CN101255607A - Method for preparing Ni3Al-based single-crystal refractory alloy by employing combination of seed crystal method and screw selecting method - Google Patents
Method for preparing Ni3Al-based single-crystal refractory alloy by employing combination of seed crystal method and screw selecting method Download PDFInfo
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- CN101255607A CN101255607A CNA200710179687XA CN200710179687A CN101255607A CN 101255607 A CN101255607 A CN 101255607A CN A200710179687X A CNA200710179687X A CN A200710179687XA CN 200710179687 A CN200710179687 A CN 200710179687A CN 101255607 A CN101255607 A CN 101255607A
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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 and the spiral crystal selection 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 one side of a wax pattern of a spiral crystal selector; the other side of the wax pattern of the spiral crystal selector is connected with a parts wax pattern; and ceramics castable refractory is smeared on the outside of the crystallon, the wax pattern of the spiral crystal selector 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
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 a kind ofly to adopt the combination of seed crystal method and two kinds of technologies of spiral crystal separation method to be prepared 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 spiral crystal separation method is meant that the superseded gradually crystal grain of the coupling of the preferential growth under unidirectional heat-flux conditions by spiral type crystal growth passage and crystal grain prepares the method for single crystal.
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.
The processing method of making the single crystal super alloy blade now in the aircraft industry mainly is the spiral crystal separation method, its monocrystalline success ratio height, but crystal separation method can not be controlled the crystalline orientation and the solidified structure of single crystal super alloy, and mainly is crystalline orientation and solidified structure to the influence factor of monocrystalline mechanical property.Though the seed crystal method can effectively be controlled the crystalline orientation and the solidified structure of monocrystalline, its monocrystalline success ratio is extremely low.
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 method and spiral crystal separation method combined preparation, and this compositions, process is by means of accurate control and the spiral crystal separation method high monocrystalline success ratio of seed crystal method to crystalline orientation and solidified structure, and makes up 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; By two kinds of combinations that prepare single crystal high-temperature alloy material technology, thus the good single crystal high-temperature alloy material of obtained performance.
The present invention is a kind of employing seed crystal method and spiral crystal separation method combined preparation Ni
3The method of Al based single-crystal high-temperature alloy, this combination process 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
3Al based single-crystal high-temperature alloy seed crystal;
Second step, preparation spiral crystal selector wax-pattern;
Wax material is melted the back inject spiral crystal selector mould under 40～120 ℃ temperature condition, and compression moulding under 0.5～10MPa pressure, make spiral crystal selector wax-pattern;
The 3rd 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 the part wax-pattern;
The 4th 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 spiral crystal selector 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 spiral crystal selector wax-pattern 2 0.5～10mm; The upper ends part wax-pattern 3 of spiral crystal selector wax-pattern 2;
At Ni
3The outside of Al based single-crystal high-temperature alloy seed crystal 1, spiral crystal selector wax-pattern 2 and part wax-pattern 3 is coated with and hangs the thick ceramic fire resistant slurry of 3～20mm, under 120～500 ℃ of temperature, dewax then, making the ceramic shell mould that has seed crystal behind roast 5～15h under 800～1700 ℃ of temperature;
The 5th 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 4, 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 employing seed crystal method and spiral crystal separation method combined preparation Ni
3The method of Al based single-crystal high-temperature alloy, this combination process 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 by hydrochloric acid HCl and hydrogen peroxide H
2O
2Form, and add 5～30ml hydrogen peroxide in every 10ml hydrochloric acid;
Described Ni
3The Al based single-crystal high-temperature alloy is Ni-(5～20) Mo-(6～10) Al-(0～0.1) B;
Second step, preparation spiral crystal selector wax-pattern;
Wax material is melted the back inject spiral crystal selector mould under 40～120 ℃ temperature condition, and compression moulding under 0.5～10MPa pressure, make spiral crystal selector wax-pattern;
Described wax material is the wax material of the π BKB 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 π C50-50 trade mark;
The 3rd 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 the part wax-pattern;
Described wax material is the wax material of the π BKB 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 π C50-50 trade mark;
Second step is relevant with the required part shape that makes with described mould (spiral crystal selector mould, component die) shape during the 3rd goes on foot.
Referring to shown in Figure 4, the 4th 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 spiral crystal selector 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 spiral crystal selector wax-pattern 2 0.5～10mm; The upper ends part wax-pattern 3 of spiral crystal selector wax-pattern 2;
At Ni
3The outside of Al based single-crystal high-temperature alloy seed crystal 1, spiral crystal selector wax-pattern 2 and part wax-pattern 3 is coated with and hangs the thick ceramic fire resistant slurry of 3～20mm, under 120～500 ℃ of temperature, dewax then, making the ceramic shell mould that has seed crystal behind roast 5～15h under 800～1700 ℃ of temperature;
The 5th 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 4, 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 form, and add 5～30ml hydrogen peroxide in every 10ml hydrochloric acid by hydrochloric acid and hydrogen peroxide;
Second step, preparation spiral crystal selector wax-pattern;
Wax material is melted the back inject spiral crystal selector mould under 40～120 ℃ temperature condition, and compression moulding under 0.5～10MPa pressure, make spiral crystal selector wax-pattern;
Described wax material is the wax material of the π BKB 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 π C50-50 trade mark;
The 3rd 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 the part wax-pattern;
Described wax material is the wax material of the π BKB 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 π C50-50 trade mark;
Referring to shown in Figure 4, the 4th 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 spiral crystal selector 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 spiral crystal selector wax-pattern 2 0.5～10mm; The upper ends part wax-pattern 3 of spiral crystal selector wax-pattern 2;
The wax material of described part wax-pattern 3 is the wax material of the π BKB 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 π C50-50 trade mark;
At Ni
3The outside of Al based single-crystal high-temperature alloy seed crystal 1, spiral crystal selector wax-pattern 2 and sample wax-pattern 3 is coated with and hangs the thick ceramic fire resistant slurry of 3～20mm, under 120～500 ℃ of temperature, dewax then, making the ceramic shell mould that has seed crystal behind roast 5～15h under 800～1700 ℃ of temperature;
The 5th 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 4, 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 form, and add 5～30ml hydrogen peroxide in every 10ml hydrochloric acid by hydrochloric acid and hydrogen peroxide;
Second step, preparation spiral crystal selector wax-pattern;
Wax material is melted the back inject spiral crystal selector mould under 40～120 ℃ temperature condition, and compression moulding under 0.5～10MPa pressure, make spiral crystal selector wax-pattern;
Described wax material is the wax material of the π BKB 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 π C50-50 trade mark;
The 3rd 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 the part wax-pattern;
Described wax material is the wax material of the π BKB 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 π C50-50 trade mark;
Referring to shown in Figure 4, the 4th 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 spiral crystal selector 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 spiral crystal selector wax-pattern 2 0.5～10mm; The upper ends sample wax-pattern 3 of spiral crystal selector wax-pattern 2;
The wax material of described sample wax-pattern 3 is the wax material of the π BKB 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 π C50-50 trade mark;
At Ni
3The outside of Al based single-crystal high-temperature alloy seed crystal 1, spiral crystal selector wax-pattern 2 and sample wax-pattern 3 is coated with and hangs the thick ceramic fire resistant slurry of 3～20mm, under 120～500 ℃ of temperature, dewax then, making the ceramic shell mould that has seed crystal behind roast 5～15h under 800～1700 ℃ of temperature;
The 5th 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 4, 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 spiral crystal selector wax-pattern;
Wax material is melted the back inject spiral crystal selector mould under 75 ℃ temperature condition, and compression moulding under 0.5MPa pressure, make spiral crystal selector wax-pattern;
Described wax material is the wax material of the π BKB trade mark;
The 3rd 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 the part wax-pattern;
Described wax material is the wax material of the π BKB trade mark;
Referring to shown in Figure 4, the 4th 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 spiral crystal selector 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 spiral crystal selector wax-pattern 2 5mm is arranged; The upper ends sample wax-pattern 3 of spiral crystal selector wax-pattern 2;
The wax material of described sample wax-pattern 3 is wax materials of the π BKB trade mark;
Be coated with the thick ceramic fire resistant slurry of extension 10mm in the outside of Ni-14Mo-7.8Al single crystal super alloy seed crystal 1, spiral crystal selector wax-pattern 2 and sample wax-pattern 3, under 140 ℃ of temperature, dewax then, making the ceramic shell mould that has seed crystal behind the roast 10h under 1000 ℃ of temperature;
The 5th 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 4, 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-13.5Mo-7.6Al-0.04B single crystal high-temperature alloy material of good solidified structure be:
The first step, the seed crystal of preparation Ni-13.5Mo-7.6Al-0.04B single crystal super alloy;
Referring to shown in Figure 2, on Ni-13.5Mo-7.6Al-0.04B 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-13.5Mo-7.6Al-0.04B 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-13.5Mo-7.6Al-0.04B 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 10ml nitric acid;
Second step, preparation spiral crystal selector wax-pattern;
Wax material is melted the back inject spiral crystal selector mould under 80 ℃ temperature condition, and compression moulding under 3MPa pressure, make spiral crystal selector wax-pattern;
Described wax material is the wax material of the OH-4 trade mark;
The 3rd 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 the part wax-pattern;
Described wax material is the wax material of the P-3 trade mark;
Referring to shown in Figure 4, the 4th step, (011) of the Ni-13.5Mo-7.6Al-0.04B single crystal super alloy seed crystal 1 that makes in the above-mentioned the first step is extended in the spiral crystal selector wax-pattern 2 that makes in above-mentioned second step towards the upper edge, and Ni-13.5Mo-7.6Al-0.04B single crystal super alloy seed crystal 1 stretches into spiral crystal selector wax-pattern 2 10mm is arranged; The upper ends sample wax-pattern 3 of spiral crystal selector wax-pattern 2;
The wax material of the wax material OH-4 trade mark of described sample wax-pattern 3;
Be coated with the thick ceramic fire resistant slurry of extension 20mm in the outside of Ni-13.5Mo-7.6Al-0.04B single crystal super alloy seed crystal 1, spiral crystal selector wax-pattern 2 and sample wax-pattern 3, under 250 ℃ of temperature, dewax then, making the ceramic shell mould that has seed crystal behind the roast 12h under 1300 ℃ of temperature;
The 5th 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-13.5Mo-7.6Al-0.04B molten metal (temperature of this molten metal is 1800 ℃) flows in the ceramic shell mould by sprue gate 4, 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-13.5Mo-7.6Al-0.04B single crystal high-temperature alloy material of solidified structure.
It is＜011〉direction that the Ni-13.5Mo-7.6Al-0.04B 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-13.5Mo-7.6Al-0.04B seed crystal is observed, adopt the Olympus metaloscope that the microtexture of the Ni-13.5Mo-7.6Al-0.04B 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-13.5Mo-7.6Al-0.04B single crystal super alloy seed crystal is prepared, the Ni-13.5Mo-7.6Al-0.04B 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 spiral crystal selector wax-pattern;
Wax material is melted the back inject spiral crystal selector mould under 120 ℃ temperature condition, and compression moulding under 10MPa pressure, make spiral crystal selector wax-pattern;
Described wax material is the wax material of the P-3 trade mark;
The 3rd 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 the part wax-pattern;
Described wax material is the wax material of the OH-1 trade mark;
Referring to shown in Figure 4, the 4th 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 spiral crystal selector 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 spiral crystal selector wax-pattern 2 0.5mm is arranged; The upper ends part wax-pattern 3 of spiral crystal selector wax-pattern 2;
The wax material of the wax material P-3 trade mark of described part wax-pattern 3;
Be coated with the thick ceramic fire resistant slurry of extension 5mm in the outside of Ni-14Mo-7.8Al-0.02B single crystal super alloy seed crystal 1, spiral crystal selector wax-pattern 2 and part wax-pattern 3, under 300 ℃ of temperature, dewax then, making the ceramic shell mould that has seed crystal behind the roast 5h under 1700 ℃ of temperature;
The 5th 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 4, 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 combination process of seed crystal method and spiral crystal separation method to prepare 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, adopt the technology of seed crystal method and spiral crystal separation method combined preparation 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 (8)
1, a kind of employing seed crystal method and spiral crystal separation method combined preparation Ni
3The method of Al based single-crystal high-temperature alloy 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 spiral crystal selector wax-pattern;
Wax material is melted the back inject spiral crystal selector mould under 40～120 ℃ temperature condition, and compression moulding under 0.5～10MPa pressure, make spiral crystal selector wax-pattern;
The 3rd 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 the part wax-pattern;
The 4th 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 spiral crystal selector 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 spiral crystal selector wax-pattern 2 0.5～10mm; The upper ends part wax-pattern 3 of spiral crystal selector wax-pattern 2;
At Ni
3The outside of Al based single-crystal high-temperature alloy seed crystal 1, spiral crystal selector wax-pattern 2 and part wax-pattern 3 is coated with and hangs the thick ceramic fire resistant slurry of 3～20mm, under 120～500 ℃ of temperature, dewax then, making the ceramic shell mould that has seed crystal behind roast 5～15h under 800～1700 ℃ of temperature;
The 5th 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 4, 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, employing seed crystal method according to claim 1 and spiral crystal separation method combined preparation Ni
3The method of Al based single-crystal high-temperature alloy is characterized in that: described Ni
3The Al based single-crystal high-temperature alloy is Ni-(5～20) Mo-(6～10) Al-(0～0.1) B.
3, employing seed crystal method according to claim 1 and spiral crystal separation method combined preparation Ni
3The method of Al based single-crystal high-temperature alloy is characterized in that: described Ni
3The Al based single-crystal high-temperature alloy is Ni-14Mo-7.8Al single crystal super alloy, Ni-13.5Mo-7.6Al-0.04B single crystal super alloy or Ni-14Mo-7.8Al-0.02B single crystal super alloy.
4, employing seed crystal method according to claim 1 and spiral crystal separation method combined preparation Ni
3The method of Al based single-crystal high-temperature alloy is characterized in that: described crystalline orientation is meant Ni
3Al based single-crystal high-temperature alloy body＜001 the orientation,＜011 the orientation or＜111 the orientation;
Described crystal face is meant (001) face, (011) face or (111) face; Described (001) face is the face of A, B, C, 4 formation of D; (011) face is the face of C, D, E, 4 formation of F; (111) face is the face of D, E, 3 formation of G.
5, employing seed crystal method according to claim 1 and spiral crystal separation method combined preparation Ni
3The method of Al based single-crystal high-temperature alloy is characterized in that: the described wax material in second step and the 3rd step is the wax material of the π BKB 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 π C50-50 trade mark.
6, employing seed crystal method according to claim 1 and spiral crystal separation method combined preparation Ni
3The method of Al based single-crystal high-temperature alloy is characterized in that: 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.
7, employing seed crystal method according to claim 1 and spiral crystal separation method combined preparation Ni
3The method of Al based single-crystal high-temperature alloy is characterized in that: described etching reagent is made up of hydrochloric acid and hydrogen peroxide, and adds 5～30ml hydrogen peroxide in every 10ml hydrochloric acid.
8, employing seed crystal method according to claim 1 and spiral crystal separation method combined preparation Ni
3The method of Al based single-crystal high-temperature alloy is characterized in that: the Ni that makes
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.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127816A (en) * | 2010-11-25 | 2011-07-20 | 北京航空航天大学 | Method for preparing Ni3A1-based rhenium-contained moncrystal alloy with liquid metal cooling method |
| CN108411371A (en) * | 2018-06-04 | 2018-08-17 | 北京航空航天大学 | A kind of seed-grain method crystal growth orientation accurately controls formwork and its manufacturing method |
| CN111216258A (en) * | 2020-02-25 | 2020-06-02 | 西北工业大学 | Method for preparing cast single crystal high-temperature alloy seed crystal by cutting |
| CN113073379A (en) * | 2021-03-04 | 2021-07-06 | 贵阳航发精密铸造有限公司 | Seed crystal preparation process for engineering application of seed crystal method growth single crystal blade |
| CN113373520A (en) * | 2021-04-28 | 2021-09-10 | 潍坊科技学院 | Single crystal high-entropy alloy with wide temperature range, high strength, high plasticity and oxidation resistance and preparation method thereof |
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2007
- 2007-12-17 CN CN200710179687A patent/CN100587135C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127816A (en) * | 2010-11-25 | 2011-07-20 | 北京航空航天大学 | Method for preparing Ni3A1-based rhenium-contained moncrystal alloy with liquid metal cooling method |
| CN108411371A (en) * | 2018-06-04 | 2018-08-17 | 北京航空航天大学 | A kind of seed-grain method crystal growth orientation accurately controls formwork and its manufacturing method |
| CN108411371B (en) * | 2018-06-04 | 2023-06-16 | 北京航空航天大学 | Mould shell for precisely controlling growth orientation of single crystal by seed crystal method and manufacturing method thereof |
| CN111216258A (en) * | 2020-02-25 | 2020-06-02 | 西北工业大学 | Method for preparing cast single crystal high-temperature alloy seed crystal by cutting |
| CN111216258B (en) * | 2020-02-25 | 2022-04-05 | 西北工业大学 | Method for preparing cast single crystal high-temperature alloy seed crystal by cutting |
| CN113073379A (en) * | 2021-03-04 | 2021-07-06 | 贵阳航发精密铸造有限公司 | Seed crystal preparation process for engineering application of seed crystal method growth single crystal blade |
| CN113373520A (en) * | 2021-04-28 | 2021-09-10 | 潍坊科技学院 | Single crystal high-entropy alloy with wide temperature range, high strength, high plasticity and oxidation resistance and preparation method thereof |
| CN113373520B (en) * | 2021-04-28 | 2023-12-15 | 潍坊科技学院 | Wide-temperature, high-strength, high-plasticity and oxidation-resistant single crystal high-entropy alloy and preparation method thereof |
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