Preparation process of environment-friendly low-energy-consumption hydrogen storage alloy material

Abstract

The invention discloses a preparation technology of an environment-friendly low-energy-consumption hydrogen storage alloy material. The preparation technology comprises the following steps that S1, raw materials are selected and pretreated; s2, wet ball milling and mixing; step S3, drying and forming; s4, performing subsequent processing and detection; the low-energy-consumption hydrogen storage alloy material with excellent hydrogen storage performance and environmental protection characteristic can be prepared through the process, and the method not only reduces energy consumption and environmental pollution in the preparation process, but also improves the performance and quality of an alloy product; the prepared hydrogen storage alloy material has a porous structure, so that rapid absorption, release and diffusion of hydrogen are facilitated, and the hydrogen storage efficiency is improved; by means of the process, energy consumption and environmental pollution are reduced, the performance and stability of the hydrogen storage alloy material are improved, and powerful support is provided for development of the hydrogen energy technology.

Description

Technical Field

[0001] The present invention belongs to the technical field of hydrogen storage material preparation, and specifically relates to a process for preparing an environmentally friendly, low-energy-consumption hydrogen storage alloy material. Background Art

[0002] With the intensification of the energy crisis and the improvement of environmental protection awareness, hydrogen energy, as a clean and efficient energy carrier, has attracted extensive attention for its storage and utilization technology. As an important hydrogen storage material, hydrogen storage alloys have the advantages of high hydrogen storage density, strong safety, and recyclability. However, the preparation process of traditional hydrogen storage alloys often has problems such as high energy consumption, environmental pollution, and unstable performance. Therefore, it is particularly important to develop an environmentally friendly and low-energy consumption hydrogen storage alloy material preparation process.

[0003] Based on this, an environmentally friendly and low-energy consumption hydrogen storage alloy material preparation process is designed. Summary of the invention

[0004] In view of the above situation, in order to overcome the defects of the prior art, the present invention provides an environmentally friendly and low-energy consumption hydrogen storage alloy material preparation process, which effectively solves the problems raised in the above background.

[0005] To achieve the above object, the present invention provides the following technical solution: a process for preparing an environmentally friendly low-energy consumption hydrogen storage alloy material, comprising the following steps:

[0006] Step S1, raw material selection and pretreatment:

[0007] S1.1, Raw material selection: According to the design requirements of the alloy, select high-purity, environmentally friendly alloy raw materials, including Ti, Zr, Mn, Cr, V4Fe and rare earth elements;

[0008] S1.2, Pretreatment: Strictly screen the selected raw materials to remove impurities and unqualified particles, and then clean them to ensure that the surface of the raw materials is clean and pollution-free;

[0009] Step S2, wet ball milling mixing:

[0010] S2.1. Weigh the raw materials: weigh various raw materials according to the formula ratio;

[0011] S2.2, wet ball milling: the weighed raw materials are placed in a nylon ball mill, and anhydrous ethanol is added as a solvent. At the same time, zirconium oxide grinding balls are added to assist the mixing and refining process. The wet ball milling is carried out in the ball mill. Through the collision and shearing action of the grinding balls, the raw materials are fully mixed and refined into uniform and fine powders;

[0012] S2.3, Vacuum treatment: During the ball milling process, the ball mill is vacuumed to reduce the impact of oxygen and other impurities on the raw materials. The vacuum degree is ≤10Pa to ensure the purity of the mixing environment;

[0013] Step S3, drying and molding:

[0014] S3.1, drying treatment: the mixed raw material powder after wet ball milling is taken out from the ball mill, placed in a vacuum oven, and dried at a temperature of 60-120°C to remove the residual anhydrous ethanol solvent for 2-4 hours;

[0015] S3.2, molding: fill the mold with the dried mixed raw material powder to ensure that the powder is evenly distributed and compacted;

[0016] S3.3, sintering: placing the formed alloy body in a hot pressing sintering furnace, and performing primary sintering in an environment with a vacuum degree lower than 10^-3Pa, the sintering temperature is 600-800℃, and the sintering time is 1-2h, and then, based on the primary sintering, secondary sintering is performed, the sintering temperature is increased to 800-1000℃, and the sintering time is 2-4h. Through the sintering process, the powder particles in the alloy body undergo solid phase reaction and diffusion to form a dense alloy structure;

[0017] Step S4, subsequent processing and detection:

[0018] S4.1. Cooling: taking the sintered hydrogen storage alloy material out of the hot pressing sintering furnace and cooling it naturally to room temperature;

[0019] S4.2, Surface treatment: The sintered alloy product is subjected to surface grinding and polishing treatment to remove defects and impurities on the surface of the product, and then the surface of the alloy is cleaned with anhydrous ethanol to remove residues, and then dried again to improve its surface finish and corrosion resistance;

[0020] S4.3, Quality testing: Perform performance testing on the prepared hydrogen storage alloy materials, including hydrogen storage capacity, cycle stability, mass transfer and heat transfer performance indicators, to ensure that they meet relevant standards and requirements;

[0021] S4.4. Packaging and storage: Qualified hydrogen storage alloy products shall be packaged, marked with product information and production date, and then stored in designated warehouses to ensure that the storage environment meets the requirements and avoid fire and corrosion hazards.

[0022] Preferably, in step S1, calculated by mass percentage, Ti: 40%-60%, Zr: 5%-15%, Mn: 30%-50%, Cr: 5%-15%, V4Fe: 10%-30% and rare earth elements: 0.1%-0.5%.

[0023] Preferably, in step S1, the raw material can be cleaned by water washing, acid washing or ultrasonic cleaning.

[0024] Preferably, water washing: placing the raw material in a cleaning tank, washing with running water for 10-20 minutes until there is no obvious contaminant on the surface, then rinsing with deionized water at 30-60°C, and finally drying with nitrogen or dry air;

[0025] Pickling: slowly add the raw materials into a dilute hydrochloric acid solution with a concentration of 5%-15%, control the temperature between 30-60℃, react for 5-30min, and stir to ensure uniform contact. After the reaction, rinse with deionized water and blow dry with nitrogen or dry air.

[0026] Ultrasonic cleaning: Place the raw materials in an ultrasonic cleaning machine, add an appropriate amount of cleaning liquid, turn on the ultrasonic generator for cleaning, the ultrasonic frequency is between 20-40kHz, and the cleaning time is 5-30 minutes. After cleaning, rinse with deionized water and then blow dry with nitrogen or dry air.

[0027] Preferably, in step S2, the concentration of anhydrous ethanol is ≥99.5%, the speed of the ball mill is 100-300 rpm, and the ball milling time is 2-4 h.

[0028] Compared with the prior art, the present invention has the following beneficial effects:

[0029] The present invention can prepare a low-energy hydrogen storage alloy material with excellent hydrogen storage performance and environmental protection characteristics through the process. This method not only reduces the energy consumption and environmental pollution in the preparation process, but also improves the performance and quality of the alloy products; and the prepared hydrogen storage alloy material has a porous structure, which is conducive to the rapid absorption and diffusion of hydrogen, thereby improving the hydrogen storage efficiency; this process not only reduces energy consumption and environmental pollution, but also improves the performance and stability of the hydrogen storage alloy material, providing strong support for the development of hydrogen energy technology. DETAILED DESCRIPTION

[0030] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments; based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0031] The present invention provides an environmentally friendly low-energy consumption hydrogen storage alloy material preparation process, comprising the following steps:

[0032] Step S1, raw material selection and pretreatment:

[0033] S1.1, Raw material selection: According to the design requirements of the alloy, select high-purity, environmentally friendly alloy raw materials, including Ti, Zr, Mn, Cr, V4Fe and rare earth elements;

[0034] S1.2, Pretreatment: Strictly screen the selected raw materials to remove impurities and unqualified particles, and then clean them to ensure that the surface of the raw materials is clean and pollution-free;

[0035] Step S2, wet ball milling mixing:

[0036] S2.1. Weigh the raw materials: weigh various raw materials according to the formula ratio;

[0037] S2.2, wet ball milling: the weighed raw materials are placed in a nylon ball mill, and anhydrous ethanol is added as a solvent. At the same time, zirconium oxide grinding balls are added to assist the mixing and refining process. The wet ball milling is carried out in the ball mill. Through the collision and shearing action of the grinding balls, the raw materials are fully mixed and refined into uniform and fine powders;

[0038] S2.3, Vacuum treatment: During the ball milling process, the ball mill is vacuumed to reduce the impact of oxygen and other impurities on the raw materials. The vacuum degree is ≤10Pa to ensure the purity of the mixing environment;

[0039] Step S3, drying and molding:

[0040] S3.1, drying treatment: the mixed raw material powder after wet ball milling is taken out from the ball mill, placed in a vacuum oven, and dried at a temperature of 60-120°C to remove the residual anhydrous ethanol solvent for 2-4 hours;

[0041] S3.2, molding: fill the mold with the dried mixed raw material powder to ensure that the powder is evenly distributed and compacted;

[0042] S3.3, sintering: placing the formed alloy body in a hot pressing sintering furnace, and performing primary sintering in an environment with a vacuum degree lower than 10^-3Pa, the sintering temperature is 600-800℃, and the sintering time is 1-2h, and then, based on the primary sintering, secondary sintering is performed, the sintering temperature is increased to 800-1000℃, and the sintering time is 2-4h. Through the sintering process, the powder particles in the alloy body undergo solid phase reaction and diffusion to form a dense alloy structure;

[0043] Step S4, subsequent processing and detection:

[0044] S4.1. Cooling: taking the sintered hydrogen storage alloy material out of the hot pressing sintering furnace and cooling it naturally to room temperature;

[0045] S4.2, Surface treatment: The sintered alloy product is subjected to surface grinding and polishing treatment to remove defects and impurities on the surface of the product, and then the surface of the alloy is cleaned with anhydrous ethanol to remove residues, and then dried again to improve its surface finish and corrosion resistance;

[0046] S4.3, Quality testing: Perform performance testing on the prepared hydrogen storage alloy materials, including hydrogen storage capacity, cycle stability, mass transfer and heat transfer performance indicators, to ensure that they meet relevant standards and requirements;

[0047] S4.4. Packaging and storage: Qualified hydrogen storage alloy products shall be packaged, marked with product information and production date, and then stored in designated warehouses to ensure that the storage environment meets the requirements and avoid fire and corrosion hazards.

[0048] In step S1 of this embodiment, calculated by mass percentage, Ti: 40%-60%, Zr: 5%-15%, Mn: 30%-50%, Cr: 5%-15%, V4Fe: 10%-30% and rare earth elements: 0.1%-0.5%.

[0049] In step S1 of this embodiment, the raw materials may be cleaned by water washing, acid washing or ultrasonic cleaning.

[0050] Washing in this embodiment: Place the raw material in a cleaning tank, rinse with running water for 10-20 minutes until there is no obvious contaminant on the surface, then rinse with deionized water at 30-60°C, and finally blow dry with nitrogen or dry air;

[0051] Pickling: slowly add the raw materials into a dilute hydrochloric acid solution with a concentration of 5%-15%, control the temperature between 30-60℃, react for 5-30min, and stir to ensure uniform contact. After the reaction, rinse with deionized water and blow dry with nitrogen or dry air.

[0052] Ultrasonic cleaning: Place the raw materials in an ultrasonic cleaning machine, add an appropriate amount of cleaning liquid, turn on the ultrasonic generator for cleaning, the ultrasonic frequency is between 20-40kHz, and the cleaning time is 5-30 minutes. After cleaning, rinse with deionized water and then blow dry with nitrogen or dry air.

[0053] In step S2 of this embodiment, the concentration of anhydrous ethanol is ≥99.5%, the speed of the ball mill is 100-300 rpm, and the ball milling time is 2-4 h.

[0054] Embodiment 1:

[0055] A process for preparing an environmentally friendly, low-energy consumption hydrogen storage alloy material comprises the following steps:

[0056] Step S1, raw material selection and pretreatment:

[0057] S1.1, Raw material selection: According to the design requirements of the alloy, select high-purity, environmentally friendly alloy raw materials, including Ti, Zr, Mn, Cr, V4Fe and rare earth elements;

[0058] S1.2, Pretreatment: Strictly screen the selected raw materials to remove impurities and unqualified particles, and then clean them to ensure that the surface of the raw materials is clean and pollution-free;

[0059] Step S2, wet ball milling mixing:

[0060] S2.1. Weigh the raw materials: weigh various raw materials according to the formula ratio;

[0061] S2.2, wet ball milling: the weighed raw materials are placed in a nylon ball mill, and anhydrous ethanol is added as a solvent. At the same time, zirconium oxide grinding balls are added to assist the mixing and refining process. The wet ball milling is carried out in the ball mill. Through the collision and shearing action of the grinding balls, the raw materials are fully mixed and refined into uniform and fine powders;

[0062] S2.3, Vacuum treatment: During the ball milling process, the ball mill is vacuumed to reduce the impact of oxygen and other impurities on the raw materials. The vacuum degree is ≤10Pa to ensure the purity of the mixing environment;

[0063] Step S3, drying and molding:

[0064] S3.1, drying treatment: the mixed raw material powder after wet ball milling is taken out from the ball mill, placed in a vacuum oven, and dried at 60°C to remove the residual anhydrous ethanol solvent for 2 hours;

[0065] S3.2, molding: fill the mold with the dried mixed raw material powder to ensure that the powder is evenly distributed and compacted;

[0066] S3.3, sintering: placing the formed alloy body in a hot pressing sintering furnace, and performing primary sintering at a vacuum of less than 10^-3Pa, with a sintering temperature of 600°C and a sintering time of 1h. Then, based on the primary sintering, secondary sintering is performed, with the sintering temperature increased to 800°C and the sintering time of 2h. Through the sintering process, the powder particles in the alloy body undergo solid phase reaction and diffusion to form a dense alloy structure;

[0067] Step S4, subsequent processing and detection:

[0068] S4.1. Cooling: taking the sintered hydrogen storage alloy material out of the hot pressing sintering furnace and cooling it naturally to room temperature;

[0069] S4.2, Surface treatment: The sintered alloy product is subjected to surface grinding and polishing treatment to remove defects and impurities on the surface of the product, and then the surface of the alloy is cleaned with anhydrous ethanol to remove residues, and then dried again to improve its surface finish and corrosion resistance;

[0070] S4.3, Quality testing: Perform performance testing on the prepared hydrogen storage alloy materials, including hydrogen storage capacity, cycle stability, mass transfer and heat transfer performance indicators, to ensure that they meet relevant standards and requirements;

[0071] S4.4. Packaging and storage: Qualified hydrogen storage alloy products shall be packaged, marked with product information and production date, and then stored in designated warehouses to ensure that the storage environment meets the requirements and avoid fire and corrosion hazards.

[0072] In step S1 of this embodiment, calculated by mass percentage, Ti: 40%, Zr: 5%, Mn: 30%, Cr: 5%, V4Fe: 10% and rare earth elements: 0.1%.

[0073] In step S1 of this embodiment, the raw materials may be cleaned by water washing, acid washing or ultrasonic cleaning.

[0074] Washing in this embodiment: Place the raw material in a cleaning tank, rinse with running water for 10 minutes until there is no obvious contaminant on the surface, then rinse with 30°C deionized water, and finally blow dry with nitrogen or dry air;

[0075] Pickling: slowly add the raw materials into a 5% dilute hydrochloric acid solution, control the temperature at 30°C, react for 5 minutes, and stir to ensure uniform contact. After the reaction, rinse with deionized water and blow dry with nitrogen or dry air.

[0076] Ultrasonic cleaning: Place the raw materials in an ultrasonic cleaning machine, add an appropriate amount of cleaning liquid, turn on the ultrasonic generator for cleaning, the ultrasonic frequency is between 20kHz, and the cleaning is for 5 minutes. After cleaning, rinse with deionized water and then blow dry with nitrogen or dry air.

[0077] In step S2 of this embodiment, the concentration of anhydrous ethanol is ≥99.5%, the ball mill speed is 100 rpm, and the ball milling time is 2 h.

[0078] Embodiment 2:

[0079] A process for preparing an environmentally friendly, low-energy consumption hydrogen storage alloy material comprises the following steps:

[0080] Step S1, raw material selection and pretreatment:

[0081] S1.1, Raw material selection: According to the design requirements of the alloy, select high-purity, environmentally friendly alloy raw materials, including Ti, Zr, Mn, Cr, V4Fe and rare earth elements;

[0082] S1.2, Pretreatment: Strictly screen the selected raw materials to remove impurities and unqualified particles, and then clean them to ensure that the surface of the raw materials is clean and pollution-free;

[0083] Step S2, wet ball milling mixing:

[0084] S2.1. Weigh the raw materials: weigh various raw materials according to the formula ratio;

[0085] S2.2, wet ball milling: the weighed raw materials are placed in a nylon ball mill, and anhydrous ethanol is added as a solvent. At the same time, zirconium oxide grinding balls are added to assist the mixing and refining process. The wet ball milling is carried out in the ball mill. Through the collision and shearing action of the grinding balls, the raw materials are fully mixed and refined into uniform and fine powders;

[0086] S2.3, Vacuum treatment: During the ball milling process, the ball mill is vacuumed to reduce the impact of oxygen and other impurities on the raw materials. The vacuum degree is ≤10Pa to ensure the purity of the mixing environment;

[0087] Step S3, drying and molding:

[0088] S3.1, drying treatment: the mixed raw material powder after wet ball milling is taken out from the ball mill, placed in a vacuum oven, and dried at 120°C to remove the residual anhydrous ethanol solvent for 4 hours;

[0089] S3.2, molding: fill the mold with the dried mixed raw material powder to ensure that the powder is evenly distributed and compacted;

[0090] S3.3, sintering: placing the formed alloy body in a hot pressing sintering furnace, and performing primary sintering in an environment with a vacuum degree lower than 10^-3Pa, the sintering temperature is 800℃, and the sintering time is 2h. Then, based on the primary sintering, secondary sintering is performed, the sintering temperature is increased to 1000℃, and the sintering time is 4h. Through the sintering process, the powder particles in the alloy body undergo solid phase reaction and diffusion to form a dense alloy structure;

[0091] Step S4, subsequent processing and detection:

[0092] S4.1. Cooling: taking the sintered hydrogen storage alloy material out of the hot pressing sintering furnace and cooling it naturally to room temperature;

[0093] S4.2, Surface treatment: The sintered alloy product is subjected to surface grinding and polishing treatment to remove defects and impurities on the surface of the product, and then the surface of the alloy is cleaned with anhydrous ethanol to remove residues, and then dried again to improve its surface finish and corrosion resistance;

[0094] S4.3, Quality testing: Perform performance testing on the prepared hydrogen storage alloy materials, including hydrogen storage capacity, cycle stability, mass transfer and heat transfer performance indicators, to ensure that they meet relevant standards and requirements;

[0095] S4.4. Packaging and storage: Qualified hydrogen storage alloy products shall be packaged, marked with product information and production date, and then stored in designated warehouses to ensure that the storage environment meets the requirements and avoid fire and corrosion hazards.

[0096] In step S1 of this embodiment, calculated by mass percentage, Ti: 60%, Zr: 15%, Mn: 50%, Cr: 15%, V4Fe: 30% and rare earth elements: 0.5%.

[0097] In step S1 of this embodiment, the raw materials may be cleaned by water washing, acid washing or ultrasonic cleaning.

[0098] Washing in this embodiment: Place the raw material in a cleaning tank, rinse with running water for 20 minutes until there is no obvious contaminant on the surface, then rinse with deionized water at 60°C, and finally blow dry with nitrogen or dry air;

[0099] Pickling: slowly add the raw materials into a 15% dilute hydrochloric acid solution, control the temperature at 60°C, react for 30 minutes, and stir to ensure uniform contact. After the reaction, rinse with deionized water and blow dry with nitrogen or dry air.

[0100] Ultrasonic cleaning: Place the raw materials in an ultrasonic cleaning machine, add an appropriate amount of cleaning liquid, turn on the ultrasonic generator for cleaning, the ultrasonic frequency is between 40kHz, and the cleaning is carried out for 30 minutes. After cleaning, rinse with deionized water and then blow dry with nitrogen or dry air.

[0101] In step S2 of this embodiment, the concentration of anhydrous ethanol is ≥99.5%, the ball mill speed is 300 rpm, and the ball milling time is 4 h.

[0102] Embodiment 3:

[0103] A process for preparing an environmentally friendly, low-energy consumption hydrogen storage alloy material comprises the following steps:

[0104] Step S1, raw material selection and pretreatment:

[0105] S1.1, Raw material selection: According to the design requirements of the alloy, select high-purity, environmentally friendly alloy raw materials, including Ti, Zr, Mn, Cr, V4Fe and rare earth elements;

[0106] S1.2, Pretreatment: Strictly screen the selected raw materials to remove impurities and unqualified particles, and then clean them to ensure that the surface of the raw materials is clean and pollution-free;

[0107] Step S2, wet ball milling mixing:

[0108] S2.1. Weigh the raw materials: weigh various raw materials according to the formula ratio;

[0109] S2.2, wet ball milling: the weighed raw materials are placed in a nylon ball mill, and anhydrous ethanol is added as a solvent. At the same time, zirconium oxide grinding balls are added to assist the mixing and refining process. The wet ball milling is carried out in the ball mill. Through the collision and shearing action of the grinding balls, the raw materials are fully mixed and refined into uniform and fine powders;

[0110] S2.3, Vacuum treatment: During the ball milling process, the ball mill is vacuumed to reduce the impact of oxygen and other impurities on the raw materials. The vacuum degree is ≤10Pa to ensure the purity of the mixing environment;

[0111] Step S3, drying and molding:

[0112] S3.1, drying treatment: the mixed raw material powder after wet ball milling is taken out from the ball mill, placed in a vacuum oven, and dried at 90°C to remove the residual anhydrous ethanol solvent for 3 hours;

[0113] S3.2, molding: fill the mold with the dried mixed raw material powder to ensure that the powder is evenly distributed and compacted;

[0114] S3.3, sintering: placing the formed alloy body in a hot pressing sintering furnace, and performing primary sintering at a vacuum of less than 10^-3Pa, with a sintering temperature of 700°C and a sintering time of 1.5h. Then, based on the primary sintering, performing secondary sintering, with the sintering temperature increased to 900°C and the sintering time of 3h. Through the sintering process, the powder particles in the alloy body undergo solid phase reaction and diffusion to form a dense alloy structure;

[0115] Step S4, subsequent processing and detection:

[0116] S4.1. Cooling: taking the sintered hydrogen storage alloy material out of the hot pressing sintering furnace and cooling it naturally to room temperature;

[0117] S4.2, Surface treatment: The sintered alloy product is subjected to surface grinding and polishing treatment to remove defects and impurities on the surface of the product, and then the surface of the alloy is cleaned with anhydrous ethanol to remove residues, and then dried again to improve its surface finish and corrosion resistance;

[0118] S4.3, Quality testing: Perform performance testing on the prepared hydrogen storage alloy materials, including hydrogen storage capacity, cycle stability, mass transfer and heat transfer performance indicators, to ensure that they meet relevant standards and requirements;

[0119] S4.4. Packaging and storage: Qualified hydrogen storage alloy products shall be packaged, marked with product information and production date, and then stored in designated warehouses to ensure that the storage environment meets the requirements and avoid fire and corrosion hazards.

[0120] In step S1 of this embodiment, calculated by mass percentage, Ti: 50%, Zr: 10%, Mn: 40%, Cr: 10%, V4Fe: 20% and rare earth elements: 0.3%.

[0121] In step S1 of this embodiment, the raw materials may be cleaned by water washing, acid washing or ultrasonic cleaning.

[0122] Washing in this embodiment: Place the raw material in a cleaning tank, rinse with running water for 15 minutes until there is no obvious contaminant on the surface, then rinse with deionized water at 45°C, and finally blow dry with nitrogen or dry air;

[0123] Pickling: slowly add the raw materials into a 10% dilute hydrochloric acid solution, control the temperature at 45°C, react for 27 minutes, and stir to ensure uniform contact. After the reaction, rinse with deionized water and blow dry with nitrogen or dry air.

[0124] Ultrasonic cleaning: Place the raw materials in an ultrasonic cleaning machine, add an appropriate amount of cleaning liquid, turn on the ultrasonic generator for cleaning, the ultrasonic frequency is between 30kHz, and the cleaning is carried out for 27 minutes. After cleaning, rinse with deionized water and then blow dry with nitrogen or dry air.

[0125] In step S2 of this embodiment, the concentration of anhydrous ethanol is ≥99.5%, the speed of the ball mill is 200 rpm, and the ball milling time is 3 h.

[0126] Embodiment 4:

[0127] A process for preparing an environmentally friendly, low-energy consumption hydrogen storage alloy material comprises the following steps:

[0128] Step S1, raw material selection and pretreatment:

[0129] S1.1, Raw material selection: According to the design requirements of the alloy, select high-purity, environmentally friendly alloy raw materials, including Ti, Zr, Mn, Cr, V4Fe and rare earth elements;

[0130] S1.2, Pretreatment: Strictly screen the selected raw materials to remove impurities and unqualified particles, and then clean them to ensure that the surface of the raw materials is clean and pollution-free;

[0131] Step S2, wet ball milling mixing:

[0132] S2.1. Weigh the raw materials: weigh various raw materials according to the formula ratio;

[0133] S2.2, wet ball milling: the weighed raw materials are placed in a nylon ball mill, and anhydrous ethanol is added as a solvent. At the same time, zirconium oxide grinding balls are added to assist the mixing and refining process. The wet ball milling is carried out in the ball mill. Through the collision and shearing action of the grinding balls, the raw materials are fully mixed and refined into uniform and fine powders;

[0134] S2.3, Vacuum treatment: During the ball milling process, the ball mill is vacuumed to reduce the impact of oxygen and other impurities on the raw materials. The vacuum degree is ≤10Pa to ensure the purity of the mixing environment;

[0135] Step S3, drying and molding:

[0136] S3.1, drying treatment: the mixed raw material powder after wet ball milling is taken out from the ball mill, placed in a vacuum oven, and dried at 80°C to remove the residual anhydrous ethanol solvent for 2.5 hours;

[0137] S3.2, molding: fill the mold with the dried mixed raw material powder to ensure that the powder is evenly distributed and compacted;

[0138] S3.3, sintering: placing the formed alloy body in a hot pressing sintering furnace, and performing primary sintering at a vacuum of less than 10^-3Pa, with a sintering temperature of 650°C and a sintering time of 1.2h. Then, based on the primary sintering, performing secondary sintering, with the sintering temperature increased to 850°C and the sintering time of 2.5h. Through the sintering process, the powder particles in the alloy body undergo solid phase reaction and diffusion to form a dense alloy structure;

[0139] Step S4, subsequent processing and detection:

[0140] S4.1. Cooling: taking the sintered hydrogen storage alloy material out of the hot pressing sintering furnace and cooling it naturally to room temperature;

[0141] S4.2, Surface treatment: The sintered alloy product is subjected to surface grinding and polishing treatment to remove defects and impurities on the surface of the product, and then the surface of the alloy is cleaned with anhydrous ethanol to remove residues, and then dried again to improve its surface finish and corrosion resistance;

[0142] S4.3, Quality testing: Perform performance testing on the prepared hydrogen storage alloy materials, including hydrogen storage capacity, cycle stability, mass transfer and heat transfer performance indicators, to ensure that they meet relevant standards and requirements;

[0143] S4.4. Packaging and storage: Qualified hydrogen storage alloy products shall be packaged, marked with product information and production date, and then stored in designated warehouses to ensure that the storage environment meets the requirements and avoid fire and corrosion hazards.

[0144] In step S1 of this embodiment, calculated by mass percentage, Ti: 45%, Zr: 8%, Mn: 38%, Cr: 8%, V4Fe: 17% and rare earth elements: 0.2%.

[0145] In step S1 of this embodiment, the raw materials may be cleaned by water washing, acid washing or ultrasonic cleaning.

[0146] Washing in this embodiment: Place the raw material in a cleaning tank, rinse with running water for 12 minutes until there is no obvious contaminant on the surface, then rinse with deionized water at 40°C, and finally blow dry with nitrogen or dry air;

[0147] Pickling: slowly add the raw materials into a dilute hydrochloric acid solution with a concentration of 5%-15%, control the temperature between 40°C, react for 20 minutes, and stir to ensure uniform contact. After the reaction, rinse with deionized water and then blow dry with nitrogen or dry air;

[0148] Ultrasonic cleaning: Place the raw materials in an ultrasonic cleaning machine, add an appropriate amount of cleaning liquid, turn on the ultrasonic generator for cleaning, the ultrasonic frequency is between 25kHz, and the cleaning is for 20 minutes. After cleaning, rinse with deionized water and then blow dry with nitrogen or dry air.

[0149] In step S2 of this embodiment, the concentration of anhydrous ethanol is ≥99.5%, the speed of the ball mill is 150 rpm, and the ball milling time is 2.5 h.

[0150] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.

[0151] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A process for preparing an environmentally friendly, low-energy consumption hydrogen storage alloy material, characterized in that: The following steps are involved: Step S1, raw material selection and pretreatment: S1.1, Raw material selection: According to the design requirements of the alloy, select high-purity, environmentally friendly alloy raw materials, including Ti, Zr, Mn, Cr, V4Fe and rare earth elements; S1.2, Pretreatment: Strictly screen the selected raw materials to remove impurities and unqualified particles, and then clean them to ensure that the surface of the raw materials is clean and pollution-free; Step S2, wet ball milling mixing: S2.

1. Weigh the raw materials: weigh various raw materials according to the formula ratio; S2.2, wet ball milling: the weighed raw materials are placed in a nylon ball mill, and anhydrous ethanol is added as a solvent. At the same time, zirconium oxide grinding balls are added to assist the mixing and refining process. The wet ball milling is carried out in the ball mill. Through the collision and shearing action of the grinding balls, the raw materials are fully mixed and refined into uniform and fine powders; S2.3, Vacuum treatment: During the ball milling process, the ball mill is vacuumed to reduce the impact of oxygen and other impurities on the raw materials. The vacuum degree is ≤10Pa to ensure the purity of the mixing environment; Step S3, drying and molding: S3.1, drying treatment: the mixed raw material powder after wet ball milling is taken out from the ball mill, placed in a vacuum oven, and dried at a temperature of 60-120°C to remove the residual anhydrous ethanol solvent for 2-4 hours; S3.2, molding: fill the mold with the dried mixed raw material powder to ensure that the powder is evenly distributed and compacted; S3.3, sintering: placing the formed alloy body in a hot pressing sintering furnace, and performing primary sintering in an environment with a vacuum degree lower than 10^-3Pa, the sintering temperature is 600-800℃, and the sintering time is 1-2h, and then, based on the primary sintering, secondary sintering is performed, the sintering temperature is increased to 800-1000℃, and the sintering time is 2-4h. Through the sintering process, the powder particles in the alloy body undergo solid phase reaction and diffusion to form a dense alloy structure; Step S4, subsequent processing and detection: S4.

1. Cooling: taking the sintered hydrogen storage alloy material out of the hot pressing sintering furnace and cooling it naturally to room temperature; S4.2, Surface treatment: The sintered alloy product is subjected to surface grinding and polishing treatment to remove defects and impurities on the surface of the product, and then the surface of the alloy is cleaned with anhydrous ethanol to remove residues, and then dried again to improve its surface finish and corrosion resistance; S4.3, Quality testing: Perform performance testing on the prepared hydrogen storage alloy materials, including hydrogen storage capacity, cycle stability, mass transfer and heat transfer performance indicators, to ensure that they meet relevant standards and requirements; S4.

4. Packaging and storage: Qualified hydrogen storage alloy products shall be packaged, marked with product information and production date, and then stored in designated warehouses to ensure that the storage environment meets the requirements and avoid fire and corrosion hazards.

2. The process for preparing an environmentally friendly, low-energy consumption hydrogen storage alloy material according to claim 1, characterized in that: In step S1, calculated by mass percentage, Among them, Ti: 40%-60%, Zr: 5%-15%, Mn: 30%-50%, Cr: 5%-15%, V4Fe: 10%-30% and rare earth elements: 0.1%-0.5%.

3. The process for preparing an environmentally friendly, low-energy-consumption hydrogen storage alloy material according to claim 1, characterized in that: In step S1, the raw material can be cleaned by water washing, acid washing or ultrasonic cleaning.

4. The process for preparing an environmentally friendly, low-energy consumption hydrogen storage alloy material according to claim 3, characterized in that: Water washing: Place the raw material in a cleaning tank and rinse with running water for 10-20 minutes until there is no obvious contaminant on the surface, then rinse with deionized water at 30-60°C, and finally blow dry with nitrogen or dry air; Pickling: slowly add the raw materials into a dilute hydrochloric acid solution with a concentration of 5%-15%, control the temperature between 30-60℃, react for 5-30min, and stir to ensure uniform contact. After the reaction, rinse with deionized water and blow dry with nitrogen or dry air. Ultrasonic cleaning: Place the raw materials in an ultrasonic cleaning machine, add an appropriate amount of cleaning liquid, turn on the ultrasonic generator for cleaning, the ultrasonic frequency is between 20-40kHz, and the cleaning time is 5-30 minutes. After cleaning, rinse with deionized water and then blow dry with nitrogen or dry air.

5. The process for preparing an environmentally friendly, low-energy-consumption hydrogen storage alloy material according to claim 1, characterized in that: In step S2, the concentration of anhydrous ethanol is ≥99.5%, the speed of the ball mill is 100-300 rpm, and the ball milling time is 2-4 h.