A Method for Synthesizing Zirconium Nickel Alloy Powder
A method for synthesizing zirconium nickel alloy powder, relating to a method for preparing zirconium nickel alloy powder using self combustion high-temperature synthesis technology, particularly suitable for the synthesis process of Zr30Ni70 alloy powder for fuse materials such as fuses in mining, artillery, missiles, and other products, as well as for getters and hydrogen storage materials in electronic products.
Zr30Ni70 alloy powder, as a new type of hydrogen storage and combustion material, is second only to Zr powder and widely used in military, mining, and electronic products. Zr30Ni70 alloy powder, as a new combustion material to replace Zr powder, is currently the trend of development. This is because pure metal zirconium powder has high activity, poses a fire risk in contact with air, and is also prone to deterioration during storage; Zr30Ni70 alloy, as an excellent hydrogen storage material, also has good research and application development prospects. In recent years, people have been actively engaged in the research of Zr30Ni70 alloy and its alloy powders.
The preparation method of Zr30Ni70 alloy powder was initially using pure metal powder mixing method. The obtained Zr30Ni70 is a non alloyed Zr, Ni mixed powder powder with unstable properties, which is no longer commonly used by people. In the future, people will use powder metallurgy methods to mix and sinter fine nickel powder and zirconium powder, and then produce powder through hydrogenation and dehydrogenation. However, this process has the disadvantages of multiple processes, low efficiency, and poor safety, and the powder is difficult to achieve complete alloying, making it difficult to ensure quality; The atomization method is a new process developed in recent years to prepare Zr30Ni70 alloy powder, which requires complex processes such as melting, atomization, and purification. The existing problems are large component segregation, complex equipment, and high cost; At present, there is still a mechanical alloying method that is only used in the laboratory to synthesize Zr30Ni70 alloy powder. Its high cost, purity, and safety are difficult to ensure, making it difficult to use in production.
The purpose of the present invention is to overcome the shortcomings of the existing technologies and provide a new method for preparing Zr30Ni70 alloy powder with high efficiency, low cost, high stability of the obtained alloy powder, high alloying process, and stable quality.
The purpose of the present invention is achieved through the following technical solutions.
A method for preparing Zr30Ni70 alloy powder, characterized in that the preparation process is as follows: first, -0.074mm Zr powder and -0.074mm Ni powder are mixed in a weight ratio of 30:70, then 10-30% Zr30Ni70 alloy powder is added as a diluent, evenly mixed, pressed into a billet, and then burned and synthesized under a protective atmosphere at a temperature of 600 ℃ -1200 ℃, The porous combustion products obtained are crushed and sieved to obtain the Zr30Ni70 alloy powder of the present invention.
The Zr30Ni70 alloy powder produced by the method of the present invention has low oxygen and impurities, good stability, and high alloying degree. Most of the indicators are superior to the atomization method, greatly reducing the processing cost compared to the atomization powder method, and has high practicality.
The method of the present invention will be further explained by combining examples below.
A method for preparing Zr30Ni70 alloy powder, which first involves mixing -0.074mm Zr powder and Ni powder in a weight ratio of 30:70 and adding 10-30% Zr30Ni70 alloy powder in a high-energy mixer for about 3 hours. Then, it is pressed into a billet under an oil pressure machine (with a pressing pressure of 10kg/cm2), and placed in an Ar, hydrogen gas, or vacuum protected reaction furnace to burn and synthesize (SHS method) at a certain temperature (around 600 ℃ -1200 ℃). After holding for 120 minutes, it is cooled out of the furnace, Obtain porous combustion products. After 2 hours of rough crushing and ball milling with a ball milling ratio of 3:1, the powder is sieved to form the finished product.
High quality Zr30Ni70 alloy powder can be mass-produced using the self-propagating high-temperature synthesis continuous production process. By comparing the performance of Zr30Ni70 alloy powder synthesized by SHS process with other powder methods, it is shown that the performance of the powder fully meets and exceeds the requirements of the US military standard (MIL-11410B), and its purity is better than that of the atomization method. The experiment shows that the powder performance is stable.
| Name | H% | S% | 0% | Fe% | Ca% | Zr% | Ni% | Average particle size um |
| SHS method | 0.046 | <0.005 | 0.15 | 0.08 | 0.02 | 28.88 | 68.12 | 4.5-6.04 |
| Atomization method | 0.13 | 0.006 | 1.27 | 0.025 | 0.02 | 27.01 | 69.18 | 1.99 |
| US military standard | <0.02 | 0.20 | 0.15 | 30+4 | 5.0+3 |
Mix nickel powder with an average particle size of 6.0um and zirconium powder with a Ni/Zr weight ratio of 70:30, then add 25% Zr Ni alloy powder and mix for 3 hours to form a billet (10kg/cm2). Then, place it in a reaction furnace for argon protection, rapidly raise the temperature to 900 ℃ for combustion reaction, and cool it out after 120 minutes to obtain porous combustion products. After 2 hours of rough crushing and ball milling, the powder is sieved to form the finished product. The analyzed product is alloyed and consists of Ni7Zr2 and Ni5Zr.
Example 2
Mix nickel powder with an average particle size of 4.5um and zirconium powder with a Ni/Zr weight ratio of 70:30, then add 30% Zr Ni alloy powder and mix for 3 hours. Press it into a billet (10kg/cm2), and then place it in a vacuum reaction furnace and vacuum it to 1 × After 10-2Pa, rapidly raise the temperature to 600 ℃ to cause combustion reaction. After holding for 120 minutes, cool the furnace and obtain porous combustion products. After being roughly crushed and ball milled for 2 hours, the powder is sieved and the finished product is analyzed
Alloying, consisting of Ni7Zr2 and Ni5Zr.
Example 3
Mix nickel powder with an average particle size of 10.6um and zirconium powder with a Ni/Zr weight ratio of 70:30, then add 10% Zr Ni alloy powder and mix for 3 hours to form a billet (10kg/cm2). Then, place it in a reaction furnace for hydrogen protection, rapidly raise the temperature to 900 ℃ for combustion reaction, and cool it out after 120 minutes to obtain porous combustion products. After rough crushing and ball milling for 2 hours (ball to material ratio of 3:1), the powder is sieved, and then the synthesized powder is dehydrogenated in a vacuum furnace at 650 ℃ for about 6 hours to achieve a vacuum degree greater than 1 × 10-2Pa, the product is ball milled for 40 minutes (material to ball ratio of 3:1), and then sieved to obtain the finished product.