CN112363076A - Dynamics testing device and method for alloy hydrogen storage material - Google Patents
Dynamics testing device and method for alloy hydrogen storage material Download PDFInfo
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 227
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 227
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 165
- 238000012360 testing method Methods 0.000 title claims abstract description 69
- 239000000956 alloy Substances 0.000 title claims abstract description 64
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 52
- 239000011232 storage material Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 30
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 61
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- 238000007599 discharging Methods 0.000 claims abstract description 28
- 230000008569 process Effects 0.000 claims abstract description 24
- 238000003860 storage Methods 0.000 claims abstract description 22
- 239000000446 fuel Substances 0.000 claims abstract description 17
- 238000012544 monitoring process Methods 0.000 claims abstract description 11
- 230000004913 activation Effects 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001994 activation Methods 0.000 claims description 10
- 239000001307 helium Substances 0.000 claims description 10
- 229910052734 helium Inorganic materials 0.000 claims description 10
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 9
- 238000001514 detection method Methods 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 150000004678 hydrides Chemical class 0.000 claims description 5
- 238000010926 purge Methods 0.000 claims description 5
- 239000006104 solid solution Substances 0.000 claims description 5
- 229910052720 vanadium Inorganic materials 0.000 claims description 5
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 229910002335 LaNi5 Inorganic materials 0.000 claims description 3
- 229910019758 Mg2Ni Inorganic materials 0.000 claims description 3
- 229910010340 TiFe Inorganic materials 0.000 claims description 3
- 229910010382 TiMn2 Inorganic materials 0.000 claims description 3
- 229910008357 ZrMn2 Inorganic materials 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 3
- 239000008187 granular material Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 238000005429 filling process Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims 2
- 238000005275 alloying Methods 0.000 claims 1
- 238000010998 test method Methods 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 238000009849 vacuum degassing Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011081 inoculation Methods 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
- G01R31/392—Determining battery ageing or deterioration, e.g. state of health
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0078—Testing material properties on manufactured objects
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
- G01R31/382—Arrangements for monitoring battery or accumulator variables, e.g. SoC
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Abstract
The invention discloses a device and a method for testing dynamics of an alloy hydrogen storage material, which consists of a pipeline system, a sample reaction tank, a temperature control system and a data acquisition and monitoring system, wherein the pipeline system realizes automatic switching of hydrogen charging and hydrogen discharging by an electromagnetic valve, the hydrogen charging process utilizes a mass flowmeter to test the instantaneous flow of hydrogen charging under certain pressure and temperature, and the hydrogen discharging process utilizes a mass flow controller to accurately control the output flow of hydrogen discharging; the heat exchange place in the temperature control system is a water bath or an oil bath, and the temperature control range is wide; data acquisition and monitoring are carried out through the PLC and the upper computer, and full-automatic operation can be realized. The invention overcomes the defects of PCT curve test of the alloy hydrogen storage material, can carry out activation performance, hydrogen charging and discharging curve and cycle life test on the alloy hydrogen storage material, and has important significance for evaluating the matching performance of the hydrogen storage alloy and the fuel cell according to the test result.
Description
Technical Field
The invention belongs to the technical field of fuel cells, and particularly relates to a dynamic testing device and a dynamic testing method for an alloy hydrogen storage material.
Background
The fuel cell is considered as a fourth generation power generation technology following thermal power, hydroelectric power and nuclear power, and is a new energy power generation technology. The fuel cell can be applied to the fields of electric automobiles, underwater power supplies, aviation power supplies, standby power supplies, fixed power stations, portable power supplies and the like, and the fuel cell is listed as the first of ten technologies of changing human lives in the 21 st century in the epoch.
The alloy hydrogen storage technology is a hydrogen source technology for fuel cells, and under a certain temperature and pressure, the alloy can absorb a large amount of hydrogen and react to generate metal hydride. The hydride heats up or lowers the hydrogen pressure and the hydride undergoes a decomposition reaction to provide hydrogen to the fuel cell. The alloy hydrogen storage technology has the characteristics of high hydrogen storage density, pure outlet hydrogen, good safety performance and the like, and is a good choice for serving as a hydrogen source for fuel cells in the fields of spaceflight, underwater and the like.
At present, PCT curve test is mainly used to evaluate the hydrogen storage performance of hydrogen storage alloys for fuel cells, and the test parameters are some thermodynamic basic parameters of the alloy materials, such as reaction enthalpy change, reaction entropy change, platform pressure, platform slope, hysteresis factor, and the like. However, as a hydrogen source technology for fuel cells, the matching performance of hydrogen storage devices and fuel cells is often of more concern, and the kinetic evaluation of alloy materials is particularly important. The activation performance, hydrogen charging and discharging curve, cycle life and the like of the hydrogen storage alloy are important indexes influencing the realization of engineering application, and the parameters can not be measured through the PCT curve of the alloy material.
Disclosure of Invention
One of the purposes of the invention is to make up the defects of the prior art, and design a dynamic testing device of a hydrogen storage alloy material to realize the evaluation of the activation performance, the hydrogen charging and discharging curve and the cycle life of the hydrogen storage alloy for the fuel cell.
The technical scheme adopted by the invention for solving the technical problems is as follows: a dynamics testing device for alloy hydrogen storage materials comprises a pipeline system, a sample reaction tank, a temperature control system and a data acquisition and monitoring system; pipeline system including the solenoid valve I, mass flow meter and the filter of connecting gradually, I entry of solenoid valve is gone through manual valve I on one hand and is connected the hydrogen import, constitutes the branch road that charges hydrogen, and one is gone through manual valve II on one hand and is connected the helium import, and two branch roads are drawn forth simultaneously to check valve I, and one connects gradually and connects the hydrogen discharge port after manual valve V, solenoid valve II, the mass flow controller, constitutes the branch road that discharges hydrogen for evacuation hydrogen, realizes the automatic switch-over that charges hydrogen and discharge by solenoid valve I and solenoid valve II: the hydrogen charging branch utilizes a mass flowmeter to test the instantaneous hydrogen charging flow under certain pressure and temperature; the hydrogen discharge branch utilizes the mass flow controller to accurately control the hydrogen discharge output flow; the sample reaction tank consists of a tank body, a flange arranged at an opening at the top of the tank body, and an air guide pipe and a tank opening valve which are arranged on the flange, the filter is connected with an outlet of the tank body, and a safety valve is also arranged at the outlet of the tank body; the temperature control system consists of a constant temperature bath and a temperature transmission controller; the data acquisition and monitoring system consists of a PLC and an upper computer, wherein the PLC is respectively connected with the electromagnetic valve I, the mass flow meter, the electromagnetic valve II, the mass flow controller and the vacuum pressure sensor at the outlet of the tank body.
The dynamics testing device for the alloy hydrogen storage material is characterized in that an explosion-proof vacuum pump is connected in parallel in a hydrogen discharge branch to realize the vacuum pumping treatment of a sample reaction tank in the activation process, and an inlet of the explosion-proof vacuum pump is connected with a filter through a manual valve VI.
According to the dynamics testing device for the alloy hydrogen storage material, a pressure reducing valve I is arranged at the front end of an electromagnetic valve I on a hydrogen charging branch in a pipeline system, a one-way valve I is arranged at the rear end of a mass flow meter, and manual valves III are connected in parallel on pipelines of the electromagnetic valve I, the mass flow meter and the one-way valve I to prevent the pipeline from being damaged by overlarge pressure and hydrogen backflow.
According to the dynamics testing device for the alloy hydrogen storage material, a pressure reducing valve II is arranged at the front end of an electromagnetic valve II, a check valve II is arranged at the rear end of a mass flow controller, and a manual valve VI is connected in parallel to pipelines of the electromagnetic valve II, the mass flow controller and the check valve II.
According to the dynamics testing device for the alloy hydrogen storage material, the tank body is made of high-temperature-resistant stainless steel, the opening of the tank body is connected with a safety valve in parallel, and when the pressure exceeds a set value, the system is subjected to pressure relief protection.
According to the dynamics testing device for the alloy hydrogen storage material, a flame arrester is arranged at a hydrogen discharge port of the dynamics testing device, so that flame propagation in an emergency situation is prevented.
The constant-temperature bath medium of the device for testing the dynamics of the alloy hydrogen storage material is a water bath or an oil bath.
The invention also aims to provide a dynamic testing method of the hydrogen storage alloy material, which comprises the following steps:
sample loading and leak detection: loading a hydrogen storage alloy sample into a tank body, sequentially connecting a gas guide pipe and a tank opening valve, placing a sample reaction tank into a constant temperature bath, connecting an outlet of the tank opening valve with a pipeline system, and performing air tightness detection by using helium gas purging and a vacuum pressure sensor;
activation treatment: setting the temperature of a constant temperature bath by an upper computer, opening an explosion-proof vacuum pump and a manual valve VII, vacuumizing a sample reaction tank, then closing the manual valve VII and the explosion-proof vacuum pump, opening a manual valve I, adjusting a pressure reducing valve I and opening a manual valve III, closing the manual valve III after hydrogen enters the sample reaction tank, and inoculating and activating the sample reaction tank under certain pressure; judging the hydrogen absorption trend of the alloy hydrogen storage material through a pressure-time curve generated by an upper computer, and repeating a plurality of cycles of vacuum degassing, full hydrogen absorption and complete hydrogen release until the hydrogen storage alloy sample is completely activated according to the actual situation;
and (3) testing a hydrogen charging and discharging curve: testing the instantaneous hydrogen charging flow of the mass flow meter at a certain temperature and pressure in the hydrogen charging process, and outputting a hydrogen charging instantaneous flow/accumulated hydrogen charging flow-time curve through an upper computer; setting a hydrogen discharge program through an upper computer and a PLC according to the actual working condition of the fuel cell in the hydrogen discharge process, and generating an output pressure/accumulated hydrogen discharge flow-time curve;
and (3) testing the cycle life: starting a program through a PLC and an upper computer, firstly inputting and determining basic parameters of a cycle period, a hydrogen charging and discharging temperature, a hydrogen charging stop flow, hydrogen charging process time, a hydrogen discharging constant flow and a hydrogen discharging stop pressure, and recording the cycle period N =0 after the constant temperature bath temperature reaches the set hydrogen charging and discharging temperature; then opening the solenoid valve I, carrying out a hydrogen charging test, generating an instantaneous flow/accumulated hydrogen charging flow-time curve by an upper computer in the hydrogen charging process, and closing the solenoid valve I to finish the hydrogen charging when the time reaches the set hydrogen charging process time and the flow is less than the set hydrogen charging stop flow; then opening an electromagnetic valve II, carrying out a hydrogen discharge test at a set constant flow, wherein an upper computer generates an output pressure/accumulated hydrogen discharge flow-time curve in the hydrogen discharge process, when the pressure is lower than a set hydrogen discharge cut-off pressure, closing the electromagnetic valve II to finish hydrogen discharge, the cycle period is N +1, the upper computer generates a hydrogen discharge volume-cycle period curve, and when the cycle period N reaches a set cycle period number, the test is finished; in the cycle life test, a hydrogen evolution volume-cycle period curve is generated. The hydrogen discharge curve test and the cycle life test can be completed under the full-automatic condition.
During the hydrogen charging process, hydrogen is regulated to a proper pressure through a pressure reducing valve I and then enters a sample reaction tank through a manual valve I, an electromagnetic valve I, a mass flow meter and a tank opening valve, the sample reaction tank provides a reaction place for the hydrogen and the hydrogen storage alloy, and the hydrogen is fully diffused through an air guide pipe and reacts with the hydrogen storage alloy sample to generate hydride; in the hydrogen releasing process, hydrogen is released from the sample reaction tank and is regulated to the required pressure through the pressure reducing valve II, and the output flow is accurately controlled through the mass flow controller.
The method for testing the dynamics of the alloy hydrogen storage material can test the type of the alloy material as LaNi5、ZrMn2、TiMn2、TiFe、Mg2Ni, vanadium-based solid solutions, etc., in the form of powder, granules, or blocks.
The invention has the beneficial effects that: according to the dynamics testing device for the alloy hydrogen storage material, a pipeline system realizes automatic switching of hydrogen charging and hydrogen discharging through the electromagnetic valve, a hydrogen charging branch utilizes the mass flowmeter to test the instantaneous hydrogen charging flow under certain pressure and temperature, and a mass flow controller is utilized in the hydrogen discharging process to accurately control the hydrogen discharging output flow. The sample reaction tank is connected by a flange, so that the sample is conveniently assembled and disassembled. The temperature range in the temperature control system is wide, and the test requirements of different alloy hydrogen storage materials can be met. The data acquisition and monitoring system consists of a PLC and an upper computer, and can realize the test of the hydrogen charging and discharging curve and the cycle life test under the full-automatic condition after the alloy hydrogen storage material is activated. The device overcomes the defect that the thermodynamic property of the alloy hydrogen storage material is evaluated only by using a PCT curve, and can be used for researching the matching property of the alloy hydrogen storage material and a fuel cell.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of the structure of a sample reaction tank according to the present invention;
fig. 3 is a control flow chart of the cyclic hydrogen charge and discharge test of the present invention.
The figures are numbered: 1-hydrogen inlet, 2-helium inlet, 3-manual valve I, 4-manual valve II, 5-pressure reducing valve I, 6-pressure gauge, 7-electromagnetic valve I, 8-mass flowmeter, 9-one-way valve I, 10-manual valve III, 11-manual valve IV, 12-filter, 13-safety valve, 14-vacuum pressure sensor, 15-sample reaction tank, 15 a-flange, 15 b-tank valve, 15 c-bolt, 15 d-gasket, 15 e-tank, 15 f-alloy material, 15 g-air duct, 16-thermostatic bath, 17-temperature transmission controller, 18-manual valve V, 19-pressure reducing valve II, 20-electromagnetic valve II, 21-mass flow controller, 22-one-way valve II, 23-manual valve VI, 24-flame arrester, 25-manual valve VII, 26-vacuum pump explosion-proof machine, 27-PLC, 28-upper computer.
Detailed Description
The present invention will be described in detail with reference to the drawings and examples, which follow.
Referring to fig. 1, the invention discloses a dynamic testing device for an alloy hydrogen storage material, which mainly comprises a pipeline system, a sample reaction tank 15, a temperature control system and a data acquisition and monitoring system.
The pipeline system comprises a pressure reducing valve I5, an electromagnetic valve I7, a mass flow meter 8, a one-way valve I9 and a filter 12 which are sequentially connected, wherein one way of an inlet of the pressure reducing valve I5 is connected with a hydrogen inlet 1 through a manual valve I3 to form a hydrogen charging branch, one way of the inlet is connected with a helium inlet 2 through a manual valve II 4, one way of helium connected with the hydrogen inlet 1 in parallel is used for pipeline purging and leak detection of a sample reaction tank 15, two branches are led out from the one-way valve I9 at the same time, a flame arrester 24 connected with a hydrogen discharge port after being sequentially connected with a manual valve V18, a pressure reducing valve II 19, an electromagnetic valve II 20, a mass flow controller 21 and a one-way valve II 22 to form a hydrogen discharge branch for discharging hydrogen, the manual valve III 10 is used for preventing the hydrogen from being damaged by overlarge pressure and hydrogen backflow, and the manual valve VI 23 is connected in parallel, the automatic switching of charging and discharging hydrogen is realized by the solenoid valve I7 and the solenoid valve II 20: the mass flowmeter 8 is utilized in the hydrogen charging branch to test the instantaneous hydrogen charging flow under certain pressure and temperature; the hydrogen discharge branch utilizes the mass flow controller 21 to accurately control the hydrogen discharge output flow. An explosion-proof vacuum pump 26 is connected in parallel in the hydrogen discharge branch to realize the vacuum pumping treatment of the sample reaction tank 15 in the activation process, and the inlet of the explosion-proof vacuum pump 26 is connected with the filter 12 through a manual valve VII 25.
Referring to fig. 2, the sample reaction tank 15 is composed of a tank body 15e made of high-temperature resistant stainless steel, a flange 15a installed at an opening at the top of the tank body 15e, an air guide pipe 15g and a tank opening valve 15b arranged on the flange 15a, a bolt 15c and a gasket 15d, the flange 15a is connected to conveniently detach and replace an alloy material 15f, the filter 12 is connected with an outlet of the tank body 15e to prevent tiny powder brought out by gas in the hydrogen discharge process from affecting a pipeline system, an analysis sampling port is arranged at the rear end of the filter, a safety valve 13 is further arranged at the outlet of the tank body 15e, and analysis sampling is performed by using a manual valve iv 11.
The temperature control system consists of a constant temperature bath 16 and a temperature transmission controller 17, the heat released by the generated hydride is taken away in the hydrogen charging process, and the heat is provided for the reverse reaction in the hydrogen discharging process; the heat exchange place in the temperature control system is a water bath or an oil bath, and the bath is connected with a heating and cooling circulating device provided with a temperature transmission controller 17.
Data acquisition and monitored control system constitute by PLC 27 and host computer 28, PLC 27 be connected with solenoid valve I7, mass flow meter 8, solenoid valve II 20, mass flow controller 21, vacuum pressure sensor 14 respectively for opening and closing of control solenoid valve I7 and solenoid valve II 20, monitoring vacuum pressure sensor 14's registration, monitoring and control constant temperature bath 16's temperature, the instantaneous flow of hydrogen process monitoring mass flow meter 8 fills, the accurate control output flow of hydrogen process through mass flow controller 21.
The test alloy material 15f type can be LaNi5、ZrMn2、TiMn2、TiFe、Mg2Ni, vanadium-based solid solutions, etc., in the form of powder, granules, or blocks.
As shown in FIG. 3, this example takes a vanadium-based solid solution hydrogen storage alloy as an example to illustrate the kinetic testing method of the alloy hydrogen storage material.
Sample loading and leak detection
Before testing, the vanadium-based solid solution hydrogen storage alloy sample 15f is placed in the tank 15e, and then the gas-guide tube 15g, the gasket 15d, the flange 15a and the bolt 15c are connected in sequence according to the mode shown in fig. 2. The sample reaction tank 15 is placed in a constant temperature bath 16 at 25 ℃, the outlet of the tank opening valve 15b is connected with a pipeline system joint, then a helium purging system is used for purging, the air tightness detection is carried out through a vacuum pressure sensor 14, and all valves are closed after the completion.
And opening a manual valve II 4, adjusting the indication number from a pressure reducing valve I5 to a pressure gauge 6 to be 4MPa, and then sequentially opening a manual valve III 10 and a tank opening valve 15b to enable helium to enter a sample reaction tank 15. After the reading of the sensor 14 increased to 4.0MPa, the manual valve III 10 was closed. And judging whether the reaction tank has a leakage condition or not through a pressure-time curve generated by the upper computer 28. After the airtightness is tested, the manual valve V18 is opened, the pressure reducing valve II 19 is adjusted, the manual valve VI 23 is slowly adjusted to release helium until the reading of the sensor 14 is micro-positive pressure, and the opened valve is closed.
Activation treatment
The surface of the hydrogen storage alloy usually adsorbs a layer of oxide film or other impurities, which prevents the normal hydrogen absorption and desorption, and the hydrogen storage alloy needs to be activated to reach the normal hydrogen absorption and desorption amount. The temperature of the constant temperature bath 16 is set to be more than or equal to 80 ℃ by the upper computer 28, the explosion-proof vacuum pump 26 and the manual valve VII 25 are opened, and the sample reaction tank 15 is vacuumized for 30 min. And (3) closing the manual valve VII 25 and the explosion-proof vacuum pump 26, opening the manual valve I3, adjusting the indication number from the pressure reducing valve I5 to the pressure gauge 6 to be 4MPa, opening the manual valve III 10, introducing hydrogen into the sample reaction tank 15, closing the manual valve III 10, and inoculating and activating for 30min under the pressure condition of 4.0 MPa. The pressure-time curve generated in the upper computer 28 is used to judge whether the alloy hydrogen storage material has the tendency of absorbing hydrogen. If there is no tendency to absorb hydrogen, the pressure in the sample reactor is released. And then repeating the vacuum degassing, pressure maintaining inoculation and pressure releasing for a plurality of cycles until the alloy material has a hydrogen absorption trend.
After having a tendency to absorb hydrogen, the temperature of the constant temperature bath 16 is adjusted to 25 ℃. The alloy material fully absorbs hydrogen to saturation under the temperature condition, then completely releases hydrogen, judges the hydrogen absorption trend of the alloy hydrogen storage material through a pressure-time curve generated by the upper computer 28, and utilizes the mass flow controller 21 to count the accumulated hydrogen release volume according to the actual situation. And after the hydrogen discharge is finished, repeating a plurality of cycles of vacuum degassing, fully absorbing hydrogen and completely discharging hydrogen until the hydrogen discharge volume of two adjacent cycles is not obviously increased, and finishing the activation of the alloy material.
Hydrogen charging and discharging curve test
After the activation is completed, the reaction pressure and the medium temperature are important factors influencing the hydrogen absorption rate of the alloy hydrogen storage material. And (3) testing a hydrogen charging curve, namely adjusting the reaction pressure of the sample reaction tank 15 through a pressure reducing valve I5, and setting the medium temperature of the constant-temperature bath 16 by the upper computer 28 to obtain a hydrogen charging instantaneous flow/hydrogen charging accumulated flow-time curve under certain temperature and pressure.
The sample retort 15 is charged with hydrogen to saturation at a certain pressure and temperature. The matching performance of the reaction tank and the fuel cell is tested, the hydrogen discharge flow is controlled by the mass flow controller 21, and the medium temperature is controlled by the temperature controller 17, so that output pressure and accumulated flow-time curves of the alloy reaction tank 15 under different working conditions can be obtained. Under different working conditions, programs are set through the PLC 27 and the upper computer 28, and the hydrogen discharge curve test is realized under the full-automatic condition.
Cycle life test
The cycle life is an important index affecting the matching of the hydrogen storage alloy with the fuel cell, and a cycle life test is performed with reference to a control flow chart shown in fig. 3. The service life test can be performed under a fully automatic condition through the PLC 27 and the upper computer 28. After the starting program, basic parameters such as a cycle period, a hydrogen charging and discharging temperature, a hydrogen charging cut-off flow, a hydrogen charging process time, a hydrogen discharging constant flow and a hydrogen discharging cut-off pressure are firstly input and determined.
After the temperature of the constant temperature bath 16 reached the set hydrogen charge/discharge temperature, the cycle period N =0 was recorded. And then opening the electromagnetic valve I7 to perform a hydrogen filling test, wherein an instantaneous flow and a hydrogen filling accumulated flow-time curve are generated in the hydrogen filling process. And when the time reaches the set hydrogen charging process time and the flow is less than the set hydrogen charging cut-off flow, closing the electromagnetic valve I7 and finishing the hydrogen charging. And then opening the electromagnetic valve II 20 to perform a hydrogen discharge test at a set constant flow, wherein an output pressure and hydrogen discharge accumulated flow-time curve is generated in the hydrogen discharge process. And when the pressure is lower than the set hydrogen discharge stop pressure, closing the electromagnetic valve II 20 and finishing the hydrogen discharge. Cycle N = N +1 and generates a hydrogen evolution volume-cycle period curve. And when the cycle period N reaches the set cycle period, ending the test, otherwise, turning to open the electromagnetic valve I7 to perform the next cycle test.
The above embodiments are merely illustrative of the principles and effects of the present invention, and some embodiments may be applied, and it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the inventive concept of the present invention, and these embodiments are within the scope of the present invention.
Claims (10)
1. A dynamic testing device for alloy hydrogen storage materials is characterized in that: comprises a pipeline system, a sample reaction tank (15), a temperature control system and a data acquisition and monitoring system;
the pipeline system comprises a solenoid valve I (7), a mass flow meter (8) and a filter (12) which are sequentially connected, one path of an inlet of the solenoid valve I (7) is connected with a hydrogen inlet (1) through a manual valve I (3) to form a hydrogen charging branch, the other path of the inlet of the solenoid valve I (7) is connected with a helium inlet (2) through a manual valve II (4), two branches are simultaneously led out from a one-way valve I (9), one branch is sequentially connected with a manual valve V (18), a solenoid valve II (20) and a mass flow controller (21) and then connected with a hydrogen discharge port to form a hydrogen discharge branch, and the solenoid valve I (7) and the solenoid valve II (20) realize automatic switching of hydrogen charging and;
the sample reaction tank (15) consists of a tank body (15 e), a flange (15 a) arranged at the opening at the top of the tank body (15 e), an air guide pipe (15 g) arranged on the flange (15 a) and a tank opening valve (15 b), and the filter (12) is connected with the outlet of the tank body (15 e);
the temperature control system consists of a constant temperature bath (16) and a temperature transmission controller (17);
the data acquisition and monitoring system is composed of a PLC (27) and an upper computer (28), wherein the PLC (27) is respectively connected with the electromagnetic valve I (7), the mass flow meter (8), the electromagnetic valve II (20) and the mass flow controller (21).
2. The device for testing the kinetics of alloy hydrogen storage materials according to claim 1, characterized in that an explosion-proof vacuum pump (26) is connected in parallel in the hydrogen discharge branch, the sample reaction tank (15) is vacuumized in the activation process, and the inlet side of the explosion-proof vacuum pump (26) is connected with the filter (12) through a manual valve VII (25).
3. The device for testing the kinetics of the alloy hydrogen storage material according to claim 1, wherein a pressure reducing valve I (5) is arranged at the front end of the electromagnetic valve I (7), a check valve I (9) is arranged at the rear end of the mass flow meter (8), and a manual valve III (10) is connected in parallel with pipelines of the electromagnetic valve I (7), the mass flow meter (8) and the check valve I (9).
4. The device for testing the kinetics of the alloy hydrogen storage material according to claim 1, wherein a pressure reducing valve II (19) is arranged at the front end of the electromagnetic valve II (20), a check valve II (22) is arranged at the rear end of the mass flow controller (21), and a manual valve VI (23) is connected in parallel with pipelines of the electromagnetic valve II (20), the mass flow controller (21) and the check valve II (22).
5. The device for testing the kinetics of the alloy hydrogen storage material according to claim 1, wherein the material of the tank body (15 e) is high temperature resistant stainless steel, and a safety valve (13) is arranged at the outlet of the tank body (15 e).
6. The kinetic testing device of an alloy hydrogen storage material as claimed in claim 1, wherein a flame arrester (24) is disposed at the hydrogen discharge port.
7. The kinetic testing device for alloy hydrogen storage materials of claim 1, wherein the constant temperature bath (16) medium is a water bath or an oil bath.
8. A test method based on the test apparatus of any of claims 1 to 7, comprising the steps of:
sample loading and leak detection: a hydrogen storage alloy sample (15 f) is placed in a tank body (15 e) and is connected with a gas guide pipe (15 g) and a tank opening valve (15 b), the sample reaction tank (15) is placed in a constant temperature bath (16), the outlet of the tank opening valve (15 b) is connected with a pipeline system, and helium is used for purging and air tightness detection;
activation treatment: setting the temperature of a constant temperature bath (16) through an upper computer (28), opening an explosion-proof vacuum pump (26) and a manual valve VII (25), vacuumizing a sample reaction tank (15), then closing the manual valve VII (25) and the explosion-proof vacuum pump (26), opening a manual valve I (3), adjusting a pressure reducing valve I (5) and opening a manual valve III (10), closing the manual valve III (10) after hydrogen enters the sample reaction tank (15), and inoculating and activating the sample reaction tank (15) under certain pressure;
and (3) testing a hydrogen charging and discharging curve: testing the instantaneous flow of hydrogen charging of the mass flowmeter (8) at a certain temperature and pressure in the hydrogen charging process, and outputting a curve of the instantaneous flow of hydrogen charging/accumulated flow of hydrogen charging-time through an upper computer (28); in the hydrogen discharge process, according to the actual working condition of the fuel cell, a hydrogen discharge program is set through an upper computer (28) and a PLC (27), and an output pressure/accumulated hydrogen discharge flow-time curve is generated;
and (3) testing the cycle life: starting a program through a PLC (27) and an upper computer (28), firstly inputting and determining basic parameters of a cycle period, a hydrogen charging and discharging temperature, a hydrogen charging cut-off flow, a hydrogen charging process time, a hydrogen discharging constant flow and a hydrogen discharging cut-off pressure, and recording the cycle period N =0 after a constant temperature bath (16) reaches a set hydrogen charging and discharging temperature; then opening the solenoid valve I (7), carrying out a hydrogen filling test, and closing the solenoid valve I (7) to finish hydrogen filling when the set hydrogen filling process time is reached and the flow is less than the set hydrogen filling stop flow; and opening the electromagnetic valve II (20), performing a hydrogen discharge test at a set constant flow, closing the electromagnetic valve II (20) to finish the hydrogen discharge when the pressure is lower than a set hydrogen discharge stop pressure, wherein the cycle period is N +1, generating a hydrogen discharge volume-cycle period curve by the upper computer (28), and finishing the test when the cycle period N reaches a set cycle period.
9. The method for testing the kinetics of the alloy hydrogen storage material according to the claim 8, characterized in that in the hydrogen charging process, hydrogen is adjusted to a proper pressure through a pressure reducing valve I (5), then enters a sample reaction tank (15) through a manual valve I (3), an electromagnetic valve I (7), a mass flow meter (8) and a tank opening valve (15 b), and the hydrogen is fully diffused through a gas guide pipe (15 g) and reacts with a hydrogen storage alloy sample (15 f) to generate hydride; in the hydrogen releasing process, hydrogen is released from the sample reaction tank (15) and is regulated to the required pressure through the pressure reducing valve II (19), and the output flow is accurately controlled through the mass flow controller (21).
10. The method of claim 9, wherein said alloying material (15 f) is LaNi5、ZrMn2、TiMn2、TiFe、Mg2Ni or vanadium based solid solutions in the form of powders, granules or blocks.
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