CN114606563B - Method for preparing single crystal superalloy with versatile and reusable seed crystal - Google Patents

Method for preparing single crystal superalloy with versatile and reusable seed crystal Download PDF

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CN114606563B
CN114606563B CN202210211478.3A CN202210211478A CN114606563B CN 114606563 B CN114606563 B CN 114606563B CN 202210211478 A CN202210211478 A CN 202210211478A CN 114606563 B CN114606563 B CN 114606563B
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seed crystal
crystal
section
seed
cooling plate
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CN114606563A (en
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胡松松
刘海淇
贺迟
白伟民
汪璞
杨泽宇
刘宇星
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Xiangtan University
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Xiangtan University
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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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22C—FOUNDRY MOULDING
    • B22C9/00—Moulds or cores; Moulding processes
    • B22C9/22—Moulds for peculiarly-shaped castings
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

A method for preparing single crystal superalloy by seed crystal can be used universally and can recycle seed crystal, which is characterized in that a pre-buried corundum tube is further improved on the basis of seed crystal section, a cooling plate is added to assist the <001> oriented seed crystal to prepare single crystal superalloy, so that the axial direction of the <001> oriented seed crystal and the axial direction of a casting form a certain angle a, and after the liquid master alloy is poured in, the crystal grows along the same crystal phase as the seed crystal, thus obtaining the casting with the <001> direction deviating from the axis a. The conical transition section enables a certain buffer between the seed crystal and the part section, so that the seed crystal and the part section are well connected together, the defect that mixed crystals are solidified at the top end of the seed crystal in the directional solidification process is avoided, the corundum tube and the cooling plate casting are sufficiently distant, the stress of the seed crystal section on the mould shell is ensured, and the corundum tube is prevented from being damaged due to the stress problem. The invention can realize that the single crystal casting with specific orientation is prepared by using the seed crystal with <001> orientation, and realize that the seed crystal is universal and can be reused.

Description

Method for preparing single crystal superalloy with versatile and reusable seed crystal
Technical Field
The invention relates to the field of preparation of single-crystal superalloy, in particular to a method for preparing single-crystal superalloy by embedding a corundum tube and adopting a cooling plate to assist <001> oriented seed crystal.
Background
The nickel-based single crystal superalloy is a preferred material for turbine blades of aircraft engines due to its excellent high temperature mechanical properties. The nickel-base single crystal superalloy can obtain the best comprehensive mechanical property when the <001> direction is consistent with the maximum stress direction of the blade. At present, in the production of single crystal superalloy, a crystal selection method is mostly adopted, the single crystal superalloy prepared by the crystal selection method has a history of forty years, the process is mature, and the cost is low. But the three-dimensional orientation of the single crystal cannot be precisely controlled by the crystal selection method. When the seed crystal method is adopted to prepare the monocrystal superalloy, the precision is high, and the three-dimensional orientation of the monocrystal can be controlled.
The existing seed crystal method for preparing the single crystal superalloy has two obvious defects, namely, single crystal with the same orientation as that of a single crystal superalloy casting is adopted as a seed crystal, and the axial direction and the directional solidification direction of the seed crystal are consistent in the preparation process. Each time a single crystal superalloy casting of different orientations is cast, a seed crystal of the corresponding orientation is prepared, and the seed crystal cannot be used universally. Secondly, when the existing seed crystal method is used for preparing the single crystal superalloy, the seed crystal remelting area often generates mixed crystals, the mixed crystals generated in the seed crystal remelting area cause the difficulty in recycling the seed crystal, new seed crystals are needed to be used each time, and the production cost is high. The invention creation of the application number CN201610389765.8 discloses a method for preparing single crystal superalloy by embedding a corundum tube in a seed crystal section, which can effectively solve the problem of impurity crystal generation in a seed crystal remelting area and solve the problem that seed crystals cannot be reused. But the problem that the seed crystal with corresponding orientation is required to be prepared according to the orientation of the crystal of the single crystal casting when the single crystal superalloy is prepared is still not solved.
Disclosure of Invention
In order to overcome the defects of poor seed crystal universality and high single crystal preparation cost caused by seed crystal orientation in the preparation of single crystal castings in the prior art, the invention provides a method for preparing single crystal superalloy by using the seed crystal which is universal and can be reused.
The specific process of the invention is as follows:
step 1, preparing a seed crystal with <001> orientation:
marking a crystal <001> direction on a nickel-based single crystal superalloy sample by the Laue method, and then directionally cutting a square single crystal, wherein the axis of the square single crystal is parallel to the crystal <001> direction, so as to obtain a seed crystal blank. Grinding and cleaning the surface of the seed crystal blank to obtain seed crystal. The length of the seed crystal is 20 mm-50 mm, and the side length is 3X 3mm.
Step 2, manufacturing a seed crystal section wax mould containing a corundum tube:
when the wax mould is manufactured, the corundum tube is placed in the seed crystal section in the mould, and the top end surface of the corundum tube is 3-6 mm away from the top inner surface of the seed crystal section. And filling the molten wax material into the mould, and cooling and solidifying to obtain the seed crystal section wax mould containing the corundum tube.
The axis of the seed crystal section in the wax mould deviates from the axis of the part section; the direction and angle of the deviations coincide with the <001> direction of the cast crystal. The deviating angle is 5-55 degrees.
The length of the seed crystal section is 40-70 mm, and the side length is 3X 3 mm-15X 15mm. The length of the corundum tube is 30-45 mm.
Step 3, manufacturing a cooling plate
When the cooling plate is manufactured, the steel plate is cut into a circular plate with the thickness of 5 mm-10 mm and the diameter of 50mm, and a cooling plate blank is obtained.
A through seed crystal insertion hole is cut in the center of the cooled slab. The seed crystal insertion hole is a square hole, and the side length of the square hole is 3X 3 mm-15X 15mm. The geometric center line of the seed crystal insertion hole is deviated from the axis of the part section; the direction and angle of deviation are coincident with the <001> direction of the cast crystal so that the entrance and exit of the cooled slab are not in the same vertical plane.
A cooling plate is obtained.
Step 4, manufacturing a mould shell with a seed crystal section containing a corundum tube:
the mould shell comprises a part section, a transition section, a seed crystal section containing corundum tubes and a cooling plate.
Firstly, paraffin wax is adopted to manufacture a part section wax mould, a transition section wax mould, a seed crystal section wax mould containing corundum tubes and a cooling plate wax mould in a segmented mode. And welding the part section wax mould, the seed crystal section wax mould containing the corundum tube and the cooling plate wax mould into a whole in sequence to obtain the whole casting wax mould.
And manufacturing the mould shell containing the corundum tube in the seed crystal section by using the obtained integral casting wax mould and adopting an investment casting process.
In the mould shell with the corundum tube in the seed crystal section: the inner diameter of the part section is 8-40 mm; the circumferential surface of the transition section is a conical surface. Connecting the large end face of the transition section with the lower end face of the part section; and connecting the small end of the transition section with the seed crystal section.
The diameter of the large end face of the transition section is 10-50 mm, the diameter of the small end face is 6-30 mm, and the length of the transition section is 5-10 mm.
Step 5, preparing the single crystal superalloy casting with the required orientation by directional solidification:
inserting the seed crystal of <001> orientation obtained in step 1 into the seed crystal insertion hole of the cooling plate; the insertion depth is 5-10 mm. And placing the cooling plate inserted with the seed crystal into the mould shell from the bottom of the mould shell containing the corundum tube, and completing the mould shell combination of the corundum tube in the seed crystal section.
And placing the combined cooling plate and the mould shell into a directional solidification furnace. Heating the directional solidification furnace to 1480-1550 ℃ to partially melt the seed crystal, and partially melt the seed crystal to generate a pasty area with the length of 7mm; preserving heat for 20-30 min.
And (3) placing the master alloy for preparing the single crystal superalloy casting in a crucible for heating, and melting into a molten state to obtain a master alloy solution.
And pouring the master alloy solution into the mould shell after the heat preservation of the seed crystal pasty area is finished, and keeping the temperature of the directional solidification furnace unchanged. And standing the master alloy solution in the mould shell for 20-30 min, and then drawing downwards at a speed of 3-9 mm/min to obtain the single-crystal superalloy casting with the <001> direction deviating from the axis.
The specific process for preparing a plurality of off-axis single crystal superalloy castings in the <001> direction is as follows:
i, recycling reusable seed crystals, and cutting the obtained single-crystal superalloy casting with the <001> direction deviating from the axis at the joint of the seed crystal section and the transition section; and taking the obtained seed crystal section as a reusable seed crystal blank, specifically, cutting off the bottom end of the obtained seed crystal blank by using linear cutting to 7mm, and ensuring that a newly generated pasty area cannot overlap with a pasty area generated by the last seed crystal use when the seed crystal is reused. Grinding and cleaning the surface of the cut seed crystal blank to obtain recovered seed crystals. The length of the recovered seed crystal is 20 mm-50 mm, and the side length of the seed crystal is 3X 3 mm-15X 15mm.
II preparing a second single crystal superalloy casting having a <001> orientation that is 5 degrees off axis. Specifically, the seed crystal is inserted into the cooling plate 5. And (5) repeating the step (5) to obtain a second single-crystal superalloy casting with the <001> direction being deviated from the axis by 5-55 degrees.
And III, repeating the process of recycling the reusable seed crystal and the process of preparing the second single-crystal superalloy casting, and sequentially completing the preparation of the rest single-crystal superalloy castings.
Step 6, preparing a plurality of single crystal superalloy castings with <001> directions deviating from the axes:
in preparing a plurality of <001> off-axis single crystal superalloy castings, reusable seed crystals are first recovered according to a set number of prepared single crystal superalloy castings, and the number of recovered seed crystals is one less than the set number of prepared single crystal superalloy castings.
A plurality of off-axis <001> orientation single crystal superalloy castings are prepared using the recovered seed crystals.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, a certain angle a is formed between the axial direction of the <001> oriented seed crystal and the axial direction of the casting, and after the liquid master alloy is poured, the crystal growth can grow along the same crystal phase as the seed crystal, so that the casting with the <001> direction deviating from the axis a can be obtained. The seed crystal is obliquely placed, and the seed crystal cannot be cooled by adopting a traditional cooling plate, so that the seed crystal is failed to melt and prepare, the mould shell is unevenly stressed due to the oblique placement of the seed crystal, and the cooling plate is used for cooling the seed crystal and supporting the mould shell in an auxiliary way, so that the bottom end of the seed crystal is ensured to keep solid phase and the integrity of the mould shell in the single crystal preparation process. Because the seed crystal section is not all contacted with the part section, the transition section is in a round table structure, so that a certain buffer exists between the seed crystal and the part section, the seed crystal and the part section can be better connected together, and the defect of mixed crystal solidification at the top end of the seed crystal in the directional solidification process is avoided. The invention can realize the preparation of single crystal castings with specific orientation by using the <001> orientation seed crystal. Meanwhile, the method of embedding the corundum tube in the seed crystal section is combined, so that the surface roughness of the inner wall of the seed crystal section of the mould shell can be effectively reduced, and the scouring speed of the seed crystal during alloy casting is reduced, thereby avoiding the formation of mixed crystals in a melting zone and enabling the seed crystal to be reused. When the corundum tube is arranged, the top of the corundum tube is 3-6 mm away from the top of the seed crystal section, so that a certain distance is ensured between the top of the corundum tube and the bottom of the transition section, and the molten casting material can stably enter the seed crystal section from the transition section, and the generation of mixed crystals is avoided. The corundum tube is arranged at the bottom of the corundum tube and is 3-6 mm away from the cooling plate, and the corundum tube is sufficiently spaced away from the cooling plate, so that the stress of the seed crystal section on the mould shell is ensured, and the corundum tube is prevented from being damaged due to the stress problem.
The invention further improves the embedded corundum tube on the basis of the seed crystal section, and adds the cooling plate to assist the <001> oriented seed crystal to prepare the single crystal superalloy. The single crystal superalloy castings produced by the present invention are shown in fig. 6 and 7, and the single crystal superalloy castings produced by the repeated use of the seed crystal are shown in fig. 8. The seed crystal remelting area does not generate miscellaneous crystals, which indicates that the invention can prepare single crystal superalloy castings with specific orientation by using <001> orientation seed crystals, and realize that the seed crystals can be used universally and can be reused for preparing single crystal superalloy castings.
Drawings
FIG. 1 is a schematic diagram of the structure of a casting wax pattern.
Fig. 2 is a schematic structural view of the transition section.
Fig. 3 is a schematic view of the structure of the seed stage + corundum tube.
Fig. 4 is a schematic structural view of the cooling plate.
FIG. 5 is a schematic illustration of a formwork arrangement of the present invention.
FIG. 6 is a schematic diagram of a cross-sectional structure of a single crystal sample prepared using the present method
FIG. 7 is a schematic diagram of the melting point region composition of a single crystal sample prepared using the present method.
FIG. 8 is a schematic diagram of a single crystal sample reflow block prepared using a reusable seed crystal.
Fig. 9 is a flow chart of the present invention.
In the figure: 1. a part section; 2. a transition section; 3. a corundum tube; 4. a seed section; 5. a cooling plate; 6. a conical surface; 7. deviation angle; 8. a seed crystal insertion hole; 9. and (5) seed crystal.
Detailed Description
Example 1
The single crystal superalloy with <001> direction deviating from the axial direction of the part section by 5 degrees is prepared by adopting the method for preparing the single crystal superalloy, wherein the seed crystal can be used universally and can be reused. In this example, two single crystal superalloy castings were prepared.
The specific steps of this embodiment are as follows:
step 1, preparing a seed crystal with <001> orientation.
Marking a crystal <001> direction on a nickel-based single crystal superalloy sample by the Laue method, and then directionally cutting a square single crystal, wherein the axis of the square single crystal is parallel to the crystal <001> direction, so as to obtain a seed crystal blank. Grinding and cleaning the surface of the seed crystal blank to obtain a seed crystal 9 with <001> orientation; the length of the seed crystal is 20 mm-50 mm, and the side length is 3X 3mm; the grinding and cleaning steps comprise the following steps: sequentially polishing with 80# sand paper, 240# sand paper, 400# sand paper, 600# sand paper and 800# sand paper, and cleaning with alcohol; the purity of the alcohol is more than 95%.
Step 2, manufacturing a seed crystal section wax mould containing corundum tube
The axis of the seed crystal section in the wax mould deviates from the axis of the part section; the direction and angle of the deviations coincide with the <001> direction of the cast crystal. In this embodiment, the offset angle 7 is 5 degrees.
When the wax mould is manufactured, the corundum tube 3 is placed in the seed crystal section 4 in the mould, and the top end surface of the corundum tube 3 is arranged to be 3mm away from the top inner surface of the seed crystal section 4. Filling the molten wax material into the mould, and cooling and solidifying to obtain the seed crystal section wax mould containing the corundum tube. The length of the seed crystal section 4 is 40mm, and the section size is 3×3mm. The length of the corundum tube 3 is 34mm.
Step 3, manufacturing a cooling plate
The cooling plate 5 is round, the thickness of the cooling plate is 5 mm-10 mm, and the diameter of the cooling plate is 50mm.
When the cooling plate is manufactured, the steel plate is cut into a circular plate with the thickness of 5 mm-10 mm and the diameter of 50mm, and a cooling plate blank is obtained.
A through seed crystal insertion hole 8 is cut in the center of the cooled slab. The seed insertion hole 8 is a square hole having a side length of 3×3mm. The geometric center line of the seed crystal insertion hole 8 is deviated from the axis of the part section; the direction and angle of deviation are coincident with the <001> direction of the cast crystal so that the entrance and exit of the cooled slab are not in the same vertical plane.
A cooling plate 5 is obtained.
And 4, manufacturing a mould shell with a corundum tube in the seed crystal section.
The mould shell comprises a part section 1, a transition section 2, a seed crystal section 4 containing a corundum tube 3 and a cooling plate 5.
Firstly, paraffin wax is adopted for manufacturing a wax mould in a segmented way: the wax mould comprises a part section wax mould, a transition section wax mould, a seed crystal section wax mould containing a corundum tube and a cooling plate wax mould. And welding the part section wax mould, the seed crystal section wax mould containing the corundum tube and the cooling plate wax mould into a whole in sequence. And trimming each welding part to make the surface of each welding part smooth, and obtaining the integral casting wax mould.
And manufacturing the mould shell with the corundum tube in the seed crystal section by using the obtained integral casting wax mould and adopting an investment casting process.
The specific dimensions of the part section 1 and the transition section 2 are as follows:
the part section is cylindrical, and the inner diameter is 10mm.
The circumferential surface of the transition section 2 is a conical surface. And connecting the large end face of the transition section with the lower end face of the part section. The diameter of the large end face of the transition section is the same as that of the part section; the small end of the transition section is connected with the seed crystal section 4.
In the mould shell with the corundum tube in the seed crystal section: the inner diameter of the part section is 10mm; the circumferential surface of the transition section is a conical surface 6. Connecting the large end face of the transition section with the lower end face of the part; and connecting the small end of the transition section with the seed crystal section.
In the embodiment, the diameter of the large end face of the transition section is 10mm, the diameter of the small end face is 6mm, and the truncated cone-shaped height of the transition section is 5mm.
And 5, directionally solidifying to prepare the single crystal superalloy casting with the required orientation.
Inserting the <001> oriented seed crystal 9 obtained in step 1 into the seed crystal insertion hole 8 of the cooling plate; the insertion depth was 5mm. And then placing the cooling plate inserted with the seed crystal into the mould shell from the bottom of the mould shell containing the corundum tube, so as to complete the mould shell combination of the corundum tube and the seed crystal section.
And placing the combined cooling plate and the mould shell into a directional solidification furnace. Heating the directional solidification furnace to 1480 ℃ according to a conventional method to partially melt the seed crystal, and partially melt the seed crystal to generate a pasty area with the length of 7mm; preserving the heat for 20min.
And (3) placing the master alloy for preparing the single crystal superalloy casting in a crucible for heating, and melting into a molten state to obtain a master alloy solution.
And pouring the master alloy solution into the mould shell after the heat preservation of the seed crystal pasty area is finished, and keeping the temperature of the directional solidification furnace unchanged. After the molten master alloy is placed in the mould shell for 20min, the molten master alloy is pulled downwards at a speed of 3mm/min, and the single-crystal superalloy casting with the <001> direction deviating from the axis is prepared. In this example, the <001> direction of the single crystal superalloy casting is 5 degrees off axis.
Step 6, preparing a plurality of single crystal superalloy castings with <001> directions deviating from the axes:
in preparing a plurality of <001> off-axis single crystal superalloy castings, reusable seed crystals are first recovered according to a set number of prepared single crystal superalloy castings, and the number of recovered seed crystals is one less than the set number of prepared single crystal superalloy castings. In this example, 2 single crystal superalloy castings were prepared, so 1 seed crystal was recovered.
A plurality of off-axis <001> orientation single crystal superalloy castings are prepared using the recovered seed crystals.
The specific process for preparing a plurality of off-axis single crystal superalloy castings in the <001> direction is as follows:
i, recycling reusable seed crystals, and cutting the obtained single-crystal superalloy casting with the <001> direction deviating from the axis at the joint of the seed crystal section and the transition section; and taking the obtained seed crystal section as a reusable seed crystal blank, specifically, cutting off the bottom end of the obtained seed crystal blank by using linear cutting to 7mm, and ensuring that a newly generated pasty area cannot overlap with a pasty area generated by the last seed crystal use when the seed crystal is reused. Grinding and cleaning the surface of the cut seed crystal blank to obtain seed crystals. The length of the seed crystal is 20mm, and the side length of the seed crystal is 3X 3mm.
II preparing a second single crystal superalloy casting having a <001> orientation that is 5 degrees off axis. Specifically, the seed crystal is inserted into the cooling plate 5. Repeating the step 5 to obtain a second single crystal superalloy casting with the <001> direction being offset from the axis by 5 degrees.
Thus, a second single crystal superalloy casting is produced using the recovered seed crystal.
And repeating the process of recycling the reusable seed crystal and the process of preparing the second single-crystal superalloy casting, and sequentially completing the preparation of the rest single-crystal superalloy castings. A plurality of off-axis single crystal superalloy castings are obtained.
Example 2
The single crystal superalloy with <001> direction deviating from the axial direction of the part section by adopting the method for preparing the single crystal superalloy, which can be used universally and can recycle the seed crystal, is prepared. In this example, two single crystal superalloy castings were prepared.
The specific steps of this embodiment are as follows:
step 1, preparing a seed crystal with <001> orientation.
Marking a crystal <001> direction on a nickel-based single crystal superalloy sample by the Laue method, and then directionally cutting a square single crystal, wherein the axis of the square single crystal is parallel to the crystal <001> direction, so as to obtain a seed crystal blank. Grinding and cleaning the surface of the seed crystal blank to obtain a seed crystal 9 with <001> orientation; the length of the seed crystal is 25mm, and the side length is 4 multiplied by 4mm; the grinding and cleaning steps comprise the following steps: sequentially polishing with 80# sand paper, 240# sand paper, 400# sand paper, 600# sand paper and 800# sand paper, and cleaning with alcohol; the purity of the alcohol is more than 95%.
Step 2, manufacturing a seed crystal section wax mould containing corundum tube
The axis of the seed crystal section in the wax mould deviates from the axis of the part section; the direction and angle of the deviations coincide with the <001> direction of the cast crystal. In this embodiment, the offset angle of the seed crystal section wax pattern is 15 degrees.
When the wax mould is manufactured, the corundum tube 3 is placed in the seed crystal section 4 in the mould, and the top end surface of the corundum tube 3 is arranged to be 3mm away from the top inner surface of the seed crystal section 4. Filling the molten wax material into the mould, and cooling and solidifying to obtain the seed crystal section wax mould containing the corundum tube. The length of the seed crystal section 4 is 45mm, and the section size is 4×4mm. The length of the corundum tube 3 is 37mm.
Step 3, manufacturing a cooling plate
The cooling plate 5 is circular, has a thickness of 5mm and a diameter of 50mm.
When the cooling plate is manufactured, the steel plate is cut into a circular plate with the thickness of 5mm and the diameter of 50mm, and a cooling plate blank is obtained.
A through seed crystal insertion hole 8 is cut in the center of the cooled slab. The seed insertion hole 8 is a square hole having a side length of 4X 4mm. The geometric center line of the seed crystal insertion hole 8 is deviated from the axis of the part section; the direction and angle of deviation are coincident with the <001> direction of the cast crystal so that the entrance and exit of the cooled slab are not in the same vertical plane.
A cooling plate 5 is obtained.
And 4, manufacturing a mould shell with a corundum tube in the seed crystal section.
The mould shell comprises a part section 1, a transition section 2, a seed crystal section 4 containing a corundum tube 3 and a cooling plate 5.
Firstly, paraffin wax is adopted for manufacturing a wax mould in a segmented way: the wax mould comprises a part section wax mould, a transition section wax mould, a seed crystal section wax mould containing a corundum tube and a cooling plate wax mould. And welding the part section wax mould, the seed crystal section wax mould containing the corundum tube and the cooling plate wax mould into a whole in sequence. And trimming each welding part to make the surface of each welding part smooth, and obtaining the integral casting wax mould.
And manufacturing the mould shell with the corundum tube in the seed crystal section by using the obtained integral casting wax mould and adopting an investment casting process.
In the mould shell with the corundum tube in the seed crystal section: the inner diameter of the part section is 15mm; the circumferential surface of the transition section is a conical surface 6. Connecting the large end face of the transition section with the lower end face of the part; and connecting the small end of the transition section with the seed crystal section.
The diameter of the big end face of the transition section is 15mm, the diameter of the small end face is 10mm, and the length of the transition section is 5mm.
And 5, directionally solidifying to prepare the single crystal superalloy casting with the required orientation.
Inserting the <001> oriented seed crystal 9 obtained in step 1 into the seed crystal insertion hole 8 of the cooling plate; the insertion depth was 5mm. And then placing the cooling plate inserted with the seed crystal into the mould shell from the bottom of the mould shell containing the corundum tube, so as to complete the mould shell combination of the corundum tube and the seed crystal section.
And placing the combined cooling plate and the mould shell into a directional solidification furnace. Heating the directional solidification furnace to 1500 ℃ according to a conventional method, and partially melting the seed crystal to generate a pasty area with the length of 7mm; preserving the heat for 20min.
And (3) placing the master alloy for preparing the single crystal superalloy casting in a crucible for heating, and melting into a molten state to obtain a master alloy solution.
And pouring the master alloy solution into the mould shell after the heat preservation of the seed crystal pasty area is finished, and keeping the temperature of the directional solidification furnace unchanged. After the molten master alloy is placed in the mould shell for 20min, the molten master alloy is pulled downwards at a speed of 3mm/min, and the single-crystal superalloy casting with the <001> direction deviating from the axis is prepared. In this example, the <001> direction of the single crystal superalloy casting is 15 degrees off axis.
Step 6, preparing a plurality of single crystal superalloy castings with <001> directions deviating from the axes:
in preparing a plurality of <001> off-axis single crystal superalloy castings, reusable seed crystals are first recovered according to a set number of prepared single crystal superalloy castings, and the number of recovered seed crystals is one less than the set number of prepared single crystal superalloy castings. In this example, 4 single crystal superalloy castings were prepared, so that 3 seed crystals were recovered.
A plurality of off-axis <001> orientation single crystal superalloy castings are prepared using the recovered seed crystals.
The specific process for preparing a plurality of off-axis single crystal superalloy castings in the <001> direction is as follows:
i, recycling reusable seed crystals, and cutting the obtained single-crystal superalloy casting with the <001> direction deviating from the axis at the joint of the seed crystal section and the transition section; and taking the obtained seed crystal section as a reusable seed crystal blank, specifically, cutting off the bottom end of the obtained seed crystal blank by using linear cutting to 7mm, and ensuring that a newly generated pasty area cannot overlap with a pasty area generated by the last seed crystal use when the seed crystal is reused. Grinding and cleaning the surface of the cut seed crystal blank to obtain seed crystals. The length of the seed crystal is 25mm, and the side length of the seed crystal is 4×4mm.
II preparing a second single crystal superalloy casting having a <001> orientation offset from the axis by 15 degrees. Specifically, the seed crystal is inserted into the cooling plate 5. Repeating the step 5 to obtain a second single crystal superalloy casting with the <001> direction being 15 degrees deviated from the axis.
Thus, a second single crystal superalloy casting is produced using the recovered seed crystal.
And repeating the process of recycling the reusable seed crystal and the process of preparing the second single-crystal superalloy casting, and sequentially completing the preparation of the rest single-crystal superalloy castings. A plurality of off-axis single crystal superalloy castings are obtained.
Example 3
The single crystal superalloy with the <001> direction deviating from the axial direction of the part section by 35 degrees is prepared by adopting the method for preparing the single crystal superalloy, wherein the seed crystal can be used universally and can be reused. In this example, two single crystal superalloy castings were prepared.
The specific steps of this embodiment are as follows:
step 1, preparing a seed crystal with <001> orientation.
Marking a crystal <001> direction on a nickel-based single crystal superalloy sample by the Laue method, and then directionally cutting a square single crystal, wherein the axis of the square single crystal is parallel to the crystal <001> direction, so as to obtain a seed crystal blank. Grinding and cleaning the surface of the seed crystal blank to obtain a seed crystal 9 with <001> orientation; the length of the seed crystal is 30mm, and the side length is 5X 5mm; the grinding and cleaning steps comprise the following steps: sequentially polishing with 80# sand paper, 240# sand paper, 400# sand paper, 600# sand paper and 800# sand paper, and cleaning with alcohol; the purity of the alcohol is more than 95%.
Step 2, manufacturing a seed crystal section wax mould containing corundum tube
The axis of the seed crystal section in the wax mould deviates from the axis of the part section; the direction and angle of the deviations coincide with the <001> direction of the cast crystal. In this embodiment, the offset angle 7 is 35 degrees.
When the wax mould is manufactured, the corundum tube 3 is placed in the seed crystal section 4 in the mould, and the top end surface of the corundum tube 3 is arranged to be 5mm away from the top inner surface of the seed crystal section 4. Filling the molten wax material into the mould, and cooling and solidifying to obtain the seed crystal section wax mould containing the corundum tube. The length of the seed crystal section 4 is 50mm, and the section size is 5×5mm. The length of the corundum tube 3 is 40mm.
Step 3, manufacturing a cooling plate
The cooling plate 5 is circular, has a thickness of 5mm and a diameter of 50mm.
When the cooling plate is manufactured, the steel plate is cut into a circular plate with the thickness of 5mm and the diameter of 50mm, and a cooling plate blank is obtained.
A through seed crystal insertion hole 8 is cut in the center of the cooled slab. The seed insertion hole 8 is a square hole having a side length of 5X 5mm. The geometric center line of the seed crystal insertion hole 8 is deviated from the axis of the part section; the direction and angle of deviation are coincident with the <001> direction of the cast crystal so that the entrance and exit of the cooled slab are not in the same vertical plane.
A cooling plate 5 is obtained.
And 4, manufacturing a mould shell with a corundum tube in the seed crystal section.
The mould shell comprises a part section 1, a transition section 2, a seed crystal section 4 containing a corundum tube 3 and a cooling plate 5.
Firstly, paraffin wax is adopted for manufacturing a wax mould in a segmented way: the wax mould comprises a part section wax mould, a transition section wax mould, a seed crystal section wax mould containing a corundum tube and a cooling plate wax mould. And welding the part section wax mould, the seed crystal section wax mould containing the corundum tube and the cooling plate wax mould into a whole in sequence. And trimming each welding part to make the surface of each welding part smooth, and obtaining the integral casting wax mould.
And manufacturing the mould shell with the corundum tube in the seed crystal section by using the obtained integral casting wax mould and adopting an investment casting process.
In the mould shell with the corundum tube in the seed crystal section: the inner diameter of the part section is 17mm; the circumferential surface of the transition section is a conical surface 6. Connecting the large end face of the transition section with the lower end face of the part; and connecting the small end of the transition section with the seed crystal section.
The diameter of the big end face of the transition section is 17mm, the diameter of the small end face is 10mm, and the length of the transition section is 5mm.
And 5, directionally solidifying to prepare the single crystal superalloy casting with the required orientation.
Inserting the <001> oriented seed crystal 9 obtained in step 1 into the seed crystal insertion hole 8 of the cooling plate; the insertion depth was 6mm. And then placing the cooling plate inserted with the seed crystal into the mould shell from the bottom of the mould shell containing the corundum tube, so as to complete the mould shell combination of the corundum tube and the seed crystal section.
And placing the combined cooling plate and the mould shell into a directional solidification furnace. Heating the directional solidification furnace to 1520 ℃ according to a conventional method, and partially melting the seed crystal to generate a pasty region with the length of 7mm; preserving the heat for 20min.
And (3) placing the master alloy for preparing the single crystal superalloy casting in a crucible for heating, and melting into a molten state to obtain a master alloy solution.
And pouring the master alloy solution into the mould shell after the heat preservation of the seed crystal pasty area is finished, and keeping the temperature of the directional solidification furnace unchanged. After the molten master alloy is placed in the mould shell for 20min, the molten master alloy is pulled downwards at a speed of 3mm/min, and the single-crystal superalloy casting with the <001> direction deviating from the axis is prepared. In this example, the <001> direction of the single crystal superalloy casting is 35 degrees off axis.
Step 6, preparing a plurality of single crystal superalloy castings with <001> directions deviating from the axes:
in preparing a plurality of <001> off-axis single crystal superalloy castings, reusable seed crystals are first recovered according to a set number of prepared single crystal superalloy castings, and the number of recovered seed crystals is one less than the set number of prepared single crystal superalloy castings. In this example, 8 single crystal superalloy castings were prepared, so 7 seed crystals were recovered.
A plurality of off-axis <001> orientation single crystal superalloy castings are prepared using the recovered seed crystals.
The specific process for preparing a plurality of off-axis single crystal superalloy castings in the <001> direction is as follows:
i, recycling reusable seed crystals, and cutting the obtained single-crystal superalloy casting with the <001> direction deviating from the axis at the joint of the seed crystal section and the transition section; and taking the obtained seed crystal section as a reusable seed crystal blank, specifically, cutting off the bottom end of the obtained seed crystal blank by using linear cutting to 7mm, and ensuring that a newly generated pasty area cannot overlap with a pasty area generated by the last seed crystal use when the seed crystal is reused. Grinding and cleaning the surface of the cut seed crystal blank to obtain seed crystals. The length of the seed crystal is 35mm, and the side length of the seed crystal is 5×5mm.
II preparing a second single crystal superalloy casting having a <001> orientation that is 35 degrees off axis. Specifically, the seed crystal is inserted into the cooling plate 5. Repeating the step 5 to obtain a second single crystal superalloy casting with the <001> direction being deviated from the axis by 35 degrees.
Thus, a second single crystal superalloy casting is produced using the recovered seed crystal.
And repeating the process of recycling the reusable seed crystal and the process of preparing the second single-crystal superalloy casting, and sequentially completing the preparation of the rest single-crystal superalloy castings. A plurality of off-axis single crystal superalloy castings are obtained.
Example 4
The single crystal superalloy with <001> direction deviating from the axial direction of the part section is prepared by adopting the method for preparing the single crystal superalloy, wherein the seed crystal can be used universally and can be reused. In this example, two single crystal superalloy castings were prepared.
The specific steps of this embodiment are as follows:
step 1, preparing a seed crystal with <001> orientation.
Marking a crystal <001> direction on a nickel-based single crystal superalloy sample by the Laue method, and then directionally cutting a square single crystal, wherein the axis of the square single crystal is parallel to the crystal <001> direction, so as to obtain a seed crystal blank. Grinding and cleaning the surface of the seed crystal blank to obtain a seed crystal 9 with <001> orientation; the length of the seed crystal is 35mm, and the side length is 6X 6mm; the grinding and cleaning steps comprise the following steps: sequentially polishing with 80# sand paper, 240# sand paper, 400# sand paper, 600# sand paper and 800# sand paper, and cleaning with alcohol; the purity of the alcohol is more than 95%.
Step 2, manufacturing a seed crystal section wax mould containing corundum tube
The axis of the seed crystal section in the wax mould deviates from the axis of the part section; the direction and angle of the deviations coincide with the <001> direction of the cast crystal. In this embodiment, the offset angle 7 is 45 degrees.
When the wax mould is manufactured, the corundum tube 3 is placed in the seed crystal section 4 in the mould, and the top end surface of the corundum tube 3 is arranged to be 3mm away from the top inner surface of the seed crystal section 4. Filling the molten wax material into the mould, and cooling and solidifying to obtain the seed crystal section wax mould containing the corundum tube. The length of the seed crystal section 4 is 60mm, and the section size is 6×6mm. The length of the corundum tube 3 is 48mm.
Step 3, manufacturing a cooling plate
The cooling plate 5 is circular, has a thickness of 5mm and a diameter of 50mm.
When the cooling plate is manufactured, the steel plate is cut into a circular plate with the thickness of 5mm and the diameter of 50mm, and a cooling plate blank is obtained.
A through seed crystal insertion hole 8 is cut in the center of the cooled slab. The seed insertion hole 8 is a square hole having a side length of 6X 6mm. The geometric center line of the seed crystal insertion hole 8 is deviated from the axis of the part section; the direction and angle of deviation are coincident with the <001> direction of the cast crystal so that the entrance and exit of the cooled slab are not in the same vertical plane.
A cooling plate 5 is obtained.
And 4, manufacturing a mould shell with a corundum tube in the seed crystal section.
The mould shell comprises a part section 1, a transition section 2, a seed crystal section 4 containing a corundum tube 3 and a cooling plate 5.
Firstly, paraffin wax is adopted for manufacturing a wax mould in a segmented way: the wax mould comprises a part section wax mould, a transition section wax mould, a seed crystal section wax mould containing a corundum tube and a cooling plate wax mould. And welding the part section wax mould, the seed crystal section wax mould containing the corundum tube and the cooling plate wax mould into a whole in sequence. And trimming each welding part to make the surface of each welding part smooth, and obtaining the integral casting wax mould.
And manufacturing the mould shell with the corundum tube in the seed crystal section by using the obtained integral casting wax mould and adopting an investment casting process.
In the mould shell with the corundum tube in the seed crystal section: the inner diameter of the part section is 20mm; the circumferential surface of the transition section is a conical surface 6. Connecting the large end face of the transition section with the lower end face of the part; and connecting the small end of the transition section with the seed crystal section.
The diameter of the big end face of the transition section is 20mm, the diameter of the small end face is 10mm, and the length of the transition section is 5mm.
And 5, directionally solidifying to prepare the single crystal superalloy casting with the required orientation.
Inserting the <001> oriented seed crystal 9 obtained in step 1 into the seed crystal insertion hole 8 of the cooling plate; the insertion depth was 7mm. And then placing the cooling plate inserted with the seed crystal into the mould shell from the bottom of the mould shell containing the corundum tube, so as to complete the mould shell combination of the corundum tube and the seed crystal section.
And placing the combined cooling plate and the mould shell into a directional solidification furnace. Heating the directional solidification furnace to 1550 ℃ according to a conventional method, and partially melting the seed crystal to generate a pasty area with the length of 7mm; preserving the heat for 20min.
And (3) placing the master alloy for preparing the single crystal superalloy casting in a crucible for heating, and melting into a molten state to obtain a master alloy solution.
And pouring the master alloy solution into the mould shell after the seed crystal pasty region is insulated, and keeping the temperature of the directional solidification furnace unchanged. After the molten master alloy is placed in the mould shell for 20min, the molten master alloy is pulled downwards at a speed of 1mm/min, and the single-crystal superalloy casting with the <001> direction deviating from the axis is prepared. In this example, the <001> direction of the single crystal superalloy casting is 45 degrees off axis.
Step 6, preparing a plurality of single crystal superalloy castings with <001> directions deviating from the axes:
in preparing a plurality of <001> off-axis single crystal superalloy castings, reusable seed crystals are first recovered according to a set number of prepared single crystal superalloy castings, and the number of recovered seed crystals is one less than the set number of prepared single crystal superalloy castings. In this example, 16 single crystal superalloy castings were prepared, so 15 seed crystals were recovered.
A plurality of off-axis <001> orientation single crystal superalloy castings are prepared using the recovered seed crystals.
The specific process for preparing a plurality of off-axis single crystal superalloy castings in the <001> direction is as follows:
i, recycling reusable seed crystals, and cutting the obtained single-crystal superalloy casting with the <001> direction deviating from the axis at the joint of the seed crystal section and the transition section; and taking the obtained seed crystal section as a reusable seed crystal blank, specifically, cutting off the bottom end of the obtained seed crystal blank by using linear cutting to 7mm, and ensuring that a newly generated pasty area cannot overlap with a pasty area generated by the last seed crystal use when the seed crystal is reused. Grinding and cleaning the surface of the cut seed crystal blank to obtain seed crystals. The length of the seed crystal is 35mm, and the side length of the seed crystal is 6X 6mm.
II preparing a second single crystal superalloy casting having a <001> orientation that is 45 degrees off axis. Specifically, the seed crystal is inserted into the cooling plate 5. Repeating the step 5 to obtain a second single crystal superalloy casting with the <001> direction being offset from the axis by 45 degrees.
Thus, a second single crystal superalloy casting is produced using the recovered seed crystal.
And repeating the process of recycling the reusable seed crystal and the process of preparing the second single-crystal superalloy casting, and sequentially completing the preparation of the rest single-crystal superalloy castings. A plurality of off-axis single crystal superalloy castings are obtained.

Claims (5)

1. A method for preparing single crystal superalloy with versatile and reusable seed crystal is characterized in that the specific process is:
step 1, preparing a seed crystal with <001> orientation:
marking a crystal <001> direction on a nickel-based single crystal superalloy sample by a Laue method, and then directionally cutting a square single crystal, wherein the axis of the square single crystal is parallel to the crystal <001> direction, so as to obtain a seed crystal blank; grinding and cleaning the surface of the seed crystal blank to obtain seed crystals;
step 2, manufacturing a seed crystal section wax mould containing a corundum tube:
when the wax mould is manufactured, the corundum tube is placed in a seed crystal section in the mould, and the top end surface of the corundum tube is 3-6 mm away from the top inner surface of the seed crystal section; filling the molten wax material into a mould, and cooling and solidifying to obtain a seed crystal section wax mould containing a corundum tube;
the axis of the seed crystal section in the wax mould deviates from the axis of the part section; the direction and angle of the deviation are consistent with the <001> direction of the casting crystal; the deviation angle is 5-55 degrees;
step 3, manufacturing a cooling plate:
when the cooling plate is manufactured, the steel plate is cut into a circular plate with the thickness of 5 mm-10 mm and the diameter of 50mm, and a cooling plate blank is obtained;
cutting a through seed crystal insertion hole in the center of the cooling plate blank; the seed crystal inserting hole is a square hole, and the side length of the square hole is 3X 3 mm-15X 15mm; the geometric center line of the seed crystal insertion hole is deviated from the axis of the part section; the direction and angle of the deviation are consistent with the <001> direction of the casting crystal, so that the inlet and the outlet of the cooling plate blank are not on the same vertical plane;
obtaining a cooling plate;
step 4, manufacturing a mould shell with a seed crystal section containing a corundum tube:
the mould shell comprises a part section, a transition section, a seed crystal section containing corundum tubes and a cooling plate;
firstly, manufacturing a part section wax mould, a transition section wax mould, a seed crystal section wax mould containing a corundum tube and a cooling plate wax mould by adopting paraffin sections; sequentially welding the part section wax pattern, the seed crystal section wax pattern containing the corundum tube and the cooling plate wax pattern into a whole to obtain a whole casting wax pattern;
manufacturing a mould shell with a seed crystal section containing a corundum tube by using the obtained integral casting wax mould and adopting an investment casting process;
step 5, preparing the single crystal superalloy casting with the required orientation by directional solidification:
inserting the seed crystal of <001> orientation obtained in step 1 into the seed crystal insertion hole of the cooling plate; the insertion depth is 5-10 mm; placing a cooling plate inserted with seed crystals into the mould shell from the bottom of the mould shell containing corundum pipes to complete the combination of the mould shell and the cooling plate;
placing the combined cooling plate and the mould shell into a directional solidification furnace; heating the directional solidification furnace to 1480-1550 ℃ to partially melt the seed crystal, and partially melt the seed crystal to generate a pasty area with the length of 7mm; preserving heat for 20-30 min;
placing the master alloy for preparing the single-crystal superalloy casting into a crucible for heating, and melting into a molten state to obtain a master alloy solution;
pouring the solution master alloy into the mould shell after the heat preservation of the seed crystal pasty area is finished, and keeping the temperature of the directional solidification furnace unchanged; after the mother alloy solution is placed in the mould shell for 20-30 min, the mother alloy solution is pulled downwards at the speed of 3-9 mm/min, and then the single crystal superalloy casting with the <001> direction deviating from the axis is prepared;
step 6, preparing a plurality of single crystal superalloy castings with <001> directions deviating from the axes:
when preparing a plurality of single crystal superalloy castings with <001> direction deviating from the axis, firstly recycling reusable seed crystals according to the set quantity of the prepared single crystal superalloy castings, and enabling the recycled seed crystals to be one less than the set quantity of the prepared single crystal superalloy castings;
the specific process for preparing a plurality of off-axis single crystal superalloy castings in the <001> direction is as follows:
i, recycling reusable seed crystals, and cutting the obtained single-crystal superalloy casting with the <001> direction deviating from the axis at the joint of the seed crystal section and the transition section; the obtained seed crystal section is used as a seed crystal blank for repeated use, specifically, the bottom end of the obtained seed crystal blank is cut off by linear cutting to 7mm, so that a pasty area newly generated when the seed crystal is reused is ensured not to overlap with a pasty area generated when the seed crystal is used last time; grinding and cleaning the surface of the cut seed crystal blank to obtain recovered seed crystals;
II preparing a second single crystal superalloy casting having a <001> orientation offset from the axis by 5 degrees; specifically, the seed crystal is inserted into a cooling plate; repeating the step 5 to obtain a second single-crystal superalloy casting with the <001> direction deviating from the axis by 5-55 degrees;
III, repeating the process of recycling the reusable seed crystal and the process of preparing a second single-crystal superalloy casting, and sequentially completing the preparation of the rest single-crystal superalloy castings;
a plurality of off-axis <001> orientation single crystal superalloy castings are prepared using the recovered seed crystals.
2. The method for producing a single crystal superalloy according to claim 1, wherein the length of the seed section is 40 to 70mm and the side length is 3X 3mm to 15X 15mm; the length of the corundum tube is 30-45 mm.
3. The method of preparing a single crystal superalloy as in claim 1 wherein the corundum containing tube is in a mold shell of a seed section: the inner diameter of the part section is 8-40 mm; the circumferential surface of the transition section is a conical surface; connecting the large end face of the transition section with the lower end face of the part section; and connecting the small end of the transition section with the seed crystal section.
4. A method of producing a single crystal superalloy as in claim 3 wherein the diameter of the large end face of the transition section is 10 to 50mm, the diameter of the small end face is 6 to 30mm, and the length of the transition section is 5 to 10mm.
5. The method for producing a single crystal superalloy according to claim 1, wherein the recovered seed crystal has a length of 20mm to 50mm and a side length of 3X 3mm to 15X 15mm.
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