CN112974731B - Method for preparing single crystal superalloy by repeatedly using solid solution state columnar crystal - Google Patents
Method for preparing single crystal superalloy by repeatedly using solid solution state columnar crystal Download PDFInfo
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- CN112974731B CN112974731B CN202110508886.0A CN202110508886A CN112974731B CN 112974731 B CN112974731 B CN 112974731B CN 202110508886 A CN202110508886 A CN 202110508886A CN 112974731 B CN112974731 B CN 112974731B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
- B22C9/02—Sand moulds or like moulds for shaped castings
- B22C9/04—Use of lost patterns
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22C3/00—Selection of compositions for coating the surfaces of moulds, cores, or patterns
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- B22—CASTING; POWDER METALLURGY
- 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
- 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
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- 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
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Abstract
According to the method for repeatedly using the solid solution state columnar crystal to prepare the single crystal high-temperature alloy, the corundum tube with the same length as the crystal starting section of the spiral crystal selector wax mold is sleeved into the crystal starting section of the spiral crystal selector wax mold, and the gap between the corundum tube and the crystal starting section is filled with the molten wax, so that the probability of chilling to form mixed crystals due to the fact that the single crystal high-temperature alloy enters the gap between the ceramic mold shell and the unmelted single crystal caused by pouring can be effectively avoided; the ceramic refractory slurry is coated outside the part wax mold, the spiral crystal selector wax mold and the corundum tube, so that the refractory performance of the formed ceramic mold shell can be improved. The invention can be smaller than the deviation range of the crystal orientation of the single crystal high-temperature alloy controlled by the crystal selection method at present, and can realize the repeated use of the solid solution columnar crystal to prepare the single crystal, thereby improving the success rate of the single crystal preparation and reducing the control cost of the single crystal orientation.
Description
Technical Field
The invention relates to the field of nickel-based single crystal manufacturing, in particular to a method for manufacturing a single crystal superalloy by repeatedly using solid solution columnar crystals.
Background
The nickel-based single crystal superalloy has excellent high-temperature comprehensive performance, is a preferred material of an aeroengine turbine blade, has remarkable anisotropy in mechanical property, and ensures that the <001> direction of the single crystal blade needs to be controlled within a certain range in the preparation process of the single crystal blade, so that the single crystal blade has longer service life. At present, the single crystal high temperature alloy is mainly prepared by a crystal selection method and a seed crystal method in industrial production. The crystal grains selected by the crystal selection method have certain randomness, and the deviation between the crystal orientation and the axial direction of a casting can be controlled within 15 degrees usually. The seed crystal method can realize the accurate control of crystal orientation, but because the seed crystal method needs to use the single crystal as the seed crystal when preparing the single crystal, the production cost is high, the process difficulty is large, and the seed crystal method is easy to form mixed crystal in a seed crystal melting zone when preparing the single crystal, the yield of the single crystal is low, so the seed crystal is difficult to be used in large scale in industrial production.
In order to further improve the front inlet temperature of the turbine and improve the performance of the aircraft engine, the content of refractory elements in the single crystal high-temperature alloy is gradually increased, the structure of a single crystal blade is more and more complex, so that the difficulty of controlling the single crystal orientation is continuously increased, the crystal selection method cannot meet the requirement on controlling the single crystal orientation, and a method which is more effective, has high success rate and is low in cost is urgently needed for controlling the crystal orientation of the single crystal high-temperature alloy.
Disclosure of Invention
The invention aims to provide a method for preparing a single crystal superalloy by repeatedly using solid solution columnar crystals, which aims to solve the technical problems of overlarge crystal orientation deviation and high preparation cost when a single crystal superalloy is prepared by a crystal selection method in the prior art.
The technical scheme of the invention is as follows: the method comprises the following steps:
firstly, preparing a wax mold of a spiral crystal selector, melting wax materials at the temperature of 60-100 ℃, injecting the melted wax materials into a part mold, and performing compression molding under the pressure of 0.5-8 MPa to prepare the part wax mold; melting the wax material at the temperature of 60-100 ℃, injecting the melted wax material into a spiral crystal selector mold, and performing compression molding under the pressure of 0.5-8 MPa to obtain the spiral crystal selector wax mold; the wax mould of the spiral crystal selector comprises a spiral section and a crystal starting section;
secondly, sleeving a corundum tube with the same length as the crystal starting section of the spiral crystal selector wax mold into the crystal starting section of the spiral crystal selector wax mold, and filling a gap between the corundum tube and the crystal starting section of the spiral crystal selector wax mold with molten wax; welding the part wax mold with one end of the spiral section of the spiral crystal selector wax mold; coating ceramic refractory slurry on the outer parts of the part wax mold, the spiral crystal selector wax mold and the corundum tube, dewaxing at the temperature of 100-200 ℃, and roasting at the temperature of 800-1300 ℃ for 2-10 hours to obtain a ceramic mold shell, wherein the ceramic mold shell is provided with a crystal starting section, a crystal selecting section and a part section;
thirdly, carrying out solid solution treatment on the columnar crystal test block, putting the directionally solidified high-temperature alloy body into a heat treatment furnace for heat preservation by adopting a one-step solid solution heat treatment method, and then cooling to obtain a solid solution columnar crystal test block;
fourthly, preparing solid solution columnar crystals, cutting a test block on the directionally solidified high-temperature alloy body along the solidification direction, and grinding the surface of the test block by adopting a grinding tool to obtain the solid solution columnar crystals; the shape of the solid solution columnar crystal is cylindrical; the height of the solid-solution columnar crystal is 20-50 mm, and the diameter of the solid-solution columnar crystal is 4-20 mm;
fifthly, preparing a single crystal high-temperature alloy casting, and filling solid solution columnar crystals into a crystal starting section of the ceramic mould shell; putting the solid-solution columnar crystal and the ceramic mould shell into a single crystal furnace together, adjusting the temperature in the single crystal furnace to 1400-1600 ℃, and preserving the temperature for 1-15 min; pouring the high-temperature alloy molten metal into a ceramic mould shell, and preserving heat for 1-15 min; moving the crystal puller downwards; after crystal pulling is finished, cooling the crystal to room temperature along with the furnace, and taking out the crystal to obtain a first monocrystal high-temperature alloy casting;
sixthly, recycling the repeatedly used columnar crystal, and removing the mould shell of the obtained single crystal high-temperature alloy test rod; disconnecting the obtained first single crystal superalloy casting from a boundary of a crystal selection section and a crystal starting section, and recovering the crystal starting section as reusable columnar crystals;
the seventh step, the recovered columnar crystals are subjected to solution treatment again, the columnar crystals recovered in the sixth step are subjected to solution treatment again in the third step, and the treated solid solution columnar crystal test block is the recovered solid solution columnar crystals;
eighthly, grinding the recovered solid solution columnar crystals; grinding the surface of the recovered solid solution columnar crystal by using a grinding tool to obtain a reusable columnar crystal;
ninth, preparing other single crystal high temperature alloy castings, and continuously preparing the single crystal high temperature alloy castings by utilizing the reusable solid solution state columnar crystals in the eighth step; filling the reusable solid solution state columnar crystal into the crystal starting section of the ceramic mould shell prepared in the second step; putting the solid-solution columnar crystal and the ceramic mould shell into a single crystal furnace together, adjusting the temperature in the single crystal furnace to 1400-1600 ℃, and preserving the temperature for 1-15 min; pouring the high-temperature alloy molten metal into a ceramic mould shell, and preserving heat for 1-15 min; moving the crystal puller downwards; after crystal pulling is finished, cooling the crystal to room temperature along with the furnace, and taking out the crystal to obtain a second single crystal high-temperature alloy casting; the temperature of the high-temperature alloy molten metal is 1400-1800 ℃.
Furthermore, in the second step, the ceramic mould shell crystal starting section takes a corundum tube as an inner wall.
Further, in the second step, the ceramic refractory slurry is coated outside the part wax mold, the spiral crystal selector wax mold and the corundum tube, and the thickness of the ceramic refractory slurry is 1-10 mm.
Further, in the third step, the temperature of the heat treatment furnace is 1100-1450 ℃, and heat preservation is carried out for 2-10 h.
Further, in the fifth step, the temperature of the high-temperature alloy molten metal is 1400-1800 ℃.
Further, in the fifth step, the gap between the solid solution columnar crystal and the inner wall of the crystal starting section of the ceramic formwork is 0.01-0.5 mm.
Further, in the ninth step, the gap between the solid solution columnar crystal and the inner wall of the crystal starting section of the ceramic mold shell is 0.01-0.5 mm.
Further, in the fifth step, the speed of downward movement of crystal pulling is 0.1-9 mm/min.
Further, in the ninth step, the speed of moving the crystal pulling downwards is 0.1-15 mm/min.
Further, in the fourth step and the eighth step, the sanding tool is 80#, 320#, 600# or 1000# sandpaper.
The invention provides a method for preparing single crystal superalloy by repeatedly using solid solution columnar crystal through improvement, compared with the prior art, the method has the following improvement and advantages:
the invention aims to prepare the single crystal high-temperature alloy by repeatedly using the solid solution state columnar crystal and combining the crystal selection method, the deviation of the crystal (001) direction from the directional solidification direction can be controlled within 5 ℃, the deviation range of the crystal orientation of the single crystal high-temperature alloy controlled by the crystal selection method can be smaller than that of the single crystal high-temperature alloy controlled by the crystal selection method at present, the single crystal can be prepared by repeatedly using the solid solution state columnar crystal, the success rate of preparing the single crystal is improved, and the cost for controlling the crystal orientation is reduced.
Secondly, the corundum tube with the same length as the crystal starting section of the spiral crystal selector wax mold is sleeved into the crystal starting section of the spiral crystal selector wax mold, and a gap between the corundum tube and the crystal starting section is filled with molten wax, so that the probability of forming mixed crystals by chilling due to the fact that single crystal high-temperature alloy enters a gap between a ceramic mold shell and unmelted single crystals caused by pouring can be effectively avoided; the ceramic refractory slurry is coated outside the part wax mold, the spiral crystal selector wax mold and the corundum tube, so that the refractory performance of the formed ceramic mold shell can be improved.
Drawings
The invention is further explained below with reference to the figures and examples:
FIG. 1 is a schematic view of a ceramic form construction;
FIG. 2 is a schematic view of a solid solution state columnar grain mold shell assembly;
FIG. 3 is a gold phase diagram of a single crystal superalloy prepared using the present method.
Description of reference numerals:
1. a ceramic mould shell crystal starting section; 2. selecting a crystal section of the ceramic mould shell; 3. a ceramic form element section; 4. a corundum tube; 5. columnar crystal.
Detailed Description
The present invention will be described in detail with reference to fig. 1 to 3, and the technical solutions in the embodiments of the present invention will be clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for repeatedly using solid solution columnar crystal to prepare single crystal superalloy by improvement, as shown in figures 1-3:
example 1:
the method for preparing the Ni-14Mo-7Al single crystal high-temperature alloy bar comprises the following specific steps:
firstly, preparing a wax mold of a spiral crystal selector, melting wax materials at the temperature of 75 ℃, injecting the melted wax materials into a part mold, and performing compression molding under the pressure of 0.5MPa to prepare the part wax mold; melting the wax material at 75 ℃, injecting the melted wax material into a spiral crystal selector mold, and performing compression molding under the pressure of 0.5MPa to obtain the spiral crystal selector wax mold; the wax mould of the spiral crystal selector comprises a spiral section and a crystal starting section;
secondly, sleeving a corundum tube with the same length as the crystal starting section of the spiral crystal selector wax mold into the crystal starting section of the spiral crystal selector wax mold, and filling a gap between the corundum tube and the crystal starting section of the spiral crystal selector wax mold with molten wax; welding the part wax mold with one end of the spiral section of the spiral crystal selector wax mold; coating 100mm ceramic refractory slurry outside a part wax mold, a spiral crystal selector wax mold and an alundum tube, dewaxing at 150 ℃, roasting at 1000 ℃ for 10 hours to obtain a ceramic mold shell, wherein the ceramic mold shell is provided with a crystal opening section, a crystal selection section and a part section corresponding to the wax mold structure, and the crystal opening section of the ceramic mold shell takes the alundum tube as an inner wall;
thirdly, carrying out solution treatment on the columnar crystal test block, putting the directionally solidified Ni-14Mo-7Al high-temperature alloy body into a heat treatment furnace at 1395 ℃ for 2h for heat preservation by adopting a one-step solution heat treatment method, and then cooling to obtain a solid solution columnar crystal test block;
fourthly, preparing solid solution columnar crystals, cutting a test block on the directionally solidified high-temperature alloy body along the solidification direction, and grinding the surface of the test block by using 80#, 320#, 600# or 1000# sand paper to obtain the solid solution columnar crystals; the shape of the solid solution columnar crystal is cylindrical; the height of the solid-solution columnar crystal is 20mm, and the diameter of the solid-solution columnar crystal is 20 mm;
fifthly, preparing a single crystal high-temperature alloy casting, and filling solid solution state columnar crystals into a crystal starting section of the ceramic formwork, wherein the gap between the solid solution state columnar crystals and the inner wall of the crystal starting section of the formwork is 0.5 mm; putting the solid-solution columnar crystal and the ceramic mould shell into a single crystal furnace together, adjusting the temperature in the single crystal furnace to 1580 ℃, and preserving the temperature for 1 min; pouring the high-temperature alloy molten metal into a ceramic mould shell, and keeping the temperature for 15 min; moving the crystal puller downwards at the speed of 3 mm/min; and after crystal pulling is finished, cooling the crystal to room temperature along with the furnace, and taking out the crystal to obtain a first monocrystal high-temperature alloy casting, wherein the temperature of the high-temperature alloy molten metal is 1400 ℃.
Sixthly, recycling the repeatedly used columnar crystal, and removing the mould shell of the obtained single crystal high-temperature alloy test rod; disconnecting the obtained first single crystal superalloy casting from a boundary of a crystal selection section and a crystal starting section, and recovering the crystal starting section as reusable columnar crystals;
seventhly, carrying out solid solution treatment on the recovered columnar crystals again, putting the columnar crystals recovered in the sixth step into a heat treatment furnace with the temperature of 1395 ℃ by adopting a one-step solid solution heat treatment method, carrying out heat preservation for 2 hours, and then cooling to obtain a solid solution columnar crystal test block; the solid solution columnar crystal test block is the recovered solid solution columnar crystal;
eighthly, grinding the recovered solid solution columnar crystals; grinding the surface of the recovered solid solution columnar crystal by using 80#, 320#, 600# or 1000# sandpaper to obtain reusable columnar crystal;
ninth, preparing other single crystal high temperature alloy castings, and continuously preparing the single crystal high temperature alloy castings by utilizing the reusable solid solution state columnar crystals in the eighth step; plugging the reusable solid solution state columnar crystal into the crystal starting section of the ceramic formwork prepared in the second step, wherein the gap between the reusable solid solution state columnar crystal and the inner wall of the crystal starting section of the formwork is 0.2 mm; putting the solid-solution columnar crystal and the ceramic mould shell into a single crystal furnace together, adjusting the temperature in the single crystal furnace to 1580 ℃, and preserving the temperature for 1 min; pouring the high-temperature alloy molten metal into a ceramic mould shell, and keeping the temperature for 15 min; moving the crystal puller downwards at the speed of 3 mm/min; after crystal pulling is finished, cooling the crystal to room temperature along with the furnace, and taking out the crystal to obtain a second single crystal high-temperature alloy casting; the temperature of the high-temperature alloy molten metal is 1400 ℃;
and repeating the sixth step to the ninth step, continuously recovering reusable solid solution state columnar crystals on the new single crystal high temperature alloy casting, and preparing the rest single crystal high temperature alloy castings by using the reusable solid solution state columnar crystals until the required number of single crystal high temperature alloy castings are obtained.
Example 2:
the preparation method of the Ni-13.5Mo-7.6 Al-0.05B single crystal high temperature alloy bar comprises the following steps:
firstly, preparing a wax mold of a spiral crystal selector, melting wax materials at the temperature of 100 ℃, injecting the melted wax materials into a part mold, and performing compression molding under the pressure of 8MPa to prepare the part wax mold; melting the wax material at 100 ℃, injecting the melted wax material into a spiral crystal selector mold, and performing compression molding under the pressure of 8MPa to obtain the spiral crystal selector wax mold; the wax mould of the spiral crystal selector comprises a spiral section and a crystal starting section;
secondly, sleeving a corundum tube with the same length as the crystal starting section of the spiral crystal selector wax mold into the crystal starting section of the spiral crystal selector wax mold, and filling a gap between the corundum tube and the crystal starting section of the spiral crystal selector wax mold with molten wax; welding the part wax mold with one end of the spiral section of the spiral crystal selector wax mold; coating 1mm of ceramic refractory slurry on the outer parts of a part wax mold, a spiral crystal selector wax mold and an alundum tube, dewaxing at the temperature of 200 ℃, and roasting at the temperature of 1300 ℃ for 2 hours to obtain a ceramic mold shell, wherein the ceramic mold shell is provided with a crystal opening section, a crystal selection section and a part section corresponding to the wax mold structure, and the crystal opening section of the mold shell takes the alundum tube as an inner wall;
thirdly, carrying out solid solution treatment on the columnar crystal test block, putting the directionally solidified Ni-13.5Mo-7.6 Al-0.05B high-temperature alloy body into a heat treatment furnace at 1100 ℃ for 10h for heat preservation by adopting a one-step solid solution heat treatment method, and then cooling to obtain a solid solution columnar crystal test block;
fourthly, preparing solid solution columnar crystals, cutting a test block on the directionally solidified high-temperature alloy body along the solidification direction, and grinding the surface of the test block by using 80#, 320#, 600# or 1000# sand paper to obtain the solid solution columnar crystals; the shape of the solid solution columnar crystal is cylindrical; the height of the solid-solution columnar crystal is 50mm, and the diameter of the solid-solution columnar crystal is 4 mm;
fifthly, preparing a single crystal high-temperature alloy casting, and filling solid solution state columnar crystals into a crystal starting section of the ceramic formwork, wherein the gap between the solid solution state columnar crystals and the inner wall of the crystal starting section of the formwork is 0.01 mm; putting the solid-solution columnar crystal and the ceramic mould shell into a single crystal furnace together, adjusting the temperature in the single crystal furnace to 1400 ℃, and preserving the temperature for 5 min; pouring the high-temperature alloy molten metal into a ceramic mould shell, and preserving heat for 10 min; moving the crystal puller downwards at the speed of 0.1 mm/min; and after crystal pulling is finished, cooling the crystal to room temperature along with the furnace, and taking out the crystal to obtain a first monocrystal high-temperature alloy casting, wherein the temperature of the high-temperature alloy molten metal is 1800 ℃.
Sixthly, recycling the repeatedly used columnar crystal, and removing the mould shell of the obtained single crystal high-temperature alloy test rod; disconnecting the obtained first single crystal superalloy casting from a boundary of a crystal selection section and a crystal starting section, and recovering the crystal starting section as reusable columnar crystals;
seventhly, carrying out solid solution treatment on the recovered columnar crystals again, putting the columnar crystals recovered in the sixth step into a heat treatment furnace with the temperature of 1100 ℃ for heat preservation for 10 hours by adopting a one-step solid solution heat treatment method, and then cooling to obtain a solid solution columnar crystal test block; the solid solution columnar crystal test block is the recovered solid solution columnar crystal;
eighthly, grinding the recovered solid solution columnar crystals; grinding the surface of the recovered solid solution columnar crystal by using 80#, 320#, 600# or 1000# sandpaper to obtain reusable columnar crystal;
ninth, preparing other single crystal high temperature alloy castings, and continuously preparing the single crystal high temperature alloy castings by utilizing the reusable solid solution state columnar crystals in the eighth step; plugging the reusable solid solution state columnar crystal into the crystal starting section of the ceramic formwork prepared in the second step, wherein the gap between the reusable solid solution state columnar crystal and the inner wall of the crystal starting section of the formwork is 0.03 mm; putting the solid-solution columnar crystal and the ceramic mould shell into a single crystal furnace together, adjusting the temperature in the single crystal furnace to 1400 ℃, and preserving the temperature for 5 min; pouring the high-temperature alloy molten metal into a ceramic mould shell, and preserving heat for 10 min; moving the crystal puller downwards at the speed of 0.1 mm/min; after crystal pulling is finished, cooling the crystal to room temperature along with the furnace, and taking out the crystal to obtain a second single crystal high-temperature alloy casting; the temperature of the high-temperature alloy molten metal is 1400 ℃;
and repeating the sixth step to the ninth step, continuously recovering reusable solid solution state columnar crystals on the new single crystal high temperature alloy casting, and preparing the rest single crystal high temperature alloy castings by using the reusable solid solution state columnar crystals until the required number of single crystal high temperature alloy castings are obtained.
Example 3:
the preparation method of the Ni-12Mo-7.2 Al-0.02B single crystal high temperature alloy casting comprises the following specific steps:
firstly, preparing a wax mold of a spiral crystal selector, melting wax materials at the temperature of 80 ℃, injecting the melted wax materials into a part mold, and performing compression molding under the pressure of 5MPa to prepare the part wax mold; melting the wax material at the temperature of 80 ℃, injecting the melted wax material into a spiral crystal selector mold, and performing compression molding under the pressure of 5MPa to obtain the spiral crystal selector wax mold; the wax mould of the spiral crystal selector comprises a spiral section and a crystal starting section;
secondly, sleeving a corundum tube with the same length as the crystal starting section of the spiral crystal selector wax mold into the crystal starting section of the spiral crystal selector wax mold, and filling a gap between the corundum tube and the crystal starting section of the spiral crystal selector wax mold with molten wax; welding the part wax mold with one end of the spiral section of the spiral crystal selector wax mold; coating 5mm ceramic refractory slurry on the outer parts of a part wax mold, a spiral crystal selector wax mold and an alundum tube, dewaxing at the temperature of 200 ℃, and roasting at the temperature of 800 ℃ for 3 hours to obtain a ceramic mold shell, wherein the ceramic mold shell is provided with a crystal opening section, a crystal selection section and a part section corresponding to the wax mold structure, and the crystal opening section of the ceramic mold shell takes the alundum tube as an inner wall;
thirdly, carrying out solid solution treatment on the columnar crystal test block, putting the directionally solidified Ni-12Mo-7.2 Al-0.02B high-temperature alloy body into a heat treatment furnace at 1250 ℃ for heat preservation for 6h by adopting a one-step solid solution heat treatment method, and then cooling to obtain a solid solution columnar crystal test block;
fourthly, preparing solid solution columnar crystals, cutting a test block on the directionally solidified high-temperature alloy body along the solidification direction, and grinding the surface of the test block by using 80#, 320#, 600# or 1000# sand paper to obtain the solid solution columnar crystals; the shape of the solid solution columnar crystal is cylindrical; the height of the solid-solution columnar crystal is 30mm, and the diameter of the solid-solution columnar crystal is 10 mm;
fifthly, preparing a single crystal high-temperature alloy casting, and filling solid solution state columnar crystals into a crystal starting section of the ceramic formwork, wherein the gap between the solid solution state columnar crystals and the inner wall of the crystal starting section of the formwork is 0.1 mm; putting the solid-solution columnar crystal and the ceramic mould shell into a single crystal furnace together, adjusting the temperature in the single crystal furnace to 1600 ℃, and preserving the temperature for 15 min; pouring the high-temperature alloy molten metal into a ceramic mould shell, and preserving heat for 1 min; moving the crystal puller downwards at the speed of 9 mm/min; and after crystal pulling is finished, cooling the crystal to room temperature along with the furnace, and taking out the crystal to obtain a first monocrystal high-temperature alloy casting, wherein the temperature of the high-temperature alloy molten metal is 1500 ℃.
Sixthly, recycling the repeatedly used columnar crystal, and removing the mould shell of the obtained single crystal high-temperature alloy test rod; disconnecting the obtained first single crystal superalloy casting from a boundary of a crystal selection section and a crystal starting section, and recovering the crystal starting section as reusable columnar crystals;
seventhly, carrying out solid solution treatment on the recovered columnar crystals again, putting the columnar crystals recovered in the sixth step into a heat treatment furnace with the temperature of 1250 ℃ for heat preservation for 6 hours by adopting a one-step solid solution heat treatment method, and then cooling to obtain a solid solution columnar crystal test block; the solid solution columnar crystal test block is the recovered solid solution columnar crystal;
eighthly, grinding the recovered solid solution columnar crystals; grinding the surface of the recovered solid solution columnar crystal by using 80#, 320#, 600# or 1000# sandpaper to obtain reusable columnar crystal;
ninth, preparing other single crystal high temperature alloy castings, and continuously preparing the single crystal high temperature alloy castings by utilizing the reusable solid solution state columnar crystals in the eighth step; plugging the reusable solid solution state columnar crystal into the crystal starting section of the ceramic formwork prepared in the second step, wherein the gap between the reusable solid solution state columnar crystal and the inner wall of the crystal starting section of the formwork is 0.15 mm; putting the solid-solution columnar crystal and the ceramic mould shell into a single crystal furnace together, adjusting the temperature in the single crystal furnace to 1600 ℃, and preserving the temperature for 30 min; pouring the high-temperature alloy molten metal into a ceramic mould shell, and preserving heat for 20 min; moving the crystal puller downwards at the speed of 9 mm/min; after crystal pulling is finished, cooling the crystal to room temperature along with the furnace, and taking out the crystal to obtain a second single crystal high-temperature alloy casting; the temperature of the high-temperature alloy molten metal is 1500 ℃;
and repeating the sixth step to the ninth step, continuously recovering reusable solid solution state columnar crystals on the new single crystal high temperature alloy casting, and preparing the rest single crystal high temperature alloy castings by using the reusable solid solution state columnar crystals until the required number of single crystal high temperature alloy castings are obtained.
Example 4:
the preparation method of the Ni-3.2Cr-1.2Mo-6Al-10Co-6W-4Re-7.98Ta single crystal high-temperature alloy casting comprises the following specific steps:
firstly, preparing a wax mold of a spiral crystal selector, melting wax materials at the temperature of 60 ℃, injecting the melted wax materials into a part mold, and performing compression molding under the pressure of 5MPa to prepare the part wax mold; melting the wax material at 60 ℃, injecting the melted wax material into a spiral crystal selector mold, and performing compression molding under the pressure of 5MPa to obtain the spiral crystal selector wax mold; the wax mould of the spiral crystal selector comprises a spiral section and a crystal starting section;
secondly, sleeving a corundum tube with the same length as the crystal starting section of the spiral crystal selector wax mold into the crystal starting section of the spiral crystal selector wax mold, and filling a gap between the corundum tube and the crystal starting section of the spiral crystal selector wax mold with molten wax; welding the part wax mold with one end of the spiral section of the spiral crystal selector wax mold; coating 7mm ceramic refractory slurry on the outer parts of a part wax mold, a spiral crystal selector wax mold and an alundum tube, dewaxing at 100 ℃, roasting at 1300 ℃ for 5 hours to obtain a ceramic mold shell, wherein the ceramic mold shell is provided with a crystal opening section, a crystal selection section and a part section corresponding to the wax mold structure, and the crystal opening section of the ceramic mold shell takes the alundum tube as an inner wall;
thirdly, carrying out solid solution treatment on the columnar crystal test block, putting the directionally solidified Ni-3.2Cr-1.2Mo-6Al-10Co-6W-4Re-7.98Ta high-temperature alloy body into a heat treatment furnace at 1350 ℃ for heat preservation for 6h by adopting a one-step solid solution heat treatment method, and then cooling to obtain a solid solution columnar crystal test block;
fourthly, preparing solid solution columnar crystals, cutting a test block on the directionally solidified high-temperature alloy body along the solidification direction, and grinding the surface of the test block by using 80#, 320#, 600# or 1000# sand paper to obtain the solid solution columnar crystals; the shape of the solid solution columnar crystal is cylindrical; the height of the solid-solution columnar crystal is 25m, and the diameter is 7 mm;
fifthly, preparing a single crystal high-temperature alloy casting, and filling solid solution state columnar crystals into a crystal starting section of the ceramic formwork, wherein the gap between the solid solution state columnar crystals and the inner wall of the crystal starting section of the formwork is 0.05 mm; putting the solid-solution columnar crystal and the ceramic mould shell into a single crystal furnace together, adjusting the temperature in the single crystal furnace to 1500 ℃, and preserving the temperature for 3 min; pouring the high-temperature alloy molten metal into a ceramic mould shell, and preserving heat for 5 min; moving the crystal puller downwards at the speed of 7 mm/min; and after crystal pulling is finished, cooling the crystal to room temperature along with the furnace, and taking out the crystal to obtain a first monocrystal high-temperature alloy casting, wherein the temperature of the high-temperature alloy molten metal is 1500 ℃.
Sixthly, recycling the repeatedly used columnar crystal, and removing the mould shell of the obtained single crystal high-temperature alloy test rod; disconnecting the obtained first single crystal superalloy casting from a boundary of a crystal selection section and a crystal starting section, and recovering the crystal starting section as reusable columnar crystals;
seventhly, carrying out solid solution treatment on the recovered columnar crystals again, putting the columnar crystals recovered in the sixth step into a heat treatment furnace with the temperature of 1350 ℃ for heat preservation for 6 hours by adopting a one-step solid solution heat treatment method, and then cooling to obtain a solid solution columnar crystal test block; the solid solution columnar crystal test block is the recovered solid solution columnar crystal;
eighthly, grinding the recovered solid solution columnar crystals; grinding the surface of the recovered solid solution columnar crystal by using 80#, 320#, 600# or 1000# sandpaper to obtain reusable columnar crystal;
ninth, preparing other single crystal high temperature alloy castings, and continuously preparing the single crystal high temperature alloy castings by utilizing the reusable solid solution state columnar crystals in the eighth step; plugging the reusable solid solution state columnar crystal into the crystal starting section of the ceramic formwork prepared in the second step, wherein the gap between the reusable solid solution state columnar crystal and the inner wall of the crystal starting section of the formwork is 0.13 mm; putting the solid-solution columnar crystal and the ceramic mould shell into a single crystal furnace together, adjusting the temperature in the single crystal furnace to 1500 ℃, and preserving the temperature for 3 min; pouring the high-temperature alloy molten metal into a ceramic mould shell, and preserving heat for 5 min; moving the crystal puller downwards at the speed of 7 mm/min; after crystal pulling is finished, cooling the crystal to room temperature along with the furnace, and taking out the crystal to obtain a second single crystal high-temperature alloy casting; the temperature of the high-temperature alloy molten metal is 1500 ℃;
and repeating the sixth step to the ninth step, continuously recovering reusable solid solution state columnar crystals on the new single crystal high temperature alloy casting, and preparing the rest single crystal high temperature alloy castings by using the reusable solid solution state columnar crystals until the required number of single crystal high temperature alloy castings are obtained.
Example 5:
the preparation method of the Ni-3Cr-1Mo-6Al-11.6Co-6.3W-4.4Re-7.95Ta-1Hf single crystal high-temperature alloy casting comprises the following specific steps:
firstly, preparing a wax mold of a spiral crystal selector, melting wax materials at the temperature of 90 ℃, injecting the melted wax materials into a part mold, and performing compression molding under the pressure of 2MPa to prepare the part wax mold; melting the wax material at the temperature of 90 ℃, injecting the melted wax material into a spiral crystal selector mold, and performing compression molding under the pressure of 2MPa to obtain the spiral crystal selector wax mold; the wax mould of the spiral crystal selector comprises a spiral section and a crystal starting section;
secondly, sleeving a corundum tube with the same length as the crystal starting section of the spiral crystal selector wax mold into the crystal starting section of the spiral crystal selector wax mold, and filling a gap between the corundum tube and the crystal starting section of the spiral crystal selector wax mold with molten wax; welding the part wax mold with one end of the spiral section of the spiral crystal selector wax mold; coating 6mm ceramic refractory slurry on the outer parts of a part wax mold, a spiral crystal selector wax mold and a corundum tube, dewaxing at 120 ℃, roasting at 850 ℃ for 4 hours to obtain a ceramic mold shell, wherein the ceramic mold shell is provided with a crystal opening section, a crystal selection section and a part section corresponding to the wax mold structure, and the crystal opening section of the ceramic mold shell takes the corundum tube as an inner wall;
thirdly, carrying out solid solution treatment on the columnar crystal test block, putting the directionally solidified Ni-3Cr-1Mo-6Al-11.6Co-6.3W-4.4Re-7.95Ta-1Hf high-temperature alloy body into a 1400 ℃ heat treatment furnace for heat preservation for 4h by adopting a one-step solid solution heat treatment method, and then cooling to obtain a solid solution columnar crystal test block;
fourthly, preparing solid solution columnar crystals, cutting a test block on the directionally solidified high-temperature alloy body along the solidification direction, and grinding the surface of the test block by using 80#, 320#, 600# or 1000# sand paper to obtain the solid solution columnar crystals; the shape of the solid solution columnar crystal is cylindrical; the height of the solid-solution columnar crystal is 20m, and the diameter of the solid-solution columnar crystal is 8 mm;
fifthly, preparing a single crystal high-temperature alloy casting, and filling solid solution state columnar crystals into a crystal starting section of the ceramic formwork, wherein the gap between the solid solution state columnar crystals and the inner wall of the crystal starting section of the formwork is 0.12 mm; putting the solid-solution columnar crystal and the ceramic mould shell into a single crystal furnace together, adjusting the temperature in the single crystal furnace to 1580 ℃, and preserving the temperature for 4 min; pouring the high-temperature alloy molten metal into a ceramic mould shell, and preserving heat for 4 min; moving the crystal puller downwards at the speed of 6 mm/min; and after crystal pulling is finished, cooling the crystal to room temperature along with the furnace, and taking out the crystal to obtain a first monocrystal superalloy casting, wherein the temperature of the molten superalloy is 1520 ℃.
Sixthly, recycling the repeatedly used columnar crystal, and removing the mould shell of the obtained single crystal high-temperature alloy test rod; disconnecting the obtained first single crystal superalloy casting from a boundary of a crystal selection section and a crystal starting section, and recovering the crystal starting section as reusable columnar crystals;
seventhly, carrying out solid solution treatment on the recovered columnar crystals again, putting the columnar crystals recovered in the sixth step into a heat treatment furnace with the temperature of 1400 ℃ for heat preservation for 4 hours by adopting a one-step solid solution heat treatment method, and then cooling to obtain a solid solution columnar crystal test block; the solid solution columnar crystal test block is the recovered solid solution columnar crystal;
eighthly, grinding the recovered solid solution columnar crystals; grinding the surface of the recovered solid solution columnar crystal by using 80#, 320#, 600# or 1000# sandpaper to obtain reusable columnar crystal;
ninth, preparing other single crystal high temperature alloy castings, and continuously preparing the single crystal high temperature alloy castings by utilizing the reusable solid solution state columnar crystals in the eighth step; plugging the reusable solid solution state columnar crystal into the crystal starting section of the ceramic formwork prepared in the second step, wherein the gap between the reusable solid solution state columnar crystal and the inner wall of the crystal starting section of the formwork is 0.2 mm; putting the solid-solution columnar crystal and the ceramic mould shell into a single crystal furnace together, adjusting the temperature in the single crystal furnace to 1580 ℃, and preserving the temperature for 4 min; pouring the high-temperature alloy molten metal into a ceramic mould shell, and preserving heat for 4 min; moving the crystal puller downwards at the speed of 6 mm/min; after crystal pulling is finished, cooling the crystal to room temperature along with the furnace, and taking out the crystal to obtain a second single crystal high-temperature alloy casting; the temperature of the high-temperature alloy molten metal is 1520 ℃;
and repeating the sixth step to the ninth step, continuously recovering reusable solid solution state columnar crystals on the new single crystal high temperature alloy casting, and preparing the rest single crystal high temperature alloy castings by using the reusable solid solution state columnar crystals until the required number of single crystal high temperature alloy castings are obtained.
The invention aims to prepare the single crystal high-temperature alloy by repeatedly using the solid solution state columnar crystal and combining the crystal selection method, the deviation of the crystal (001) direction from the directional solidification direction can be controlled within 5 ℃, the deviation range of the crystal orientation of the single crystal high-temperature alloy controlled by the crystal selection method can be smaller than that of the single crystal high-temperature alloy controlled by the crystal selection method at present, the single crystal can be prepared by repeatedly using the solid solution state columnar crystal, the success rate of the single crystal preparation is improved, and the control cost of the single crystal orientation is reduced;
the corundum tube with the same length as the crystal starting section of the spiral crystal selector wax mold is sleeved into the crystal starting section of the spiral crystal selector wax mold, and a gap between the corundum tube and the crystal starting section is filled with molten wax, so that the probability of forming mixed crystals by chilling due to the fact that single crystal high-temperature alloy enters a gap between a ceramic mold shell and unmelted single crystals caused by pouring can be effectively avoided; the ceramic refractory slurry is coated outside the part wax mold, the spiral crystal selector wax mold and the corundum tube, so that the refractory performance of the formed ceramic mold shell can be improved.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. A method for manufacturing a single crystal superalloy by repeatedly using solid solution columnar crystals, wherein a <001> direction of the crystals is controlled to be within 5 degrees from a directional solidification direction, the method comprising the steps of:
firstly, preparing a part wax mold and a spiral crystal selector wax mold, melting wax materials, injecting the melted wax materials into the part mold, and performing compression molding to obtain the part wax mold; melting the wax material, injecting the melted wax material into a spiral crystal selector mold, and performing compression molding to obtain a spiral crystal selector wax mold; the wax mould of the spiral crystal selector comprises a spiral section and a crystal starting section;
secondly, sleeving a corundum tube with the same length as the crystal starting section of the spiral crystal selector wax mold into the crystal starting section of the spiral crystal selector wax mold, and filling a gap between the corundum tube and the crystal starting section of the spiral crystal selector wax mold with molten wax; welding the part wax mold with one end of the spiral section of the spiral crystal selector wax mold; coating ceramic refractory slurry on the outer parts of the part wax mould, the spiral crystal selector wax mould and the corundum tube, dewaxing at a certain temperature, and roasting for a certain time to obtain a ceramic mould shell, wherein the ceramic mould shell is provided with a crystal starting section, a crystal selecting section and a part section;
thirdly, carrying out solid solution treatment on the columnar crystal test block, putting the directionally solidified high-temperature alloy body into a heat treatment furnace for heat preservation by adopting a one-step solid solution heat treatment method, and then cooling to obtain a solid solution columnar crystal test block, wherein the temperature of the heat treatment furnace is 1100-1450 ℃, and the heat preservation is carried out for 2-10 h;
fourthly, preparing solid solution columnar crystals, cutting a test block on the directionally solidified high-temperature alloy body along the solidification direction, and grinding the surface of the test block by using a grinding tool to obtain the solid solution columnar crystals, wherein the solid solution columnar crystals are cylindrical; the height of the solid-solution columnar crystal is 20-50 mm, and the diameter of the solid-solution columnar crystal is 4-20 mm;
fifthly, preparing a single crystal high-temperature alloy casting, and filling solid solution columnar crystals into a crystal starting section of the ceramic mould shell; putting the solid-solution columnar crystal and the ceramic mould shell into a single crystal furnace together, adjusting the temperature in the single crystal furnace, and preserving the temperature for a certain time; pouring high-temperature alloy molten metal into a ceramic mould shell, and preserving heat for a certain time; moving the crystal puller downwards; after crystal pulling is finished, cooling the crystal to room temperature along with the furnace, and taking out the crystal to obtain a first monocrystal high-temperature alloy casting;
sixthly, recycling the repeatedly used columnar crystal, and removing the mould shell of the obtained single crystal high-temperature alloy test rod; disconnecting the obtained first single crystal superalloy casting from a boundary of a crystal selection section and a crystal starting section, and recovering the crystal starting section as reusable columnar crystals;
the seventh step, the recovered columnar crystals are subjected to solution treatment again, the columnar crystals recovered in the sixth step are subjected to solution treatment again in the third step, and the treated solid solution columnar crystal test block is the recovered solid solution columnar crystals;
eighthly, grinding the recovered solid solution columnar crystals; grinding the surface of the recovered solid solution columnar crystal by using a grinding tool to obtain a reusable columnar crystal;
ninth, preparing other single crystal high temperature alloy castings, and continuously preparing the single crystal high temperature alloy castings by utilizing the reusable solid solution state columnar crystals in the eighth step; filling the reusable solid solution state columnar crystal into the crystal starting section of the ceramic mould shell prepared in the second step; putting the solid solution columnar crystal and the ceramic mould shell into a single crystal furnace together, adjusting the temperature in the single crystal furnace, preserving heat for a certain time, pouring high-temperature alloy molten metal into the ceramic mould shell, and preserving heat for a certain time; moving the crystal puller downwards; after crystal pulling is finished, cooling the crystal to room temperature along with the furnace, and taking out the crystal to obtain a second single crystal high-temperature alloy casting; in the second step, the ceramic mould shell crystal starting section takes a corundum tube as an inner wall;
in the fifth step, the solid-solution columnar crystal and the ceramic mould shell are placed into a single crystal furnace together, the temperature in the single crystal furnace is adjusted to 1400-1600 ℃, and the temperature is kept for 1-15 min; pouring the high-temperature alloy molten metal into a ceramic mould shell, keeping the temperature for 1-15 min, and moving downwards to pull the crystal; the temperature of the high-temperature alloy molten metal is 1400-1800 ℃, and the gap between the solid-solution columnar crystal and the inner wall of the crystal starting section of the ceramic formwork is 0.01-0.5 mm;
in the fifth step, the speed of downward movement of crystal pulling is 7-9 mm/min;
in the ninth step, the speed of downward movement of crystal pulling is 7-15 mm/min.
2. The method for repeatedly using a solid solution columnar crystal to produce a single crystal superalloy as in claim 1, wherein in the first step, a wax material is melted at a temperature of 60 to 100 ℃, injected into a part mold, and press-molded at a pressure of 0.5 to 8MPa to produce a part wax mold; melting the wax material at the temperature of 60-100 ℃, injecting the melted wax material into a spiral crystal selector mold, and performing compression molding under the pressure of 0.5-8 MPa to obtain the spiral crystal selector wax mold.
3. The method for repeatedly using a solid solution columnar grain single crystal superalloy as in claim 1, wherein in the second step, the ceramic mold shell is obtained by dewaxing at a temperature of 100 to 200 ℃ and baking at a temperature of 800 to 1300 ℃ for 2 to 10 hours, and the ceramic refractory slurry is coated outside the part wax mold, the spiral grain selector wax mold and the corundum tube to a thickness of 1 to 10 mm.
4. The method for producing a single crystal superalloy according to claim 1, wherein the gap between the solid solution columnar crystals and the inner wall of the initial phase of the ceramic mold shell in the ninth step is 0.01 to 0.5 mm.
5. The method of claim 1, wherein the fourth to ninth steps are repeated to continue recovering reusable solid solution columnar crystals from the new single crystal superalloy casting, and using the reusable solid solution columnar crystals to produce the remaining single crystal superalloy castings until a desired number of single crystal superalloy castings are obtained.
6. The method of reusing solid solution columnar crystallized single crystal superalloy as in claim 1, wherein in the fourth step and the eighth step, the grinding tool is 80#, 320#, 600# or 1000# sandpaper.
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