A hydrogen storage reactor for increasing the contact area of hydrogen storage material with hydrogen

Abstract

The present application belongs to the hydrogen energy utilization technology field in the clean energy and new energy field, and relates to a hydrogen storage reactor for increasing the contact area between hydrogen storage material and hydrogen, which comprises a reactor main body and a screen assembly, the screen assembly is arranged in the reactor main body, the screen assembly comprises an upper screen, a lower screen and a weighted fixing piece, the upper screen and the lower screen are fixed through the weighted fixing piece, and the upper screen, the lower screen and the weighted fixing piece form a hydrogen storage material sample powder particle reaction space. The reactor adopts the screen assembly to realize convenient sample loading, simple operation, non-blowing, zero sample loss and zero accumulation. The reactor is designed to be through from top to bottom, so that the powder sample particles are contacted with hydrogen in all directions, the reaction with hydrogen is fully realized, hydrogen can quickly enter the interstitial space of the alloy lattice, the hydrogen absorption speed is improved, and the hydrogen storage kinetic performance is improved. At the same time, the error experiment error is minimized, and the data accuracy is improved.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of hydrogen energy utilization technology in the field of clean energy and new energy, and specifically relates to an energy optimization utilization technology with hydrogen energy storage as the core, and relates to a hydrogen storage reactor for increasing the contact area between hydrogen storage material and hydrogen. BACKGROUND

[0002] Energy is the basis for the survival and development of modern society, and the supply capacity of energy is closely related to the sustainable development of the national economy and is one of the strategic foundations of national security. Due to the rapid economic development, traditional non-renewable fossil fuels and other energy sources are becoming increasingly scarce, and governments around the world are pinning their hopes on emerging energy sources such as hydrogen energy, solar energy, and wind energy. Hydrogen energy, as a green energy source with abundant reserves, a wide range of sources, and high energy density, is attracting widespread attention. The key factor to solve the problem of energy crisis anxiety is to vigorously develop and utilize hydrogen energy. Hydrogen energy utilization needs to solve the following three problems: hydrogen production, storage and transportation, and hydrogen energy storage and transportation are the key to hydrogen energy application. At present, hydrogen storage methods can be divided into three categories: high-pressure gaseous hydrogen storage, low-temperature liquid hydrogen storage, and solid hydrogen storage. High-pressure gaseous hydrogen storage compresses hydrogen into high-density gas by high pressure and stores it in a storage tank. Although the charging and discharging process can be completed at room temperature, the hydrogen storage density is greatly affected by the pressure and the material of the storage tank, and the risk coefficient is too high. The hydrogen storage density of low-temperature liquid hydrogen storage is 845 times that of high-pressure gaseous hydrogen storage, but this method has high cost and poor safety performance, and is not suitable for large-scale use. Solid-state hydrogen storage can be divided into activated carbon adsorption hydrogen storage, metal hydrogen storage, and carbon nanotube hydrogen storage.

[0003] Since the late 1960s, metal hydrogen storage LaNi5, TiFe, Mg2Ni and other types have been discovered by researchers, and hydrogen storage alloys have developed rapidly. Compared with high-pressure hydrogen storage and low-temperature liquid hydrogen storage, solid hydrogen storage has the highest safety performance and is more suitable for mass production. Hydrogen storage alloys with good hydrogen storage performance and wide application range have been continuously developed. High-entropy hydrogen storage alloy has become a research hotspot in the field of hydrogen storage alloy due to its good hydrogen storage performance.

[0004] For the study of hydrogen storage performance of hydrogen storage alloy, many types of PCT hydrogen storage performance testers have been designed and produced in China. The reactor is a crucial component of the PCT hydrogen storage performance tester. The traditional reactor sample placement part has a narrow channel, and the powder sample will accumulate at the channel. When hydrogen is introduced, the contact area between the sample and the hydrogen is small, which leads to incomplete reaction of the sample with the hydrogen and large errors. SUMMARY

[0005] OBJECTIVE

[0006] The application aims to provide a hydrogen storage reactor which increases the contact area of hydrogen storage material and hydrogen, and through comparison of the hydrogen storage performance of the reactor in the application and a conventional reactor using TiVZrNb high-entropy alloy hydrogen storage material, it is found that the TiVZrNb high-entropy alloy hydrogen storage material used in the reactor of the application has a larger hydrogen absorption capacity and better kinetic performance.

[0007] To achieve the above-mentioned purpose, the application provides the following technical scheme.

[0008] The hydrogen storage reactor which increases the contact area of hydrogen storage material and hydrogen comprises a reactor main body and a screen assembly, the screen assembly is arranged in the reactor main body, the screen assembly comprises an upper screen, a lower screen and a weighted fixing piece,

[0009] The upper screen and the lower screen are fixed together through the weighted fixing piece, and the upper screen, the lower screen and the weighted fixing piece enclose a hydrogen storage material sample powder particle reaction space.

[0010] In one of the embodiments, the reactor main body has a sample reaction part at the upper part and a gas inlet part at the lower part, the sample reaction part has an installation table arranged in the circumferential direction, and the screen assembly is fixed on the installation table; the inner diameter of the gas inlet part is smaller than that of the sample reaction part, and the cross section of the gas inlet part is conical.

[0011] In one of the embodiments, the hydrogen storage reactor further comprises hydrogen storage material sample powder particles, the hydrogen storage material sample powder particles are arranged in the hydrogen storage material sample powder particle reaction space, and the particle size of the hydrogen storage material sample powder particles is 170-200 mesh, and the pore size of the upper screen and the lower screen is selected to be 450-550 mesh.

[0012] In one of the embodiments, the lower screen is fixedly arranged at the bottom of the weighted fixing piece, the upper screen is arranged at the top of the weighted fixing piece, the upper screen has a fixing piece connecting section and an opening section, the fixing piece connecting section is fixedly arranged at the top of the weighted fixing piece in the circumferential direction, and the opening section is fixedly arranged at the top of the weighted fixing piece through a connecting fastener; and the weighted fixing piece is placed on the installation table of the sample reaction part.

[0013] In one of the embodiments, the diameter of the upper screen is the same as that of the screen, the net distance between the upper screen and the lower screen is 0.2-0.5 cm, and an upper annular clamping groove with an upward opening is further arranged on the inner wall of the sample reaction part, the upper edge frame of the weighted fixing piece is in abutment with the annular boss, the top of the upper edge frame is outwardly extended in the circumferential direction and then downwardly bent, and the upper edge frame is clamped with the upper annular clamping groove.

[0014] A method for preparing hydrogen storage material sample powder particles using the above-mentioned hydrogen storage reactor for increasing the contact area between hydrogen storage material and hydrogen, comprising the following steps:

[0015] Step one: prepare high-purity raw materials Ti, V, Zr and Nb particles, Ti x V y Zr z Nb m The high-entropy alloy hydrogen storage material is prepared by weighing the raw materials according to the atomic percentage, and the main elements of the alloy are Ti 28%-33%, V 27%-28%, Zr 5%-10%, and Fe 30%-40%;

[0016] Step two: put the raw materials in step one into the copper crucible of the non-consumable vacuum arc melting furnace according to the proportion, and after vacuumizing, fill in argon for protection melting, get the button ingot, repeat the turning and repeat the melting, and cool to get the non-equal molar ratio Ti x V y Zr z Nb m High-entropy alloy button ingot;

[0017] Step three: mechanically crush the non-equal molar ratio Ti x V y Zr z Nb m High-entropy alloy obtained by melting, and filter the hydrogen storage material sample powder particles after crushing with a 100-mesh sieve;

[0018] Step four: put the filtered hydrogen storage material sample powder particles obtained in step three into a stainless steel ball mill jar, mix the stainless steel ball milling beads and the hydrogen storage material sample powder particles according to the mass ratio of 12-15:1, and ball mill in the ball mill at a speed of 250 rad / min, the ball milling time is 20-30 min;

[0019] Step five: filter the hydrogen storage material sample powder particles into a 200-mesh sieve, and uniformly put them into the hydrogen storage material sample powder particle reaction space, then clamp the sieve assembly on the upper annular clamping groove for fixation, and connect the PCT hydrogen storage tester;

[0020] Step six: vacuumize the PCT hydrogen storage tester, and then introduce hydrogen after stabilization;

[0021] Step seven: heating the hydrogen storage reactor to a first predetermined temperature and keeping the temperature; then filling the PCT hydrogen storage tester with hydrogen, so that the hydrogen storage material sample powder particles fully absorb hydrogen, discharging the hydrogen in the PCT hydrogen storage tester after vacuumizing, then heating the hydrogen storage reactor to a specific temperature to completely release hydrogen, and repeating the cycle; Step eight: heating the hydrogen storage reactor to a first temperature threshold and keeping the temperature, then filling the hydrogen to make the hydrogen storage material sample powder particles fully absorb hydrogen, then discharging the hydrogen in the PCT hydrogen storage tester after vacuumizing, and heating the reactor to a second temperature threshold to completely release hydrogen;

[0022] The temperature of the hydrogen storage reactor is adjusted to a third temperature threshold and kept for a period of time, and then hydrogen is introduced to make the hydrogen storage material sample powder particles fully absorb hydrogen.

[0023] In one of the embodiments, the vacuum degree in step two is -0.101 MPa, the hydrogen pressure in step two is 1 MPa, and the stabilization time in step two is 10-20 min.

[0024] In one of the embodiments, the first predetermined temperature in step three is 300℃, and the temperature is kept at the first predetermined temperature for 1.5-2 hours, the hydrogen pressure filled in the PCT hydrogen storage tester in step three is 3 MPa; the hydrogen pressure introduced after the temperature of the hydrogen storage reactor is adjusted to the third temperature threshold and kept for a period of time is 3 MPa; the specific temperature in step three is 400℃, and the number of repeated cycles in step three is 4.

[0025] In one of the embodiments, the first temperature threshold in step eight is 150℃, the temperature is kept at the first temperature threshold for 1h-1.5h, the hydrogen pressure introduced in step eight is 3 MPa, the second temperature threshold in step eight is 400℃, the third temperature threshold in step eight is 250℃, and the temperature is kept at the third temperature threshold for 0.8h-1.2h.

[0026] Advantages and effects

[0027] The screen assembly is adopted in the reactor to realize convenient sample loading, simple operation, non-blowing, zero loss and zero accumulation of the sample. The up-down through design of the reactor enables the hydrogen storage material sample powder particles to be contacted with hydrogen from all directions, realizes sufficient reaction with hydrogen, enables hydrogen to quickly enter the interstitial space of the alloy lattice, improves the hydrogen absorption speed and the hydrogen storage kinetic performance, and at the same time, minimizes the experimental error and improves the accuracy of the data. BRIEF DESCRIPTION OF DRAWINGS

[0028] Figure 1This is a cross-sectional view of a hydrogen storage reactor according to an embodiment of the present invention, which increases the contact area between the hydrogen storage material and hydrogen.

[0029] Figure 2 for Figure 1 3D view of the middle screen assembly;

[0030] Figure 3 for Figure 1 Top view of the sample after it has been loaded onto the middle and lower sieves;

[0031] Figure 4 for Figure 1 Schematic diagram of the structure for fixing the middle screen assembly;

[0032] Figure 5 For Ti 0.280 V 0.270 Zr 0.005 Nb 0.400 Organizational chart;

[0033] Figure 6 For Ti 0.305 V 0.275 Zr 0.100 Nb 0.320 Organizational chart;

[0034] Figure 7 For Ti 0.280 V 0.270 Zr 0.005 Nb 0.400 The graph after activation;

[0035] Figure 8 For Ti 0.305 V 0.275 Zr 0.100 Nb 0.320 The graph after activation;

[0036] Figure 9 This is a comparison graph showing the performance of Example 1 and Comparative Example 1 at 150°C and 250°C.

[0037] Figure 10 The graph shows a performance comparison between Example 2 and Comparative Example 2 at 150℃ and 250℃.

[0038] Explanation of reference numerals in the attached drawings: 1. External thread of the reactor; 2. Reactor body; 201. Mounting platform; 202. Upper annular groove; 3. Upper screen; 4. Weighted fixing component; 5. Lower screen; 6. Bottom of the inner wall of the reactor; 7. Hydrogen storage material sample powder particles. Detailed Implementation

[0039] The technical solution of the present invention will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments.

[0040] In order to more clearly illustrate the technical solutions in the specific embodiments of the present application or the prior art, the accompanying drawings required to be used in the specific embodiments or prior art description will be briefly introduced as follows. Obviously, the accompanying drawings in the following description are some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without any creative effort on the basis of these drawings.

[0041] The components of the embodiments of the present application described and shown in the accompanying drawings herein can be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of the present application provided in the accompanying drawings is not intended to limit the scope of the claimed present application, but only represents selected embodiments of the present application.

[0042] As shown in Figure 1 A hydrogen storage reactor for increasing the contact area of hydrogen storage material with hydrogen gas, comprising a reactor body 2 and a screen assembly, wherein the screen assembly is arranged in the reactor body 2, the screen assembly comprising an upper screen 3, a lower screen 5 and a weighted fixing piece 4,

[0043] The upper screen 3 and the lower screen 5 are fixed together by the weighted fixing piece 4, and the upper screen 3, the lower screen 5 and the weighted fixing piece 4 enclose a hydrogen storage material sample powder particle reaction space. The hydrogen storage reactor of the present application uses the cooperation of the basic upper screen 3, the lower screen 5 and the weighted fixing piece 4 to realize convenient sample loading, simple operation, non-blowing, zero sample loss and zero accumulation. The reactor is designed to be through from top to bottom, so that the hydrogen storage material sample powder particles 7 are in full contact with hydrogen gas, realizing sufficient reaction with hydrogen gas, enabling hydrogen gas to quickly enter the interstitial space of the alloy lattice, improving the hydrogen absorption speed and improving the hydrogen storage kinetics; at the same time, the experimental error is minimized, the accuracy of the data is improved, and the experimental error is minimized.

[0044] The reactor body 2 of the embodiment of the present application has an upper sample reaction part and a lower gas inlet part, the sample reaction part has a mounting table 201, and the screen assembly is fixed on the mounting table 201; the inner diameter of the gas inlet part is smaller than the inner diameter of the sample reaction part, and the cross section of the gas inlet part is conical.

[0045] The hydrogen storage reactor of the embodiment of the present application further comprises hydrogen storage material sample powder particles 7, which are arranged in the hydrogen storage material sample powder particle reaction space, and the particle size of the hydrogen storage material sample powder particles 7 is 170-200 mesh, and the pore size of the upper screen 3 and the lower screen 5 is selected to be 450-550 mesh.

[0046] The lower sieve screen 5 of the embodiment of the present application is fixedly arranged at the bottom of the weight fixing member 4, the upper sieve screen 3 is arranged at the top of the weight fixing member 4, the upper sieve screen 3 has a fixing member connecting section and an opening section, the fixing member connecting section is fixedly arranged at the top of the weight fixing member 4 in a circumferential direction, and the opening section is fixedly arranged at the top of the weight fixing member 4 through a connecting fastener; and the weight fixing member 4 is placed on the mounting table 201 of the sample reaction part.

[0047] The diameter of the upper sieve screen 3 is the same as that of the sieve screen 9, the clear distance between the upper sieve screen 3 and the lower sieve screen 5 is 0.2cm-0.5cm, an upper annular clamping groove 202 with an upward opening is further arranged on the inner wall of the sample reaction part, the upper edge frame of the weight fixing member 4 is in abutment with the annular boss, the top of the upper edge frame is outwardly extended in a circumferential direction and then downwardly bent, and the upper edge frame is in clamping connection with the upper annular clamping groove 202.

[0048] The upper sieve screen 3, the lower sieve screen 5 and the weight fixing member 4 are integrated, the weight fixing member 4 is a cylindrical side wall, and the weight fixing member 4 can firmly fix the sample container in the reactor and prevent the sample container from shaking due to its large weight. In addition, the diameter of the sample container is larger than the upper diameter of the reactor area 6. Therefore, the sample container can be stably fixed above the reactor area 6.

[0049] A method for preparing sample powder particles of a hydrogen storage material using the hydrogen storage reactor for increasing the contact area between the hydrogen storage material and hydrogen gas, the method comprising the following steps:

[0050] Step one: prepare high-purity raw material Ti, V, Zr and Nb particles, Ti x V y Zr z Nb m The high-entropy alloy hydrogen storage material is prepared by weighing the raw materials according to the atomic percentage, and the main elements of the alloy are Ti 28%-33%, V 27%-28%, Zr 5%-10%, and Fe 30%-40%;

[0051] Step two: put the raw materials in step one into a copper crucible of a non-consumable vacuum arc melting furnace according to the proportioning, and then perform protection melting after vacuumizing and filling with argon, repeatedly turn over the button ingot and repeatedly melt, and cool to obtain a non-equi-molar ratio Ti x V y Zr z Nb m high-entropy alloy button ingot;

[0052] In the vacuum melting in step two, the vacuum degree is 1×10 -3 Pa-4×10 -3 Pa, the furnace gas pressure is 0.03MPa-0.1MPa, and the pressure maintaining gas is high-purity argon;

[0053] In the vacuum smelting in step two, the electric current of the electric arc furnace is 100A-550A, and the time is 1min-5min; the cooling circulating water flow rate is 1m / s-5m / s; in step two, the turning of the button ingot is operated by the mechanical hand of the furnace, the initial smelted alloy ingot is turned over, and then smelted again, and the smelting state is maintained for 10s-50s, and the number of times of smelting is 5-10 times;

[0054] Step three: non-equi-molar ratio Ti x V y Zr z Nb m The high-entropy alloy is mechanically crushed, and the crushed hydrogen storage material sample powder particles 7 are filtered by using a 100-mesh sieve;

[0055] Step four: the filtered hydrogen storage material sample powder particles 7 obtained in step three are placed in a stainless steel ball mill jar, stainless steel ball milling beads and hydrogen storage material sample powder particles 7 are mixed in a mass ratio of 12-15:1, and ball milling is carried out in a ball mill at a speed of 250rad / min, and the ball milling time is 20-30min;

[0056] Step five: the hydrogen storage material sample powder particles 7 are poured into a 200-mesh sieve, uniformly placed in the hydrogen storage material sample powder particle reaction space, and then the sieve assembly is clamped on the upper annular clamping groove 202 for fixation, and connected with the PCT hydrogen storage tester;

[0057] Step six: the PCT hydrogen storage tester is vacuumed, and then hydrogen is introduced after stabilization;

[0058] Step seven: the hydrogen storage reactor is heated to a first predetermined temperature and kept at the temperature; then hydrogen is filled into the PCT hydrogen storage tester, so that the hydrogen storage material sample powder particles 7 fully absorb hydrogen, the hydrogen in the PCT hydrogen storage tester is discharged, and then vacuumized, and then the hydrogen storage reactor is heated to a specific temperature to completely release hydrogen, and the cycle is repeated.

[0059] The temperature of the hydrogen storage reactor is adjusted to a third temperature threshold and kept for a period of time, the hydrogen storage material sample powder particles 7 are uniformly heated for a period of time to reach a uniform constant temperature, hydrogen is introduced, and the hydrogen storage material sample powder particles 7 can fully absorb hydrogen.

[0060] The vacuum degree in the step six is -0.101 MPa, the hydrogen pressure in the step six is 1 MPa, and the stabilization time in the step six is 10-20 min. The operation can prevent the measurement error caused by the loose connection of the reactor interface, and the leakage during the measurement can be prevented by the leakage treatment in the step.

[0061] The first predetermined temperature in the step seven is 300℃, and the holding time at the first predetermined temperature is 1.5-2 hours. The hydrogen pressure of the PCT hydrogen storage tester in the step seven is 3 MPa. The hydrogen pressure after the hydrogen storage reactor is heated to the third temperature threshold and held for a period of time is 3 MPa. The specific temperature in the step seven is 400℃, and the number of repeated cycles in the step seven is 4. The operation can make the hydrogen storage material sample powder particles 7 uniformly heated at the first predetermined temperature of 300℃, and fully absorb hydrogen in the 3 MPa hydrogen environment, and fully release hydrogen at the high temperature of 400℃. After 4 times of such hydrogen absorption and release cycles, the hydrogen storage material sample powder particles 7 are completely activated.

[0062] The first temperature threshold in the step eight is 150℃, the holding time after heating to the first temperature threshold is 1h, the hydrogen pressure of the hydrogen gas in the step eight is 3 MPa, the second temperature threshold in the step eight is 400℃, the third temperature threshold in the step eight is 250℃, and the holding time after heating to the third temperature threshold is 0.8h-1.2h. The eighth step is a hydrogen storage performance test, which tests the hydrogen storage performance at 150℃. The hydrogen storage material sample powder particles 7 are uniformly heated at 150℃ for 1h, then a 3 MPa hydrogen environment is introduced to make them fully absorb hydrogen, and the hydrogen absorption amount is recorded. In order to facilitate the test of hydrogen absorption capacity at another temperature, the hydrogen absorbed at 150℃ needs to be released at a high temperature of 400℃.

[0063] Example 1

[0064] Ti 0.280 V 0.270 Zr 0.005 Nb 0.400 The method for storing hydrogen by using the reactor of the application comprises the following steps:

[0065] Step one: prepare high-purity raw materials Ti, V, Zr and Nb particles, according to Ti 0.280 V 0.270 Zr 0.005 Nb 0.400 The alloy composition design is to weigh the matching mass of the above raw materials according to the atomic percentage.

[0066] In the step one, the metal raw materials are prepared according to the following raw materials in atomic percentage:

[0067] Ti is 28%, V is 27%, Zr is 5%, and Fe is 40%,

[0068] Step two: the raw materials in step one are put into the copper crucible of the non-consumable vacuum arc furnace in sequence according to the proportion, vacuum is extracted, and then argon is filled for protection melting, the button ingot is obtained, and the surface is repeated and repeatedly melted for multiple times, after the multiple melting process is completed, the non-equal molar ratio Ti 0.280 V 0.270 Zr 0.005 Nb 0.400 High-entropy alloy button ingot

[0069] In step two, the vacuum degree is 4*10 -3 Pa, the furnace gas pressure is 0.1 MPa, and the pressure maintaining gas is high-purity argon;

[0070] In step two, the current of the arc furnace is 100 A during vacuum melting, and the time is 5 min; the cooling circulating water flow rate is 1 m / s;

[0071] In step two, the button ingot is turned over by using the mechanical hand of the furnace, and then the initial melting alloy ingot is continuously melted again, and the molten state is maintained for 10 s, and the multiple melting in step two is 10 times;

[0072] Step three: the non-equal molar ratio Ti 0.280 V 0.270 Zr 0.005 Nb 0.400 The high-entropy alloy is mechanically crushed, and the crushed hydrogen storage material sample powder particles 7 are filtered by using a 100-mesh sieve;

[0073] Step four: the filtered hydrogen storage material sample powder particles 7 obtained in step three are put into a stainless steel ball milling tank, stainless steel ball milling beads and hydrogen storage material sample powder particles 7 are mixed according to a mass ratio of 12:1, and ball milling is carried out in a ball mill at a rotating speed of 250 rad / min, and the ball milling time is 20 min;

[0074] Step five: the hydrogen storage material sample powder particles 7 are poured into a 200-mesh sieve for filtration, and are uniformly placed in the hydrogen storage material sample powder particle reaction space, then the sieve assembly is clamped on the upper annular clamping groove 202 for fixation, and is connected with the PCT hydrogen storage tester;

[0075] Step six: the PCT hydrogen storage tester is vacuumed, and then hydrogen is introduced after stabilization;

[0076] Step seven: heating the hydrogen storage reactor to a first predetermined temperature and keeping the temperature constant; then filling the PCT hydrogen storage tester with hydrogen, so that the hydrogen storage material sample powder particles 7 fully absorb hydrogen, discharging the hydrogen in the PCT hydrogen storage tester and vacuumizing, then heating the hydrogen storage reactor to a specific temperature to completely release hydrogen, and repeating the cycle.

[0077] The temperature of the hydrogen storage reactor is adjusted to a third temperature threshold and kept constant for a period of time, and hydrogen is introduced so that the hydrogen storage material sample powder particles 7 fully absorb hydrogen.

[0078] The vacuum degree in step six is -0.101 MPa, the hydrogen pressure in step six is 1 MPa, and the stabilization time in step six is 10 min.

[0079] The first predetermined temperature in step seven is 300°C, and the temperature is kept constant at the first predetermined temperature for 1.5 hours, wherein the hydrogen pressure in the PCT hydrogen storage tester in step seven is 3 MPa; the hydrogen pressure introduced after the temperature of the hydrogen storage reactor is adjusted to the third temperature threshold and kept constant for a period of time is 3 MPa; wherein the specific temperature in step seven is 400°C, and the number of repeated cycles in step seven is 4.

[0080] The first temperature threshold in step eight is 150°C, and the temperature is kept constant for 1-1.5 hours after heating to the first temperature threshold, the hydrogen pressure in step eight is 3 MPa, the second temperature threshold in step eight is 400°C, the third temperature threshold in step eight is 250°C, and the temperature is kept constant for 0.8 hours after heating to the third temperature threshold.

[0081] Example 2

[0082] Ti 0.305 V 0.275 Zr 0.100 Nb 0.320 The method for storing hydrogen in the reactor using the new invention includes the following steps:

[0083] Step one: prepare high-purity raw materials Ti, V, Zr and Nb particles, according to Ti 0.305 V 0.275 Zr 0.100 Nb 0.320 The alloy composition design is to weigh the matching mass of the raw materials according to the atomic percentage.

[0084] The metal raw materials in step one are prepared according to the following atomic percentage: Ti is 30.5%, V is 27.5%, Zr is 10%, and Fe is 32%;

[0085] Step two: the raw materials in step one are sequentially placed into a copper crucible of a non-consumable vacuum arc furnace according to the proportion, vacuumized, and then filled with argon for protection smelting, and the button ingot is repeatedly turned and repeatedly smelted for multiple times. After the multiple smelting process is completed, the non-equimolar ratio Ti 0.305 V 0.275 Zr 0.100 Nb 0.320 high-entropy alloy button ingot;

[0086] In step two, the vacuum smelting is performed at a vacuum degree of 1*10 -3 Pa, and the furnace gas pressure is 0.03 MPa, and the pressure maintaining gas is high-purity argon;

[0087] In step two, the electric current of the arc furnace is 550 A during the vacuum smelting, and the time is 1 min; and the cooling circulating water flow rate is 5 m / s;

[0088] In step two, the button ingot is turned by using a mechanical hand of the furnace to turn the initially smelted alloy ingot, and then smelted again, and the smelting state is maintained for 50 s. The multiple smelting in step two is 5 times;

[0089] Step three: the non-equimolar ratio Ti0.280V0.270Zr0.005Nb0.400 high-entropy alloy obtained by smelting is mechanically crushed, and the crushed hydrogen storage material sample powder particles 7 are filtered by using a 100-mesh sieve;

[0090] Step four: the filtered sample obtained in step three is placed into a 250-ml stainless steel ball mill jar, and stainless steel ball milling beads and the sample are mixed according to a mass ratio of 13:1. The ball milling is performed in a star-shaped ball mill at a speed of 250 rad / min, and the ball milling time is 25 min;

[0091] Step five: the hydrogen storage material sample powder particles 7 are poured into a 200-mesh sieve for filtration, and then uniformly placed into a hydrogen storage material sample powder particle reaction space, and then the sieve assembly is clamped on the upper annular clamping groove 202 for fixation, and connected with a PCT hydrogen storage tester;

[0092] Step six: the PCT hydrogen storage tester is vacuumized, and then hydrogen is introduced after stabilization;

[0093] Step seven: heating the hydrogen storage reactor to a first predetermined temperature and keeping the temperature; then filling the PCT hydrogen storage tester with hydrogen, so that the hydrogen storage material sample powder particles 7 fully absorb hydrogen, discharging the hydrogen in the PCT hydrogen storage tester and vacuumizing, then heating the hydrogen storage reactor to a specific temperature to completely release hydrogen, and repeating the cycle.

[0094] After the hydrogen storage reactor temperature is adjusted to the third temperature threshold and kept for a period of time, hydrogen is introduced to allow the hydrogen storage material sample powder particles 7 to fully absorb hydrogen.

[0095] The vacuum degree in step six is -0.101 MPa, the hydrogen pressure introduced in step six is 1 MPa, and the stabilization time in step six is 20 min.

[0096] The first predetermined temperature in step seven is 300°C, and the temperature is kept at the first predetermined temperature for 2 hours, wherein the hydrogen pressure filled in the PCT hydrogen storage tester in step seven is 3 MPa; the hydrogen pressure introduced after the hydrogen storage reactor temperature is adjusted to the third temperature threshold and kept for a period of time is 3 MPa; wherein the specific temperature in step seven is 400°C, and the number of repeated cycles in step seven is 4.

[0097] The first temperature threshold in step eight is 150°C, and the temperature is kept at the first temperature threshold for 1-1.5 hours, the hydrogen pressure introduced in step eight is 3 MPa, the second temperature threshold in step eight is 400°C, the third temperature threshold in step eight is 250°C, and the temperature is kept at the third temperature threshold for 1 hour.

[0098] Example 3

[0099] Ti 0.330 V 0.280 Zr 0.090 Nb 0.300 The method for storing hydrogen by using the new reactor of the application comprises the following steps:

[0100] Step one: preparing high-purity raw materials Ti, V, Zr and Nb particles, according to Ti 0.330 V 0.280 Zr 0.090 Nb 0.300 The alloy component design is to weigh the matching mass of the raw materials according to the atomic percentage.

[0101] In step one, the metal raw materials are prepared according to the following raw materials: Ti is 33%, V is 28%, Zr is 9%, and Fe is 30%.

[0102] Step two: Put the raw materials in step one into the copper crucible of the non-consumable vacuum arc furnace according to the ratio in sequence, and after vacuumizing, fill in argon for protection smelting, get the button ingot, repeat the turning and repeat the smelting for many times, after the end of the multiple smelting process, cool to get the non-equal molar ratio Ti 0.330 V 0.280 Zr 0.090 Nb 0.300 High-entropy alloy button ingot

[0103] In step two, the vacuum smelting is carried out at a vacuum degree of 1*10 -3 Pa, the furnace gas pressure is 0.03 MPa, and the pressure maintaining gas is high-purity argon;

[0104] In step two, the electric current of the arc furnace is 350 A during vacuum smelting, and the time is 3 min; the cooling circulating water flow rate is 4 m / s;

[0105] In step two, the button ingot is turned over by using the mechanical hand of the furnace to continue to smelt, and the molten state is maintained for 50 s; the multiple smelting in step two is 5 times;

[0106] Step three: mechanically crush the non-equal molar ratio Ti 0.330 V 0.280 Zr 0.090 Nb 0.300 High-entropy alloy, and filter the crushed hydrogen storage material sample powder particles 7 using a 100-mesh sieve;

[0107] Step four: Put the filtered sample obtained in step three into a 250-ml stainless steel ball mill jar, and mix the stainless steel ball milling beads and the sample according to the mass ratio of 15:1. Ball mill in the star-shaped ball mill at a speed of 250 rad / min, and the ball milling time is 30 min;

[0108] Step five: Pour the hydrogen storage material sample powder particles 7 into a 200-mesh sieve, filter, and uniformly put them into the hydrogen storage material sample powder particle reaction space, then clamp the sieve assembly on the upper annular clamping groove 202 to fix, and connect the PCT hydrogen storage tester;

[0109] Step six: vacuumize the PCT hydrogen storage tester, and then introduce hydrogen gas after stabilization;

[0110] Step seven: heating the hydrogen storage reactor to a first predetermined temperature and keeping the temperature; then filling the PCT hydrogen storage tester with hydrogen, so that the hydrogen storage material sample powder particles 7 fully absorb hydrogen, discharging the hydrogen in the PCT hydrogen storage tester and vacuumizing, then heating the hydrogen storage reactor to a specific temperature to completely release hydrogen, and repeating the cycle.

[0111] After the hydrogen storage reactor temperature is adjusted to the third temperature threshold and kept for a period of time, hydrogen is introduced to make the hydrogen storage material sample powder particles 7 fully absorb hydrogen.

[0112] The vacuum degree in step six is -0.101 MPa, the hydrogen pressure introduced in step six is 1 MPa, and the stabilization time in step six is 15 min;

[0113] The first predetermined temperature in step seven is 300℃, and the temperature is kept at the first predetermined temperature for 1.8 hours, wherein the hydrogen pressure filled in the PCT hydrogen storage tester in step seven is 3 MPa; the hydrogen pressure introduced after the hydrogen storage reactor temperature is adjusted to the third temperature threshold and kept for a period of time is 3 MPa; wherein the specific temperature in step seven is 400℃, and the number of repeated cycles in step seven is 4.

[0114] The first temperature threshold in step eight is 150℃, and the temperature is kept at the first temperature threshold for 1h-1.5h, the hydrogen pressure introduced in step eight is 3 MPa, the second temperature threshold in step eight is 400℃, the third temperature threshold in step eight is 250℃, and the temperature is kept at the third temperature threshold for 1.2h.

[0115] Comparative Example 1

[0116] Ti 0.280 V 0.270 Zr 0.005 Nb 0.400 Prepared by using a conventional reactor and using the same preparation method as the hydrogen storage reactor of the embodiment of the present application, including the following steps:

[0117] Step one: preparing high-purity raw materials Ti, V, Zr and Nb particles, according to Ti 0.280 V 0.270 Zr 0.005 Nb 0.400 The alloy component design is to weigh the matching mass of the raw materials according to the atomic percentage, and the metal raw materials in step one are prepared according to the atomic percentage as follows: Ti is 28%, V is 27%, Zr is 5%, and Fe is 40%.

[0118] Step two: Put the raw materials in step one into the copper crucible of the non-consumable vacuum arc furnace according to the ratio in sequence, perform vacuumizing, and then fill in argon gas for protection smelting, obtain the button ingot, repeat the turning and repeated smelting for multiple times, and after the multiple smelting process, cool to obtain the non-equal molar ratio Ti 0.325 V 0.275 Zr 0.075 Nb 0.325 high-entropy alloy button ingot;

[0119] In step two, the vacuum smelting is performed at a vacuum degree of 4*10 -3 Pa, the furnace gas pressure is 0.1 MPa, and the pressure maintaining gas is high-purity argon;

[0120] In step two, the electric current of the arc furnace is 100 A during the vacuum smelting, and the time is 5 min; the cooling circulating water flow rate is 1 m / s;

[0121] In step two, the button ingot turning is operated by using the mechanical hand of the furnace to turn the initial smelting alloy ingot, continue to smelt again, and the smelting state is maintained for 10 s, and the multiple smelting is 10 times;

[0122] Step three: mechanically crush the non-equal molar ratio Ti 0.325 V 0.275 Zr 0.075 Nb 0.325 high-entropy alloy, and filter the crushed hydrogen storage material sample powder particles 7 using a 100-mesh sieve;

[0123] Step four: Put the filtered hydrogen storage material sample powder particles 7 obtained in step three into a stainless steel ball milling tank, mix the stainless steel ball milling beads and the hydrogen storage material sample powder particles 7 according to a mass ratio of 12:1, and perform ball milling in the ball mill at a rotating speed of 250 rad / min, and the ball milling time is 20 min;

[0124] Step five: pour the hydrogen storage material sample powder particles 7 into a 200-mesh sieve for filtering, and uniformly put them into the hydrogen storage material sample powder reaction space, then clamp the sieve assembly on the upper annular clamping groove 202 for fixation, and connect the PCT hydrogen storage tester;

[0125] Step six: vacuumize the PCT hydrogen storage tester, and then introduce hydrogen gas after stabilization;

[0126] Step seven: heating the hydrogen storage reactor to a first predetermined temperature and keeping the temperature; then filling the PCT hydrogen storage tester with hydrogen, so that the hydrogen storage material sample powder particles 7 fully absorb hydrogen, discharging the hydrogen in the PCT hydrogen storage tester and vacuumizing, then heating the hydrogen storage reactor to a specific temperature to completely release hydrogen, and repeating the cycle; step eight: heating the hydrogen storage reactor to a first temperature threshold and keeping the temperature, then filling the hydrogen to make the hydrogen storage material sample powder particles 7 fully absorb hydrogen, discharging the hydrogen in the PCT hydrogen storage tester and vacuumizing, then heating the reactor to a second temperature threshold to completely release hydrogen,

[0127] After the temperature of the hydrogen storage reactor is adjusted to a third temperature threshold and kept for a period of time, hydrogen is filled to make the hydrogen storage material sample powder particles 7 fully absorb hydrogen.

[0128] The vacuum degree in the above step six is -0.101 MPa, the hydrogen pressure filled in step six is 1 MPa, and the stabilization time in step six is 10 min;

[0129] The first predetermined temperature in the above step seven is 300℃, and the temperature is kept at the first predetermined temperature for 1.5 hours, wherein the hydrogen pressure filled in the PCT hydrogen storage tester in step seven is 3 MPa; the hydrogen pressure filled after the temperature of the hydrogen storage reactor is adjusted to a third temperature threshold and kept for a period of time is 3 MPa; wherein the specific temperature in step seven is 400℃, and the number of repeated cycles in step seven is 4.

[0130] The first temperature threshold in the above step eight is 150℃, the temperature is kept at the first temperature threshold for 1h, the hydrogen pressure filled in step eight is 3 MPa, the second temperature threshold in step eight is 400℃, the third temperature threshold in step eight is 250℃, and the temperature is kept at the third temperature threshold for 0.8h.

[0131] Comparative Example 2

[0132] Ti 0.305 V 0.275 Zr 0.100 Nb 0.320 The traditional reactor is prepared, and the same preparation method as the hydrogen storage reactor of the embodiment of the application is adopted, including the following steps:

[0133] Step one: preparing high-purity raw materials Ti, V, Zr and Nb particles, according to the alloy composition design, the mass of the raw materials is weighed according to the atomic percentage, and the metal raw materials in step one are prepared according to the following raw materials: Ti is 30.5%, V is 27.5%, Zr is 10%, and Fe is 32%.

[0134] Step two: Put the raw materials in step one into the copper crucible of the non-consumable vacuum arc furnace according to the proportion in sequence, and then perform protection smelting after vacuumizing and filling in argon. Repeat the turning of the button ingot and the smelting for multiple times after obtaining the button ingot. After the multiple smelting processes, cool to obtain the non-equi-molar ratio Ti 0.305 V 0.275 Zr 0.100 Nb 0.320 high-entropy alloy button ingot

[0135] In step two, the vacuum degree is 1*10 -3 Pa, the furnace gas pressure is 0.03 MPa, and the pressure maintaining gas is high-purity argon.

[0136] In step two, the current of the arc furnace is 550 A during vacuum smelting, and the time is 1 min; the cooling circulating water flow rate is 5 m / s.

[0137] In step two, the button ingot is turned over by using the mechanical hand of the furnace to continue smelting again, and the molten state is maintained for 50 s. The multiple smelting in step two is 5 times.

[0138] Step three: mechanically crush the non-equi-molar ratio Ti0.280V0.270Zr0.005Nb0.400 high-entropy alloy obtained by smelting, and filter the crushed hydrogen storage material sample powder particles 7 using a 100-mesh sieve.

[0139] Step four: Put the filtered sample obtained in step three into a 250-ml stainless steel ball mill jar, and mix the stainless steel ball milling beads and the sample according to the mass ratio of 13:1. Perform ball milling in a star-shaped ball mill at a speed of 250 rad / min, and the ball milling time is 25 min.

[0140] Step five: filter the hydrogen storage material sample powder particles 7 into a 200-mesh sieve, and uniformly put them into the hydrogen storage material sample powder particle reaction space. Then, clamp the sieve assembly on the upper annular clamping groove 202 to fix it, and connect the PCT hydrogen storage tester.

[0141] Step six: vacuumize the PCT hydrogen storage tester, and then introduce hydrogen gas after stabilization.

[0142] Step 7: Heat the hydrogen storage reactor to a first predetermined temperature and maintain this temperature; then, introduce hydrogen gas into the PCT hydrogen storage tester to allow the hydrogen storage material sample powder particles 7 to fully absorb hydrogen. After purging the hydrogen gas from the PCT hydrogen storage tester, evacuate the system. Then, heat the hydrogen storage reactor to a specific temperature to completely release the hydrogen, and repeat the cycle. Step 8: Heat the hydrogen storage reactor to a first temperature threshold and maintain this temperature. Then, introduce hydrogen gas to allow the hydrogen storage material sample powder particles 7 to fully absorb hydrogen. After purging the hydrogen gas from the PCT hydrogen storage tester, evacuate the system. Then, heat the reactor to a second temperature threshold to completely release the hydrogen.

[0143] After adjusting the temperature of the hydrogen storage reactor to the third temperature threshold and maintaining it for a period of time, hydrogen gas is introduced to allow the hydrogen storage material sample powder particles 7 to fully absorb hydrogen.

[0144] The vacuum level in step six is ​​-0.101 MPa, the hydrogen pressure of the hydrogen gas introduced in step six is ​​1 MPa, and the stabilization time in step six is ​​20 min.

[0145] In step seven above, the first predetermined temperature is 300℃, and the temperature is maintained at the first predetermined temperature for 2 hours. In step seven, the hydrogen pressure of the hydrogen gas introduced into the PCT hydrogen storage tester is 3MPa. After the temperature of the hydrogen storage reactor is adjusted to the third temperature threshold and maintained for a period of time, the hydrogen gas pressure introduced is 3MPa. In step seven, the specific temperature is 400℃, and the number of times the cycle in step seven is repeated is 4.

[0146] In step eight above, the first temperature threshold is 150°C, and the holding time after heating to the first temperature threshold is 1h-1.5h. The hydrogen pressure of the hydrogen gas introduced in step eight is 3MPa. The second temperature threshold in step eight is 400°C. The third temperature threshold in step eight is 250°C, and the holding time after heating to the third temperature threshold is 1h.

[0147] from Figure 5 and Figure 6 As can be seen, with the increase of Zr / Nb, the dendritic crystals in the alloy microstructure become significantly coarser.

[0148] and Figure 7 and Figure 8 The figure shows the activation effect of hydrogen storage material sample powder particles 7 in the new reactor. As can be seen from the figure, the hydrogen storage material sample powder particles 7 were fully activated in the fourth hydrogen absorption and desorption cycle. Since there was no accumulation of hydrogen storage material sample powder particles 7, the hydrogen absorption rate was relatively fast, and the hydrogen absorption amount reached saturation within 2 minutes in each hydrogen absorption process.

[0149] Figure 9 Example 1: Ti 0.280 V 0.270 Zr 0.005 Nb0.400 Alloy powder and the same mass of Comparative Example 1: Ti 0.280 V 0.270 Zr 0.005 Nb 0.400 Comparison chart of hydrogen storage performance of alloy powder at two different temperatures.

[0150] Figure 10 For Example 2: Ti 0.305 V 0.275 Zr 0.100 Nb 0.320 Alloy powder and the same mass of Comparative Example 2: Ti 0.305 V 0.275 Zr 0.100 Nb 0.320 Comparison chart of hydrogen storage performance of alloy powder at two different temperatures. It can be seen that the maximum hydrogen storage capacity and hydrogen storage rate of the example are higher than those of the comparative example at two different temperatures. The reason is that the new hydrogen storage reactor, compared with the old reactor, has no accumulation and splashing of hydrogen storage material sample powder particles 7, so that the contact area between the hydrogen storage material sample powder particles 7 and hydrogen is increased, the hydrogen storage is more complete, the hydrogen storage rate is higher, the experimental error is reduced, and the experimental result is more accurate. In summary, the anti-accumulation and anti-splashing effect of the present application greatly reduces the experimental error.

[0151] Obviously, the above embodiments of the present application are only examples for clearly illustrating the present application, and are not a limitation on the embodiments of the present application. For ordinary skilled in the art, on the basis of the above description, other different forms of changes or variations can also be made, and it is impossible to enumerate all the embodiments here. Any changes or variations that belong to the technical solutions of the present application and are obvious are still within the protection scope of the present application.

Claims

1. A hydrogen storage reactor for increasing the contact area of a hydrogen storage material with hydrogen gas, characterized by, The reactor comprises a reactor body (2) and a screen assembly arranged in the reactor body (2), wherein the screen assembly comprises an upper screen (3), a lower screen (5) and a weighted fixing member (4), The upper screen (3) and the lower screen (5) are fixed together by the weighted fixing member (4), and the upper screen (3), the lower screen (5) and the weighted fixing member (4) enclose a hydrogen storage material sample powder particle reaction space; The reactor body (2) has a sample reaction part at an upper portion and a gas inlet part at a lower portion, the sample reaction part has a mounting table (201) arranged in a circumferential direction, and the screen assembly is fixed on the mounting table (201); the gas inlet part has an inner diameter smaller than that of the sample reaction part, and a cross section of the gas inlet part is conical; The hydrogen storage material sample powder particles (7) are arranged in the hydrogen storage material sample powder particle reaction space, and the hydrogen storage material sample powder particles (7) have a particle size of 170-200 mesh, and the upper screen (3) and the lower screen (5) have a pore size of 450-550 mesh; The diameter of the upper screen (3) is the same as that of the screen (9), a clear distance between the upper screen (3) and the lower screen (5) is 0.2-0.5 cm, and an upper annular clamping groove (202) is arranged on an inner wall of the sample reaction part and opens upward, an upper edge of the weighted fixing member (4) abuts against the annular boss, a top portion of the upper edge extends outward in the circumferential direction and is then bent downward, and the upper edge is clamped with the upper annular clamping groove (202).

2. The hydrogen storage reactor for increasing the contact area of hydrogen storage material with hydrogen gas according to claim 1, wherein: The lower screen (5) is fixed at a bottom portion of the weighted fixing member (4), the upper screen (3) is arranged at a top portion of the weighted fixing member (4), the upper screen (3) has a fixing member connecting section and an opening section, the fixing member connecting section is fixed at the top portion of the weighted fixing member (4) in the circumferential direction, and the opening section is fixed at the top portion of the weighted fixing member (4) by a connecting fastener, and the weighted fixing member (4) is placed on the mounting table (201) of the sample reaction part.

3. A method for preparing a sample powder particle of a hydrogen storage material using the hydrogen storage reactor for increasing the contact area between the hydrogen storage material and hydrogen gas according to claim 2, characterized by, The method comprises the following steps: Step one: prepare high-purity raw materials Ti, V, Zr and Nb particles, Ti x V y Zr z Nb m The high-entropy alloy hydrogen storage material is prepared by taking the raw materials according to the atomic percentage, and the main elements of the alloy are Ti 28%-33%, V 25%-28%, Zr 5%-10%, and Fe 30%-40%. Step two: Put the raw materials in step one into the copper crucible of the non-consumable vacuum arc furnace according to the proportion, melt and protect by filling argon after vacuumizing, repeat turning over and melting after getting the button ingot, and cool to get the non-equal molar ratio Ti x V y Zr z Nb m High-entropy alloy button ingot Step three: melt the non-equimolar ratio Ti x V y Zr z Nb m The high-entropy alloy is mechanically pulverized, and the hydrogen storage material sample powder particles (7) after pulverization are filtered using a 100-mesh sieve. Step four: the filtered hydrogen storage material sample powder particles (7) obtained in step three are put into a stainless steel ball mill tank, stainless steel ball milling beads and the hydrogen storage material sample powder particles (7) are mixed at a mass ratio of 12-15:1, and ball milling is performed in a ball mill at a rotating speed of 250 rad / min, and the ball milling time is 20-30 min; Step five: the hydrogen storage material sample powder particles (7) are poured into a 200 mesh sieve for filtration, and then are uniformly put into the hydrogen storage material sample powder particle reaction space, the screen assembly is clamped on the upper annular clamping groove for fixation, and a PCT hydrogen storage tester is connected; Step six: the PCT hydrogen storage tester is vacuumized, and then hydrogen is introduced after stabilization; Step seven: the hydrogen storage reactor is heated to a first predetermined temperature and is kept at the temperature, then hydrogen is filled into the PCT hydrogen storage tester, the hydrogen storage material sample powder particles (7) are fully hydrogenated, the hydrogen in the PCT hydrogen storage tester is discharged, the hydrogen storage reactor is vacuumized again, the hydrogen is completely released by heating the hydrogen storage reactor to a specific temperature, and the cycle is repeated. Step eight: heating the hydrogen storage reactor to a first temperature threshold and keeping the temperature, then introducing hydrogen to make the hydrogen storage material sample powder particles (7) fully absorb hydrogen, then discharging the hydrogen in the PCT hydrogen storage tester and vacuumizing, then heating the reactor to a second temperature threshold to completely release hydrogen; Step eight: heating the hydrogen storage reactor to a first temperature threshold and keeping the temperature, then introducing hydrogen to make the hydrogen storage material sample powder particles (7) fully absorb hydrogen, then discharging the hydrogen in the PCT hydrogen storage tester and vacuumizing, then heating the reactor to a second temperature threshold to completely release hydrogen; 4. The method of claim 3, wherein the method further comprises: The vacuumizing in step six is at a vacuum degree of -0.101 MPa, the hydrogen pressure introduced in step six is 1 MPa, and the stabilization time in step six is 10-20 min.

5. The method of claim 3, wherein the method further comprises: The first predetermined temperature in step seven is 300℃, and the temperature is kept at the first predetermined temperature for 1.5-2 hours, the hydrogen pressure introduced in the PCT hydrogen storage tester in step seven is 3 MPa, the hydrogen pressure introduced after the temperature of the hydrogen storage reactor is adjusted to the third temperature threshold and kept for a period of time in step seven is 3 MPa, the specific temperature in step seven is 400℃, and the number of repeated cycles in step seven is 4.

6. The method of claim 3, wherein the method further comprises: The first temperature threshold in step eight is 150℃, the temperature is kept for 1h-1.5h after being heated to the first temperature threshold, the hydrogen pressure introduced in step eight is 3 MPa, the second temperature threshold in step eight is 400℃, the third temperature threshold in step eight is 250℃, and the temperature is kept for 0.8h-1.2h after being heated to the third temperature threshold.

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