液相腐蚀环境中进行电化学测试的装置,其特征在于,所述导电介质(3-1)与腐蚀性液体(2)成分相同。3 . The device for electrochemical testing in a high temperature liquid phase corrosive environment according to claim 1 , wherein the conductive medium ( 3 - 1 ) has the same composition as the corrosive liquid ( 2 ). 4 . 4.根据权利要求3所述的一种高温液相腐蚀环境中进行电化学测试的装置,其特征在于,所述盐桥(3)两端由多孔玻璃过滤器(3-2)密封。4 . The device for electrochemical testing in a high temperature liquid phase corrosion environment according to claim 3 , wherein both ends of the salt bridge ( 3 ) are sealed by a porous glass filter ( 3 - 2 ). 5 . 5.根据权利要求1所述的一种高温液相腐蚀环境中进行电化学测试的装置,其特征在于,所述参比液体(4-1)的成分与参比电极(5)中的液体成分相同。5. The device for carrying out electrochemical testing in a high temperature liquid phase corrosion environment according to claim 1, wherein the composition of the reference liquid (4-1) and the liquid in the reference electrode (5) The ingredients are the same. 6.根据权利要求1所述的一种高温液相腐蚀环境中进行电化学测试的装置,其特征在于,所述加热台(9)连接有伸入腐蚀性液体(2)中的热电偶(12)。6. The device for carrying out electrochemical testing in a high temperature liquid phase corrosive environment according to claim 1, wherein the heating table (9) is connected with a thermocouple (2) extending into the corrosive liquid (2). 12). 7.一种使用如权利要求1~6中任一权利要求所述的装置在高温液相腐蚀环境中进行电化学测试的方法,其特征在于,该方法包括以下步骤:7. A method for conducting electrochemical testing in a high temperature liquid phase corrosion environment using the device according to any one of claims 1 to 6, wherein the method comprises the following steps: 步骤一、将腐蚀性液体(2)倒入玻璃反应釜(1),然后将玻璃反应釜(1)放在加热台(9),随后连接热电偶(12)、冷凝管(8)、盐桥(3)和敞口容器(4),得到初步装置;所述盐桥(3)中装有导电介质(3-1),所述敞口容器(4)中装有参比液体(4-1),所述盐桥(3)的中部浸入在冷却容器(11)盛放的冷水中;Step 1. Pour the corrosive liquid (2) into the glass reactor (1), then place the glass reactor (1) on the heating table (9), then connect the thermocouple (12), the condenser tube (8), the salt A bridge (3) and an open container (4) are used to obtain a preliminary device; a conductive medium (3-1) is installed in the salt bridge (3), and a reference liquid (4) is installed in the open container (4). -1), the middle part of described salt bridge (3) is immersed in the cold water that cooling container (11) holds; 步骤二、将初步装置中玻璃反应釜(1)内放入待测试样品(7)和辅助电极(6),然后将参比电极(5)、辅助电极(6)和待测试样品(7)与电化学工作站(10)连接,得到电化学测试装置;Step 2. Put the sample to be tested (7) and the auxiliary electrode (6) in the glass reactor (1) of the preliminary device, and then place the reference electrode (5), the auxiliary electrode (6) and the sample to be tested (7) Connect with the electrochemical workstation (10) to obtain an electrochemical test device; 步骤三、将步骤二中得到的电化学测试装置的冷凝管(8)通入冷凝水,然后打开加热台(9),至玻璃反应釜(1)中的腐蚀性液体(2)达到指定温度后打开电化学工作站(10),进行高温液相腐蚀环境中的电化学测试。Step 3, pass the condensation pipe (8) of the electrochemical test device obtained in the step 2 into condensed water, then open the heating table (9), until the corrosive liquid (2) in the glass reactor (1) reaches the specified temperature Afterwards, the electrochemical workstation (10) is opened to perform electrochemical tests in a high temperature liquid phase corrosion environment. 8.根据权利要求7所述的方法,其特征在于,步骤三中所述达到指定温度60min~240min后打开电化学工作站(10)。8 . The method according to claim 7 , wherein the electrochemical workstation ( 10 ) is turned on after reaching the specified temperature for 60 min to 240 min in step 3 .
CN202111281652.3A 2021-11-01 2021-11-01 A device and method for electrochemical testing in a high temperature liquid phase corrosion environment Pending CN113945509A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111281652.3A CN113945509A (en) 2021-11-01 2021-11-01 A device and method for electrochemical testing in a high temperature liquid phase corrosion environment

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111281652.3A CN113945509A (en) 2021-11-01 2021-11-01 A device and method for electrochemical testing in a high temperature liquid phase corrosion environment

Publications (1)

Publication Number Publication Date
CN113945509A true CN113945509A (en) 2022-01-18

Family

ID=79337411

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111281652.3A Pending CN113945509A (en) 2021-11-01 2021-11-01 A device and method for electrochemical testing in a high temperature liquid phase corrosion environment

Country Status (1)

Country Link
CN (1) CN113945509A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114878451A (en) * 2022-05-05 2022-08-09 东南大学 A device and method for testing the electrochemical properties of wire rod stress corrosion
CN115683997A (en) * 2022-12-14 2023-02-03 西安稀有金属材料研究院有限公司 Rotary coupon corrosion experiment device and method

Citations (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4906348A (en) * 1987-08-21 1990-03-06 Hitachi, Ltd. Flow-through cell provided with reference electrode
JPH0821815A (en) * 1994-05-31 1996-01-23 Shukuji Asakura Corroded state detecting method and device for water feed/drainage device and water feed/drainage device equipped with this detecting device
JP2005339902A (en) * 2004-05-25 2005-12-08 Toyota Motor Corp Corrosion evaluation apparatus, fuel cell separator, fuel cell and vehicle
CN101639459A (en) * 2008-08-01 2010-02-03 中国科学院理化技术研究所 Method and device for detecting chemical oxygen demand of water body
CN102937616A (en) * 2011-12-27 2013-02-20 北京化工大学 Electrolytic cell with controllable temperature used for electrochemical measurement
CN102937569A (en) * 2011-12-27 2013-02-20 北京化工大学 A stress corrosion test device
CN203720141U (en) * 2013-12-13 2014-07-16 中国科学院大连化学物理研究所 Reference electrode system applied to non-normal temperature electrochemical experiment
CN204255822U (en) * 2014-09-03 2015-04-08 中石化洛阳工程有限公司 A kind of nickel-base alloy pitting resistance evaluating apparatus
CN204945086U (en) * 2015-08-07 2016-01-06 刘桓肇 For the external pressure balance type Ag/AgCl contrast electrode system of high temperature and pressure experiment
CN105388103A (en) * 2014-09-03 2016-03-09 中石化洛阳工程有限公司 Evaluation method and device for pitting corrosion resistance of nickel base alloy
CN105973795A (en) * 2016-06-17 2016-09-28 南京钢铁股份有限公司 Simple composite electrode for experiment in erosive electrochemistry
CN207396305U (en) * 2017-08-23 2018-05-22 于安泓 A kind of static corrosion test device
CN109752425A (en) * 2017-11-06 2019-05-14 杨钟明 A kind of PH measuring device for pyrosol
CN109900630A (en) * 2019-01-31 2019-06-18 中国科学院金属研究所 It is a kind of to evaluate complicated metal pair to the test device and method of galvanic corrosion
CN210953753U (en) * 2019-10-29 2020-07-07 西安热工研究院有限公司 Device for using saturated calomel reference electrode for corrosion electrochemical measurement under high temperature condition
CN113777021A (en) * 2021-08-23 2021-12-10 中国科学院金属研究所 An experimental device for simulating three-phase corrosion of boiling nitric acid in spent fuel reprocessing
CN113933366A (en) * 2021-08-26 2022-01-14 上海空间电源研究所 A fuel cell bipolar plate electrochemical test device

Patent Citations (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4906348A (en) * 1987-08-21 1990-03-06 Hitachi, Ltd. Flow-through cell provided with reference electrode
JPH0821815A (en) * 1994-05-31 1996-01-23 Shukuji Asakura Corroded state detecting method and device for water feed/drainage device and water feed/drainage device equipped with this detecting device
JP2005339902A (en) * 2004-05-25 2005-12-08 Toyota Motor Corp Corrosion evaluation apparatus, fuel cell separator, fuel cell and vehicle
CN101639459A (en) * 2008-08-01 2010-02-03 中国科学院理化技术研究所 Method and device for detecting chemical oxygen demand of water body
CN102937616A (en) * 2011-12-27 2013-02-20 北京化工大学 Electrolytic cell with controllable temperature used for electrochemical measurement
CN102937569A (en) * 2011-12-27 2013-02-20 北京化工大学 A stress corrosion test device
CN203720141U (en) * 2013-12-13 2014-07-16 中国科学院大连化学物理研究所 Reference electrode system applied to non-normal temperature electrochemical experiment
CN105388103A (en) * 2014-09-03 2016-03-09 中石化洛阳工程有限公司 Evaluation method and device for pitting corrosion resistance of nickel base alloy
CN204255822U (en) * 2014-09-03 2015-04-08 中石化洛阳工程有限公司 A kind of nickel-base alloy pitting resistance evaluating apparatus
CN204945086U (en) * 2015-08-07 2016-01-06 刘桓肇 For the external pressure balance type Ag/AgCl contrast electrode system of high temperature and pressure experiment
CN105973795A (en) * 2016-06-17 2016-09-28 南京钢铁股份有限公司 Simple composite electrode for experiment in erosive electrochemistry
CN207396305U (en) * 2017-08-23 2018-05-22 于安泓 A kind of static corrosion test device
CN109752425A (en) * 2017-11-06 2019-05-14 杨钟明 A kind of PH measuring device for pyrosol
CN109900630A (en) * 2019-01-31 2019-06-18 中国科学院金属研究所 It is a kind of to evaluate complicated metal pair to the test device and method of galvanic corrosion
CN210953753U (en) * 2019-10-29 2020-07-07 西安热工研究院有限公司 Device for using saturated calomel reference electrode for corrosion electrochemical measurement under high temperature condition
CN113777021A (en) * 2021-08-23 2021-12-10 中国科学院金属研究所 An experimental device for simulating three-phase corrosion of boiling nitric acid in spent fuel reprocessing
CN113933366A (en) * 2021-08-26 2022-01-14 上海空间电源研究所 A fuel cell bipolar plate electrochemical test device

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
胡会利 等: "《电化学测量》", 国防工业出版社, pages: 68 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114878451A (en) * 2022-05-05 2022-08-09 东南大学 A device and method for testing the electrochemical properties of wire rod stress corrosion
CN115683997A (en) * 2022-12-14 2023-02-03 西安稀有金属材料研究院有限公司 Rotary coupon corrosion experiment device and method

Similar Documents

Publication Publication Date Title
JP5503972B2 (en) Method and specimen for pretreatment of fuel rod cladding for material testing
CN113945509A (en) A device and method for electrochemical testing in a high temperature liquid phase corrosion environment
TWI649549B (en) Electrochemical detection of corrosion in molten salt at high temperature and corrosion rate of metal
CN113848174B (en) Electrochemical corrosion test device under boiling and strong corrosive solution environment and application thereof
Yang et al. Electrochemical study on the kinetic properties of Fe2+/Fe, Ni2+/Ni, Cr2+/Cr and Cr3+/Cr2+ in molten MgCl2-KCl-NaCl salts
CN106370510A (en) Method for microwave digestion of glass body
JP4538640B2 (en) Hydrogen sensor
Bai et al. In Situ Monitoring Techniques and Analysis Theory for Electrochemical Corrosion in Subcritical and Supercritical Aqueous Systems
CN110687019A (en) A device and method for electrochemical hydrogen permeation measurement in high temperature environment
JPH0212051A (en) Apparatus and method for measuring concentration of hydrogen in water
CN115112551B (en) A dissolution kinetic reaction device resistant to acid corrosion and its experimental method
RU2096773C1 (en) Gear measuring thermal conductivity
Pecsok et al. Determination of Molybdenum by Ion Exchange and Polarography
de Jong et al. Coatings for heat storage reactors with hygroscopic salts
CN217277296U (en) High-pressure sealing digestion device for measuring chemical oxygen demand by volumetric method
CN109507101B (en) Electrode device, high-temperature high-pressure pitting potential detection device and high-temperature high-pressure pitting potential detection method
CN107843794A (en) One kind analysis oxygen Ni―Ti anode accelerating lifetime testing device and method of testing
CN106644915A (en) Device and method for evaluating nitric acid corrosion
Lefevre et al. Potentiometry up to 275 C: example of pH titrations of cobalt ferrite particles
CN205449973U (en) Water quality monitoring devices with survey water sample preheating device
CN216900315U (en) Critical point corrosion temperature test system
CN117629869B (en) Method, device and system for detecting equipment damage rate
Wang et al. The Effects of Cl− and Selected Deoxidizers on the High-Temperature Corrosion Electrochemistry of Alloy 690 in Nuclear Steam Generator Water
CN118858139A (en) A method for measuring the critical pitting temperature of stainless steel and its weld in Cl- environment
CN119757179A (en) An electrochemical testing device and testing method suitable for high temperature inflation conditions

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20220118