CN112695377B - Shuttering and method for preparing [011] or [111] oriented single crystal high-temperature alloy - Google Patents

Shuttering and method for preparing [011] or [111] oriented single crystal high-temperature alloy Download PDF

Info

Publication number
CN112695377B
CN112695377B CN202011457073.5A CN202011457073A CN112695377B CN 112695377 B CN112695377 B CN 112695377B CN 202011457073 A CN202011457073 A CN 202011457073A CN 112695377 B CN112695377 B CN 112695377B
Authority
CN
China
Prior art keywords
single crystal
seed crystal
casting
axial direction
amplifier
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202011457073.5A
Other languages
Chinese (zh)
Other versions
CN112695377A (en
Inventor
李树索
胡斌
裴延玲
宫声凯
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beihang University Sichuan International Center For Innovation In Western China Co ltd
Original Assignee
Beihang University Sichuan International Center For Innovation In Western China Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Beihang University Sichuan International Center For Innovation In Western China Co ltd filed Critical Beihang University Sichuan International Center For Innovation In Western China Co ltd
Priority to CN202011457073.5A priority Critical patent/CN112695377B/en
Publication of CN112695377A publication Critical patent/CN112695377A/en
Application granted granted Critical
Publication of CN112695377B publication Critical patent/CN112695377B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/10Crucibles or containers for supporting the melt
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22CFOUNDRY MOULDING
    • B22C9/00Moulds or cores; Moulding processes
    • B22C9/02Sand moulds or like moulds for shaped castings
    • B22C9/04Use of lost patterns
    • B22C9/043Removing the consumable pattern
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C19/00Alloys based on nickel or cobalt
    • C22C19/03Alloys based on nickel or cobalt based on nickel
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C19/00Alloys based on nickel or cobalt
    • C22C19/03Alloys based on nickel or cobalt based on nickel
    • C22C19/05Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/051Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
    • C22C19/057Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being less 10%
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/52Alloys
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B33/00After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/08Etching
    • C30B33/10Etching in solutions or melts

Landscapes

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

Abstract

The invention provides a mold shell and a method for preparing [011] or [111] oriented single crystal high-temperature alloy, belonging to the technical field of single crystal high-temperature alloy preparation. The mould shell provided by the invention comprises an amplifier, seed crystals, an angle regulator and a casting, wherein the angle regulator realizes the axial direction adjustment of the casting; the axial direction of the casting is consistent with the [011] direction or the [111] direction of the seed crystal. According to the invention, the formwork can enable the growth direction of the dendritic crystal in the casting to be consistent with the heat flow direction, so that intersection between dendritic crystal trunks can be effectively avoided, elements are uniformly distributed, a weak area generated by asymmetric growth of the dendritic crystal is eliminated, and the mechanical property of the single crystal high-temperature alloy is improved.

Description

Shuttering and method for preparing [011] or [111] oriented single crystal high-temperature alloy
Technical Field
The invention relates to the field of single crystal high temperature alloy preparation, in particular to a mold shell and a method for preparing [011] or [111] oriented single crystal high temperature alloy.
Background
The nickel-based single crystal superalloy is widely applied to blade materials of advanced aeroengines due to excellent tensile, lasting, oxidation resistance and corrosion resistance. The nickel-based single crystal superalloy is a solid solution with a face-centered cubic structure and has a preferred orientation in the [001] direction.
The preparation of the nickel-based single crystal superalloy mainly adopts a directional solidification technology, when the solidification direction is consistent with the preferred growth direction of [001], the dry spacing of primary dendrites is uniform and is arranged parallel to the solidification direction, the secondary dendrites are symmetrically distributed, and the cross section presents a cross flower shape. When the solidification direction is along [011] or [111], i.e. deviating from the [001] direction by a certain angle, the primary dendrite trunk still grows along the [001] direction, and when the growth is limited by the geometric dimension of the casting, the secondary dendrite, the tertiary dendrite and other high-order dendrite grow upwards. In the solidification process, when dendrite trunks grown from dendrite arms meet each other, the faster growing one hinders the growth of the other, and the dendrite trunks intersect with each other. A closed area is formed at the front edge of the hindered dendritic crystal stem, so that gamma' phase forming elements are enriched, the structure is uneven, and a weak area is formed, so that the mechanical property of the alloy is influenced.
Disclosure of Invention
In view of this, the present invention provides a mold shell and a method for preparing [011] or [111] oriented single crystal superalloy, the mold shell provided by the present invention makes the growth direction of dendrite in the casting consistent with the heat flow direction, and improves the mechanical properties of single crystal superalloy.
The invention provides a mold shell for preparing [011] or [111] oriented single crystal high-temperature alloy, which comprises an amplifier; the amplifier comprises a positive hemisphere at the lower part and a hopper-shaped structure positioned above the positive hemisphere;
the seed crystal extends into the amplifier through the bottom opening of the positive hemisphere, and the axial direction of the seed crystal is consistent with the axial direction of the amplifier; the axial direction of the seed crystal is consistent with the direction of the seed crystal [001 ];
an angle adjuster located on the bucket structure;
the casting is positioned on the angle adjuster, and the axial direction of the casting is adjusted through the angle adjuster; the axial direction of the casting is consistent with the [011] direction or the [111] direction of the seed crystal;
the amplifier, the angle regulator and the casting are of shell-shaped structures with communicated interiors.
Preferably, the axial direction of the casting is deviated towards the direction of the seed crystal [100] and is 45 degrees with the axial direction of the seed crystal.
Preferably, the axial direction of the casting is deviated towards the direction of the seed crystal [110] and is 55 degrees with the axial direction of the seed crystal.
Preferably, the radius of the positive hemisphere is 6-9 mm.
Preferably, the bucket-shaped structure is a quadrangular prism with two trapezoidal surfaces and four rectangular surfaces; one rectangular surface of the quadrangular prism is in contact with the circular surface of the regular hemisphere.
Preferably, the height of the bucket-shaped structure is 40-60 mm, and the thickness of the bucket-shaped structure is 5-20 mm.
Preferably, the distance of the seed crystal extending into the amplifier is 3-12 mm.
Preferably, the seed crystal is prepared by a method comprising the steps of:
calibrating the [001] direction on a single crystal high-temperature alloy sample, and directionally cutting to obtain a square single crystal; the side normal direction of the square single crystal is the [100] or [110] direction;
and polishing and corroding the square single crystal to obtain the seed crystal.
Preferably, the corrosion treatment is chemical reagent corrosion, the chemical reagent is a mixed solution of hydrogen peroxide and hydrochloric acid, and the volume ratio of the hydrogen peroxide to the hydrochloric acid is 1: 2-1: 5; the mass concentration of the hydrogen peroxide is 30%, and the mass concentration of the hydrochloric acid is 25-40%.
The invention also provides a method for preparing the [011] or [111] oriented single crystal superalloy, which comprises the following steps:
melting the master alloy, pouring the obtained molten liquid into a mould shell, preserving heat for 5-15 min, and drawing downwards to obtain [011] or [111] oriented single crystal high-temperature alloy;
the temperature of the mould shell is 1500-1600 ℃;
the downward drawing speed is 1-10 mm/min;
the formwork is the formwork of the technical scheme.
The invention provides a mold shell for preparing [011] or [111] oriented single crystal high-temperature alloy, which comprises an amplifier; the amplifier comprises a positive hemisphere at the lower part and a hopper-shaped structure positioned above the positive hemisphere; the seed crystal extends into the amplifier through the bottom opening of the positive hemisphere, and the axial direction of the seed crystal is consistent with the axial direction of the amplifier; the axial direction of the seed crystal is consistent with the direction of the seed crystal [001 ]; an angle adjuster located on the bucket structure; the casting is positioned on the angle adjuster, and the axial direction of the casting is adjusted through the angle adjuster; the axial direction of the casting is consistent with the [011] direction or the [111] direction of the seed crystal; the amplifier, the angle regulator and the casting are of shell-shaped structures with communicated interiors. According to the invention, the die shell can enable the growth direction of the dendritic crystal in the casting to be consistent with the heat flow direction, effectively avoids intersection between dendritic crystal stems, enables elements to be uniformly distributed, eliminates a weak area generated by asymmetric growth of the dendritic crystal, and improves the mechanical property of the single crystal high-temperature alloy.
The invention also provides a method for preparing the [011] or [111] oriented single crystal high-temperature alloy by using the mould shell of the technical scheme, and the single crystal high-temperature alloy prepared by the invention has uniformly dispersed elements and good mechanical property. The data of the examples show that: the dendritic crystal growth rule of the single crystal high-temperature alloy obtained by the invention has no intercross condition.
The data of the examples show that: the preparation method of the invention is utilized to obtain the dendritic crystal growth rule of the single crystal high temperature alloy without the condition of intercrossing; [011] the tensile strength of the oriented single crystal superalloy at 980 ℃ is 556 MPa; [111] the tensile strength of the oriented single crystal superalloy at 980 ℃ is 510 MPa.
Drawings
FIG. 1 is a schematic view of a formwork arrangement of the present invention, wherein: 1 is seed crystal, 2 is amplifier, 2-1 is a positive hemisphere, 2-2 is a hopper-shaped structure, 3 is an angle regulator, and 4 is a casting;
FIG. 2 is a schematic view of a bucket structure used in the embodiments;
FIG. 3 is a schematic diagram of the structure of a mold shell for producing a [011] oriented single crystal superalloy;
FIG. 4 is a [011] plane phase diagram of the [011] oriented single crystal superalloy obtained in example 1;
FIG. 5 is a schematic structural diagram of a mold shell for producing a [111] oriented single crystal superalloy;
FIG. 6 is a crystal phase diagram of the [111] oriented single crystal superalloy obtained in example 2;
FIG. 7 is a longitudinal sectional view of a cast of a [111] oriented single crystal superalloy obtained in comparative example 2.
Detailed Description
The invention provides a mold shell for preparing [011] or [111] oriented single crystal high-temperature alloy, which comprises an amplifier; the amplifier comprises a positive hemisphere at the lower part and a hopper-shaped structure positioned above the positive hemisphere;
the seed crystal extends into the amplifier through the bottom opening of the positive hemisphere, and the axial direction of the seed crystal is consistent with the axial direction of the amplifier; the axial direction of the seed crystal is consistent with the direction of the seed crystal [001 ];
an angle adjuster located on the bucket structure;
the casting is positioned on the angle adjuster, and the axial direction of the casting is adjusted through the angle adjuster; the axial direction of the casting is consistent with the [011] direction or the [111] direction of the seed crystal;
the amplifier, the angle regulator and the casting are of shell-shaped structures with communicated interiors.
FIG. 1 is a schematic view of a formwork arrangement of the present invention, and the following description is provided in conjunction with FIG. 1.
The formwork provided by the invention comprises an amplifier 2, wherein the amplifier comprises a positive hemisphere 2-1 at the lower part and a hopper-shaped structure 2-2 positioned above the positive hemisphere; the radius of the positive hemispheroid is preferably 6-9 mm, and more preferably 7.5 mm. In a specific embodiment of the present invention, the bucket-shaped structure is preferably a quadrangular prism with two trapezoidal surfaces and four rectangular surfaces; the specific structure is shown in figure 2; one rectangular surface of the quadrangular prism is in contact with the circular surface of the regular hemisphere; the height of the hopper-shaped structure is 40-60 mm, namely the value of h in the figure 2 is 40-60 mm; the thickness of the bucket-shaped structure is 5-20 mm, more preferably 15mm, namely the value of a in figure 2 is 5-20 mm.
The mould shell provided by the invention comprises a seed crystal 1, wherein the seed crystal extends into an amplifier through an opening at the bottom of a positive hemisphere, and the distance of the seed crystal extending into the amplifier is preferably 3-12 mm, and particularly preferably 7mm or 9 mm. In the invention, the axial direction of the seed crystal is consistent with the axial direction of the amplifier; the axial direction of the seed crystal is consistent with the direction of the seed crystal [001 ].
In the present invention, the seed crystal is preferably prepared by a method comprising the steps of:
calibrating the [001] direction on a single crystal high-temperature alloy sample, and directionally cutting to obtain a square single crystal; the side normal direction of the square single crystal is the [100] or [110] direction;
and polishing and corroding the square single crystal to obtain the seed crystal.
In the present invention, the calibration method is preferably a Laue method or an X-ray diffractometer method. The directional cutting mode is not particularly limited in the invention, and the directional cutting means well known to those skilled in the art can be used for cutting.
In the present invention, the polishing preferably comprises the steps of: the materials are sequentially ground by 60#, 240#, 600#, 1000#, 1500# and 2000# sandpaper and then polished by 1mm diamond abrasive paste. In the present invention, the etching treatment is preferably chemical etching, the chemical etching is preferably a mixed solution of hydrogen peroxide and hydrochloric acid, and the volume ratio of hydrogen peroxide to hydrochloric acid is preferably 1: 2-1: 5, more preferably 4: 6; the mass concentration of the hydrogen peroxide is preferably 30%, and the mass concentration of the hydrochloric acid is preferably 25-40%, and more preferably 38% or 30%. In the invention, the cross section of the seed crystal is preferably 3 x 3mm, and the length of the seed crystal is preferably 18-27 mm.
The formwork of the present invention includes an angle adjuster 3 located on the bucket structure. In the invention, the angle adjuster can realize the adjustment of the axial direction of the casting. In a particular embodiment of the invention, the shape of the angle adjuster is preferably a triangular prism; one rectangular face of the triangular prism contacts the upper top face of the funnel-like structure of the amplifier. In the invention, the axial direction of the casting is adjusted by adjusting the slope angle of the triangular prism.
The membrane shell provided by the invention comprises a casting 4; the casting is positioned on the angle adjuster; the axial direction of the casting is consistent with the [011] direction or the [111] direction of the seed crystal. The shape of the casting is not particularly limited, and the casting can be set according to actual requirements. In a specific embodiment of the invention, when preparing a [011] oriented single crystal superalloy, the axial direction of the casting is deviated towards the direction of the seed crystal [100] and forms an angle of 45 degrees with the axial direction of the seed crystal; when preparing a [111] oriented single crystal superalloy, the axial direction of the casting is offset toward the seed crystal [110] and is 55 degrees from the seed crystal axial direction.
In the present invention, the material of the mold shell is preferably a ceramic refractory material, and the ceramic refractory material is not particularly limited in the present invention, and may be a ceramic refractory material well known to those skilled in the art.
In the present invention, the formwork is preferably prepared by:
assembling the seed crystal, the amplifier wax mould, the angle regulator wax mould and the casting wax mould to obtain a combined wax mould;
and coating ceramic refractory slurry with the thickness of 5-20 mm on the outer part of the combined wax mold, dewaxing at 200-500 ℃, and roasting at 800-1100 ℃ for 8-12 h to obtain the mold shell.
In the invention, the placing angles of the seed crystal, the amplifier wax mould, the angle regulator wax mould and the casting wax mould are preferably consistent with the technical scheme so as to obtain the mould shell structure meeting the requirements.
The material of the ceramic refractory slurry is not particularly required, and the ceramic refractory slurry known by the technical personnel in the field can be adopted.
The invention also provides a method for preparing the [011] or [111] oriented single crystal superalloy, which comprises the following steps:
melting the master alloy, pouring the obtained molten liquid into a mould shell, preserving heat for 5-15 min, and drawing downwards to obtain [011] or [111] oriented single crystal high-temperature alloy;
the temperature of the mould shell is 1500-1600 ℃;
the downward drawing speed is 1-10 mm/min;
the formwork is the formwork of the technical scheme.
The material of the master alloy is not particularly limited, and those skilled in the art can select the master alloy according to the material of the desired single crystal superalloy, and in the specific embodiment of the present invention, the master alloy is preferably 77.5Ni-6Al-6Ta-3W-3Mo-3Re-1.5Cr or 80Ni-6Al-3Ta-6W-1Re-4 Co. The temperature and time for melting the master alloy are not particularly limited in the present invention as long as the master alloy can be melted.
In the present invention, the temperature of the formwork is preferably controlled by placing the formwork in a directional solidification furnace; in the present invention, the temperature of the mold shell is the crystallization temperature; the temperature of the die casing is preferably set according to the type of master alloy selected. The parameters of the casting are not particularly limited in the present invention, and casting means well known to those skilled in the art may be used. In the invention, the master alloy melt is preferably poured over the mold shell.
In the invention, the downward drawing speed is preferably 1-10 mm/min, and particularly preferably 3.5mm/min or 5 mm/min. The drawing time is not particularly limited, and the crystal pulling is finished.
The mold shell and the method for preparing [011] or [111] oriented single crystal superalloy provided by the present invention are described in detail below with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Example 1
This example is to prepare a [011] oriented single crystal superalloy
Preparing seed crystals:
marking the [001] direction and the [100] direction on the Ni-based single crystal superalloy pattern by adopting a Laue method, and directionally cutting out a square single crystal, wherein the axial direction of the square single crystal is the [001] direction, and the side normal direction is the [100] direction.
Then polishing and grinding the square single crystal and carrying out corrosion treatment to obtain seed crystals, wherein the size of the cross section of each seed crystal is 3 x 3mm, and the length of each seed crystal is 27 mm; the polishing and grinding comprises the following steps: sequentially grinding 60#, 240#, 600#, 1000#, 1500# and 2000# sand paper, and polishing by using 1mm diamond grinding paste; the corrosion treatment is chemical reagent corrosion, the chemical reagent is a hydrogen peroxide and hydrochloric acid mixed solution, the mass concentration of the hydrogen peroxide is 30%, the mass concentration of the hydrochloric acid is 38%, and the volume ratio of the hydrogen peroxide to the hydrochloric acid is 4: 6.
manufacturing a formwork:
providing a wax mould of the amplifier, wherein the wax mould of the amplifier comprises a right hemispheroid wax mould at the lower part and a funnel-shaped structure wax mould at the upper part;
extending the seed crystal prepared in the step into an amplifier wax mould through the bottom opening of the positive hemispheroid wax mould, wherein the extending distance is 9 mm;
placing an angle regulator and a casting wax mold on the amplifier wax mold, controlling the axial direction of the casting wax mold to deviate towards the direction of the seed crystal [100] and form an angle of 45 degrees with the axial direction of the seed crystal (namely the direction of the seed crystal [001 ]), and finally obtaining a combined wax mold;
coating ceramic refractory slurry with the thickness of 10mm on the outer part of the combined wax mould, dewaxing at the temperature of 250 ℃, and roasting at the temperature of 900 ℃ for 10 hours to prepare a mould shell with seed crystals;
in the obtained formwork, the radius of the positive hemispheroid is 7.5mm, the specific structure of the hopper-shaped structure is shown in figure 2, the height h of the hopper-shaped structure is 45mm, and the thickness a is 15 mm; the axial direction of the casting deviates to the direction of the seed crystal [100] and forms an angle of 45 degrees with the axial direction of the seed crystal (namely the direction of the seed crystal [001 ]); FIG. 3 is a schematic view of a formwork of the present embodiment.
The preparation process of the single crystal high temperature alloy comprises the following steps:
and (3) putting the mould shell into a directional solidification furnace, heating the directional solidification furnace to 1550 ℃, putting 77.5Ni-6Al-6Ta-3W-3Mo-3Re-1.5Cr master alloy into a crucible of the directional solidification furnace to be melted, pouring the melted master alloy into the mould shell, keeping the temperature for 10min, drawing downwards at the speed of 4.5mm/min, and obtaining a [011] oriented single crystal high-temperature alloy casting after crystal pulling is finished.
FIG. 4 is a [011] plane phase diagram of the [011] oriented single crystal superalloy obtained in this example. As can be seen from fig. 4: the integrity of the single crystal is good, and the dendritic structure is uniform.
Comparative example 1
The [011] oriented single crystal high temperature alloy casting is prepared by adopting the [011] oriented seed crystal positive axis growth.
The tensile strength of the single crystal superalloy castings obtained in example 1 and comparative example 1 was tested by using HB5195-1996 metal high temperature tensile test method, and the results were: the tensile strength of the [011] oriented single crystal superalloy casting prepared in the comparative example 1 at 980 ℃ is 522MPa, and the tensile strength of the [011] curved single crystal superalloy casting obtained in the example 1 at 980 ℃ is 556 MPa.
Example 2
This example is to prepare a [111] oriented single crystal superalloy
Preparing seed crystals;
marking the [001] direction and the [110] direction on the Ni-based single crystal superalloy pattern by adopting a Laue method, and directionally cutting out a square single crystal, wherein the axis of the single crystal in the direction is the [001] direction, and the normal direction of the side surface is the [110] direction.
Then polishing and grinding and corroding the square single crystal to obtain seed crystals; the cross section of the seed crystal is 3 multiplied by 3mm, and the length of the seed crystal is 21 mm; the polishing and grinding comprises the following steps: sequentially grinding 60#, 240#, 600#, 1000#, 1500# and 2000# sand paper, and polishing by using 1mm diamond grinding paste; the corrosion treatment is chemical reagent corrosion, the chemical reagent is a hydrogen peroxide and hydrochloric acid mixed solution, the mass concentration of the hydrogen peroxide is 30%, the mass concentration of the hydrochloric acid is 30%, and the volume ratio of the hydrogen peroxide to the hydrochloric acid is 4: 6.
manufacturing a formwork:
providing a wax mould of the amplifier, wherein the wax mould of the amplifier comprises a right hemispheroid wax mould at the lower part and a funnel-shaped structure wax mould at the upper part;
extending the seed crystal prepared in the step into an amplifier wax mould through the bottom opening of the positive hemispheroid wax mould, wherein the extending distance is 7 mm;
placing an angle regulator wax mould and a casting wax mould on the amplifier wax mould, controlling the axial direction of the casting wax mould to deviate towards the direction of the seed crystal [110] and form an angle of 55 degrees with the axial direction of the seed crystal (namely the direction of the seed crystal [001 ]), and finally obtaining a combined wax mould;
coating ceramic refractory slurry with the thickness of 10mm on the outer part of the combined wax mould, dewaxing at the temperature of 250 ℃, and roasting at the temperature of 900 ℃ for 10 hours to prepare a mould shell with seed crystals;
in the obtained formwork, the radius of the positive hemispheroid is 7.5mm, the specific structure of the hopper-shaped structure is shown in figure 2, the thickness a of the hopper-shaped structure is 15mm, and the height h of the hopper-shaped structure is 50 mm; the axial direction of the casting deviates to the direction of the seed crystal [110] and forms 55 degrees with the axial direction of the seed crystal (namely the direction of the seed crystal [001 ]); FIG. 5 is a schematic view of a formwork of the present embodiment.
The preparation process comprises the following steps:
and (3) putting the mould shell into a directional solidification furnace, heating the directional solidification furnace to 1540 ℃, putting 80Ni-6Al-3Ta-6W-1Re-4Co mother alloy into a crucible of the directional solidification furnace to be melted, pouring the melted mother alloy into the mould shell, keeping the temperature for 10min, drawing the mother alloy downwards at the speed of 3mm/min, and obtaining the [111] oriented single crystal high-temperature alloy casting after finishing crystal pulling.
FIG. 6 is a crystal phase diagram of the [111] oriented single crystal superalloy obtained in this example. As can be seen from fig. 6: the growth direction of the dendrite is consistent with the direction of heat flow, and along the [001] direction, the growth rule of the dendrite does not have the condition of mutual intersection.
Comparative example 2
Adopting the positive axis growth of the [111] oriented seed crystal to prepare the [111] oriented single crystal high-temperature alloy casting.
FIG. 7 is a longitudinal sectional view of a cast [111] oriented single crystal superalloy casting obtained in comparative example 2, as seen in FIG. 7: the dendritic crystals of the casting grow more disorderly and intersect with each other.
The tensile strength of the single crystal superalloy castings obtained in example 2 and comparative example 2 was tested by using HB5195-1996 metal high temperature tensile test method, and the results are as follows: the tensile strength of the cast product of the 111 oriented single crystal superalloy prepared in the comparative example 2 at 980 ℃ is 484MPa, and the tensile strength of the cast product of the 111 oriented single crystal superalloy obtained in the example 2 at 980 ℃ is 510 MPa.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and improvements can be made without departing from the principle of the present invention, and these modifications and improvements should also be construed as the protection scope of the present invention.

Claims (4)

1. A mold shell for preparing a [011] or [111] oriented single crystal superalloy, comprising an amplifier; the amplifier comprises a positive hemisphere at the lower part and a hopper-shaped structure positioned above the positive hemisphere;
the seed crystal extends into the amplifier through the bottom opening of the positive hemisphere, and the axial direction of the seed crystal is consistent with the axial direction of the amplifier; the axial direction of the seed crystal is consistent with the direction of the seed crystal [001 ];
an angle adjuster located on the bucket structure;
the casting is positioned on the angle adjuster, and the axial direction of the casting is adjusted through the angle adjuster; the axial direction of the casting is consistent with the [011] direction or the [111] direction of the seed crystal;
the amplifier, the angle regulator and the casting are of shell-shaped structures with communicated interiors;
the axial direction of the casting deviates to the direction of the seed crystal [100] and forms an angle of 45 degrees with the axial direction of the seed crystal;
the axial direction of the casting deviates to the direction of the seed crystal [110] and forms an angle of 55 degrees with the axial direction of the seed crystal;
the radius of the positive hemispheroid is 6-9 mm;
the bucket-shaped structure is a quadrangular prism with two trapezoidal surfaces and four rectangular surfaces; one rectangular surface of the quadrangular prism is in contact with the circular surface of the regular hemisphere;
the height of the bucket-shaped structure is 40-60 mm, and the thickness of the bucket-shaped structure is 5-20 mm;
the distance that the seed crystal stretches into the amplifier is 3-12 mm.
2. A formwork in accordance with claim 1 wherein said seed crystal is produced by a method comprising the steps of:
calibrating the [001] direction on a single crystal high-temperature alloy sample, and directionally cutting to obtain a square single crystal; the side normal direction of the square single crystal is the [100] or [110] direction;
and polishing and corroding the square single crystal to obtain the seed crystal.
3. A formwork in accordance with claim 2, wherein the etching treatment is chemical etching, the chemical etching is a mixture of hydrogen peroxide and hydrochloric acid, and the volume ratio of hydrogen peroxide to hydrochloric acid is 1: 2-1: 5; the mass concentration of the hydrogen peroxide is 30%, and the mass concentration of the hydrochloric acid is 25-40%.
4. A method for preparing a [011] or [111] oriented single crystal superalloy, comprising the steps of:
melting the master alloy, pouring the obtained molten liquid into a mould shell, preserving heat for 5-15 min, and drawing downwards to obtain [011] or [111] oriented single crystal high-temperature alloy;
the temperature of the mould shell is 1500-1600 ℃;
the downward drawing speed is 1-10 mm/min;
the formwork is as claimed in any one of claims 1 to 3.
CN202011457073.5A 2020-12-10 2020-12-10 Shuttering and method for preparing [011] or [111] oriented single crystal high-temperature alloy Active CN112695377B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011457073.5A CN112695377B (en) 2020-12-10 2020-12-10 Shuttering and method for preparing [011] or [111] oriented single crystal high-temperature alloy

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011457073.5A CN112695377B (en) 2020-12-10 2020-12-10 Shuttering and method for preparing [011] or [111] oriented single crystal high-temperature alloy

Publications (2)

Publication Number Publication Date
CN112695377A CN112695377A (en) 2021-04-23
CN112695377B true CN112695377B (en) 2022-01-28

Family

ID=75508993

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011457073.5A Active CN112695377B (en) 2020-12-10 2020-12-10 Shuttering and method for preparing [011] or [111] oriented single crystal high-temperature alloy

Country Status (1)

Country Link
CN (1) CN112695377B (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112974732B (en) * 2021-05-12 2021-07-30 中国航发北京航空材料研究院 Method for preparing single crystal superalloy by combining solid solution columnar crystal with crystal selection
CN114606563B (en) * 2022-03-05 2023-06-06 湘潭大学 Method for preparing single crystal superalloy with versatile and reusable seed crystal
CN114622270B (en) * 2022-03-11 2024-02-09 中国航发北京航空材料研究院 Method for preparing single crystal superalloy test bar
CN114775041B (en) * 2022-04-11 2023-09-08 北航(四川)西部国际创新港科技有限公司 Preparation method of [111] orientation single crystal superalloy
CN116329530B (en) * 2023-05-12 2023-08-04 山西昌鸿电力器材有限公司 Intelligent casting process for hardware fitting

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2164192C2 (en) * 1999-02-26 2001-03-20 Всероссийский научно-исследовательский институт авиационных материалов Method of producing castings from high-temperature alloys with directed or single-crystal structure
CN107059133A (en) * 2017-01-04 2017-08-18 西北工业大学 A kind of accurate control single-crystal orientation selects crystal method
CN107574473A (en) * 2017-10-31 2018-01-12 泰州市金鹰精密铸造有限公司 A kind of Z-type crystal selector
CN111360234A (en) * 2020-03-26 2020-07-03 成都航大新材料有限公司 Single crystal high temperature alloy thin-wall casting based on secondary orientation control and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2164192C2 (en) * 1999-02-26 2001-03-20 Всероссийский научно-исследовательский институт авиационных материалов Method of producing castings from high-temperature alloys with directed or single-crystal structure
CN107059133A (en) * 2017-01-04 2017-08-18 西北工业大学 A kind of accurate control single-crystal orientation selects crystal method
CN107574473A (en) * 2017-10-31 2018-01-12 泰州市金鹰精密铸造有限公司 A kind of Z-type crystal selector
CN111360234A (en) * 2020-03-26 2020-07-03 成都航大新材料有限公司 Single crystal high temperature alloy thin-wall casting based on secondary orientation control and preparation method thereof

Also Published As

Publication number Publication date
CN112695377A (en) 2021-04-23

Similar Documents

Publication Publication Date Title
CN112695377B (en) Shuttering and method for preparing [011] or [111] oriented single crystal high-temperature alloy
KR101858779B1 (en) A method for the preparation of doped garnet structure single crystals with diameters of up to 500 mm
CN108624959B (en) Method for preparing single crystal superalloy using solution treated seed crystal
US3494709A (en) Single crystal metallic part
CN111364096B (en) Substrate-triggered single crystal high-temperature alloy directional solidification process
CN110777284B (en) High-defect-tolerance single-crystal high-temperature alloy component and preparation method thereof
US10421121B2 (en) Method of manufacturing Ni alloy casting and Ni alloy casting
CN104947175A (en) Method for preparing single crystal high temperature alloy block material through laser 3D printing
NO154909B (en) PROCEDURE FOR DIRECTIVE STRENGTHENING OF A METAL MELT.
KR20010040128A (en) Controlling casting grain spacing
Wang et al. Substrate stimulating technique for Ni-based single crystal superalloy preparation during direction solidification
JP7072146B2 (en) Single crystal growth method for iron gallium alloy
EP0059549A2 (en) Method of casting an article
CN114775041B (en) Preparation method of [111] orientation single crystal superalloy
CN102672102A (en) Preparation method of plane thin-wall casting
CN112974732B (en) Method for preparing single crystal superalloy by combining solid solution columnar crystal with crystal selection
US5161602A (en) Graphite mold for single crystal growth of active materials and a process for manufacturing the same
US4108676A (en) Mixed oxide compounds for casting advanced superalloy materials
CN1150185A (en) Technique for preparing monocrystal of metal material
RU2285580C2 (en) Apparatus for producing cast products by directional crystallization
CN115255336B (en) Composite component monocrystalline thin-wall component and preparation method thereof
CN113373502B (en) Process method for controlling freckle defect in single crystal casting
JP7318884B2 (en) Single crystal growth method for iron-gallium alloy
CN110644043A (en) Large-size artificial alumina doped colored gemstone and production method thereof
CN114618993B (en) Method for preparing single crystal superalloy by using cooling plate with holes to assist <001> oriented seed crystal

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant