CN112746329A - Seed crystal preparation method for TiAl-based alloy directional solidification - Google Patents
Seed crystal preparation method for TiAl-based alloy directional solidification Download PDFInfo
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- CN112746329A CN112746329A CN202011516112.4A CN202011516112A CN112746329A CN 112746329 A CN112746329 A CN 112746329A CN 202011516112 A CN202011516112 A CN 202011516112A CN 112746329 A CN112746329 A CN 112746329A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/52—Alloys
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/14—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method characterised by the seed, e.g. its crystallographic orientation
Abstract
The invention discloses a seed crystal preparation method for TiAl-based alloy directional solidification, which comprises the following steps: s1, preparing titanium sponge, high-purity aluminum and high-purity silicon respectively, wherein the Al accounts for 43-46 at.%, the Mo accounts for 0-1.5 at.%, the Si accounts for 0.8-3 at.%, and the balance is Ti; s2, adding seed crystal raw materials into a vacuum induction melting furnace in a layered manner; s3, vacuumizing the smelting chamber, and introducing argon; s4, turning on a power supply, increasing the power of the power supply to 55-60 kW, and smelting; s5, reducing the power of a power supply to 50-55 kW, and preserving heat to obtain a 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 seed crystal ingot for directional solidification of the TiAl-based alloy. The seed crystal shrinkage hole area obtained by the preparation method provided by the invention is small.
Description
Technical Field
The invention relates to the technical field of casting, in particular to a seed crystal preparation method for TiAl-based alloy directional solidification.
Background
The TiAl-based alloy has lower density and good high-temperature strengthCreep resistance, oxidation resistance, and a large elastic modulus have been of great interest to researchers. 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, the preparation of the seed crystal is a crucial step, and the liquid state shrinkage phenomenon is often generated when the seed crystal is prepared by the conventional method. Based on the defects in the prior art, the invention provides a seed crystal preparation method for TiAl-based alloy directional solidification.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a seed crystal preparation method for TiAl-based alloy directional solidification.
A seed crystal preparation method for directional solidification of TiAl-based alloy comprises the following steps:
s1, preparing seed crystal raw materials respectively, wherein the seed crystal raw materials comprise sponge titanium, high-purity aluminum and high-purity silicon, wherein the mass percent of Al is 43-46 at.%, the mass percent of Mo is 0-1.5 at.%, the mass percent of Si is 0.8-3 at.%, and the balance is Ti;
s2, adding the seed crystal raw materials prepared in the step S1 into a water-cooled copper crucible vacuum induction melting furnace in a layered mode;
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, 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 3-5 min;
s5, 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 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 seed crystal ingot for directional solidification of the TiAl-based alloy.
Preferably, in step S1, the titanium sponge is 0-grade titanium sponge.
Preferably, in step S1, the seed crystal raw material has 43 at.% of Al, 0 at.% of Mo, 3 at.% of Si, and the balance Ti.
Preferably, in step S1, the seed crystal raw material has 46 at.% of Al, 1.5 at.% of Mo, 1 at.% of Si, and the balance Ti.
Preferably, in step S2, the layered layers are, from bottom to top, a titanium sponge layer, a high purity aluminum layer, a high purity silicon layer, and a titanium sponge layer.
Preferably, in step S4, the power supply power is increased at a rate of 5 kw/min.
Preferably, in step S4, the temperature decrease rate of the power supply is 0.5 kw/min.
Compared with the prior art, the invention has the beneficial effects that:
the method comprises the steps of preparing seed crystal raw materials, adding the raw materials into a smelting furnace in a layered mode, vacuumizing, introducing argon, smelting under the condition of high power, reducing power and preserving heat, and chilling a water-cooled copper crucible to obtain the seed crystal for TiAl-based alloy directional solidification, wherein the raw materials are added in a layered mode before smelting, namely a titanium sponge layer, a high-purity aluminum layer, a high-purity silicon layer and a titanium sponge layer from bottom to top respectively; in the high-power melting process, the alloy has higher superheat degree, can produce larger liquid state to shrink in the traditional cooling process, apt to form the larger shrinkage cavity area, the invention adopts and reduces the power of the power slowly first, after homogenizing the melt, chill and prepare the seed crystal with the crucible, can reduce the superheat degree of the liquid metal apparently, reduce the liquid state to shrink, thus has obviously reduced the shrinkage cavity area of the seed crystal material.
Drawings
FIG. 1 is a schematic view of a macroscopic structure observed from a transverse cross section of a Ti-43Al-3Si seed crystal prepared in example 1 of the present invention which is transversely cast by wire electrical discharge machining;
FIG. 2 is a schematic view of a microstructure observed from a longitudinal cross section of a Ti-43Al-3Si seed crystal prepared in example 1 of the present invention which is longitudinally cast by wire electrical discharge machining;
FIG. 3 is a schematic view of a macroscopic structure observed from a transverse cross section of Ti-46Al-1.5Mo-1Si seed crystals prepared in example 1 of the present invention which are laterally thrown away by wire electrical discharge machining;
FIG. 4 is a schematic view showing a microstructure observed from a longitudinal cross section of a Ti-46Al-1.5Mo-1Si seed crystal prepared in example 1 of the present invention, which is longitudinally cast by wire electrical discharge machining.
Detailed Description
The invention will be further illustrated with reference to specific embodiments, with reference to fig. 1-4.
Example 1
The invention provides a seed crystal preparation method for TiAl-based alloy directional solidification, which comprises the following steps:
s1, preparing seed crystal raw materials respectively, wherein the seed crystal raw materials comprise 0-grade sponge titanium, high-purity aluminum and high-purity silicon, wherein Al accounts for 43 at.%, Mo accounts for 0 at.%, Si accounts for 3 at.%, and the balance is Ti;
s2, adding the seed crystal raw materials prepared in the step S1 into a water-cooled copper crucible vacuum induction smelting furnace in a layered mode, wherein the seed crystal raw materials are respectively a 0-level titanium sponge layer, a high-purity aluminum layer, a high-purity silicon layer and a 0-level titanium sponge layer from bottom to top;
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 0.03Pa below Pa;
s4, turning on a power supply, increasing the power of the power supply to 55kW at a speed of 5kW/min, and smelting for 3 min;
s5, reducing the power of a power supply to 50kW at the rate of 0.4kW/min, and continuing to keep the temperature for 2min to obtain a 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-43Al-3Si seed crystal ingot.
Example 2
The invention provides a seed crystal preparation method for TiAl-based alloy directional solidification, which comprises the following steps:
s1, preparing seed crystal raw materials respectively, wherein the seed crystal raw materials comprise 0-grade sponge titanium, high-purity aluminum and high-purity silicon, wherein the Al accounts for 46 at.%, the Mo accounts for 1.5 at.%, the Si accounts for 1 at.%, and the balance is Ti;
s2, adding the seed crystal raw materials prepared in the step S1 into a water-cooled copper crucible vacuum induction smelting furnace in a layered mode, wherein the seed crystal raw materials are respectively a 0-level titanium sponge layer, a high-purity aluminum layer, a high-purity silicon layer and a 0-level titanium sponge layer from bottom to top;
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 0.07Pa 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 3 min;
s5, reducing the power of the power supply to 55kW at the rate of 0.6kW/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-1.5Mo-1.0Si seed crystal ingot.
Example 3
The invention provides a seed crystal preparation method for TiAl-based alloy directional solidification, which comprises the following steps:
s1, preparing seed crystal raw materials respectively, wherein the seed crystal raw materials comprise 0-grade sponge titanium, high-purity aluminum and high-purity silicon, wherein the Al accounts for 46 at.%, the Mo accounts for 1.5 at.%, the Si accounts for 1.2 at.%, and the balance is Ti;
s2, adding the seed crystal raw materials prepared in the step S1 into a water-cooled copper crucible vacuum induction smelting furnace in a layered mode, wherein the seed crystal raw materials are respectively a 0-level titanium sponge layer, a high-purity aluminum layer, a high-purity silicon layer and a 0-level titanium sponge layer from bottom to top;
s3, vacuumizing a smelting chamber in the vacuum induction smelting furnace to 2 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 rate of 3kW/min, and smelting for 5 min;
s5, reducing the power of the power supply to 55kW at the rate of 0.5kW/min, and continuing to keep the temperature for 5min 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 a seed crystal ingot, namely the Ti-46Al-1.5Mo-1.2Si seed crystal ingot.
Example 4
The invention provides a seed crystal preparation method for TiAl-based alloy directional solidification, which comprises the following steps:
s1, preparing seed crystal raw materials respectively, wherein the seed crystal raw materials comprise 0-grade sponge titanium, high-purity aluminum and high-purity silicon, wherein the Al accounts for 46 at.%, the Mo accounts for 1.5 at.%, the Si accounts for 0.8 at.%, and the balance is Ti;
s2, adding the seed crystal raw materials prepared in the step S1 into a water-cooled copper crucible vacuum induction smelting furnace in a layered mode, wherein the seed crystal raw materials are respectively a 0-level titanium sponge layer, a high-purity aluminum layer, a high-purity silicon layer and a 0-level titanium sponge layer from bottom to top;
s3, vacuumizing a smelting chamber in the vacuum induction smelting furnace to 1 x 10-3Introducing argon into the vacuum induction melting furnace to 0.05Pa below Pa;
s4, turning on a power supply, increasing the power of the power supply to 55kW at the speed of 6kW/min, and smelting for 3-5 min;
s5, reducing the power of a power supply to 50kW at the rate of 0.4kW/min, and continuing to keep the temperature for 5min to obtain a 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-1.5Mo-0.8Si seed crystal ingot.
Comparative example 1
A seed crystal preparation method for directional solidification of TiAl-based alloy comprises the following steps:
s1, preparing seed crystal raw materials respectively, wherein the seed crystal raw materials comprise 0-grade sponge titanium, high-purity aluminum and high-purity silicon, wherein Al accounts for 43 at.%, Mo accounts for 0 at.%, Si accounts for 3 at.%, and the balance is Ti;
s2, directly 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 0.03Pa below Pa;
s4, turning on a power supply, increasing the power of the power supply to 55kW at a speed of 5kW/min, and smelting for 3 min;
s5, reducing the power of a power supply to 50kW at the rate of 0.4kW/min, and continuing to keep the temperature for 2min to obtain a 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-43Al-3Si seed crystal ingot.
Comparative example 2
A seed crystal preparation method for directional solidification of TiAl-based alloy comprises the following steps:
s1, preparing seed crystal raw materials respectively, wherein the seed crystal raw materials comprise 0-grade sponge titanium, high-purity aluminum and high-purity silicon, wherein Al accounts for 43 at.%, Mo accounts for 0 at.%, Si accounts for 3 at.%, and the balance is Ti;
s2, adding the seed crystal raw materials prepared in the step S1 into a water-cooled copper crucible vacuum induction smelting furnace in a layered mode, wherein the seed crystal raw materials are respectively a 0-level titanium sponge layer, a high-purity aluminum layer, a high-purity silicon layer and a 0-level titanium sponge layer from bottom to top;
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 0.03Pa below Pa;
s4, turning on a power supply, increasing the power of the power supply to 55kW at a speed of 5kW/min, and smelting for 3min to obtain seed crystal melt;
and S5, 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-43Al-3Si seed crystal ingot.
Comparative example 3
The Ti-43Al-3Si seed crystal ingot is prepared by the traditional directional solidification method of gold.
Compared with comparative example 3, the shrinkage area of example 1 is only 65.4% of that of comparative example 3, compared with comparative example 3, the shrinkage area of comparative example 1 is only 89.4% of that of comparative example 3, and compared with comparative example 3, the shrinkage area of comparative example 2 is only 85.4% of that of comparative example 3. The experimental result shows that the seed crystal shrinkage cavity area obtained by the embodiment of the invention is obviously smaller than that of 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 (7)
1. A seed crystal preparation method for TiAl-based alloy directional solidification 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 and high-purity silicon, wherein the mass percent of Al is 43-46 at.%, the mass percent of Mo is 0-1.5 at.%, the mass percent of Si is 0.8-3 at.%, and the balance is Ti;
s2, adding the seed crystal raw materials prepared in the step S1 into a water-cooled copper crucible vacuum induction melting furnace in a layered mode;
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, 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 3-5 min;
s5, 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 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 seed crystal ingot for directional solidification of the TiAl-based alloy.
2. A seed crystal preparation method for TiAl-based alloy directional solidification according to claim 1, wherein in step S1, the titanium sponge is grade 0 titanium sponge.
3. A seed crystal preparation method for directional solidification of TiAl-based alloy according to claim 1, wherein in step S1, Al in the seed crystal raw material is 43 at.%, Mo is 0 at.%, Si is 3 at.%, and the rest is Ti.
4. A seed crystal preparation method for directional solidification of TiAl-based alloy according to claim 1, wherein in step S1, Al in the seed crystal raw material is 46 at.%, Mo is 1.5 at.%, Si is 1 at.%, and the rest is Ti.
5. A seed crystal preparation method for TiAl-based alloy directional solidification according to claim 1, wherein in step S2, the layered titanium sponge layer, the high purity aluminum layer, the high purity silicon layer and the titanium sponge layer are respectively from bottom to top.
6. A seed crystal preparation method for TiAl-based alloy directional solidification according to claim 1, wherein in step S4, the power supply power is increased at a rate of 5 kw/min.
7. A seed crystal preparation method for TiAl-based alloy directional solidification according to claim 1, wherein in step S4, the cooling rate of power supply power is 0.5 kw/min.
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| CN103695708A (en) * | 2013-12-04 | 2014-04-02 | 北京工业大学 | W-containing and high-Nb novel beta-gammaTiAl intermetallic compound material and preparation method thereof |
| CN103820676A (en) * | 2014-03-12 | 2014-05-28 | 北京工业大学 | Cr and V alloying beta phase solidifying high Nb-TiAl alloy and preparation method thereof |
| CN105088329A (en) * | 2015-02-02 | 2015-11-25 | 西北工业大学 | Preparation method of TiAl alloy quasi seed crystals |
| US20170268127A1 (en) * | 2014-10-09 | 2017-09-21 | Nanjing University Of Science And Technology | Tial intermetallic compound single crystal material and preparation method therefor |
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2020
- 2020-12-21 CN CN202011516112.4A patent/CN112746329A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103695708A (en) * | 2013-12-04 | 2014-04-02 | 北京工业大学 | W-containing and high-Nb novel beta-gammaTiAl intermetallic compound material and preparation method thereof |
| CN103820676A (en) * | 2014-03-12 | 2014-05-28 | 北京工业大学 | Cr and V alloying beta phase solidifying high Nb-TiAl alloy and preparation method thereof |
| US20170268127A1 (en) * | 2014-10-09 | 2017-09-21 | Nanjing University Of Science And Technology | Tial intermetallic compound single crystal material and preparation method therefor |
| CN105088329A (en) * | 2015-02-02 | 2015-11-25 | 西北工业大学 | Preparation method of TiAl alloy quasi seed crystals |
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