A high-temperature shaping and purification integrated production equipment and process for metal powder

Abstract

The present invention discloses an integrated production equipment and process for high-temperature shaping and purification of metal powders. The integrated production equipment for high-temperature shaping and purification of metal powders includes: a furnace body; a first support seat provided on one side of the furnace body; a second support seat provided on the other side of the furnace body; a working container provided inside the furnace body, with a first rotating support pipe and a second rotating support pipe that extend out of the furnace body and are coaxial at both ends. The first rotating support pipe is supported by the first support seat, and the second rotating support pipe is supported by the second support seat; a vacuum pumping device for pumping the working container into a vacuum; a gas filling device for filling the working container with the required gas; and a driving mechanism for driving the working container to rotate around the axis of the first rotating support pipe. The present invention integrates the five steps of hydrogenation, crushing, dehydrogenation, shaping, and purification, reduces the operation steps, improves the efficiency, and has good effects on the crushing and spheroidization of metal powders, improving the utilization rate of titanium metal.

Description

Technical Field

[0001] The present invention relates to a processing device for metals, and particularly to an integrated production device and process for high-temperature shaping and purification of metal powders. Background Art

[0002] Powder metallurgy forming processes such as 3D printing and injection molding are widely used. The powder metallurgy process has relatively high requirements for the properties of titanium powder raw materials. In addition to particle size and its composition and oxygen content properties, particularly high requirements are put forward for the powder fluidity. For example, titanium metal, due to its low density, good corrosion resistance, high specific strength, and excellent biocompatibility, is widely used in fields such as aerospace, petrochemical, energy, and biomedical applications. The powder metallurgy process has relatively high requirements for the properties of titanium powder raw materials. In addition to particle size and its composition and oxygen content properties, particularly high requirements are put forward for the powder fluidity. Because the powder fluidity directly affects the powder forming quality, therefore, powder metallurgy processes such as 3D printing and injection molding usually use spherical titanium powder with better powder fluidity as raw materials. At present, methods for preparing titanium metal powder with high quality and low cost include electrode vacuum induction gas atomization, rotating electrode vacuum gas atomization, and plasma vacuum gas atomization. The fine powder yield in the production process is generally low (usually the fine powder yield is below 40%), leaving a large number of titanium metal coarse particles useless, resulting in serious waste of resources; the reuse rate of a large amount of titanium chips left by mechanical processing of titanium metal is also low, causing serious waste. Summary of the Invention

[0003] The present invention aims to at least solve one of the technical problems existing in the prior art. For this purpose, the present invention provides an integrated production device for high-temperature shaping and purification of metal powders, which integrates multiple steps and improves the fine powder yield.

[0004] The integrated production device for high-temperature shaping and purification of metal powders according to the first aspect embodiment of the present invention includes: a furnace body; a first support seat provided on one side of the furnace body; a second support seat provided on the other side of the furnace body; a working container provided inside the furnace body, with a first rotating support tube and a second rotating support tube that extend out of the furnace body and are coaxial at both ends. The first rotating support tube is supported by the first support seat, and the second rotating support tube is supported by the second support seat; a vacuum pumping device for pumping vacuum in the working container; a gas filling device for filling the working container with the required gas; and a driving mechanism for driving the working container to rotate around the axis of the first rotating support tube.

[0005] The high-temperature shaping and purification integrated production equipment for metal powder according to the embodiments of the present invention has at least the following beneficial effects: The gas charging device can charge hydrogen, and under the action of the high-temperature furnace body, hydrogenation is realized; the working container rotates to drive the kinetic energy carrier in the working container to crush titanium metal; then dehydrogenation of titanium metal is realized by means of vacuum pumping and high-temperature treatment; and the continuous rotation of the working container can remove the sharp corners and edges on the surface of the metal powder, gradually forming a spherical or quasi-spherical effect, while discharging the gas impurities separated at high temperature, achieving the effects of spheroidization and purification, integrating the five steps of hydrogenation, crushing, dehydrogenation, shaping and purification, reducing the operation steps and improving the efficiency; the crushing and spheroidization effects of the metal powder are good, improving the utilization rate of titanium metal.

[0006] According to some embodiments of the present invention, the gas charging device is connected to the first rotating support pipe through a first rotating joint.

[0007] According to some embodiments of the present invention, the first rotating joint is connected to the first rotating support pipe through a sealing valve.

[0008] According to some embodiments of the present invention, the first rotating joint is provided with a first movable flange, the sealing valve is provided with a second movable flange, and the first movable flange and the second movable flange are provided with corresponding holes for connection and fixation by bolts.

[0009] According to some embodiments of the present invention, the vacuum pumping device is connected to the second rotating support pipe, and a second rotating joint and a first filtering device are sequentially arranged between the two.

[0010] According to some embodiments of the present invention, a turning frame is hinged to the upper end of the first support seat. The turning frame is provided with a limiting through hole. The first rotating support pipe passes through the limiting through hole and is axially fixed to the turning frame. The upper end of the furnace body is openable; after the upper end of the furnace body is opened, the working container can be turned over along with the turning frame.

[0011] According to some embodiments of the present invention, the driving mechanism is a motor installed on the turning frame. A transmission sleeve is sleeved on the outer periphery of the first rotating support pipe. The motor is in transmission connection with the transmission sleeve to drive the first rotating support pipe and the working container to rotate.

[0012] According to some embodiments of the present invention, a lifting and rotating device is further included. The lifting and rotating device is sleeved on the second rotating support pipe and axially fixed, and the lifting and rotating device can rotate around the second rotating support pipe.

[0013] According to some embodiments of the present invention, the lifting and rotating device includes a lifting frame, a lifting hook, and rollers. The lifting frame is sleeved on the second rotating support pipe. The lifting hook is arranged on the outer periphery of the lifting frame. The rollers are circumferentially arranged on the inner ring of the lifting frame. A track sleeve is fixedly arranged on the peripheral wall of the second rotating support pipe. The track sleeve is provided with an annular track adapted to the rollers, and the rollers can roll along the annular track.

[0014] The high-temperature shaping and purification integrated production process of metal powder according to the embodiments of the first aspect of the present invention includes the following steps:

[0015] S1. After discharging moisture and harmful substances in the working container, load titanium metal raw materials and kinetic carriers into the working container.

[0016] S2. Open the vacuum pumping device to discharge gas impurities in the working container.

[0017] S3. Heat the furnace body to make the temperature in the working container between 250°C and 800°C. The gas charging device fills hydrogen into the working container and keeps the pressure constant between 50 kPa and 400 kPa. The driving mechanism drives the working container to rotate to hydrogenate the titanium metal.

[0018] S4. Adjust the temperature of the working container to between 300°C and 900°C, and introduce inert gas with the pressure constant between 10 kPa and 90 kPa. The rotation of the working container breaks the titanium metal under the impact energy of the movement of the kinetic carrier.

[0019] S5. After opening the vacuum pumping device to pump out the gas in the working container, introduce inert gas to keep the pressure in the working container constant between -500 kPa and 0 kPa, adjust the temperature of the working container to between 500°C and 950°C, and keep the working container rotating to realize hydrogenation and dehydrogenation of the titanium metal.

[0020] S6. Adjust the temperature to between 200°C and 950°C, keep the pressure of the inert gas constant between 1 kPa and 30 kPa, and keep the working container rotating to realize shaping, spheroidization and purification of the titanium metal.

[0021] S7. Seal and discharge the material when the temperature drops below 100°C and the pressure of the inert gas is between 0 kPa and 5 kPa.

[0022] According to some embodiments of the present invention, the metal is one of the metal elements in the sixth period of the periodic table of elements.

[0023] The high-temperature shaping and purification integrated production process of metal powder according to the embodiments of the present invention has at least the following beneficial effects: integrating the four steps of hydrogenation, crushing, dehydrogenation and shaping and purification, reducing the operation steps, improving the efficiency, having good crushing and spheroidization effects on the metal powder, improving the utilization rate of titanium metal, and having low oxygen content and gas impurities.

[0024] Additional aspects and advantages of the present invention will be given in part in the following description, become apparent in part from the following description, or be learned through the practice of the present invention. Brief Description of the Drawings

[0025] The present invention will be further described below in conjunction with the drawings and embodiments, where:

[0026] Figure 1 is a schematic structural diagram of an embodiment of the high-temperature shaping and purification integrated production equipment for metal powder of the present invention;

[0027] Figure 2 is a schematic structural diagram of the lifting and rotating device;

[0028] Figure 3 is Figure 2 the sectional view taken along line A-A of Detailed Embodiments

[0029] Embodiments of the present invention will be described in detail below. Examples of the embodiments are shown in the drawings, where the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the drawings are exemplary only for explaining the present invention and should not be construed as limiting the present invention.

[0030] In the description of the present invention, it should be understood that the orientation or positional relationship indicated by terms such as up and down, etc., is based on the orientation or positional relationship shown in the drawings. This is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention.

[0031] In the description of the present invention, "plural" means more than two. If the first and second are described only for the purpose of distinguishing technical features, they should not be construed as indicating or implying relative importance or implicitly indicating the quantity of the indicated technical features or the sequence of the indicated technical features.

[0032] In the description of the present invention, unless otherwise clearly defined, terms such as "set", "installed", "connected", etc. should be understood in a broad sense. Those skilled in the art can reasonably determine the specific meanings of the above terms in the present invention in combination with the specific content of the technical solution.

[0033] Refer to Figure 1As shown in the figure, an integrated production device for high-temperature shaping and purification of metal powder provided by an embodiment of the present invention includes a furnace body 100, a first support base 200, a second support base 300, a working container 400, a vacuum pumping device 500, a gas filling device 600, and a driving mechanism 700. It is used to make coarse metal particles into fine spherical metal powder. The metal powder can be one of the transition metal elements in the sixth period of the periodic table of metal elements, such as titanium, tantalum, zirconium, hafnium, etc.

[0034] The furnace body 100 is provided with a heating element 130 inside, which can be electrically heated. The first support base 200 is arranged on one side of the furnace body 100, and the second support base 300 is arranged on the other side of the furnace body 100; the working container 400 is arranged inside the furnace body 100. The two ends of the working container 400 are respectively provided with a first rotating support pipe 410 and a second rotating support pipe 420 that extend out of the furnace body 100 and are coaxial. The first rotating support pipe 410 is supported by the first support base 200, and the second rotating support pipe 420 is supported by the second support base 300. The stable support of the working container 400 is realized through the first support base 200 and the second support base 300. The vacuum pumping device 500 is used to pump vacuum for the working container 400 to discharge or replace the gas inside the working container 400 to meet the process requirements. The gas filling device 600 is used to fill the working container 400 with the required gas. The required gas can be various, and multiple gas sources are set to realize the filling of multiple gases. The driving mechanism 700 is used to drive the working container 400 to rotate around the axis of the first rotating support pipe 410. The working container 400 can tumble titanium metal to achieve uniform processing, and can realize continuous crushing, shaping and spheroidization, improving the utilization rate of titanium metal.

[0035] An integrated production device for high-temperature shaping and purification of metal powder provided by an embodiment of the present invention. The gas filling device 600 can fill hydrogen, and under the action of a high-temperature furnace body, hydrogenation is realized; the rotation of the working container 400 drives the kinetic energy carriers inside the working container 400 to crush titanium metal; then vacuum pumping and high-temperature treatment are used to realize the dehydrogenation of titanium metal; and the continuous rotation of the working container 400 can remove the sharp corners and edges on the surface of the metal powder, gradually forming a spherical or quasi-spherical effect, and at the same time discharging the gas impurities separated at high temperature, achieving the effects of spheroidization and purification. The five steps of hydrogenation, crushing, dehydrogenation, shaping and purification are integrated, reducing the operation steps and improving the efficiency. Moreover, the crushing and spheroidization effects of the metal powder are good, improving the utilization rate of titanium metal. The kinetic energy carriers can be hard spheres, which can be made of metal or non-metal materials, with high temperature resistance, wear resistance, high specific gravity and high hardness, such as alumina balls, zirconia balls, cemented carbide balls, titanium balls, stainless steel balls, or metal balls of one of the metals in the sixth period of the periodic table of elements, etc. They can continuously squeeze, crush and spheroidize titanium metal as the working container 400 rotates. The remaining titanium metal coarse particles in the traditional process of preparing titanium metal powder or the titanium metal chips left by titanium metal machining can be further utilized.

[0036] Referring to Figure 1 , it can be understood that in some embodiments of the present invention, the inflation device 600 is connected to the first rotating support pipe 410 through the first rotary joint 610, so that the rotation of the first rotating support pipe 410 will not drive the inflation device 600 to rotate, avoiding the entanglement of the pipeline.

[0037] It can be understood that in some embodiments of the present invention, the first rotary joint 610 is connected to the first rotating support pipe 410 through the sealing valve 620. When feeding is required, the sealing valve 620 is opened and the connection between the sealing valve 620 and the first rotating support pipe 410 is disassembled. Specifically, the first rotary joint 610 is provided with a first movable flange 611, the sealing valve 620 is provided with a second movable flange 621, and the first movable flange 611 and the second movable flange 621 are provided with corresponding holes for connection and fixation by bolts. The connection and fixation are realized through the flange, which is convenient for installation, firm in connection, and can also be disassembled, facilitating the disassembly of the first rotary joint 610 during feeding. The rotary joint usually has a fixed cylinder and a movable cylinder, and the movable cylinder can rotate relative to the fixed cylinder. The inflation device 600 is usually an air pump, and the air pump is connected to the movable cylinder through a pipeline. The first movable flange 611 is arranged on the movable cylinder, and the movable cylinder is fixedly connected to the sealing valve 620 through the first movable flange 611. The rotary joint belongs to the conventional prior art and will not be elaborated here.

[0038] In addition, in order to prevent the kinetic energy carrier from being discharged due to feeding, the outlet end of the sealing valve 620 is provided with a second filtering device. The second filtering device allows the metal powder with qualified particle size to be discharged, but can prevent the kinetic energy carrier from being discharged, so that the kinetic energy carrier can be reused without repeated addition.

[0039] It can be understood that in some embodiments of the present invention, the vacuum pumping device 500 is connected to the second rotating support pipe 420, and a second rotary joint 510 and a first filtering device 511 are arranged between them in sequence. The first filtering device 511 can prevent the powder or particles in the working chamber from escaping, and the second rotary joint 510 can prevent the vacuum pumping device 500 from rotating together with the second rotating support pipe 420, causing pipeline entanglement and structural interference. Of course, in some other embodiments, a valve can also be arranged between the second rotary joint 510 and the first filtering device 511 to realize the sealing and switching of the outlet of the second rotating support pipe 420.

[0040] It can be understood that in some embodiments of the present invention, a turnover frame 210 is hinged to the upper end of the first support base 200, and the bottom of the turnover frame 210 is hinged to the first support base 200 through a horizontally arranged rotating shaft. The turnover frame 210 is provided with a limit through hole, and the first rotating support tube 410 is inserted through the limit through hole and axially fixed to the turnover frame 210. The axial fixation can be achieved by means of shoulders on the first rotating support tube 410 and limit structures (nuts, circlips) connected to the outer periphery of the first rotating support tube 410, etc. The upper end of the furnace body 100 is openable; after the upper end of the furnace body 100 is opened, the working container 400 can be turned over with the turnover frame 210. Specifically, the furnace body 100 includes a furnace main body 110 and a furnace cover 120. The furnace cover 120 is installed at the upper end of the furnace main body 110 by means of hinge or sliding, etc., and is opened and closed by means of rotation or sliding or other movement methods. After the furnace cover 120 is opened, it can avoid structural interference with the turnover of the working container 400.

[0041] It can be understood that in some embodiments of the present invention, the driving mechanism 700 is a motor installed on the turnover frame 210. A transmission sleeve 710 is sleeved on the outer periphery of the first rotating support tube 410, and the motor is in transmission connection with the transmission sleeve 710 to drive the first rotating support tube 410 and the working container 400 to rotate. Specifically, the transmission sleeve 710 is fixed on the outer periphery of the first rotating support tube 410, and the transmission sleeve 710 and the output shaft of the motor are in transmission through a conveyor belt. Even when the working container 400 needs to be unloaded while being turned over with the turnover frame 210, the working container 400 can still be driven to rotate by the driving mechanism 700, so that the material can slide smoothly along the inclined surface to achieve unloading.

[0042] Refer to Figure 2 and Figure 3 , it further includes a hoisting and rotating device 800. The hoisting and rotating device 800 is sleeved on the second rotating support tube 420 and axially fixed. The hoisting and rotating device 800 can rotate around the second rotating support tube 420. In this way, when unloading, the hoisting and rotating device 800 can be lifted by a hoisting device, so that the working container 400, the first rotating support tube 410 and the second rotating support tube 420 can rotate and incline with the turnover frame to achieve unloading. And because the hoisting and rotating device 800 can rotate around the second rotating support tube 420, when the second rotating support tube 420 rotates for unloading, it will not drive the hoisting and rotating device 800 to rotate, avoiding affecting the hoisting.

[0043] It can be understood that in some embodiments of the present invention, the lifting and rotating device 800 includes a lifting frame 810, a lifting hook 820, and rollers 830. The lifting frame 810 is sleeved on the second rotating support tube 420. The lifting hook 820 is provided on the outer periphery of the lifting frame 810. The rollers 830 are circumferentially arranged on the inner ring of the lifting frame 810. A track sleeve 421 is fixedly provided on the peripheral wall of the second rotating support tube 420. The track sleeve 421 is provided with an annular track 422 adapted to the rollers 830, and the rollers 830 can roll along the annular track 422. The lifting hook 820 facilitates the lifting of the lifting device, and the rollers 830 reduce the friction force of the relative rotation between the lifting and rotating device 800 and the second rotating support tube 420. The annular track 422 not only guides the rolling of the rollers 830 but also axially fixes the lifting frame 810, preventing the lifting frame 810 from sliding along the second rotating support tube 420 and affecting the lifting.

[0044] To avoid the high-pressure bursting of the working container 400 and cause potential safety hazards, an explosion-proof device 430 is connected to the part of the first rotating support tube 410 or the second rotating support tube 420 extending out of the furnace body 100. The explosion-proof device 430 can be a pressure relief valve or a sealing structure. When the pressure is too high and exceeds the force-bearing limit of the sealing structure, the sealing structure is damaged to achieve rapid pressure relief.

[0045] The present invention also provides a high-temperature shaping and purification integrated production process for metal powder, including steps S1, S2, S3, S4, S5, S6, and S7.

[0046] S1: After discharging the moisture and harmful substances in the working container, load titanium metal raw materials and kinetic carriers into the working container. The specific steps are as follows: First, heat the working container to 100 - 300 °C for drying, then turn on the vacuum pumping device to pump vacuum while the gas charging device passes in an inert gas to displace the moisture or harmful substances in the working container. After cooling to below 80 °C and pressure balance, remove the second rotary joint 510 and load titanium metal raw materials and kinetic carriers into the second rotating support tube 420.

[0047] S2: Turn on the vacuum pumping device to discharge the gas impurities in the working container.

[0048] S3: Turn on the heating element 130 to heat the furnace body, so that the temperature in the working container reaches between 250 - 800 °C. The gas charging device passes hydrogen into the working container and keeps the pressure constant between 50 - 400 kPa. The driving mechanism drives the working container to rotate to hydrogenate the titanium metal. Specifically, the rotation of the working container can be between 5 - 200 r / min and the time is kept between 30 - 500 min, so that the titanium metal powder fully absorbs hydrogen by more than 2% to achieve a crisp effect.

[0049] S4. Adjust the temperature of the working container to between 300 - 900 °C, introduce an inert gas with a pressure constant between 10 - 90 kPa, and rotate the working container to break the titanium metal under the impact energy of the kinetic carrier. Specifically, the rotation of the working container is between 5 - 200 r / min and the time is maintained between 10 - 400 min, so that the brittle titanium metal powder is broken into powder less than 53 μm under the impact energy of the spherical kinetic carrier.

[0050] S5. After opening the vacuum pumping device to evacuate the gas in the working container, introduce an inert gas to keep the pressure in the working container constant between - 500 - 0 kPa, adjust the temperature of the working container to between 500 - 950 °C, and maintain the rotation of the working container to achieve titanium metal hydrogenation and dehydrogenation. Specifically, open the vacuum pumping device to displace gas impurities once or more, the rotation of the working container is between 5 - 500 r / min, and the time is maintained between 100 - 800 min to detach and displace the hydrogen element adsorbed by the titanium metal powder and discharge it.

[0051] S6. Adjust the temperature to between 200 - 950 °C, keep the pressure of the inert gas constant between 1 - 30 kPa, and maintain the rotation of the working container to achieve the shaping, spheroidization and purification of titanium metal. Step S6 can utilize the impact of the ball and the kinetic friction of the rotation of the working container near the soft spots of the titanium metal powder to remove the sharp corners and edges on the powder surface, gradually forming a spherical or quasi-spherical effect, while separating and finally discharging gas impurities at high temperature.

[0052] S7. Seal and discharge the material when the temperature drops below 100 °C and the pressure of the inert gas is between 0 - 5 kPa. Specifically, close the sealing valve 620, disassemble the first movable flange 611 and the first rotary joint 610, connect the discharge tank to the second movable flange 621, evacuate and fill the discharge tank with argon gas until it is clean, then open the sealing valve 620, and it is possible to discharge the material obliquely. After discharging, close the sealing valve 620, and remove the storage tank and the sealing valve 620 together and put them into the vacuum glove box for subsequent screening, packaging and other treatments.

[0053] The following combines with embodiments to better understand the technical solution of the present invention.

[0054] Embodiment 1

[0055] This embodiment provides a high-temperature shaping and purification integrated production process for metal powder, and the specific steps are as follows:

[0056] S1: After draining the moisture and harmful substances from the working container, load the titanium metal raw material and the kinetic energy carrier into the working container. The specific steps are as follows: First, heat the working container to 100 - 300 °C for drying, then turn on the vacuum pumping device to pump vacuum while the gas charging device passes in an inert gas to displace the moisture or harmful substances in the working container. After cooling to below 80 °C and pressure balance, remove the second rotary joint 510, and load the titanium metal raw material and the kinetic energy carrier into the second rotary support pipe 420;

[0057] S2: Turn on the vacuum pumping device to discharge the gas impurities in the working container.

[0058] S3: Turn on the heating element 130 to heat the furnace body, so that the temperature in the working container reaches 250 °C. The gas charging device passes hydrogen into the working container and keeps the pressure constant at 50 kPa. The driving mechanism drives the working container to rotate to hydrogenate the titanium metal. Specifically, the rotation speed of the working container is 5 r / min, and the time is kept for 30 min, so that the titanium metal powder absorbs hydrogen by more than 2% to achieve a crisp effect.

[0059] S4: Adjust the temperature of the working container to 300 °C, pass in an inert gas with a constant pressure of 10 kPa, and the rotation of the working container causes the titanium metal to break under the impact energy of the movement of the kinetic energy carrier. Specifically, the rotation speed of the working container is 5 r / min, and the time is kept for 10 min, so that the crisp titanium metal powder breaks into powder less than 53 μm under the impact energy of the movement of the spherical kinetic energy carrier.

[0060] S5: After turning on the vacuum pumping device to pump out the gas in the working container, pass in an inert gas to keep the pressure in the working container constant at -500 kPa, adjust the temperature of the working container to 500 °C, and keep the working container rotating to achieve hydrogenation and dehydrogenation of the titanium metal. Specifically, turn on the vacuum pumping device to displace the gas impurities once or more, the rotation speed of the working container is 5 r / min, and the time is kept for 100 min to remove and displace the hydrogen element adsorbed by the titanium metal powder.

[0061] S6: Adjust the temperature to 200 °C, keep the pressure of the inert gas constant at 1 kPa, and keep the working container rotating to achieve shaping, spheroidization and purification of the titanium metal. Step S6 can utilize the impact of the ball and the kinetic friction of the rotation of the working container near the soft spots of the titanium metal powder to remove the sharp corners and edges on the powder surface, gradually forming a spherical or quasi-spherical effect, and at the same time separating and finally discharging the gas impurities at high temperature.

[0062] S7: Discharge the material when the temperature drops below 100 °C and the pressure of the inert gas is 0 kPa.

[0063] The final result obtained:

[0064] The breakage rate is 35% (the proportion of coarse particles broken into powders smaller than 53 μm).

[0065] The spheroidization rate is 50% (the proportion of irregular particles with sharp-angled edges formed into spherical or quasi-spherical powders).

[0066] The oxygen content is 0.14%.

[0067] Example 2

[0068] This example provides a high-temperature shaping and purification integrated production process for metal powders, and the specific steps are as follows:

[0069] S1: After discharging the moisture and harmful substances in the working container, load the titanium metal raw material and the kinetic energy carrier into the working container. The specific steps are as follows: First, heat the working container to 100 - 300 °C for drying, then turn on the vacuum pumping device to pump vacuum while the gas charging device passes in an inert gas to displace the moisture or harmful substances in the working container. After cooling to below 80 °C and pressure balance, disassemble the second rotary joint 510, and load the titanium metal raw material and the kinetic energy carrier into the second rotary support pipe 420;

[0070] S2: Turn on the vacuum pumping device to discharge the gas impurities in the working container.

[0071] S3: Turn on the heating element 130, heat the furnace body to make the temperature in the working container reach 500 °C, the gas charging device passes hydrogen into the working container, and keep the pressure constant at 200 kpa. The driving mechanism drives the working container to rotate to hydrogenate the titanium metal. Specifically, the rotation speed of the working container is 100 r / min, and the time is kept for 200 min to make the titanium metal powder fully absorb hydrogen by more than 2% to achieve a crisp effect.

[0072] S4: Adjust the temperature of the working container to 600 °C, pass in an inert gas with a pressure constant at 50 kpa, and the rotation of the working container causes the titanium metal to break under the impact energy of the movement of the kinetic energy carrier. Specifically, the rotation speed of the working container is 100 r / min, and the time is kept for 200 min to break the crisp titanium metal powder into powders smaller than 53 μm under the impact energy of the movement of the spherical kinetic energy carrier.

[0073] S5: After turning on the vacuum pumping device to pump out the gas in the working container, pass in an inert gas to keep the pressure of the working container constant at -300 kpa, adjust the temperature of the working container to 700 °C, and keep the working container rotating to achieve the dehydrogenation of the titanium metal hydride. Specifically, turn on the vacuum pumping device to displace the gas impurities once or more, the rotation speed of the working container is 300 r / min, and the time is kept for 100 min to displace and discharge the hydrogen element adsorbed by the titanium metal powder.

[0074] S6. Adjust the temperature to 600 °C, keep the pressure of the inert gas constant at 15 kPa, and maintain the rotation of the working container to achieve the spheroidization and purification of titanium metal. In step S6, near the soft points of the titanium metal powder, the impact of the balls and the kinetic energy friction caused by the rotation of the working container can be utilized to remove the sharp corners and edges on the powder surface, gradually forming a spherical or near-spherical effect. Meanwhile, gas impurities are separated at high temperature and finally discharged.

[0075] S7. Discharge the material when the temperature drops below 100 °C and the pressure of the inert gas is 2 kPa.

[0076] The final results obtained:

[0077] The crushing rate is 86% (the proportion of coarse particles crushed into powder with a size below 53 μm);

[0078] The spheroidization rate is 35% (the proportion of irregular particles with sharp corners and edges formed into spherical or near-spherical powder);

[0079] The oxygen content is 0.16%.

[0080] Example 3

[0081] This example provides a high-temperature shaping and purification integrated production process for metal powder. The specific steps are as follows:

[0082] S1: After discharging the moisture and harmful substances in the working container, load the titanium metal raw material and the kinetic energy carrier into the working container. The specific steps are as follows: First, heat the working container to 100 - 300 °C for drying, then turn on the vacuum pumping device to pump vacuum while the gas filling device fills the inert gas to displace the moisture or harmful substances in the working container. After cooling to below 80 °C and pressure balance, remove the second rotary joint 510, and load the titanium metal raw material and the kinetic energy carrier into the second rotary support tube 420;

[0083] S2: Turn on the vacuum pumping device to discharge the gas impurities in the working container.

[0084] S3: Turn on the heating element 130, heat the furnace body to raise the temperature in the working container to 800 °C. The gas filling device fills hydrogen into the working container and keeps the pressure constant at 400 kPa. The driving mechanism drives the working container to rotate to hydrogenate the titanium metal. Specifically, the rotation speed of the working container is 200 r / min, and the time is maintained for 500 min to enable the titanium metal powder to absorb hydrogen by more than 2% to achieve a crisp effect.

[0085] S4. The temperature of the working container is adjusted to 900 °C, an inert gas is introduced, and the pressure is kept constant at 90 kPa. The rotation of the working container causes the titanium metal to break under the impact energy of the moving kinetic energy carriers. Specifically, the rotation speed of the working container is 200 r / min, and the time is maintained for 400 min, so that the brittle titanium metal powder is broken into powder smaller than 53 μm under the impact energy of the moving spherical kinetic energy carriers.

[0086] S5. After opening the vacuum device to pump out the gas in the working container, an inert gas is introduced to keep the pressure in the working container constant at 0 kPa. The temperature of the working container is adjusted to 900 °C, and the rotation of the working container is maintained to achieve hydrogenation and dehydrogenation of titanium metal. Specifically, the vacuum device is opened to replace the gas impurities once or more. The rotation speed of the working container is 500 r / min, and the time is maintained for 100 min to remove and replace the hydrogen element adsorbed by the titanium metal powder.

[0087] S6. The temperature is adjusted to 950 °C, the inert gas pressure is kept constant at 30 kPa, and the rotation of the working container is maintained to achieve shaping, spheroidization, and purification of titanium metal. Step S6 can utilize the impact of the balls and the kinetic friction of the rotation of the working container near the soft spots of the titanium metal powder to remove the sharp corners and edges on the powder surface, gradually forming a spherical or near-spherical effect. At the same time, gas impurities are separated and finally discharged at high temperature.

[0088] S7. The temperature is lowered below 100 °C, the inert gas pressure is 5 kPa, and the material is sealed for discharge.

[0089] The final results obtained are as follows:

[0090] The crushing rate is 100% (the proportion of coarse particles broken into powder smaller than 53 μm);

[0091] The spheroidization rate is 89% (the proportion of irregular particles with sharp corners and edges shaped into spherical or near-spherical powder);

[0092] The oxygen content is 0.17%.

[0093] The embodiments of the present invention have been described in detail above in conjunction with the accompanying drawings. However, the present invention is not limited to the above embodiments. Within the scope of knowledge possessed by those of ordinary skill in the art, various changes can be made without departing from the spirit of the present invention.

Claims

1. A high-temperature shaping and purification integrated production equipment for metal powder, characterized in that, Comprising: A furnace body (100); A first support base (200) provided on one side of the furnace body (100); A second support base (300) provided on the other side of the furnace body (100); A working container (400) is provided inside the furnace body (100), and a first rotating support tube (410) and a second rotating support tube (420) that extend out of the furnace body (100) and are coaxial are respectively provided at both ends. The first rotating support tube (410) is supported by the first support base (200), and the second rotating support tube (420) is supported by the second support base (300); A vacuum pumping device (500) for pumping vacuum on the working container (400); An inflation device (600) for filling the working container (400) with the required gas; A driving mechanism (700) for driving the working container (400) to rotate around the axis of the first rotating support tube (410); A flip frame (210) is hinged at the upper end of the first support base (200). The flip frame (210) is provided with a limit perforation. The first rotating support tube (410) passes through the limit perforation and is axially fixed to the flip frame (210). The upper end of the furnace body (100) is openable; after the upper end of the furnace body (100) is opened, the working container (400) can be flipped with the flip frame (210); The driving mechanism (700) is a motor installed on the flip frame (210). A transmission sleeve (710) is sleeved on the outer periphery of the first rotating support tube (410). The motor is in transmission connection with the transmission sleeve (710) to drive the first rotating support tube (410) and the working container (400) to rotate; The metal powder high-temperature shaping and purification integrated production equipment further includes a lifting and rotating device (800). The lifting and rotating device (800) is sleeved on the second rotating support tube (420) and is axially fixed. The lifting and rotating device (800) can rotate around the second rotating support tube (420); The lifting and rotating device (800) includes a lifting frame (810), a hook (820), and rollers (830). The lifting frame (810) is sleeved on the second rotating support tube (420). The hook (820) is provided on the outer periphery of the lifting frame (810). The rollers (830) are circumferentially arranged on the inner ring of the lifting frame (810). A track sleeve (421) is fixedly provided on the peripheral wall of the second rotating support tube (420). The track sleeve (421) is provided with an annular track (422) adapted to the rollers (830). The rollers (830) can roll along the annular track (422); 2. The high-temperature shaping and purification integrated production equipment for metal powder according to claim 1, wherein: The inflation device (600) is connected to the first rotating support tube (410) through a first rotary joint (610).

3. The high-temperature shaping and purification integrated production equipment for metal powder according to claim 2, wherein: The first rotary joint (610) is connected to the first rotating support tube (410) through a sealing valve (620).

4. The high-temperature shaping and purification integrated production equipment for metal powder according to claim 3, wherein: The first rotary joint (610) is provided with a first movable flange (611). The sealing valve (620) is provided with a second movable flange (621). The first movable flange (611) and the second movable flange (621) are provided with corresponding hole positions for connection and fixation by bolts; 5. A high-temperature shaping and purification integrated production process for metal powder, based on the high-temperature shaping and purification integrated production equipment for metal powder described in claim 1, characterized in that, Including the following steps: S1. After discharging moisture and harmful substances from the working container (400), load metal raw materials and kinetic carriers into the working container (400) so that the metal can be crushed and spheroidized when the working container (400) rotates; S2. Open the vacuum extraction device (500) to discharge gas impurities in the working container (400); S3. Heat the furnace body (100) to make the temperature in the working container (400) between 250 - 800 °C. The gas charging device (600) fills hydrogen into the working container (400) and keeps the pressure constant between 50 - 400 kPa. The driving mechanism (700) drives the working container (400) to rotate to hydrogenate the metal; S4. Adjust the temperature of the working container (400) to between 300 - 900 °C, and introduce an inert gas with a pressure constant between 10 - 90 kPa. The rotation of the working container (400) causes the metal to be crushed under the impact energy of the kinetic carrier; S5. After opening the vacuum extraction device (500) to extract the gas in the working container (400), introduce an inert gas to keep the pressure in the working container (400) constant between -500 - 0 kPa. Adjust the temperature of the working container (400) to between 500 - 950 °C and keep the working container (400) rotating to achieve metal hydrogenation and dehydrogenation; S6. Adjust the temperature to between 200 - 950 °C, keep the pressure of the inert gas constant between 1 - 30 kPa, and keep the working container (400) rotating to achieve shaping, spheroidization and purification of the metal; S7. Seal and discharge the material when the temperature drops below 100 °C and the pressure of the inert gas is between 0 - 5 kPa.

6. The high-temperature shaping and purification integrated production process of metal powder according to claim 5, characterized in that: The metal is one of the metal elements in the sixth period of the periodic table.

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