CN100587134C - Method for preparing Ni3Al based single-crystal high-temperature alloy by employing seed crystal - Google Patents

Method for preparing Ni3Al based single-crystal high-temperature alloy by employing seed crystal Download PDF

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CN100587134C
CN100587134C CN200710179684A CN200710179684A CN100587134C CN 100587134 C CN100587134 C CN 100587134C CN 200710179684 A CN200710179684 A CN 200710179684A CN 200710179684 A CN200710179684 A CN 200710179684A CN 100587134 C CN100587134 C CN 100587134C
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crystal
temperature alloy
based single
temperature
seed crystal
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CN101255605A (en
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韩雅芳
李树索
蒋立武
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Beihang University
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Beihang University
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Abstract

The invention discloses a method of preparing a Ni<3>Al-based monocrystal high-temperature alloy through the crystallon method, comprising: firstly a crystallon which is provided with a certain crystal orientation is cut directionally on the Ni<3>Al-based monocrystal high-temperature alloy; the crystallon is extended into a parts wax pattern; and ceramics castable refractory is smeared on the outside of the crystallon and the parts wax pattern; then a ceramics shuttering provided with the crystallon is manufactured via dewaxing and burning; and the Ni<3>Al-based monocrystal high-temperature alloy material is teemed, shaped and manufactured by making use of the ceramics shuttering in a monocrystal furnace. The invention relates to a monocrystal preparation technology which can accurately control crystal orientation of the monocrystal and fine texture to manufacture the high quality Ni<3>Al-based monocrystal high-temperature alloy material.

Description

A kind of Ni 3The Al based single-crystal high-temperature alloy adopts the method for seed crystal preparation
Technical field
The present invention relates to a kind of Ni 3Al based single-crystal high-temperature alloy preparation methods is more particularly said, is meant that a kind of employing seed crystal legal system is equipped with Ni 3The method of Al based single-crystal high-temperature alloy.
Background technology
The high development of aeronautical and space technology requires engine to have the higher working efficiency when of having an high regard for, and this just requires engine to have higher working temperature.At present, single crystal super alloy is a critical material of making advanced aero engine turbine blades and turning vane owing to have advantages such as fusing point height, hot strength and creep-resistant property be good.Single crystal super alloy is in the directional freeze process, the direction of growth shows tangible preferred orientation, this preferred orientation often with the certain drift angle of axial existence, the performance of single crystal casting is significantly descended, widespread use for aircraft engine brings disadvantageous effect, so the control of crystalline orientation is particularly important.
The seed crystal method is meant the seed crystal that cuts certain crystalline orientation on the good single crystal of choosing, and adopts to go out single crystal in the seed crystal face epitaxy, and the crystalline orientation of obtained single crystal is consistent with the crystalline orientation of seed crystal.
Summary of the invention
The objective of the invention is to propose a kind of Ni 3The Al based single-crystal high-temperature alloy adopts the method for seed crystal preparation, and this method is accurately controlled crystalline orientation and solidified structure by seed crystal, and the Ni that makes 3The Al based single-crystal high-temperature alloy has and Ni 3The crystalline orientation of Al based single-crystal high-temperature alloy seed crystal unanimity, identical solidified structure; Thereby the Ni that obtained performance is good 3Al based single-crystal high-temperature alloy material.
The present invention is a kind of Ni 3The Al based single-crystal high-temperature alloy adopts the method for seed crystal preparation, comprises following preparation steps:
The first step, preparation Ni 3The seed crystal of Al based single-crystal high-temperature alloy;
At Ni 3Orientation cuts out the test block with certain crystalline orientation on the Al based single-crystal high-temperature alloy body, and the crystal face of test block is carried out polished finish and surface corrosion processing, obtains Ni 3Al based single-crystal high-temperature alloy seed crystal;
Polished finish condition: adopt the crystal face of 150#, 360#, 500#, 1000#, 2000# silicon carbide paper polishing test block, on polishing machine, carry out polished finish then;
The surface corrosion treatment condition: the test block after will polishing is taken out after adopting etching reagent surface treatment 2～10min, promptly gets Ni 3A1 based single-crystal high-temperature alloy seed crystal;
Described Ni 3Al based single-crystal high-temperature alloy body is Ni-(5～20) Mo-(6～10) Al-(0～a 0.1) B material;
Described etching reagent is nitric acid HNO 3, hydrofluoric acid HF and glycerine C 3H 8O 3Form, and add 10～50ml hydrofluoric acid and 40～100ml glycerine in every 10ml nitric acid;
Perhaps described etching reagent is by hydrochloric acid HCl and hydrogen peroxide H 2O 2Form, and add 5～30ml hydrogen peroxide in every 10ml hydrochloric acid;
Second step, preparation part wax-pattern;
Wax material is melted the back inject component die under 40～120 ℃ temperature condition, and compression moulding under 0.5～10MPa pressure, make part wax-pattern 2;
The 3rd step is with the Ni that makes in the above-mentioned the first step 3The crystal face of Al based single-crystal high-temperature alloy seed crystal 1 extends in the part wax-pattern 2 that makes in above-mentioned second step to the upper edge, and Ni 3Al based single-crystal high-temperature alloy seed crystal 1 stretches into part wax-pattern 2 0.5～10mm;
At Ni 3The outside of Al based single-crystal high-temperature alloy seed crystal 1 and part wax-pattern 2 is coated with and hangs the thick ceramic fire resistant slurry of 3～20mm, dewaxes under 120～500 ℃ of temperature then, is making the ceramic shell mould that has seed crystal behind roast 5～15h under 800～1700 ℃ of temperature;
The 4th step, the ceramic shell mould that makes in above-mentioned the 3rd step is put into single crystal growing furnace, temperature to 1400 in the adjusting single crystal growing furnace～1950 ℃, Ni-(5～20) Mo-(6～10) Al-(0～0.1) B molten metal flows in the ceramic shell moulds by sprue gate 3, behind insulation wait 2～30min; Speed with 0.1～15mm/min moves down crystal pulling, after crystal pulling finishes, takes out after cooling to room temperature with the furnace, promptly makes and Ni 3The make peace Ni of good solidified structure of Al based single-crystal high-temperature alloy seed crystal orientation one 3Al based single-crystal high-temperature alloy material; The temperature of described molten metal is 1400～1800 ℃.
Description of drawings
Fig. 1 is Ni 3On the Al based single-crystal high-temperature alloy body＜001 the orientation synoptic diagram.
Fig. 2 is Ni 3On the Al based single-crystal high-temperature alloy body＜011 the orientation synoptic diagram.
Fig. 3 is Ni 3On the Al based single-crystal high-temperature alloy body＜111 the orientation synoptic diagram.
Fig. 4 is a wax-pattern model assembling synoptic diagram.
Fig. 5 A is Ni 3The metallograph of Al based single-crystal high-temperature alloy seed crystal.
Fig. 5 B is the Ni that makes through the inventive method 3The metallograph of Al based single-crystal high-temperature alloy.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
The present invention is a kind of Ni 3The Al based single-crystal high-temperature alloy adopts the method for seed crystal preparation, comprises following preparation steps:
The first step, preparation Ni 3The seed crystal of Al based single-crystal high-temperature alloy;
Referring to shown in Figure 1, at Ni 3Orientation cuts out and has＜001〉orientation test block on the Al based single-crystal high-temperature alloy body, and (001) face of test block is carried out polished finish and surface corrosion is handled, and obtains Ni 3Al based single-crystal high-temperature alloy seed crystal;
Described (001) face is the face of A, B, C, 4 formation of D;
Polished finish condition: adopt (001) face of 150#, 360#, 500#, 1000#, 2000# silicon carbide paper polishing test block, on polishing machine, carry out polished finish then;
The surface corrosion treatment condition: the test block after will polishing is taken out after adopting etching reagent surface treatment 2～10min, promptly gets Ni 3Al based single-crystal high-temperature alloy seed crystal;
Described etching reagent is nitric acid HNO 3, hydrofluoric acid HF and glycerine C 3H 8O 3Form, and add 10～50ml hydrofluoric acid and 40～100ml glycerine in every 10ml nitric acid;
Perhaps described etching reagent is by hydrochloric acid HCl and hydrogen peroxide H 2O 2Form, and add 5～30ml hydrogen peroxide in every 10ml hydrochloric acid;
Described Ni 3Al based single-crystal high-temperature alloy body is Ni-(5～20) Mo-(6～10) Al-(0～a 0.1) B material;
Second step, preparation part wax-pattern;
Wax material is melted the back inject component die under 40～120 ℃ temperature condition, and compression moulding under 0.5～10MPa pressure, make part wax-pattern 2;
Described wax material is the wax material of the П BK Б trade mark, the wax material of the OH-1 trade mark, the wax material of the OH-2 trade mark, the wax material of the OH-3 trade mark, the wax material of the OH-4 trade mark, the wax material of the P-3 trade mark, the wax material of the B-1 trade mark or the wax material of the П C50-50 trade mark;
In the present invention, the component die shape is relevant with the required part shape that makes.
Referring to shown in Figure 4, the 3rd step is with the Ni that makes in the above-mentioned the first step 3(001) of Al based single-crystal high-temperature alloy seed crystal 1 extends in the part wax-pattern 2 that makes in above-mentioned second step towards the upper edge, and Ni 3Al based single-crystal high-temperature alloy seed crystal 1 stretches into part wax-pattern 2 0.5～10mm;
Then at Ni 3The outside of Al based single-crystal high-temperature alloy seed crystal 1 and part wax-pattern 2 is coated with and hangs the thick ceramic fire resistant slurry of 3～20mm, dewaxes under 120～500 ℃ of temperature then, is making the ceramic shell mould that has seed crystal behind roast 5～15h under 800～1700 ℃ of temperature;
The 4th step, the ceramic shell mould that makes in above-mentioned the 3rd step is put into single crystal growing furnace, temperature to 1400 in the adjusting single crystal growing furnace～1950 ℃, Ni-(5～20) Mo-(6～10) Al-(0～0.1) B molten metal flows in the ceramic shell moulds by sprue gate 3, behind insulation wait 2～30min; Speed with 0.1～15mm/min moves down crystal pulling, after crystal pulling finishes, takes out after cooling to room temperature with the furnace, promptly make to have＜001〉orientation and good solidified structure Ni 3Al based single-crystal high-temperature alloy material.The temperature of molten metal is 1400～1800 ℃.
In order to prepare the Ni of different orientation 3The Al based single-crystal high-temperature alloy, in the first step of the present invention, can be at Ni 3On the Al based single-crystal high-temperature alloy body orientation cut out have＜011〉orientation or＜111〉orientation test block, adopt method same as described above preparation＜011 then〉Ni of orientation and good solidified structure 3Al based single-crystal high-temperature alloy material, perhaps＜111〉Ni of orientation and good solidified structure 3Al based single-crystal high-temperature alloy material.
Preparation＜011〉orientation and the good Ni of solidified structure 3The step of Al based single-crystal high-temperature alloy material is:
The first step, preparation Ni 3The seed crystal of Al based single-crystal high-temperature alloy;
Referring to shown in Figure 2, at Ni 3Orientation cuts out and has＜011〉orientation test block on the Al based single-crystal high-temperature alloy body, and (011) face of test block is carried out polished finish and surface corrosion is handled, and obtains Ni 3Al based single-crystal high-temperature alloy seed crystal;
Described (011) face is the face of C, D, E, 4 formation of F;
Polished finish condition: adopt (011) face of 150#, 360#, 500#, 1000#, 2000# silicon carbide paper polishing test block, on polishing machine, carry out polished finish then;
The surface corrosion treatment condition: the test block after will polishing is taken out after adopting etching reagent surface treatment 2～10min, promptly gets Ni 3Al based single-crystal high-temperature alloy seed crystal;
Described etching reagent is that nitric acid, hydrofluoric acid and glycerine are formed, and adds 10～50ml hydrofluoric acid and 40～100ml glycerine in every 10ml nitric acid;
Perhaps described etching reagent is made up of hydrochloric acid and hydrogen peroxide, and adds 5～30ml hydrogen peroxide in every 10ml hydrochloric acid;
Described Ni 3Al based single-crystal high-temperature alloy body is Ni-(5～20) Mo-(6～10) Al-(0～a 0.1) B material;
Second step, preparation part wax-pattern;
Wax material is melted the back inject component die under 40～120 ℃ temperature condition, and compression moulding under 0.5～10MPa pressure, make part wax-pattern 2;
Described wax material is the wax material of the П BK Б trade mark, the wax material of the OH-1 trade mark, the wax material of the OH-2 trade mark, the wax material of the OH-3 trade mark, the wax material of the OH-4 trade mark, the wax material of the P-3 trade mark, the wax material of the B-1 trade mark or the wax material of the П C50-50 trade mark;
Referring to shown in Figure 4, the 3rd step is with the Ni that makes in the above-mentioned the first step 3(011) of Al based single-crystal high-temperature alloy seed crystal 1 extends in the part wax-pattern 2 that makes in above-mentioned second step towards the upper edge, and Ni 3Al based single-crystal high-temperature alloy seed crystal 1 stretches into part wax-pattern 2 0.5～10mm;
Then at Ni 3The outside of Al based single-crystal high-temperature alloy seed crystal 1 and part wax-pattern 2 is coated with and hangs the thick ceramic fire resistant slurry of 3～20mm, dewaxes under 120～500 ℃ of temperature, is making the ceramic shell mould that has seed crystal behind roast 5～15h under 800～1700 ℃ of temperature;
The 4th step, the ceramic shell mould that makes in above-mentioned the 3rd step is put into single crystal growing furnace, temperature to 1400 in the adjusting single crystal growing furnace～1950 ℃, Ni-(5～20) Mo-(6～10) Al-(0～0.1) B molten metal flows in the ceramic shell moulds by sprue gate 3, behind insulation wait 2～30min; Speed with 0.1～15mm/min moves down crystal pulling, after crystal pulling finishes, takes out after cooling to room temperature with the furnace, promptly make to have＜011〉orientation and good solidified structure Ni 3Al based single-crystal high-temperature alloy material.The temperature of molten metal is 1400～1800 ℃.
Preparation＜111〉orientation and the good Ni of solidified structure 3The step of Al based single-crystal high-temperature alloy material is:
The first step, preparation Ni 3The seed crystal of Al based single-crystal high-temperature alloy;
Referring to shown in Figure 3, at Ni 3Orientation cuts out and has＜111〉orientation test block on the Al based single-crystal high-temperature alloy body, and (111) face of test block is carried out polished finish and surface corrosion is handled, and obtains Ni 3Al based single-crystal high-temperature alloy seed crystal;
Described (111) face is the face of C, D, E, 4 formation of F;
Polished finish condition: adopt (111) face of 150#, 360#, 500#, 1000#, 2000# silicon carbide paper polishing test block, on polishing machine, carry out polished finish then;
The surface corrosion treatment condition: the test block after will polishing is taken out after adopting etching reagent surface treatment 2～10min, promptly gets Ni 3Al based single-crystal high-temperature alloy seed crystal;
Described etching reagent is that nitric acid, hydrofluoric acid and glycerine are formed, and adds 10～50ml hydrofluoric acid and 40～100ml glycerine in every 10ml nitric acid;
Perhaps described etching reagent is made up of hydrochloric acid and hydrogen peroxide, and adds 5～30ml hydrogen peroxide in every 10ml hydrochloric acid;
Described Ni 3Al based single-crystal high-temperature alloy body is Ni-(5～20) Mo-(6～10) Al-(0～a 0.1) B material;
Second step, preparation part wax-pattern;
Wax material is melted the back inject component die under 40～120 ℃ temperature condition, and compression moulding under 0.5～10MPa pressure, make part wax-pattern 2;
Described wax material is the wax material of the П BK Б trade mark, the wax material of the OH-1 trade mark, the wax material of the OH-2 trade mark, the wax material of the OH-3 trade mark, the wax material of the OH-4 trade mark, the wax material of the P-3 trade mark, the wax material of the B-1 trade mark or the wax material of the П C50-50 trade mark;
Referring to shown in Figure 4, the 3rd step is with the Ni that makes in the above-mentioned the first step 3(111) of Al based single-crystal high-temperature alloy seed crystal 1 extend in the part wax-pattern 2 that makes in above-mentioned second step towards the upper edge, and Ni 3Al based single-crystal high-temperature alloy seed crystal 1 stretches into part wax-pattern 2 0.5～10mm;
Then at Ni 3The outside of Al based single-crystal high-temperature alloy seed crystal 1 and part wax-pattern 2 is coated with and hangs the thick ceramic fire resistant slurry of 3～20mm, dewaxes under 120～500 ℃ of temperature, is making the ceramic shell mould that has seed crystal behind roast 5～15h under 800～1700 ℃ of temperature;
The 4th step, the ceramic shell mould that makes in above-mentioned the 3rd step is put into single crystal growing furnace, temperature to 1400 in the adjusting single crystal growing furnace～1950 ℃, Ni-(5～20) Mo-(6～10) Al-(0～0.1) B molten metal flows in the ceramic shell moulds by sprue gate 3, behind insulation wait 2～30min; Speed with 0.1～15mm/min moves down crystal pulling, after crystal pulling finishes, takes out after cooling to room temperature with the furnace, promptly make to have＜111〉orientation and good solidified structure Ni 3Al based single-crystal high-temperature alloy material.The temperature of molten metal is 1400～1800 ℃.
Embodiment 1:
Preparation has＜001〉orientation and the step of the Ni-14Mo-7.8Al single crystal high-temperature alloy material of good solidified structure be:
The first step, the seed crystal of preparation Ni-14Mo-7.8Al single crystal super alloy;
Referring to shown in Figure 1, orientation cuts out and has＜001〉orientation test block on Ni-14Mo-7.8Al single crystal super alloy body, and (001) face of test block is carried out polished finish and surface corrosion is handled, and obtains Ni-14Mo-7.8Al single crystal super alloy seed crystal;
Described (001) face is the face of A, B, C, 4 formation of D;
The polished finish condition: adopt (001) face of 150#, 360#, 500#, 1000#, 2000# silicon carbide paper polishing test block, (precision instrumentation company limited in Shanghai carries out polished finish on PG-1A) at polishing machine then;
The surface corrosion treatment condition: the test block after will polishing is taken out after adopting etching reagent surface treatment 5min, promptly gets Ni-14Mo-7.8Al single crystal super alloy seed crystal;
Described etching reagent is that nitric acid, hydrofluoric acid and glycerine are formed, and adds 30ml hydrofluoric acid and 50ml glycerine in every 10ml nitric acid;
Second step, preparation part wax-pattern;
Wax material is melted the back inject component die under 75 ℃ temperature condition, and compression moulding under 0.5MPa pressure, make part wax-pattern 2; Described wax material is the wax material of the П BK Б trade mark;
Referring to shown in Figure 4, the 3rd step, (001) of the Ni-14Mo-7.8Al single crystal super alloy seed crystal 1 that makes in the above-mentioned the first step is extended in the part wax-pattern 2 that makes in above-mentioned second step towards the upper edge, and Ni-14Mo-7.8Al single crystal super alloy seed crystal 1 stretches into part wax-pattern 2 5mm is arranged;
Be coated with in the outside of Ni-14Mo-7.8Al single crystal super alloy seed crystal 1 and part wax-pattern 2 then and hang the thick ceramic fire resistant slurry of 10mm, under 140 ℃ of temperature, dewax, making the ceramic shell mould that has seed crystal behind the roast 10h under 1000 ℃ of temperature;
The 4th step, the ceramic shell mould that makes in above-mentioned the 3rd step is put into single crystal growing furnace (German DZG-0.025 N-type waferN growth furnace), regulate in the single crystal growing furnace temperature to 1580 ℃, Ni-14Mo-7.8Al molten metal (temperature of this molten metal is 1400 ℃) flows in the ceramic shell mould by sprue gate 3, after 2min is waited in insulation; Speed with 3mm/min moves down crystal pulling, after crystal pulling finishes, takes out after cooling to 20 ℃ with the furnace, promptly make＜001〉orientation and the good Ni-14Mo-7.8Al single crystal high-temperature alloy material of solidified structure.
It is＜001〉direction that the Ni-14Mo-7.8Al single crystal high-temperature alloy material employing X ray back scattering Laue method of above-mentioned preparation is measured crystalline orientation.
Adopt the Olympus metaloscope that the microtexture of Ni-14Mo-7.8Al seed crystal is observed, its metallograph is shown in Fig. 5 A; Adopt the Olympus metaloscope that the microtexture of the Ni-14Mo-7.8Al single crystal super alloy that makes through the inventive method is observed, its metallograph is shown in Fig. 5 B.By the photo contrast to Fig. 5 A and Fig. 5 B, its microtexture pattern is identical, and visible primary dendritic spacing is identical, and the secondary dendrite pattern is identical, so have good solidified structure.
Adopt the above-mentioned second identical step to the 5th step, to have＜011〉orientation,＜111〉orientation Ni-14Mo-7.8Al single crystal super alloy seed crystal is prepared, the Ni-14Mo-7.8Al single crystal super alloy that makes measures crystalline orientation through X ray back scattering Laue method and is respectively＜011〉orientation,＜111〉orientation.
Embodiment 2:
Preparation has＜011〉orientation and the step of the Ni-14Mo-7.8Al-0.05B single crystal high-temperature alloy material of good solidified structure be:
The first step, the seed crystal of preparation Ni-14Mo-7.8Al-0.05B single crystal super alloy;
Referring to shown in Figure 2, on Ni-14Mo-7.8Al-0.05B single crystal super alloy body orientation cut out have＜011 the orientation test block, and (011) face of test block carried out polished finish and surface corrosion is handled, obtain Ni-14Mo-7.8Al-0.05B single crystal super alloy seed crystal;
Described (011) face is the face of A, B, C, 4 formation of D;
The polished finish condition: adopt (011) face of 150#, 360#, 500#, 1000#, 2000# silicon carbide paper polishing test block, (precision instrumentation company limited in Shanghai carries out polished finish on PG-1A) at polishing machine then;
The surface corrosion treatment condition: the test block after will polishing is taken out after adopting etching reagent surface treatment 2min, promptly gets Ni-14Mo-7.8Al-0.05B single crystal super alloy seed crystal;
Described etching reagent is that nitric acid, hydrofluoric acid and glycerine are formed, and adds 30ml hydrofluoric acid and 60ml glycerine in every 10mi nitric acid;
Second step, preparation part wax-pattern;
Wax material is melted the back inject component die under 100 ℃ temperature condition, and compression moulding under 0.5MPa pressure, make part wax-pattern 2; Described wax material is the wax material of the P-3 trade mark;
Referring to shown in Figure 4, the 3rd step, (011) of the Ni-14Mo-7.8Al-0.05B single crystal super alloy seed crystal 1 that makes in the above-mentioned the first step is extended in the part wax-pattern 2 that makes in above-mentioned second step towards the upper edge, and Ni-14Mo-7.8Al-0.05B single crystal super alloy seed crystal 1 stretches into part wax-pattern 2 10mm is arranged;
Be coated with in the outside of Ni-14Mo-7.8Al-0.05B single crystal super alloy seed crystal 1 and part wax-pattern 2 then and hang the thick ceramic fire resistant slurry of 20mm, under 250 ℃ of temperature, dewax then, making the ceramic shell mould that has seed crystal behind the roast 12h under 1300 ℃ of temperature;
The 4th step, the ceramic shell mould that makes in above-mentioned the 3rd step is put into single crystal growing furnace (German DZG-0.025 N-type waferN growth furnace), regulate in the single crystal growing furnace temperature to 1800 ℃, Ni-14Mo-7.8Al-0.05B molten metal (temperature of this molten metal is 1800 ℃) flows in the ceramic shell mould by sprue gate 3, after 10min is waited in insulation; Speed with 15mm/min moves down crystal pulling, after crystal pulling finishes, takes out after cooling to 20 ℃ with the furnace, promptly make＜011〉orientation and the good Ni-14Mo-7.8Al-0.05B single crystal high-temperature alloy material of solidified structure.
It is＜011〉direction that the Ni-14Mo-7.8Al-0.05B single crystal high-temperature alloy material employing X ray back scattering Laue method of above-mentioned preparation is measured crystalline orientation.
Adopt the Olympus metaloscope that the microtexture of Ni-14Mo-7.8Al-0.05B seed crystal is observed, adopt the Olympus metaloscope that the microtexture of the Ni-14Mo-7.8Al-0.05B single crystal super alloy that makes through the inventive method is observed, both microtexture patterns are identical, as seen primary dendritic spacing is identical, the secondary dendrite pattern is identical, so have good solidified structure.
Adopt the above-mentioned second identical step to the 5th step, to have＜001〉orientation,＜111〉orientation Ni-14Mo-7.8Al-0.05B single crystal super alloy seed crystal is prepared, the Ni-14Mo-7.8Al-0.05B single crystal super alloy that makes measures crystalline orientation through X ray back scattering Laue method and is respectively＜001〉orientation,＜111〉orientation.
Embodiment 3:
Preparation has＜111〉orientation and the step of the Ni-14Mo-7.8Al-0.02B single crystal high-temperature alloy material of good solidified structure be:
The first step, the seed crystal of preparation Ni-14Mo-7.8Al-0.02B single crystal super alloy;
Referring to shown in Figure 3, on Ni-14Mo-7.8Al-0.02B single crystal super alloy body orientation cut out have＜111 the orientation test block, and (111) face of test block carried out polished finish and surface corrosion is handled, obtain Ni-14Mo-7.8Al-0.02B single crystal super alloy seed crystal;
Described (111) face is the face of A, B, C, 4 formation of D;
The polished finish condition: adopt (111) face of 150#, 360#, 500#, 1000#, 2000# silicon carbide paper polishing test block, (precision instrumentation company limited in Shanghai carries out polished finish on PG-1A) at polishing machine then;
The surface corrosion treatment condition: the test block after will polishing is taken out after adopting etching reagent surface treatment 10min, promptly gets Ni-14Mo-7.8Al-0.02B single crystal super alloy seed crystal;
Described etching reagent is that hydrochloric acid and hydrogen peroxide are formed, and adds the 10ml hydrogen peroxide in every 10ml hydrochloric acid;
Second step, preparation part wax-pattern;
Wax material is melted the back inject component die under 75 ℃ temperature condition, and compression moulding under 0.5MPa pressure, make part wax-pattern 2; Described wax material is the wax material of the OH-1 trade mark;
Referring to shown in Figure 4, the 3rd step, (111) of the Ni-14Mo-7.8Al-0.02B single crystal super alloy seed crystal 1 that makes in the above-mentioned the first step are extended in the part wax-pattern 2 that makes in above-mentioned second step towards the upper edge, and Ni-14Mo-7.8Al-0.02B single crystal super alloy seed crystal 1 stretches into part wax-pattern 2 0.5mm is arranged;
Be coated with in the outside of Ni-14Mo-7.8Al-0.02B single crystal super alloy seed crystal 1 and part wax-pattern 3 then and hang the thick ceramic fire resistant slurry of 5mm, under 300 ℃ of temperature, dewax, making the ceramic shell mould that has seed crystal behind the roast 5h under 1700 ℃ of temperature;
The 4th step, the ceramic shell mould that makes in above-mentioned the 3rd step is put into single crystal growing furnace (German DZG-0.025 N-type waferN growth furnace), regulate in the single crystal growing furnace temperature to 1700 ℃, Ni-14Mo-7.8Al-0.02B molten metal (temperature of this molten metal is 1600 ℃) flows in the ceramic shell mould by sprue gate 3, after 5min is waited in insulation; Speed with 4mm/min moves down crystal pulling, after crystal pulling finishes, takes out after cooling to 20 ℃ with the furnace, promptly make＜111〉orientation and the good Ni-14Mo-7.8Al-0.02B single crystal high-temperature alloy material of solidified structure.
It is＜111〉direction that the Ni-14Mo-7.8Al-0.02B single crystal high-temperature alloy material employing X ray back scattering Laue method of above-mentioned preparation is measured crystalline orientation.
Adopt the Olympus metaloscope that the microtexture of Ni-14Mo-7.8Al-0.02B seed crystal is observed, adopt the Olympus metaloscope that the microtexture of the Ni-14Mo-7.8Al-0.02B single crystal super alloy that makes through the inventive method is observed, both microtexture patterns are identical, as seen primary dendritic spacing is identical, the secondary dendrite pattern is identical, so have good solidified structure.
Adopt the above-mentioned second identical step to the 5th step, to have＜001〉orientation,＜011〉orientation Ni-14Mo-7.8Al-0.02B single crystal super alloy seed crystal is prepared, the Ni-14Mo-7.8Al-0.02B single crystal super alloy that makes measures crystalline orientation through X ray back scattering Laue method and is respectively＜001〉orientation,＜011〉orientation.
The present invention adopts the seed crystal legal system to be equipped with Ni 3Al based single-crystal high-temperature alloy material not only can obtain high monocrystalline success ratio, can also guarantee the controllability of crystalline orientation and solidified structure simultaneously, makes it have good performance, effectively reduces the manufacturing cost of aircraft engine.Therefore, the technology that adopts the seed crystal legal system to be equipped with the monocrystalline high-temperature structural material can further satisfy the requirement that the aero gas turbine engine machine develops to high thrust-weight ratio, low-cost direction.

Claims (7)

1, a kind of Ni 3The Al based single-crystal high-temperature alloy adopts the method for seed crystal preparation, it is characterized in that including the following step:
The first step, preparation Ni 3The seed crystal of Al based single-crystal high-temperature alloy;
At Ni 3Orientation cuts out the test block with certain crystalline orientation on the Al based single-crystal high-temperature alloy body, and the crystal face of test block is carried out polished finish and surface corrosion processing, obtains Ni 3Al based single-crystal high-temperature alloy seed crystal;
Polished finish condition: adopt the crystal face of 150#, 360#, 500#, 1000#, 2000# silicon carbide paper polishing test block, on polishing machine, carry out polished finish then;
The surface corrosion treatment condition: the test block after will polishing is taken out after adopting etching reagent surface treatment 2～10min, promptly gets Ni 3Al based single-crystal high-temperature alloy seed crystal;
Second step, preparation part wax-pattern;
Wax material is melted the back inject component die under 40～120 ℃ temperature condition, and compression moulding under 0.5～10MPa pressure, make part wax-pattern ℃ 2);
The 3rd step is with the Ni that makes in the above-mentioned the first step 3The crystal face of Al based single-crystal high-temperature alloy seed crystal (1) extends in the part wax-pattern (2) that makes in above-mentioned second step to the upper edge, and Ni 3Al based single-crystal high-temperature alloy seed crystal (1) stretches into part wax-pattern (2) 0.5～10mm;
Then at Ni 3The outside of Al based single-crystal high-temperature alloy seed crystal (1) and part wax-pattern (2) is coated with and hangs the thick ceramic fire resistant slurry of 3～20mm; Under 120～500 ℃ of temperature, dewax, making the ceramic shell mould that has seed crystal behind roast 5～15h under 800～1700 ℃ of temperature;
The 4th step, the ceramic shell mould that makes in above-mentioned the 3rd step is put into single crystal growing furnace, temperature to 1400 in the adjusting single crystal growing furnace～1950 ℃, molten metal flows in the ceramic shell mould by sprue gate (3), behind insulation wait 2～30min; Speed with 0.1～15mm/min moves down crystal pulling, after crystal pulling finishes, takes out after cooling to room temperature with the furnace, promptly makes and Ni 3The make peace Ni of good solidified structure of Al based single-crystal high-temperature alloy seed crystal orientation one 3Al based single-crystal high-temperature alloy material; The temperature of described molten metal is 1400～1800 ℃.
2, Ni according to claim 1 3The Al based single-crystal high-temperature alloy adopts the method for seed crystal preparation, it is characterized in that:
Ni described in the first step 3Al based single-crystal high-temperature alloy body is Ni-(5～20) Mo-(6～10) Al-(0～a 0.1) B material.
3, Ni according to claim 1 3The Al based single-crystal high-temperature alloy adopts the method for seed crystal preparation, it is characterized in that:
The described Ni that the 4th step made 3The Al based single-crystal high-temperature alloy is Ni-14Mo-7.8Al single crystal super alloy, Ni-14Mo-7.8Al-0.05B single crystal super alloy or Ni-14Mo-7.8Al-0.02B single crystal super alloy.
4, Ni according to claim 1 3The Al based single-crystal high-temperature alloy adopts the method for seed crystal preparation, it is characterized in that:
Described wax material in second step is the wax material of the ∏ BK Б trade mark, the wax material of the OH-1 trade mark, the wax material of the OH-2 trade mark, the wax material of the OH-3 trade mark, the wax material of the OH-4 trade mark, the wax material of the P-3 trade mark, the wax material of the B-1 trade mark or the wax material of the ∏ C50-50 trade mark.
5, Ni according to claim 1 3The Al based single-crystal high-temperature alloy adopts the method for seed crystal preparation, it is characterized in that:
Etching reagent described in the first step is that nitric acid, hydrofluoric acid and glycerine are formed, and adds 10～50ml hydrofluoric acid and 40～100ml glycerine in every 10ml nitric acid.
6, Ni according to claim 1 3The Al based single-crystal high-temperature alloy adopts the method for seed crystal preparation, it is characterized in that:
Etching reagent described in the first step is made up of hydrochloric acid and hydrogen peroxide, and adds 5～30ml hydrogen peroxide in every 10ml hydrochloric acid.
7, Ni according to claim 1 3The Al based single-crystal high-temperature alloy adopts the method for seed crystal preparation, it is characterized in that:
The Ni that the 4th step made 3Al based single-crystal high-temperature alloy and Ni 3The primary dendritic spacing of Al based single-crystal high-temperature alloy seed crystal is identical, and the secondary dendrite pattern is identical.
CN200710179684A 2007-12-17 2007-12-17 Method for preparing Ni3Al based single-crystal high-temperature alloy by employing seed crystal Expired - Fee Related CN100587134C (en)

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