CN211741016U - Test system for evaluating metal under deep sea low-temperature and low-oxygen conditions - Google Patents

Test system for evaluating metal under deep sea low-temperature and low-oxygen conditions Download PDF

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CN211741016U
CN211741016U CN202020151439.5U CN202020151439U CN211741016U CN 211741016 U CN211741016 U CN 211741016U CN 202020151439 U CN202020151439 U CN 202020151439U CN 211741016 U CN211741016 U CN 211741016U
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electrolytic cell
oxygen
electrode
deep sea
test system
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吴波
白鹭飞
吴建华
杨阳
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Jimei University
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Abstract

The utility model relates to the technical field of galvanic corrosion testing devices, in particular to a testing system for evaluating metals under the condition of deep sea low temperature and low oxygen, which comprises an electrolytic cell device arranged in a temperature-controllable sealed space; the electrolytic cell body is used for storing corrosive media; the gas inlet pipe penetrates through the electrolytic cell cover and extends into the corrosive medium, and is used for introducing gas to adjust the oxygen content in the electrolytic cell body; the gas outlet pipe penetrates through the electrolytic cell cover and extends into a space between the electrolytic cell cover and the corrosive medium; the test electrode comprises an electrode clamp, a reference electrode and an auxiliary electrode which are all arranged on the electrolytic cell cover and extend into the corrosive medium; the sensor is mounted on the electrolytic cell cover and extends into the corrosive medium; the utility model provides a test system can deal with the metal corrosion test under low temperature, the low oxygen condition, and cooperation electrochemistry workstation can carry out multiunit experiment synchronization experiment, effective control experimental time simultaneously.

Description

Test system for evaluating metal under deep sea low-temperature and low-oxygen conditions
Technical Field
The utility model relates to a galvanic corrosion testing arrangement technical field, in particular to evaluation metal test system under deep sea low temperature low oxygen condition.
Background
Different metals with different properties are usually required to be matched for use in ocean engineering equipment, and when the metal materials are in direct contact or are electrically connected through other media, galvanic cells can be formed due to different self-corrosion potentials of each metal material, so that galvanic corrosion is caused. At present, the bimetallic galvanic corrosion problem is more concerned, but in the ocean equipment, the inevitable existence of complex metal coupling is as follows: the submarine pressure shell, the non-pressure shell and the condenser brass pipe. When the submarine is in service, the submarine enters a deep sea environment. Compared with surface seawater, the main influencing factors in the deep sea corrosion environment are as follows: the temperature, the oxygen content and the pressure are all changed obviously, and the galvanic corrosion behavior and mechanism are also changed obviously.
Aiming at metal materials in service and marine engineering, marine equipment and deep sea pipeline corrosion environments, low-temperature low-oxygen galvanic corrosion performance evaluation needs to be carried out on equipment, structures, functional parts and the like which are connected with complex metal materials in a coupling mode. And (3) mastering the galvanic corrosion rate, the galvanic corrosion action mechanism and the crevice corrosion risk when a plurality of metal materials are coupled, optimizing the coupled metal materials and inspecting the applicability of the complex metal connection.
At present, the device or method for detecting the galvanic corrosion tendency of complex metals under low temperature, low oxygen and different humidity in deep sea in the field is less, so that the applicability of the complex metal material in the deep sea low temperature and low oxygen corrosion medium cannot be comprehensively and accurately evaluated, the test period of the existing test device is longer, the galvanic corrosion performance of the complex metal couple under the deep sea low temperature and low oxygen condition cannot be quickly evaluated, the test system is very complex, the test cost is high, the evaluation result of the galvanic corrosion is far from the actual engineering, and the like, and the reliable evaluation cannot be provided for the optimization and the applicability of the field metal material.
Therefore, a testing system capable of detecting the galvanic corrosion performance under the low-temperature and low-oxygen environment is urgently needed in the market.
SUMMERY OF THE UTILITY MODEL
In order to solve the problems mentioned in the background art, the existing test system can not meet the requirement of galvanic corrosion performance detection under the low-temperature and low-oxygen environment, the utility model provides a test system for evaluating metals under the deep-sea low-temperature and low-oxygen condition, which comprises an electrolytic cell device arranged in a temperature-controllable sealed space;
the electrolytic cell device comprises an electrolytic cell body, an electrolytic cell cover, an air inlet pipe, an air outlet pipe, a test electrode and a sensor;
the electrolytic cell body is used for storing corrosive media; the gas inlet pipe penetrates through the electrolytic cell cover and extends into the corrosive medium, and is used for introducing gas to adjust the oxygen content in the electrolytic cell body; the gas outlet pipe penetrates through the electrolytic cell cover and extends into a space between the electrolytic cell cover and the corrosive medium;
the test electrode comprises an electrode clamp, a reference electrode and an auxiliary electrode which are all arranged on the electrolytic cell cover and extend into the corrosive medium; the sensor is mounted on the electrolytic cell cover and extends into the corrosive medium;
the electrode clamp, the reference electrode, the auxiliary electrode and the sensor are connected with the multi-channel electrochemical workstation.
On the basis of the structure, the air inlet pipe is further connected with an air supply device; the gas supply device comprises an oxygen supply device and a nitrogen supply device.
On the basis of the structure, the oxygen supply device and the nitrogen supply device are further connected with the air inlet pipe through a three-way valve;
the oxygen supply device comprises an oxygen bottle, an oxygen pressure reducing valve on the opening of the oxygen bottle, an oxygen supply pipeline connecting the oxygen bottle and the three-way valve, and an oxygen flowmeter arranged on the oxygen supply pipeline;
the nitrogen supply device comprises a nitrogen bottle, a nitrogen pressure reducing valve on the opening of the nitrogen bottle, a nitrogen supply pipeline connecting the nitrogen bottle and the three-way valve, and a nitrogen flowmeter arranged on the nitrogen supply pipeline.
On the basis of the structure, the electrolytic cell body is connected with the electrolytic cell cover in a sealing mode through threads.
On the basis of the structure, the end of the air inlet pipe, which extends into the corrosive medium, is provided with an aeration pipe.
On the basis of the structure, furthermore, a Lujin capillary tube is arranged at the lower end of the reference electrode, and the tip of the Lujin capillary tube extends into a corrosive medium and is aligned with a working electrode fixed below the electrode clamp.
On the basis of the structure, a humidifying water tank for adjusting the humidity in the space is further arranged in the sealed space.
On the basis of the structure, a water seal structure is further arranged at the outer side end of the air outlet pipe.
On the basis of the structure, the multi-channel electrochemical workstation is further connected with a multifunctional analyzer.
In addition to the above configuration, the plurality of electrode holders may be sequentially connected in series.
The utility model provides a pair of evaluation metal test system under deep sea low temperature low oxygen condition compares with prior art, has following advantage:
the utility model provides a test system can deal with the metal corrosion test under low temperature, the low oxygen condition, and cooperation electrochemistry workstation can carry out multiunit experiment synchronization experiment, effective control experimental time simultaneously.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive labor.
FIG. 1 is a schematic structural diagram of a testing system for evaluating metals under deep-sea low-temperature and low-oxygen conditions according to the present invention;
FIG. 2 is a schematic view of a part of the structure of an electrolytic cell device provided by the present invention;
FIG. 3 is a schematic structural view of another part of an electrolytic cell device provided by the present invention;
FIG. 4 is a top view of an electrolytic cell cover according to the present invention;
FIG. 5 is a diagram of the galvanic potential and galvanic current of TA2/B10/Q235B at 0 ℃;
FIG. 6 is a plot of the polarization of TA2/B10/Q235B at 0 ℃;
FIG. 7 is a graph of the galvanic potential and current of TA2/B10/Q235B under 0.3mg/L (hypoxia) condition;
FIG. 8 is a plot of the polarization of TA2/B10/Q235B under 0.3mg/L (hypoxia) conditions;
fig. 9 is a schematic structural diagram of a test system for evaluating metals under deep sea low-temperature and low-oxygen conditions according to the present invention.
Reference numerals:
100 cell unit 110 cell body 120 cell cover
130 air inlet pipe 131 and aeration pipe 140 air outlet pipe
141 water seal structure 150 test electrode 151 electrode clamp
152 reference electrode 153 auxiliary electrode 154 luggin capillary
155 working electrode 160 sensor 200 electrochemical workstation
300 air supply device 310 oxygen supply device 311 oxygen cylinder
312 oxygen pressure reducing valve 313 oxygen supply pipeline 314 oxygen flow meter
320 nitrogen supply device 321 nitrogen bottle 322 nitrogen pressure reducing valve
323 nitrogen supply pipe 324 nitrogen gas flowmeter 330 three-way valve
400 humidifying water tank 500 multifunctional analyzer
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for convenience of description and simplification of the description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
The utility model provides a test system for evaluating metals under deep sea low-temperature and low-oxygen conditions, which comprises an electrolytic cell device 100 arranged in a temperature-controllable sealed space;
during the concrete implementation, electrolytic cell device 100 sets up in the sealed space with the controllable temperature, of course, can set up one or more electrolytic cell device 100 in the sealed space, the sealed space of controllable temperature is preferred but not limited to the high low temperature alternation humid heat case of Shanghai constant technology limited company BPHJS-060C model, high low temperature alternation humid heat case can realize that low temperature control is at-50 deg.C ~ 20 deg.C, and humidity control is at 0% ~ 100%, thereby can carry out the regulating variable according to own experimental condition, can also consider that single variable factor is experimental to have accuracy and high efficiency, in order to keep the reliability of experimental data, this device still is equipped with temperature and humidity calculation function, can see the change curve of temperature and humidity.
Specifically, the electrolytic cell device 100 comprises an electrolytic cell body 110, an electrolytic cell cover 120, an air inlet pipe 130, an air outlet pipe 140, a test electrode 150 and a sensor 160;
specifically, the electrolytic cell body 110 is used for storing corrosive media;
in particular, as shown in fig. 1-2, the electrolytic cell assembly 100 includes an electrolytic cell body 110 and an electrolytic cell cover 120; the electrolytic cell cover 120 is placed on the electrolytic cell body 110 to seal the inside of the electrolytic cell body 110, and a certain volume of corrosive medium is contained in the electrolytic cell body 110, in this embodiment, the adopted corrosive medium is a 3.5% NaCl solution, and of course, other corrosive media can be used according to experimental needs.
Specifically, the gas inlet pipe 130 is arranged on the electrolytic cell cover 120 in a penetrating manner and extends into the corrosive medium, and is used for introducing gas to adjust the oxygen content in the electrolytic cell body 110; the gas outlet pipe 140 penetrates through the electrolytic cell cover 120 and extends into a space between the electrolytic cell cover 120 and the corrosive medium;
in specific implementation, as shown in fig. 3, the air inlet pipe 130 is disposed through the electrolytic cell cover 120 and extends into the 3.5% NaCl solution, and the air outlet pipe 140 is disposed through the electrolytic cell cover 120 and extends into the space between the 3.5% NaCl solution and the electrolytic cell cover 120 in the electrolytic cell body 110, when the oxygen content in the electrolytic cell body 110 needs to be adjusted, gas, preferably nitrogen, or other gases, is continuously introduced into the electrolytic cell body 110 through the air inlet pipe 130 and is then discharged from the air outlet pipe 140, so that the oxygen content in the corrosion medium is reduced.
Specifically, the test electrode 150 includes an electrode clamp 151, a reference electrode 152, and an auxiliary electrode 153, all mounted on the cell cover 120 and extending into the corrosive medium; the sensor 160 is mounted on the cell cover 120 and extends into the corrosive medium.
In specific implementation, as shown in fig. 2 to 3, the test electrode 150 includes an electrode clamp 151, a reference electrode 152 and an auxiliary electrode 153, which are all mounted on the electrolytic cell cover 120, a clamping end of the electrode clamp 151 extends into the corrosive medium, and the reference electrode 152 and the auxiliary electrode 153 also extend into the corrosive medium; the clamping end of the electrode clamp 151 may be used to clamp a metallic working electrode 155; the sensor 160 is also installed on the electrolytic cell cover 120 and extends into the corrosive medium, and is mainly used for testing the temperature, the dissolved oxygen amount and the humidity in the corrosive medium, the electrode clamp 151 is preferably made of a polytetrafluoroethylene shell, a copper wire penetrates through the electrode clamp, the lower portion of the electrode clamp 151 can be connected with working electrodes 155 in different shapes, the working electrodes can be rectangular (with the length of 1-5 cm and the width of 1-5 cm), square (with the side length of 1-5 cm), round (with the radius of 1-3 cm) and thickness of 1-5 mm), the shape and the size can be adjusted according to own experimental conditions, and the sensor can also be self-adjusted according to various metal materials involved in the actual service deep sea environment, such as high-strength steel in different types, corrosion-resistant titanium alloy and copper alloy used by a condensation system in the deep sea.
Specifically, the electrode holder 151, the reference electrode 152, the auxiliary electrode 153, and the sensor 160 are connected to the multi-channel electrochemical workstation 200.
In specific implementation, as shown in fig. 1-2, the electrode holder 151, the reference electrode 152, the auxiliary electrode 153, and the sensor 160 are all electrically connected to a multi-channel electrochemical workstation 200, and the multi-channel electrochemical workstation 200 can be used for setting test contents and time, recording experiment start time and experiment period, setting according to actual requirements and related standards, and simultaneously generating test ac impedance, polarization curves, and the like to match with each electrode to realize metal testing; the multi-channel electrochemical workstation 200 is preferably, but not limited to, PGSTAT-302N, Vanton, Switzerland, the sensor 160 is preferably, but not limited to, DZS-708L, Shanghai Tech-electro Co., Ltd; the workstation can be multichannel, and the passageway quantity is more, and the number of groups of testing is more each time, can carry out multiunit experiment simultaneously, practices thrift experimental time and experimental volume, can also test the respective alternating current impedance and the polarization curve of complicated coupling system through the collocation setting of a plurality of electrode holder 151, and the setting of a plurality of electrode holders 151 does not do this again and does not do too much to describe as a preferred scheme.
Through the structure design, the utility model provides a test system can deal with the metal corrosion test under low temperature, the low oxygen condition, and cooperation electrochemistry workstation can carry out multiunit experiment synchronization experiment, effective control experimental time simultaneously.
Preferably, a temperature and humidity detection device is arranged in the sealed space.
During the concrete implementation, still be equipped with the detection device of temperature and humidity in the confined space, can be for temperature, humidity transducer etc. further guarantee the accuracy of experiment.
Preferably, the air inlet pipe 130 is connected with an air supply device 300; the gas supply device 300 includes an oxygen supply device 310 and a nitrogen supply device 320.
In specific implementation, as shown in fig. 1 and 9, in order to facilitate the regulation of the oxygen content in the electrolytic cell body 110 or the corrosive medium, the air inlet pipe 130 is connected to the air supply device 300, and the air supply device 300 includes an oxygen supply device 310 and a nitrogen supply device 320, and respectively supplies oxygen and nitrogen to the electrolytic cell body 110 according to actual needs, so as to meet the test requirements of different environmental conditions.
Preferably, the oxygen supply device 310 and the nitrogen supply device 320 are connected to the gas inlet pipe 130 through a three-way valve 330;
the oxygen supply device 310 comprises an oxygen bottle 311, an oxygen pressure reducing valve 312 on the mouth of the oxygen bottle 311, an oxygen supply pipeline 313 for connecting the oxygen bottle 311 and the three-way valve 330, and an oxygen flow meter 314 arranged on the oxygen supply pipeline 313;
the nitrogen supply device 320 comprises a nitrogen gas bottle 321, a nitrogen pressure reducing valve 322 on the mouth of the nitrogen gas bottle 321, a nitrogen supply pipeline 323 connecting the nitrogen gas bottle 321 and the three-way valve 330, and a nitrogen gas flowmeter 324 arranged on the nitrogen supply pipeline 323.
In a specific implementation, as shown in fig. 1, the oxygen supply device 310 and the nitrogen supply device 320 are connected to the air inlet pipe 130 through a three-way valve 330;
the oxygen supply device 310 comprises an oxygen cylinder 311, an oxygen pressure reducing valve 312 is arranged on the mouth of the oxygen cylinder 311, the oxygen cylinder 311 is connected with a three-way valve 330 through an oxygen supply pipeline 313, and an oxygen flow meter 314 is arranged on the oxygen supply pipeline 313;
the nitrogen supply device 320 comprises a nitrogen gas bottle 321, a nitrogen pressure reducing valve 322 is arranged on the mouth of the nitrogen gas bottle 321, the nitrogen gas bottle 321 is connected with a three-way valve 330 through a nitrogen supply pipeline 323, and a nitrogen gas flowmeter 324 is arranged on the nitrogen supply pipeline 323;
by the arrangement, the on-off and the flow of nitrogen and oxygen can be effectively controlled, the precision of the whole testing system is improved, and the oxygen content can be controlled to be 0 mg/L-9 mg/L, so that the variable can be adjusted according to own experimental conditions.
Preferably, the electrolytic cell body 110 and the electrolytic cell cover 120 are hermetically connected by screw threads.
In specific implementation, the electrolytic cell cover 120 and the electrolytic cell body 110 are fixedly connected in a rotating sealing manner through threads, and a sealing ring is sleeved on the threads of the electrolytic cell cover 120, so that the sealing performance of the electrolytic cell is further ensured;
preferably, the cover 120 is made of teflon to ensure good corrosion resistance.
Preferably, the electrolytic cell body 110 has an inner and outer layer structure, and there is no space between the inner and outer layers.
During concrete implementation, through inside and outside two-layer structure, be favorable to reinforcing device's gas tightness, have better effect simultaneously in the controlled temperature for the simulation effect of environment is more accurate.
Preferably, the air inlet pipe 130 and the air outlet pipe 140 are connected with the electrolytic cell cover 120 in a ground mode, and are sleeved with rubber rings to prevent air leakage.
Preferably, the end of the air inlet pipe 130 extending into the corrosive medium is provided with an aeration pipe 131.
In specific implementation, as shown in fig. 3, an aeration pipe 131 is arranged below the air inlet pipe 130, and the aeration pipe 131 is used for enabling air to uniformly diffuse and overflow in a bubble form, and simultaneously facilitating the oxygen to be dissolved into the corrosive medium.
Preferably, the reference electrode 152 is provided with a luggin capillary 154 at the lower end, and the tip of the luggin capillary 154 extends into the corrosive medium and is aligned with a working electrode 155 fixed below the electrode clamp 151.
In specific implementation, as shown in fig. 2, the luggin capillary 154 belongs to one of the salt bridges, and is mainly used for eliminating the liquid connection potential and the solution resistance, reducing the ohmic potential drop, and greatly improving the accuracy of experimental data; depending on the size of the reference electrode 152, its tip is preferably centered on the working electrode 155.
Preferably, a humidifying water tank 400 for adjusting the humidity in the space is provided in the sealed space.
In specific implementation, as shown in fig. 1, a humidification water tank 400 for adjusting humidity in the space is arranged in the sealed space, the sealed space can be a high-low temperature alternating wet-heat tank, and the temperature-controllable sealed space is preferably, but not limited to, a high-low temperature alternating wet-heat tank of the BPHJS-060C model of shanghai-constant technology ltd.
Preferably, a water sealing structure 141 is arranged at the outer end of the air outlet pipe 140.
In specific implementation, as shown in fig. 3, a water seal structure 141 is further disposed at the outer side end of the gas outlet pipe 140, and the water seal structure 141 resists the change of internal and external pressures by using a certain height of hydrostatic pressure, so as to prevent gas outside the electrolytic cell from entering the interior of the electrolytic cell and interfering with the environment of corrosive media.
Preferably, the multi-channel electrochemical workstation 200 is connected to a multi-functional analyzer 500.
In specific implementation, the multi-channel electrochemical workstation 200 is further connected to the multifunctional analyzer 500, and the multifunctional analyzer 500 is used for analyzing the temperature and the oxygen content.
Preferably, the electrode holders 151 are provided in plurality and sequentially connected in series.
In specific implementation, as shown in fig. 1 to 4, the number of the electrode holders 151 may be 1, 2, 3, or more, in this embodiment, a working electrode 155 is clamped below each electrode holder 151, the working electrode 155 may be a metal sample with different shapes to be tested, and meanwhile, the following pretreatment operations are preferably performed: the working electrode 155 needs to be sealed, only one working surface is reserved, the other surfaces are sealed by epoxy resin, the reserved metal surface is preferably polished by sand paper and polishing cloth, and then the working electrode 155 is clamped by the electrode clamp 151 and is placed in the electrolytic cell body 110;
when corrosion among three metals needs to be detected, the electrode clamps 151 need to be connected in series on the electrolytic cell cover 120 through the crocodile clamps in sequence to form a loop, for example, A, B, C three metals exist, namely, A is connected with B, B is connected with C, and C is connected with A, so that the loop is formed; when corrosion between two metals needs to be detected, the electrode clamps 151 of the two metals are directly connected through the alligator clamps; when only one metal corrosion condition needs to be detected, no additional connection is needed.
As a preferred embodiment of the test system of a pair of evaluation metal under deep sea low temperature low oxygen condition, adopt three kinds of metals that await measuring to test, include the embodiment as follows:
before testing, sequentially using abrasive paper with different meshes to polish the metal sample and using a polishing agent to polish, sequentially cleaning deionized water and absolute ethyl alcohol, drying by using a drying oven, and weighing by using a ten-thousandth balance to record respective mass (M)1、M2、M3) Making a first galvanic couple sample, a second galvanic couple sample and a third galvanic couple sample corresponding to three or more metals to be tested, respectively clamping the first galvanic couple sample, the second galvanic couple sample and the third galvanic couple sample by using electrode clamps 151 and sealing by using epoxy resin, and detecting whether a circuit is on or off by using a universal meter diode function;
pouring the prepared 3.5% NaCl solution as a corrosion medium into the electrolytic cell body 110, placing the first galvanic couple sample, the second galvanic couple sample and the third galvanic couple sample in the corrosion medium, connecting the parts, extending out of the electrolytic cell cover 120, of the electrode clamps 151 corresponding to the first galvanic couple sample, the second galvanic couple sample and the third galvanic couple sample in pairs through alligator clamps, and detecting whether the circuit is on or off by using a universal meter diode function;
then, the air inlet pipe 130 and the aeration pipe 131 extend out of the electrolytic cell cover 120, the air outlet pipe 140 extends out of the outer side of the electrolytic cell cover 120, and a small amount of water is filled in the water seal structure 141; the Rough capillary 154 is fixed at the lower end of the reference electrode 152, the distance between the tip part at the lower end of the Rough capillary 154 and the working electrode 155 is 1-2 mm, and the Rough capillary 154 can be rotationally aligned to different working electrodes 155 when different working electrodes 155 are tested; the auxiliary electrode 153 penetrates through the electrolytic cell cover 120 and extends into the corrosive medium, the above structures penetrating through the electrolytic cell cover 120 and extending into the electrolytic cell body 110 are connected with the electrolytic cell cover 120 through ground openings, and sealing is performed by using a sealing ring to ensure good sealing performance of the electrolytic cell. The temperature, humidity and oxygen content sensors are arranged on the electrolytic cell cover 120 in a penetrating way and extend into the corrosive medium, and meanwhile, the sensors are connected through signal wires and penetrate out of the high-low temperature alternating wet-heat box to be connected to the multifunctional analyzer 500; then the electrolytic cell cover 120 is sleeved with a sealing ring and the electrolytic cell body 110 is screwed up in a rotating way and is placed into a high-low temperature alternating humidity-heating box;
a nitrogen pressure reducing valve 322 is installed in the nitrogen cylinder 321, one end of a nitrogen supply pipe 323 is connected to the nitrogen pressure reducing valve 322, and a nitrogen flow meter 324 is provided in the middle of the nitrogen supply pipe 323 to control the flow rate of nitrogen. The oxygen pressure reducing valve 312 is arranged on the oxygen bottle 311, one end of the oxygen supply pipeline 313 is connected to the oxygen pressure reducing valve 312, and the middle of the oxygen supply pipeline 313 is provided with an oxygen flow meter 314 for controlling the oxygen flow; the nitrogen supply pipeline 323 and the oxygen supply pipeline 313 are respectively connected through a three-way valve 330, pass through the high-low temperature alternating wet heat box and are connected to the air inlet pipe 130 on the electrolytic cell cover 120, and the electrode clamp 151, the reference electrode 152, the auxiliary electrode 153 and the temperature and humidity oxygen content sensor on the electrolytic cell cover 120 are connected out from the high-low temperature alternating wet heat box through pipelines and are respectively connected with the multi-channel electrochemical workstation 200 and the multifunctional analyzer 500. In order to ensure the accuracy of the experiment, the temperature and humidity monitoring device is also arranged in the high-low temperature alternating wet heat box 10, and the condition change of the corrosive medium can be monitored and displayed in real time by matching with the temperature and humidity oxygen content sensor. The conditions of the temperature and the oxygen content in the corrosion medium where the metal is located can be intuitively known through the temperature, humidity and oxygen content monitoring device, so that the accurate control is facilitated, and the convenience of operation and the accuracy of a test result are improved.
After the preparation of the work is completed, the electrolytic cell device 100 is in a sealed state, high-purity nitrogen is introduced into the corrosive medium through the air inlet pipe 130 to remove oxygen for 1-2 h, the corrosive medium is attached to the corrosive environment of the metal material actually serving in the deep sea environment through the removal of oxygen, and the reliability and the accuracy of a test result are ensured. After deoxygenation is finished, opening the high-low temperature alternating wet and hot box, the nitrogen cylinder 321, the oxygen cylinder 311, the nitrogen pressure reducing valve 322 and the oxygen pressure reducing valve 312, respectively adjusting the gas flow of the nitrogen flow meter 324 and the oxygen flow meter 314 and the temperature in the high-low temperature alternating wet and hot box according to own experimental conditions, and matching with the multifunctional analyzer 500 to detect the temperature and the oxygen content to realize adjustment;
connecting the leads of different channels of the multi-channel electrochemical workstation 200 with the connecting wires of the motors on the electrolytic cell cover 120 in a one-to-one correspondence manner, opening the multi-channel electrochemical workstation 200 for software setting, wherein the software setting comprises the steps of testing content and time, recording the starting time of an experiment, setting an experiment period according to actual requirements and relevant standards, detecting the galvanic couple potential and the galvanic couple current once every 0.5h, 1h, 2h, 4h, 8h, 12h and 24h, detecting the galvanic couple potential and the galvanic couple current once every other day, and testing the alternating current impedance and the polarization curve.
During the experiment, the corrosion occurring part is observed, the corrosion product form is recorded, the corrosion product components and the corrosion mechanism and process are analyzed, the galvanic potential and the galvanic current value of the complex metal couple under the low-temperature and low-oxygen condition are obtained, the polarity, the galvanic corrosion rate and the like of each metal under the low-temperature and low-oxygen condition can be judged according to the test result, and multiple groups of experiments can be simultaneously carried out.
And after the experiment is finished, closing the nitrogen, oxygen and high-low temperature alternating wet heat box. Taking out the electrolytic cell device 100, opening the electrolytic cell cover 120, taking out the galvanic corrosion samples, observing the corrosion occurrence parts on the surfaces of the samples, recording the forms of corrosion products, analyzing the components and the corrosion mechanism and process of the corrosion products by means of analysis methods such as SEM, EDS, XRD and the like, cleaning the corrosion samples, measuring the contact area of the metal samples, weighing and recording the mass (M) of the metal samples after galvanic corrosion by using a ten-thousandth balance after drying1’、M2’、M3') in g. Calculating the corrosion rate:
Figure DEST_PATH_GDA0002654893790000121
in the formula: vtCorrosion rate mm/a, M-sample mass g, M before experiment1Mass g, S of sample after experiment-total area cm of sample2T-test time h, D-Density of Material kg/m3. The corrosion current density calculated by a polarization curve tested by an electrochemical means and the corrosion rate calculated by a weightlessness experiment are mutually verified to verify the corrosion mechanism and the corrosion rate of the complex metal couple under the conditions of low temperature and low oxygen, so that the accuracy of the experiment is further greatly improved.
Figure DEST_PATH_GDA0002654893790000131
In the formula: icorr-corrosion current density A/m2Vt-etch Rate g/m2H, n-the amount of species that undergo 1mol of electrode reaction to gain or lose electrons, M-molar mass g/mol, F-Faraday constant C/mol, taken as 26.8 A.h.
The test system provided by the utility model is applied to test three metal materials of TA2, B10 and Q235B under different conditions, the result is shown in figures 5-8, and figure 5 is a diagram of galvanic potential and galvanic current of TA2/B10/Q235B under the condition of 0 ℃; FIG. 6 is a plot of the polarization of TA2/B10/Q235B at 0 ℃; FIG. 7 is a diagram showing the galvanic potential and galvanic current of TA2/B10/Q235B under 0.3mg/L (hypoxia) condition, and FIG. 8 is a diagram showing the polarization curve of TA2/B10/Q235B under 0.3mg/L (hypoxia) condition.
Although terms such as an electrolytic cell device, an electrolytic cell body, an electrolytic cell cover, an air inlet pipe, an aeration pipe, an air outlet pipe, a water seal structure, a test electrode, an electrode clamp, a reference electrode, an auxiliary electrode, a lujin capillary tube, a working electrode, a sensor, an electrochemical workstation, a gas supply device, an oxygen cylinder, an oxygen pressure reducing valve, an oxygen supply pipeline, an oxygen flow meter, a nitrogen supply device, a nitrogen cylinder, a nitrogen pressure reducing valve, a nitrogen supply pipeline, a nitrogen flow meter, a three-way valve, a humidifying water tank, a multifunctional analyzer, and the like are used more often herein, the possibility of using other terms is not excluded. These terms are used merely to more conveniently describe and explain the nature of the present invention; they are to be construed in a manner that is inconsistent with the spirit of the invention.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention.

Claims (10)

1. A test system for evaluating metals under deep sea low temperature and low oxygen conditions, comprising: comprises an electrolytic cell device (100) arranged in a temperature-controllable sealed space;
the electrolytic cell device (100) comprises an electrolytic cell body (110), an electrolytic cell cover (120), an air inlet pipe (130), an air outlet pipe (140), a test electrode (150) and a sensor (160);
the electrolytic cell body (110) is used for storing corrosive media; the gas inlet pipe (130) penetrates through the electrolytic cell cover (120) and extends into the corrosive medium, and is used for introducing gas to adjust the oxygen content in the electrolytic cell body (110); the gas outlet pipe (140) is arranged on the electrolytic cell cover (120) in a penetrating way and extends into a space between the electrolytic cell cover (120) and the corrosive medium;
the test electrode (150) comprises an electrode clamp (151), a reference electrode (152) and an auxiliary electrode (153) which are all arranged on the electrolytic cell cover (120) and extend into the corrosive medium; the sensor (160) is mounted on the cell cover (120) and extends into the corrosive medium;
the electrode holder (151), the reference electrode (152), the auxiliary electrode (153) and the sensor (160) are connected with a multi-channel electrochemical workstation (200).
2. The test system for evaluating metals under deep sea low temperature and low oxygen conditions according to claim 1, wherein: the air inlet pipe (130) is connected with an air supply device (300); the gas supply device (300) comprises an oxygen supply device (310) and a nitrogen supply device (320).
3. The test system for evaluating metals under deep sea low temperature and low oxygen conditions according to claim 2, wherein: the oxygen supply device (310) and the nitrogen supply device (320) are connected with the air inlet pipe (130) through a three-way valve (330);
the oxygen supply device (310) comprises an oxygen bottle (311), an oxygen pressure reducing valve (312) on the opening of the oxygen bottle (311), an oxygen supply pipeline (313) for connecting the oxygen bottle (311) and the three-way valve (330), and an oxygen flow meter (314) arranged on the oxygen supply pipeline (313);
the nitrogen supply device (320) comprises a nitrogen gas bottle (321), a nitrogen pressure reducing valve (322) on the opening of the nitrogen gas bottle (321), a nitrogen supply pipeline (323) connecting the nitrogen gas bottle (321) and the three-way valve (330), and a nitrogen gas flow meter (324) arranged on the nitrogen supply pipeline (323).
4. The test system for evaluating metals under deep sea low temperature and low oxygen conditions according to claim 1, wherein: the electrolytic cell body (110) is hermetically connected with the electrolytic cell cover (120) through threads.
5. The test system for evaluating metals under deep sea low temperature and low oxygen conditions according to claim 1, wherein: and an aeration pipe (131) is arranged at the end of the air inlet pipe (130) extending into the corrosive medium.
6. The test system for evaluating metals under deep sea low temperature and low oxygen conditions according to claim 1, wherein: the lower end of the reference electrode (152) is provided with a Lujin capillary tube (154), and the tip end of the Lujin capillary tube (154) extends into a corrosive medium and is aligned with a working electrode (155) fixed below the electrode clamp (151).
7. The test system for evaluating metals under deep sea low temperature and low oxygen conditions according to claim 1, wherein: a humidifying water tank (400) for adjusting the humidity in the space is arranged in the sealed space.
8. The test system for evaluating metals under deep sea low temperature and low oxygen conditions according to claim 1, wherein: and a water seal structure (141) is arranged at the outer side end of the air outlet pipe (140).
9. The test system for evaluating metals under deep sea low temperature and low oxygen conditions according to claim 1, wherein: the multi-channel electrochemical workstation (200) is connected with a multifunctional analyzer (500).
10. The test system for evaluating metals under deep sea low temperature and low oxygen conditions according to claim 1, wherein: the electrode clamps (151) are arranged in a plurality and are sequentially connected in series.
CN202020151439.5U 2020-02-04 2020-02-04 Test system for evaluating metal under deep sea low-temperature and low-oxygen conditions Active CN211741016U (en)

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CN113155724A (en) * 2021-04-28 2021-07-23 中国石油天然气股份有限公司 Multifunctional coupon corrosion evaluation device
CN113640209A (en) * 2021-09-15 2021-11-12 南昌航空大学 Galvanic corrosion and hydrogen diffusion testing device for titanium/aluminum dissimilar metal welded joint
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113155724A (en) * 2021-04-28 2021-07-23 中国石油天然气股份有限公司 Multifunctional coupon corrosion evaluation device
CN113029931A (en) * 2021-05-06 2021-06-25 中国船舶重工集团公司第七二五研究所 Multi-working-condition galvanic corrosion test device
CN113029931B (en) * 2021-05-06 2023-02-21 中国船舶重工集团公司第七二五研究所 Multi-working-condition galvanic corrosion test device
CN113640209A (en) * 2021-09-15 2021-11-12 南昌航空大学 Galvanic corrosion and hydrogen diffusion testing device for titanium/aluminum dissimilar metal welded joint
CN116315042A (en) * 2023-03-23 2023-06-23 清华大学 Single-particle microelectrode reaction tank and manufacturing method thereof
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