CN-117415314-B - Preparation method of hydrogen storage nano titanium-based composite powder

Abstract

The invention discloses a preparation method of hydrogen storage nano titanium-based composite powder, which comprises the steps of adding ferric trichloride hexahydrate and tetrabutyl titanate into distilled water according to a mass ratio of 1:5-7, stirring to enable the ferric trichloride hexahydrate and the tetrabutyl titanate to be fully dissolved and dispersed, adding absolute ethyl alcohol after uniformly mixing, stirring uniformly, adjusting the pH value of the solution to 8-9, carrying out hydrothermal reaction on the obtained mixture at 120-150 ℃ for 16-20H to obtain a composite powder product, washing the composite powder product with distilled water, filtering the powder product, drying the powder product at 50-60 ℃ for 20-24H after filtering and cleaning for multiple times, placing the dried product into a tubular furnace, sintering the product at 750-800 ℃ for 2-3H under H 2 , reducing the obtained product, and grinding to obtain nano titanium-iron composite powder. The composite powder obtained by the invention has the advantages of irregular shape, small particle size and large specific surface area, improves the hydrogen storage and release amount, and improves the convenience and safety of hydrogen storage and transportation.

Inventors

• YUAN DONGDONG
• CHEN WENGE
• ZHOU CHUANHUA
• WANG JUANHUA

Assignees

• 陕西钛普稀有金属材料有限公司

Dates

Publication Date

20260512

Application Date

20230914

Claims (6)

1. 1. The preparation method of the hydrogen storage nano titanium-based composite powder is characterized by comprising the following steps of: S1, adding ferric trichloride hexahydrate and tetrabutyl titanate into distilled water according to a mass ratio of 1:5-7, stirring to fully dissolve and disperse the ferric trichloride hexahydrate and the tetrabutyl titanate, adding absolute ethyl alcohol after uniformly mixing, uniformly stirring, and then adjusting the pH value of the solution to 8-9; S2, carrying out hydrothermal reaction on the obtained mixture at 120-150 ℃ for 16-20 hours to obtain a composite powder product; s3, washing with distilled water, filtering a powder product, filtering and cleaning for multiple times, and drying at 50-60 ℃ for 20-24 hours; s4, placing the dried product into a tube furnace, sintering for 2-3 hours at a temperature rise rate of between 8 and 10 ℃ per minute at a temperature rise rate of between 750 and 800 ℃ in an H 2 atmosphere, reducing the obtained product, and grinding to obtain nano ferrotitanium composite powder; In the step S1, ammonia water is adopted to adjust the pH value; in the step S4, the ball material volume ratio during grinding is 1:1-1.5, and the charging amount is 40-50% of the grinding tank volume; In the step S4, the grinding time is 15-20 hours, and the rotating speed is 200-300 revolutions per minute.
2. 2. The preparation method of the hydrogen storage nano titanium-based composite powder according to claim 1, wherein in the step S1, absolute ethyl alcohol is added and stirred for 2-3 hours.
3. 3. The method for preparing hydrogen storage nano titanium-based composite powder according to claim 1, wherein in the step S2, the reaction kettle is TC 4 titanium alloy.
4. 4. The method for preparing hydrogen storage nano titanium-based composite powder according to claim 1, wherein in the step S4, a 1Cr18Ni9Ti stainless steel tank is adopted as a grinding tank.
5. 5. The method for preparing hydrogen storage nano titanium-based composite powder according to claim 1, wherein in the step S4, stainless steel balls are adopted as grinding balls.
6. 6. The method for preparing hydrogen storage nano titanium-based composite powder according to claim 1, wherein in S4, grinding is performed under the protection of nitrogen or argon.

Description

Preparation method of hydrogen storage nano titanium-based composite powder Technical Field The invention belongs to the technical field of solid hydrogen storage, and relates to a preparation method of hydrogen storage nano titanium-based composite powder. Background With the aggravation of global greenhouse emission reduction problems, countries around the world are turning to clean low-carbonization energy. Hydrogen energy is one of the most important forms of clean energy and is therefore becoming increasingly important. The hydrogen energy is a secondary energy source which is rich in source, green, low in carbon and wide in application, is the main stream development direction of a new energy system in the 21 st century, and has the characteristic of high combustion heat value, and is 3 times of gasoline, 3.9 times of alcohol and 4.5 times of coke. The hydrogen energy is used as an energy source form with wide application, and can be used as fuel to directly provide energy power for traffic and industry. And because the energy storage device can be used for liquid storage and also can be used as an energy storage device, the energy storage device can be integrated with multiple types of energy sources (renewable energy sources, fossil energy sources and nuclear energy sources), realizes flexible energy storage according to supply and demand relations, and solves the problem of space-time balance of energy supply and demand. Moreover, the hydrogen energy source is used as an important basic raw material for industrial production and industrial decarburization, can be used for preparing products, and can be combined with CO 2 trapped in industrial production to be converted into chemical products. The hydrogen energy source can be said to be a renewable "petroleum" resource. However, hydrogen storage and transportation is a bottleneck problem in the hydrogen energy industry chain of "storage and transportation". At present, the hydrogen is stored in 3 modes of high-pressure gaseous hydrogen storage, liquid hydrogen storage and solid hydrogen storage. In hydrogen storage applications, safe and high density storage is a primary concern, followed by economy and convenience. The solid-state hydrogen storage has the characteristic closest to the primary problem of hydrogen storage in nature, and can provide an important solution for high-density and high-safety storage and transportation of hydrogen energy, and the reasons are that firstly, the volume hydrogen storage density is the highest, and secondly, the hydrogen storage safety is good. Titanium is an important strategic resource and is widely applied to many fields of national defense, aerospace, aviation and national economy, and long-term experimental and industrial production practices prove that titanium and titanium alloy are recognized as materials capable of replacing steel, stainless steel, copper and alloys thereof and ideal metal structural materials for solving the corrosion problem of equipment. Because the chemical property of titanium is very active, hydrogen is stored in gaps, defects or intermetallic compounds in the form of atoms, molecules or hydrides, and the hydrogen is repeatedly absorbed and released under certain conditions, the hydrogen storage amount is 1000-1300 times of the volume of the material, and the hydrogen storage alloy has great potential as a main hydrogen absorption component of the hydrogen storage alloy. Titanium-based hydrogen storage alloys in solid hydrogen storage generally include Ti-Fe, ti-Mn, ti-Cr, ti-Zr, etc., and are mainly represented by AB-type TiFe alloys. The TiFe hydrogen storage alloy has low cost, easy preparation, high hydrogen absorption and desorption speed at room temperature, long cycle life which can reach more than 2000 times, 4 times of the rare earth hydrogen storage alloy, and the cost of raw materials is only one third of the rare earth hydrogen storage alloy. However, a dense TiO 2 layer is easily formed and is difficult to activate, and after activation, the activated TiO 2 layer is easily contacted with impurity gases such as O 2、CO2、H2 O in the air and loses the activity of absorbing and releasing hydrogen. At present, the problems are mainly solved by means of element alloying, surface treatment and the like, and transition elements such as Ni, mn, cr and the like are generally adopted to replace part of Fe in TiFe, so that the activation performance of the alloy is improved. The preparation methods of the titanium-based hydrogen storage alloy are different, so that the difference of the structure, the thermal stability and the hydrogen absorption and desorption of the titanium-based hydrogen storage alloy is larger. The Ti-Fe complex is prepared by vacuum smelting to obtain block, high-energy ball milling to obtain nanometer powder, spinning to obtain film, atomizing to obtain superfine powder, etc. and magnetic suspension smelting to obtain TiFe 0.86Mn0.1-xCox alloy in Haiqin Qu