High-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder

Abstract

The invention belongs to the technical field of powder metallurgy, and particularly relates to a high-energy ball-milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder, which comprises the following steps of: pouring raw material molybdenum powder into a high-energy ball-milling tank, and performing high-energy ball-milling micro-oxidation in the high-energy ball-milling tank; the molybdenum powder subjected to micro-oxidation treatment is added into an ammonia water solution to be fully stirred, and precipitates are filtered out after reaction; and the precipitate is cleaned and then dried in a protective atmosphere, and the spherical molybdenum powder is obtained. The method is efficient in overall process and low in cost, and the spherical molybdenum powder obtained through the method is high in sphericity, good in fluidity and high in purity. The method can be used for producing the spherical molybdenum powder with various particle sizes, the sphericity and fluidity of the molybdenum powder are greatly improved through targeted regulation and control of technological parameters, and the method has wide application prospects.

Description

Technical Field

[0001] The invention relates to the technical field of powder metallurgy, in particular to a high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder. Background Art

[0002] Metallic molybdenum is a strategically important refractory rare metal with high temperature strength and hardness, high melting point, good electrical and thermal conductivity, small expansion coefficient, excellent thermal shock resistance and thermal fatigue resistance. Spherical molybdenum powder has high fluidity and high bulk density, and is widely used in 3D printing, thermal spraying, surfacing, contact material preparation, powder metallurgy and other fields. The preparation methods of spherical molybdenum powder include rotating electrode method, spray granulation method, plasma spheroidization method and the like. Among them, the plasma spheroidization method and the rotating electrode method for preparing spherical powder have complex equipment and high energy consumption, while the spherical molybdenum powder prepared by the spray granulation method has the disadvantages of high oxygen content, large powder particle size and wide particle size distribution range. With the development of technology, spherical molybdenum powder needs to better meet the requirements of high sphericity, high purity, high fluidity, high tap density, high dispersibility, low energy consumption and low cost. Therefore, it is imperative to seek the most optimized equipment and method for preparing spherical molybdenum powder. Summary of the invention

[0003] In order to solve the problems existing in the prior art, the main purpose of the present invention is to propose a high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder.

[0004] To solve the above technical problems, according to one aspect of the present invention, the present invention provides the following technical solutions:

[0005] A high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder comprises the following steps:

[0006] S1, pouring raw molybdenum powder into a high-energy ball mill, and performing high-energy ball milling micro-oxidation in the ball mill;

[0007] S2, adding the molybdenum powder that has been subjected to micro-oxidation treatment into an ammonia solution and stirring for 1 to 60 minutes, and filtering out the precipitate after the reaction;

[0008] S3, washing the precipitate, and then drying it under a protective atmosphere to obtain spherical molybdenum powder.

[0009] As a preferred embodiment of the high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder described in the present invention, wherein: in the step S1, the raw material molybdenum powder is molybdenum powder with irregular morphology.

[0010] As a preferred embodiment of the high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder described in the present invention, wherein: in the step S1, oxygen or air is filled into the ball milling tank.

[0011] As a preferred embodiment of the high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder described in the present invention, wherein: in the step S1, the micro-oxidation time is 1 to 300 minutes.

[0012] As a preferred embodiment of the high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder described in the present invention, wherein: in the step S2, the concentration of the ammonia solution is 1 to 28 wt%.

[0013] As a preferred embodiment of the high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder described in the present invention, wherein: in the step S2, the solution temperature during the stirring process is 20-100°C.

[0014] As a preferred embodiment of the high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder described in the present invention, wherein: in the step S3, the precipitate is washed with deionized water or alcohol.

[0015] As a preferred embodiment of the high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder described in the present invention, wherein: in the step S3, the drying temperature is 20-100°C.

[0016] As a preferred embodiment of the high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder described in the present invention, wherein: in the step S3, the protective atmosphere is one of argon, hydrogen and nitrogen.

[0017] To solve the above technical problem, according to another aspect of the present invention, the present invention provides the following technical solution:

[0018] A spherical molybdenum powder prepared by the high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder.

[0019] The beneficial effects of the present invention are as follows:

[0020] The present invention proposes a high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder, which comprises pouring raw molybdenum powder into a high-energy ball milling tank, and performing high-energy ball milling micro-oxidation in the ball milling tank; adding the molybdenum powder treated with micro-oxidation into an ammonia solution and stirring it fully, filtering out the precipitate after the reaction; washing the precipitate, and then drying it under a protective atmosphere to obtain spherical molybdenum powder. The overall process of the method of the present invention is efficient and low in cost, and the spherical molybdenum powder obtained by the method of the present invention has high sphericity, good fluidity and high purity. The present invention can be used to produce spherical molybdenum powders of various particle sizes, and the sphericity and fluidity of the molybdenum powder are greatly improved through targeted regulation of process parameters, and has broad application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the structures shown in these drawings without paying creative work.

[0022] Figure 1 This is a scanning electron microscope photograph of the spherical molybdenum powder prepared in Example 1 of the present invention.

[0023] Figure 2 This is a scanning electron microscope photograph of the molybdenum powder prepared in Comparative Example 1 of the present invention.

[0024] The realization of the purpose, functional features and advantages of the present invention will be further explained in conjunction with embodiments and with reference to the accompanying drawings. DETAILED DESCRIPTION

[0025] The following will be described clearly and completely in conjunction with the technical solutions in the embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0026] The main purpose of the present invention is to propose a high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder. Irregular molybdenum powder is placed in a high-energy ball mill for surface oxidation treatment. The purpose is to grind and oxidize the edges and corners of the irregular molybdenum powder. High-energy ball milling has a shaping effect on irregular molybdenum powder from a mechanical point of view. The heat in the process is used to micro-oxidize the molybdenum powder in an air or oxygen environment. The molybdenum powder after micro-oxidation is then immersed in an ammonia solution for ammonia stripping treatment. The overall process is efficient and low-cost. The high-energy ball milling micro-oxidation-ammonia stripping method of the present invention prepares spherical molybdenum powder. High-energy ball milling micro-oxidation not only ensures the overall uniformity of powder micro-oxidation, so that each edge and corner of the irregular molybdenum powder is uniformly oxidized, and the accompanying mechanical grinding further enhances the sphericity and fluidity of the spherical molybdenum powder finally obtained. The whole process is simple to operate and is conducive to mass production and processing.

[0027] The technical solution of the present invention is further described below in conjunction with specific embodiments.

[0028] Example 1

[0029] A method for preparing spherical molybdenum powder comprises the following steps: screening the initial raw material molybdenum powder, pouring the raw material molybdenum powder with an irregular morphology and an average particle size of 5 μm after screening into a high-energy ball mill, filling the ball mill with oxygen, and setting the high-energy ball milling micro-oxidation time to 20 minutes. The molybdenum powder that has been subjected to micro-oxidation treatment is added to an ammonia solution with a concentration of 26 wt%, and stirred for 10 minutes at a temperature of 20°C. After the reaction, the precipitate is filtered out. The precipitate after ammonia stripping is washed with deionized water, and the washed powder is dried at 80°C under argon protection to finally obtain spherical molybdenum powder, and its scanning electron microscope photograph is shown as follows: Figure 1 As shown, it can be seen that the spherical molybdenum powder obtained by the present invention has high sphericity, good fluidity and high purity.

[0030] Example 2

[0031] A method for preparing spherical molybdenum powder comprises the following steps: screening the initial raw material molybdenum powder, pouring the raw material molybdenum powder with an irregular morphology and an average particle size of 5 μm after screening into a high-energy ball mill, filling the ball mill with oxygen, and setting the high-energy ball milling micro-oxidation time to 30 minutes. The molybdenum powder treated with micro-oxidation is added into an ammonia solution with a concentration of 26 wt%, fully stirred at a temperature of 20° C. for 10 minutes, and filtering out the precipitate after the reaction. The precipitate after ammonia stripping is washed with deionized water, and the washed powder is dried at 80° C. under argon protection to finally obtain spherical molybdenum powder.

[0032] Example 3

[0033] A method for preparing spherical molybdenum powder comprises the following steps: screening the initial raw material molybdenum powder, pouring the raw material molybdenum powder with an irregular morphology and an average particle size of 10 μm after screening into a high-energy ball mill, filling the ball mill with air, and setting the high-energy ball milling micro-oxidation time to 30 minutes. The molybdenum powder treated with micro-oxidation is added into an ammonia solution with a concentration of 26 wt%, fully stirred at a temperature of 50° C. for 10 minutes, and filtering out the precipitate after the reaction. The precipitate after ammonia stripping is washed with deionized water, and the washed powder is dried at 80° C. under argon protection to finally obtain spherical molybdenum powder.

[0034] Example 4

[0035] A method for preparing spherical molybdenum powder comprises the following steps: screening the initial raw material molybdenum powder, pouring the raw material molybdenum powder with an irregular morphology and an average particle size of 10 μm after screening into a high-energy ball mill, filling the ball mill with air, and setting the high-energy ball milling micro-oxidation time to 30 minutes. The molybdenum powder treated with micro-oxidation is added into an ammonia solution with a concentration of 26 wt%, fully stirred at a temperature of 60° C. for 10 minutes, and filtering out the precipitate after the reaction. The precipitate after ammonia stripping is washed with deionized water, and the washed powder is dried at 80° C. under argon protection to finally obtain spherical molybdenum powder.

[0036] Example 5

[0037] A method for preparing spherical molybdenum powder comprises the following steps: screening the initial raw material molybdenum powder, pouring the raw material molybdenum powder with an irregular morphology and an average particle size of 15 μm after screening into a high-energy ball mill, filling the ball mill with oxygen, and setting the high-energy ball milling micro-oxidation time to 10 minutes. The molybdenum powder treated with micro-oxidation is added into an ammonia solution with a concentration of 15 wt%, fully stirred at a temperature of 60° C. for 20 minutes, and filtering out the precipitate after the reaction. The precipitate after ammonia stripping is washed with deionized water, and the washed powder is dried at 80° C. under argon protection to finally obtain spherical molybdenum powder.

[0038] Comparative Example 1

[0039] A method for preparing molybdenum powder comprises screening the initial raw material molybdenum powder, adding the raw material molybdenum powder with an average particle size of 5 μm after screening and irregular morphology to an ammonia solution with a concentration of 26 wt%, stirring the mixture for 10 minutes at a temperature of 20°C, filtering out the precipitate after the reaction, washing the precipitate after ammonia stripping with deionized water, drying the washed powder at 80°C under argon protection, and finally obtaining a molybdenum powder such as Figure 2 As shown, the molybdenum powder has obvious edges and corners, and has no obvious change compared with the raw material molybdenum powder.

[0040] The present invention pours raw molybdenum powder into a high-energy ball mill, and performs high-energy ball milling micro-oxidation in the ball mill; adds the molybdenum powder treated with micro-oxidation into an ammonia solution and stirs it thoroughly, and filters out the precipitate after the reaction; washes the precipitate, and then dries it under a protective atmosphere to obtain spherical molybdenum powder. The overall process of the method of the present invention is efficient and low in cost. The spherical molybdenum powder obtained by the method of the present invention has high sphericity, good fluidity and high purity. The present invention can be used to produce spherical molybdenum powders of various particle sizes. Through targeted regulation of process parameters, the sphericity and fluidity of the molybdenum powder are greatly improved, and it has broad application prospects.

[0041] The above description is only a preferred embodiment of the present invention, and does not limit the patent scope of the present invention. All equivalent structural changes made by using the contents of the present invention specification under the inventive concept of the present invention, or direct / indirect application in other related technical fields are included in the patent protection scope of the present invention.

Claims

1. A high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder, characterized in that: The steps include: S1, pouring raw molybdenum powder into a high-energy ball mill, and performing high-energy ball milling micro-oxidation in the ball mill; S2, adding the molybdenum powder that has been subjected to micro-oxidation treatment into an ammonia solution and stirring for 1 to 60 minutes, and filtering out the precipitate after the reaction; S3, washing the precipitate, and then drying it under a protective atmosphere to obtain spherical molybdenum powder.

2. The high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder according to claim 1, characterized in that: In the step S1, the raw material molybdenum powder is molybdenum powder with irregular morphology.

3. The high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder according to claim 1, characterized in that: In the step S1, oxygen or air is filled into the ball mill.

4. The high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder according to claim 1, characterized in that: In the step S1, the micro-oxidation time is 1 to 300 minutes.

5. The high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder according to claim 1, characterized in that: In step S2, the concentration of the ammonia solution is 1-28 wt%.

6. The high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder according to claim 1, characterized in that: In step S2, the solution temperature is 20-100° C. during stirring.

7. The high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder according to claim 1, characterized in that: In step S3, the precipitate is washed with deionized water or alcohol.

8. The high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder according to claim 1, characterized in that: In step S3, the drying temperature is 20-100°C.

9. The high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder according to claim 1, characterized in that: In step S3, the protective atmosphere is one of argon, hydrogen and nitrogen.

10. Spherical molybdenum powder prepared by the high-energy ball milling micro-oxidation-ammonia stripping method for preparing spherical molybdenum powder according to any one of claims 1 to 9.

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