CN113848174A - Electrochemical corrosion test device in boiling and strong corrosive solution environment and application thereof - Google Patents
Electrochemical corrosion test device in boiling and strong corrosive solution environment and application thereof Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/02—Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Abstract
The invention discloses an electrochemical corrosion test device in boiling and strong corrosive solution environment and application thereof, wherein the test device comprises a test container, a sample support body interface, a reference electrode interface, an auxiliary electrode interface and a steam circulation pressure reducer interface are arranged on the test container, and the sample support body interface, the reference electrode interface, the auxiliary electrode interface and the steam circulation pressure reducer interface are respectively provided with a working electrode sample support body, a reference electrode support body, an auxiliary electrode and a steam circulation pressure reducer; the working electrode sample support and the reference electrode support are each provided with a cooling unit, and the lead of the working electrode sample support is subjected to heat insulation treatment. The invention effectively solves the problem of electrochemical signal short circuit caused by the damage of a sealing element under the environment of high temperature and strong corrosive medium, effectively solves the problems of overlarge pressure in the device and cooling of a reference electrode by the serial design of double condensing loops, and realizes the sealing problem of the measuring device by combining the design of a ground interface and a steam circulation pressure reducer.
Description
Technical Field
The invention relates to the technical field of electrochemistry, in particular to an electrochemical corrosion test device in boiling and strong corrosive solution environment and application thereof.
Background
The traditional material corrosion performance evaluation usually adopts an exposure test method, namely, the material is soaked for a long time in a corresponding medium environment, and a sample after soaking is subjected to microscopic analysis and corrosion performance test. The method has long period and large workload, and cannot reveal the microscopic mechanism of corrosion of the material. Correspondingly, the electrochemical test method is a rapid evaluation method for material corrosion, and has the advantages of short evaluation time and capability of revealing the tendency of electrochemical corrosion and the corrosion rate of the material from the aspects of thermodynamics and kinetics. For non-volatile and less corrosive media (such as NaCl solution and nuclear power loop H)2BO3LiOH solution), the electrochemical corrosion test can be completed by matching a common glass container with a three-electrode system generally at normal temperature, and the electrochemical test at high temperature and high pressure is completed by matching an autoclave with a measuring electrode. However, in the chemical industry, a medium having a strong corrosiveness is often used. For example, in the treatment of spent fuel after combustion, which is typically carried out using uranyl nitrate (containing nitric acid) during the reactor nuclear fuel cycle, it is necessary to verify the corrosion performance of the structural materials used in the vessels under boiling or near boiling uranyl nitrate conditions. For the electrochemical corrosion test under the boiling and strong corrosive solution environment, the sealing effect of a common measuring device is difficult to realize, and meanwhile, the medium corrosivity is often stronger at high temperature, so that the device and an electrode can be directly damaged, and the electrochemical test loop is short-circuited and fails.
Therefore, it is necessary to design an electrochemical corrosion test applicable to a high-temperature and highly corrosive solution environment, which can ensure the sealing, pressure reduction and signal normality of the measurement process.
Disclosure of Invention
The invention aims to provide an electrochemical corrosion test device under a boiling and strong corrosive solution environment, which can stably and accurately obtain electrochemical corrosion data of materials under the boiling and strong corrosive solution.
In addition, the invention also provides application of the device.
The invention is realized by the following technical scheme:
the electrochemical corrosion test device under the boiling and strong corrosive solution environment comprises a test container, wherein the test container is made of glass, a sample support body interface, a reference electrode interface, an auxiliary electrode interface and a steam circulation pressure reducer interface are arranged on the test container, and a working electrode sample support body, a reference electrode support body, an auxiliary electrode and a steam circulation pressure reducer are respectively installed on the sample support body interface, the reference electrode interface, the auxiliary electrode interface and the steam circulation pressure reducer interface in a ground connection mode;
the sample support with the working electrode comprises a support interface, a lead and a sample, wherein the support interface is arranged on the sample support interface, a guide pipe is inserted into the support interface, the lead is arranged in the guide pipe in a penetrating way, the sample is fixed at the lower end of the lead, a heat insulation pipe is sleeved at least on the part of the lead, which extends into a solution, a resin layer used for fixing the lead and sealing the guide pipe is arranged at the lower end of the guide pipe, and a spiral condensation pipe is arranged at the outer side of the guide pipe;
the reference electrode support body comprises a salt bridge, a spherical grinding opening matched with a reference electrode interface is arranged in the middle of the salt bridge, a condensing tube is arranged on the outer side of the upper portion of the salt bridge, namely the upper portion of the spherical grinding opening is designed to be a double-layer glass sleeve, the inner layer of the spherical grinding opening is the salt bridge, the outer layer of the spherical grinding opening is the condensing sleeve, and the top of the salt bridge is provided with the reference electrode.
Preferably, in order to reduce the circulating water, the condensation pipe is arranged in series with the spiral condensation pipe.
The pipe and the spiral condensation and support body interface are integrated, and the glass is directly cast and molded by using a mold.
The guide pipe, the spiral condenser pipe, the salt bridge and the condenser pipe are all made of glass; the lead enters the test container through the guide pipe and is connected with the sample through a spot welding machine in a spot welding mode, the reference electrode is a saturated calomel electrode, and the steam circulation pressure reducer plays a role in backflow cooling of boiling liquid.
The working electrode sample support of the present invention is prepared as follows:
the heat insulation pipe is sleeved outside the lead and is thermally shrunk, the middle of the bottom of the groove is provided with a small hole, and the diameter of the hole is slightly larger than that of the lead; and (4) enabling the lead to pass through the small hole, pouring resin into the concave groove, and cooling for use.
The working electrode sample support is a special structure designed according to high-temperature (boiling) and corrosive solution environments, ensures that the lead can be suitable for the high-temperature environment by carrying out heat insulation treatment on the lead, is provided with the resin layer, has the advantage of corrosion resistance, and can effectively solve the problem of electrochemical signal short circuit caused by the damage of a sealing piece in a strong corrosive environment; the invention avoids the use of a rubber sealing ring, and avoids the situations that a sealing element fails due to high-temperature corrosion solution and electrochemical test fails due to the solution entering a lead part.
The invention effectively solves the problems of overlarge pressure in the device and cooling of the reference electrode by the serial design of the double condensation loops, realizes the sealing problem of the measuring device by combining the ground interface design and the steam circulation pressure reducer, and avoids the volatilization of corrosive media into the atmospheric environment.
The invention adopts the design of double condensation loops in series connection, and can simultaneously have three effects: ensuring the cooling and depressurization inside the device during the electrochemical test; the resin can be ensured not to be softened at higher temperature; the device has the advantages that the effect of cooling the reference electrode is achieved, meanwhile, the pressure in the test container can be reduced by connecting the double condensation loops in series and the steam circulation pressure reducer, and potential safety hazards caused by overlarge pressure under boiling conditions are avoided.
The electrochemical corrosion test device can stably and accurately obtain the electrochemical corrosion data of the material under the boiling and strong corrosion solution, and provides a new idea and method for verifying the corrosion performance of the structural material in the chemical field of strong acid and strong alkali and the post-treatment field of spent fuel.
Furthermore, the two ends of the spiral condenser pipe are respectively provided with a first condenser pipe inlet and a first condenser pipe outlet, the first condenser pipe inlet and the first condenser pipe outlet are penetrated out through the support body interface, the first condenser pipe outlet is penetrated out through the support body interface, the lower end of the spiral condenser pipe is bent upwards to form a straight pipe, one end of the straight pipe extends into the support body interface, and then the end part of the straight pipe is horizontally bent to form the first condenser pipe outlet.
Further, the lower end of the spiral condensation pipe is lower than the bottom of the resin layer.
The spiral condenser pipe is arranged to cool the resin layer, and the boiling solution is prevented from melting the resin during the test.
Further, the lower end of the conduit is recessed upwards to form a groove, and the resin layer is placed in the groove.
Further, the lower extreme of pipe is provided with the location body, the location body is L shape structure, the horizontal segment of L shape structure is provided with the through-hole that is used for passing the wire, the wire passes the through-hole and passes through positioning bolt fixed.
The positioning body is made of glass, the aperture of the through hole is slightly larger than the diameter of the lead, and the positioning bolt is a glass bolt.
Further, the heat insulation pipe is a polytetrafluoroethylene pipe, and the heat insulation pipe is attached to the outer side of the lead in a heat shrinkage mode.
Furthermore, a micropore ceramic tube is arranged at the bottom of the salt bridge; the condenser pipe comprises a condenser sleeve, a second condenser pipe inlet and a second condenser pipe outlet are formed in the condenser sleeve, and the second condenser pipe inlet is communicated with the first condenser pipe outlet.
Further, the steam circulation pressure reducer is a reflux-type steam circulation pressure reducer.
Furthermore, the auxiliary electrode interface comprises a first auxiliary electrode interface and a second auxiliary electrode interface, a first auxiliary electrode and a second auxiliary electrode are respectively installed on the first auxiliary electrode interface and the second auxiliary electrode interface, and the lower ends of the first auxiliary electrode and the second auxiliary electrode are both platinum sheets.
The electrochemical corrosion test device is applied to electrochemical corrosion tests in boiling and strong corrosive solution environments.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention can realize sealing and decompression under the environment of normal pressure boiling, and can be used for electrochemical corrosion tests under the environment of boiling and strong corrosive solution.
2. The working electrode sample support body designed by the invention does not adopt a seal ring design, the phenomenon of liquid inlet short circuit caused by heating corrosive solution to damage the seal ring can not occur, and the stability and the accuracy of an electrochemical measurement signal are ensured.
3. The main body of the device is made of glass, the processing difficulty coefficient is low, the production cost is greatly reduced, and the device is favorable for batch production.
4. The invention adopts the design of double condensation loops in series connection, and can simultaneously have three effects: ensuring the cooling and depressurization inside the device during the electrochemical test; the resin can be ensured not to be softened at higher temperature; and functions to cool the reference electrode.
5. The structure with the groove and the hole at the bottom of the conduit designed by the invention can realize the replacement of the conductor: after the lead passes through the lead, the lead is sealed by high-temperature resin, and when the lead is excessively consumed, the resin can be melted by heating, and the lead can be reused after being replaced by a new lead.
6. The invention provides a new idea and method for verifying the corrosion performance of structural materials in the chemical field of strong acid and strong alkali and the post-treatment field of spent fuel
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is a schematic view of the overall structure of the test apparatus of the present invention;
FIG. 2 is a schematic diagram of the structure of a working electrode sample support;
FIG. 3 is a partial enlarged view of FIG. 2A;
FIG. 4 is a schematic diagram of the structure of a reference electrode support;
FIG. 5 is an electrochemical polarization curve of Zr-3 alloy obtained in the electrochemical corrosion test of example 1;
FIG. 6 is an electrochemical polarization curve of Ti55 alloy obtained by the electrochemical corrosion test of example 2;
FIG. 7 is the electrochemical polarization curve of W-Mo alloy obtained in the electrochemical corrosion test of example 3.
Reference numbers and corresponding part names in the drawings:
1-test container, 2-sample support interface, 3-reference electrode interface, 4-first auxiliary electrode interface, 5-steam circulation pressure reducer interface, 6-second auxiliary electrode interface, 7-working electrode sample support, 8-reference electrode support, 9-first auxiliary electrode, 10-steam circulation pressure reducer, 11-second auxiliary electrode, 12-platinum sheet, 71-first condenser pipe inlet, 72-first condenser pipe outlet, 73-spiral condenser pipe, 74-support interface, 75-conduit, 76-resin layer, 77-sample, 78-lead, 79-positioning body, 710-positioning bolt, 81-salt bridge, 82-condenser pipe, 83-reference electrode, 84-micropore ceramic pipe, 85-second condenser inlet, 86-second condenser outlet.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1:
as shown in fig. 1 to 4, the electrochemical corrosion test device in boiling and highly corrosive solution environment comprises a test container 1, wherein the test container 1 is made of glass, a sample support body interface 2, a reference electrode interface 3, an auxiliary electrode interface and a steam circulation pressure reducer interface 5 are arranged on the test container 1, and a working electrode sample support body 7, a reference electrode support body 8, an auxiliary electrode and a steam circulation pressure reducer 10 are respectively installed on the sample support body interface 2, the reference electrode interface 3, the auxiliary electrode interface and the steam circulation pressure reducer interface 5 in a ground connection manner;
the sample support 7 with the working electrode comprises a support interface 74, a lead wire 78 and a sample 77, wherein the support interface 74 is installed on the sample support interface 2, a guide pipe 75 is inserted into the support interface 74, the lead wire 78 is arranged in the guide pipe 75 in a penetrating manner, the sample 77 is fixed at the lower end of the lead wire 78, a heat insulation pipe is sleeved on at least a part of the lead wire 78 extending into a solution, a resin layer 76 for fixing the lead wire 78 and sealing the guide pipe 75 is arranged at the lower end of the guide pipe 75, specifically, the lower end of the guide pipe 75 is recessed upwards to form a groove, the resin layer 76 is arranged in the groove, a spiral condensation pipe 73 is arranged on the outer side of the guide pipe 75, two ends of the spiral condensation pipe 73 are respectively a first condensation pipe inlet 71 and a first condensation pipe outlet 72, and both the first condensation pipe inlet 71 and the first condensation pipe outlet 72 penetrate out from the support interface 74, the lower end of the spiral condensation duct 73 is lower than the bottom of the resin layer 76;
the reference electrode supporting body 8 comprises a salt bridge 81, a spherical ground matched with the reference electrode interface 3 is arranged in the middle of the salt bridge 81, a condensing pipe is arranged on the outer side of the upper portion of the salt bridge 81, a reference electrode 83 is arranged at the top of the salt bridge 81, and the reference electrode 83 is a saturated calomel electrode.
In this embodiment, in order to reduce one path of circulating water, the condenser pipe and the spiral condenser pipe 73 are arranged in series, so that compared with the case where the condenser pipe and the spiral condenser pipe 73 are arranged independently, one path of circulating water is reduced, and the operation is simpler; a microporous ceramic tube 84 is arranged at the bottom of the salt bridge 81; the condensation pipe comprises a condensation sleeve 82, a second condensation pipe inlet 85 and a second condensation pipe outlet 86 are arranged on the condensation sleeve 82, and the second condensation pipe inlet 85 is communicated with the first condensation pipe outlet 72.
In this embodiment, the heat insulation pipe is a teflon pipe, and the heat insulation pipe is attached to the outer side of the wire 78 in a heat shrinkage manner.
In this embodiment, in order to better realize the positioning of the test sample 77, the lower end of the conduit 75 is provided with a positioning body 79, the positioning body 79 is an L-shaped structure, the horizontal section of the L-shaped structure is provided with a through hole for passing the lead wire 78, and the lead wire 78 passes through the through hole and is fixed by a positioning bolt 710.
In this embodiment, in order to better realize the pressure reduction in the test container 1, the steam circulation reducer 10 is a reflux-type steam circulation reducer, and this embodiment specifically adopts a P-type steam circulation reducer, and the P-type steam circulation reducer specifically means that the shape of the air flow passage inside the steam circulation reducer is similar to a P-type.
In this embodiment, the auxiliary electrode interface includes a first auxiliary electrode interface 4 and a second auxiliary electrode interface 6, a first auxiliary electrode 9 and a second auxiliary electrode 11 are respectively installed on the first auxiliary electrode interface 4 and the second auxiliary electrode interface 6, and the lower ends of the first auxiliary electrode 9 and the second auxiliary electrode 11 are both platinum sheets 12.
In the present embodiment, the device main body is made of glass.
Electrochemical polarization curve measurement in boiling nitric acid environment was performed using the apparatus described in this example:
the test material is Zr-3 alloy, and the size of the electrochemical corrosion sample is
The wafer of (1). And (3) carefully grinding the Zr-3 wafer by using 600#, 800#, 1000# and 1500# water grinding sand paper specified in GB/T2481.1. And (4) washing the polished sample with deionized water, ultrasonically cleaning the sample with alcohol, taking out the cleaned sample, quickly drying the surface of the sample, and placing the sample in a drying dish for storage. The test medium is 6mol/L nitric acid, and the test temperature is in a boiling state. Before the test, deionized water is used for preparing a nitric acid solution with the concentration, the solution is added to the position of a liquid level line shown in figure 1, the prepared sample 77, namely the working electrode, is taken out and cleaned with alcohol again, the sample is dried by blowing, and the sample is welded with a lead 78 by using an electric welding machine. After welding, the fittings were assembled as shown in FIG. 1 with the microporous ceramic tube 84 facing one side of the sample at a distance of 1-2 cm. Using the electrochemical test apparatus described in this example (FIG. 1), electrochemical polarization curve scanning was performed using a PARSTAT 4000 electrochemical workstation, which had WE, RE, CE connectionsIn FIG. 1, the working electrode sample support 7, the reference electrode support 8, and the first auxiliary electrode 9 are connected. Sample preparation was performed prior to testing. And (5) introducing circulating water for cooling. And (3) placing the device into an oil bath pan, heating to boil, and measuring Open Circuit Potential (OCP) until the potential is stable, wherein the fluctuation amplitude is not more than +/-10 mV. Potentiodynamic polarization curve scans were performed at a scan rate of 10mV/min, starting at 250mV below the open circuit potential, until either the anode current density reached 500. mu.A/cm 2 or the electrode potential reached 1.6V.
In the test process, the test temperature is 118 ℃, and the device can well seal boiling HNO in the whole measurement process3And the solution does not have the phenomena of liquid leakage and electrode flushing caused by overlarge pressure of the test container 1. The electrochemical curve shows that the signal is stable, and the final measurement obtains an electrochemical polarization curve as shown in fig. 5.
Example 2:
the electrochemical polarization curve measurement under the spent fuel post-treatment simulation feed liquid environment is carried out by utilizing the test device of the embodiment:
the test material is Ti55 alloy of a spent fuel post-processing large rotating wheel material, and the size of an electrochemical corrosion sample is 10mm multiplied by 1mm square. The test samples were carefully sanded using 600#, 800#, 1000#, 1500# water-sanded sandpaper specified in GB/T2481.1. And (4) washing the polished sample with deionized water, ultrasonically cleaning the sample with alcohol, taking out the cleaned sample, quickly drying the surface of the sample, and placing the sample in a drying dish for storage. The test medium is a simulation feed liquid, and the specific component is 6mol/L HNO3+2.24g/L Ru +0.2g/L Cr +2.06g/L Ce +1.70g/L V, test temperature 95 ℃. + -. 1 ℃. Before the test, deionized water is used for preparing a nitric acid solution with the concentration, the solution is added to the position of a liquid level line shown in figure 1, the prepared sample 77, namely the working electrode, is taken out and cleaned with alcohol again, the sample is dried by blowing, and the sample is welded with a lead by using an electric welding machine. After welding, the parts were assembled as shown in FIG. 1, and the front end of the reference electrode support 8, i.e., the microporous ceramic tube 84, was opposed to the sample side at a distance of 1-2 cm. Electrochemical test apparatus of example 1 was used to scan electrochemical polarization curves using a PARSTAT 4000 electrochemical workstation, in which the WE, RE, CE connections were made in FIG. 1The sample support 7 as an electrode, the reference electrode support 8, and the first auxiliary electrode 9 are connected. Sample preparation is carried out before the test; and (5) accessing circulating water. And (3) placing the device into an oil bath pan, heating to boil, and measuring Open Circuit Potential (OCP) until the potential is stable, wherein the fluctuation amplitude is not more than +/-10 mV. Potentiodynamic polarization curve scans were performed at a scan rate of 20mV/min, starting at 250mV below the open circuit potential, until either the anode current density reached 500. mu.A/cm 2 or the electrode potential reached 1.6V.
The device can well seal boiling simulation solution in the test process, and liquid leakage does not occur and the pressure of the test container 1 is not too high. The electrochemical curve shows that the signal is stable, and the final measurement obtains an electrochemical polarization curve as shown in fig. 6.
Example 3:
electrochemical polarization curve measurement in boiling concentrated sulfuric acid environment was performed using the experimental apparatus shown in example 1:
the test material is a shielding material W-Mo alloy, and the size of the electrochemical corrosion sample is a square piece of 5mm multiplied by 1 mm. The test samples were carefully sanded using 600#, 800#, 1000#, 1500# water-sanded sandpaper specified in GB/T2481.1. And (4) washing the polished sample with deionized water, ultrasonically cleaning the sample with alcohol, taking out the cleaned sample, quickly drying the surface of the sample, and placing the sample in a drying dish for storage. The test medium is 10mol/L H2SO4The test temperature is boiling condition. Before the test, 1.61g/mL concentrated H is utilized2SO4Adding deionized water to dilute and prepare a test solution, adding the solution to the position of a liquid level line shown in figure 1, taking out the prepared sample 77, namely the working electrode, cleaning the sample again with alcohol, drying the sample by blowing, and welding the sample with a lead 78 by using an electric welding machine. After welding, the parts were assembled as shown in FIG. 1, with the front end of the reference electrode support 8 facing the sample side, at a distance of 1-2 cm. Electrochemical polarization curve scanning was performed using the electrochemical test apparatus shown in the example (fig. 1) using a parastat model 4000 electrochemical workstation, to which the connectors labeled WE, RE, CE were attached to the working electrode sample support 7, the reference electrode support 8, and the first auxiliary electrode 9, respectively, in fig. 1. Sample preparation is carried out before the test; and connecting the circulating water. Putting the device into an oil bath pan and heating toAfter boiling, Open Circuit Potential (OCP) measurement is carried out until the potential is stable, and the fluctuation amplitude does not exceed +/-10 mV. Potentiodynamic polarization curve scans were performed at a scan rate of 20mV/min, starting at 250mV below the open circuit potential, until either the anode current density reached 500. mu.A/cm 2 or the electrode potential reached 1.6V.
The device can well seal boiling simulation solution in the test process, and liquid leakage does not occur and the pressure of the test container 1 is not too high. The electrochemical curve shows that the signal is stable, and the final measurement results in an electrochemical polarization curve as shown in fig. 7.
Comparative example 1:
the experimental setup used in this comparative example is based on example 1, and differs from example 1 in that:
the working electrode sample support 7 is sealed by replacing resin with a sealing ring made of PEEK material.
And carrying out electrochemical polarization curve measurement on the Zr-3 alloy in a boiling nitric acid environment. The size of the electrochemical corrosion sample is
The wafer of (1). And (3) carefully grinding the Zr-3 wafer by using 600#, 800#, 1000# and 1500# water grinding sand paper specified in GB/T2481.1. And (3) after polishing, washing the sample 77 with deionized water, ultrasonically cleaning with alcohol, taking out after cleaning, quickly drying the surface, and placing in a drying vessel for storage. The test medium is 6mol/L nitric acid, and the test temperature is in a boiling state. A nitric acid solution of this concentration was prepared with deionized water prior to testing. This 500mL solution was added to the test vessel 1 after the test had started.
The prepared sample 77 is taken out, washed again with alcohol, dried, and fitted into the bottom of the lead 78 of the working electrode sample support 7. The working electrode sample support 7 is sealed with a seal ring made of a PEEK material. Electrochemical polarization curve scans were performed using a PARSTAT model 4000 electrochemical workstation. The device is placed into an oil bath pan to be heated from normal temperature to a boiling state, and Open Circuit Potential (OCP) measurement is carried out in the heating process. The OCP signal is found to be disordered when the temperature rises to 95 ℃ in the test, the measurement of the polarization curve is started, the workstation displays the current overload, and the measurement is automatically stopped. And stopping measuring, taking the device out after the temperature is reduced to the room temperature, observing and finding that liquid enters the conduit, and the rubber ring is seriously corroded to cause sealing failure so as to cause the short circuit of the electrochemical measurement loop.
Comparative example 2:
the experimental setup used in this comparative example is based on example 1, and differs from example 1 in that:
the working electrode sample support 7 is sealed by replacing resin with a sealing ring made of polyether-ether-ketone material.
Electrochemical polarization curve measurement of Ti-35 alloy is carried out under the environment of spent fuel post-treatment simulation feed liquid (6mol/L HNO3+2.24g/L Ru +0.2g/L Cr +2.06g/L Ce +1.70g/L V), and the test temperature is boiling (about 120 ℃). The size of the electrochemical corrosion test piece is 10mm multiplied by 1 mm. The test was carefully sanded using 600#, 800#, 1000#, 1500# water-sanded sandpaper specified in GB/T2481.1. And (3) after polishing, washing the sample 77 with deionized water, ultrasonically cleaning with alcohol, taking out after cleaning, quickly drying the surface, and placing in a drying vessel for storage. A nitric acid solution of this concentration was prepared with deionized water prior to testing. The 500mL solution was added to a five-necked test vial after the start of the test.
The prepared sample 77 is taken out, washed again with alcohol, dried, and fitted into the bottom of the lead 78 of the working electrode sample support 7. The working electrode sample support 7 is sealed with a seal ring made of a polyether ether ketone material. Electrochemical polarization curve scans were performed using a PARSTAT model 4000 electrochemical workstation. The device is placed in an oil bath pan and heated from normal temperature to boiling state. It was found that when the liquid boiled, the pressure in the test vessel 1 rose rapidly, and the working electrode sample support 7, the reference electrode support 8, and the auxiliary electrode were reopened by the gas pressure, and contained HNO3Into the atmosphere. At this time, the time polarization curve measurement is carried out, and the workstation displays that the current overload stops measuring. Stopping measuring, taking out the device after the temperature is reduced to the room temperature,the observation shows that liquid enters the conduit, and the rubber sealing ring is seriously corroded, so that the sealing failure is caused, and the electrochemical measurement loop is short-circuited.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The electrochemical corrosion test device under the boiling and strong corrosive solution environment comprises a test container (1), wherein the test container (1) is made of glass, and is characterized in that a sample support body interface (2), a reference electrode interface (3), an auxiliary electrode interface and a steam circulation pressure reducer interface (5) are arranged on the test container (1), and a working electrode sample support body (7), a reference electrode support body (8), an auxiliary electrode and a steam circulation pressure reducer (10) are respectively installed on the sample support body interface (2), the reference electrode interface (3), the auxiliary electrode interface and the steam circulation pressure reducer interface (5) in a ground connection mode;
the sample support (7) with the working electrode comprises a support interface (74), a lead (78) and a sample (77), wherein the support interface (74) is installed on the sample support interface (2), a guide pipe (75) is inserted into the support interface (74), the lead (78) is arranged in the guide pipe (75) in a penetrating mode, the sample (77) is fixed to the lower end of the lead (78), at least one part, extending into the solution, of the lead (78) is sleeved with a heat insulation pipe, a resin layer (76) used for fixing the lead (78) and sealing the guide pipe (75) is arranged at the lower end of the guide pipe (75), and a spiral condensation pipe (73) is arranged on the outer side of the guide pipe (75);
the reference electrode supporting body (8) comprises a salt bridge (81), a spherical ground matched with the reference electrode interface (3) is arranged in the middle of the salt bridge (81), a condensing tube is arranged on the outer side of the upper portion of the salt bridge (81), and a reference electrode (83) is arranged at the top of the salt bridge (81).
2. The electrochemical corrosion test device under boiling and strong corrosive solution environment according to claim 1, wherein the two ends of the spiral condenser tube (73) are respectively a first condenser tube inlet (71) and a first condenser tube outlet (72), and both the first condenser tube inlet (71) and the first condenser tube outlet (72) are penetrated by a support interface (74).
3. The electrochemical corrosion test device in boiling, highly corrosive solution environment according to claim 1, wherein the lower end of the spiral-shaped condensation pipe (73) is lower than the bottom of the resin layer (76).
4. The electrochemical corrosion test device in boiling environment with strong corrosive solution according to claim 1, wherein the lower end of the conduit (75) is recessed upwards to form a groove, and the resin layer (76) is disposed in the groove.
5. The electrochemical corrosion test device under boiling and strong corrosive solution environment according to claim 1, characterized in that the lower end of the conduit (75) is provided with a positioning body (79), the positioning body (79) is an L-shaped structure, the horizontal section of the L-shaped structure is provided with a through hole for passing a lead (78), and the lead (78) passes through the through hole and is fixed by a positioning bolt (710).
6. The electrochemical corrosion test device under boiling and strong corrosive solution environment according to claim 1, wherein the heat insulation pipe is a polytetrafluoroethylene pipe, and the heat insulation pipe is attached to the outer side of the conducting wire (78) in a heat shrinkage mode.
7. The electrochemical corrosion test device in boiling environment with strong corrosive solution according to claim 1, wherein the bottom of the salt bridge (81) is provided with a microporous ceramic tube (84); the condenser pipe comprises a condenser sleeve (82), a second condenser pipe inlet (85) and a second condenser pipe outlet (86) are formed in the condenser sleeve (82), and the second condenser pipe inlet (85) is communicated with the first condenser pipe outlet (72).
8. The electrochemical corrosion test device in boiling, highly corrosive solution environment according to claim 1, characterized in that said steam cycle pressure reducer (10) is a reflux steam cycle pressure reducer.
9. The electrochemical corrosion test device under boiling and strong corrosive solution environment according to any one of claims 1 to 8, wherein the auxiliary electrode interface comprises a first auxiliary electrode interface (4) and a second auxiliary electrode interface (6), a first auxiliary electrode (9) and a second auxiliary electrode (11) are respectively installed on the first auxiliary electrode interface (4) and the second auxiliary electrode interface (6), and the lower ends of the first auxiliary electrode (9) and the second auxiliary electrode (11) are both platinum sheets (12).
10. Use of the electrochemical corrosion test device according to any one of claims 1 to 9 in an environment of boiling, strongly corrosive solution for electrochemical corrosion testing.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115165722A (en) * | 2022-07-29 | 2022-10-11 | 上海交通大学 | Heat exchange characteristic testing method for practical environment application of surface modified plate-shaped element |
| CN115223738A (en) * | 2022-07-15 | 2022-10-21 | 西安交通大学 | Experiment segment for measuring temperature and potential of cladding and measuring method |
| CN116840138A (en) * | 2023-09-01 | 2023-10-03 | 中铁十七局集团第二工程有限公司 | Three-pipe communicating vessel type reinforcing steel bar anodic polarization test device |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR19980040516U (en) * | 1996-12-23 | 1998-09-15 | 김종진 | Corrosion test equipment in steam in multi-stage condenser |
| CN101175719A (en) * | 2005-05-11 | 2008-05-07 | 索尼株式会社 | Process for producing functional molecule capable of ionic dissociation and process for producing raw molecule thereof |
| CN102004074A (en) * | 2010-10-27 | 2011-04-06 | 中国石油化工股份有限公司 | High-temperature high-pressure gas-liquid two-phase corrosion simulated experiment device and experimental method thereof |
| CN102507428A (en) * | 2011-10-19 | 2012-06-20 | 上海大学 | Condensed fluid corrosion simulation test device in automobile exhaust system |
| CN105277482A (en) * | 2014-07-07 | 2016-01-27 | 中石化洛阳工程有限公司 | Distillation apparatus tower top system dew point corrosion test method |
-
2021
- 2021-10-13 CN CN202111192897.9A patent/CN113848174B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR19980040516U (en) * | 1996-12-23 | 1998-09-15 | 김종진 | Corrosion test equipment in steam in multi-stage condenser |
| CN101175719A (en) * | 2005-05-11 | 2008-05-07 | 索尼株式会社 | Process for producing functional molecule capable of ionic dissociation and process for producing raw molecule thereof |
| CN102004074A (en) * | 2010-10-27 | 2011-04-06 | 中国石油化工股份有限公司 | High-temperature high-pressure gas-liquid two-phase corrosion simulated experiment device and experimental method thereof |
| CN102507428A (en) * | 2011-10-19 | 2012-06-20 | 上海大学 | Condensed fluid corrosion simulation test device in automobile exhaust system |
| CN105277482A (en) * | 2014-07-07 | 2016-01-27 | 中石化洛阳工程有限公司 | Distillation apparatus tower top system dew point corrosion test method |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115223738A (en) * | 2022-07-15 | 2022-10-21 | 西安交通大学 | Experiment segment for measuring temperature and potential of cladding and measuring method |
| CN115223738B (en) * | 2022-07-15 | 2024-01-26 | 西安交通大学 | Experimental section and measuring method for measuring temperature and potential of cladding |
| CN115165722A (en) * | 2022-07-29 | 2022-10-11 | 上海交通大学 | Heat exchange characteristic testing method for practical environment application of surface modified plate-shaped element |
| CN116840138A (en) * | 2023-09-01 | 2023-10-03 | 中铁十七局集团第二工程有限公司 | Three-pipe communicating vessel type reinforcing steel bar anodic polarization test device |
| CN116840138B (en) * | 2023-09-01 | 2023-12-12 | 中铁十七局集团第二工程有限公司 | Three-pipe communicating vessel type reinforcing steel bar anodic polarization test device |
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