CN115007869A - Preparation method of titanium-aluminum powder for powder metallurgy with service temperature of 850 DEG C - Google Patents
Preparation method of titanium-aluminum powder for powder metallurgy with service temperature of 850 DEG C Download PDFInfo
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- 238000004663 powder metallurgy Methods 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 249
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- 238000000034 method Methods 0.000 claims abstract description 78
- 238000002844 melting Methods 0.000 claims abstract description 52
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- 239000001301 oxygen Substances 0.000 claims abstract description 18
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- 239000010949 copper Substances 0.000 claims description 10
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- 230000009471 action Effects 0.000 claims description 8
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- 244000046052 Phaseolus vulgaris Species 0.000 claims description 6
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
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Classifications
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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
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
-
- 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
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T50/00—Aeronautics or air transport
- Y02T50/60—Efficient propulsion technologies, e.g. for aircraft
Abstract
A preparation method of titanium-aluminum powder for powder metallurgy with the service temperature of 850 ℃ is characterized in that medium-content Nb and a small amount of Ta are added into peritectic TiAl alloy to improve the performance of the TiAl alloy and realize the tissue refinement and strengthening and toughening. And (3) adding Nb and Ta elements in the form of Nb powder and Ta powder by vacuum arc melting to obtain the casting alloy with uniform components. The powder metallurgy forming process can avoid component segregation caused by adding Nb and Ta and further refine the grain structure. The high sphericity of the powder obtained by the invention is beneficial to improving the compactness of a powder metallurgy part, the low content of impurities and the low content of hollow powder are both beneficial to reducing potential crack sources of the powder metallurgy part, and the low content of oxygen is beneficial to improving the high-temperature mechanical property of the material, so that the TiAl- (Nb, Ta) metal powder can meet the high-temperature service requirement of 850 ℃ after powder metallurgy forming and heat treatment tissue regulation.
Description
Technical Field
The invention relates to the field of powder metallurgy light high-temperature materials, in particular to a preparation method of metal powder for powder metallurgy titanium-aluminum alloy with the service temperature of 850 ℃.
Background
The TiAl alloy has excellent performances of high specific strength, high creep resistance, excellent oxidation resistance and the like, and the density of the TiAl alloy is only half of that of the nickel-based high-temperature alloy, so the TiAl alloy is considered to be an optimal candidate material for replacing the nickel-based high-temperature alloy within the range of 800-900 ℃ and realizing weight reduction and efficiency improvement. In 2012, a GEnx engine made of Ti4822 alloy (Ti-48Al-2Cr-2Nb) cast low-pressure turbine blades formally starts commercial flight on a Boeing 787 passenger plane, marks that the TiAl alloy is applied in the field of aerospace active equipment after more than 30 years of engineering development. Immediately thereafter, the forged TNM alloy (Ti-43Al-4Nb-1Mo-0.1B) developed in the European Union was also applied to the airbus A320 passenger aircraft engine and successfully carried on the first flight. In addition, the application process of the cast XD alloy (Ti-48Al-2Mn-2Nb-1B) in the field of aeroengines is also rapidly advancing. However, the service temperature of the TiAl alloy is about 700 ℃, and the development and application of the novel TiAl alloy are restricted by the insufficiency of high-temperature mechanical property.
The solid-to-liquid ratio of the over-peritectic TiAl alloy is 1:1, feeding can be carried out, so that casting defects are few, and the over-peritectic solidified TiAl alloy has optimal room-temperature plasticity. Alloying is a common means for improving the performance of the TiAl alloy, and the addition of alloy elements can influence the microstructure of the TiAl alloy, thereby changing the room temperature plasticity, the high temperature strength, the oxidation resistance, the creep resistance and the like of the TiAl alloy. Nb and Ta belong to VB group, the high-temperature strength, creep resistance and oxidation resistance of the TiAl alloy can be improved, in addition, Ta can relax the metastable phase transition cooling rate condition of the peritectic TiAl alloy, and the grain refinement is realized through metastable structure evolution. However, both Nb and Ta are easy to cause component segregation to influence the material performance, and high alloying is more obvious. The addition of the medium content of Nb in the TiAl alloy can obviously improve the component segregation and ensure that the alloy keeps good mechanical properties. A proper amount of Ta is added into the over-peritectic TiAl alloy, and the formation of various metastable structures can be promoted by reducing the substructure energy, so that the grain refinement and the strengthening and toughening are realized. Therefore, the addition of Nb and Ta is expected to increase the service temperature of the TiAl alloy to 850 ℃.
Powder metallurgy is an effective technological means for realizing grain refinement and performance improvement of materials, can avoid the defects of component segregation, inconsistent tissue and the like in the ingot metallurgy process, can eliminate looseness and shrinkage cavity, can directly prepare near-net-shaped products, and has more remarkable forming advantages for TiAl alloys with poor plasticity and difficult processing.
The high-quality metal powder is a premise of a powder metallurgy material with excellent performance, however, the titanium-aluminum alloy powder prepared by the prior art is difficult to meet the requirement of higher use temperature of the titanium-aluminum alloy in component design, and the powder has poor performance in the aspects of sphericity, hollow powder rate, oxygen content and the like, thereby affecting the comprehensive mechanical properties of the powder metallurgy part.
The invention with the application number of 2020113279653 discloses TiAl alloy powder and a preparation method and application thereof. The titanium-aluminum alloy disclosed in the invention comprises the following chemical components: al: 34% -35%, Nb: 4.5% -5.1%, Cr: 2.4% -2.7%, Gd: 0 to 0.02%, C: greater than 0 and not greater than 150ppm, N: greater than 0 and not greater than 200ppm, H: greater than 0 and not greater than 100ppm, O: more than 0 and not more than 700ppm, the balance Ti, the preparation method is a plasma rotating electrode method, the main parameters are current 1700-1900A, rotating speed 15000-25000r/min, and the powder is applied to the additive manufacturing of the electron beam powder bed. The components of the method are different from those of the invention, and the method has no potential of grain refinement, high temperature performance improvement and service temperature increase, the TiAl alloy which is different from the method and is not suitable for the components of the invention has disadvantages in the aspects of powder granularity, hollow powder, oxygen increase control and the like, the application is only limited to the molding mode of electron beam powder bed additive manufacturing, and the application range is different from that of the invention.
The invention with the application number of 201611174413 discloses a preparation method of high-quality gamma TiAl spherical powder, which discloses titanium-aluminum alloy chemical components as follows: al: 20-40 wt%, Nb: 10-20 wt% of Ti as a matrix, and 0-10 wt% of B, V, Cr, W and Y alloy elements, wherein the chemical components of the method are different from those of the invention, and the method has no potential of grain refinement, high temperature performance improvement and service temperature increase.
The invention with the application number of 2020114370993 discloses rare earth modified TiAl alloy powder for additive manufacturing and a preparation method thereof. The method comprises the steps of pretreating a TiAl alloy, a Zr simple substance and an Al-Sc intermediate alloy, adding the Zr simple substance or the Al-Sc intermediate alloy in the TiAl alloy atomizing smelting process, and screening and grading to obtain the TiAl alloy powder meeting the material increase manufacturing process requirements. The invention with the application number of 2018112985873 discloses laser cladding coating powder and a preparation method thereof, and does not particularly relate to a preparation method of TiAl powder. The invention with the application number of 2017103676522 discloses a method for forming fine-grain titanium-aluminum powder, and TiAl powder used is a preparation method of elemental powder of Ti, Al and the like or gas atomization TiAl alloy powder. The TiAl powder disclosed by the invention is different from the components disclosed by the invention, different in preparation method and different in expected application, the components do not have the potential of grain refinement, high-temperature performance improvement and service temperature improvement, the key characteristics of powder such as powder granularity, hollow powder and oxygen increment are not described in detail or obvious disadvantages exist, and the TiAl alloy meeting the service requirement of 850 ℃ cannot be obtained through powder metallurgy forming and heat treatment tissue regulation.
In the invention creation application No. 2017103051776, a cast γ -TiAl alloy suitable for use at 800 ℃ is disclosed. The TiAl alloy is added with Nb and Ta elements with higher density, and the casting alloy has the phenomena of component segregation and nonuniform structure which are difficult to avoid, influences the application of materials, and is difficult to realize long-time high-temperature service and further improve the service temperature. The powder metallurgy method can well improve the phenomenon of uneven components and structures caused by the ingot metallurgy process and improve the service performance of the material, and the preparation method of the high-quality metal powder is the premise of the high-performance powder metallurgy material, namely the preparation method of the metal powder for the powder metallurgy TiAl alloy with the service temperature of 850 ℃. In addition, the method adds B element in the cast TiAl alloy, which can increase the room temperature brittleness of the TiAl alloy and is difficult to machine and add the bar material required by the powder making process (SS-PREP) of the plasma rotating electrode with ultrahigh rotating speed.
At present, no research reports about a preparation method of metal powder for powder metallurgy TiAl- (Nb, Ta) alloy at a service temperature of 850 ℃ such as domestic and foreign patents, academic papers and the like are searched.
Disclosure of Invention
In order to overcome the defect that the TiAl alloy in the prior art cannot meet the service requirement of 850 ℃ in the aspects of component design, physical characteristics, tissue regulation potential and the like, the invention provides a preparation method of titanium-aluminum powder for powder metallurgy with the service temperature of 850 ℃.
The specific process of the invention is as follows:
step 1, pressing a TiAl- (Nb, Ta) alloy electrode:
preparing materials according to the components of the TiAl- (Nb, Ta) alloy, uniformly mixing in a mixer, and pressing in an oil press to obtain a TiAl- (Nb, Ta) alloy electrode;
the TiAl- (Nb, Ta) alloy comprises 40-60 wt% of Ti, 30-32 wt% of Al, 5.5-7.5 wt% of Nb and 4.4-8.7 wt% of Ta.
The Nb powder and the Ta powder are both powdery, the Nb powder is-325 meshes, the Ta powder is-325 meshes, Ti is added in the form of sponge titanium, and Al is added in the form of aluminum beans.
When the TiAl- (Nb, Ta) alloy electrode is pressed, the volatile burning loss of Al element in the smelting process is considered, and the Al element is compensated and increased by 2-8 wt% on the basis of a target value of 30-32 wt% in the material mixing process.
Step 2, preparing TiAl- (Nb, Ta) alloy ingot;
placing the TiAl- (Nb, Ta) alloy electrode in a vacuum arc melting furnace for melting; the smelting process is carried out for three times, electromagnetic stirring is adopted, and the method specifically comprises the following steps:
the first smelting is carried out, the vacuum degree of the vacuum arc melting furnace is 3 multiplied by 10 -3 Pa～3×10 -2 Pa, 2200-2500A of current, 20-40V of voltage and 30-55 mm/min of melting speed. And continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer.
The vacuum degree of the vacuum arc melting furnace is 3 multiplied by 10 for the second melting -3 Pa～3×10 -2 Pa, 2200-2500A of current, 20-40V of voltage and 35-60 mm/min of melting speed. And continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer.
The third smelting is carried out, the vacuum degree of the vacuum arc smelting furnace is 3 multiplied by 10 -3 Pa～3×10 -2 Pa, 2200-2500A of current, 20-40V of voltage and 40-65 mm/min of melting speed. And continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer.
Obtaining TiAl- (Nb, Ta) alloy cast ingots.
In the third smelting process, the current of the electromagnetic stirrer is 20-120A, and the frequency of the electromagnetic stirrer is 1-10 Hz. The flow of the cooling water is 1-10 m 3 The temperature is 10-35 ℃ per hour.
After the smelting is finished and the furnace is opened to take out the cast ingot, cleaning each slit of the copper crucible to prevent the condensed shell from excessively wetting the slit in the next smelting.
In the TiAl- (Nb, Ta) alloy ingot, Ti accounts for 40-60%; 30-32% of Al; 5.5 to 7.5 percent of Nb; ta is 4.4-8.7%, and the sum of the mass percentages of the components is 100%.
Step 3, preparing TiAl- (Nb, Ta) alloy bar blank
And carrying out homogenization annealing on the obtained TiAl- (Nb, Ta) alloy ingot.
And placing the TiAl- (Nb, Ta) alloy ingot into a heat treatment furnace. Heating the heat treatment furnace to 1200-1420 ℃, and preserving heat for 1-30 h; and after the heat preservation is finished, cooling along with the furnace. And obtaining the TiAl- (Nb, Ta) alloy ingot after homogenization annealing.
Cutting off a riser of the annealed TiAl- (Nb, Ta) alloy ingot; obtaining a blank of the TiAl- (Nb, Ta) alloy rod by wire cutting;
step 4, finely turning a TiAl- (Nb, Ta) alloy rod blank;
step 5, preparing SS-PREP powder making atmosphere:
placing the obtained TiAl- (Nb, Ta) alloy rod blank in a reaction furnace; the reaction chamber is evacuated to 10 deg.C -3 Pa～10 -1 Pa; and filling helium-argon mixed gas into the reaction chamber to ensure that the pressure of the helium-argon mixed gas is 0.01-2 MPa, thereby obtaining the ambient atmosphere in the atomization chamber required by the powder preparation process.
Step 6, preparing TiAl- (Nb, Ta) alloy powder:
heating the end part of the TiAl- (Nb, Ta) alloy bar blank by using plasma; uniformly melting the end part of the TiAl- (Nb, Ta) alloy rod, throwing atomized liquid drops out of the end part of the TiAl- (Nb, Ta) alloy rod under the action of centrifugal force to form fine liquid drops, rapidly cooling the liquid drops in an inert gas environment to form spherical particles, and falling into a collector at the bottom of a reaction chamber to obtain the full-granularity TiAl- (Nb, Ta) alloy powder.
Heating the end part of the TiAl- (Nb, Ta) alloy rod by using plasma to uniformly melt the end part of the TiAl- (Nb, Ta) alloy rod, throwing atomized liquid drops out of the end part of the TiAl- (Nb, Ta) alloy rod under the action of centrifugal force to form fine liquid drops, rapidly cooling the liquid drops in an inert gas environment to form spherical particles, and falling into a collector at the bottom of a reaction chamber to obtain the full-granularity TiAl- (Nb, Ta) alloy powder.
The power of the plasma gun is 100 kW-250 kW; the rotation speed of the TiAl- (Nb, Ta) alloy rod is 20000r/min to 35000 r/min.
And 7, post-treating the TiAl- (Nb, Ta) alloy powder:
screening, shaping and mixing the obtained TiAl- (Nb, Ta) alloy powder in an inert gas protection environment during post-treatment;
and in the screening, the obtained full-granularity TiAl- (Nb, Ta) alloy powder is subjected to granularity screening by using a square-hole woven screen with the aperture consistent with the required powder specification to obtain metal powder with the particle size suitable for a corresponding powder metallurgy forming process, wherein an ultrasonic generator is required to be started in the screening process to improve the screening effect, and the powder feeding rate is less than 5 kg/min.
And the shaping is to sequentially pass the sieved powder through 2 round hole plate sieves with the hole diameter size not smaller than the upper limit of the required powder specification to treat the metal powder so as to remove the special-shaped powder, and obtain TiAl- (Nb, Ta) alloy powder with the optimal sphericity, wherein the addition of the powder in single treatment is not more than 3kg, and the vibration treatment is not less than 5 min.
And the mixing is to put the shaped powder into a mixer for mixing treatment so as to ensure that the powder is uniformly distributed in different thicknesses, wherein the single addition amount is not more than 200kg, and the mixing treatment is not less than 2 hours.
Obtaining the titanium-aluminum powder for powder metallurgy with the service temperature of 850 ℃.
The hollow powder rate of the titanium-aluminum powder for powder metallurgy with the service temperature of 850 ℃ is less than 0.1 percent, the sphericity is more than 95 percent, and the tap density is more than 2.7g/cm 3 The Hall flow rate is less than or equal to 27s/50g, the oxygen content is less than or equal to 800ppm, and the average particle size is 50-150 mu m.
The invention solves the defects of the existing TiAl powder in the aspects of component design, physical characteristics, tissue regulation potential and the like.
The technical scheme adopted by the invention is that,
the TiAl alloy consists of Ti, Al, Nb and Ta, wherein the weight ratio of Ti: 40-60 wt%; al: 30-32 wt%; nb: 5.5-7.5 wt%; ta: 4.4-8.7 wt%. Fe impurities can be introduced into the TiAl alloy in the smelting process, wherein Fe is less than or equal to 0.08 wt%. The TiAl alloy can introduce O impurities in the smelting and powder preparation processes, wherein O is less than or equal to 0.08 wt%.
The invention adds proper amount of Nb and Ta, namely 5.5-7.5 wt% of Nb and 4.4-8.7 wt% of Ta, on the basis of the peritectic TiAl alloy with 30-32 wt% of Al content. Nb and Ta can improve the high-temperature strength, creep resistance and oxidation resistance of the TiAl alloy, the Ta has more obvious improvement effect than Nb, and in addition, Ta element can also relax the metastable phase transition cold rate condition of peritectic TiAl alloy, and grain refinement is realized through metastable structure evolution. However, both Nb and Ta are also prone to cause component segregation and affect material properties, high alloying is more obvious, and addition of a large amount of Ta increases alloy density and cost, so that excessive addition is not desirable from an engineering perspective.
TiAl- (Nb, Ta) alloy ingots with uniform components and few internal defects are obtained by vacuum arc consumable melting, wherein Nb and Ta elements are added in the form of Nb powder and Ta powder, so that the Nb and Ta elements are distributed more uniformly, and the component segregation generated in the melting process is further avoided. TiAl- (Nb, Ta) alloy bars with high appearance precision are prepared by finish turning and finish grinding, TiAl- (Nb, Ta) metal powder is prepared by using an ultrahigh rotating speed plasma rotating electrode process (SS-PREP), the powder is classified by a metal woven screen, the powder is shaped by a metal plate screen, the particle size distribution homogenization treatment is carried out by a mixer, wherein the whole process of smelting, milling, screening, shaping, mixing and packaging is carried out under vacuum or inert atmosphere, the TiAl- (Nb, Ta) alloy powder with uniform tissue components, less hollow powder, low oxygen content, high sphericity and less impurities can be prepared, the requirements of different powder metallurgy processes such as hot isostatic pressing, electron beam powder bed melting, hot pressing, discharge and the like can be met by screening and grading, the problem of component segregation caused by adding Nb and Ta can be reduced and TiAl alloy with uniform and fine component structure can be obtained by powder metallurgy forming, fine full lamellar structure can be obtained after the heat treatment structure is regulated, and the formed part can meet the application requirement of 850 ℃ service.
The invention has the beneficial effects that:
the medium-content Nb and a small amount of Ta are added into the peritectic TiAl alloy, so that the high-temperature strength, creep resistance and oxidation resistance of the TiAl alloy can be improved, the high-content Al element and the small amount of Ta element in the peritectic TiAl alloy act together, the formation energy of gamma-phase metastable tissues is reduced, favorable conditions are provided for rich metastable tissue evolution and tissue regulation, and tissue refinement and toughening can be realized. And (3) adding Nb and Ta elements in the form of Nb powder and Ta powder by vacuum arc melting to obtain the casting alloy with uniform components. The powder metallurgy forming process can avoid component segregation caused by adding Nb and Ta and can further refine the grain structure. The premise of the high-performance powder metallurgy material is a high-quality metal powder raw material, so the high-quality TiAl- (Nb, Ta) metal powder prepared by the method has the potential of subsequent tissue regulation and control in component design, has the advantages of uniform components, less hollow powder, low oxygen content, high sphericity and less impurities, and lays a foundation for the uniform components of subsequent powder metallurgy parts, the high sphericity is favorable for improving the compactness of the powder metallurgy parts, the less impurities and the less hollow powder are favorable for reducing the potential crack sources of the powder metallurgy parts, and the low oxygen content is favorable for improving the high-temperature mechanical property of the material.
Drawings
FIG. 1 is a scanning electron micrograph of the present invention; FIG. 1a is a photograph showing the appearance of the powder, and FIG. 1b is a photograph showing the cross-section of the powder, as shown, the powder is excellent in sphericity and free from impurities.
FIG. 2 is the results of an energy line sweep analysis of the present invention; fig. 2a is a schematic diagram of the cross-sectional morphology and the line scanning area of the powder, and fig. 2b is a result of the component line scanning, in which 1 is Ti element, 2 is Al element, 3 is Nb element, 4 is Ta element, and 5 is C element, and the fluctuation of the composition curve is small, and it can be seen that the components are uniformly distributed.
FIG. 3 shows the result of Mapping analysis of the energy spectrum of the present invention; FIG. 3a shows the distribution of Ti element, FIG. 3b shows the distribution of Al element, FIG. 3c shows the distribution of Nb element, and FIG. 3d shows the distribution of Ta element, each element being uniformly distributed.
FIG. 4 shows the results of Micro-CT tomography according to the present invention; fig. 3a is a schematic cross-sectional view and fig. 3b is a schematic three-dimensional view, and it can be seen that there is little hollow powder.
FIG. 5 shows the EBSD analysis results of the present invention: FIG. 5a is a phase composition diagram, and FIG. 5b is a grain orientation diagram. The TiAl- (Nb, Ta) powder being mainly alpha 2 Phase and gamma phase, in which 2 The phases are abundant. There are a plurality of grains of different orientations within the powder particles, the grain size being 70-80 μm.
FIG. 6 is a flow chart of the present invention
Detailed Description
The invention relates to metal powder for powder metallurgy titanium-aluminum alloy with the service temperature of 850 ℃, which comprises the following specific steps:
step 1, pressing a TiAl- (Nb, Ta) alloy electrode:
preparing materials according to the components of the TiAl- (Nb, Ta) alloy, uniformly mixing in a mixer, and pressing in an oil press to obtain a TiAl- (Nb, Ta) alloy electrode;
the TiAl- (Nb, Ta) alloy comprises 40-60 wt% of Ti, 30-32 wt% of Al, 5.5-7.5 wt% of Nb and 4.4-8.7 wt% of Ta.
The Nb powder and the Ta powder are both powdery, the Nb powder is-325 meshes, the Ta powder is-325 meshes, Ti is added in the form of sponge titanium, and Al is added in the form of aluminum beans.
Considering the easily volatile burning loss of Al element in the smelting process, the Al element is compensated and increased by 2-8 wt% on the basis of a target value of 30-32 wt% during material preparation.
Step 2, preparing TiAl- (Nb, Ta) alloy ingot;
placing the obtained TiAl- (Nb, Ta) alloy electrode in a vacuum arc melting furnace for melting; the smelting process is carried out for three times, electromagnetic stirring is adopted, and the method specifically comprises the following steps:
the first smelting is carried out, the vacuum degree of the vacuum arc melting furnace is 3 multiplied by 10 -3 Pa～3×10 -2 Pa, 2200-2500A of current, 20-40V of voltage and 30-55 mm/min of melting speed. And continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer.
The current of the electromagnetic stirrer is 20-120A, and the frequency of the electromagnetic stirrer is 1-10 Hz.
The flow of the cooling water is 1-10 m 3 The temperature is 10-35 ℃.
And after the smelting is finished and the furnace is opened to take out the cast ingot, cleaning each slit of the copper crucible to prevent the condensed shell from excessively wetting the slit in the next smelting.
The second smelting is carried out, the vacuum degree of the vacuum arc melting furnace is 3 multiplied by 10 -3 Pa～3×10 -2 Pa, 2200-2500A of current, 20-40V of voltage and 35-60 mm/min of melting speed. And continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer.
The current of the electromagnetic stirrer is 20-120A, and the frequency of the electromagnetic stirrer is 1-10 Hz.
The flow of the cooling water is 1-10 m 3 The temperature is 10-35 ℃.
And after the smelting is finished and the furnace is opened to take out the cast ingot, cleaning each slit of the copper crucible to prevent the condensed shell from excessively wetting the slit in the next smelting.
The third smelting is carried out, the vacuum degree of the vacuum arc smelting furnace is 3 multiplied by 10 -3 Pa～3×10 -2 Pa, 2200-2500A of current, 20-40V of voltage and 40-65 mm/min of melting speed. And continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer.
The current of the electromagnetic stirrer is 20-120A, and the frequency of the electromagnetic stirrer is 1-10 Hz.
The flow of the cooling water is 1-10 m 3 The temperature is 10-35 ℃.
In the TiAl- (Nb, Ta) alloy ingot by three times of vacuum melting, the ratio of Ti: 40-60; al: 30-32; nb: 5.5 to 7.5; ta: 4.4 to 8.7, and the sum of the mass percentages of the components is 100 percent.
Step 3, preparing TiAl- (Nb, Ta) alloy bar blank
And carrying out homogenization annealing on the obtained TiAl- (Nb, Ta) alloy ingot.
And placing the TiAl- (Nb, Ta) alloy ingot into a heat treatment furnace. Heating the heat treatment furnace to 1200-1420 ℃, and preserving heat for 1-30 h; and after the heat preservation is finished, cooling along with the furnace. And obtaining the TiAl- (Nb, Ta) alloy ingot after homogenization annealing. The TiAl- (Nb, Ta) alloy ingot is subjected to homogenizing annealing to promote component homogenization and avoid component segregation powder particles generated in the powder making process of a rod material with component segregation.
Cutting off a riser of the annealed TiAl- (Nb, Ta) alloy ingot, and obtaining a TiAl- (Nb, Ta) alloy rod blank with the diameter of 30-60 mm and the length of 300-700 mm by wire cutting;
step 4, finishing the blank of the TiAl- (Nb, Ta) alloy rod
And carrying out finish turning on the obtained blank of the TiAl- (Nb, Ta) alloy rod, wherein the processed TiAl- (Nb, Ta) alloy rod has the following characteristics: the diameter deviation of a single bar is less than 0.1mm, the excircle runout is less than 0.1mm, and the surface roughness is less than 2 mu m.
Step 5, preparing SS-PREP powder making atmosphere:
placing the obtained TiAl- (Nb, Ta) alloy rod blank in a reaction furnace; the reaction chamber is evacuated to 10 deg.C -3 Pa～10 -1 And Pa, filling helium-argon mixed gas into the reaction chamber to ensure that the pressure in the chamber is 0.01-2 MPa, and obtaining the ambient atmosphere in the atomization chamber required by the powder preparation process.
Step 6, preparing TiAl- (Nb, Ta) alloy powder:
the plasma gun power of the SS-PREP powder making equipment is 100 kW-250 kW, the end part of the TiAl- (Nb, Ta) alloy rod is heated by plasma, the rotating speed of the TiAl- (Nb, Ta) alloy rod is 20000 r/min-35000 r/min, so that the end part of the TiAl- (Nb, Ta) alloy rod is uniformly melted, atomized liquid drops are thrown out from the end part of the TiAl- (Nb, Ta) alloy rod under the action of centrifugal force to form fine liquid drops, the liquid drops are rapidly cooled into spherical particles in an inert gas environment and fall into a collector at the bottom of a reaction chamber, and the full-granularity TiAl- (Nb, Ta) alloy powder is obtained.
And 7, post-treating the TiAl- (Nb, Ta) alloy powder:
screening, shaping and mixing the prepared TiAl- (Nb, Ta) alloy powder under the protection of inert gas, wherein the screening is to screen the granularity of the obtained full-granularity TiAl- (Nb, Ta) alloy powder by using a square-hole woven screen with the aperture consistent with the specification of the required powder to obtain metal powder with the granularity suitable for a corresponding powder metallurgy forming process, an ultrasonic generator is required to be started in the screening process to improve the screening effect, and the powder feeding rate is less than 5 kg/min. And the shaping is to sequentially pass the sieved powder through 2 round hole plate sieves with the hole diameter size not smaller than the upper limit of the required powder specification to treat the metal powder so as to remove the special-shaped powder, and obtain TiAl- (Nb, Ta) alloy powder with the optimal sphericity, wherein the addition of the powder in single treatment is not more than 3kg, and the vibration treatment is not less than 5 min. And the mixing is to put the shaped powder into a mixer for mixing treatment, wherein the single addition amount is not more than 200kg, and the mixing treatment is not less than 2 h.
Wherein the hollow powder rate of the TiAl- (Nb, Ta) alloy powder is less than 0.1 percent, the sphericity is more than 95 percent, and the tap density is more than 2.7g/cm 3 The Hall flow rate is less than or equal to 27s/50g, the oxygen content is less than or equal to 800ppm, and the average particle size is 50-150 mu m.
The scanning electron microscope image of the TiAl- (Nb, Ta) alloy powder prepared by the invention is shown in figure 1. As can be seen from fig. 1, the powder has a very good sphericity and is free of any foreign matter. The energy spectrum line scanning result of the TiAl- (Nb, Ta) alloy powder prepared by the method is shown in FIG. 2. As can be seen from fig. 2, the chemical components of the powder are uniformly distributed. The Micro-CT tomography result of the TiAl- (Nb, Ta) alloy powder prepared by the method is shown in figure 3. As can be seen from FIG. 3, there was almost no hollow powder in the powder.
The powder properties are shown in table 1, and it can be seen from table 1 that the TiAl- (Nb, Ta) alloy powder prepared by the method has very excellent sphericity and fluidity, the sphericity of which is greater than 95%, the hall flow rate of 50g of powder is less than 27s, the oxygen content is less than 800ppm, and almost no inclusions exist, while the sphericity of the TiAl- (Nb, Ta) alloy powder prepared by the conventional method is usually less than 85%, the hall flow rate of 50g of powder is greater than 35s, even the powder cannot flow when detected by using a hall flow meter, the oxygen content is usually greater than 1500ppm, the Nb and Ta elements have obvious segregation, and the inclusions are difficult to avoid.
TABLE 1 typical Properties of TiAl- (Nb, Ta) alloy powders prepared by the method
| Specification of powder | 15～45μm | 45～106μm | 106～250μm | 45～250μm |
| Degree of sphericity | 98.8％ | 97.8％ | 97.4％ | 97.8％ |
| Hall flow rate | 26.8s | 23s | 24.2s | 23.9s |
| Oxygen content | 780ppm | 750ppm | 680ppm | 710ppm |
| Hollow powder fraction | 0.01％ | 0.05％ | 0.08％ | 0.07％ |
The super-high-speed plasma rotating electrode powder process (SS-PREP) is a most advanced PREP powder process device abroad, and is independently researched, developed and improved according to the physicochemical characteristics of raw material alloys and expected powder characteristics. The SS-PREP also has special requirements on raw material bars due to the unique production process, and as-cast TiAl- (Nb, Ta) alloy bars prepared by the conventional smelting process have coarse grain structures, ingredient segregation and internal crack defects, and cracks, holes and coarse grains can cause the breakage along the grains in the SS-PREP powder-making super-high-speed rotation process so that the tearing of the bars integrally flies out. Therefore, aiming at the special requirements of the SS-PREP process on the raw material bar, the invention improves the smelting process of the TiAl- (Nb, Ta) alloy so as to ensure that the TiAl- (Nb, Ta) alloy powder meeting the requirements of the powder metallurgy process is obtained.
As Nb and Ta with high melting points are added in the TiAl alloy, in order to avoid the existence of local refractory Nb and Ta segregation structures in the TiAl alloy bar, Nb and Ta segregation powder and even unmelted powder slag are formed in the powder making process, the powder making process of the plasma rotating electrode with ultrahigh rotating speed is improved, so that the TiAl- (Nb, Ta) alloy powder meeting the requirements of the powder metallurgy process is obtained.
The TiAl- (Nb, Ta) alloy powder with high sphericity, good purity, excellent fluidity, low oxygen content, less hollow powder and uniform components can be prepared by preparing a TiAl- (Nb, Ta) alloy bar with uniform component structure, few internal defects and high appearance precision, pulverizing by using an ultrahigh rotating speed plasma rotating electrode process (SS-PREP), combining screening, shaping and mixing treatment, and carrying out the whole processes of smelting, pulverizing, screening, shaping, mixing and packaging in a vacuum or inert atmosphere, the requirements of different powder metallurgy processes such as hot isostatic pressing, additive manufacturing and the like can be met by screening and grading, and the formed part can meet the application requirements of corresponding fields.
The invention can obtain 0-300 mu m TiAl- (Nb, Ta) alloy powder by adjusting process parameters, has high powder sphericity, good purity, excellent fluidity, low oxygen content, less hollow powder and uniform components, and can meet the high-temperature service requirement of 850 ℃ after powder metallurgy forming and heat treatment tissue regulation.
Example 1
The invention relates to metal powder for powder metallurgy titanium-aluminum alloy with the service temperature of 850 ℃, which is implemented by the following steps:
step 1, pressing TiAl- (Nb, Ta) alloy into an electrode:
proportioning according to the components of TiAl- (Nb, Ta) alloy, uniformly mixing in a mixer, and pressing an electrode in an oil press, wherein: ti: 55.3 wt%; al: 31.5 wt%; nb: 6.5 wt%; ta: 6.7 wt%.
The Nb powder and the Ta powder are both powdery, the Nb powder is-325 meshes, the Ta powder is-325 meshes, Ti is added in the form of sponge titanium, and Al is added in the form of aluminum beans.
Considering the easy volatilization and burning loss of Al element in the smelting process, the Al element is compensated and increased by 4.5 wt% on the basis of 31.5 wt% during the material mixing.
Step 2, preparing a TiAl- (Nb, Ta) alloy ingot;
smelting the pressed electrode block welding electrode through a three-time vacuum arc melting furnace, and adopting electromagnetic stirring, wherein the method specifically comprises the following steps:
the first smelting is carried out, the vacuum degree of the vacuum arc melting furnace is 9 multiplied by 10 -3 Pa, current 2300A, voltage 30V, and melting speed 50 mm/min. And continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer.
The current of the electromagnetic stirrer is 100A, and the frequency of the electromagnetic stirrer is 8 Hz.
The flow rate of the cooling water is 5m 3 H, temperature 15 ℃.
And after the smelting is finished and the furnace is opened to take out the cast ingot, cleaning each slit of the copper crucible to prevent the condensed shell from excessively wetting the slit in the next smelting.
The vacuum degree of the vacuum arc melting furnace is 9 multiplied by 10 for the second melting -3 Pa, current 2300A, voltage 30V, and melting speed 55 mm/min. And continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer.
The current of the electromagnetic stirrer is 100A, and the frequency of the electromagnetic stirrer is 8 Hz.
The flow rate of the cooling water is 5m 3 H, temperature 15 ℃.
After the smelting is finished and the furnace is opened to take out the cast ingot, cleaning each slit of the copper crucible to prevent the condensed shell from excessively wetting the slit in the next smelting.
The third smelting is carried out, the vacuum degree of the vacuum arc smelting furnace is 9 multiplied by 10 -3 Pa, current 2300A, voltage 30V, and melting speed 60 mm/min. And continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer.
The current of the electromagnetic stirrer is 100A, and the frequency of the electromagnetic stirrer is 8 Hz.
The flow rate of the cooling water is 5m 3 H, temperature 15 ℃.
And 3, preparing a TiAl- (Nb, Ta) alloy rod blank.
And carrying out homogenization annealing on the obtained TiAl- (Nb, Ta) alloy ingot.
And placing the TiAl- (Nb, Ta) alloy ingot in a heat treatment furnace. Heating the heat treatment furnace to 1400 ℃, and preserving heat for 10 hours; and after the heat preservation is finished, cooling along with the furnace. Obtaining the TiAl- (Nb, Ta) alloy ingot after homogenization annealing.
Cutting off a riser of the annealed TiAl- (Nb, Ta) alloy ingot, and obtaining a TiAl- (Nb, Ta) alloy rod blank with the diameter of 58mm and the length of 600mm by wire cutting;
and 4, preparing a finishing TiAl- (Nb, Ta) alloy rod.
The TiAl- (Nb, Ta) alloy rod blank obtained is subjected to finish turning, and the TiAl- (Nb, Ta) alloy rod after processing has the following characteristics: the diameter deviation of a single bar is less than 0.1mm, the excircle runout is less than 0.1mm, and the surface roughness is less than 2 mu m.
Step 5, SS-PREP powder making atmosphere preparation
Loading TiAl- (Nb, Ta) alloy rods into the reaction chamber, and evacuating the reaction chamber to 8 × 10 -2 Pa, filling helium-argon mixed gas into the reaction chamber, and enabling the pressure in the chamber to be 1.1 MPa.
And 6, preparing TiAl- (Nb, Ta) alloy powder.
The plasma gun power of the SS-PREP powder making equipment is 180kW, the end part of the TiAl- (Nb, Ta) alloy rod is heated by plasma, the rotating speed of the TiAl- (Nb, Ta) alloy rod is 22000r/min, the end part of the TiAl- (Nb, Ta) alloy rod is uniformly melted, atomized liquid drops are thrown out from the end part of the TiAl- (Nb, Ta) alloy rod under the action of centrifugal force to form fine liquid drops, and the liquid drops are rapidly cooled into spherical particles in an inert gas environment and fall into a collector at the bottom of a reaction chamber to obtain full-granularity TiAl- (Nb, Ta) alloy powder.
Step 7, screening, shaping and mixing the prepared TiAl- (Nb, Ta) alloy powder under the protection of inert gas, wherein the screening is to screen the granularity of the obtained full-granularity TiAl- (Nb, Ta) alloy powder by a square-hole woven screen with the aperture of 60 meshes and 325 meshes, an ultrasonic generator is started in the screening process, the powder feeding rate is 4kg/min, the shaping is to process the metal powder by sequentially passing the screened powder through circular-hole plate screens with the apertures of 300 mu m and 250 mu m, the powder addition amount is 3kg after single treatment, and the vibration treatment is 15min, wherein the mixing is to put the shaped powder into a mixer for mixing treatment, the single addition is 150kg, and the mixing treatment is 5 h;
wherein the hollow powder rate of the TiAl- (Nb, Ta) alloy powder is 0.07 percent;
the sphericity of the TiAl- (Nb, Ta) alloy powder is 98%;
the tap density of the TiAl- (Nb, Ta) alloy powder was 2.75g/cm 3 ；
The Hall flow rate of the TiAl- (Nb, Ta) alloy powder is 25.6s/50 g;
the oxygen content of the TiAl- (Nb, Ta) alloy powder was 750 ppm;
the average particle size of the TiAl- (Nb, Ta) alloy powder was 118. mu.m.
Example 2
The invention relates to metal powder for powder metallurgy titanium-aluminum alloy with the service temperature of 850 ℃, which is implemented by the following steps:
step 1, pressing TiAl- (Nb, Ta) alloy into an electrode:
proportioning according to the components of TiAl- (Nb, Ta) alloy, uniformly mixing in a mixer, and pressing an electrode in an oil press, wherein: ti: 56.8 wt%; al: 31.2 wt%; nb: 5.9 wt%; ta: 6.1 wt%.
The Nb powder and the Ta powder are both powdery, the Nb powder is-325 meshes, the Ta powder is-325 meshes, Ti is added in the form of sponge titanium, and Al is added in the form of aluminum beans.
Considering the easy volatilization and burning loss of Al element in the smelting process, the Al element is compensated and increased by 4 wt% on the basis of 31.2 wt% during the material mixing.
Step 2, preparing TiAl- (Nb, Ta) alloy ingot;
smelting the pressed electrode block welding electrode through a three-time vacuum arc melting furnace, and adopting electromagnetic stirring, wherein the method specifically comprises the following steps:
the first smelting is carried out, the vacuum degree of the vacuum arc melting furnace is 1 multiplied by 10 -2 Pa, current 2250A, voltage 35V, and melting speed 45 mm/min. And continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer.
The current of the electromagnetic stirrer was 50A and the frequency of the electromagnetic stirrer was 8 Hz.
Cooling water flow of 4m 3 The temperature of the cooling water was 13 ℃.
And after the smelting is finished and the furnace is opened to take out the cast ingot, cleaning each slit of the copper crucible to prevent the condensed shell from excessively wetting the slit in the next smelting.
The vacuum degree of the vacuum arc melting furnace is 1 multiplied by 10 for the second melting -2 Pa, current 2250A, voltage 35V, and melting speed 50 mm/min. And continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer.
The current of the electromagnetic stirrer was 50A and the frequency of the electromagnetic stirrer was 8 Hz.
Cooling water flow of 4m 3 The temperature of the cooling water was 13 ℃.
And after the smelting is finished and the furnace is opened to take out the cast ingot, cleaning each slit of the copper crucible to prevent the condensed shell from excessively wetting the slit in the next smelting.
The third smelting is carried out, the vacuum degree of the vacuum arc smelting furnace is 1 multiplied by 10 -2 Pa, current of 2250AThe voltage was 35V and the melting rate was 55 mm/min. And continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer.
The current of the electromagnetic stirrer was 50A and the frequency of the electromagnetic stirrer was 8 Hz.
Cooling water flow of 4m 3 The temperature of the cooling water was 13 ℃.
And 3, preparing a TiAl- (Nb, Ta) alloy rod blank.
And carrying out homogenization annealing on the obtained TiAl- (Nb, Ta) alloy ingot.
And placing the TiAl- (Nb, Ta) alloy ingot in a heat treatment furnace. Heating the heat treatment furnace to 1380 ℃, and preserving heat for 15 hours; and after the heat preservation is finished, cooling along with the furnace. And obtaining the TiAl- (Nb, Ta) alloy ingot after homogenization annealing.
Cutting off a riser of the annealed TiAl- (Nb, Ta) alloy ingot, and obtaining a TiAl- (Nb, Ta) alloy rod blank with the diameter of 35mm and the length of 450mm by wire cutting;
and 4, preparing a finishing TiAl- (Nb, Ta) alloy rod.
The TiAl- (Nb, Ta) alloy rod blank obtained is subjected to finish turning, and the TiAl- (Nb, Ta) alloy rod after processing has the following characteristics: the diameter deviation of a single bar is less than 0.1mm, the excircle runout is less than 0.1mm, and the surface roughness is less than 2 mu m.
Step 5, SS-PREP powder making atmosphere preparation
Loading TiAl- (Nb, Ta) alloy rods into a reaction chamber, and vacuumizing the reaction chamber to 2 x 10 -2 Pa, the reaction chamber was filled with a helium-argon mixture to set the pressure in the chamber at 0.1 MPa.
And 6, preparing TiAl- (Nb, Ta) alloy powder.
The plasma gun power of the SS-PREP powder making equipment is 150kW, the end part of the TiAl- (Nb, Ta) alloy rod is heated by plasma, the rotating speed of the TiAl- (Nb, Ta) alloy rod is 31000r/min, the end part of the TiAl- (Nb, Ta) alloy rod is uniformly melted, atomized liquid drops are thrown out from the end part of the TiAl- (Nb, Ta) alloy rod under the action of centrifugal force to form fine liquid drops, and the liquid drops are rapidly cooled into spherical particles in an inert gas environment and fall into a collector at the bottom of a reaction chamber to obtain full-granularity TiAl- (Nb, Ta) alloy powder.
Step 7, screening, shaping and mixing the prepared TiAl- (Nb, Ta) alloy powder under the protection of inert gas, wherein the screening is to screen the granularity of the obtained full-granularity TiAl- (Nb, Ta) alloy powder by a square-hole woven screen with the pore diameter of 100 meshes and 270 meshes, an ultrasonic generator is started in the screening process, the powder feeding rate is 3kg/min, the shaping is to process the metal powder by sequentially passing the screened powder through circular-hole plate screens with the pore diameters of 180 microns and 150 microns to obtain the TiAl- (Nb, Ta) alloy powder with the optimal sphericity, the addition amount of the powder is 1kg after single treatment, and the vibration treatment is 10min, wherein the mixing is to load the shaped powder into a mixer for mixing treatment, the addition amount is 100kg once, and the mixing treatment is 4 h;
wherein the hollow powder rate of the TiAl- (Nb, Ta) alloy powder is 0.05 percent;
the sphericity of the TiAl- (Nb, Ta) alloy powder is 96%;
the tap density of the TiAl- (Nb, Ta) alloy powder was 2.77g/cm 3 ；
The Hall flow rate of the TiAl- (Nb, Ta) alloy powder is 25s/50 g;
the oxygen content of the TiAl- (Nb, Ta) alloy powder was 680 ppm;
the average particle size of the TiAl- (Nb, Ta) alloy powder was 78 μm.
Example 3
The invention relates to metal powder for powder metallurgy titanium-aluminum alloy with service temperature of 850 ℃, which is implemented according to the following steps:
step 1, pressing TiAl- (Nb, Ta) alloy into an electrode:
proportioning according to the components of TiAl- (Nb, Ta) alloy, uniformly mixing in a mixer, and pressing an electrode in an oil press, wherein: ti: 53.9 wt%; al: 31.8 wt%; nb: 7.2 wt%; ta: 7.1 wt%.
The Nb powder and the Ta powder are both powdery, the Nb powder is-325 meshes, the Ta powder is-325 meshes, Ti is added in the form of sponge titanium, and Al is added in the form of aluminum beans.
Considering the easily volatile burning loss of Al element in the smelting process, the Al element is compensated and increased by 5 wt% on the basis of 31.8 wt% during material preparation.
Step 2, preparing TiAl- (Nb, Ta) alloy ingot;
smelting the pressed electrode block welding electrode through a three-time vacuum arc melting furnace, and adopting electromagnetic stirring, wherein the method specifically comprises the following steps:
the first smelting is carried out, the vacuum degree of the vacuum arc melting furnace is 5 multiplied by 10 -3 Pa, current 2400A, voltage 25V, and melting speed 55 mm/min. And continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer.
The current of the electromagnetic stirrer was 110A and the frequency of the electromagnetic stirrer was 9 Hz.
Cooling water flow of 8m 3 The temperature of the cooling water was 19 ℃.
And after the smelting is finished and the furnace is opened to take out the cast ingot, cleaning each slit of the copper crucible to prevent the condensed shell from excessively wetting the slit in the next smelting.
The vacuum degree of the vacuum arc melting furnace is 5 multiplied by 10 for the second melting -3 Pa, current 2400A, voltage 25V, and melting speed 60 mm/min. And continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer.
The current of the electromagnetic stirrer was 110A and the frequency of the electromagnetic stirrer was 9 Hz.
Cooling water flow of 8m 3 The temperature of the cooling water was 19 ℃.
And after the smelting is finished and the furnace is opened to take out the cast ingot, cleaning each slit of the copper crucible to prevent the condensed shell from excessively wetting the slit in the next smelting.
The third smelting is carried out, the vacuum degree of the vacuum arc smelting furnace is 5 multiplied by 10 -3 Pa, current 2400A, voltage 25V, and melting speed 65 mm/min. And continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer.
The current of the electromagnetic stirrer was 110A and the frequency of the electromagnetic stirrer was 9 Hz.
Cooling water flow of 8m 3 The temperature of the cooling water was 19 ℃.
And 3, preparing a TiAl- (Nb, Ta) alloy rod blank.
And carrying out homogenization annealing on the obtained TiAl- (Nb, Ta) alloy ingot.
And placing the TiAl- (Nb, Ta) alloy ingot in a heat treatment furnace. Heating the heat treatment furnace to 1350 ℃, and preserving heat for 25 h; and after the heat preservation is finished, cooling along with the furnace. And obtaining the TiAl- (Nb, Ta) alloy ingot after homogenization annealing.
Cutting off a dead head of the annealed TiAl- (Nb, Ta) alloy ingot, and obtaining a TiAl- (Nb, Ta) alloy rod blank with the diameter of 47mm and the length of 500mm by wire cutting;
and 4, preparing a finishing TiAl- (Nb, Ta) alloy rod.
The TiAl- (Nb, Ta) alloy rod blank obtained is subjected to finish turning, and the TiAl- (Nb, Ta) alloy rod after processing has the following characteristics: the diameter deviation of a single bar is less than 0.1mm, the excircle runout is less than 0.1mm, and the surface roughness is less than 2 mu m.
Step 5, SS-PREP powder making atmosphere preparation
Loading TiAl- (Nb, Ta) alloy rods into the reaction chamber, and evacuating the reaction chamber to 8 × 10 -3 Pa, filling helium-argon mixed gas into the reaction chamber, and enabling the pressure in the chamber to be 1.2 MPa.
And 6, preparing TiAl- (Nb, Ta) alloy powder.
The plasma gun power of the SS-PREP powder making equipment is 210kW, the end part of the TiAl- (Nb, Ta) alloy rod is heated by plasma, the rotating speed of the TiAl- (Nb, Ta) alloy rod is 27000r/min, the end part of the TiAl- (Nb, Ta) alloy rod is uniformly melted, atomized liquid drops are thrown out from the end part of the TiAl- (Nb, Ta) alloy rod under the action of centrifugal force to form fine liquid drops, and the liquid drops are rapidly cooled into spherical particles in an inert gas environment and fall into a collector at the bottom of a reaction chamber to obtain full-granularity TiAl- (Nb, Ta) alloy powder.
Step 7, screening, shaping and mixing the prepared TiAl- (Nb, Ta) alloy powder under the protection of inert gas, wherein the screening is to screen the granularity of the obtained full-granularity TiAl- (Nb, Ta) alloy powder by a square-hole woven screen with the pore diameter of 80 meshes and 400 meshes, an ultrasonic generator is started in the screening process, the powder feeding rate is 2kg/min, the shaping is to process the metal powder by sequentially passing the screened powder through circular-hole plate screens with the pore diameters of 200 mu m and 180 mu m, the powder addition amount is 0.5kg after single treatment, and the vibration treatment is 5min, wherein the mixing is to put the shaped powder into a mixer for mixing treatment, the powder addition amount is 80kg once, and the mixing treatment is 2 h;
wherein the hollow powder rate of the TiAl- (Nb, Ta) alloy powder is 0.06 percent;
the sphericity of the TiAl- (Nb, Ta) alloy powder is 98%;
the tap density of the TiAl- (Nb, Ta) alloy powder is 2.77g/cm 3 ；
The Hall flow rate of the TiAl- (Nb, Ta) alloy powder is 26.2s/50 g;
the oxygen content of the TiAl- (Nb, Ta) alloy powder was 720 ppm;
the average particle size of the TiAl- (Nb, Ta) alloy powder was 97 μm.
Claims (7)
1. A preparation method of titanium-aluminum powder for powder metallurgy with service temperature of 850 ℃ is characterized by comprising the following specific steps:
step 1, pressing a TiAl- (Nb, Ta) alloy electrode:
preparing materials according to the components of the TiAl- (Nb, Ta) alloy, uniformly mixing in a mixer, and pressing in an oil press to obtain a TiAl- (Nb, Ta) alloy electrode;
the TiAl- (Nb, Ta) alloy comprises 40-60 wt% of Ti, 30-32 wt% of Al, 5.5-7.5 wt% of Nb and 4.4-8.7 wt% of Ta;
step 2, preparing TiAl- (Nb, Ta) alloy ingot;
placing the TiAl- (Nb, Ta) alloy electrode in a vacuum arc melting furnace for melting; the smelting process is carried out for three times, electromagnetic stirring is adopted, and the method specifically comprises the following steps:
the first smelting is carried out, the vacuum degree of the vacuum arc melting furnace is 3 multiplied by 10 -3 Pa～3×10 -2 Pa, the current is 2200 to 2500A, the voltage is 20 to 40V, and the melting speed is 30 to 55 mm/min; continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer;
the vacuum degree of the vacuum arc melting furnace is 3 multiplied by 10 for the second melting -3 Pa～3×10 -2 Pa, the current is 2200 to 2500A, the voltage is 20 to 40V, and the melting speed is 35 to 60 mm/min; continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer;
the third smelting is carried out, the vacuum degree of the vacuum arc smelting furnace is 3 multiplied by 10 -3 Pa～3×10 -2 Pa, the current is 2200 to 2500A, the voltage is 20 to 40V, and the melting speed is 40 to 65 mm/min; continuously stirring the molten metal in the molten pool by using an electromagnetic stirrer, and introducing cooling water into the crystallizer;
obtaining TiAl- (Nb, Ta) alloy cast ingots;
step 3, preparing TiAl- (Nb, Ta) alloy bar blank
Carrying out homogenization annealing on the obtained TiAl- (Nb, Ta) alloy ingot;
placing the TiAl- (Nb, Ta) alloy ingot in a heat treatment furnace; heating the heat treatment furnace to 1200-1420 ℃, and preserving heat for 1-30 h; after the heat preservation is finished, cooling along with the furnace; obtaining a TiAl- (Nb, Ta) alloy ingot subjected to homogenization annealing;
cutting off a riser of the annealed TiAl- (Nb, Ta) alloy ingot; obtaining a blank of the TiAl- (Nb, Ta) alloy rod by wire cutting;
step 4, finely turning a TiAl- (Nb, Ta) alloy rod blank;
step 5, preparing SS-PREP powder making atmosphere:
placing the obtained TiAl- (Nb, Ta) alloy rod blank in a reaction furnace; the reaction chamber is evacuated to 10 deg.C -3 Pa～10 - 1 Pa; filling helium-argon mixed gas into the reaction chamber to ensure that the pressure of the helium-argon mixed gas is 0.01 MPa-2 MPa, and obtaining the ambient atmosphere in the atomization chamber required by the powder preparation process;
step 6, preparing TiAl- (Nb, Ta) alloy powder:
heating the end part of the TiAl- (Nb, Ta) alloy bar blank by using plasma; uniformly melting the end part of the TiAl- (Nb, Ta) alloy rod, throwing atomized liquid drops out of the end part of the TiAl- (Nb, Ta) alloy rod under the action of centrifugal force to form fine liquid drops, rapidly cooling the liquid drops in an inert gas environment to form spherical particles, and falling into a collector at the bottom of a reaction chamber to obtain full-granularity TiAl- (Nb, Ta) alloy powder;
heating the end part of the TiAl- (Nb, Ta) alloy rod by using plasma to uniformly melt the end part of the TiAl- (Nb, Ta) alloy rod, throwing atomized liquid drops out of the end part of the TiAl- (Nb, Ta) alloy rod under the action of centrifugal force to form fine liquid drops, rapidly cooling the liquid drops in an inert gas environment to form spherical particles, and falling into a collector at the bottom of a reaction chamber to obtain full-granularity TiAl- (Nb, Ta) alloy powder;
and 7, post-treating the TiAl- (Nb, Ta) alloy powder:
the obtained TiAl- (Nb, Ta) alloy powder is screened, shaped and mixed under the protection of inert gas during post-treatment;
the screening is to screen the granularity of the obtained full-granularity TiAl- (Nb, Ta) alloy powder by using a square-hole woven screen with the aperture consistent with the required powder specification to obtain metal powder with the particle size suitable for a corresponding powder metallurgy forming process, wherein an ultrasonic generator is required to be started in the screening process to improve the screening effect, and the powder feeding rate is less than 5 kg/min;
the shaping is to sequentially pass the sieved powder through 2 round hole plate sieves with the hole diameter size not smaller than the upper limit of the required powder specification to treat the metal powder so as to remove the special-shaped powder, and obtain TiAl- (Nb, Ta) alloy powder with the optimal sphericity, wherein the addition of the powder treated once is not more than 3kg, and the vibration treatment is not less than 5 min;
the mixing is to put the shaped powder into a mixer for mixing treatment so as to ensure that the powder with different thicknesses is uniformly distributed, wherein the single addition does not exceed 200kg, and the mixing treatment is not less than 2 hours;
obtaining titanium-aluminum powder for powder metallurgy with the service temperature of 850 ℃;
the hollow powder rate of the titanium-aluminum powder for powder metallurgy with the service temperature of 850 ℃ is less than 0.1 percent, the sphericity is more than 95 percent, and the tap density is more than 2.7g/cm 3 The Hall flow rate is less than or equal to 27s/50g, the oxygen content is less than or equal to 800ppm, and the average particle size is 50-150 mu m.
2. The method of claim 1, wherein the Nb powder and Ta powder are both in the form of powder, and the Nb powder is-325 mesh, Ta is-325 mesh, Ti is added as titanium sponge, and Al is added as aluminum bean.
3. The method for preparing titanium-aluminum powder for powder metallurgy with a service temperature of 850 ℃ according to claim 1, wherein when pressing the TiAl- (Nb, Ta) alloy electrode, the Al element is compensated and increased by 2-8 wt% on the basis of a target value of 30-32 wt% in the batching considering the volatile burning loss of Al element in the smelting process.
4. The method for preparing the titanium-aluminum powder for powder metallurgy with the service temperature of 850 ℃ according to claim 1, wherein in the three smelting processes, the current of the electromagnetic stirrer ranges from 20A to 120A, and the frequency of the electromagnetic stirrer ranges from 1Hz to 10 Hz; the flow of the cooling water is 1-10 m 3 The temperature is 10-35 ℃.
5. The method for preparing titanium-aluminum powder for powder metallurgy with the service temperature of 850 ℃ according to claim 1, wherein after the smelting is finished and the ingot is taken out, all slits of the copper crucible are cleaned to prevent the condensed shells from excessively wetting the slits in the next smelting.
6. The method for preparing titanium-aluminum powder for powder metallurgy with the service temperature of 850 ℃ according to claim 1, wherein in the TiAl- (Nb, Ta) alloy ingot, Ti is 40-60%; 30-32% of Al; 5.5 to 7.5 percent of Nb; ta is 4.4-8.7%, and the sum of the mass percentages of the components is 100%.
7. The method for preparing titanium-aluminum powder for powder metallurgy with the service temperature of 850 ℃ according to claim 1, wherein the power of the plasma gun is 100kW to 250 kW; the rotation speed of the TiAl- (Nb, Ta) alloy rod is 20000r/min to 35000 r/min.
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| CN115502412A (en) * | 2022-09-28 | 2022-12-23 | 中国航空制造技术研究院 | Electron beam selective melting additive manufacturing method of TiAl single crystal material |
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