Method for reducing dehydrogenation sintering of high-purity titanium powder

Abstract

The invention discloses a method for reducing dehydrogenation sintering of high-purity titanium powder, which comprises the following steps: at the temperature of 500-700 DEG C and the vacuum degree of more than 0.1 Pa, moving titanium hydride powder upwards to the top and falling through a spiral stirring mechanism which is longitudinally arranged in a vertical dehydrogenation furnace until dehydrogenation is finished, and continuously carrying the titanium hydride powder upwards through the spiral stirring mechanism, and after reaching the top, the titanium hydride particles freely fall, the titanium hydride particles are always in a dynamic movement process to form dynamic dehydrogenation, the adhesion phenomenon among the titanium hydride particles in the process is reduced, the sintering agglomeration phenomenon is greatly reduced, and the yield of the titanium powder is greatly improved.

Description

Technical Field

[0001] The present invention relates to the field of material technology, and in particular to a method for reducing dehydrogenation sintering of high-purity titanium powder. Background Art

[0002] High-purity titanium powder refers to a group of titanium particles with a purity of ≥99.99%. It can be divided into spherical and non-spherical powders according to its particle shape. It is currently mainly used in the development of high-tech industries such as very large-scale integrated circuits, powder metallurgy, and 3D printing.

[0003] Hydrodehydrogenation (HDH) is a process for preparing titanium powder by utilizing the reversible properties of titanium and hydrogen. Titanium absorbs hydrogen to form brittle titanium hydride, which is then mechanically crushed to produce titanium hydride powder. This is then dehydrogenated in a high-temperature vacuum environment and mechanically crushed to produce titanium powder.

[0004] However, titanium hydride powder is prone to sintering into agglomerates due to particle adhesion during the dehydrogenation process. This phenomenon causes the yield of titanium powder prepared by the conventional static dehydrogenation process to be less than 30%, which needs to be improved. Summary of the Invention

[0005] To solve at least one of the above technical deficiencies, the present invention provides the following technical solutions:

[0006] This application document discloses a method for reducing the dehydrogenation sintering of high-purity titanium powder. At a temperature of 500-700°C and a vacuum degree of more than 0.1 Pa, a spiral stirring mechanism arranged longitudinally in a vertical dehydrogenation furnace is used to move the hydride titanium powder upward to the top and then drop it down, continuing until the dehydrogenation is completed.

[0007] The titanium hydride powder is continuously transported upward by a spiral stirring mechanism, and falls freely after reaching the top. The titanium hydride particles are always in a dynamic motion process, forming dynamic dehydrogenation. In this process, the adhesion between the titanium hydride particles is reduced, and the sintering into agglomerates is greatly reduced.

[0008] Furthermore, the distance between the side of the spiral blade in the spiral stirring mechanism and the wall of the dehydrogenation furnace is less than 2 cm, which can more fully transport the titanium hydride powder in the furnace, thereby putting more titanium hydride powder in a dynamic process.

[0009] Furthermore, the distance between the side of the spiral blade in the spiral stirring mechanism and the wall of the dehydrogenation furnace is 1±0.2 cm.

[0010] Furthermore, the rotation speed of the spiral stirring mechanism is 10-30 r / min, and within this rotation speed limit, more titanium hydride powder is in a dynamic process.

[0011] Furthermore, the rotation speed of the spiral stirring mechanism is 20 r / min.

[0012] Furthermore, the ratio of the longitudinal extension height of the spiral blades in the spiral stirring mechanism to the height of the dehydrogenation furnace chamber is 1:1.2-1.5, which helps to reduce the sintering agglomeration phenomenon.

[0013] Compared with the prior art, the present invention has the following beneficial effects:

[0014] 1. The present invention converts conventional static dehydrogenation into dynamic dehydrogenation through a bolt stirring mechanism. The effect brought about by this accidental conversion far exceeds expectations. According to calculations, the yield rate of titanium powder is increased from the conventional 15-30% to 70-90%. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. 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 these drawings without creative work.

[0016] Figure 1 This is a schematic diagram of the placement structure of the spiral stirring mechanism in the vertical dehydrogenation furnace in Example 1;

[0017] Figure 2 This is a physical picture of the titanium powder sintered into agglomerates in Comparative Example 1;

[0018] Figure 3 This is a physical picture of the titanium powder sintered into agglomerates in Comparative Example 2;

[0019] Wherein, the accompanying drawings are marked as follows:

[0020] 1. Dehydrogenation furnace; 2. Spiral stirring mechanism; 21. Spiral blade; d: distance between the side of the spiral blade and the wall of the dehydrogenation furnace chamber. DETAILED DESCRIPTION

[0021] The present invention will be further described below with reference to the accompanying drawings and specific embodiments.

[0022] like Figure 1 As shown, a spiral stirring mechanism is installed in the vertical dehydrogenation furnace along the longitudinal direction. The spiral stirring mechanism can be selected from the market according to demand. In this example, the spiral stirring mechanism is demonstrated using a common configuration as an example. For example, a spiral blade extending axially spirally is installed on the rotating shaft. The distance d between the side of the spiral blade and the corresponding dehydrogenation furnace chamber wall should be less than 2 cm, and the ratio of the longitudinal extension height of the spiral blade to the height inside the dehydrogenation furnace chamber is 1:1.2-1.5.

[0023] Example 1

[0024] In this example, a method for reducing the dehydrogenation sintering of high-purity titanium powder is used. Figure 1In the vertical dehydrogenation furnace shown in , the distance between the side of the spiral blade and the corresponding dehydrogenation furnace chamber wall is 1 cm, and the ratio of the longitudinal extension height of the spiral blade to the height of the dehydrogenation furnace chamber is 1:1.2.

[0025] Titanium hydride powder was added into the dehydrogenation furnace, the temperature in the dehydrogenation furnace was raised to 500°C, the vacuum degree was 0.1 Pa, and the spiral stirring mechanism was started to move the titanium hydride powder upward to the top and drop it down at a speed of 20 r / min, which continued until the dehydrogenation was completed, which took 3 hours.

[0026] Example 2

[0027] Compared with Example 1, the difference is that in this example, the distance d between the side of the spiral blade and the corresponding dehydrogenation furnace chamber wall is 1.2 cm, and the ratio of the longitudinal extension height of the spiral blade to the height of the dehydrogenation furnace chamber is 1:1.3.

[0028] Example 3

[0029] Compared with Example 1, the difference is that in this example, the temperature in the dehydrogenation furnace is raised to 620° C. and the vacuum degree is 0.5 Pa.

[0030] Example 4

[0031] Compared with Example 1, the difference is that in this example, the temperature in the dehydrogenation furnace is raised to 700° C. and the vacuum degree is 0.8 Pa.

[0032] Comparative Example 1

[0033] Compared with Example 1, the difference is that in this example, the distance d between the side of the spiral blade and the corresponding dehydrogenation furnace chamber wall is 5 cm.

[0034] Comparative Example 2

[0035] Compared with Example 1, the difference is that there is no spiral stirring mechanism in this example.

[0036] The above dehydrogenated product was mechanically crushed to prepare titanium powder, and then tested. The yield rate is shown in Table 1, where the yield rate refers to the mass ratio between qualified titanium powder and raw material.

[0037] Table 1

[0038] Yield rate (%) Example 1 85.6％ Example 2 85.4％ Example 3 90％ Example 4 85.4％ Comparative Example 1 56.8％ Comparative Example 2 28％

[0039] As can be seen from Table 1, the yield of titanium powder prepared by the dynamic dehydrogenation process is significantly higher than that of the conventional static dehydrogenation process. Figure 2 、 Figure 3 It can be seen that the completely static dehydrogenation process and the spiral stirring mechanism cannot fully put the hydrogenated titanium powder under dynamic conditions. The prepared titanium powder is easily sintered into agglomerates, and the yield of titanium powder is low.

[0040] The above are merely preferred embodiments of the present invention. The scope of protection of the present invention is not limited to the above embodiments. All technical solutions based on the principles of the present invention are within the scope of protection of the present invention. It should be noted that improvements and modifications that do not depart from the principles of the present invention are within the scope of protection of the present invention.

Claims

1. A method for reducing dehydrogenation sintering of high-purity titanium powder, characterized in that: At a temperature of 500-700°C and a vacuum degree of more than 0.1 Pa, the titanium hydride powder is moved upward to the top and falls down through a spiral stirring mechanism arranged longitudinally in the vertical dehydrogenation furnace, and this process continues until the dehydrogenation is completed.

2. The method for reducing dehydrogenation sintering of high-purity titanium powder according to claim 1, characterized in that: The distance between the side of the spiral blade in the spiral stirring mechanism and the wall of the dehydrogenation furnace is less than 2 cm.

3. The method for reducing dehydrogenation sintering of high-purity titanium powder according to claim 2, characterized in that: The distance between the side of the spiral blade in the spiral stirring mechanism and the wall of the dehydrogenation furnace is 1±0.2 cm.

4. The method for reducing dehydrogenation sintering of high-purity titanium powder according to claim 1, wherein: The rotating speed of the spiral stirring mechanism is 10-30 r / min.

5. The method for reducing dehydrogenation sintering of high-purity titanium powder according to claim 4, characterized in that: The rotation speed of the spiral stirring mechanism is 20 r / min.

6. The method for reducing dehydrogenation sintering of high-purity titanium powder according to claim 1, characterized in that: The ratio of the longitudinal extension height of the spiral blades in the spiral stirring mechanism to the height inside the dehydrogenation furnace chamber is 1:1.2-1.5.

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