CN113996797A - Low-cost recovery and powder preparation process for titanium alloy spherical coarse powder - Google Patents
Low-cost recovery and powder preparation process for titanium alloy spherical coarse powder Download PDFInfo
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- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
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- B22F2003/1042—Sintering only with support for articles to be sintered
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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Abstract
A low-cost recovery and powdering process of titanium alloy spherical coarse powder comprises the following steps: selecting a ceramic tube or a titanium alloy thin-walled tube with a proper specification, cleaning, drying and plugging the bottom; filling the titanium alloy spherical coarse powder into a ceramic tube or a titanium tube, wherein the powder filling density reaches 2.6-3.0 g/cm3The above; vertically placing the ceramic tube or the titanium alloy thin-walled tube into a vacuum sintering furnace, carrying out pressureless sintering at the sintering temperature of 1000-1050 ℃, preserving heat for 2-6 hours, and cooling along with the furnace; cooling, discharging, removing the alumina tube and the gasket, and processing into electrode bars according to requirements; and (4) pulverizing the electrode bar. The invention provides a simple and low-cost crude titanium powder recycling technology, which has the characteristics of simple process, easy operation, high material utilization rate and low cost, reduces resource waste and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of metal powder preparation, and relates to a low-cost recovery and powder preparation process of titanium alloy spherical coarse powder.
Background
The EIGA (electrode induced gas atomization) process is the mainstream process for producing high-quality spherical titanium powder for additive manufacturing at home and abroad at present in large scale, and accounts for more than 90% of the market of the spherical titanium powder. The particle size of 15-53 mu m in the titanium alloy spherical powder prepared by the EIGA process accounts for about 30-40% of the total weight of the powder, and the titanium alloy spherical powder can be directly used in the titanium alloy additive manufacturing industry; the granularity of more than 53 mu m accounts for 50-70% of the total weight of the powder, the powder contains hollow powder, satellite powder and the like in a certain proportion, the powder is mainly used as an additive for steel smelting or fireworks, the recycling price is lower than the price of basic raw materials such as sponge titanium and the like, and the market digestion capacity is very limited, so that the profit level and the market competitiveness of the powder preparation are directly influenced by a large amount of high-quality coarse titanium powder, huge resource and energy waste is also caused, the titanium powder belongs to powder which is easy to burn, and huge potential safety hazards exist. Therefore, the development of a low-cost recycling technology of the high-purity low-oxygen titanium alloy spherical coarse powder is a common technical problem which is urgently needed to be solved in the powder making industry.
The spheroidized titanium powder produced by the EIGA process has the characteristics of high purity and low oxygen, the oxygen and nitrogen content of the coarse powder is lower than that of the fine powder in the same batch, the oxygen content is about 500-600 ppm, the nitrogen content is about 30-50 ppm, and the spheroidized titanium powder is equivalent to that of an original alloy bar. The spherical meal is therefore extremely advantageous in terms of material purity, with the disadvantage that a short-path, low-cost conversion to high-value-added titanium products is necessary for the meal to increase the value-added. Because the spherical titanium powder for additive manufacturing is in an explosion trend in recent years, aiming at the situation that the spherical coarse titanium powder does not have a mature and high-added-value application field, the application of the spherical coarse titanium powder is mainly used in the traditional applications of steelmaking additives, firework industries and the like, and the cost is higher when the complete smelting recovery of the coarse titanium powder is compared with the smelting of sponge titanium in consideration of the particularity and the process difficulty of the titanium smelting industry, the main reason is that: the smelting of titanium mainly adopts a vacuum consumable smelting furnace to firstly smelt sponge titanium into a titanium rod or a titanium ingot through multiple consumable smelting, and then the titanium ingot is remelted and cast into a final product of titanium, wherein the coarse titanium powder is in a regular spherical shape and has extremely high hardness, and the coarse titanium powder is pressed without deformation and mutual occlusion, so that the electrode is difficult to be pressed like the sponge titanium, and the smelting difficulty is extremely high. In addition, the casting industry of titanium generally uses titanium ingots instead of primary raw materials (titanium powder and titanium sponge) of titanium as raw materials for smelting, mainly considering the problem of component uniformity, and whether a plasma furnace, an electron beam furnace or an induction heating furnace is used, the heating efficiency of crushed materials is low, so that the smelting time is greatly prolonged, and the production efficiency is very unfavorable.
In addition, Chinese patent with patent application number CN201910791706.7 reports a recovery processing method of additive manufacturing waste titanium or titanium alloy powder, and the waste titanium or titanium alloy powder is subjected to the following operations under the conditions of room temperature of 10-20 ℃ and inert gas protection, wherein the steps are as follows: adding sodium amalgam into the additive manufacturing waste titanium or titanium alloy powder to obtain mixed slurry; step 2: mixing the mixed slurry obtained in the step 1 to enable the mixed slurry to reach a fluidized state; step 3, introducing inert gas into the fluidized mixed slurry obtained in the step 2, driving titanium or titanium alloy powder to generate shearing friction through bubbles generated in the mixed slurry and convection action among the slurries, accelerating evaporation of sodium amalgam in the slurry, and separating to obtain solid-phase titanium or titanium alloy powder; and 4, step 4: and (3) washing the titanium or titanium alloy powder obtained in the step (3), and drying to obtain the titanium or titanium alloy powder which can be used for additive manufacturing again. The method has the advantages of complex process steps and long flow, is only used for processing additive manufacturing waste titanium or titanium alloy powder, does not change the particle size of the powder, and is not suitable for processing coarse titanium powder except additive manufacturing powder.
Therefore, the recycling of the coarse titanium powder is also a very challenging technical problem, and the traditional thinking needs to be broken through to innovate in the process and application targets.
Disclosure of Invention
The invention aims to solve the technical problem of providing a low-cost recovery and re-pulverization process of titanium alloy spherical coarse powder, which has the characteristics of simple process, high material utilization rate and low cost, and simultaneously reduces resource waste.
The technical scheme adopted by the invention for solving the technical problems is as follows: a low-cost recovery and powdering process of titanium alloy spherical coarse powder is characterized by comprising the following steps:
1) selecting a ceramic tube or a titanium alloy thin-walled tube with a proper specification, cleaning and drying the ceramic tube or the titanium alloy thin-walled tube, and plugging the bottom of the ceramic tube or the titanium alloy thin-walled tube by using a flat ceramic plate or a flat titanium plate;
2) vertically standing a ceramic tube or a titanium alloy thin-walled tube in a sintering molybdenum boat and fixing, filling titanium alloy spherical coarse powder into the ceramic tube or the titanium alloy thin-walled tube, knocking or vibrating to compact the titanium alloy spherical coarse powder, wherein the powder filling density reaches 2.6-3.0 g/cm3The above;
3) vertically placing the ceramic tube or the titanium alloy thin-wall tube filled with the powder and the molybdenum boat into a vacuum sintering furnace, closing a furnace door, vacuumizing, performing pressureless sintering at the sintering temperature of 1000-1050 ℃, preserving heat for 2-6 hours, and cooling along with the furnace;
4) discharging the titanium alloy thin-walled tube after cooling, removing the ceramic tube and the gasket, processing the titanium alloy thin-walled tube into an electrode rod according to the requirement without removing the titanium alloy thin-walled tube, and using no liquid cooling medium in the processing process;
5) and (3) putting the electrode rod into an electrode cabin of an EIGA gas atomization powder making furnace, heating and remelting by using a conical induction coil, and preparing titanium alloy spherical powder with a certain particle size range through a high-pressure argon nozzle.
Preferably, the wall thickness of the ceramic tube in the step 1) is more than or equal to 3mm, and the wall thickness of the titanium alloy thin-walled tube is 0.3-1.0 mm.
Further, the titanium alloy spherical coarse powder in the step 2) is a byproduct of a spherical titanium powder product for additive manufacturing prepared by an air atomization process, and the particle size of the titanium alloy spherical coarse powder is 53-150 microns.
Further, the vacuum degree of the vacuumizing of the step 3) is 10-2Pa above, cooling to below 50 ℃ along with the furnace cooling, and discharging.
Preferably, the remelting powder preparation process parameters in the step 5) are as follows: the smelting (feeding) speed is 40-70 mm/min, the smelting power is 18-30 kW, and the atomization pressure is 3.5-5.0 MPa.
Finally, the finally obtained titanium alloy spherical powder in the step 5) has the granularity range of 5-150 mu m and the d50Is 40 to 70 μm.
Compared with the prior art, the invention has the advantages that:
(1) the non-pressure sintering process is adopted to directly sinter the coarse titanium powder into bars, so that the problems of conventional complex processes such as molding sintering, smelting and the like and impurity control and the like caused by the complex processes are avoided;
(2) the thin-wall titanium tube is used as a sintering container, powder is directly prepared subsequently, the material utilization rate is high, and no waste is caused;
(3) the low-cost and non-compact sintered titanium rod is used for replacing a high-price compact titanium rod, the same-quality degradation substitution of materials is realized, and meanwhile, the EIGA process is remelting powder preparation, so that the final fine powder yield and the powder impurity content are not influenced;
the method has the characteristics of simple process, easy operation, high material utilization rate and low cost, reduces resource waste and has wide application prospect.
Drawings
FIG. 1 is a photograph of a thin-walled titanium tube filled with coarse titanium powder according to example 2 of the present invention;
FIG. 2 is a photograph of a titanium rod sintered in example 2;
FIG. 3 is an SEM photograph of a powder prepared by an EIGA process of a sintered titanium rod (electrode) of example 2.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Example 1
A low-cost recovery and powder preparation process of titanium alloy spherical coarse powder, wherein the particle size of the recovered titanium alloy spherical coarse powder is 53-150 mu m. The embodiment is to use a ceramic tube to prepare titanium rod through pressureless sintering and then prepare powder, and the method comprises the following steps:
(1) cleaning a ceramic tube with the outer diameter of 63mm, the inner diameter of 51mm and the length of 500mm, and drying the ceramic tube in an oven at 500 ℃;
(2) selecting a matched boss type ceramic plate to plug the lower part of a pipe orifice, vertically standing a ceramic pipe in a sintering molybdenum boat and fixing, filling titanium alloy spherical coarse powder into the ceramic pipe, knocking or vibrating to compact the titanium alloy spherical coarse powder, wherein the powder filling amount is more than 2.8kg according to the size of the ceramic pipe, and in order to ensure the sintering effect, the powder filling density is required to reach 2.6-3.0 g/cm3The above
(3) Putting the ceramic tube filled with the powder and the molybdenum boat into a vacuum sintering furnace, and vacuumizing to 10 DEG-3Heating after Pa, keeping the sintering temperature at 1050 ℃ for 3h, and cooling along with the furnace;
(4) cooling to below 50 ℃ and discharging, knocking out the ceramic tube after discharging, polishing the surface of the sintered titanium rod, machining an electrode according to the size requirement, and not allowing any liquid cooling medium to be used during machining so as to avoid sucking the sintered titanium rod into the rod;
(5) putting a titanium electrode bar into an electrode cabin of an EIGA gas atomization powder making furnace for powder making, remelting the sintered electrode bar by using a conical induction coil, and making titanium alloy spherical powder with a certain particle size range through a high-pressure argon nozzle; the remelting powder preparation uses the following technological parameters: the smelting power is 20kW, the smelting (feeding) speed is 55mm/min, and the atomization powder preparation pressure is 4.5MPa, so that the spherical titanium powder is obtained, and the particle size range is 5-150 mu m.
Example 2
A low-cost recovery and powder preparation process of titanium alloy spherical coarse powder, wherein the particle size of the recovered titanium alloy spherical coarse powder is 53-150 mu m. The embodiment is to use a thin-wall titanium tube to prepare a titanium rod through pressureless sintering and then prepare powder, and the method comprises the following steps:
(1) cleaning and drying a phi 48 multiplied by 0.5 multiplied by 500mm thin-wall titanium tube, and welding a round titanium sheet at the bottom for sealing;
(2) vertically standing a titanium tube in a sintering molybdenum boat and fixing, filling titanium alloy spherical coarse powder into the titanium tube, knocking or vibrating to compact the titanium tube, wherein the powder filling amount is more than 2.6kg according to the size of the titanium tube, and filling the titanium tube with the coarse titanium powder to form a thin-wall titanium tube as shown in figure 1; in order to ensure the sintering effect, the powder loading density is 2.6-3.0 g/cm3The above;
(3) putting the titanium tube filled with the powder and the molybdenum boat into a vacuum sintering furnace, and vacuumizing to 10 DEG-3Heating after Pa, keeping the sintering temperature at 1020 ℃, keeping the temperature for 5h, cooling along with the furnace, and taking a picture of the titanium rod after sintering as shown in figure 2;
(4) cooling to below 50 ℃, discharging, processing the electrode according to the size requirement, and not allowing any liquid cooling medium to be used during processing so as to avoid sucking the liquid cooling medium into the bar stock;
(5) putting a titanium electrode bar into an electrode cabin of an EIGA gas atomization powder making furnace for powder making, remelting the sintered electrode bar by using a conical induction coil, and making titanium alloy spherical powder with a certain particle size range through a high-pressure argon nozzle; the remelting powder preparation uses the following technological parameters: the smelting power is 25kW, the smelting (feeding) speed is 60mm/min, the atomization powder preparation pressure is 4.5MPa, the spherical titanium powder is obtained, the particle size range is 5-150 mu m, and the SEM photograph of the powder obtained by preparation is shown in figure 3.
It can be seen from FIG. 3 that the prepared powder has a better particle size distribution and sphericity. The sintered titanium rod with low cost and non-compact state is used for replacing a compact titanium rod with high price, so that the material degradation replacement is realized, and meanwhile, the EIGA process is remelting powder preparation, so that the final fine powder yield and the powder impurity content are not influenced. Because the non-pressure sintering process is adopted to directly sinter the coarse titanium powder into the bar, the problems of the conventional complex processes such as molding sintering, smelting and the like, impurity control and the like are avoided; the thin-wall titanium tube is used as a sintering container, powder is directly prepared subsequently, the material utilization rate is high, and no waste is caused.
Claims (6)
1. A low-cost recovery and powdering process of titanium alloy spherical coarse powder is characterized by comprising the following steps:
1) selecting a ceramic tube or a titanium alloy thin-walled tube with a proper specification, cleaning and drying the ceramic tube or the titanium alloy thin-walled tube, and plugging the bottom of the ceramic tube or the titanium alloy thin-walled tube by using a flat ceramic plate or a flat titanium plate;
2) vertically standing a ceramic tube or a titanium alloy thin-walled tube in a sintering molybdenum boat and fixing, filling titanium alloy spherical coarse powder into the ceramic tube or the titanium alloy thin-walled tube, knocking or vibrating to compact the titanium alloy spherical coarse powder, wherein the powder filling density reaches 2.6-3.0 g/cm3The above;
3) vertically placing the ceramic tube or the titanium alloy thin-wall tube filled with the powder and the molybdenum boat into a vacuum sintering furnace, closing a furnace door, vacuumizing, performing pressureless sintering at the sintering temperature of 1000-1050 ℃, preserving heat for 2-6 hours, and cooling along with the furnace;
4) discharging the titanium alloy thin-walled tube after cooling, removing the ceramic tube and the gasket, processing the titanium alloy thin-walled tube into an electrode rod according to the requirement without removing the titanium alloy thin-walled tube, and using no cooling medium in the processing process;
5) and (3) putting the electrode rod into an electrode cabin of an EIGA gas atomization powder making furnace, heating and remelting by using a conical induction coil, and preparing titanium alloy spherical powder with a certain particle size range through a high-pressure argon nozzle.
2. The low-cost recovery and pulverization process of claim 1, wherein: the wall thickness of the ceramic tube in the step 1) is 3-10 mm, and the wall thickness of the titanium alloy thin-walled tube is 0.3-1.0 mm.
3. The low-cost recovery and pulverization process of claim 1, wherein: the particle size range of the titanium alloy spherical coarse powder in the step 2) is 53-150 mu m.
4. The low-cost recovery and pulverization process of claim 1, wherein: the vacuum degree of the vacuumizing of the step 3) is 10-2Pa above, cooling to below 50 ℃ along with the furnace cooling, and discharging.
5. The low-cost recovery and pulverization process of claim 1, wherein: the remelting powder preparation process of the step 5) comprises the following process parameters: the smelting feeding speed is 40-70 mm/min, the smelting power is 18-30 kW, and the atomization pressure is 3.5-5.0 MPa.
6. The low-cost recovery and pulverization process of claim 1, wherein: the titanium alloy spherical powder obtained in the step 5) has a particle size range of 5-150 mu m, d50Is 40 to 70 μm.
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