CN112191802B - Preparation method of Nb-Si-based ultrahigh-temperature alloy directional solidification blade simulation piece - Google Patents
Preparation method of Nb-Si-based ultrahigh-temperature alloy directional solidification blade simulation piece Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22C7/00—Patterns; Manufacture thereof so far as not provided for in other classes
- B22C7/02—Lost patterns
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22C3/00—Selection of compositions for coating the surfaces of moulds, cores, or patterns
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
- B22C9/02—Sand moulds or like moulds for shaped castings
- B22C9/04—Use of lost patterns
- B22C9/043—Removing the consumable pattern
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C9/00—Moulds or cores; Moulding processes
- B22C9/12—Treating moulds or cores, e.g. drying, hardening
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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D31/00—Cutting-off surplus material, e.g. gates; Cleaning and working on castings
Abstract
The invention relates to a preparation method of a Nb-Si-based ultrahigh temperature alloy directional solidification blade simulation piece, wherein the powder-liquid mass ratio, the sand spraying amount and the drying time of a filler and yttrium sol in a shell surface layer, a facing surface layer, a shell intermediate layer, a back layer and facing back layer slurry of a shell are different; the mass ratio of the filler of the slurry used for preparing the shell surface layer to the yttrium sol powder and the sand spraying mesh number are higher, so that the Nb-Si-based ultrahigh temperature alloy directional solidification blade simulation piece finally molded by the shell prepared by the method has higher surface quality. The mesh number of the electrofused yttrium oxide sand scattered on the middle layer and the back layer of the shell is gradually reduced so as to ensure that the whole shell is not cracked during sintering and has higher strength and thermal shock resistance finally. According to the invention, the Nb-Si based ultra-high temperature alloy blades with different oriented structures can be obtained by adjusting the process parameters, so that the performance requirements of the blades under different working conditions are met.
Description
Technical Field
The invention belongs to the technical field of ultra-high temperature alloy material forming processes, and relates to a preparation method of a Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece.
Background
The traditional niobium alloy, particularly the solid solution alloy, generally has good toughness, extensibility and cold processing performance, and can be processed into products with various complex shapes by deformation such as stamping, rolling, drawing, spinning, bending and the like at room temperature. In contrast, because niobium alloys are very sensitive to impurity levels and become hard and brittle with only trace amounts of oxygen, hydrogen, or carbon, which results in slagging during the casting process, residual alloy in the sprue and riser cannot be re-melted and recycled, making investment casting less economical, and thus rarely used in conventional niobium alloy forming.
As the latest derivative alloy in the niobium alloy family, the Nb-Si based ultra-high temperature alloy has the potential to be applied to the turbine blade of the next generation of aeroengine with high thrust-weight ratio. However, the intermetallic compound Nb5Si3The plasticity of the alloy is far less than that of other niobium alloys, and the low-temperature processability is correspondingly greatly reduced. Even when hot forged at high temperature, the alloy tends to crack. Investment casting is the most promising forming process to apply to this alloy. However, the alloy has a high melting point, and the contents of active elements, such as Hf and Ti, are high, so that the selection of the shell material and the molding requirements thereof are also extremely strict. In addition, turbine blades in aero-engines are generally prepared by a directional solidification method to improve the comprehensive mechanical properties of the turbine blades, and the process has clear requirements on the refractoriness and thermal shock resistance of the shell. Therefore, although the research history of the alloy has been in the past thirty years, the literature reports the preparation process of turbine blade forming parts, especially directional solidification forming parts.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a preparation method of a Nb-Si based ultrahigh temperature alloy directional solidification blade simulation piece, which is applied to the field of forming of turbine blades made of high melting point alloys.
Technical scheme
A preparation method of a Nb-Si based ultrahigh temperature alloy directional solidification blade simulation piece is characterized by comprising the following steps:
a. preparing a wax mould: drawing a three-dimensional graphic model of a turbine blade wax mold, and then preparing the wax mold by a rapid forming method, wherein the wax mold consists of a bottom support mounting part, a lower edge plate, a blade body, an upper edge plate, a riser and a holding part;
b. preparing slurry: stirring yttrium sol, adding a filler into the stirred yttrium sol, adding a defoaming agent n-octanol, and stirring to obtain slurry; the mass ratio of the filler to the yttrium sol in the slurry of the shell surface layer and the facing layer is 3-5: 1; the powder-liquid mass ratio of the filler to the yttrium sol in the shell intermediate layer slurry is 1-3: 1; the powder-liquid mass ratio of the filler to the yttrium sol in the back layer slurry and the backing layer slurry is 1-3: 1; the powder-liquid ratio of the filler to the yttrium sol in the sealing slurry is 1-3: 1;
c. preparing a shell: dipping the wax mold into the slurry, sanding, drying at room temperature and relative humidity of 50-70%, repeating the processes of slurry hanging, sanding and drying for 6-12 times, and finally dipping the wax mold into the slurry for sealing and drying; sanding the shell surface layer and the facing surface layer is made of fused yttrium oxide of 100-120 meshes, and drying for 10-30 h; sanding the intermediate layer of the shell is 50-80 meshes of fused yttrium oxide, and drying for 10-30 h; the back layer and the face back layer are sanded by fused yttrium oxide of 16-36 meshes and dried for 10-30 h; sealing and drying the slurry for 20-40 h;
d. dewaxing the shell: opening the top and the bottom of the shell subjected to sealing slurry drying respectively, and placing the shell in a resistance furnace for dewaxing at 500 ℃ for 30-60 min;
e. and (3) shell sintering: placing the dewaxed shell into an air atmosphere sintering furnace, sintering for 1h at 800-1200 ℃ and 1200-1600 ℃ respectively, then sintering for 1h at 1600-1800 ℃ and 1800-2100 ℃ respectively in a vacuum furnace, cooling along with the furnace, and finishing the shell preparation;
a. feeding: calculating the total mass of the casting according to the density of the Nb-Si-based ultrahigh temperature alloy and the volume of the casting; putting Nb-Si-based ultrahigh-temperature alloy which is 2-3 times of the total calculated mass of the casting into the prepared shell riser in a block or strip shape;
b. charging: installing the shell filled with the materials on a drawing rod in the crystallizer through a molybdenum support, fixedly charging the materials into the furnace, and adjusting the position of the drawing rod to enable the bottommost part of the shell to be flush with a molybdenum shielding layer on the crystallizer; coating yttrium oxide slurry with the mass ratio of powder to liquid being 6-10: 1 on the joint of the shell and the molybdenum support, and drying; the shell is vertical to the drawing rod and the molybdenum support in a line, cannot be inclined and is vertical to the molybdenum shielding layer on the crystallizer, after the shell is charged, the crystallizer is lifted, and the hearth of the directional solidification furnace is closed;
c. directional solidification: the vacuum of the directional solidification furnace chamber is pumped to 2 x 10-4～2×10-2Heating is started when the pressure is Pa; when the temperature reaches 500-800 ℃, preserving the heat for 30-60 min, and then controlling pre-drawing to finish pre-burning of yttrium oxide slurry at the joint of the shell and the molybdenum support; stopping vacuumizing when the temperature reaches 800-1200 ℃, and filling high-purity argon; continuously heating to 1850-2200 ℃, keeping the temperature for 10-30 min, and drawing the shell downwards into a crystallizer at a drawing speed of 5-200 mu m/s;
And 3, after the step 3 is finished, improving the surface quality of the Nb-Si-based ultrahigh temperature alloy directional solidification blade simulation piece by adopting a sand blasting or direct grinding machine polishing method.
The prepared slurry filler is pure electric melting yttrium oxide powder or mixed powder of electric melting yttrium oxide, electric melting zirconium oxide and doped oxide; the adding range of the fused zirconia and the doped oxide in the mixed powder is 5-10 mol%.
The doped oxide is CaO and La2O3、CeO2Or MgO.
During charging, the shell is required to be vertical to the drawing rod and the molybdenum support in a line, cannot be inclined and is vertical to the molybdenum shielding layer on the crystallizer.
Advantageous effects
The invention provides a preparation method of a Nb-Si-based ultrahigh temperature alloy directional solidification blade simulation piece. The shell surface layer and the facing layer of the shell, the shell intermediate layer and the back layer and the facing layer of the shell are different in the powder-liquid mass ratio of the filler to the yttrium sol, the sanding amount and the drying time; the mass ratio of the filler of the slurry used for preparing the shell surface layer to the yttrium sol powder and the sand spraying mesh number are higher, so that the Nb-Si-based ultrahigh temperature alloy directional solidification blade simulation piece finally molded by the shell prepared by the method has higher surface quality. The mesh number of the electrofused yttrium oxide sand scattered on the middle layer and the back layer of the shell is gradually reduced so as to ensure that the whole shell is not cracked during sintering and has higher strength and thermal shock resistance finally. Melting the Nb-Si based ultra-high temperature alloy in the riser of the shell by a directional solidification furnace, then enabling the alloy melt to fall into a cavity, and directly forming the Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece after the alloy melt is directionally pulled to a crystallizer. The directional solidification structure of the Nb-Si based ultrahigh temperature alloy is regulated and controlled by changing the process parameters such as the melt temperature, the drawing speed and the like, so that the performance requirement on the blade in the actual working condition is met.
In the step c of the step 2, the alloy structure of the blade simulation piece formed at the melt temperature of 1850-2000 ℃ consists of Nbss dendrites and Nbss/gamma- (Nb, X)5Si3A eutectic cell composition, and wherein the higher the melt temperature, the finer the Nbss dendrites; under the condition of melt temperature of 2000-2200 ℃, the alloy structure of the blade simulation piece is Nbss/gamma- (Nb, X)5Si3Forming eutectic cells; nbss/gamma- (Nb, X) in the alloy structure of the blade simulation with a drawing rate of 5 μm/s up to 200 μm/s5Si3The cross-sectional dimension of the cocell decreases from 450 μm to 20 μm.
The invention can form a Nb-Si base ultra-high temperature alloy blade simulation piece with a near-net-shape smooth surface and directional solidification structure characteristic. By adjusting the process parameters, the Nb-Si based ultra-high temperature alloy blades with different oriented structures can be obtained, and further the performance requirements on the blades under different working conditions are met.
Drawings
FIG. 1 is a three-dimensional graphical model of a wax mold for a Nb-Si based ultra-high temperature alloy directional solidification turbine blade shell;
FIG. 2 is the appearance of a Nb-Si based ultra-high temperature alloy directionally solidified turbine blade shell;
FIG. 3 is the appearance of a Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece;
FIG. 4 is a microstructure of a blade back of a Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece.
In the drawings:
1-bottom support installation part, 2-lower edge plate, 3-blade body, 4-upper edge plate, 5-riser, 6-suspension hole and 7-holding part
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
the technical scheme of the invention is that the method for preparing the Nb-Si-based ultrahigh temperature alloy directional solidification blade simulation piece comprises the following steps:
(1) preparing a shell suitable for a directional solidification blade simulation piece:
a. preparing a wax mould: drawing a three-dimensional graphic model of a turbine blade wax mold, and then preparing the wax mold by a rapid forming method, wherein the wax mold consists of a bottom support mounting part, a lower edge plate, a blade body, an upper edge plate, a riser and a holding part;
b. preparing slurry: stirring the yttrium sol at a constant speed, weighing the filler, adding the filler into the yttrium sol under stirring, adding n-octanol serving as a defoaming agent, and stirring uniformly to obtain slurry;
c. preparing a shell: dipping the wax mold into the slurry, sanding, drying at room temperature and relative humidity of 50-70%, repeating the processes of slurry hanging, sanding and drying for 6-12 times, and finally dipping the wax mold into the slurry for sealing and drying;
d. dewaxing the shell: opening the top and the bottom of the shell subjected to sealing slurry drying respectively, and placing the shell in a resistance furnace for dewaxing at 500 ℃ for 30-60 min;
e. and (3) shell sintering: and (3) putting the dewaxed shell into an air atmosphere sintering furnace, sintering for 1h at 800-1200 ℃ and 1200-1600 ℃ respectively, then sintering for 1h at 1600-1800 ℃ and 1800-2100 ℃ respectively in a vacuum furnace, cooling along with the furnace, and finishing the shell preparation.
(2) Preparing a Nb-Si-based ultrahigh temperature alloy directional solidification blade simulation piece:
a. feeding: the density of the Nb-Si based ultra-high temperature alloy is 7g/cm3Calculating the total mass of the casting according to the volume of the casting; putting Nb-Si-based ultrahigh-temperature alloy which is 2-3 times of the total calculated mass of the casting into the prepared shell riser in a block or strip shape;
b. charging: installing the shell filled with the materials on a drawing rod in the crystallizer through a molybdenum support, fixedly charging the materials into the furnace, and adjusting the position of the drawing rod to enable the bottommost part of the shell to be flush with a molybdenum shielding layer on the crystallizer; coating prepared yttrium oxide slurry with the mass ratio of powder to liquid being 6-10: 1 at the joint of the shell and the molybdenum support and drying; the shell is vertical to the drawing rod and the molybdenum support in a line, cannot be inclined and is vertical to the molybdenum shielding layer on the crystallizer, after the shell is charged, the crystallizer is lifted, and the hearth of the directional solidification furnace is closed;
c. directional solidification: the vacuum of the directional solidification furnace chamber is pumped to 2 x 10-4～2×10-2Heating is started when the pressure is Pa; when the temperature reaches 500-800 ℃, preserving the heat for 30-60 min, and then controlling pre-drawing through a computer to finish pre-burning of yttrium oxide slurry at the joint of the shell and the molybdenum support; stopping vacuumizing when the temperature reaches 800-1200 ℃, and filling high-purity argon; and continuously heating to 1850-2200 ℃, keeping the temperature for 10-30 min, and drawing the shell downwards into the crystallizer at a drawing speed of 5-200 mu m/s.
(3) Post-treatment of the Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece:
after removing the shell, cutting off the dead head, the bottom support and other parts of the Nb-Si-based ultrahigh-temperature alloy directional solidification blade simulation casting by adopting electrospark wire cutting or diamond cutting; the surface quality of the Nb-Si based ultrahigh temperature alloy directional solidification blade simulation piece is improved by adopting a sand blasting or direct grinding method.
The invention is further illustrated below:
the filler for preparing the slurry is pure electric melting yttrium oxide powder, or electric melting yttrium oxide, electric melting zirconium oxide and doped oxide (CaO, La)2O3、CeO2And one of MgO). Wherein the adding range of the fused zirconia and the doped oxide in the mixed powder is 5-10 mol%. All the fillers have a particle size of 325 mesh.
Wherein, because the yttria has higher inertia, the yttria can hardly react with each element in the Nb-Si base ultra-high temperature alloy melt at high temperature, and is a modeling material suitable for preparing Nb-Si base ultra-high temperature alloy investment casting shell. However, yttria reacts with water and is used with water-based bindersThe prepared slurry has short service life. In particular, yttria has a melting point as high as 2430 ℃, and thus it is difficult to achieve higher densification by conventional pressureless sintering. In addition, the surface of the Nb-Si-based ultrahigh temperature alloy casting cast by the shell prepared by pure yttrium oxide has a more serious sand-sticking phenomenon. The service life of the yttria slurry can be properly prolonged by doping the fused zirconia, and CaO and La are doped2O3、CeO2And one of MgO oxide, which can improve the sintering property of yttrium oxide and also can relieve the sand-sticking phenomenon on the surface of the Nb-Si-based ultra-high temperature alloy casting cast by the shell prepared by the yttrium oxide.
The mass ratio of the filler to the yttrium sol in the slurry of the shell surface layer and the facing layer is 3-5: 1, the sand is fused yttrium oxide with the particle size of 100-120 meshes, and the drying is carried out for 10-30 h; powder-liquid mass ratio of the filler to the yttrium sol in the shell intermediate layer slurry is 1-3: 1, sanding is performed by electrically melting yttrium oxide with 50-80 meshes, and drying is performed for 10-30 hours; the powder-liquid mass ratio of the filler to the yttrium sol in the back layer slurry and the backing layer slurry is 1-3: 1, the sanding is 16-36 meshes of fused yttrium oxide, and the drying is carried out for 10-30 h; and drying the sealing slurry for 20-40 hours, wherein the powder-liquid ratio of the filler to the yttrium sol in the sealing slurry is 1-3: 1.
The mass ratio of the filler of the slurry used for preparing the shell surface layer to the yttrium sol powder and the sand spraying mesh number are higher, so that the Nb-Si-based ultrahigh temperature alloy directional solidification blade simulation piece finally molded by the shell prepared by the method has higher surface quality. The mesh number of the electrofused yttrium oxide sand scattered on the middle layer and the back layer of the shell is gradually reduced so as to ensure that the whole shell is not cracked during sintering and has higher strength and thermal shock resistance finally.
In this patent, Nb-Si based ultra high temperature alloys are formed into blade simulators by drop casting and directional solidification.
The method comprises the steps of melting Nb-Si-based ultrahigh-temperature alloy in a riser of a shell by a directional solidification furnace, then enabling the alloy melt to fall into a cavity, and directly forming the Nb-Si-based ultrahigh-temperature alloy directional solidification blade simulation piece after the alloy melt is directionally pulled to a crystallizer.
Under the condition of a melt temperature of 1850-2000 ℃, the alloy structure of the formed blade simulation piece is formed by a first edgeNbss/gamma- (Nb, X) with axial growth of blade5Si3A co-cell and Nbss dendrites, and wherein the higher the melt temperature, the finer the Nbss dendrites; under the condition of melt temperature of 2000-2200 ℃, the alloy structure of the blade simulation piece is formed by Nbss/gamma- (Nb, X) growing along the axial direction of the blade5Si3Forming eutectic cells; nbss/gamma- (Nb, X) in the alloy structure of the blade simulation with a drawing rate of 5 μm/s up to 200 μm/s5Si3The average diameter of the cross section of the cocell is reduced from 450 μm to 20 μm.
The directional solidification structure of the Nb-Si based ultrahigh temperature alloy can be regulated and controlled by changing the process parameters such as the melt temperature, the drawing speed and the like, so that the performance requirement on the blade in the actual working condition is met.
The specific embodiment is as follows:
example 1: the Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece is prepared by adopting a pure yttrium oxide shell under the conditions that the melt temperature is 1850 ℃ and the drawing rate is 5 mu m/s, and the technical process and the steps in the embodiment are as follows:
(1) preparing a wax mould: drawing a three-dimensional graphic model of the turbine blade wax mold, and then preparing the wax mold by a rapid forming method;
(2) preparing slurry: weighing a measuring cup of yttrium sol, and stirring at a constant speed; weighing electrofused yttrium oxide powder, and then adding the electrofused yttrium oxide powder into the yttrium sol which is being stirred; adding n-octanol serving as a defoaming agent, and uniformly stirring to obtain slurry;
(3) preparing a shell: and (3) immersing the wax mould into the slurry, sanding, drying at room temperature and 50% of relative humidity, repeating the processes of sizing, sanding and drying for 6 times, and finally immersing the wax mould into the slurry for sealing and drying. Wherein, the powder-liquid ratio of the slurry used for preparing the shell surface layer and the facing layer is 4:1, the sand is 100 meshes of electric melting yttrium oxide, and then the shell surface layer and the facing layer are dried for 10 hours; preparing a shell intermediate layer by using slurry with a powder-liquid ratio of 3:1, sanding by using 50-mesh fused yttrium oxide, and then drying for 10 hours; preparing slurry for the shell back layer and the face back layer, wherein the powder-liquid ratio of the slurry is 2:1, the sand is 16-mesh fused yttrium oxide, and then drying is carried out for 20 hours; the slurry powder-liquid ratio for sealing slurry is 2:1, and drying is carried out for 30 hours;
(4) dewaxing the shell: respectively opening the top and the bottom of the shell subjected to sealing slurry drying, and placing the shell in a resistance furnace for dewaxing at 500 ℃ for 30 min;
(5) and (3) shell sintering: placing the dewaxed shell into an air atmosphere sintering furnace to be sintered for 1h at 800 ℃ and 1200 ℃ respectively, then sintering for 1h at 1800 ℃ and 2100 ℃ respectively in a vacuum furnace, cooling along with the furnace, and finishing the preparation of the shell;
(6) feeding: putting Nb-Si-based ultrahigh-temperature alloy which is 2 times of the total calculated mass of the casting into the prepared shell riser in a block shape;
(7) charging: installing the shell filled with the materials on a drawing rod in the crystallizer through a molybdenum support, fixedly charging the materials into the furnace, and adjusting the position of the drawing rod to enable the bottommost part of the shell to be flush with a molybdenum shielding layer on the crystallizer; coating prepared yttrium oxide slurry with the powder-liquid mass ratio of 6:1 at the joint of the shell and the molybdenum support and drying; the shell is vertical to the drawing rod and the molybdenum support in a line, cannot be inclined and is vertical to the molybdenum shielding layer on the crystallizer, after the shell is charged, the crystallizer is lifted, and the hearth of the directional solidification furnace is closed;
(8) directional solidification: the vacuum of the directional solidification furnace chamber is pumped to 2 x 10-3Heating is started when the pressure is Pa; when the temperature reaches 500 ℃, preserving the heat for 30min, and then controlling pre-drawing through a computer to finish pre-burning of yttrium oxide slurry at the joint of the shell and the molybdenum support; stopping vacuumizing when the temperature reaches 800 ℃, and filling high-purity argon; the temperature is continuously increased to 1850 ℃, and after the temperature is kept for 30min, the shell is drawn downwards into the crystallizer at the drawing speed of 5 mu m/s.
(9) Post-treatment of the Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece: after removing the shell, cutting off the dead head, the bottom support and other parts of the casting by adopting a wire electrical discharge machining method; the surface quality of the casting is improved by adopting a sand blasting method; finally obtaining the directional solidification blade simulation piece of the Nb-Si base ultra-high temperature alloy. The alloy structure of the blade simulation piece is formed by Nbss/gamma- (Nb, X) growing along the axial direction of the blade5Si3A co-cell and Nbss dendrites. Wherein, Nbss/gamma- (Nb, X)5Si3The average diameter of the cross section of the cocell is around 450 μm.
Example 2: using doped ZrO2+ CaO yttria-based shells in the meltThe Nb-Si based ultrahigh temperature alloy directional solidification blade simulation piece is prepared under the conditions that the temperature is 1950 ℃ and the drawing speed is 20 mu m/s, and the technological process and the steps in the embodiment are as follows:
(1) preparing a wax mould: drawing a three-dimensional graphic model of the turbine blade wax mold, and then preparing the wax mold by a rapid forming method;
(2) preparing slurry: weighing a measuring cup of yttrium sol, and stirring at a constant speed; preparing mixed powder of fused yttrium oxide powder, fused zirconium oxide and calcium oxide, wherein ZrO2And CaO accounts for 5 mol% and 10 mol%, respectively; then adding the mixed powder into the yttrium sol under stirring; adding n-octanol serving as a defoaming agent, and uniformly stirring to obtain slurry;
(3) preparing a shell: and (3) immersing the wax mould into the slurry, sanding, drying at room temperature and relative humidity of 60%, repeating the processes of sizing, sanding and drying for 9 times, and finally immersing the wax mould into the slurry for sealing and drying. Wherein, the powder-liquid ratio of the slurry used for preparing the shell surface layer and the facing layer is 3:1, the sand is 110-mesh electric melting yttrium oxide, and then the shell surface layer and the facing layer are dried for 20 hours; preparing a shell interlayer by using slurry with a powder-liquid ratio of 2:1, sanding by using 60-mesh fused yttrium oxide, and then drying for 20 hours; preparing slurry for the shell back layer and the face back layer, wherein the powder-liquid ratio of the slurry is 1:1, the sand is 20-mesh fused yttrium oxide, and then drying is carried out for 20 hours; drying for 20 hours, wherein the powder-liquid ratio of slurry for sealing slurry is 3: 1;
(4) dewaxing the shell: opening the top and the bottom of the shell which is sealed and dried with the slurry respectively, and placing the shell in a resistance furnace for dewaxing for 40min at 500 ℃;
(5) and (3) shell sintering: placing the dewaxed shell in an air atmosphere sintering furnace to be sintered for 1h at 900 ℃ and 1300 ℃ respectively, then sintering for 1h at 1700 ℃ and 2000 ℃ respectively in a vacuum furnace, cooling along with the furnace, and finishing the preparation of the shell;
(6) feeding: putting Nb-Si-based ultrahigh-temperature alloy which is 2.5 times of the total calculated mass of the casting into the prepared shell riser in a block shape;
(7) charging: installing the shell filled with the materials on a drawing rod in the crystallizer through a molybdenum support, fixedly charging the materials into the furnace, and adjusting the position of the drawing rod to enable the bottommost part of the shell to be flush with a molybdenum shielding layer on the crystallizer; coating prepared yttrium oxide slurry with the mass ratio of powder to liquid being 7:1 at the joint of the shell and the molybdenum support and drying; the shell is vertical to the drawing rod and the molybdenum support in a line, cannot be inclined and is vertical to the molybdenum shielding layer on the crystallizer, after the shell is charged, the crystallizer is lifted, and the hearth of the directional solidification furnace is closed;
(8) directional solidification: the vacuum of the directional solidification furnace chamber is pumped to 2 x 10-4Heating is started when the pressure is Pa; when the temperature reaches 600 ℃, preserving the heat for 40min, and then controlling pre-drawing through a computer to finish pre-sintering of yttrium oxide slurry at the joint of the shell and the molybdenum support; stopping vacuumizing when the temperature reaches 900 ℃, and filling high-purity argon; the temperature is continuously increased to 1950 ℃, and after the temperature is kept for 30min, the shell is drawn downwards into the crystallizer at the drawing speed of 20 mu m/s.
(9) Post-treatment of the Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece: after the shell is removed, the parts of a casting, such as a riser, a bottom support and the like, are cut off by a diamond cutting method; the surface quality of the casting is improved by adopting a sand blasting and straight grinding machine polishing method; finally obtaining the directional solidification blade simulation piece of the Nb-Si base ultra-high temperature alloy. The alloy structure of the blade simulation piece is formed by Nbss/gamma- (Nb, X) growing along the axial direction of the blade5Si3A co-cell and Nbss dendrites. Wherein, Nbss/gamma- (Nb, X)5Si3The average diameter of the cross section of the cocells is around 300 μm.
Example 3: using doped ZrO2The Nb-Si based ultrahigh temperature alloy directionally solidified blade simulation piece is prepared by using an MgO yttria-based shell under the conditions that the melt temperature is 2050 ℃ and the drawing rate is 100 mu m/s, and the technical process and the steps in the embodiment are as follows:
(1) preparing a wax mould: drawing a three-dimensional graphic model of the turbine blade wax mold, and then preparing the wax mold by a rapid forming method;
(2) preparing slurry: weighing a measuring cup of yttrium sol, and stirring at a constant speed; preparing mixed powder of fused yttrium oxide powder, fused zirconium oxide and magnesium oxide, wherein ZrO2And MgO accounts for 10 mol% and 10 mol% respectively; then adding the mixed powder into the yttrium sol under stirring; adding n-octanol serving as a defoaming agent, and uniformly stirring to obtain slurry;
(3) preparing a shell: and (3) immersing the wax mould into the slurry, sanding, drying at room temperature and 70% of relative humidity, repeating the processes of sizing, sanding and drying for 12 times, and finally immersing the slurry for sealing and drying. Wherein, the powder-liquid ratio of the slurry used for preparing the shell surface layer and the facing layer is 5:1, the sand is 120 meshes of electric melting yttrium oxide, and then the shell surface layer and the facing layer are dried for 30 hours; preparing a shell intermediate layer by using slurry with a powder-liquid ratio of 1:1, sanding by using 70-mesh fused yttrium oxide, and then drying for 30 hours; preparing slurry for the shell back layer and the face back layer, wherein the powder-liquid ratio of the slurry is 1:1, the sand is 28-mesh fused yttrium oxide, and then drying is carried out for 30 hours; drying for 40 hours with the slurry powder-liquid ratio of 1: 1;
(4) dewaxing the shell: opening the top and the bottom of the shell which is sealed and dried with slurry respectively, and placing the shell in a resistance furnace for dewaxing for 50min at 500 ℃;
(5) and (3) shell sintering: placing the dewaxed shell into an air atmosphere sintering furnace to be sintered for 1h at 1000 ℃ and 1400 ℃ respectively, then sintering for 1h at 1800 ℃ and 1900 ℃ respectively in a vacuum furnace, cooling along with the furnace, and finishing the shell preparation;
(6) feeding: putting Nb-Si-based ultrahigh-temperature alloy which is 3 times of the total calculated mass of the casting into the prepared shell riser in a block shape;
(7) charging: installing the shell filled with the materials on a drawing rod in the crystallizer through a molybdenum support, fixedly charging the materials into the furnace, and adjusting the position of the drawing rod to enable the bottommost part of the shell to be flush with a molybdenum shielding layer on the crystallizer; coating prepared yttrium oxide slurry with the mass ratio of powder to liquid being 8:1 at the joint of the shell and the molybdenum support and drying; the shell is vertical to the drawing rod and the molybdenum support in a line, cannot be inclined and is vertical to the molybdenum shielding layer on the crystallizer, after the shell is charged, the crystallizer is lifted, and the hearth of the directional solidification furnace is closed;
(8) directional solidification: the vacuum of the directional solidification furnace chamber is pumped to 2 x 10-2Heating is started when the pressure is Pa; when the temperature reaches 700 ℃, preserving the heat for 50min, and then controlling pre-drawing through a computer to finish pre-burning of yttrium oxide slurry at the joint of the shell and the molybdenum support; stopping vacuumizing when the temperature reaches 1000 ℃, and filling high-purity argon; continuously heating to 2050 ℃, keeping the temperature for 30min, and drawing the shell downwards into a crystallizer at a drawing speed of 100 mu m/sIn (1).
(9) Post-treatment of the Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece: after the shell is removed, the parts of a casting, such as a riser, a bottom support and the like, are cut off by adopting an electric spark cutting method; the surface quality of the casting is improved by adopting a sand blasting and straight grinding machine polishing method; finally obtaining the directional solidification blade simulation piece of the Nb-Si base ultra-high temperature alloy. The alloy structure of the blade simulation piece is formed by Nbss/gamma- (Nb, X) growing along the axial direction of the blade5Si3And (4) forming a eutectic cell. Wherein, Nbss/gamma- (Nb, X)5Si3The average diameter of the cross section of the cocell is around 90 μm.
Example 4: using doped ZrO2+La2O3The yttria-based shell is used for preparing the Nb-Si-based ultrahigh temperature alloy directionally solidified blade simulation piece under the conditions that the melt temperature is 2200 ℃ and the drawing speed is 200 mu m/s, and the technical process and the steps in the embodiment are as follows:
(1) preparing a wax mould: drawing a three-dimensional graphic model of the turbine blade wax mold, and then preparing the wax mold by a rapid forming method;
(2) preparing slurry: weighing a measuring cup of yttrium sol, and stirring at a constant speed; preparing mixed powder of fused yttrium oxide powder, fused zirconium oxide and lanthanum oxide, wherein ZrO2And La2O3The occupied mole fractions are respectively 10 mol% and 5 mol%; then adding the mixed powder into the yttrium sol under stirring; adding n-octanol serving as a defoaming agent, and uniformly stirring to obtain slurry;
(3) preparing a shell: and (3) immersing the wax mould into the slurry, sanding, drying at room temperature and relative humidity of 60%, repeating the processes of sizing, sanding and drying for 10 times, and finally immersing the wax mould into the slurry for sealing and drying. Wherein, the powder-liquid ratio of the slurry used for preparing the shell surface layer and the facing layer is 5:1, the sand is 120 meshes of electric melting yttrium oxide, and then the shell surface layer and the facing layer are dried for 20 hours; preparing a shell interlayer by using slurry with a powder-liquid ratio of 2:1, sanding by using 80-mesh fused yttrium oxide, and drying for 20 hours; preparing slurry for the shell back layer and the face back layer, wherein the powder-liquid ratio of the slurry is 1:1, the sand is 36-mesh fused yttrium oxide, and then drying is carried out for 20 hours; drying for 40 hours with the slurry powder-liquid ratio of 2: 1;
(4) dewaxing the shell: respectively opening the top and the bottom of the shell subjected to sealing slurry drying, and placing the shell in a resistance furnace for dewaxing at 500 ℃ for 60 min;
(5) and (3) shell sintering: placing the dewaxed shell in an air atmosphere sintering furnace to be sintered for 1h at 1000 ℃ and 1400 ℃ respectively, then sintering for 1h at 1700 ℃ and 2000 ℃ respectively in a vacuum furnace, cooling along with the furnace, and finishing the preparation of the shell;
(6) feeding: putting Nb-Si-based ultrahigh-temperature alloy which is 3 times of the total calculated mass of the casting into the prepared shell riser in a block shape;
(7) charging: installing the shell filled with the materials on a drawing rod in the crystallizer through a molybdenum support, fixedly charging the materials into the furnace, and adjusting the position of the drawing rod to enable the bottommost part of the shell to be flush with a molybdenum shielding layer on the crystallizer; coating prepared yttrium oxide slurry with the powder-liquid mass ratio of 10:1 at the joint of the shell and the molybdenum support and drying; the shell is vertical to the drawing rod and the molybdenum support in a line, cannot be inclined and is vertical to the molybdenum shielding layer on the crystallizer, after the shell is charged, the crystallizer is lifted, and the hearth of the directional solidification furnace is closed;
(8) directional solidification: the vacuum of the directional solidification furnace chamber is pumped to 1 x 10-3Heating is started when the pressure is Pa; when the temperature reaches 500 ℃, preserving the heat for 30min, and then controlling pre-drawing through a computer to finish pre-burning of yttrium oxide slurry at the joint of the shell and the molybdenum support; stopping vacuumizing when the temperature reaches 1000 ℃, and filling high-purity argon; the temperature is continuously increased to 2200 ℃, and the shell is drawn downwards into the crystallizer at the drawing speed of 200 mu m/s after heat preservation for 10 min.
(9) Post-treatment of the Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece: after the shell is removed, the parts of a casting, such as a riser, a bottom support and the like, are cut off by adopting an electric spark cutting method; the surface quality of the casting is improved by adopting a sand blasting and straight grinding machine polishing method; finally obtaining the directional solidification blade simulation piece of the Nb-Si base ultra-high temperature alloy. The alloy structure of the blade simulation piece is formed by Nbss/gamma- (Nb, X) growing along the axial direction of the blade5Si3And (4) forming a eutectic cell. Wherein, Nbss/gamma- (Nb, X)5Si3The average diameter of the cross section of the cocells is around 20 μm.
Example 5: using doped ZrO2+CeO2The Nb-Si based ultrahigh temperature alloy directional solidification blade simulation piece is prepared by the yttrium oxide based shell under the conditions that the melt temperature is 2050 ℃ and the drawing rate is 20 mu m/s, and the technical process and the steps in the embodiment are as follows:
(1) preparing a wax mould: drawing a three-dimensional graphic model of the turbine blade wax mold, and then preparing the wax mold by a rapid forming method;
(2) preparing slurry: weighing a measuring cup of yttrium sol, and stirring at a constant speed; preparing mixed powder of fused yttrium oxide powder, fused zirconium oxide and cerium oxide, wherein ZrO2And CeO2The occupied mole fractions are respectively 5 mol% and 10 mol%; then adding the mixed powder into the yttrium sol under stirring; adding n-octanol serving as a defoaming agent, and uniformly stirring to obtain slurry;
(3) preparing a shell: and (3) immersing the wax mould into the slurry, sanding, drying at room temperature and relative humidity of 60%, repeating the processes of sizing, sanding and drying for 9 times, and finally immersing the wax mould into the slurry for sealing and drying. Wherein, the powder-liquid ratio of the slurry used for preparing the shell surface layer and the facing layer is 4:1, the sand is 100 meshes of electric melting yttrium oxide, and then the shell surface layer and the facing layer are dried for 24 hours; preparing a shell intermediate layer by using slurry with a powder-liquid ratio of 2:1, sanding 80-mesh fused yttrium oxide, and drying for 24 hours; preparing slurry for the shell back layer and the face back layer, wherein the powder-liquid ratio of the slurry is 2:1, the sand is 16-mesh fused yttrium oxide, and then drying is carried out for 24 hours; drying for 40 hours with the slurry powder-liquid ratio of 2: 1;
(4) dewaxing the shell: respectively opening the top and the bottom of the shell subjected to sealing slurry drying, and placing the shell in a resistance furnace for dewaxing at 500 ℃ for 30 min;
(5) and (3) shell sintering: placing the dewaxed shell in an air atmosphere sintering furnace to be sintered for 1h at 1000 ℃ and 1400 ℃ respectively, then sintering for 1h at 1700 ℃ and 2000 ℃ respectively in a vacuum furnace, cooling along with the furnace, and finishing the preparation of the shell;
(6) feeding: putting Nb-Si-based ultrahigh-temperature alloy which is 2.5 times of the total calculated mass of the casting into the prepared shell riser in a block shape;
(7) charging: installing the shell filled with the materials on a drawing rod in the crystallizer through a molybdenum support, fixedly charging the materials into the furnace, and adjusting the position of the drawing rod to enable the bottommost part of the shell to be flush with a molybdenum shielding layer on the crystallizer; coating prepared yttrium oxide slurry with the mass ratio of powder to liquid being 8:1 at the joint of the shell and the molybdenum support and drying; the shell is vertical to the drawing rod and the molybdenum support in a line, cannot be inclined and is vertical to the molybdenum shielding layer on the crystallizer, after the shell is charged, the crystallizer is lifted, and the hearth of the directional solidification furnace is closed;
(8) directional solidification: the vacuum of the directional solidification furnace chamber is pumped to 1 x 10-2Heating is started when the pressure is Pa; when the temperature reaches 600 ℃, preserving the heat for 30min, and then controlling pre-drawing through a computer to finish pre-sintering of yttrium oxide slurry at the joint of the shell and the molybdenum support; stopping vacuumizing when the temperature reaches 1000 ℃, and filling high-purity argon; and continuously heating to 2050 ℃, keeping the temperature for 20min, and drawing the shell downwards into the crystallizer at a drawing speed of 20 mu m/s.
(9) Post-treatment of the Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece: after the shell is removed, the parts of a casting, such as a riser, a bottom support and the like, are cut off by adopting an electric spark cutting method; the surface quality of the casting is improved by adopting a sand blasting and straight grinding machine polishing method; finally obtaining the directional solidification blade simulation piece of the Nb-Si base ultra-high temperature alloy. The alloy structure of the blade simulation piece is formed by Nbss/gamma- (Nb, X) growing along the axial direction of the blade5Si3And (4) forming a eutectic cell. Wherein, Nbss/gamma- (Nb, X)5Si3The average diameter of the cross section of the cocells is around 300 μm.
Claims (6)
1. A preparation method of a Nb-Si based ultrahigh temperature alloy directional solidification blade simulation piece is characterized by comprising the following steps:
step 1, preparing a shell suitable for a directionally solidified blade simulation piece:
a. preparing a wax mould: drawing a three-dimensional graphic model of a turbine blade wax mold, and then preparing the wax mold by a rapid forming method, wherein the wax mold consists of a bottom support mounting part, a lower edge plate, a blade body, an upper edge plate, a riser and a holding part;
b. preparing slurry: stirring yttrium sol, adding a filler into the stirred yttrium sol, adding a defoaming agent n-octanol, and stirring to obtain slurry; the mass ratio of the filler to the yttrium sol in the slurry of the shell surface layer and the facing layer is 3-5: 1; the powder-liquid mass ratio of the filler to the yttrium sol in the shell intermediate layer slurry is 1-3: 1; the powder-liquid mass ratio of the filler to the yttrium sol in the back layer slurry and the backing layer slurry is 1-3: 1; the powder-liquid ratio of the filler to the yttrium sol in the sealing slurry is 1-3: 1;
c. preparing a shell: dipping the wax mold into the slurry, sanding, drying at room temperature and relative humidity of 50-70%, repeating the processes of slurry hanging, sanding and drying for 6-12 times, and finally dipping the wax mold into the slurry for sealing and drying; sanding the shell surface layer and the facing surface layer is made of fused yttrium oxide of 100-120 meshes, and drying for 10-30 h; sanding the intermediate layer of the shell is 50-80 meshes of fused yttrium oxide, and drying for 10-30 h; the back layer and the face back layer are sanded by fused yttrium oxide of 16-36 meshes and dried for 10-30 h; sealing and drying the slurry for 20-40 h;
d. dewaxing the shell: opening the top and the bottom of the shell subjected to sealing slurry drying respectively, and placing the shell in a resistance furnace for dewaxing at 500 ℃ for 30-60 min;
e. and (3) shell sintering: placing the dewaxed shell into an air atmosphere sintering furnace, sintering for 1h at 800-1200 ℃ and 1200-1600 ℃ respectively, then sintering for 1h at 1600-1800 ℃ and 1800-2100 ℃ respectively in a vacuum furnace, cooling along with the furnace, and finishing the shell preparation;
step 2, preparing a Nb-Si-based ultrahigh temperature alloy directional solidification blade simulation piece:
a. feeding: calculating the total mass of the casting according to the density of the Nb-Si-based ultrahigh temperature alloy and the volume of the casting; putting Nb-Si-based ultrahigh-temperature alloy which is 2-3 times of the total calculated mass of the casting into the prepared shell riser in a block or strip shape;
b. charging: installing the shell filled with the materials on a drawing rod in the crystallizer through a molybdenum support, fixedly charging the materials into the furnace, and adjusting the position of the drawing rod to enable the bottommost part of the shell to be flush with a molybdenum shielding layer on the crystallizer; coating yttrium oxide slurry with the mass ratio of powder to liquid being 6-10: 1 on the joint of the shell and the molybdenum support, and drying; the shell is vertical to the drawing rod and the molybdenum support in a line, cannot be inclined and is vertical to the molybdenum shielding layer on the crystallizer, after the shell is charged, the crystallizer is lifted, and the hearth of the directional solidification furnace is closed;
c. directional solidification: the vacuum of the directional solidification furnace chamber is pumped to 2 x 10-4～2×10-2At Pa, begin to addHeating; when the temperature reaches 500-800 ℃, preserving the heat for 30-60 min, and then controlling pre-drawing to finish pre-burning of yttrium oxide slurry at the joint of the shell and the molybdenum support; stopping vacuumizing when the temperature reaches 800-1200 ℃, and filling high-purity argon; continuously heating to 1850-2200 ℃, keeping the temperature for 10-30 min, and drawing the shell downwards into a crystallizer at a drawing speed of 5-200 mu m/s; wherein the alloy structure of the blade simulation piece formed at the melt temperature of 1850-2000 ℃ consists of Nbsss dendrite and Nbss/gamma- (Nb, X)5Si3A eutectic cell composition, and wherein the higher the melt temperature, the finer the Nbss dendrites; under the condition of melt temperature of 2000-2200 ℃, the alloy structure of the blade simulation piece is Nbss/gamma- (Nb, X)5Si3Forming eutectic cells; nbss/gamma- (Nb, X) in the alloy structure of the blade simulation with a drawing rate of 5 μm/s up to 200 μm/s5Si3The cross section size of the cocell is reduced from 450 μm to 20 μm;
step 3, post-processing of the Nb-Si based ultrahigh temperature alloy directional solidification blade simulation piece: and after the shell is removed, cutting off the dead head and the bottom support part of the Nb-Si-based ultrahigh temperature alloy directional solidification blade simulation casting.
2. The method for preparing the Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece according to claim 1, characterized in that: and 3, after the step 3 is finished, improving the surface quality of the Nb-Si-based ultrahigh temperature alloy directional solidification blade simulation piece by adopting a sand blasting or direct grinding machine polishing method.
3. The method for preparing the Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece according to the claim 1 or 2, characterized in that: and 3, cutting off the riser and the bottom support by adopting wire cut electrical discharge machining or diamond cutting.
4. The method for preparing the Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece according to the claim 1 or 2, characterized in that: the prepared slurry filler is pure electric melting yttrium oxide powder or mixed powder of electric melting yttrium oxide, electric melting zirconium oxide and doped oxide; the adding range of the fused zirconia and the doped oxide in the mixed powder is 5-10 mol%.
5. The method for preparing the Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece according to claim 4, is characterized in that: the doped oxide is CaO and La2O3、CeO2Or MgO.
6. The method for preparing the Nb-Si based ultra-high temperature alloy directional solidification blade simulation piece according to claim 4, is characterized in that: during charging, the shell is required to be vertical to the drawing rod and the molybdenum support in a line, cannot be inclined and is vertical to the molybdenum shielding layer on the crystallizer.
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