CN107748094B - Preparation method of TA15 titanium alloy powder product - Google Patents
Preparation method of TA15 titanium alloy powder product Download PDFInfo
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Abstract
A method for preparing a TA15 titanium alloy powder part comprises the steps of firstly carrying out first-step solution treatment on a TA15 titanium alloy subjected to powder hot isostatic pressing, namely carrying out solution treatment at 1050 ℃ for 0.5h to completely dissolve α phase in an initial structure, cooling to 850-950 ℃ at a cooling speed of 10 ℃/min, keeping the temperature for 1h, controlling β grain size, precipitating a primary α phase, then carrying out water quenching to room temperature to precipitate a small amount of secondary α phase, heating the TA15 alloy subjected to the two-step solution treatment to 600 ℃ to carry out aging for 4h, then carrying out air cooling to room temperature, adjusting the content of the secondary α phase and stabilizing the structure.
Description
Technical Field
The invention belongs to the field of powder metallurgy titanium alloy, and provides a preparation method capable of improving the microstructure and the mechanical property of a TA15 titanium alloy powder workpiece. In particular to a TA15 titanium alloy material and a finished product formed by powder hot isostatic pressing.
Background
The TA15 nominal component Ti-6.5Al-2Zr-1Mo-1V belongs to a near α type titanium alloy with high Al equivalent weight, has good heat strength, medium room temperature and high temperature strength and good heat stability, and is mainly used for manufacturing airplanes, engine parts and welding force-bearing parts which work for a long time below 500 ℃In three published papers of high-temperature plastic deformation behavior of metallurgy TA15 titanium alloy, a TA15 titanium alloy compact is prepared by a hot isostatic pressing method, a Gleeble-1500 thermal simulator is adopted to perform a thermal compression test on powder metallurgy TA15 titanium alloy, and the strain rate of the alloy at 850-1050 ℃ is studied to be 0.001-0.01 s-1In the range, the high-temperature plastic deformation behavior is performed, a hot working diagram is drawn, meanwhile, the high-temperature creep behavior at 500-525 ℃ and the stress of 250-350 MPa is studied, the occurrence of structural nonuniformity is not studied, in the invention, the TA15 titanium ingot microstructure prepared by the powder metallurgy hot isostatic pressing method has the nonuniform α phase structure characteristic, equiaxial α phase is distributed on the boundary of original particles, and lamellar α phase is distributed in the original particles, as shown in figure 2.
The invention with the publication number of CN1830617A provides a forging and heat treatment process for a TA15 alloy ring piece and a die forging piece, the method is suitable for preparing the TA15 alloy ring piece and the die forging piece, the adopted heat treatment system is 830-850 ℃, the temperature is kept for 2h, air cooling is carried out, good structure and mechanical property can be obtained, and the tensile strength can reach 1057 MPa. However, the heat treatment process was used for powder metallurgically prepared TA15 titanium alloy having a tensile strength of only about 922MPa, as detailed in Table 1.
Zhao Huijun studied the influence of vacuum heat treatment process on TA15 alloy mechanical properties in "influence of vacuum annealing on TA15 alloy sheet structure and mechanical properties" published in "Chinese non-ferrous metals article (English edition)"2015 (6) ("1881-" 1888 "), and when the heat treatment process was 930 ℃/2h/AC +600 ℃/2h/AC, the best tensile strength 1070MPa could be obtained, but the invention adopts the heat treatment process, which could not improve the uneven α structure morphology existing in the hot isostatic pressing state, as shown in FIG. 4, the tensile strength was 946MPa, see Table 1 for details.
In summary, the TA15 titanium alloy prepared by the powder hot isostatic pressing method adopts the existing heat treatment process, the tissue inheritance of the hot isostatic pressing state cannot be effectively improved and eliminated, and the strong plasticity matching is poor. At present, few reports on improving the structure and the performance of the TA15 titanium alloy in powder metallurgy are reported. Therefore, it is urgently needed to provide a method for improving the structural property of the TA15 titanium alloy.
Disclosure of Invention
In order to overcome the defects that the tissue inheritance of a hot isostatic pressing state cannot be effectively improved and eliminated and the strong plasticity matching is poor in the prior art, the invention provides a preparation method of a TA15 titanium alloy powder product.
The specific process of the invention is as follows:
The specific process for pressing the titanium ingot comprises the following steps:
the prepared TA15 prealloyed powder was loaded into a cylindrical carbon steel jacket. And placing the carbon steel sheath filled with the TA15 prealloying powder on a vibration platform for tapping, so that the density of the TA15 prealloying powder reaches 66-68%.
Heating and degassing the carbon steel sheath at 500-550 ℃ until the vacuum reaches 10 DEG C-4And keeping the temperature for 4 hours after Pa. And after the heat preservation is finished, carrying out oxyacetylene seal welding and degassing port on the carbon steel sheath.
Placing the sealed and welded carbon steel sheath in a hot isostatic pressing furnace for pressing; the hot isostatic pressing temperature is 950 ℃, the pressure maintaining pressure is 150MPa, and the heat and pressure maintaining test piece is 4 h; obtaining the cylindrical titanium ingot with the density reaching 99.8 percent.
And 2, cutting a tensile sample.
2 tensile specimens were cut out from the core and the edge of the obtained titanium ingot. The tensile test samples are all rod-like.
And 3, carrying out heat treatment.
The obtained tensile specimens were placed in a heat treatment furnace to be heat-treated. The heat treatment process comprises two steps of solution treatment and aging treatment.
The specific process is as follows:
the specific process of the two-step solution treatment is as follows:
i, heating the heat treatment furnace to 1050 ℃ and preserving heat for 0.5 h.
And II, after the heat preservation is finished, cooling to 850-950 ℃ in a cooling speed furnace at the speed of 10 ℃/min, and then preserving the heat for 1 h. And (5) after heat preservation, quenching the mixture to room temperature.
Aging treatment: heating the tensile sample subjected to the two-step solution treatment to 600 ℃ for 4h for aging, discharging and air-cooling to room temperature.
The obtained tensile specimens were placed in a heat treatment furnace to be heat-treated. The heat treatment process comprises two steps of solution treatment and aging treatment.
And finishing the heat treatment process to obtain the titanium alloy tensile sample.
The method comprises the steps of firstly carrying out first-step solution treatment on TA15 titanium alloy subjected to powder hot isostatic pressing, namely carrying out solution treatment at 1050 ℃ for 0.5h to completely dissolve α phase in an initial structure, cooling to 850-950 ℃ of second-step solution temperature in a cooling speed furnace at 10 ℃/min, keeping the temperature for 1h, controlling β grain size, precipitating a primary α phase, then carrying out water quenching to room temperature to precipitate a small amount of secondary α phase, heating TA15 alloy subjected to two-step solution treatment to 600 ℃ for 4h to carry out aging, then carrying out air cooling to room temperature, adjusting the content of the secondary α phase and stabilizing the structure.
The process of the invention comprises the following steps: (1) performing first-step solution treatment, keeping the temperature at 1050 ℃ for 0.5h, then cooling to (2) a second-step solution temperature of 850-950 ℃ in a cooling speed furnace at 10 ℃/min, keeping the temperature for 1h, and then performing water quenching to room temperature; (3) and (3) reheating the TA15 alloy subjected to the two-step solution treatment to 600 ℃, carrying out aging for 4h, discharging from the furnace, and carrying out air cooling to room temperature. See fig. 1.
According to the invention, a TA15 titanium alloy after powder hot isostatic pressing is heated to 1050 ℃/0.5h in a β single-phase region to be subjected to solution treatment, so that α phase in an initial structure is completely dissolved, α phase which is unevenly distributed in a powder hot isostatic pressing structure is eliminated, then the temperature is reduced to 850-950 ℃ in a cooling speed furnace at 10 ℃/min, the temperature is kept for 1h, β grain size is controlled, primary α phase is precipitated, water quenching is carried out, the structure morphology at high temperature is retained, supersaturated solid solution which is rich in solid solution is obtained, the TA15 titanium ingot prepared by the powder metallurgy method is further heated to 600 ℃ to be subjected to aging treatment for 4h, so that solid solution is decomposed to precipitate secondary α phase, the secondary α phase content is adjusted by optimizing aging time and the aim of stabilizing the structure is achieved, the microstructure of a TA15 titanium ingot prepared by the powder metallurgy method has the characteristics of uneven α phase structure, equiaxed α phase is distributed at the boundary of the original particles, a lamella α phase is distributed inside the original particles, as shown in a drawing 1, direct annealing and the two-phase region is subjected to the aging treatment, the genetic morphology, the characteristics of the uniform solution treatment of the TA 6326 phase, the tensile strength of the TA 2 titanium alloy, the tensile strength is improved by the annealing and the hot isostatic pressing process, the hot isostatic pressing process is obviously improved by the approximate tensile strength of the hot isostatic pressing structure, the hot isostatic pressing process, the TA 8548 MPa, the approximate tensile strength of the TA 858 MPa, the hot isostatic pressing process, the TA 8548 MPa, the TA15 titanium alloy, the hot isostatic pressing process, the hot isostatic pressing structure, the hot isostatic pressing process, the hot isostatic pressing.
TABLE 1 room temperature tensile properties of powder HIP TA15 titanium alloys
Drawings
FIG. 1 is a schematic view of the process of the present invention.
FIG. 2 is a microstructure of TA15 titanium alloy in powder HIP, at 100 × magnification.
FIG. 3 is a microstructure of TA15 titanium alloy at 200 magnification 200 × after 850 deg.C/2 h direct anneal.
FIG. 4 is the microstructure of TA15 titanium alloy after 930 deg.C/2 h/AC solutionizing +600 deg.C/4 h/AC aging treatment, at 200 magnification 200 ×.
FIG. 5 shows the microstructure of TA15 titanium alloy after the two-step solution treatment of 1050 ℃/0.5h/FC (10 ℃/min) → 850 ℃/1h/WQ and the aging treatment of 600 ℃/4h/AC in example 1 of the present invention, the magnification being 100 ×.
FIG. 6 shows the microstructure of TA15 titanium alloy after the two-step solution treatment of 1050 ℃/0.5h/FC (10 ℃/min) → 850 ℃/1h/WQ and the aging treatment of 600 ℃/4h/AC in example 1 of the present invention, the magnification being 500 × respectively.
FIG. 7 shows the microstructure of TA15 titanium alloy after the two-step solution treatment of 1050 ℃/0.5h/FC (10 ℃/min) → 900 ℃/1h/WQ and the aging treatment of 600 ℃/4h/AC in example 2 of the present invention, the magnification being 100 ×.
FIG. 8 shows the microstructure of TA15 titanium alloy after the two-step solution treatment of 1050 ℃/0.5h/FC (10 ℃/min) → 900 ℃/1h/WQ + the aging treatment of 600 ℃/4h/AC in example 2 of the present invention, the magnification being 500 × respectively.
FIG. 9 shows the microstructure of TA15 titanium alloy after the two-step solution treatment of 1050 ℃/0.5h/FC (10 ℃/min) → 950 ℃/1h/WQ and the aging treatment of 600 ℃/4h/AC in example 3 of the present invention, each at a magnification of 100 ×.
FIG. 10 shows the microstructure of TA15 titanium alloy after two-step solution treatment of 1050 ℃/0.5h/FC (10 ℃/min) → 950 ℃/1h/WQ and aging treatment of 600 ℃/4h/AC in example 3 of the present invention, the magnifications being 100 × and 500 ×, respectively.
FIG. 11 is a flow chart of the present invention.
Detailed Description
Example 1
The embodiment is a preparation method capable of improving the microstructure of a powder product of TA15 titanium alloy in powder metallurgy, wherein the powder product is a titanium ingot. The specific process is as follows:
A rotating electrode powder preparation method is selected to prepare TA15 pre-alloyed powder, and the particle size distribution of the powder is 60-250 mu m.
The prepared TA15 prealloyed powder was loaded into a cylindrical carbon steel jacket. And placing the carbon steel sheath filled with the TA15 prealloying powder on a vibration platform for tapping, so that the density of the TA15 prealloying powder reaches 66-68%.
Heating and degassing the carbon steel sheath at 500-550 ℃ until the vacuum reaches 10 DEG C-4And keeping the temperature for 4 hours after Pa. After the heat preservation is finished, the carbon steel sheath is subjected to oxyacetylene seal weldingAnd an air removal port.
Placing the sealed and welded carbon steel sheath in a hot isostatic pressing furnace for pressing; the hot isostatic pressing temperature is 950 ℃, the pressure maintaining pressure is 150MPa, and the heat and pressure maintaining test piece is 4 h. Obtaining a cylindrical titanium ingot with the density reaching 99.8 percent; the microstructure of the titanium ingot is shown in FIG. 2, and the characteristic of nonuniform microstructure is obvious.
And 2, cutting a tensile sample.
2 tensile specimens were cut out by wire cutting from the core and the edge of the obtained cylindrical titanium ingot. The tensile test samples are all rod-like.
And 3, carrying out heat treatment.
The obtained tensile specimens were placed in a heat treatment furnace to be heat-treated. The heat treatment process comprises two steps of solution treatment and aging treatment.
The specific process is as follows:
the specific process of the two-step solution treatment is as follows:
i, heating the heat treatment furnace to 1050 ℃ and preserving heat for 0.5 h.
And II, after the heat preservation is finished, cooling to 850 ℃ in a cooling speed furnace at the speed of 10 ℃/min, and then preserving the heat for 1 h. And (5) after heat preservation, quenching the mixture to room temperature.
Aging treatment: heating the tensile sample subjected to the two-step solution treatment to 600 ℃ for 4h for aging, discharging and air-cooling to room temperature.
And finishing the heat treatment process to obtain the heat-treated tensile sample.
This example was tested to yield tensile specimens of titanium alloy having a uniform lamellar structure, as shown in fig. 5 and 6, which significantly improved the non-uniform α phase structure characteristic of the hiped state.
Example 2
This example is a method for preparing a powder article of TA15 titanium alloy, which is a hollow stepped shaft, with improved microstructure. The specific process is as follows:
A rotating electrode powder preparation method is selected to prepare TA15 pre-alloyed powder, and the particle size distribution of the powder is 60-250 mu m.
The prepared TA15 prealloyed powder was loaded into the carbon steel jacket of a hollow stepped shaft. And placing the carbon steel sheath filled with the TA15 prealloying powder on a vibration platform for tapping, so that the density of the TA15 prealloying powder reaches 66-68%.
Heating and degassing the carbon steel sheath at 500-550 ℃ until the vacuum reaches 10 DEG C-4And keeping the temperature for 4 hours after Pa. And after the heat preservation is finished, carrying out oxyacetylene seal welding and degassing port on the carbon steel sheath.
Placing the sealed and welded carbon steel sheath in a hot isostatic pressing furnace for pressing; the hot isostatic pressing temperature is 950 ℃, the pressure maintaining pressure is 150MPa, and the heat and pressure maintaining test piece is 4 h. Obtaining a hollow stepped shaft powder part with the density reaching 99.8 percent; the microstructure of the titanium ingot is shown in FIG. 2, and the characteristic of nonuniform microstructure is obvious.
And 2, cutting a tensile sample.
2 tensile specimens were cut out of the resulting hollow stepped shafts by wire cutting. The tensile test samples are all rod-like.
And 3, carrying out heat treatment.
The obtained tensile specimens were placed in a heat treatment furnace to be heat-treated. The heat treatment process comprises two steps of solution treatment and aging treatment.
The specific process is as follows:
the specific process of the two-step solution treatment is as follows:
i, heating the heat treatment furnace to 1050 ℃ and preserving heat for 0.5 h.
And II, after the heat preservation is finished, cooling to 900 ℃ in a cooling speed furnace at the speed of 10 ℃/min, and then preserving the heat for 1 h. And (5) after heat preservation, quenching the mixture to room temperature.
Aging treatment: heating the tensile sample subjected to the two-step solution treatment to 600 ℃ for 4h for aging, discharging and air-cooling to room temperature.
And finishing the heat treatment process to obtain the titanium alloy tensile sample.
This example was tested to yield tensile specimens of titanium alloy having a uniform lamellar structure, as shown in fig. 7 and 8, which significantly improved the non-uniform α phase structure characteristic of the hiped state.
Example 3
This example is a method for improving the microstructure of a powder metallurgical TA15 titanium alloy powder article, which is an annular article. The specific process is as follows:
A rotating electrode powder preparation method is selected to prepare TA15 pre-alloyed powder, and the particle size distribution of the powder is 60-250 mu m.
The prepared TA15 prealloyed powder was loaded into an annular cylindrical carbon steel jacket. And placing the carbon steel sheath filled with the TA15 prealloying powder on a vibration platform for tapping, so that the density of the TA15 prealloying powder reaches 66-68%.
Heating and degassing the carbon steel sheath at 500-550 ℃ until the vacuum reaches 10 DEG C-4And keeping the temperature for 4 hours after Pa. And after the heat preservation is finished, carrying out oxyacetylene seal welding and degassing port on the carbon steel sheath.
Placing the sealed and welded carbon steel sheath in a hot isostatic pressing furnace for pressing; the hot isostatic pressing temperature is 950 ℃, the pressure maintaining pressure is 150MPa, and the heat and pressure maintaining test piece is 4 h. Obtaining an annular piece with the density reaching 99.8 percent; the microstructure of the titanium ingot is shown in FIG. 2, and the characteristic of nonuniform microstructure is obvious.
And 2, cutting a tensile sample.
2 tensile specimens were cut out of the resulting annular ring walls by wire cutting. The tensile test samples are all rod-like.
And 3, carrying out heat treatment.
The obtained tensile specimens were placed in a heat treatment furnace to be heat-treated. The heat treatment process comprises two steps of solution treatment and aging treatment.
The specific process is as follows:
the specific process of the two-step solution treatment is as follows:
i, heating the heat treatment furnace to 1050 ℃ and preserving heat for 0.5 h.
And II, after the heat preservation is finished, cooling to 950 ℃ in a cooling speed furnace at the speed of 10 ℃/min, and then preserving the heat for 1 h. And (5) after heat preservation, quenching the mixture to room temperature.
Aging treatment: heating the tensile sample subjected to the two-step solution treatment to 600 ℃ for 4h for aging, discharging and air-cooling to room temperature.
And finishing the heat treatment process to obtain the titanium alloy tensile sample.
This example was tested to yield tensile specimens of titanium alloy having a uniform lamellar structure, as shown in fig. 9 and 10, which significantly improved the non-uniform α phase structure characteristic of the hiped state.
Claims (2)
1. A preparation method of a TA15 titanium alloy powder product is characterized by comprising the following specific steps:
step 1, pressing a titanium ingot;
the prepared TA15 prealloying powder is filled into a cylindrical carbon steel sheath; placing the carbon steel sheath filled with the TA15 prealloying powder on a vibration platform for tapping to ensure that the density of the TA15 prealloying powder reaches 66-68%;
heating and degassing the carbon steel sheath at 500-550 ℃ until the vacuum reaches 10 DEG C-4Keeping the temperature for 4 hours after Pa; after the heat preservation is finished, performing oxyacetylene seal welding gas removal on the carbon steel sheath;
placing the sealed and welded carbon steel sheath in a hot isostatic pressing furnace for pressing; the hot isostatic pressing temperature is 950 ℃, the pressure maintaining pressure is 150MPa, and the heat and pressure maintaining test piece is 4 h; obtaining a cylindrical titanium ingot with the density reaching 99.8 percent;
step 2, cutting a tensile sample;
respectively cutting 2 tensile samples at the core part and the edge part of the obtained titanium ingot; the tensile samples are all rod-shaped;
step 3, heat treatment;
the specific process is as follows:
the specific process of the two-step solution treatment is as follows:
i, heating a heat treatment furnace to 1050 ℃ and preserving heat for 0.5h to completely dissolve α phase in the initial structure;
II, after the heat preservation is finished, cooling to 850-950 ℃ in a cooling speed furnace at the speed of 10 ℃/min, preserving the heat for 1h, controlling the size of β crystal grains, precipitating a primary α phase, and performing water quenching to room temperature after the heat preservation is finished to precipitate a small amount of secondary α phases;
aging treatment: heating the tensile sample subjected to the two-step solution treatment to 600 ℃ for 4h for aging, discharging and air-cooling to room temperature;
placing each obtained tensile sample in a heat treatment furnace for heat treatment, wherein the heat treatment process comprises two steps of solution treatment and aging treatment, adjusting the content of secondary α phase and stabilizing the structure;
and finishing the heat treatment process to obtain the titanium alloy tensile sample.
2. The method of making a TA15 titanium alloy powder article of claim 1, wherein the TA15 alloy powder pressed into a titanium ingot has a particle size of 60 to 250 μm.
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