CN110499483B - High-alloying GH4720Li alloy single-stage homogenization annealing process - Google Patents
High-alloying GH4720Li alloy single-stage homogenization annealing process Download PDFInfo
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Abstract
The invention discloses a high-alloying GH4720Li alloy single-stage homogenization annealing process, which comprises the following steps: step one, heating the high-alloying GH4720Li alloy to 1120 ℃ at a heating rate of 10-20 ℃/min; and step two, heating the high-alloying GH4720Li alloy heated to 1120 ℃ in the step one to 1180-1230 ℃ at a heating rate of 1-5 ℃/min, preserving heat for 8-28 h, and then carrying out furnace cooling. According to the invention, the (gamma + gamma') eutectic phase and boride low-melting-point precipitated phase existing in the high-alloying GH4720Li alloy are eliminated by controlling the single-stage homogenization temperature rise rate, temperature and heat preservation time, so that the Al, Ti, W and Mo elements are promoted to be fully diffused, the element segregation is eliminated, the overburning phenomenon cannot occur in the annealing process, and the high-alloying GH4720Li alloy with uniform components is obtained.
Description
Technical Field
The invention belongs to the field of metal materials and processing thereof, and particularly relates to a high-alloying GH4720Li alloy single-stage homogenization annealing process.
Background
The high-temperature alloy is a key hot-end material of an advanced aerospace engine, comprises hot-end components such as a turbine disc, a turbine blade, a guide blade and a combustion chamber, and is applied to the advanced aerospace engine in a proportion of more than 40%. In order to meet the requirement of rapid development of modern aviation industry, higher content of gamma' phase elements such as Al and Ti and refractory metal elements such as W, Mo and Nb are often added into the high-temperature alloy, so that the macro and micro segregation degree is higher. Further, with the increase in the degree of alloying and the enlargement of the ingot form, the solidification segregation tendency of the alloy is increased, and the severe solidification segregation causes the dendritic structure of the ingot to be developed sufficiently, and a large amount of harmful brittle phases are formed between the dendrites, thereby deteriorating the hot workability of the alloy. In the prior art, the ingot type is high-alloying GH4720Li alloy with phi 508mm which is smelted by adopting a triple process of vacuum induction smelting (VIM), protective atmosphere electroslag remelting (ESR) and vacuum consumable remelting (VAR), wherein the defects of serious segregation of elements such as Al, Ti, W, Mo and the like, formation of a large amount of (gamma + gamma') eutectic phase among dendrites, precipitation of low melting points such as boride and the like exist. Therefore, the melted high-alloying high-temperature alloy is generally subjected to homogenization annealing to dissolve the interdendritic eutectic phase and the low-melting-point precipitation phase and eliminate element segregation as much as possible before cogging forging, so that the hot workability of the high-alloying high-temperature alloy is improved.
The research on the homogenization annealing process of high-alloying high-temperature alloys such as GH4169 is relatively mature, and corresponding standards and databases are formed, so that the problem of segregation of Al, Ti, W, Mo and other elements such as Nb is well solved, and the hot-working performance of the alloy is improved. However, for the high-alloying GH4720Li alloy with the ingot shape of phi 508mm, which is smelted by adopting the triple process of vacuum induction smelting, protective atmosphere electroslag remelting and vacuum consumable remelting, a low-melting-point precipitated phase is easy to over-burn to form holes, and the diffusion rule is more complicated due to the interaction among elements such as Al, Ti, W, Mo and the like. If the homogenization annealing system is not properly selected, serious tissue problems can easily occur in the forging, such as that strip tissues are not completely formed in the forging due to incomplete segregation elimination, and the forging is scrapped. At present, a multi-stage homogenization annealing process is often adopted for high-alloying high-temperature alloy, the annealing process is complex and long in period, and the production cost is high, so that the establishment of a reasonable homogenization annealing system is particularly important for the high-alloying high-temperature alloy.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-alloying GH4720Li alloy single-stage homogenizing annealing process aiming at the defects of the prior art, and the process eliminates (gamma + gamma') eutectic phase and boride low-melting-point precipitated phase of the high-alloying GH4720Li alloy by controlling the process parameters of the temperature rise rate, the temperature and the heat preservation time of the single-stage homogenizing annealing, simultaneously promotes the Al, Ti, W and Mo elements among dendrites and dendrite stems to be fully diffused, eliminates element segregation, does not generate an overburning phenomenon in the annealing process, and solves the problems of easy overburning and element segregation residue in the homogenizing annealing process of the high-alloying GH4720Li alloy.
In order to solve the technical problems, the invention adopts the technical scheme that: a high-alloying GH4720Li alloy single-stage homogenization annealing process is characterized by comprising the following steps:
step one, heating a high-alloying GH4720Li alloy ingot casting sample to 1120 ℃ at a heating rate of 10-20 ℃/min; the high-alloying GH4720Li alloy cast ingot is obtained by smelting through a triple process of vacuum induction smelting, protective atmosphere electroslag remelting and vacuum consumable remelting, and the ingot shape is phi 508 mm;
step two, heating the high-alloying GH4720Li alloy ingot casting sample heated to 1120 ℃ in the step one to 1180-1230 ℃ at a heating rate of 1-5 ℃/min, preserving heat for 8-28 h, and then cooling along with the furnace; the time of the heat preservation is reduced along with the increase of the heating temperature.
The invention firstly heats the high alloying GH4720Li alloy to 1120 ℃ at the heating rate of 10-20 ℃/min, then heats the alloy to 1180-1230 ℃ at the heating rate of 1-5 ℃/min, and then keeps the temperature for 8-28 h. The invention adopts the rapid heating of 10-20 ℃/min to 1120 ℃, improves the production efficiency, is easy to realize in industrial production, ensures the slow re-dissolution of (gamma + gamma') eutectic phase and the gradual re-dissolution of Al, Ti, Mo and W elements among dendrites and dendrites of the high-alloying GH4720Li alloy by adopting the heating rate of 1-5 ℃/min, and inhibits the phenomena of overburning of the low-melting-point precipitated phase and insufficient diffusion of the Al, Ti, W and Mo elements caused by the over-high heating rate, meanwhile, the heating time is saved, the production efficiency is improved, the heat preservation is carried out for 8 to 28 hours after the heating is carried out to 1180 to 1230 ℃, in the continuous heating and heat preservation process, the eutectic phase (gamma + gamma ') of the high-alloying GH4720Li alloy is eliminated, the low-melting-point precipitated phase of boride is dissolved back, Al, Ti, W and Mo elements among dendrites and dry dendrites are fully diffused, the element segregation is eliminated, the overburning phenomenon cannot occur, the problems of easy overburning and element segregation residue in the homogenization annealing process of the high-alloying GH47 4720Li alloy are solved, the aim of homogenization annealing is achieved, the heating and heat preservation temperature range is 1180 to 1230 ℃, the gamma' dissolving temperature of the high-alloying GH47 4720Li alloy is above 1160 ℃ and below 1250 ℃, the requirement of the annealing temperature is met, the low-melting-point precipitated phase can be eliminated after the long-time heat preservation is close to 1180 ℃, but the efficiency is lower, and when the temperature is higher than 1230 ℃, the low-melting-point precipitated phase is easy to cause overb, the heat preservation time of 8-28 h is determined by the heating temperature, the diffusion coefficient of Al, Ti, W and Mo elements increases exponentially along with the temperature rise, longer heat preservation time is needed to realize the full diffusion of the elements at lower heat preservation temperature, and the higher heat preservation temperature can shorten the heat preservation time and further improve the production efficiency.
In the single-stage homogenization annealing process of the high-alloying GH4720Li alloy, the temperature rise rate in the second step is 3-5 ℃/min. The heating rate adopted by the invention is 3-5 ℃/min, the slow re-dissolution of (gamma + gamma') eutectic phase and boride low-melting-point precipitated phase of the high-alloying GH4720Li alloy and the slow diffusion of Al, Ti, Mo and W elements are ensured, the heating time is shortened, the production efficiency is improved, and the overburning of the low-melting-point precipitated phase and the insufficient diffusion of the Al, Ti, W and Mo elements caused by the over-high heating rate are inhibited.
In the second step, the high-alloying GH4720Li alloy single-stage homogenization annealing process is carried out for 8 hours after the heating to 1230 ℃. The invention adopts the heat preservation for 8h after heating to 1230 ℃, the higher temperature can shorten the heat preservation time, improve the production efficiency, simultaneously avoid the overburning caused by long-time heat preservation at the lower temperature, realize the elimination of the (gamma + gamma') eutectic phase and the boride low-melting-point precipitated phase of the high-alloying GH4720Li alloy, promote the sufficient diffusion of Al, Ti, W and Mo elements among dendrites and dendrite trunks, eliminate the element segregation, and avoid the overburning phenomenon in the annealing process, thereby solving the problems of easy overburning and element segregation residue in the homogenization annealing process of the high-alloying GH4720Li alloy.
The high-alloying GH4720Li alloy single-stage homogenization annealing process has the temperature rise rate of 5 ℃/min. The heating rate adopted by the invention is 5 ℃/min, the heating time is saved, and the production efficiency is improved.
Compared with the prior art, the invention has the following advantages:
1. the high-alloying GH4720Li alloy obtained by triple melting of vacuum induction melting, protective atmosphere electroslag remelting and vacuum consumable remelting is subjected to single-stage homogenization annealing, so that (gamma + gamma') eutectic phases and boride low-melting-point precipitated phases of the high-alloying GH4720Li alloy are eliminated, Al, Ti, W and Mo elements among dendrites and dendrite trunks are promoted to be fully diffused, element segregation is eliminated, an overburning phenomenon cannot occur in the annealing process, the problems of easy overburning and element segregation residue in the homogenization annealing process of the high-alloying GH47 4720Li alloy are solved, and the high-alloying GH4720Li alloy with uniform components is obtained.
2. The invention realizes the single-stage homogenization annealing of the high-alloying GH4720Li alloy by controlling the process parameters of the heating rate, the temperature and the heat preservation time of the single-stage homogenization annealing, the heating rate of 10-20 ℃/min is adopted to quickly heat up below 1120 ℃, the production efficiency is improved, the heating rate of 1-5 ℃/min is adopted above 1120 ℃, the overburning of low-melting-point phase easily caused by the overhigh heating rate is avoided, the heating time is saved, the production efficiency is improved, the heating to 1230 ℃ is adopted to preserve heat for 8 hours, the heat preservation time is shortened, and the production efficiency is improved.
3. The invention has the advantages of simple process operation, high production efficiency, low production cost and wider applicability.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1a is an OM picture of a high alloying GH4720Li alloy used in example 1 of the present invention.
FIG. 1b is an SEM image of a high alloying GH4720Li alloy used in example 1 of the present invention.
FIG. 2 is an SEM image of a highly alloyed GH4720Li alloy after a single-stage homogenizing anneal in example 1 of the present invention.
FIG. 3 is an SEM image of a highly alloyed GH4720Li alloy after a single stage homogenizing anneal according to comparative example 1 of the present invention.
FIG. 4 is an SEM image of a high alloyed GH4720Li alloy after two stage homogenizing annealing of comparative example 2 of the present invention.
FIG. 5 is an SEM image of a highly alloyed GH4720Li alloy after a single-stage homogenizing anneal in accordance with example 2 of the invention.
Detailed Description
Example 1
The embodiment comprises the following steps:
firstly, cutting a high-alloying GH4720Li alloy ingot with the ingot shape of phi 508mm, which is smelted by adopting a triple process of vacuum induction smelting, protective atmosphere electroslag remelting and vacuum consumable remelting, from the head to obtain an ingot slice with the thickness of 20mm, then cutting a high-alloying GH4720Li alloy sample with the thickness of 10mm multiplied by 10mm (length multiplied by width multiplied by height) at the core of the ingot slice, then placing the high-alloying GH4720Li alloy sample in a high-temperature box furnace, and heating to 1120 ℃ at the heating rate of 10 ℃/min;
and step two, heating the high-alloying GH4720Li alloy sample heated to 1120 ℃ in the step one to 1230 ℃ at the heating rate of 5 ℃/min, preserving the heat for 8 hours, and then cooling along with the furnace.
Fig. 1a is a diagram of an as-cast structure OM of a high-alloying GH4720Li alloy used in the present embodiment, fig. 1b is a SEM diagram of a high-alloying GH4720Li alloy used in the present embodiment, and it can be seen from fig. 1a and 1b that (γ + γ') eutectic phase and low-melting-point precipitation phase defects exist in the as-cast structure of the high-alloying GH4720Li alloy with the ingot shape of Φ 508mm which is smelted by the triple remelting process of vacuum induction smelting, protective atmosphere electroslag remelting and vacuum consumable electrode remelting.
Fig. 2 is an SEM image of the high-alloying GH4720Li alloy after the single-stage homogenizing annealing in this embodiment, and it can be seen from fig. 2 that the high-alloying GH4720Li alloy after the single-stage homogenizing annealing has residual carbides, no (γ + γ') eutectic phase and low-melting-point precipitated phase defects are found around the residual carbides, no obvious holes exist, and no overburning occurs, which illustrates that the segregation of Al, Ti, W, and Mo elements in the high-alloying GH4720Li alloy after the single-stage homogenizing annealing in this embodiment is fully diffused and completely eliminated, and a good single-stage homogenizing annealing effect is obtained.
As can be seen from comparison of fig. 1a, fig. 1b and fig. 2, the (γ + γ ') eutectic phase and the low-melting-point precipitated phase of the high-alloying GH4720Li alloy after single-stage homogenization annealing in the present embodiment are eliminated, and no obvious holes exist, which indicates that the (γ + γ') eutectic phase and the low-melting-point precipitated phase of boride of the high-alloying GH4720Li alloy after single-stage homogenization annealing are relatively completely re-dissolved, no overburning occurs, and a good single-stage homogenization annealing effect is obtained.
Comparative example 1
This comparative example comprises the following steps:
firstly, cutting a high-alloying GH4720Li alloy ingot with the ingot shape of phi 508mm, which is smelted by adopting a triple process of vacuum induction smelting, protective atmosphere electroslag remelting and vacuum consumable remelting, from the head to obtain an ingot slice with the thickness of 20mm, then cutting a high-alloying GH4720Li alloy sample with the thickness of 10mm multiplied by 10mm (length multiplied by width multiplied by height) at the core of the ingot slice, then placing the high-alloying GH4720Li alloy sample in a high-temperature box furnace, and heating to 1120 ℃ at the heating rate of 10 ℃/min;
and step two, heating the high-alloying GH4720Li alloy sample heated to 1120 ℃ in the step one to 1230 ℃ at the heating rate of 10 ℃/min, preserving the heat for 8 hours, and then cooling along with the furnace.
FIG. 3 is an SEM image of a high-alloying GH4720Li alloy after a single-stage homogenizing annealing in the comparative example, and it can be seen from FIG. 3 that the high-alloying GH4720Li alloy after the single-stage homogenizing annealing has obvious carbide residues, and holes formed by overburning of a low-melting-point phase are formed around the carbide residues.
As can be seen by comparing FIG. 2 with FIG. 3, the high alloying GH4720Li alloy after single-stage homogenizing annealing of the comparative example obviously has pores formed by overburning, which indicates that the temperature rise rate used by the comparative example is too high, so that the low melting point precipitation phase of the high alloying GH4720Li alloy generates pores by overburning, and the high alloying GH4720Li alloy is rejected.
Comparative example 2
This comparative example comprises the following steps:
firstly, cutting a high-alloying GH4720Li alloy ingot with the ingot shape of phi 508mm, which is smelted by adopting a triple process of vacuum induction smelting, protective atmosphere electroslag remelting and vacuum consumable remelting, from the head to obtain an ingot slice with the thickness of 20mm, then cutting a high-alloying GH4720Li alloy sample with the thickness of 10mm multiplied by 10mm (length multiplied by width multiplied by height) at the core of the ingot slice, then placing the high-alloying GH4720Li alloy sample in a high-temperature box furnace, and heating to 1120 ℃ at the heating rate of 10 ℃/min;
and step two, heating the high-alloying GH4720Li alloy sample heated to 1120 ℃ in the step one to 1180 ℃ at the heating rate of 10 ℃/min, preserving heat for 24 hours, then heating to 1230 ℃ at the heating rate of 10 ℃/min, preserving heat for 28 hours, and then cooling along with the furnace.
FIG. 4 is an SEM image of a high-alloying GH4720Li alloy after the two-stage homogenizing annealing in this comparative example, and it can be seen from FIG. 4 that the high-alloying GH4720Li alloy obtained by the two-stage homogenizing annealing in the prior art in this comparative example has carbide residue and holes formed by overburning of low-melting precipitation phase around the carbide residue.
As can be seen by comparing FIG. 2 with FIG. 4, the high-alloying GH4720Li alloy obtained by the two-stage homogenizing annealing in the prior art of the comparative example obviously has pores formed by overburning, which indicates that the high-alloying GH4720Li alloy is scrapped because the overburning of the low-melting-point precipitation phase still exists in the case of the high-alloying GH4720Li alloy by the two-stage homogenizing annealing.
Example 2
The embodiment comprises the following steps:
firstly, cutting a high-alloying GH4720Li alloy ingot with the ingot shape of phi 508mm, which is smelted by adopting a triple process of vacuum induction smelting, protective atmosphere electroslag remelting and vacuum consumable remelting, from the head to obtain an ingot slice with the thickness of 20mm, then cutting a high-alloying GH4720Li alloy sample with the thickness of 10mm multiplied by 10mm (length multiplied by width multiplied by height) at the core of the ingot slice, then placing the high-alloying GH4720Li alloy sample in a high-temperature box furnace, and heating to 1120 ℃ at the temperature rising rate of 15 ℃/min;
and step two, heating the high-alloying GH4720Li alloy sample heated to 1120 ℃ in the step one to 1180 ℃ at the heating rate of 1 ℃/min, preserving heat for 28h, and then cooling along with the furnace.
Fig. 5 is an SEM image of the high-alloying GH4720Li alloy after single-stage homogenization annealing in this example, and it can be seen from fig. 5 that there is carbide residue in the high-alloying GH4720Li alloy after single-stage homogenization annealing, no (γ + γ') eutectic phase and low-melting precipitation phase defects are found around the carbide residue, no obvious holes exist, and no overburning occurs, which illustrates that the segregation of Al, Ti, W, and Mo elements in the high-alloying GH4720Li alloy after single-stage homogenization annealing in this example is fully diffused and completely eliminated, and a good single-stage homogenization annealing effect is obtained.
Example 3
The embodiment comprises the following steps:
firstly, cutting a high-alloying GH4720Li alloy ingot with the ingot shape of phi 508mm, which is smelted by adopting a triple process of vacuum induction smelting, protective atmosphere electroslag remelting and vacuum consumable remelting, from the head to obtain an ingot slice with the thickness of 20mm, then cutting a high-alloying GH4720Li alloy sample with the thickness of 10mm multiplied by 10mm (length multiplied by width multiplied by height) at the core of the ingot slice, then placing the high-alloying GH4720Li alloy sample in a high-temperature box furnace, and heating to 1120 ℃ at the heating rate of 20 ℃/min;
and step two, heating the high-alloying GH4720Li alloy sample heated to 1120 ℃ in the step one to 1200 ℃ at the heating rate of 3 ℃/min, preserving heat for 16h, and then cooling along with the furnace.
The detection shows that the (gamma + gamma') eutectic phase and the boride low-melting-point precipitated phase of the high-alloying GH4720Li alloy subjected to single-stage homogenizing annealing in the embodiment are completely redissolved, no obvious holes exist, no overburning phenomenon occurs, the segregation of Al, Ti, W and Mo elements is fully diffused, the segregation is thoroughly eliminated, and a good homogenizing annealing effect is obtained.
Example 4
The embodiment comprises the following steps:
firstly, cutting a high-alloying GH4720Li alloy ingot with the ingot shape of phi 508mm, which is smelted by adopting a triple process of vacuum induction smelting, protective atmosphere electroslag remelting and vacuum consumable remelting, from the head to obtain an ingot slice with the thickness of 20mm, then cutting a high-alloying GH4720Li alloy sample with the thickness of 10mm multiplied by 10mm (length multiplied by width multiplied by height) at the core of the ingot slice, then placing the high-alloying GH4720Li alloy sample in a high-temperature box furnace, and heating to 1120 ℃ at the heating rate of 10 ℃/min;
and step two, heating the high-alloying GH4720Li alloy sample heated to 1120 ℃ in the step one to 1230 ℃ at the heating rate of 4 ℃/min, preserving the heat for 8h, and then cooling along with the furnace.
The detection shows that the (gamma + gamma') eutectic phase and the boride low-melting-point precipitated phase of the high-alloying GH4720Li alloy subjected to single-stage homogenizing annealing in the embodiment are completely redissolved, no obvious holes exist, no overburning phenomenon occurs, the segregation of Al, Ti, W and Mo elements is fully diffused, the segregation is thoroughly eliminated, and a good homogenizing annealing effect is obtained.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (4)
1. A high-alloying GH4720Li alloy single-stage homogenization annealing process is characterized by comprising the following steps:
step one, heating a high-alloying GH4720Li alloy ingot casting sample to 1120 ℃ at a heating rate of 10-20 ℃/min; the high-alloying GH4720Li alloy cast ingot is obtained by smelting through a triple process of vacuum induction smelting, protective atmosphere electroslag remelting and vacuum consumable remelting, and the ingot shape is phi 508 mm;
step two, heating the high-alloying GH4720Li alloy ingot casting sample heated to 1120 ℃ in the step one to 1180-1230 ℃ at a heating rate of 1-5 ℃/min, preserving heat for 8-28 h, and then cooling along with the furnace; the time of the heat preservation is reduced along with the increase of the heating temperature.
2. The process according to claim 1, wherein the temperature increase rate in the second step is 3 ℃/min to 5 ℃/min.
3. The process according to claim 2, wherein in step two, the temperature is maintained for 8h after heating to 1230 ℃.
4. The process of claim 2, wherein the temperature increase rate in step two is 5 ℃/min.
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| US5120373A (en) * | 1991-04-15 | 1992-06-09 | United Technologies Corporation | Superalloy forging process |
| CN106636848A (en) * | 2017-01-18 | 2017-05-10 | 东南大学 | Preparation method of abrasion-proof and corrosion-resistant nickel-based alloy wire |
| CN108441704A (en) * | 2018-03-15 | 2018-08-24 | 江苏理工学院 | A kind of Refractoloy material and its preparation process |
| CN109022925A (en) * | 2018-08-23 | 2018-12-18 | 重庆材料研究院有限公司 | A method of reducing Laves phase in nickel base superalloy steel ingot |
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| GB2475064B (en) * | 2009-11-04 | 2011-12-14 | Rolls Royce Plc | A method of producing an oxide coated nickel-base superalloy and a method of producing an oxide dispersion strengthened nickel-base superalloy |
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|---|---|---|---|---|
| US5120373A (en) * | 1991-04-15 | 1992-06-09 | United Technologies Corporation | Superalloy forging process |
| CN106636848A (en) * | 2017-01-18 | 2017-05-10 | 东南大学 | Preparation method of abrasion-proof and corrosion-resistant nickel-based alloy wire |
| CN108441704A (en) * | 2018-03-15 | 2018-08-24 | 江苏理工学院 | A kind of Refractoloy material and its preparation process |
| CN109022925A (en) * | 2018-08-23 | 2018-12-18 | 重庆材料研究院有限公司 | A method of reducing Laves phase in nickel base superalloy steel ingot |
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