CN112746187A - Preparation method of large-size TiAl-based alloy seed crystal - Google Patents
Preparation method of large-size TiAl-based alloy seed crystal Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/04—Influencing the temperature of the metal, e.g. by heating or cooling the mould
- B22D27/045—Directionally solidified castings
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- 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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
Abstract
The invention discloses a preparation method of a large-size TiAl-based alloy seed crystal, which comprises the following steps: s1, preparing titanium sponge, high-purity aluminum, an aluminum-tungsten intermediate alloy and high-purity silicon respectively, wherein Al accounts for 46-47 at.%, W accounts for 0.5-1 at.%, Si accounts for 0.5 at.%, and the balance is Ti; s2, adding seed crystal raw materials into a smelting furnace; s3, vacuumizing the smelting furnace and introducing argon; s4, adding a modifier into the smelting furnace under the protection of argon; s5, turning on a power supply, increasing the power of the power supply to 55-60 kW, and smelting; s6, reducing the power of a power supply to 50-55 kW, and preserving heat to obtain a seed crystal melt; and S7, directly cutting off a power supply, chilling the seed crystal melt in the water-cooled copper crucible by using the water-cooled copper crucible, and cooling to room temperature to obtain the seed crystal ingot. The preparation method provided by the invention is simple and convenient to operate, is easy for actual production, and the obtained seed crystal has large size and stable growth of columnar crystal.
Description
Technical Field
The invention relates to the technical field of casting, in particular to a preparation method of a large-size TiAl-based alloy seed crystal.
Background
TiAl-based alloys have drawn much attention from researchers because of their relatively low density, good high temperature strength, creep resistance, oxidation resistance, and relatively high elastic modulus. The room temperature structure of TiAl-based alloys is generally composed of a gamma phase (TiAl) and an alpha phase2Phase (Ti)3Al) according to the gamma phase and alpha phase in the structure2The TiAl-based alloy generally has various types of structures such as a fully lamellar structure, a nearly fully lamellar structure, a bimodal structure, a gamma lath structure and the like at room temperature due to different phase morphologies and contents. Among them, the TiAl-based alloy of the fully lamellar structure has the best comprehensive properties. The performance test of the TiAl-based alloy by using the PST crystal material by a Japanese scholars shows that the full lamellar structure performance has obvious anisotropy, when the external load is parallel to the lamellar direction, the yield strength and the elongation rate reach the optimal combination, and the room-temperature elongation rate can reach 5-10 percent. Therefore, the adoption of the directional solidification technology to obtain the fully lamellar structure consisting of parallel columnar crystals is one of effective ways for improving the performance of the TiAl-based alloy. But the conventional directional solidification method cannot obtain a directional full-lamellar structure parallel to the growth direction.
Depending on the primary phase, the orientation of the lamellae can be controlled by directional solidification processes using seeded methods or directional solidification processes using non-seeded methods that change the solidification path. Among them, the former are more common. In the directional solidification of the seed crystal method, the preparation of the seed crystal is a crucial step, and the seed crystal prepared by the existing method is generally small in size and unstable in columnar crystal growth. Based on the defects of the prior art, the invention provides a preparation method of a large-size TiAl-based alloy seed crystal.
Disclosure of Invention
The invention aims to provide a preparation method of a large-size TiAl-based alloy seed crystal, which aims to solve the problems that the seed crystal obtained by the existing seed crystal preparation method is small in size and unstable in columnar crystal growth.
A preparation method of a large-size TiAl-based alloy seed crystal comprises the following steps:
s1, preparing seed crystal raw materials respectively, wherein the seed crystal raw materials comprise sponge titanium, high-purity aluminum, aluminum-tungsten intermediate alloy and high-purity silicon, the Al content is controlled to be 46-47 at.%, the W content is controlled to be 0.5-1 at.%, the Si content is controlled to be 0.5 at.%, and the balance is Ti;
s2, adding the seed crystal raw material prepared in the step S1 into a water-cooled copper crucible vacuum induction melting furnace;
s3, vacuumizing a smelting chamber in the vacuum induction smelting furnace to 1 x 10-3～3×10-3Introducing argon into the vacuum induction melting furnace to 0.03-0.07 Pa below Pa;
s4, under the protection of argon, adding a modifier which is 0.06-0.09% of the total mass of seed crystal raw materials into a smelting furnace;
s5, turning on a power supply, increasing the power of the power supply to 55-60 kW at a rate of 3-6 kW/min, and smelting for 2-5 min;
s6, reducing the power of a power supply to 50-55 kW at a rate of 0.4-0.6 kW/min, and continuing to keep the temperature for 2-5 min to obtain a seed crystal melt;
and S7, directly cutting off a power supply, chilling the seed crystal melt in the water-cooled copper crucible by using the water-cooled copper crucible, and cooling to room temperature to obtain the seed crystal ingot.
Preferably, in step S1, the titanium sponge is 0-grade titanium sponge.
Preferably, in step S1, the seed crystal raw material has 46 at.% of Al, 0.5 at.% of W, 0.5 at.% of Si, and the balance Ti.
Preferably, in step S1, the seed crystal raw material has 47 at.% of Al, 1 at.% of W, 0.5 at.% of Si, and the balance Ti.
Preferably, in step S4, the modifier is Na2CO3And V2O5Is prepared by the following steps.
Preferably, the modifier is prepared by the following method: firstly, preparing Na according to the mass ratio of 3-4: 12CO3And V2O5In the second step, Na is added2CO3Ultrasonic dispersion in Na2CO3And V2O5Heptadecyl imidazoline 10-15 times of total massTo obtain a mixture, and in a third step, adding V2O5And (3) placing the mixture into a reaction bottle, adding the mixture into the reaction bottle under the protection of inert gas, sealing, heating to 40-50 ℃, and stirring for reaction for 1-2 hours to obtain the modified substance.
Compared with the prior art, the invention has the beneficial effects that:
the method adopts the steps of preparing seed crystal raw materials, adding the raw materials into a smelting furnace, vacuumizing, introducing argon, adding a modifier, smelting under the condition of high power, reducing power, preserving heat and chilling a water-cooled copper crucible to obtain the TiAl-based alloy seed crystal with large size, has simple and convenient operation and stable columnar crystal growth, is easy to apply in actual production, and is added with Na before smelting2CO3、V2O5The modifier prepared from heptadecyl imidazole and the subsequent high-power melting process are matched, so that the melting effect of the seed crystal raw material can be obviously improved, the subsequent quenching of a crucible to prepare large-size seed crystals is also obviously promoted, and experiments prove that Na is independently added2CO3Or V2O5Or without heptadecylimidazole to Na2CO3And V2O5The size of the obtained seed crystal is not ideal after the treatment.
Drawings
FIG. 1 is a schematic view of a macroscopic structure observed from a transverse cross section of a Ti-46Al-0.5W-0.5Si seed crystal prepared in example 1 of the present invention which is laterally disclinated by a wire electrical discharge machining method;
FIG. 2 is a schematic view of a microstructure observed from a longitudinal section of a Ti-46Al-0.5W-0.5Si seed crystal prepared in example 1 of the present invention, which is longitudinally cast by wire electrical discharge machining.
Detailed Description
The present invention is further illustrated with reference to specific embodiments in the following, with reference to fig. 1-2.
Example 1
The invention provides a preparation method of a large-size TiAl-based alloy seed crystal, which comprises the following steps:
s1, seed crystal raw materials are respectively prepared, wherein the seed crystal raw materials comprise 0-grade sponge titanium, high-purity aluminum, aluminum-tungsten intermediate alloy and high-purity silicon, the Al content is controlled to be 46 at.%, the W content is controlled to be 0.5 at.%, the Si content is controlled to be 0.5 at.%, and the balance is Ti;
s2, adding the seed crystal raw material prepared in the step S1 into a water-cooled copper crucible vacuum induction melting furnace;
s3, vacuumizing a smelting chamber in the vacuum induction smelting furnace to 3 multiplied by 10-3Introducing argon into the vacuum induction melting furnace to 0.05Pa below Pa;
s4, under the protection of argon, adding a modifier which is 0.07 percent of the total mass of seed crystal raw materials into the smelting furnace;
the modifier is prepared by the following method: firstly, preparing Na according to the mass ratio of 3:12CO3And V2O5In the second step, Na is added2CO3Ultrasonic dispersion in Na2CO3And V2O5A mixture is obtained in heptadecyl imidazoline with 15 times of the total mass, and the third step is that V is added2O5Placing the mixture into a reaction bottle, adding the mixture into the reaction bottle under the protection of inert gas, sealing, heating to 40 ℃, and stirring for reaction for 2 hours to obtain a modified substance;
s5, turning on a power supply, increasing the power of the power supply to 60kW at a speed of 5kW/min, and smelting for 2 min;
s6, reducing the power of the power supply to 55kW at the rate of 0.45kW/min, and continuing to keep the temperature for 2min to obtain seed crystal melt;
and S7, directly cutting off a power supply, chilling the seed crystal melt in the water-cooled copper crucible by using the water-cooled copper crucible, and cooling to room temperature to obtain the Ti-46Al-0.5W-0.5Si seed crystal ingot.
Example 2
The invention provides a preparation method of a large-size TiAl-based alloy seed crystal, which comprises the following steps:
s1, seed crystal raw materials are respectively prepared, wherein the seed crystal raw materials comprise 0-grade sponge titanium, high-purity aluminum, aluminum-tungsten intermediate alloy and high-purity silicon, wherein Al is 47 at.%, W is 1 at.%, Si is 0.5 at.%, and the balance is Ti;
s2, adding the seed crystal raw material prepared in the step S1 into a water-cooled copper crucible vacuum induction melting furnace;
s3, vacuumizing a smelting chamber in the vacuum induction smelting furnace to 1 x 10-3Introducing argon into the vacuum induction melting furnace to 0.03Pa below Pa;
s4, adding a modifier which accounts for 0.09% of the total mass of seed crystal raw materials into the smelting furnace under the protection of argon;
the modifier is prepared by the following method: firstly, preparing Na according to the mass ratio of 4:12CO3And V2O5In the second step, Na is added2CO3Ultrasonic dispersion in Na2CO3And V2O5A mixture is obtained in heptadecyl imidazoline with the total mass being 10 times, and the third step is that V is added2O5Placing the mixture into a reaction bottle, adding the mixture into the reaction bottle under the protection of inert gas, sealing, heating to 50 ℃, and stirring for reaction for 1h to obtain a modified substance;
s5, turning on a power supply, increasing the power of the power supply to 55kW at the speed of 6kW/min, and smelting for 5 min;
s6, reducing the power of the power supply to 50kW at the rate of 0.6kW/min, and continuing to keep the temperature for 5min to obtain seed crystal melt;
and S7, directly cutting off a power supply, chilling the seed crystal melt in the water-cooled copper crucible by using the water-cooled copper crucible, and cooling to room temperature to obtain the Ti-47Al-1W-0.5Si seed crystal ingot.
Comparative example 1
A preparation method of a large-size TiAl-based alloy seed crystal comprises the following steps:
s1, seed crystal raw materials are respectively prepared, wherein the seed crystal raw materials comprise 0-grade sponge titanium, high-purity aluminum, aluminum-tungsten intermediate alloy and high-purity silicon, the Al content is controlled to be 46 at.%, the W content is controlled to be 0.5 at.%, the Si content is controlled to be 0.5 at.%, and the balance is Ti;
s2, adding the seed crystal raw material prepared in the step S1 into a water-cooled copper crucible vacuum induction melting furnace;
s3, vacuumizing a smelting chamber in the vacuum induction smelting furnace to 3 multiplied by 10-3Introducing argon into the vacuum induction melting furnace to 0.05Pa below Pa;
s4, turning on a power supply, increasing the power of the power supply to 60kW at a speed of 5kW/min, and smelting for 2 min;
s5, reducing the power of the power supply to 55kW at the rate of 0.45kW/min, and continuing to keep the temperature for 2min to obtain seed crystal melt;
and S6, directly cutting off a power supply, chilling the seed crystal melt in the water-cooled copper crucible by using the water-cooled copper crucible, and cooling to room temperature to obtain the Ti-46Al-0.5W-0.5Si seed crystal ingot.
Comparative example 2
A preparation method of a large-size TiAl-based alloy seed crystal comprises the following steps:
s1, seed crystal raw materials are respectively prepared, wherein the seed crystal raw materials comprise 0-grade sponge titanium, high-purity aluminum, aluminum-tungsten intermediate alloy and high-purity silicon, the Al content is controlled to be 46 at.%, the W content is controlled to be 0.5 at.%, the Si content is controlled to be 0.5 at.%, and the balance is Ti;
s2, adding the seed crystal raw material prepared in the step S1 into a water-cooled copper crucible vacuum induction melting furnace;
s3, vacuumizing a smelting chamber in the vacuum induction smelting furnace to 3 multiplied by 10-3Introducing argon into the vacuum induction melting furnace to 0.05Pa below Pa;
s4, under the protection of argon, adding a modifier which is 0.07 percent of the total mass of seed crystal raw materials into the smelting furnace;
the modifier is prepared by the following method: first, adding Na2CO3Ultrasonically dispersing the mixture in heptadecyl imidazoline with the same dosage as that of the embodiment 1 to obtain a mixture, and secondly, adding the prepared mixture into a reaction bottle under the protection of inert gas, sealing, heating to 40 ℃, and stirring for reaction for 2 hours to obtain a modified substance;
s5, turning on a power supply, increasing the power of the power supply to 60kW at a speed of 5kW/min, and smelting for 2 min;
s6, reducing the power of the power supply to 55kW at the rate of 0.45kW/min, and continuing to keep the temperature for 2min to obtain seed crystal melt;
and S7, directly cutting off a power supply, chilling the seed crystal melt in the water-cooled copper crucible by using the water-cooled copper crucible, and cooling to room temperature to obtain the Ti-46Al-0.5W-0.5Si seed crystal ingot.
Comparative example 3
A preparation method of a large-size TiAl-based alloy seed crystal comprises the following steps:
s1, seed crystal raw materials are respectively prepared, wherein the seed crystal raw materials comprise 0-grade sponge titanium, high-purity aluminum, aluminum-tungsten intermediate alloy and high-purity silicon, the Al content is controlled to be 46 at.%, the W content is controlled to be 0.5 at.%, the Si content is controlled to be 0.5 at.%, and the balance is Ti;
s2, adding the seed crystal raw material prepared in the step S1 into a water-cooled copper crucible vacuum induction melting furnace;
s3, vacuumizing a smelting chamber in the vacuum induction smelting furnace to 3 multiplied by 10-3Introducing argon into the vacuum induction melting furnace to 0.05Pa below Pa;
s4, under the protection of argon, adding a modifier which is 0.07 percent of the total mass of seed crystal raw materials into the smelting furnace;
the modifier is prepared by the following method: in the first step, heptadecyl imidazoline and V in the same amount as in example 1 are used2O5In the second step, V is2O5Placing the mixture into a reaction bottle, adding heptadecyl imidazoline into the reaction bottle under the protection of inert gas, sealing, heating to 40 ℃, and stirring for reaction for 2 hours to obtain a modified substance;
s5, turning on a power supply, increasing the power of the power supply to 60kW at a speed of 5kW/min, and smelting for 2 min;
s6, reducing the power of the power supply to 55kW at the rate of 0.45kW/min, and continuing to keep the temperature for 2min to obtain seed crystal melt;
and S7, directly cutting off a power supply, chilling the seed crystal melt in the water-cooled copper crucible by using the water-cooled copper crucible, and cooling to room temperature to obtain the Ti-46Al-0.5W-0.5Si seed crystal ingot.
Comparative example 4
A preparation method of a large-size TiAl-based alloy seed crystal comprises the following steps:
s1, seed crystal raw materials are respectively prepared, wherein the seed crystal raw materials comprise 0-grade sponge titanium, high-purity aluminum, aluminum-tungsten intermediate alloy and high-purity silicon, the Al content is controlled to be 46 at.%, the W content is controlled to be 0.5 at.%, the Si content is controlled to be 0.5 at.%, and the balance is Ti;
s2, adding the seed crystal raw material prepared in the step S1 into a water-cooled copper crucible vacuum induction melting furnace;
s3, sensing the vacuumThe smelting chamber in the smelting furnace is vacuumized to 3 x 10-3Introducing argon into the vacuum induction melting furnace to 0.05Pa below Pa;
s4, under the protection of argon, adding a modifier which is 0.07 percent of the total mass of seed crystal raw materials into the smelting furnace;
the modifier is prepared by the following method: firstly, preparing Na according to the mass ratio of 3:12CO3And V2O5In the second step, V is2O5Placing the mixture in a reaction bottle, and adding Na under the protection of inert gas2CO3Adding into a reaction bottle, sealing, heating to 40 ℃, and stirring for reaction for 2h to obtain a modified substance;
s5, turning on a power supply, increasing the power of the power supply to 60kW at a speed of 5kW/min, and smelting for 2 min;
s6, reducing the power of the power supply to 55kW at the rate of 0.45kW/min, and continuing to keep the temperature for 2min to obtain seed crystal melt;
and S7, directly cutting off a power supply, chilling the seed crystal melt in the water-cooled copper crucible by using the water-cooled copper crucible, and cooling to room temperature to obtain the Ti-46Al-0.5W-0.5Si seed crystal ingot.
Comparative example 5
The Ti-46Al-0.5W-0.5Si seed crystal ingot is prepared by the traditional directional solidification method of gold.
Example 1 compared to comparative example 5, the resulting seed size increased by 19.6%; compared with the comparative example 5, the size of the obtained seed crystal is increased by 0.31 percent in the comparative example 1; compared with the comparative example 5, the size of the obtained seed crystal is increased by 16.1 percent in the comparative example 2; compared with the comparative example 5, the size of the obtained seed crystal is increased by 15.3 percent in the comparative example 3; comparative example 4 compared to comparative example 5, the resulting seed size increased by 14.6%; the experimental results show that the seed crystal size obtained in example 1 of the present invention is significantly larger than the comparative example.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. A preparation method of a large-size TiAl-based alloy seed crystal is characterized by comprising the following steps:
s1, preparing seed crystal raw materials respectively, wherein the seed crystal raw materials comprise sponge titanium, high-purity aluminum, aluminum-tungsten intermediate alloy and high-purity silicon, the Al content is controlled to be 46-47 at.%, the W content is controlled to be 0.5-1 at.%, the Si content is controlled to be 0.5 at.%, and the balance is Ti;
s2, adding the seed crystal raw material prepared in the step S1 into a water-cooled copper crucible vacuum induction melting furnace;
s3, vacuumizing a smelting chamber in the vacuum induction smelting furnace to 1 x 10-3～3×10-3Introducing argon into the vacuum induction melting furnace to 0.03-0.07 Pa below Pa;
s4, under the protection of argon, adding a modifier which is 0.06-0.09% of the total mass of seed crystal raw materials into a smelting furnace;
s5, turning on a power supply, increasing the power of the power supply to 55-60 kW at a rate of 3-6 kW/min, and smelting for 2-5 min;
s6, reducing the power of a power supply to 50-55 kW at a rate of 0.4-0.6 kW/min, and continuing to keep the temperature for 2-5 min to obtain a seed crystal melt;
and S7, directly cutting off a power supply, chilling the seed crystal melt in the water-cooled copper crucible by using the water-cooled copper crucible, and cooling to room temperature to obtain the seed crystal ingot.
2. The method for preparing large-sized TiAl-based alloy seed crystals as claimed in claim 1, wherein in step S1, the titanium sponge is grade 0 titanium sponge.
3. The method for preparing a large-sized TiAl-based alloy seed crystal according to claim 1, wherein in step S1, Al in the seed crystal raw material is 46 at.%, W is 0.5 at.%, Si is 0.5 at.%, and the balance is Ti.
4. The method for preparing a large-sized TiAl-based alloy seed crystal according to claim 1 or 3, wherein in step S1, Al in the seed crystal raw material is 47 at.%, W is 1 at.%, Si is 0.5 at.%, and the balance is Ti.
5. The method for preparing a large-sized TiAl-based alloy seed crystal according to claim 1, wherein in step S4, the modifier is Na2CO3And V2O5Is prepared by the following steps.
6. The method for preparing a large-sized TiAl-based alloy seed crystal according to claim 1 or 5, wherein the modifier is prepared by the following method: firstly, preparing Na according to the mass ratio of 3-4: 12CO3And V2O5In the second step, Na is added2CO3Ultrasonic dispersion in Na2CO3And V2O5A mixture is obtained from heptadecyl imidazoline with the total mass of 10-15 times, and step three, V is added2O5And (3) placing the mixture into a reaction bottle, adding the mixture into the reaction bottle under the protection of inert gas, sealing, heating to 40-50 ℃, and stirring for reaction for 1-2 hours to obtain the modified substance.
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