CN114894661A - Device and method for automatically testing hydrogen evolution rate of magnesium-based metal material - Google Patents
Device and method for automatically testing hydrogen evolution rate of magnesium-based metal material Download PDFInfo
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Abstract
The invention discloses a device and a method for automatically testing the hydrogen evolution rate of a magnesium-based metal material. The device comprises an experimental tank, a hydrogen collector, an electric lifter, a liquid storage tank, a constant temperature and humidity device, a temperature and humidity sensor, a control mainboard, a visual control system and the like. Firstly, respectively injecting a solution required by testing and a sample to be tested into a liquid storage tank and fixing the solution and the sample to be tested in a sample rack, then setting experimental parameters in a visual control system, automatically starting the device when each parameter in the device reaches a set value, injecting the liquid in the liquid storage tank into an experimental tank and reaching a default liquid level, controlling an electric lifter and a measuring instrument to cooperatively operate by an operation control system, realizing automatic continuous measurement of the volume of hydrogen, and displaying the test results of the volume of hydrogen, the hydrogen evolution rate and the like in real time by the visual control system. The method can efficiently and stably test the hydrogen evolution rate of the magnesium-based metal material for a long time, can avoid the influence of the environmental temperature on the gas volume and the corrosion rate, and improves the accuracy of the test result.
Description
Technical Field
The invention belongs to the field of corrosion, and particularly relates to an automatic hydrogen evolution corrosion rate testing device and method, which are particularly suitable for testing the hydrogen evolution rate of magnesium, magnesium alloy and magnesium-based composite materials.
Background
With the increasingly prominent energy problem and the increasing demand for light weight in the fields of automobiles, aerospace and the like, magnesium alloy is one of ideal light weight materials as the lightest structural material. The magnesium alloy has the characteristics of abundant resources, high specific strength, environmental friendliness, good damping performance, electromagnetic shielding performance, biocompatibility and the like. Magnesium alloys have achieved some large-scale applications as structural materials in the fields of automobiles, 3C products, aerospace, energy industry, biomedical materials, and the like. The development and application of the magnesium alloy are beneficial to the realization of lightweight in China manufacturing, and the realization of the aim of promoting 'double carbon' by greatly promoting energy conservation and emission reduction.
Since the electrode potential of the magnesium alloy is extremely negative and the PB ratio is less than 1, the corrosion resistance of the magnesium alloy is poor. Poor corrosion resistance of magnesium alloys is one of the main reasons that restrict the large-scale application of magnesium alloys. The development of novel corrosion-resistant magnesium alloy is a research hotspot of the current magnesium alloy, the corrosion rate is an important index for evaluating the corrosion resistance of the magnesium alloy, and the corrosion rate of the magnesium alloy in a working condition environment is inevitably required to be used as a use basis for realizing large-scale application. Therefore, a convenient magnesium alloy corrosion rate testing device is indispensable.
In the field of magnesium alloy corrosion research, methods for measuring the corrosion rate of magnesium alloy mainly comprise an electrochemical method, a weight loss method and a hydrogen evolution method. The weight loss method is the mass loss of metal before and after corrosion divided by the corrosion area and corrosion time, and is the most reliable corrosion rate determination method recognized in the field of metal materials. However, the method is usually large in experimental amount and complicated in experimental process, and the obtained corrosion rate is the average corrosion rate of the corrosion process, so that the change condition of the corrosion rate cannot be reflected. The 'negative difference effect' of magnesium makes the difference between the test result of the electrochemical method and the actual value larger, and can only be used as a qualitative analysis means.
Magnesium is highly reactive and corrosion of magnesium is actually a process of reacting with water to form hydrogen:
Mg+2H 2 O＝Mg(OH) 2 ↓+H 2 ↑
the hydrogen evolution method for measuring the corrosion rate of the magnesium is to collect the hydrogen generated in the corrosion process, and the hydrogen evolution rate represents the corrosion rate of the magnesium or the mass loss of the magnesium is converted into the weight loss corrosion rate according to the volume of the collected hydrogen.
At present, the device for measuring the corrosion rate of magnesium and magnesium alloy according to the hydrogen evolution method is formed by combining an inverted funnel and a burette, for example, a special experimental device for measuring the corrosion rate of magnesium or magnesium alloy is disclosed in Chinese patent CN 102564932A. The device has simple structure, low cost and convenient use. But also has some disadvantages: (1) the volume of the collected evolved hydrogen needs to be recorded by experimenters at regular time, and time and labor are consumed. (2) The burette has limited volume and needs to be manually replaced in time after exceeding the measuring range, so that the burette needs to be supervised by experimenters in the whole process. (3) When the test is carried out for a long time, the data recording at night is inconvenient. (4) The influence of temperature on the gas molar volume Vm was not considered, and the calculation formula used the gas molar volume 22.4L/mol in the standard state (0 ℃, 101.33kPa) when calculating the weight loss rate of hydrogen evolution rate conversion. According to the ideal gas equation PV ═ nRT, Vm ═ V/n ═ (RT)/P, at standard atmospheric pressure, the gas molar volume is proportional to the ambient temperature; when the experimental environment temperature is 50 ℃, the gas molar volume is 26.5L/mol. Therefore, the corrosion rate test result has larger error due to the change of the experimental temperature, so that the influence of the temperature on the gas volume needs to be considered when calculating the weight loss corrosion rate of hydrogen evolution rate conversion, the calculation result is more accurate, and the gas molar volume in a standard state cannot be simply used.
Disclosure of Invention
In order to solve the problems described in the background, the invention provides a device and a method for automatically testing the hydrogen evolution rate of magnesium, magnesium alloy and magnesium-based composite materials, the device can automatically obtain the experimental result in real time under a controllable environment, and the specific technical scheme is as follows:
a device for automatically testing the hydrogen evolution rate of a magnesium-based metal material comprises an experiment cabin, an auxiliary cabin, an operation control cabin and a visual control system, wherein the experiment cabin comprises an experiment groove, a full-automatic liquid level control valve is arranged at one side of the experiment groove, a plurality of sample racks are arranged at the bottom in the groove and used for fixing a sample to be tested, and the sample is the magnesium-based metal material; a hydrogen collector array is arranged right above the sample; the hydrogen collector is fixed on the tray; a temperature sensor and a humidity sensor are also arranged in the experiment cabin; the auxiliary cabin comprises a constant temperature and humidity device and a liquid storage barrel, the liquid storage barrel is provided with a heating rod and is communicated with the experiment groove through a guide pipe; the operation control cabin comprises a control main board and an electric lifter array, the electric lifter consists of a servo motor and a telescopic lifting rod, and the front end of the lifting rod is connected with the tray; the visual control system can control all parts of the device to run coordinately according to set experimental parameters, and processes and visually displays the acquired data in real time.
Further, the magnesium-based metal material comprises magnesium, magnesium alloy and magnesium-based composite material.
Furthermore, a full-automatic liquid level control valve arranged on one side of the experiment groove can be automatically opened when the liquid level in the experiment groove is lower than a set value, so that the solution is injected into the experiment groove from the liquid storage groove through the guide pipe, and the valve is closed after the liquid level is restored to the set height.
Furthermore, the hydrogen collector consists of a laser range finder, an electromagnetic valve and a gas collecting bottle; the adjustable range of the data acquisition time interval of the laser range finder is 1-360 min/time, and the laser range finder is used for measuring the height change of the liquid level in the gas collecting bottle caused by collecting hydrogen at regular time; the electromagnetic valve is used for controlling the connection and disconnection of the gas collecting bottle and the outside; the effective volume of the gas collecting bottle is the volume between the scale line of the highest liquid level and the scale line of the lowest liquid level of the gas collecting bottle; three hydrogen collectors are in a group, and three parallel samples are tested at the same time to obtain an average value as a final result; the hydrogen collectors are not less than one group and can be increased according to the test requirements.
Furthermore, the electric lifters are arranged at two ends of the tray, and the electric lifters at the two ends are linked to further drive the group of hydrogen collectors to move up and down; the electric lifter is provided with three gears, namely a standby gear, a working gear and a liquid level reset gear, and has the functions of lifting the hydrogen collector to the highest point to facilitate taking out the experiment tank for cleaning, semi-immersing the hydrogen collector in the solution to facilitate collecting hydrogen, immersing the hydrogen collector in the solution of the experiment tank and opening the electromagnetic valve to enable the liquid level in the gas collecting bottle to be restored to the highest liquid level scale mark.
Further, the temperature and humidity in the experiment cabin are respectively regulated by the constant temperature and humidity device within the range of 0-80 ℃ and 0-99% RH; the heating rod can heat the liquid storage tank seed reagent within the range of 0-80 ℃; when the set values of the temperature and the humidity are-1 in the visual control system, the heating rods in the constant temperature and humidity device and the liquid storage barrel do not work, and an actual environment temperature experiment is adopted.
Furthermore, the control mainboard is a data collection and operation instruction transmission module, is connected with the hydrogen collector, the temperature and humidity sensor, the constant temperature and humidity device, the heating rod and the electric lifter through leads, can acquire measurement data of all parts in real time and control the coordinated operation of all parts, and transmits the measurement data to the visual control system.
Furthermore, the visual control system can issue an operation instruction according to set experimental parameters to control the coordinated operation of each part of the whole device, and carry out real-time processing and visual data display on the acquired data;
data processing calculation formula:
V t ＝mV max +πr 2 (h 0 -h t ) (1)
according to the ideal gas equation: PV-nRT
In formula (1): v t To measure the volume of hydrogen at time t(ml), m is the number of times of liquid level restoration, V max Is the effective volume (ml) of the hydrogen collector, r is the inner radius (mm) of the gas collecting bottle, h 0 Is the initial liquid level height (mm), h t The liquid level height (mm) at the test time t is measured;
in the formula (2): p is H To test the hydrogen evolution rate (ml cm) at time t -2 ·h -1 )，V H Volume of hydrogen evolution per unit area under t (ml. cm) -2 ) T is the test time (h);
in formula (3): p w Hydrogen evolution rate (g cm) expressed for weight loss method -2 ·h -1 ) T is the set experimental temperature (K);
in formula (4): p d Hydrogen evolution rate (mm. y) expressed by depth method -1 ) Rho is the density (g cm) of the material to be measured -3 )；
The hydrogen evolution volume V can be obtained by the formula t Hydrogen evolution rate P H Weight loss corrosion rate P w And depth method corrosion rate P d And drawing a visual curve graph according to the relation data of the corresponding test time.
The use method of the device for automatically testing the hydrogen evolution rate of the magnesium-based metal material is based on the above method, and the method specifically comprises the following steps:
(1) firstly, preparing a required solution, injecting the solution into a liquid storage tank, preparing samples to be detected, enabling each group of samples to be parallel to 3 samples, and fixing the samples to be detected on a sample rack after measuring the exposed area of the samples;
(2) opening a visual control system, setting parameters such as working temperature and humidity of the experiment chamber, solution heating temperature of a liquid storage tank, test time interval, total test time, material density and the like, clicking a start button to start the equipment, starting the constant temperature and humidity device and the heating rod to work, and monitoring the temperature and the humidity in the experiment chamber in real time by the temperature sensor and the humidity sensor;
(3) after the temperature and humidity parameters reach a set value (if the parameters are set to be-1, waiting is not needed), the full-automatic liquid level control valve is opened, the solution is injected into the experiment tank from the liquid storage tank, the full-automatic liquid level control valve is automatically closed after the set height is reached, and the solution can be automatically supplemented after the solution is lower than the set height in the experiment process;
(4) starting the electric lifter, extending the telescopic rod to drive the hydrogen collector to descend to a liquid level reset gear, opening the electromagnetic valve to fill the gas collecting bottle with the solution, closing the electromagnetic valve when the liquid level in the gas collecting bottle is restored to the highest liquid level scale mark, driving the hydrogen collector to ascend to a working gear by the electric lifter, and starting the laser range finder and reading the initial liquid level height;
(5) the laser range finder detects the liquid level height in real time, and transmits data back to the visual control system for data processing and result display;
(6) when the laser range finder detects that the liquid level in the gas collecting bottle is close to the lowest liquid level scale mark, the visual control system issues an instruction to repeat the actions of the steps (4) and (5) so as to achieve the purpose of continuous long-time testing, wherein the time for the step is controlled within 30 s;
(7) after the set test time is reached or the experiment stopping button is clicked by manual operation, the laser range finder reads the final liquid level height;
(8) the method comprises the following steps that (1) an equipment start termination instruction is given, firstly, an electromagnetic valve of a hydrogen collector is opened, solution in a gas collecting bottle is discharged, then, an electric lifter drives the hydrogen collector to return to a standby gear, and the electromagnetic valve is closed;
(9) the visual control system processes and displays the final data, and the experimental result can be derived according to the requirement;
(10) and finally, cleaning the experimental equipment, treating the experimental waste liquid, and closing the equipment.
The technical key points of the invention are as follows:
1. the design of the laser range finder in the hydrogen collector has the function of automatically acquiring the height of the liquid level at regular time without manual reading; the design of the electromagnetic valve of the hydrogen collector can automatically recover the liquid level in the gas collecting bottle under the coordination with the liquid level reset gear of the electric lifter; compared with the prior art of using the burette for manual reading, the automatic reading device is more automatic and efficient.
2. The design of the constant temperature and humidity device enables the experimental test environment to be carried out under the controllable temperature and humidity condition, the hydrogen evolution rate of the material under different temperatures and humidity can be researched, the constant temperature and humidity device is not influenced by the temperature and humidity of the external environment, and the prior art is an open environment which is greatly influenced by the fluctuation of the temperature and humidity of the external environment, so that the accurate measurement of the volume of the hydrogen is influenced.
3. The visualized control software can automatically process and convert the data of the change of the liquid level height along with the time, which is acquired by the hydrogen collector, into the data of the change of the hydrogen volume along with the time according to the formula (1), calculate the hydrogen evolution corrosion rate, the weight loss corrosion rate and the depth method corrosion rate under the corresponding corrosion time according to the formulas (2) to (4), draw a curve graph for visualized display, and the process does not need manual intervention.
The technical scheme of the invention has the beneficial effects that: the invention can carry out long-time experimental test under the conditions of constant temperature and constant humidity, can avoid the influence on the gas volume caused by early-late temperature difference and seasonal temperature change, takes the influence of the temperature on the gas volume into consideration when converting the hydrogen evolution volume rate into the magnesium weight loss rate, substitutes the gas molar volume under the experimental set temperature into calculation instead of uniformly using the gas molar volume under the standard state, and ensures that the calculation result is more accurate; in addition, the mechanical automatic operation of the device saves the manpower.
Drawings
FIG. 1 is a schematic view of an apparatus of the present invention;
FIG. 2 is a cross-sectional view taken at line A-A of FIG. 1;
FIG. 3 is an enlarged view of the hydrogen trap in the apparatus of the present invention;
figure 4 shows the evolution of hydrogen volume and hydrogen evolution rate over time for two materials.
In the figure:
1-experimental groove; 2-full automatic level control valve;
3-sample holder; 4-test sample;
5-hydrogen collector; 5A-laser rangefinder;
5B-electromagnetic valve; 5C-gas collecting bottle;
5D-highest liquid level scale mark; 5E-lowest liquid level scale mark;
6-a support; 7-temperature sensor;
8-humidity sensor; 9-constant temperature and humidity device;
10-liquid storage barrel; 11-heating rod;
12-a catheter; 13-electric lifter;
14-control motherboard; 15-visual control system.
Detailed Description
The invention will be further described with reference to the following drawings and specific embodiments, but the scope of the invention is not limited to the following embodiments. That is, all simple equivalent changes and modifications made by the disclosure of the present invention should fall within the scope of the protection of the patent of the present invention.
[ example 1 ]
The hydrogen evolution corrosion rate of the AZ 31-based composite material in 3.5 wt% NaCl solution is tested by adopting the invention and is compared with the AZ31 matrix, so that two groups of hydrogen collectors are needed to be arranged to collect hydrogen generated by the AZ31 matrix and the AZ 31-based composite material respectively, as shown in the attached figure 2, the specific implementation process is as follows:
1. firstly, preparing 15L of 3.5 wt% NaCl solution, adjusting the pH value of the solution to 7, and then injecting the solution into a liquid storage tank (10);
2. 3 samples of AZ 31-and AZ 31-based composite materials each having a size of 10 mm. times.10 mm were prepared, and exposed to an area of 1cm by epoxy sealing 2 After being polished to 2000#, the silicon carbide abrasive paper is adopted to clean and dry, and then the samples are respectively fixed on a sample rack (3);
3. opening a visual control system (15), setting experiment parameters as shown in table 1, and clicking a start button to start an experiment;
table 1 experimental parameter settings
| Temperature of experiment chamber | Humidity of experiment chamber | Temperature of liquid storage barrel | Sampling interval | Time of measurement | Density of |
Density of |
| 20℃ | 30％RH | 20℃ | 1h | 168h | 1.78g/cm 3 | 1.8g/cm 3 |
4. The temperature sensor (7) and the humidity sensor (8) monitor the temperature and the humidity in the experiment chamber in real time and display the temperature and the humidity on the visual control system (15), the constant temperature and humidity device (9) works, after the temperature and the humidity in the experiment chamber and the solution temperature in the liquid storage barrel (10) reach set values, the full-automatic liquid level control valve (2) is opened, the solution in the liquid storage barrel (10) is injected into the experiment groove (1), and when the liquid level height of the experiment groove (1) reaches the set values, the full-automatic liquid level control valve (2) is closed;
5. when the solution is injected into the experiment groove (1), the electric lifter (13) is automatically started to drive the hydrogen collector (5) to descend to a liquid level reset gear, the electromagnetic valve (5B) is opened at the same time, the solution enters the gas collecting bottle (5C), the electromagnetic valve (5B) is closed after the liquid level reaches the highest liquid level scale mark (5D), the electric lifter (13) drives the hydrogen collector (5) to move upwards to return to a working gear, at the moment, the laser range finder (5A) is started to obtain the initial height value of the liquid level in the gas collecting bottle (5C), and the experiment timing is started;
6. in the experiment process, when the liquid level in the gas collecting bottle (5C) reaches the lowest liquid level scale mark (5E), the hydrogen collector (5) repeats the step 5 to enable the experiment to run for a long time;
7. after the set experiment time is 168h, the visual control system (15) issues an operation stop instruction, the laser range finder (5A) acquires the final liquid level height and transmits data back to the visual control system (15), the electromagnetic valve (5B) of the hydrogen collector (5) is opened, the solution in the gas collecting bottle (5C) is discharged, the electric lifter (13) drives the hydrogen collector (5) to return to a standby gear, and meanwhile the electromagnetic valve (5B) is closed;
8. the data are stored in a visual control system (15) and experimental results are derived according to requirements, and as shown in figure 4, the change curves of hydrogen evolution volumes and hydrogen evolution rates of two materials along with time are shown;
9. the laboratory effluent is properly treated according to the laboratory protocol, the equipment is then cleaned and shut down for the next use.
The method can simply, accurately and efficiently test the hydrogen evolution corrosion rate of the magnesium-based material, avoids the complicated process of manual recording and operation, reduces the manual error, and can promote the standardization and normalization of the hydrogen evolution corrosion rate measurement of the magnesium-based material.
[ example 2 ]
The invention tests the use of AZ31/6061 laminated composite material in the simulation of marine atmosphere solution (1g/L NaCl +0.5 g/LNa) 2 SO 4 +0.5g/L CaCl 2 ) The specific implementation process of the hydrogen evolution corrosion rate is as follows:
1. firstly, 1g/L NaCl +0.5g/L Na is prepared 2 SO 4 +0.5g/L CaCl 2 Adjusting the pH value of the solution to 7 by 10L of the solution, and then injecting the solution into a liquid storage tank (10);
2. 3 samples of AZ 31-and AZ 31-based composite materials each having a size of 10 mm. times.10 mm were prepared, and exposed to an area of 1cm by epoxy sealing 2 After being polished to 2000# by silicon carbide abrasive paperCleaning and drying, and then respectively fixing the samples on the sample rack (3);
3. opening a visual control system (15), setting experiment parameters as shown in table 2, and clicking a start button to start an experiment;
TABLE 2 set points of the experimental parameters
| Temperature of experiment chamber | Humidity of experiment chamber | Temperature of liquid storage barrel | Sampling interval | Time of measurement | Density of |
| 40℃ | 80％RH | 40℃ | 0.5h | 72h | 1.78g/cm 3 |
4. The temperature sensor (7) and the humidity sensor (8) monitor the temperature and the humidity in the experiment chamber in real time and display the temperature and the humidity on the visual control system (15), the constant temperature and humidity device (9) works, after the temperature and the humidity in the experiment chamber and the solution temperature in the liquid storage barrel (10) reach set values, the full-automatic liquid level control valve (2) is opened, the solution in the liquid storage barrel (10) is injected into the experiment groove (1), and when the liquid level height of the experiment groove (1) reaches the set values, the full-automatic liquid level control valve (2) is closed;
5. when the solution is injected into the experiment groove (1), the electric lifter (13) is automatically started to drive the hydrogen collector (5) to descend to a liquid level reset gear, the electromagnetic valve (5B) is opened at the same time, the solution enters the gas collecting bottle (5C), the electromagnetic valve (5B) is closed after the liquid level reaches the highest liquid level scale mark (5D), the electric lifter (13) drives the hydrogen collector (5) to move upwards to return to a working gear, at the moment, the laser range finder (5A) is started to obtain the initial height value of the liquid level in the gas collecting bottle (5C), and the experiment timing is started;
6. in the experiment process, when the liquid level in the gas collecting bottle (5C) reaches the lowest liquid level scale mark (5E), the hydrogen collector (5) repeats the step 5 to enable the experiment to run for a long time;
7. after the set experiment time is 72 hours, the visual control system (15) issues an operation stop instruction, the laser range finder (5A) acquires the final liquid level height and transmits data back to the visual control system (15), the electromagnetic valve (5B) of the hydrogen collector (5) is opened, the solution in the gas collecting bottle (5C) is discharged, the electric lifter (13) drives the hydrogen collector (5) to return to a standby gear, and meanwhile, the electromagnetic valve (5B) is closed;
8. the data are saved in a visual control system (15) and experimental results are derived according to requirements;
9. the laboratory effluent is properly treated according to the laboratory protocol, the equipment is then cleaned and shut down for the next use.
Claims (9)
1. The utility model provides an automatic test magnesium-based metallic material separates device of hydrogen rate which characterized in that: the device consists of four parts, namely an experiment cabin, an auxiliary cabin, an operation control cabin and a visual control system, wherein the experiment cabin comprises an experiment groove, one side of the experiment groove is provided with a full-automatic liquid level control valve, the bottom in the groove is provided with a plurality of sample racks for fixing a sample to be tested, and the sample is made of magnesium-based metal materials; a hydrogen collector array is arranged right above the sample; the hydrogen collector is fixed on the tray; a temperature sensor and a humidity sensor are also arranged in the experiment cabin; the auxiliary cabin comprises a constant temperature and humidity device and a liquid storage barrel, a heating rod is arranged in the liquid storage barrel and is communicated with the full-automatic liquid level control valve through a guide pipe; the operation control cabin comprises an electric lifter and a control main board array, and the front end of a telescopic rod of the electric lifter is connected with the tray; the visual control system can control all parts of the device to run coordinately according to set experimental parameters, and processes and visually displays the acquired data in real time.
2. The apparatus for automatically testing the hydrogen evolution rate of the magnesium-based metal material as claimed in claim 1, wherein: the magnesium-based metal material comprises magnesium, magnesium alloy and magnesium-based composite material.
3. The apparatus for automatically testing the hydrogen evolution rate of the magnesium-based metal material as claimed in claim 1, wherein: the full-automatic liquid level control valve arranged on one side of the experimental tank can be automatically opened when the liquid level in the experimental tank is lower than a set value, so that the solution is injected into the experimental tank from the liquid storage tank through the guide pipe, and the valve is closed after the liquid level is restored to the set height.
4. The apparatus for automatically testing the hydrogen evolution rate of the magnesium-based metal material as claimed in claim 1, wherein: the hydrogen collector consists of a laser range finder, an electromagnetic valve and a gas collecting bottle; the adjustable range of the data acquisition time interval of the laser range finder is 1-360 min/time, and the laser range finder is used for measuring the height change of the liquid level in the gas collecting bottle caused by collecting hydrogen at regular time; the electromagnetic valve is used for controlling the connection and disconnection of the gas collecting bottle and the outside; the effective volume of the gas collecting bottle is the volume between the scale line of the highest liquid level and the scale line of the lowest liquid level of the gas collecting bottle; three hydrogen collectors are in a group, and three parallel samples are tested at the same time to obtain an average value as a final result; the hydrogen collectors are not less than one group and can be increased according to the test requirements.
5. The apparatus for automatically testing the hydrogen evolution rate of the magnesium-based metal material as claimed in claim 1, wherein: the electric lifters are arranged at the two ends of the tray, and the electric lifters at the two ends are linked to further drive the group of hydrogen collectors to move up and down; the electric lifter is provided with three gears, namely a standby gear, a working gear and a liquid level reset gear, and has the functions of lifting the hydrogen collector to the highest point so as to take out the experiment tank for cleaning, semi-immersing the hydrogen collector in the solution so as to collect hydrogen, immersing the hydrogen collector in the solution of the experiment tank and opening the electromagnetic valve so as to restore the liquid level in the gas collecting bottle to the highest liquid level scale mark.
6. The apparatus for automatically testing the hydrogen evolution rate of the magnesium-based metal material as claimed in claim 1, wherein: the temperature and humidity in the experiment cabin are respectively regulated by the constant temperature and humidity device within the range of 0-80 ℃ and 0-99% RH; the heating rod can heat the reagent in the liquid storage tank within the range of 0-80 ℃; when the set value of the parameters is-1 in the visual control system, the system does not work, and the actual environment temperature and humidity are adopted for carrying out experiments.
7. The apparatus for automatically testing the hydrogen evolution rate of the magnesium-based metal material as claimed in claim 1, wherein: the control mainboard is a data collection and operation instruction transmission module, is connected with each part through a wire, can acquire the measurement data of each part in real time and control coordinated operation, and transmits the measurement data to the visual control system for data processing.
8. The apparatus for automatically testing the hydrogen evolution rate of the magnesium-based metal material as claimed in claim 1, wherein: the visual control system can issue an operation instruction according to set experimental parameters to control the coordinated operation of each part of the whole device, and carry out real-time processing and visual data display on the acquired data;
data processing calculation formula:
V t ＝mV max +πr 2 (h 0 -h t ) (1)
according to the ideal gas equation: PV-nRT
In formula (1): v t The volume (ml) of hydrogen at the time t is measured, m is the number of liquid level resets, V max Effective volume (ml) of hydrogen collector, r is inner radius (mm) of gas collecting bottle, h 0 Is the initial liquid level height (mm), h t The liquid level height (mm) at the test time t is measured;
in formula (2): p H To test the hydrogen evolution rate (ml cm) at time t -2 ·h -1 )，V H Volume of hydrogen evolution per unit area under t (ml. cm) -2 ) T is the test time (h);
in formula (3): p w Hydrogen evolution rate (g cm) expressed for weight loss method -2 ·h -1 ) T is the set experimental temperature (K);
in formula (4): p d Hydrogen evolution rate (mm. y) expressed by depth method -1 ) Rho is the density (g cm) of the material to be measured -3 )；
The hydrogen evolution volume V can be obtained by the formula t Hydrogen evolution rate P H Weight loss corrosion rate P w And depth method corrosion rate P d And drawing a visual curve graph according to the relation data of the corresponding test time.
9. A method for automatically testing the hydrogen evolution rate of a magnesium-based metal material based on the device of claims 1-8, which is characterized by comprising the following steps:
(1) injecting a prepared solution into a liquid storage tank, fixing a sample to be tested on a sample rack, and measuring the exposed area of the sample, wherein each group of parallel samples comprises 3 samples;
(2) starting a visual control system, setting working temperature, humidity, liquid storage tank solution temperature, test time and sampling interval parameters of the experiment chamber, clicking to start equipment, starting a constant temperature and humidity device and a heating rod to work, and monitoring the temperature and the humidity in the experiment chamber in real time by a temperature sensor and a humidity sensor;
(3) after each temperature and humidity parameter reaches a set value, a valve of the full-automatic liquid level control valve is opened, the solution in the liquid storage tank is injected into the experiment tank through the conduit, the valve is closed after the solution reaches a set height, and if the temperature and humidity set values are-1, waiting is not needed;
(4) the electric lifter drives the hydrogen collector to descend to a liquid level reset gear, the electromagnetic valve is opened at the moment to enable the solution to fill the gas collecting bottle, the electromagnetic valve is closed when the liquid level in the gas collecting bottle is restored to the highest liquid level scale mark, the lifter drives the hydrogen collector to ascend to a working gear, and then the laser range finder is started and reads an initial liquid level height value;
(5) the laser range finder detects the height change of the liquid level in real time and transmits data back to the visual control system for data processing and result display; demonstration results include, but are not limited to, hydrogen evolution rate P H (ml·cm -2 ·h -1 ) Magnesium corrosion rate P W (g·cm -2 ·h -1 Or mm. y -1 ) And the time variation of the two graphs;
(6) when the laser range finder detects that the liquid level in the gas collecting bottle reaches the lowest liquid level scale mark, the visual control system issues an instruction to repeat the actions of the steps (4) and (5) so as to achieve the purpose of continuous long-time testing;
(7) after the set test time is reached or the experiment stopping button is clicked by manual operation, the laser range finder reads the final liquid level height;
(8) the method comprises the following steps that (1) an equipment start termination instruction is given, firstly, an electromagnetic valve of a hydrogen collector is opened, solution in a gas collecting bottle is discharged, then, an electric lifter drives the hydrogen collector to return to a standby gear, and the electromagnetic valve is closed;
(9) the visual control system processes and displays the final data, and the experimental result can be derived according to the requirement;
(10) and finally, cleaning the experimental equipment, treating the experimental waste liquid, and closing the equipment.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210394555.3A CN114894661A (en) | 2022-04-13 | 2022-04-13 | Device and method for automatically testing hydrogen evolution rate of magnesium-based metal material |
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| CN202210394555.3A CN114894661A (en) | 2022-04-13 | 2022-04-13 | Device and method for automatically testing hydrogen evolution rate of magnesium-based metal material |
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