A performance test platform for solid-state hydrogen storage materials

Abstract

The present invention relates to a performance test platform for solid-state hydrogen storage materials, comprising a cabinet, a gas circuit system and a high-temperature test device; the high-temperature test device includes a tube furnace and a first sample chamber disposed inside the tube furnace. A through accommodation cavity is machined along the axis inside the first sample tube. The upper part of the accommodation cavity is a first accommodation portion, and the lower part is a second accommodation portion. A sample cup is disposed below the first accommodation portion, and there is no seal between the bottom of the sample cup and the second accommodation portion; the temperature sensor extends into the second accommodation portion from the lower side, and the end of the temperature sensor contacts the bottom of the sample cup. In the present invention, the sample cup is closer to the temperature sensor, and the temperature feedback during testing is more timely and accurate. The temperature sensor installation portion extends out of the tube furnace, and the lower end of the temperature sensor installation portion is sealingly connected to the temperature sensor through a high-temperature resistant rubber sealing ring. Since the temperature sensor installation portion is disposed outside the tube furnace, the high-temperature resistant rubber sealing ring is not easily damaged by high temperature, and the increase in test cost caused by using a disposable VCR gasket for sealing at the temperature sensor installation portion is avoided.

Description

Technical Field

[0001] The present invention belongs to the technical field of new energy, and particularly relates to a performance test platform for solid hydrogen storage materials. Background Art

[0002] Existing hydrogen storage technologies can be divided into three types. One is gaseous hydrogen storage technology, where hydrogen gas is compressed and stored in high-pressure containers; the second is liquid hydrogen storage technology, where hydrogen gas is liquefied at low temperature and high pressure and stored in adiabatic containers; the third is solid hydrogen storage technology, where hydrogen gas is combined with solid hydrogen storage materials physically or chemically. These three methods are widely used in different fields. Among them, solid hydrogen storage technology has its own unique advantages due to its good safety, miniaturization, and applicability in multiple scenarios. The key to solid hydrogen storage technology lies in the hydrogen storage capacity and service life of solid hydrogen storage materials. Engineers conduct performance tests on solid hydrogen storage materials with a large number of different compositions and ratios, and respectively select the solid hydrogen storage materials that perform best under different usage environments. Solid hydrogen storage material performance testing instruments are used in these performance tests.

[0003] Solid hydrogen storage material performance testing instruments are a type of gas-solid reaction testing equipment used to measure the gas cycle adsorption / desorption performance of metal materials. This testing equipment studies and evaluates the hydrogen adsorption and desorption performance of hydrogen storage materials under different conditions by changing pressure, composition, and temperature conditions. The PCT (pressure-concentration-temperature) test of this type of hydrogen storage material testing device usually adopts the hydrogen charging and discharging methods of ΔP or ΔC, corresponding to dynamic and static hydrogen charging and discharging methods respectively. Currently, automated testing can be achieved, which is used to measure the gas adsorption, thermodynamic performance, cycle performance, and phase composition of samples.

[0004] Currently, the test temperature of solid hydrogen storage material performance testing instruments is usually in the range of 0 to 600 °C. There is no test requirement or corresponding test means for the performance testing of solid hydrogen storage materials at lower temperatures. However, in fact, with the development of solid hydrogen storage material technology and the gradual popularization of hydrogen energy, in the relatively cold Northeast and Northwest regions of China in winter, as long as there are suitable low-temperature solid hydrogen storage materials, hydrogen energy may also be applicable in winter in these regions; therefore, it is necessary to propose an instrument that can test the performance of solid hydrogen storage materials at lower temperatures.

[0005] In addition, the sample chamber for holding hydrogen storage materials is a key component in the hydrogen absorption and desorption cycle life test of hydrogen storage materials; the temperature sensing device for temperature measurement generally requires to be placed close to the internal sample cup, and the temperature sensing device of the sample chamber is generally set at the bottom or side of the sample tube.

[0006] In a Chinese patent with the patent number 2022105344096 and the title "A Performance Testing Device and Method for Hydrogen Storage Materials", a performance testing device and method for hydrogen storage materials are disclosed, which relate to the technical field of performance testing of hydrogen storage materials. It includes a pressurization subsystem, a gas storage subsystem, an exhaust subsystem, and a main pipeline. A first installation valve, a fourth stop valve, and a third electric control valve are sequentially installed on the main pipeline. The gas storage subsystem, the evacuation subsystem, and the reaction subsystem are sequentially connected behind the third electric control valve, and the pressurization subsystem is connected in front of the first installation valve. Through this system, the calibration of the reaction chamber volume, the measurement of the leakage rate of the reaction chamber, the performance testing of hydrogen storage materials under different hydrogen purities, etc. can be completed. It is controlled by a computer, is convenient to operate, has complete measurement parameters, and has a relatively high accuracy, so as to better obtain the performance of hydrogen storage materials under different hydrogen charging purities. For the performance testing device of hydrogen storage materials disclosed in this patent, this type of structure is widely used in China at present, and its sample chamber is representative, that is, a blind hole is opened at the bottom of the sample tube, and the temperature sensor is placed in the blind hole. The disadvantage of this structure is that during testing, the conduction of temperature takes time, and the time for heat to conduct to the temperature sensor and the sample cup may be out of sync. When the high-temperature furnace is heating up, the temperature measured by the temperature sensor often tends to be slightly higher than the instantaneous temperature of the hydrogen storage material, which may lead to the deviation of the measurement curve.

[0007] In view of this, it is necessary to propose a performance testing platform for solid-state hydrogen storage materials that can test the performance of solid-state hydrogen storage materials at lower temperatures, has a temperature sensor closer to the hydrogen storage material, is more convenient to use, and can effectively control the cost. Summary of the Invention

[0008] The purpose of the present invention is to provide a performance testing platform for solid-state hydrogen storage materials that can test the performance of solid-state hydrogen storage materials in a low-temperature environment, has more accurate temperature feedback, and lower testing costs.

[0009] To solve the above technical problems, the present invention discloses a performance testing platform for solid-state hydrogen storage materials, which includes a cabinet body and a gas path system arranged in the cabinet body, and a high-temperature testing device arranged in the open space on one side of the cabinet body; the high-temperature testing device includes a tube furnace with a heating temperature of 0°C to 600°C and a first sample chamber arranged in the tube furnace. The first sample chamber is communicated with the gas path system. The first sample chamber includes a first sample tube, a gas guiding rod inserted into the first sample tube, and a sample cup. A through accommodation cavity is machined along the axis in the first sample tube. The upper part of the accommodation cavity is a first accommodation part for accommodating the gas guiding rod, and the lower part of the accommodation cavity is a second accommodation part for accommodating the temperature sensor. The diameter of the first accommodation part is larger than that of the second accommodation part; the diameter of the sample cup is larger than that of the second accommodation part but smaller than that of the first accommodation part. The sample cup is arranged below the first accommodation part, and there is no seal between the bottom of the sample cup and the second accommodation part;

[0010] The temperature sensor extends into the second accommodating part from the lower side, and the end of the temperature sensor is in contact with the bottom of the sample cup.

[0011] Preferably, it further includes a water bath pot arranged outside the cabinet body. A second sample chamber group communicated with the gas path system is arranged in the water bath pot, and the second sample chamber group includes a plurality of second sample chambers.

[0012] Preferably, the water bath pot uses liquid nitrogen, water or oil as a heat conduction medium to provide a low-temperature test environment of -140°C to room temperature or -30°C to 100°C.

[0013] Preferably, the second sample chamber group includes four second sample chambers. During the test, the same hydrogen storage material is placed in the second sample chamber group. The four second sample chambers are tested separately or simultaneously. In addition to performing PCT, hydrogen absorption and desorption kinetics performance, volume calibration, maximum hydrogen absorption capacity, and cycle life tests on the solid hydrogen storage material, it is also used to take out one second sample chamber at different temperatures to observe the change of the crystal image structure of the solid hydrogen storage material in different low-temperature environments.

[0014] Preferably, the diameter of the air guide rod is smaller than the diameter of the first accommodating part. There is a gap for hydrogen to flow between the air guide rod and the first accommodating part. Several groups of side air pipes arranged up and down are provided on the upper part of the air guide rod. A main air pipe is arranged in the air guide rod, and the main air pipe is communicated with the gap between the air guide rod and the first accommodating part through the side air pipes.

[0015] Preferably, an extended temperature sensor installation part is provided at the lower part of the sample tube, and the temperature sensor installation part extends out of the tube furnace from the lower side.

[0016] Preferably, the part of the bottom of the first accommodating part in contact with the bottom of the sample cup is processed into a rough surface, or provided with air guide grooves or protrusions, so that the residual gas in the second accommodating part can be smoothly discharged during exhaust.

[0017] Preferably, a threaded interface with a high-temperature resistant rubber sealing ring is provided at the lower end of the temperature sensor installation part, and the temperature sensor is hermetically connected to the temperature sensor installation part through the threaded interface.

[0018] Preferably, a cooling device is provided on the cabinet body below the tube furnace, and the cooling device is used to cool the temperature sensor installation part.

[0019] Preferably, the cooling device includes an air cooling pipe, and the air outlet of the air cooling pipe faces the temperature sensor installation part.

[0020] The performance test platform for the solid hydrogen storage material of the present invention has at least the following advantages:

[0021] (1) The temperature sensor installation part is extended and protrudes out of the tube furnace. The lower end of the temperature sensor installation part is hermetically connected to the temperature sensor through a high-temperature resistant rubber sealing ring. Since the temperature sensor installation part is located outside the tube furnace, the high temperature generated by the heating of the tube furnace is not easily conducted to the high-temperature resistant rubber sealing ring, making it difficult for the high-temperature resistant rubber sealing ring to be damaged by the high temperature generated by the tube furnace during testing. Therefore, the high-temperature resistant rubber sealing ring can be reused, avoiding the increase in testing costs caused by using disposable VCR gaskets for sealing at the temperature sensor installation part, which is beneficial to controlling testing costs.

[0022] (2) By setting up a cooling device, the temperature of the temperature sensor installation part is ensured to be controlled within a safe range, further ensuring the safety of the high-temperature resistant rubber sealing ring.

[0023] (3) The accommodation cavity is provided in a through manner, and the first accommodation part and the second accommodation part are connected and communicated, enabling the temperature sensor to be placed from the lower part and come into contact with the sample cup. There is only one sample cup bottom between the solid-state hydrogen storage material and the temperature sensor, so that the temperature sensor can more timely and accurately sense the temperature of the solid-state hydrogen storage material, making the experimental data more accurate.

[0024] (4) Occasionally, the sample cup in the conventional sample chamber will be stuck by the sample tube and be difficult to take out, causing trouble for cleaning the sample tube. However, in the present invention, since the first accommodation part and the second accommodation part are connected and communicated, when cleaning the sample chamber, if the sample cup is stuck by the inner wall of the sample tube, a rigid rod can be inserted from the lower second accommodation part and pushed slightly to push out the sample cup, which well solves such troubles. Description of the Drawings

[0025] Figure 1 It is a schematic structural diagram of a performance test platform for a solid-state hydrogen storage material.

[0026] Figure 2 It is Figure 1 The schematic structural diagram of the performance test platform for the solid-state hydrogen storage material from another perspective (the upper cover is hidden).

[0027] Figure 3 It is a schematic structural diagram of a first sample chamber.

[0028] Figure 4 It is Figure 3 The A-direction sectional view of the first sample chamber in

[0029] Figure 5 It is a schematic structural diagram of a water bath (in a top view position).

[0030] The reference numerals in the figure are: 1 - cabinet body, 2 - gas circuit system, 3 - high-temperature test device, 4 - tube furnace, 5 - first sample chamber, 510 - first sample tube, 520 - gas guide rod, 521 - side ventilation pipe, 522 - main ventilation pipe, 530 - sample cup, 540 - accommodation cavity, 541 - first accommodation part, 542 - second accommodation part, 550 - temperature sensor installation part, 560 - part where the bottom of the first accommodation part contacts the bottom of the sample cup, 561 - threaded interface, 562 - high-temperature resistant rubber sealing ring, 6 - temperature sensor, 7 - water bath, 710 - notch. Detailed implementation mode

[0031] The present invention will be further described in detail below through embodiments, so that those skilled in the art can implement it with reference to the text of the specification.

[0032] It should be understood that the terms such as "having", "comprising" and "including" used herein do not exclude the presence or addition of one or more other elements or their combinations.

[0033] As Figure 1-2 shown, a performance test platform for solid hydrogen storage materials includes a cabinet body 1 and a gas circuit system 2 arranged in the cabinet body, and a high-temperature test device 3 arranged in the open space on one side of the cabinet body; the high-temperature test device includes a tube furnace 4 with a heating temperature of 0°C to 600°C and a first sample chamber 5 arranged in the tube furnace, and the first sample chamber is communicated with the gas circuit system. In this embodiment, the gas circuit system is composed of a hydrogen pipeline, a purging pipeline, a venting pipeline, a vacuum pumping pipeline, a heat dissipation copper pipe and various manual diaphragm valves, and manual diaphragm valves are used for connecting each pipeline part to the gas source / atmosphere. Among them, the hydrogen pipeline uses 99.999% high-purity hydrogen with a pressure of 0 to 10 MPa, and is equipped with a manual valve, a filter, a pressure regulating valve, a pressure gauge and a one-way angle seat valve at the front end. The purging gas uses nitrogen with a pressure of 0.4 to 0.6 MPa, and is equipped with a manual valve, a filter, a pressure regulating valve, a pressure gauge and a one-way angle seat valve at the front end. The lower limit pressure of the venting pipeline is 0.2 to 0.3 MPa. While protecting the normal operation of the vacuum pump, the lower limit pressure shall not be lower than 0.2 MPa to avoid air backflow into the gas circuit under negative pressure, causing accidents. At the same time, a check valve or a flame arrester valve is installed at the end of the venting pipeline. The tube furnace is a tube resistance furnace with a heating power of 1 kW, a heating rate of 20°C / min, and a heating range of 0 to 600°C. The outer shell is made of cold-rolled carbon structural steel, and the furnace lining material is silicon carbide, which has high-temperature resistance and good thermal conductivity. The middle part is insulated with alumina polycrystalline fiber material, and the melting point is 1840°C.

[0034] As Figure 3-4As shown in the figure, the first sample chamber includes a first sample tube 510, a gas guiding rod 520 and a sample cup 530 inserted into the first sample tube. A through accommodating cavity 540 is machined along the axis inside the first sample tube. The upper part of the accommodating cavity is a first accommodating part 541 for accommodating the gas guiding rod, and the lower part of the accommodating cavity is a second accommodating part 542 for accommodating the temperature sensor. The diameter of the first accommodating part is larger than that of the second accommodating part; the diameter of the sample cup is larger than that of the second accommodating part but smaller than that of the first accommodating part. The sample cup is arranged below the first accommodating part, and there is no seal between the bottom of the sample cup and the second accommodating part, that is, the gas remaining in the second accommodating part during exhaust can be discharged from between the bottom of the sample cup and the second accommodating part; when cleaning the sample chamber, if the sample cup is stuck by the inner wall of the sample tube and is difficult to take out, a rigid rod is inserted into the second accommodating part from the lower side to push out the sample cup.

[0035] The temperature sensor 6 extends into the second accommodating part from the lower side, and the end of the temperature sensor contacts the bottom of the sample cup.

[0036] As Figure 5 As shown in the figure, it further includes a water bath 7 arranged outside the cabinet. A second sample chamber group communicated with the gas path system is arranged in the water bath. The second sample chamber group includes four second sample chambers. The second sample chamber can adopt a conventional sample chamber or a sample chamber with the same structure as the first sample chamber. Four notches 710 for clamping and fixing the second sample chamber are machined on the lid of the water bath; during the test, the same hydrogen storage material is placed in the second sample chamber group, and the four second sample chambers are tested separately or simultaneously. In addition to performing PCT, hydrogen absorption and desorption kinetics performance, volume calibration, maximum hydrogen absorption amount, and cycle life tests on solid hydrogen storage materials, it is also used to take out a second sample chamber at different temperatures to observe the change of the crystal image structure of the solid hydrogen storage material in different low-temperature environments. For example, when observing the change of the crystal image structure of the solid hydrogen storage material in different low-temperature environments, the temperature is increased in a gradient of 10°C, and it is maintained at -30°C, -20°C, -10°C, and 0°C for a certain time and pressure respectively. One sample chamber is taken out at each temperature, and a high-magnification microscope is used to view the change of the crystal image structure of the sample. By analyzing the change of the crystal structure of the solid hydrogen storage material in a low-temperature environment, corresponding strategies for the optimization of the ratio, storage, hydrogen charging and discharging, and safety of the solid hydrogen storage material in a low-temperature environment are formulated.

[0037] Further, the water bath can use liquid nitrogen, water or oil as the heat conduction medium to provide a low-temperature test environment of -140°C to room temperature or -30°C to 100°C. In this embodiment, the water bath is a commercially available product, with a temperature control range of room temperature to 100°C (ice cubes can be added when lower temperatures are required), an accuracy of ±0.1°C, a constant temperature fluctuation of ≤±0.5°C, a constant temperature uniformity of ≤±1°C, and a heating rate of 2°C / min. Using liquid nitrogen as the heat conduction medium can obtain very low test temperatures, but currently, the research on solid hydrogen storage materials below -30°C only has scientific research significance and not much practical value. For the performance testing of solid hydrogen storage materials oriented towards practical applications, water is mostly used as the heat conduction medium, and the temperature is controlled at -30°C to 100°C. For example, near 25°C and under a pressure of about 3 MPa, the hydrogen absorption capacity of the AB5 material is about 1.4 wt%, that is, 100 grams of alloy material can adsorb 1.4 grams of hydrogen. However, if this material is at -15°C, its hydrogen absorption capacity will drop significantly. It can be seen that the development of solid hydrogen storage materials suitable for low temperatures is still in its infancy and is very difficult, requiring a large number of tests.

[0038] The diameter of the gas guide rod is smaller than the diameter of the first accommodating part. There is a gap for hydrogen to flow between the gas guide rod and the first accommodating part. Several groups of side ventilation pipes 521 arranged vertically are provided on the upper part of the gas guide rod. A main ventilation pipe 522 is provided inside the gas guide rod, and the main ventilation pipe is connected to the gap between the gas guide rod and the first accommodating part through the side ventilation pipes.

[0039] An extended temperature sensor installation part 550 is provided at the lower part of the sample tube, and the temperature sensor installation part extends out of the tube furnace from the lower side.

[0040] The part 560 where the bottom of the first accommodating part contacts the bottom of the sample cup is processed into a rough surface, so that the residual gas in the second accommodating part can be smoothly discharged during exhaust, and the dust overflowing from the sample cup during testing will not enter the second accommodating part.

[0041] The lower end of the temperature sensor installation part is provided with a threaded interface 561 with a high-temperature resistant rubber sealing ring 562. The temperature sensor is hermetically connected to the temperature sensor installation part through the threaded interface. It is advisable that the high-temperature resistant rubber sealing ring be made of rubber material resistant to temperatures above 200°C. In the invention patent named "A Sample Chamber for Hydrogen Charging and Discharging Tests of Solid Hydrogen Storage Materials" proposed by our company, it is disclosed that a first accommodating part and a second accommodating part are connected in communication, enabling the temperature sensor to be inserted from the lower part and contact the sample cup. At the joint (compression nut) and the connection between the sample cup and the bottom of the first accommodating part, a VCR sealing gasket needs to be placed at each position. In this way, the cost of two VCR sealing gaskets for one test is 20 yuan (the cost of a single VCR sealing gasket is about 10 yuan, for one-time use). If the use of VCR sealing gaskets can be reduced, the cost savings for a large number of tests will be quite substantial. In this embodiment, by setting an external thread at the lower end of the temperature sensor installation part, placing a cap-shaped high-temperature resistant rubber sealing ring inside the mouth of the temperature sensor installation part, and setting a nut at the lower end of the temperature sensor, tightening the nut on the temperature sensor installation part can achieve a sealed connection. In this way, there is no need to set a VCR sealing gasket at the connection between the sample cup and the bottom of the first accommodating part, reducing the test cost.

[0042] In addition, there are also many other ways to hermetically connect the lower end of the temperature sensor installation part and the temperature sensor. For example, an internal threaded hole is set at the lower end of the installation part, a high-temperature resistant rubber sealing ring is set at the top of the internal threaded hole, a bolt is hermetically welded to the lower part of the temperature sensor, and the bolt can be installed in the internal threaded hole to achieve a sealed connection; the setting method of the high-temperature rubber sealing ring is not limited to the specific details and the embodiments shown and described here.

[0043] Furthermore, a cooling device is provided on the cabinet below the tube furnace, and the cooling device is used to cool down the temperature sensor installation part. The longer the temperature sensor installation part, the less heat is transferred to the high-temperature resistant rubber sealing ring. However, if due to reasons such as space and temperature sensor size limitations, the temperature sensor installation part cannot be set to be longer, the cooling device can be turned on to cool down the temperature sensor installation part when the heating temperature of the tube furnace is relatively high to protect the high-temperature resistant rubber sealing ring. In this embodiment, the cooling device includes an air-cooling pipe, and the air outlet of the air-cooling pipe faces the temperature sensor installation part.

[0044] Although the embodiments of the present invention have been disclosed as above, it is not limited to only the applications listed in the specification and embodiments. It can be fully applied to various fields suitable for the present invention. For those familiar with the field, additional modifications can be easily made. Therefore, without departing from the general concept defined by the claims and the equivalent scope, the present invention is not limited to the specific details and the embodiments shown and described here.

Claims

1. A solid-state hydrogen storage material performance testing platform, characterized in that: It comprises a cabinet and a gas circuit system arranged in the cabinet, and a high-temperature testing device arranged in an open space on one side of the cabinet; the high-temperature testing device comprises a tubular furnace with a heating temperature of 0°C to 600°C and a first sample chamber arranged in the tubular furnace, the first sample chamber is connected to the gas circuit system, the first sample chamber comprises a first sample tube and a gas guide rod and a sample cup inserted into the first sample tube, a through accommodating cavity is processed along the axis in the first sample tube, the upper part of the accommodating cavity is a first accommodating part for accommodating the gas guide rod, the lower part of the accommodating cavity is a second accommodating part for accommodating a temperature sensor, and the diameter of the first accommodating part is larger than that of the second accommodating part; the diameter of the sample cup is larger than that of the second accommodating part but smaller than that of the first accommodating part, the sample cup is arranged at the lower part of the first accommodating part, and the bottom of the sample cup is not sealed from the second accommodating part; The temperature sensor extends into the second accommodating portion from the lower side, and the end of the temperature sensor contacts the bottom of the sample cup; The diameter of the gas guide rod is smaller than the diameter of the first accommodating portion, and there is a gap between the gas guide rod and the first accommodating portion for hydrogen flow. The upper part of the gas guide rod is provided with a plurality of groups of side ventilation pipes arranged vertically, and a main ventilation pipe is provided inside the gas guide rod, and the main ventilation pipe is connected with the gap between the gas guide rod and the first accommodating portion through the side ventilation pipe; An extended temperature sensor installation portion is provided at the lower part of the sample tube, and the temperature sensor installation portion extends from the lower side of the tube furnace; A threaded interface with a high-temperature resistant rubber sealing ring is provided at the lower end of the temperature sensor mounting portion, and the temperature sensor is sealed and connected to the temperature sensor mounting portion via the threaded interface; A cooling device is provided on the cabinet below the tube furnace, and the cooling device is used to cool down the temperature sensor installation part; The portion of the bottom of the first accommodating portion that contacts the bottom of the sample cup is processed into a rough surface, so that the residual gas in the second accommodating portion can be discharged smoothly during exhaust.

2. The solid-state hydrogen storage material performance testing platform according to claim 1, characterized in that: It also includes a water bath pot arranged outside the cabinet, in which a second sample chamber group connected with the gas path system is arranged, and the second sample chamber group includes a plurality of second sample chambers.

3. The solid-state hydrogen storage material performance testing platform according to claim 2, characterized in that: The water bath uses liquid nitrogen, water or oil as heat conduction medium.

4. The solid-state hydrogen storage material performance testing platform according to claim 3, characterized in that: The second sample chamber group includes four second sample chambers. During testing, the same hydrogen storage material is placed in the second sample chamber group, and the four second sample chambers are tested separately or simultaneously. In addition to conducting PCT, hydrogen absorption and desorption kinetics, volume calibration, maximum hydrogen absorption capacity, and cycle life tests on solid-state hydrogen storage materials, they are also used to take out a second sample chamber at different temperatures to observe the changes in the crystal structure of the solid-state hydrogen storage material under different low-temperature environments.

5. The solid-state hydrogen storage material performance testing platform according to claim 1, characterized in that: The cooling device comprises an air cooling pipe, and an air outlet of the air cooling pipe faces the temperature sensor installation part.

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