CN113492213A - Preparation method and equipment of high-sphericity low-oxygen-content TiAl alloy powder - Google Patents
Preparation method and equipment of high-sphericity low-oxygen-content TiAl alloy powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 110
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 84
- 239000000956 alloy Substances 0.000 title claims abstract description 84
- 229910010038 TiAl Inorganic materials 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000012545 processing Methods 0.000 claims abstract description 80
- 239000001301 oxygen Substances 0.000 claims abstract description 56
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 56
- 239000007789 gas Substances 0.000 claims abstract description 44
- 229910052751 metal Inorganic materials 0.000 claims abstract description 31
- 239000002184 metal Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 29
- 230000008859 change Effects 0.000 claims abstract description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000005266 casting Methods 0.000 claims abstract description 11
- 238000011049 filling Methods 0.000 claims abstract description 8
- 238000002844 melting Methods 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- 239000001307 helium Substances 0.000 claims abstract description 7
- 229910052734 helium Inorganic materials 0.000 claims abstract description 7
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000006698 induction Effects 0.000 claims abstract description 7
- 238000004806 packaging method and process Methods 0.000 claims abstract description 7
- 238000012216 screening Methods 0.000 claims abstract description 7
- 238000003754 machining Methods 0.000 claims abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 46
- 239000011261 inert gas Substances 0.000 claims description 30
- 239000010936 titanium Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000009792 diffusion process Methods 0.000 claims description 17
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 16
- 229910052719 titanium Inorganic materials 0.000 claims description 16
- 238000000859 sublimation Methods 0.000 claims description 15
- 230000008022 sublimation Effects 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000010791 quenching Methods 0.000 claims description 8
- 230000000171 quenching effect Effects 0.000 claims description 8
- 238000005496 tempering Methods 0.000 claims description 8
- 239000000523 sample Substances 0.000 claims description 7
- 230000007704 transition Effects 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 description 24
- 230000008569 process Effects 0.000 description 18
- 238000009690 centrifugal atomisation Methods 0.000 description 9
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- 238000004519 manufacturing process Methods 0.000 description 9
- 239000012535 impurity Substances 0.000 description 8
- 239000002245 particle Substances 0.000 description 7
- 238000001513 hot isostatic pressing Methods 0.000 description 6
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 229910002065 alloy metal Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
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- 238000001878 scanning electron micrograph Methods 0.000 description 2
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- 229910000838 Al alloy Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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- 238000004220 aggregation Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
Abstract
The invention relates to a preparation method and equipment of high-sphericity low-oxygen content TiAl alloy powder, wherein the preparation method comprises the following steps: s1, carrying out vacuum induction melting at least twice, and casting to obtain a TiAl alloy bar; s2, performing high-temperature phase change treatment on the bar; s3, machining the bar to obtain a finish-machined bar; s4, taking the finish machining bar as a consumable electrode and placing the consumable electrode in a machining bin; s5, starting a vacuum system pump set and a vacuum valve; s6, filling a mixed gas of argon and helium into the processing bin; s7, starting the driver so that the driver drives the consumable electrode to rotate, and the metal molten drops are rapidly solidified into TiAl alloy spherical metal powder; and S8, screening and packaging the metal powder. The preparation equipment comprises a processing bin, and a driver for driving the consumable electrode to rotate is arranged on the processing bin. The TiAl alloy powder prepared by the method has improved comprehensive performance indexes.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy, and particularly relates to a preparation method and equipment of high-sphericity low-oxygen content TiAl alloy powder.
Background
TiAl alloys have become important high-temperature structural materials, especially the main materials of low-pressure turbine blades of aircraft engines, due to the excellent high-temperature performance and low density of the TiAl alloys. The traditional process generally adopts a casting mode to prepare the TiAl alloy blade, but the blade blank processing difficulty is large due to the intrinsic brittleness of the TiAl alloy, and the yield of the blade is low. The hot isostatic pressing technology or the additive manufacturing technology uses TiAl alloy powder as a raw material to realize the near-net forming of the low-pressure turbine blade. The blade manufactured by the two technologies has small processing amount and high yield. The aeroengine low pressure turbine blade fabrication technology has therefore been gradually replaced by conventional casting with hot isostatic pressing or additive manufacturing.
The key to the performance of the low-pressure turbine blade prepared by the hot isostatic pressing or additive manufacturing technology is the quality of the raw material powder. The high sphericity powder has the advantages of good purity, high surface smoothness, difficult bridging among powder particles and the like, and is characterized in that the powder sphericity is better in a hot isostatic pressing or additive manufacturing technology, the higher the tap density and the filling rate of the powder are, the fewer pores or cracks are generated in the part forming process, the fewer pores and cracks are, and the service performance of the part, particularly the high-temperature fatigue performance is better.
Compared with other powder preparation technologies, the centrifugal atomization technology has the advantages of ultra-clean processing environment, no introduction of non-metal impurities and the like, and compared with other powder preparation technologies, the powder prepared by the technology has the characteristics of good sphericity, high purity and the like, so that the centrifugal atomization technology becomes a preferred raw material preparation mode in hot isostatic pressing and additive manufacturing technologies. Although the centrifugal atomization technology can obtain high-sphericity powder compared with other powder preparation technologies, the TiAl alloy, the titanium alloy and the aluminum alloy have different material types and belong to intermetallic compounds, and the plasticity of the alloy is different from that of other two types (the elongation is only 1%), so that the bar is easy to crack in the powder preparation process, and the risk that the smelting process cannot be carried out is easy to cause; in addition, the material has poor self-thermal conductivity (the thermal conductivity is only 22.5 Wm)−1 K−1) The solidification speed of the metal molten drops is lower than that of other metal materials, and the solidification process is easy to deform in a different direction, so that the sphericity of the powder is often inferior to that of other centrifugally atomized powder. This can be interpreted as: in the centrifugal atomization technology, the metal molten drops spontaneously solidify into balls by overcoming surface tension in the flight process, the larger the size of the metal molten drops, the higher the flight speed is, and the lower the sphericity of the powder is caused by insufficient solidification of the molten drops. In addition, compared with other powder preparation technologies, the centrifugal atomization technology adopts pre-vacuumizing and then high-purity inert gas is filled, the powder processing environment is purer, and therefore the oxygen content of the powder is lower than that of other preparation technologies; however, in the traditional centrifugal atomization technology, the processing environment is a non-closed loop inert gas environment, gas is in a continuous in-and-out flowing state in the processing bin, and the gas in the bin needs to be continuously supplied if the pressure in the processing bin is constant, so that the use cost of the gas is increased, the purity of original pre-vacuumizing is damaged, and the oxygen content in the processing bin is increased. For TiAl alloy, the TiAl alloy is easy to react with oxygen, nitrogen and hydrogen at 300-500 ℃, and the plasticity of the alloy is seriously influenced. Therefore, how to improve the sphericity of the TiAl alloy powder and reduce the oxygen content in the powder is the key to influence the service life of the low-pressure turbine blade of the aeroengine.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method and equipment of high-sphericity low-oxygen content TiAl alloy powder, which improve the comprehensive performance of the TiAl alloy powder, reduce the oxygen content in the powder, improve the performance of hot isostatic pressing or material-increasing manufacturing parts and finally prolong the service life of a low-pressure turbine blade.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of high-sphericity low-oxygen content TiAl alloy powder is characterized by comprising the following steps:
s1, carrying out vacuum induction melting at least twice, and casting to obtain a TiAl alloy bar;
s2, performing high-temperature phase change treatment on the bar prepared in the step S1;
s3, machining the bar processed in the step S2 to obtain a finished bar;
s4, taking the finish-machined bar material prepared in the step S3 as a consumable electrode, and placing the consumable electrode in a processing bin;
s5, opening a pump set and a vacuum valve of the vacuum system to ensure that the vacuum degree in the processing bin is lower than 10-3Pa, closing a pump set and a vacuum valve of the vacuum system;
s6, filling the mixed gas of argon and helium into the processing bin until the pressure in the processing bin is 2x 101Pa, the oxygen content is lower than 50ppm, the gas cylinder filled with the mixed gas is closed, and the inert gas closed-loop system is opened;
s7, starting a driver so that the driver drives the consumable electrode to rotate at a speed of 30000-33000 rpm, starting a plasma gun controller to generate a plasma arc with power of 50-60 kw, heating the end face of the consumable electrode rotating at a high speed by the plasma arc to melt the consumable electrode to form a liquid level and form a metal droplet, and quickly solidifying the metal droplet into TiAl alloy spherical metal powder;
s8, screening and packaging the metal powder prepared in the step S7 under the environment of high-purity inert gas.
Further, the high temperature phase change process in step S2 is performed in a vacuum environment with a vacuum degree of less than 10-2Heating to 1330-1350 ℃ at Pa, preserving heat for 1-4 h, and cooling by water quenching; then tempering treatment is carried out in a vacuum environment, namely heating to 1300-1320 ℃, and then maintainingAnd (5) heating for 1-4 h, and cooling in a furnace.
Further, the sphericity of the TiAl alloy spherical metal powder in the step S7 is not less than 98%, and the oxygen content of the TiAl alloy spherical metal powder is less than 50 ppm.
The equipment for realizing the preparation method of the TiAl alloy powder with high sphericity and low oxygen content is characterized by comprising a processing bin, wherein a driver for driving a consumable electrode to rotate is arranged on the processing bin, a plasma gun is arranged at a position corresponding to the driver, the plasma gun is controlled by a plasma gun controller, a vacuum system pump set is connected to the processing bin, and the vacuum system pump set is connected with an oxygen probe arranged on the processing bin through a control system.
Further, still be provided with inert gas closed loop system on the processing storehouse, inert gas closed loop system includes the gas circulation pipeline, the input and the output of gas circulation pipeline are connected with the processing storehouse respectively, gas filter and compressor have connected gradually on the gas circulation pipeline.
Furthermore, the vacuum system pump group comprises a mechanical pump and a diffusion pump which are connected with the processing bin, and the mechanical pump and the diffusion pump are both connected with the control system.
Further, a titanium sublimation pump is connected between the processing bin and the diffusion pump, and the titanium sublimation pump is connected with the control system.
Compared with the prior art, the invention has the following beneficial effects:
the method carries out high-temperature phase change treatment on the TiAl alloy cast bar, and provides a tissue foundation for obtaining centrifugally atomized fine molten drops; the invention can effectively improve the sphericity of the powder and improve the comprehensive performance index of the powder; the titanium sublimation pump is designed in the pump set of the vacuum system and is used for further reducing the oxygen content in the processing bin and ensuring that the oxygen content of the prepared TiAl alloy powder is lower than 50 ppm; the invention adds an inert gas closed loop system, reduces the use cost of inert gas in the powder preparation process and simultaneously reduces the oxygen content in the alloy powder; the TiAl alloy bar is smelted at least twice, so that the content of impurity elements in the TiAl alloy is reduced to the maximum extent, and the purity of the alloy is improved.
Other features of the present invention and advantages thereof will become apparent from the following detailed description of exemplary embodiments thereof, which proceeds with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.
FIG. 1 is a structural diagram of a high sphericity low oxygen content TiAl alloy powder manufacturing apparatus according to the present invention;
FIG. 2 is a scanning electron micrograph of TiAl alloy powder prepared by the technique of the present invention;
FIG. 3 is a scanning electron micrograph of TiAl alloy powder prepared using conventional techniques;
FIG. 4 is a microstructure of a section of a TiAl alloy low pressure turbine blade produced from TiAl alloy powder prepared by the technique of the present invention;
wherein: 1. a processing bin; 2. a consumable electrode; 3. a gas circulation line; 4. plasma arc; 5. an oxygen probe.
Detailed Description
Reference will now be made in detail to the exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Rather, they are merely examples of apparatus consistent with certain aspects of the invention, as detailed in the appended claims.
In order to make those skilled in the art better understand the technical solution of the present invention, the following detailed description of the present invention is provided with reference to the accompanying drawings and examples.
A preparation method of high-sphericity low-oxygen content TiAl alloy powder comprises the following steps:
s1, carrying out vacuum induction melting at least twice, and casting to obtain a TiAl alloy bar; the TiAl alloy bar is smelted at least twice, so that the content of impurity elements in the TiAl alloy is reduced to the maximum extent, and the purity of the alloy is improved;
s2, performing high-temperature phase change treatment on the bar prepared in the step S1;
s3, machining the bar processed in the step S2 to obtain a finished bar;
s4, taking the finished bar material prepared in the step S3 as a consumable electrode 2, and placing the consumable electrode 2 in a processing bin 1;
s5, opening a pump set and a vacuum valve of the vacuum system to ensure that the vacuum degree in the processing bin 1 is lower than 10-3Pa, closing a pump set and a vacuum valve of the vacuum system;
s6, filling the mixed gas of argon and helium into the processing bin 1 until the pressure in the processing bin 1 is 2 multiplied by 101Pa, the oxygen content is lower than 50ppm, the gas cylinder filled with the mixed gas is closed, and the inert gas closed-loop system is opened; the opening of the inert gas closed-loop system is used for keeping the pressure in the processing bin 1 constant, so that the use cost of the inert gas in the powder making process is reduced, and the oxygen content in the alloy powder is reduced;
s7, starting a driver so that the driver drives the consumable electrode 2 to rotate at a speed of 30000-33000 rpm, starting a plasma gun controller to generate a plasma arc 4 with power of 50-60 kw, wherein the plasma arc 4 heats the end face of the consumable electrode 2 rotating at a high speed so that the consumable electrode 2 is melted to form a liquid surface and a metal molten drop is formed, and the metal molten drop is rapidly solidified into TiAl alloy spherical metal powder; the sphericity of the powder is improved, the average sphericity of the powder is improved from 85% to 99%, and the comprehensive performance index of the powder is improved;
s8, screening and packaging the metal powder prepared in the step S7 under the environment of high-purity inert gas.
The TiAl alloy comprises the following components in percentage by weight:
28-35 wt% of Al, less than or equal to 0.35 wt% of B, and Si: less than or equal to 0.2wt.%, Mn: less than or equal to 4 wt%, Fe less than or equal to 0.1 wt%, C less than or equal to 0.05 wt%, and the balance of Ti and inevitable impurity elements.
Further, the high temperature phase transition processing in step S2 is performed in a vacuum environment with a vacuum degree of less than 10-2Heating to 1330-1350 ℃ at Pa, preserving heat for 1-4 h, and cooling by water quenching; and then tempering in a vacuum environment, namely heating to 1300-1320 ℃, preserving heat for 1-4 h, and cooling in a furnace.
The water quenching cooling has high water cooling speed, inhibits the rapid growth of crystal grains, aims to provide more nucleation mass points for the next tempering treatment and forms a large amount of gamma-phase and gamma/alpha-phase fine lamellar structures in the first high-temperature heating process; the tempering treatment aims at promoting the growth of nucleation particles generated by water quenching and forming a fine gamma/alpha phase alternate uniform full-lamellar structure. The high-temperature phase change treatment aims at refining the TiAl alloy structure, converting a coarse cast structure into a fine lamellar structure, reducing the size of lamellar crystal aggregates to about 100 mu m, providing a structure foundation for obtaining fine molten drops through centrifugal atomization, ensuring that the final TiAl alloy powder has high sphericity and improving the comprehensive performance index of the powder.
Further, the vacuum system pump set in step S5 includes a mechanical pump and a diffusion pump connected to the processing chamber 1, and both the mechanical pump and the diffusion pump are connected to the control system.
The mechanical pump is a pre-pumping pump and is used for preliminarily reducing the vacuum degree in the processing bin 1 to 10-1Pa, the diffusion pump is a main pump of a vacuum system pump set and is used for ensuring that the vacuum degree of the processing bin 1 is lower than 10-3Pa。
Further, a titanium sublimation pump is connected between the processing bin 1 and the diffusion pump, and the titanium sublimation pump is connected with the control system.
The titanium sublimation pump is used for absorbing oxygen in the processing bin 1, so that the oxygen content in the processing bin 1 is further reduced, and the oxygen content in the prepared TiAl alloy metal powder is ensured to be lower than 50 ppm.
Further, the inert gas closed-loop system in step S6 is used for drying and purifying the inert gas used in circulation, and includes a gas circulation pipeline 3 having an input end and an output end respectively connected to the processing bin 1, and the gas circulation pipeline 3 is sequentially connected to a gas filter and a compressor.
Further, the sphericity of the TiAl alloy spherical metal powder in the step S7 is not less than 98%, and the oxygen content of the TiAl alloy spherical metal powder is less than 50 ppm.
The equipment comprises a processing bin 1, wherein a driver used for driving a consumable electrode 2 to rotate is arranged on the processing bin 1, a plasma gun is arranged at a position corresponding to the driver and is controlled by a plasma gun controller, a vacuum system pump set is connected to the processing bin 1, and the vacuum system pump set is connected with an oxygen probe 5 arranged on the processing bin 1 through a control system.
Further, still be provided with inert gas closed loop system on the processing storehouse 1, inert gas closed loop system includes gas circulation pipeline 3, gas circulation pipeline 3's input and output are connected with processing storehouse 1 respectively, gas circulation pipeline 3 is last to be connected with gas filter and compressor in proper order.
The inert gas closed-loop system is used for drying and purifying the inert gas used circularly, so that the use cost of the inert gas in the powder making process is reduced, and the oxygen content in the alloy powder is reduced.
Further, the vacuum system pump group comprises a mechanical pump and a diffusion pump which are connected with the processing bin 1, and the mechanical pump and the diffusion pump are both connected with the control system.
The mechanical pump is a pre-pumping pump and is used for preliminarily reducing the vacuum degree in the processing bin 1 to 10-1Pa, the diffusion pump is a main pump of the vacuum system and is used for ensuring that the vacuum degree of the processing bin 1 is lower than 10-3Pa。
Further, a titanium sublimation pump is connected between the processing bin 1 and the diffusion pump, and the titanium sublimation pump is connected with the control system.
The titanium sublimation pump is used for absorbing oxygen in the processing bin 1, so that the oxygen content in the processing bin 1 is further reduced, and the oxygen content in the prepared TiAl alloy metal powder is ensured to be lower than 50 ppm.
The following is described with reference to specific process procedures:
example 1:
the invention provides a preparation method of high-sphericity low-oxygen content TiAl alloy powder, which is implemented by the following steps:
step 1: performing vacuum induction melting twice, and casting to obtain a TiAl4522XD alloy bar;
the TiAl4522XD alloy comprises the following components in percentage by weight:
30wt.% of Al, 0.2wt.% of B, 0.1wt.% of Si, 3wt.% of Mn, 0.07wt.% of Fe, 0.02wt.% of C, 40ppm of O, and the balance Ti and inevitable impurity elements.
Step 2: performing high-temperature phase change treatment on the bar prepared in the step 1, namely performing phase change treatment on the bar prepared in the step 1 under the condition that the vacuum degree is 9 multiplied by 10-3Heating to 1350 ℃ in a vacuum environment of Pa, preserving heat for 2h, and performing water quenching and cooling; tempering treatment in vacuum environment, namely heating to 1310 ℃, preserving heat for 2h, and carrying out furnace cooling and high-temperature phase change treatment.
And step 3: and (4) finely turning the bar subjected to the high-temperature phase change treatment in the step (2).
And 4, step 4: and (4) taking the finish-machined bar material prepared in the step (3) as a consumable electrode 2 and placing the consumable electrode in a processing bin 1 of a powder making device.
And 5: opening the valve a, the valve d and the mechanical pump in the vacuum system to the vacuum gauge e to display the vacuum degree of 10-1Pa; the diffusion pump, the valve c and the valve b are opened until the vacuum gauge g displays that the vacuum degree reaches 10-2Pa; starting the titanium sublimation pump until the vacuum degree is lower than 10 as shown by the vacuum gauge f-3Pa; and closing the valves a, b, c and d.
Step 6: filling mixed gas of argon and helium with the volume ratio of 1:9 into the processing bin 1 through the gas assembly until the pressure in the processing bin 1 is 2 multiplied by 101Pa; the gas cylinder filled with the mixed gas is closed, the compressor and the gas filter in the inert gas closed loop system are opened, and the pressure in the processing bin 1 is ensured to be constant at 2 multiplied by 101Pa, oxygen probe 5 showed an oxygen content below 50 ppm.
And 7: and starting a driver to drive the consumable electrode 2 to rotate at a high speed of 33000rpm, starting a plasma gun controller to generate a plasma arc 4 with the power of 58kw, heating the end face of the consumable electrode 2 by the plasma arc 4 to melt the consumable electrode 2 to form a liquid level, throwing the liquid level out of the end face of the consumable electrode 2 under the action of centrifugal force, rapidly solidifying the thrown molten drop into spherical metal powder in the motion process, and collecting the metal powder by a powder collecting bin.
And 8: and (3) screening and packaging the metal powder prepared in the step (7) in a high-purity inert gas environment: the sieve is powder with the particle size of 15-53 mu m, the average sphericity of the powder is 99% as detected by a dynamic image analysis method, and the oxygen content of TiAl4522XD alloy powder is 40ppm as tested by an oxygen-nitrogen-hydrogen analyzer.
As can be seen from FIGS. 2 to 3, the sphericity of TiAl alloy powder which is not prepared by the method is poor; the TiAl alloy powder prepared by the method has high sphericity, and the average value is 99 percent; as can be seen from FIG. 4, the section microstructure of the TiAl alloy low-pressure turbine blade produced by the TiAl alloy powder prepared by the technology of the invention has no defects such as pores and the like.
Comparing the comprehensive performance of the powder prepared by the TiAl alloy powder prepared by the invention with the powder prepared by the traditional centrifugal atomization technology and having the same particle size, as shown in Table 1; a comparison of the oxygen content in the powders prepared by the different processes is shown in Table 2.
TABLE 1 comprehensive performance comparison table of TiAl alloy powder
TABLE 2 comparison table of oxygen content of TiAl alloy powder
As can be seen from Table 1, the sphericity, the apparent density and the tap density of the TiAl alloy powder obtained by the method for preparing the TiAl alloy powder with high sphericity and low oxygen content are all higher than those of the TiAl alloy powder prepared by the traditional technology, and the Hall flow rate is lower than that of the traditional technology.
As shown in Table 2, the TiAl alloy powder prepared by the method for preparing the high-sphericity low-oxygen content TiAl alloy powder has lower oxygen content than the TiAl alloy powder prepared by the traditional technology.
Therefore, the powder comprehensive performance index of the TiAl alloy powder obtained by the method is obviously improved, the powder sphericity is improved, and the oxygen content of the powder is reduced.
Example 2:
the invention provides a preparation method of high-sphericity low-oxygen content TiAl alloy powder, which is implemented by the following steps:
step 1: carrying out three times of vacuum induction melting and casting to obtain a TiAl4822 alloy bar;
the TiAl4822 alloy comprises the following components in percentage by weight:
35wt.% of Al, 0.01wt.% of Si, 0.1wt.% of Fe, 0.025wt.% of C, 40ppm of O, and the balance Ti and inevitable impurity elements.
Step 2: performing high-temperature phase change treatment on the bar prepared in the step 1, namely performing phase change treatment on the bar prepared in the step 1 under the condition that the vacuum degree is 8.8 multiplied by 10-3Heating to 1340 ℃ in a Pa vacuum environment, preserving heat for 1.5h, and performing water quenching and cooling; tempering treatment in vacuum environment, namely heating to 1300 ℃, preserving heat for 1.5h, and carrying out furnace cooling and high-temperature phase change treatment.
And step 3: and (4) finely turning the bar subjected to the high-temperature phase change treatment in the step (2).
And 4, step 4: and (4) taking the finish-machined bar material prepared in the step (3) as a consumable electrode 2 and placing the consumable electrode in a processing bin 1 of a powder making device.
And 5: opening the valve a, the valve d and the mechanical pump in the vacuum system until the vacuum gauge e displays that the vacuum degree reaches 10-1Pa; the diffusion pump, the valve c and the valve b are opened until the vacuum gauge g displays that the vacuum degree reaches 10-2Pa; starting the titanium sublimation pump until the vacuum degree is lower than 10 as shown by the vacuum gauge f-3Pa; and closing the valves a, b, c and d.
Step 6: filling mixed gas of argon and helium with the volume ratio of 1:9 into the processing bin 1 through the gas assembly until the pressure in the processing bin 1 is 2 multiplied by 101Pa; the gas cylinder filled with the mixed gas is closed, the compressor and the gas filter in the inert gas closed loop system are opened, and the pressure in the processing bin 1 is ensured to be constant at 2 multiplied by 101Pa, oxygen probe 5 showed an oxygen content below 50 ppm.
And 7: and starting a driver to drive the consumable electrode 2 to rotate at an ultra high speed of 32000rpm, starting a plasma gun controller to generate a plasma arc 4 with power of 55kw, heating the end face of the consumable electrode 2 by the plasma arc 4 to melt the consumable electrode 2 to form a liquid level, throwing the liquid level out of the end face of the consumable electrode 2 under the action of centrifugal force, and rapidly solidifying the thrown molten drop into spherical metal powder in the motion process.
And 8: and (3) screening and packaging the metal powder prepared in the step (7) in a high-purity inert gas environment: sieving the powder into powder with the particle size of 45-75 mu m, wherein the average sphericity of the powder is 98.5% as detected by a dynamic image analysis method, and the oxygen content of the TiAl4822 alloy powder is 40ppm as detected by an oxygen-nitrogen-hydrogen analyzer.
Example 3:
the invention provides a preparation method of high-sphericity low-oxygen content TiAl alloy powder, which is implemented by the following steps:
step 1: performing vacuum induction melting for four times, and casting to obtain a TiAl4722 alloy bar; the TiAl4722 alloy comprises the following components in percentage by weight:
28wt.% Al, 45ppm O, balance Ti and inevitable impurity elements.
Step 2: performing high-temperature phase change treatment on the bar prepared in the step 1, namely performing phase change treatment on the bar prepared in the step 1 under the condition that the vacuum degree is 8.5 multiplied by 10-3Heating to 1330 ℃ in a Pa vacuum environment, preserving heat for 3 hours, and performing water quenching and cooling; tempering treatment in vacuum environment, namely heating to 1320 ℃, preserving heat for 3h, and carrying out furnace cooling and high-temperature phase change treatment.
And step 3: and (4) finely turning the bar subjected to the high-temperature phase change treatment in the step (2).
And 4, step 4: and (4) taking the finish-machined bar material prepared in the step (3) as a consumable electrode 2 and placing the consumable electrode in a processing bin 1 of a powder making device.
And 5: opening the valve a, the valve d and the mechanical pump in the vacuum system until the vacuum gauge e displays that the vacuum degree reaches 10-1Pa; the diffusion pump, the valve c and the valve b are opened until the vacuum gauge g displays that the vacuum degree reaches 10-2Pa; starting the titanium sublimation pump until the vacuum degree is lower than 10 as shown by the vacuum gauge f-3Pa; and closing the valves a, b, c and d.
Step 6: filling volume into the processing chamber 1 by a gas assemblyThe mixed gas of argon and helium with the ratio of 1:9 is added until the pressure in the processing bin 1 is 2 multiplied by 101Pa; the gas cylinder filled with the mixed gas is closed, the compressor and the gas filter in the inert gas closed loop system are opened, and the pressure in the processing bin 1 is ensured to be constant at 2 multiplied by 101Pa, oxygen probe 5 showed an oxygen content below 50 ppm.
And 7: and starting a driver to drive the consumable electrode 2 to rotate at a high speed of 31000rpm, starting a plasma gun controller to generate a plasma arc 4 with the power of 56kw, heating the end face of the consumable electrode 2 by the plasma arc 4 to melt the consumable electrode 2 to form a liquid level, throwing the liquid level out of the end face of the consumable electrode 2 under the action of centrifugal force, and rapidly solidifying the thrown molten drop into spherical metal powder in the motion process.
And 8: and (3) screening and packaging the metal powder prepared in the step (7) in a high-purity inert gas environment: sieving the powder into powder with the particle size of 25-90 mu m, detecting the average sphericity of the powder to be 99% by a dynamic image analysis method, and detecting the oxygen content of the Ti2AlNb alloy powder to be 45ppm by an oxygen-nitrogen-hydrogen analyzer.
TiAl alloy is poor in intrinsic brittleness, cracks are easy to occur in the forging or drawing process, the traditional bar manufacturing mode is only casting molding after smelting, the casting process is influenced by multiple factors such as cooling rate, the internal structure of the alloy is thick and has strong dendritic crystals, the aggregation degree of defects and impurity elements at crystal boundaries is high, the melting point is relatively low in the crystal interior, the crystal boundaries are preferentially melted in the centrifugal atomization process, thick crystal grains and the strong dendritic crystals can inevitably form large-size molten drops, the large-size molten drops are easy to deform and solidify into non-spherical powder, the smaller the crystal grains after tissue refinement, the smaller the molten drops are, the faster the cooling speed is, the higher the corresponding spheroidizing rate is, and the better the sphericity of the formed powder is.
In the process, the consumable electrode rotates at a super high speed of 30000-33000 rpm, and according to the following formula, under the condition that the material and the diameter of the consumable electrode are determined, the larger the rotation speed of the consumable electrode is, the smaller the size of the obtained molten drop is, the smaller the deformation of the corresponding fine molten drop in the rapid solidification process is, and the better the sphericity of the powder is.
Wherein: omega is the rotation speed of the consumable electrode, D is the diameter of the consumable electrode, rho is the density of the consumable electrode, gamma is the surface tension of the molten drop, and D is the diameter of the powder particles.
The titanium sublimation pump designed by the ultrahigh vacuum system takes titanium as an air suction material, adsorbs oxygen in the processing bin 1, and simultaneously ensures that the vacuum degree in the processing bin 1 is extremely low (lower than 10) by combining a diffusion pump with high pumping speed-3Pa), because the oxygen content in the processing bin 1 is mainly determined by a vacuum system, and the inert gas closed-loop system ensures that the processing bin 1 is in a positive pressure environment in the processing process, so that the outside air cannot be sucked into the processing bin 1, and the oxygen content in the processing bin 1 is ensured to be lower than 50 ppm.
The foregoing are merely exemplary embodiments of the present invention, which enable those skilled in the art to understand or practice the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention.
It is to be understood that the present invention is not limited to what has been described above, and that various modifications and changes may be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.
Claims (7)
1. A preparation method of high-sphericity low-oxygen content TiAl alloy powder is characterized by comprising the following steps: s1, carrying out vacuum induction melting at least twice, and casting to obtain a TiAl alloy bar;
s2, performing high-temperature phase change treatment on the bar prepared in the step S1;
s3, machining the bar processed in the step S2 to obtain a finished bar;
s4, taking the finished bar material prepared in the step S3 as a consumable electrode (2), and placing the consumable electrode (2) in a processing bin (1);
s5, opening a vacuum system pump set and a vacuum valve,so that the vacuum degree in the processing bin (1) is lower than 10-3Pa, closing a pump set and a vacuum valve of the vacuum system;
s6, filling the mixed gas of argon and helium into the processing bin (1) until the pressure in the processing bin (1) is 2x 101Pa, the oxygen content is lower than 50ppm, the gas cylinder filled with the mixed gas is closed, and the inert gas closed-loop system is opened;
s7, starting a driver so that the driver drives the consumable electrode (2) to rotate at a speed of 30000-33000 rpm, starting a plasma gun controller to generate a plasma arc (4) with power of 50-60 kw, heating the end face of the consumable electrode (2) rotating at a high speed by the plasma arc (4) so that the consumable electrode is melted to form a liquid surface and a metal molten drop is formed, and quickly solidifying the metal molten drop into TiAl alloy spherical metal powder;
s8, screening and packaging the metal powder prepared in the step S7 under the environment of high-purity inert gas.
2. The method according to claim 1, wherein the high temperature phase transition treatment in step S2 is performed under vacuum with a degree of vacuum of less than 10-2Heating to 1330-1350 ℃ at Pa, preserving heat for 1-4 h, and cooling by water quenching; and then tempering in a vacuum environment, namely heating to 1300-1320 ℃, preserving heat for 1-4 h, and cooling in a furnace.
3. The preparation method according to claim 1, wherein the sphericity of the TiAl alloy spherical metal powder in the step S7 is not less than 98%, and the oxygen content of the TiAl alloy spherical metal powder is less than 50 ppm.
4. The equipment for realizing the preparation method of the TiAl alloy powder with high sphericity and low oxygen content according to claim 1, wherein the equipment comprises a processing bin (1), a driver for driving a consumable electrode (2) to rotate is arranged on the processing bin (1), a plasma gun is arranged at a position corresponding to the driver, the plasma gun is controlled by a plasma gun controller, a vacuum system pump set is connected to the processing bin (1), and the vacuum system pump set is connected with an oxygen probe (5) arranged on the processing bin (1) through a control system.
5. The equipment according to claim 4, characterized in that the processing bin (1) is further provided with an inert gas closed loop system, the inert gas closed loop system comprises a gas circulation pipeline (3), the input end and the output end of the gas circulation pipeline (3) are respectively connected with the processing bin (1), and a gas filter and a compressor are sequentially connected on the gas circulation pipeline (3).
6. The apparatus according to claim 4, characterized in that the vacuum system pump set comprises a mechanical pump and a diffusion pump connected to the processing silo (1), both of which are connected to the control system.
7. The apparatus according to claim 4, characterized in that a titanium sublimation pump is connected between the processing bin (1) and the diffusion pump, and the titanium sublimation pump is connected with a control system.
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|---|---|---|---|---|
| CN114749678A (en) * | 2022-03-02 | 2022-07-15 | 北京科技大学 | Preparation method for gamma-based high-temperature TiAl composite material coaxial powder feeding 3D printing |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02156003A (en) * | 1988-12-07 | 1990-06-15 | Nippon Steel Weld Prod & Eng Co Ltd | Manufacture of alloy powder containing titanium-aluminum intermetallic compound |
| JPH0797607A (en) * | 1993-09-29 | 1995-04-11 | Takeshi Masumoto | Amorphous metallic hyper fine particle and production thereof |
| CN101259536A (en) * | 2008-04-23 | 2008-09-10 | 北京科技大学 | Method for preparing high niobium containing titanium aluminium alloy powder |
| CN104308167A (en) * | 2014-09-25 | 2015-01-28 | 西安欧中材料科技有限公司 | Preparation method of IN718 alloy spherical powder |
| CN104357783A (en) * | 2014-10-20 | 2015-02-18 | 中国人民解放军装甲兵工程学院 | Titanium-aluminum alloy powder material for thermal spraying and preparation method thereof |
| CN104550991A (en) * | 2015-01-12 | 2015-04-29 | 西南交通大学 | Preparation method for titanium-aluminum alloy superfine powder |
| CN105689730A (en) * | 2016-02-24 | 2016-06-22 | 西安欧中材料科技有限公司 | Method for preparing Inconel 625 alloy spherical powder |
| CN106853535A (en) * | 2016-12-19 | 2017-06-16 | 西安欧中材料科技有限公司 | A kind of preparation method of high-quality γ TiAl spherical powders |
| CN111618310A (en) * | 2020-06-04 | 2020-09-04 | 四川容克斯科技有限公司 | Spherical vanadium alloy powder and preparation method and application thereof |
| CN111734826A (en) * | 2020-07-23 | 2020-10-02 | 西安赛隆金属材料有限责任公司 | Composite sealing assembly, plasma rotating electrode atomization powder making equipment and powder making method |
| CN112575221A (en) * | 2020-11-24 | 2021-03-30 | 钢铁研究总院 | TiAl alloy powder and preparation method and application thereof |
-
2021
- 2021-09-07 CN CN202111040685.9A patent/CN113492213B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02156003A (en) * | 1988-12-07 | 1990-06-15 | Nippon Steel Weld Prod & Eng Co Ltd | Manufacture of alloy powder containing titanium-aluminum intermetallic compound |
| JPH0797607A (en) * | 1993-09-29 | 1995-04-11 | Takeshi Masumoto | Amorphous metallic hyper fine particle and production thereof |
| CN101259536A (en) * | 2008-04-23 | 2008-09-10 | 北京科技大学 | Method for preparing high niobium containing titanium aluminium alloy powder |
| CN104308167A (en) * | 2014-09-25 | 2015-01-28 | 西安欧中材料科技有限公司 | Preparation method of IN718 alloy spherical powder |
| CN104357783A (en) * | 2014-10-20 | 2015-02-18 | 中国人民解放军装甲兵工程学院 | Titanium-aluminum alloy powder material for thermal spraying and preparation method thereof |
| CN104550991A (en) * | 2015-01-12 | 2015-04-29 | 西南交通大学 | Preparation method for titanium-aluminum alloy superfine powder |
| CN105689730A (en) * | 2016-02-24 | 2016-06-22 | 西安欧中材料科技有限公司 | Method for preparing Inconel 625 alloy spherical powder |
| CN106853535A (en) * | 2016-12-19 | 2017-06-16 | 西安欧中材料科技有限公司 | A kind of preparation method of high-quality γ TiAl spherical powders |
| CN111618310A (en) * | 2020-06-04 | 2020-09-04 | 四川容克斯科技有限公司 | Spherical vanadium alloy powder and preparation method and application thereof |
| CN111734826A (en) * | 2020-07-23 | 2020-10-02 | 西安赛隆金属材料有限责任公司 | Composite sealing assembly, plasma rotating electrode atomization powder making equipment and powder making method |
| CN112575221A (en) * | 2020-11-24 | 2021-03-30 | 钢铁研究总院 | TiAl alloy powder and preparation method and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114749678A (en) * | 2022-03-02 | 2022-07-15 | 北京科技大学 | Preparation method for gamma-based high-temperature TiAl composite material coaxial powder feeding 3D printing |
| CN114749678B (en) * | 2022-03-02 | 2022-11-15 | 北京科技大学 | Preparation method for gamma-based high-temperature TiAl composite material coaxial powder feeding 3D printing |
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