CN102127816B - Method for preparing Ni3A1-based rhenium-contained moncrystal alloy with liquid metal cooling method - Google Patents

Method for preparing Ni3A1-based rhenium-contained moncrystal alloy with liquid metal cooling method Download PDF

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CN102127816B
CN102127816B CN2011100643939A CN201110064393A CN102127816B CN 102127816 B CN102127816 B CN 102127816B CN 2011100643939 A CN2011100643939 A CN 2011100643939A CN 201110064393 A CN201110064393 A CN 201110064393A CN 102127816 B CN102127816 B CN 102127816B
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rhenium
alloy
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CN102127816A (en
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徐惠彬
汤林志
宫声凯
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Beihang University
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Beihang University
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Abstract

The invention provides a method for preparing Ni3A1-based rhenium-contained moncrystal alloy with a liquid metal cooling method, which concretely comprises the following steps of: firstly, preparing a liquid metal cooling medium; secondly, preparing a Ni3A1-based rhenium-contained alloy coupon; and thirdly, preparing a Ni3A1-based rhenium-free alloy seed crystal and the like. In the method, liquid metal (such as gallium and indium alloy or tin) is used as the cooling medium so that the cooling speed of a casting and the temperature gradient (200-350 K/cm) of a solid and liquid interface are increased; and a Ni3A1-based rhenium-contained moncrystal high-temperature alloy with small primary dendrite arm spacing, uniform tissues and low segregation is prepared with a seed crystal method through changing solidification process parameters such as heating temperature, pulling rate and the like, thereby obtaining Ni3A1-based rhenium-contained moncrystal alloy with excellent mechanical property.

Description

A kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing 3The method of Al base single crystal alloy
Technical field
The invention belongs to the alloy technology field, be specifically related to a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing 3The method of Al base single crystal alloy.
Background technology
Ni 3Al intermetallic compound fusing point is 1395 ℃, has higher high temperature strength, creep resistance and high specific tenacity, and ys has positive temperature effect, single crystal Ni below peak temperature 3Al has higher plasticity, but polycrystal Ni 3Al is fragility.Therefore consider with Ni 3Al might break through the use temperature of existing nickel-base alloy for the alloy of base.
At present, at power, petrochemical industry, transportation, particularly industrial circle such as aviation and space flight, require mover to have higher thrust-weight ratio and working efficiency, this just requires mover to have higher working temperature.Usually HMP elements such as W, Ta, Re and Ru have been added in the single crystal alloy that adopts; And traditional rapid solidification method adopts water as heat-eliminating medium; Speed of cooling and thermograde are lower by (30～80K/cm); Make the HMP element in process of setting, cause the even component segregation of tissue odds, influenced the work-ing life of alloy.
The directional solidification method of widespread use at present is " the solidifying (HRS) method at a high speed " of being invented in late 1960s; According to reference 1: Hu Hanqi. metal freezing principle [M]. Beijing: China Machine Press; Put down in writing among the 2000:80-190, this method realizes positive thermograde through insulation heating zone and foundry goods bottom water-cooled pallet and heat loss through radiation in the oriented monocrystalline stove (KT5-084 type).But pull out from soak zones with foundry goods, it is main that heat radiation gradually becomes with radiation, and radiating efficiency descends very soon; Cause the thermograde of solidified front constantly to reduce; The foundry goods tissue odds that is produced is even, is prone to form freckle and low angle boundary, and the microsegregation height is prone to cause TCP to separate out mutually.Particularly for the production of large size gas turbine blades (＞60mm), the above-mentioned shortcoming of HRS method is very outstanding.
Summary of the invention
To the problem that exists in the prior art, the present invention proposes a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing 3The method of Al base single crystal alloy; This method uses heat-eliminating medium to be liquid metal (like gallium indium alloy or tin); With the thermograde that improves cooling velocity of casting and solid-liquid interface (200K/cm～350K/cm); Adopt the seed crystal method, through changing the solidifying process parameter, the Ni of the rhenium-containing of, homogeneous microstructure little and low segregation like preparation primary dendritic spacings such as Heating temperature, pulling rates 3Al base single crystal alloy, thereby the Ni of acquisition good mechanical performance rhenium-containing 3Al base single crystal alloy.
A kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing that the present invention proposes 3The method of Al base single crystal alloy specifically comprises following step:
The first step: preparation liquid-metal-coolant;
Described liquid-metal-coolant is gallium indium alloy or metallic tin.The preparation of said gallium indium alloy: with raw material high purity gallium (Ga) and high purity indium (In); By weight percentage: gallium 10～30wt%, all the other are indium, take by weighing; Put into beaker be heated to 80～200 ℃ its reaction is in a liquid state after; Pour in the liquid metal cooling tank as heat-eliminating medium, adopt the vacuum pump oil heating to make the cooling tank temperature maintenance around the liquid metal cooling tank, make the gallium indium alloy keep liquid more than 15 ℃;
The preparation of said metallic tin: the raw material high purity tin is heated to melting temperature (232 ℃) it is in a liquid state; Pour into then in the liquid metal cooling tank; Adopting the vacuum pump oil heating to make the cooling tank temperature around the liquid metal cooling tank is 250～300 ℃, makes metallic tin keep liquid.Described vacuum pump oil is preferably the VM100 vacuum pump oil.
Second step: the Ni of preparation rhenium-containing 3Al base alloy coupon;
(1) will prepare the Ni of rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo) and high-purity rhenium (Re) by weight percentage: the Al of 7～8wt%, 8～13% Mo, the Re of 0.0005～3wt%, all the other take by weighing for Ni, (as the Ni for preparing rhenium-containing 3Al base alloy also contains more than one Dy, Y or Hf; With more than one Dy, Y or Hf; Dy, Y or Hf are respectively the Dy of 0.05～0.5wt%, the Y of 0.1～1wt% or the Hf of 0.05～0.5wt% according to weight percent and take by weighing respectively); And, Ni, Mo and Re are put into vacuum induction furnace (as the Ni of the rhenium-containing for preparing with after acetone and the oven dry 3When also comprising more than one Dy, Y or Hf in the composition of Al base alloy, more than one Dy, Y or Hf put into vacuum induction furnace with Ni, Mo and Re), described vacuum induction furnace is preferably ZGJL-0.025 type vacuum induction furnace.
(2) vacuum induction furnace is evacuated to below the 1Pa, 1510 ± 10 ℃ of feeding temperature-raising to alloying smelting temperature, alloying smelting is after 10～30 minutes; After being warming up to 1560 ± 10 ℃; Be incubated 5～10 minutes, outage is cooled to 1500 ± 10 ℃, adds rafifinal (Al); Again proceeded alloying smelting 5～10 minutes to electricity, the Ni of rhenium-containing is processed in charged casting 3Al base alloy bar material.
(3) at the Ni of rhenium-containing 3Using wire cutting method to cut out diameter on the Al base alloy bar material is 15～20mm, and length with cleaning, drying after the polished finish of this cylinder coupon A surface finish, obtains the Ni of rhenium-containing smaller or equal to the cylinder coupon A of 200mm 3Al base alloy coupon.
The 3rd step: prepare the not Ni of rhenium-containing 3Al base alloy seed crystal;
Ni at common not rhenium-containing 3Al base single crystal alloy raw material (preferred (100) or (111) direction of orientation; The orientation irrelevance is less than 12 °) reach the standard grade that to cut out diameter be 6～12mm; Length is the cylinder coupon B of 30～60mm, after this cylinder coupon B surface economy-combat grinding and polishing optical processing and corrosion treatment, obtains the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is with this Ni of rhenium-containing not 3Al base single crystal alloy seed crystal is enclosed in the ceramic shell mould with alumina slurry, keeps the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is coaxial with ceramic shell mould, and is in the central position of ceramic shell mould, puts into drying baker, in 130～150 ℃, is incubated 2～4 hours;
The Ni of described common not rhenium-containing 3The composition of Al base single crystal alloy according to weight percent is: the Al of 7～8wt%, and 8～13% Mo, all the other are Ni.
Described ceramic shell mould is preferably the round ceramic formwork, is preferably 99 porcelain ceramic shell moulds, and diameter is 17～22mm, and length is smaller or equal to 250mm; Described polished finish is specially: adopt 400# and 800#SiO successively 2Coated abrasive working, polished finish on polishing machine then; Described corrosion treatment is specially: behind the employing of the sample after polished finish etching reagent corrosion 10～15min, take out and dry with the clean back of ultrasonic cleaning; Described etching reagent is preferably the mixing liquid of hydrochloric acid and hydrogen peroxide, adds 60～100ml hydrogen peroxide in every 100ml hydrochloric acid; Described alumina slurry is 80～320 purpose Al by granularity 2O 3The mixed slurry that powder and silica gel are formed, every 100gAl 2O 3Add 50～60ml silica gel in the powder.
The 4th step: with the Ni of rhenium-containing 3Al base alloy coupon is vertically put into and is had the not Ni of rhenium-containing 3In the ceramic shell mould of Al base alloy seed crystal, will have the Ni of rhenium-containing again 3The Al base alloy coupon and the Ni of rhenium-containing not 3The ceramic shell mould of Al base single crystal alloy seed crystal is put into the oriented monocrystalline stove together;
The 5th step: the vacuum of oriented monocrystalline stove is evacuated to 1 * 10 -1～5 * 10 -1Pa regulates in the oriented monocrystalline stove temperature to 1600 ℃～1650 ℃, is incubated 5～10 minutes, treats the Ni of rhenium-containing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal melts fully, makes the Ni of the rhenium-containing of ceramic shell mould, thawing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal moves down in the entering liquid metal cooling tank with the pulling rate of 2～10mm/min; Ni according to rhenium-containing 3The length (smaller or equal to 200mm) of Al base alloy coupon and pulling rate are calculated the crystal pulling time, and (the crystal pulling time equals the Ni of rhenium-containing 3The length of Al base alloy coupon is divided by pulling rate), after reaching the crystal pulling time, crystal pulling finishes, and takes out after cooling to room temperature with the furnace, obtains the Ni of rhenium-containing 3Al base single crystal alloy.
The advantage that has of the present invention is:
1, a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing of the present invention's proposition 3The method of Al base single crystal alloy reduces the element segregation of alloy significantly; Suppressing the interdendritic lower melting point separates out mutually; Reduce primary dendritic spacing and interdendritic region area, its uniform distribution of refinement γ ' mutual-assistance, this makes the probability that produces defective in the alloy graining process reduce.
2, a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing of the present invention's proposition 3The Ni of the rhenium-containing of the method preparation of Al base single crystal alloy 3Al base single crystal alloy in hot conditions, has very high creep rupture strength and plasticity, and its high temperature endurance performance under 1100 ℃/130MPa condition can reach 281.25 hours.
3, a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing of the present invention's proposition 3The Ni of the rhenium-containing of the method preparation of Al base single crystal alloy 3Al base single crystal alloy adopts the monocrystalline coupon orientation irrelevance of landfill seed crystal method preparation lower, and the success ratio of single crystal preparation is higher.
Description of drawings
Fig. 1: a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing that utilizes the present invention to propose 3The metallograph of Al base single crystal alloy;
Fig. 2: a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing that utilizes the present invention to propose 3The Ni of the rhenium-containing that the method for Al base single crystal alloy prepares under 1600 ℃ of different pulling rates 3The primary dendritic spacing variation diagram of Al base single crystal alloy;
Fig. 3: a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing that utilizes the present invention to propose 3The Ni of the rhenium-containing that the method for Al base single crystal alloy prepares under 1600 ℃ of different pulling rates 3The enduring quality variation diagram of Al base single crystal alloy;
Fig. 4: a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing that the present invention proposes 3Seed crystal is enclosed the structural representation in the ceramic shell mould in the method for Al base single crystal alloy;
Fig. 5: a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing that the present invention proposes 3Employed oriented monocrystalline stove synoptic diagram in the method for Al base single crystal alloy.
Among the figure: 1-liquid metal cooling tank; The 2-basetray.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed description.
A kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing that the present invention proposes 3The method of Al base single crystal alloy specifically comprises following step:
The first step: preparation liquid-metal-coolant;
Described liquid-metal-coolant is gallium indium alloy or metallic tin.The preparation of said gallium indium alloy: with raw material high purity gallium (Ga) and high purity indium (In), by weight percentage: gallium 10～30wt%, all the other are indium; Take by weighing; Put into beaker be heated to 80～200 ℃ its reaction is in a liquid state after, pour in the liquid metal cooling tank 1 as heat-eliminating medium, like Fig. 5; Adopt the vacuum pump oil heating to make the cooling tank temperature maintenance around the liquid metal cooling tank 1, make the gallium indium alloy keep liquid more than 15 ℃;
The preparation of said metallic tin: the raw material high purity tin is heated to melting temperature (232 ℃) it is in a liquid state; Pour into then in the liquid metal cooling tank 1; Adopting the vacuum pump oil heating to make the cooling tank temperature around the liquid metal cooling tank 1 is 250～300 ℃, makes metallic tin keep liquid.Described vacuum pump oil is preferably the VM100 vacuum pump oil.
Second step: the Ni of preparation rhenium-containing 3Al base alloy coupon;
(1) will prepare the Ni of rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo) and high-purity rhenium (Re) by weight percentage: the Al of 7～8wt%, 8～13% Mo, the Re of 0.0005～3wt%, all the other take by weighing for Ni, as the Ni of rhenium-containing to be prepared 3When more than one Dy in the Al base alloy, Y or Hf; Composition is respectively the Dy of 0.05～0.5wt%, the Y of 0.1～1wt% or the Hf of 0.05～0.5wt% by weight percentage and takes by weighing; And, Ni, Mo and Re are put into vacuum induction furnace (as the Ni of the rhenium-containing for preparing with after acetone and the oven dry 3Al base alloy also comprises more than one Dy, Y or Hf, and more than one Dy, Y or Hf also put into vacuum induction furnace), described vacuum induction furnace is preferably ZGJL-0.025 type vacuum induction furnace.
(2) vacuum induction furnace is evacuated to below the 1Pa, 1510 ± 10 ℃ of feeding temperature-raising to alloying smelting temperature, alloying smelting is after 10～30 minutes; After being warming up to 1560 ± 10 ℃; Be incubated 5～10 minutes, outage is cooled to 1500 ± 10 ℃, adds rafifinal (Al); Again proceeded alloying smelting 5～10 minutes to electricity, the Ni of rhenium-containing is processed in charged casting 3Al base alloy bar material.
(3) at the Ni of rhenium-containing 3Using wire cutting method to cut out diameter on the Al base alloy bar material is 15～20mm, and length with cleaning, drying after the polished finish of this cylinder coupon A surface finish, obtains the Ni of rhenium-containing smaller or equal to the cylinder coupon A of 200mm 3Al base alloy coupon.
The 3rd step: prepare the not Ni of rhenium-containing 3Al base alloy seed crystal;
Ni at common not rhenium-containing 3Al base single crystal alloy raw material (preferred (100) or (111) direction of orientation; The orientation irrelevance is less than 12 °) reach the standard grade that to cut out diameter be 6～12mm; Length is the cylinder coupon B of 30～60mm, after this cylinder coupon B surface economy-combat grinding and polishing optical processing and corrosion treatment, obtains the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is with this Ni of rhenium-containing not 3Al base single crystal alloy seed crystal is enclosed in the ceramic shell mould with alumina slurry, and is as shown in Figure 4, keeps the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is coaxial with ceramic shell mould, and is in the central position of ceramic shell mould, puts into drying baker, in 130～150 ℃, is incubated 2～4 hours;
The Ni of described common not rhenium-containing 3The composition of Al base single crystal alloy according to weight percent is: the Al of 7～8wt%, and 8～13% Mo, all the other are Ni.
Described ceramic shell mould is preferably the round ceramic formwork, is preferably 99 porcelain ceramic shell moulds, and diameter is 17～22mm, and length is smaller or equal to 250mm; Described polished finish is specially: adopt 400# and 800#SiO successively 2Coated abrasive working, polished finish on polishing machine then; Described corrosion treatment is specially: behind the employing of the sample after polished finish etching reagent corrosion 10～15min, take out and dry with the clean back of ultrasonic cleaning; Described etching reagent is preferably the mixing liquid of hydrochloric acid and hydrogen peroxide, adds 60～100ml hydrogen peroxide (concentration is 30%) in every 100ml hydrochloric acid (concentration is 36%～38%); Described alumina slurry is 80～320 purpose Al by granularity 2O 3The mixed slurry that powder and silica gel are formed, every 100gAl 2O 3Add 50～60ml silica gel in the powder.
The 4th step: with the Ni of rhenium-containing 3Al base alloy coupon is vertically put into and is had the not Ni of rhenium-containing 3In the ceramic shell mould of Al base alloy seed crystal, will have the Ni of rhenium-containing again 3The Al base alloy coupon and the Ni of rhenium-containing not 3The ceramic shell mould of Al base single crystal alloy seed crystal is put into the oriented monocrystalline stove together;
The 5th step: the vacuum of oriented monocrystalline stove is evacuated to 1 * 10 -1～5 * 10 -1Pa regulates in the oriented monocrystalline stove temperature to 1600 ℃～1650 ℃, is incubated 5～10 minutes, treats the Ni of rhenium-containing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal melts fully, makes the Ni of the rhenium-containing of ceramic shell mould, thawing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal moves down in the entering liquid metal cooling tank 1 with the pulling rate of 2～10mm/min; Ni according to rhenium-containing 3The length (smaller or equal to 200mm) of Al base alloy coupon and pulling rate are calculated the crystal pulling time, and (the crystal pulling time equals the Ni of rhenium-containing 3The length of Al base alloy coupon is divided by pulling rate), after reaching the crystal pulling time, crystal pulling finishes, and takes out after cooling to room temperature with the furnace, obtains the Ni of rhenium-containing 3Al base single crystal alloy.
A kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing that utilizes the present invention to propose 3The metallograph of Al base single crystal alloy is as shown in Figure 1, and have dendrite and do and the interdendritic structure, when all being in 1600 ℃, the Ni of the rhenium-containing for preparing under the different pulling rates 3The primary dendritic spacing of Al base single crystal alloy is different, and as shown in Figure 2, along with the increase of pulling rate, primary dendritic spacing diminishes gradually.As shown in Figure 3, high temperature endurance performance is along with the increase of pulling rate under 1100 ℃/130MPa condition, and high-temperature duration life also increases gradually.
The oriented monocrystalline stove that uses among the present invention is based on conventional oriented monocrystalline stove (being preferably the KT5-084 type) improvement and forms; As shown in Figure 5; Liquid metal cooling tank 1 is installed on the basetray 2 of conventional oriented monocrystalline stove, and is carried out encapsulation process, put into gallium indium alloy GaIn or metallic tin Sn liquid-metal-coolant in the cooling tank; Beginning along with crystal pulling; Sample progresses into liquid-metal-coolant, and then (gallium indium alloy GaIn thermograde is generally 200K/cm～350K/cm, metallic tin Sn70K/cm～100K/cm) to realize big thermograde.
Embodiment 1:
A kind of Ni of rhenium-containing 3The preparation method of Al base single crystal alloy mainly comprises following step:
The first step: preparation liquid-metal-coolant;
Described liquid-metal-coolant is the gallium indium alloy.The preparation of said gallium indium alloy: with raw material high purity gallium (Ga) and high purity indium (In); By weight percentage: gallium 10wt%, all the other are indium, take by weighing; Put into beaker be heated to 80 ℃ its reaction is in a liquid state after; Pour in the liquid metal cooling tank 1 as heat-eliminating medium, adopt the vacuum pump oil heating to make the cooling tank temperature maintenance on 15 ℃ around the liquid metal cooling tank 1, make the gallium indium alloy keep liquid;
Second step: the Ni of preparation rhenium-containing 3Al base alloy coupon;
(1) will prepare the Ni of rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo), high-purity rhenium (Re), high-purity dysprosium (Dy) and high-purity yttrium (Y) by weight percentage: the Al of 7.4wt%; 13% Mo, 0.5% Re, the Dy of 0.1wt%; The Y of 0.1wt%; All the other take by weighing for Ni, and with after acetone and the oven dry, Ni, Mo, Re, Dy and Y are put into ZGJL-0.025 type vacuum induction furnace.
(2) vacuum induction furnace is evacuated to below the 0.5Pa, 1500 ℃ of feeding temperature-raising to alloying smelting temperature, alloying smelting is after 10 minutes; After being warming up to 1550 ℃; Be incubated 5 minutes, outage is cooled to 1500 ℃, adds rafifinal (Al); Again proceeded alloying smelting 6 minutes to electricity, the Ni of rhenium-containing is processed in charged casting 3Al base alloy bar material.
(3) at the Ni of rhenium-containing 3Use wire cutting method to cut out diameter on the Al base alloy bar material and be 15mm, length equals the cylinder coupon A of 200mm, with cleaning, drying after the polished finish of this cylinder coupon A surface finish, obtains the Ni of rhenium-containing 3Al base alloy coupon.
The 3rd step: prepare the not Ni of rhenium-containing 3Al base alloy seed crystal;
Ni at common not rhenium-containing 3Al base single crystal alloy raw material (crystalline orientation is (100), and the orientation irrelevance is less than 12 °) is reached the standard grade and cut out diameter is 6mm, and length is the cylinder coupon B of 30mm, after this cylinder coupon B surface economy-combat grinding and polishing optical processing and corrosion treatment, obtains the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is with this Ni of rhenium-containing not 3Al base single crystal alloy seed crystal is enclosed in the ceramic shell mould with alumina slurry, keeps the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is coaxial with ceramic shell mould, and is in the central position of ceramic shell mould, puts into drying baker, in 130 ℃, is incubated 2 hours;
The Ni of described common not rhenium-containing 3The composition of Al base single crystal alloy according to weight percent is: the Al of 7.4wt%, and 13% Mo, all the other are Ni.
Described ceramic shell mould is 99 porcelain ceramic shell moulds, and diameter is 17～22mm, and length equals 250mm; Described polished finish is specially: adopt 400# and 800#SiO successively 2Coated abrasive working, polished finish on polishing machine then; Described corrosion treatment is specially: behind the employing of the sample after polished finish etching reagent corrosion 10min, take out and dry with the clean back of ultrasonic cleaning; Described etching reagent is preferably the mixing liquid of hydrochloric acid and hydrogen peroxide, adds 60ml hydrogen peroxide (concentration is 30%) in every 100ml hydrochloric acid (concentration is 38%); Described alumina slurry is 80 purpose Al by granularity 2O 3The mixed slurry that powder and silica gel are formed, every 100gAl 2O 3Add 50ml silica gel in the powder.
The 4th step: with the Ni of rhenium-containing 3Al base alloy coupon is vertically put into and is had the not Ni of rhenium-containing 3In the ceramic shell mould of Al base alloy seed crystal, will have the Ni of rhenium-containing again 3The Al base alloy coupon and the Ni of rhenium-containing not 3The ceramic shell mould of Al base single crystal alloy seed crystal is put into the oriented monocrystalline stove together;
The 5th step: the vacuum of oriented monocrystalline stove is evacuated to 0.36Pa, regulates in the oriented monocrystalline stove temperature to 1596 ℃, be incubated 5 minutes, treat the Ni of rhenium-containing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal melts fully, makes the Ni of the rhenium-containing of ceramic shell mould, thawing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal moves down in the entering liquid metal cooling tank 1 with the pulling rate of 2mm/min; Behind the crystal pulling 93min, crystal pulling finishes, and takes out after cooling to room temperature with the furnace, obtains the Ni of rhenium-containing 3Al base single crystal alloy.
The Ni of the rhenium-containing that obtains 3The density of Al base single crystal alloy is 7.84g/cm 3, crystalline orientation is (100), the orientation irrelevance is less than 12 °.Carry out mechanical property test and find the Ni of this rhenium-containing 3The high-temperature duration life of Al base single crystal alloy under 1100 ℃/130MPa is 181.35h.The Ni of this rhenium-containing 3Al base single crystal alloy unit elongation is 7.12%, and the end face shrinking percentage is 23.5%.
Embodiment 2:
A kind of Ni of rhenium-containing 3The preparation method of Al base single crystal alloy specifically comprises following step:
The first step: preparation liquid-metal-coolant;
Described liquid-metal-coolant is gallium indium alloy or metallic tin.The preparation of said gallium indium alloy: with raw material high purity gallium (Ga) and high purity indium (In); By weight percentage: gallium 30wt%, all the other are indium, take by weighing; Put into beaker be heated to 200 ℃ its reaction is in a liquid state after; Pour in the liquid metal cooling tank 1 as heat-eliminating medium, adopt the vacuum pump oil heating to make the cooling tank temperature maintenance around the liquid metal cooling tank 1, make the gallium indium alloy keep liquid at 18 ℃;
Second step: the Ni of preparation rhenium-containing 3Al base alloy coupon;
(1) will prepare the Ni of rhenium-containing 3The Al of Al base alloy materials: 7.5wt%, 11% Mo, 1% Re, the Dy of 0.05wt%, the Y of 0.5wt%, all the other are Ni, take by weighing, and with after acetone and the oven dry, Ni, Mo, Re, Dy and Y are put into ZGJL-0.025 type vacuum induction furnace.
(2) vacuum induction furnace is evacuated to 1Pa, 1507 ℃ of feeding temperature-raising to alloying smelting temperature, alloying smelting is after 10 minutes; After being warming up to 1570 ℃; Be incubated 10 minutes, outage is cooled to 1507 ℃, adds rafifinal (Al); Again proceeded alloying smelting 8 minutes to electricity, the Ni of rhenium-containing is processed in charged casting 3Al base alloy bar material.
(3) at the Ni of rhenium-containing 3Use wire cutting method to cut out diameter on the Al base alloy bar material and be 20mm, length equals the cylinder coupon A of 200mm, with cleaning, drying after the polished finish of this cylinder coupon A surface finish, obtains the Ni of rhenium-containing 3Al base alloy coupon.
The 3rd step: prepare the not Ni of rhenium-containing 3Al base alloy seed crystal;
Ni at common not rhenium-containing 3Al base single crystal alloy raw material (crystalline orientation is (111), and the orientation irrelevance is less than 12 °) is reached the standard grade and cut out diameter is 12mm, and length is the cylinder coupon B of 60mm, after this cylinder coupon B surface economy-combat grinding and polishing optical processing and corrosion treatment, obtains the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is with this Ni of rhenium-containing not 3Al base single crystal alloy seed crystal is enclosed in the ceramic shell mould with alumina slurry, keeps the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is coaxial with ceramic shell mould, and is in the central position of ceramic shell mould, puts into drying baker, in 150 ℃, is incubated 4 hours;
The Ni of described common not rhenium-containing 3The composition of Al base single crystal alloy according to weight percent is: the Al of 7.5wt%, and 11% Mo, all the other are Ni.
Described ceramic shell mould is 99 porcelain ceramic shell moulds, and diameter is 17～22mm, and length equals 250mm; Described polished finish is specially: adopt 400# and 800#SiO successively 2Coated abrasive working, polished finish on polishing machine then; Described corrosion treatment is specially: behind the employing of the sample after polished finish etching reagent corrosion 15min, take out and dry with the clean back of ultrasonic cleaning; Described etching reagent is preferably the mixing liquid of hydrochloric acid and hydrogen peroxide, adds 100ml hydrogen peroxide (concentration is 30%) in every 100ml hydrochloric acid (concentration is 36%); Described alumina slurry is 320 purpose Al by granularity 2O 3The mixed slurry that powder and silica gel are formed, every 100gAl 2O 3Add 60ml silica gel in the powder.
The 4th step: with the Ni of rhenium-containing 3Al base alloy coupon is vertically put into and is had the not Ni of rhenium-containing 3In the ceramic shell mould of Al base alloy seed crystal, will have the Ni of rhenium-containing again 3The Al base alloy coupon and the Ni of rhenium-containing not 3The ceramic shell mould of Al base single crystal alloy seed crystal is put into the oriented monocrystalline stove together;
The 5th step: the vacuum of oriented monocrystalline stove is evacuated to 0.27Pa, regulates in the oriented monocrystalline stove temperature to 1598 ℃, be incubated 10 minutes, treat the Ni of rhenium-containing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal melts fully, makes the Ni of the rhenium-containing of ceramic shell mould, thawing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal moves down in the entering liquid metal cooling tank 1 with the pulling rate of 5mm/min; Behind crystal pulling 40min, crystal pulling finishes, and takes out after cooling to room temperature with the furnace, obtains the Ni of rhenium-containing 3Al base single crystal alloy.
The Ni of the rhenium-containing that obtains 3The density of Al base single crystal alloy is 7.83g/cm 3, crystalline orientation is (111), the orientation irrelevance is less than 12 °.Carry out mechanical property test and find the Ni of this rhenium-containing 3The high-temperature duration life of Al base single crystal alloy under 1100 ℃/130MPa is 140.13h.The Ni of this rhenium-containing 3Al base single crystal alloy unit elongation is 8.91%, and the end face shrinking percentage is 26.2%.
Embodiment 3:
A kind of Ni of rhenium-containing 3The preparation method of Al base single crystal alloy specifically comprises following step:
The first step: preparation liquid-metal-coolant;
The preparation of said metallic tin: the raw material high purity tin is heated to melting temperature (232 ℃) it is in a liquid state; Pour into then in the liquid metal cooling tank 1; Adopting the heating of VM100 vacuum pump oil to make the cooling tank temperature around the liquid metal cooling tank 1 is 250 ℃, makes metallic tin keep liquid.
Second step: the Ni of preparation rhenium-containing 3Al base alloy coupon;
(1) will prepare the Ni of rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo), high-purity rhenium (Re), high-purity dysprosium (Dy) and high-purity yttrium (Y) by weight percentage: the Al of 7.6wt%, 12.5% Mo, 1.5% Re; The Dy of 0.08wt%; The Y of 0.3wt%, all the other are Ni, take by weighing; And, Ni, Mo, Re, Dy and Y are put into ZGJL-0.025 type vacuum induction furnace with after acetone and the oven dry.
(2) vacuum induction furnace is evacuated to below the 0.8Pa, 1511 ℃ of feeding temperature-raising to alloying smelting temperature, alloying smelting is after 16 minutes; After being warming up to 1555 ℃; Be incubated 10 minutes, outage is cooled to 1511 ℃, adds rafifinal (Al); Again proceeded alloying smelting 5 minutes to electricity, the Ni of rhenium-containing is processed in charged casting 3Al base alloy bar material.
(3) at the Ni of rhenium-containing 3Use wire cutting method to cut out diameter on the Al base alloy bar material and be 18mm, length equals the cylinder coupon A of 200mm, with cleaning, drying after the polished finish of this cylinder coupon A surface finish, obtains the Ni of rhenium-containing 3Al base alloy coupon.
The 3rd step: prepare the not Ni of rhenium-containing 3Al base alloy seed crystal;
Ni at common not rhenium-containing 3It is 8mm that Al base single crystal alloy raw material (crystalline orientation is (111), and the orientation irrelevance is less than 12 °) line cuts out diameter, and length is the cylinder coupon B of 40mm, after this cylinder coupon B surface economy-combat grinding and polishing optical processing and corrosion treatment, obtains the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is with this Ni of rhenium-containing not 3Al base single crystal alloy seed crystal is enclosed in the ceramic shell mould with alumina slurry, keeps the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is coaxial with ceramic shell mould, and is in the central position of ceramic shell mould, puts into drying baker, in 140 ℃, is incubated 3 hours;
The Ni of described common not rhenium-containing 3The composition of Al base single crystal alloy according to weight percent is: the Al of 7.6wt%, and 12.5% Mo, all the other are Ni.
Described ceramic shell mould diameter is 20mm, and length equals 250mm; Described polished finish is specially: adopt 400# and 800#SiO successively 2Coated abrasive working, polished finish on polishing machine then; Described corrosion treatment is specially: behind the employing of the sample after polished finish etching reagent corrosion 10～15min, take out and dry with the clean back of ultrasonic cleaning; Described etching reagent is preferably the mixing liquid of hydrochloric acid and hydrogen peroxide, adds 80ml hydrogen peroxide (concentration is 30%) in every 100ml hydrochloric acid (concentration is 36%); Described alumina slurry is 100 purpose Al by granularity 2O 3The mixed slurry that powder and silica gel are formed, every 100gAl 2O 3Add 52ml silica gel in the powder.
The 4th step: with the Ni of rhenium-containing 3Al base alloy coupon is vertically put into and is had the not Ni of rhenium-containing 3In the ceramic shell mould of Al base alloy seed crystal, will have the Ni of rhenium-containing again 3The Al base alloy coupon and the Ni of rhenium-containing not 3The ceramic shell mould of Al base single crystal alloy seed crystal is put into the oriented monocrystalline stove together;
The 5th step: the vacuum of oriented monocrystalline stove is evacuated to 0.18Pa, regulates in the oriented monocrystalline stove temperature to 1600 ℃, be incubated 6 minutes, treat the Ni of rhenium-containing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal melts fully, makes the Ni of the rhenium-containing of ceramic shell mould, thawing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal moves down in the entering liquid metal cooling tank 1 with the pulling rate of 7mm/min; Behind crystal pulling 30min, crystal pulling finishes, and takes out after cooling to room temperature with the furnace, obtains the Ni of rhenium-containing 3Al base single crystal alloy.
The Ni of the rhenium-containing that obtains 3The density of Al base single crystal alloy is 7.84g/cm 3, crystalline orientation is (111), the orientation irrelevance is less than 12 °.Carry out mechanical property test and find the Ni of this rhenium-containing 3The high-temperature duration life of Al base single crystal alloy under 1100 ℃/130MPa is 230.44h.The Ni of this rhenium-containing 3Al base single crystal alloy unit elongation is 9.4%, and the end face shrinking percentage is 33.0%.
Embodiment 4:
A kind of Ni of rhenium-containing 3The preparation method of Al base single crystal alloy specifically comprises following step:
The first step: preparation liquid-metal-coolant;
The preparation of said metallic tin: the raw material high purity tin is heated to melting temperature (232 ℃) it is in a liquid state; Pour into then in the liquid metal cooling tank 1; Adopting the heating of VM100 vacuum pump oil to make the cooling tank temperature around the liquid metal cooling tank 1 is 300 ℃, makes metallic tin keep liquid.
Second step: the Ni of preparation rhenium-containing 3Al base alloy coupon;
(1) will prepare the Ni of rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo), high-purity rhenium (Re), high-purity dysprosium (Dy) and high-purity yttrium (Y) be the Al of 7.8wt% by weight percentage; 11% Mo, 2% Re, the Dy of 0.2wt%; The Y of 0.8wt%; All the other take by weighing for Ni, and with after acetone and the oven dry, Ni, Mo, Re, Dy and Y are put into ZGJL-0.025 type vacuum induction furnace.
(2) vacuum induction furnace is evacuated to below the 0.5Pa, 1515 ℃ of feeding temperature-raising to alloying smelting temperature, alloying smelting is after 19 minutes; After being warming up to 1552 ℃; Be incubated 8 minutes, outage is cooled to 1515 ℃, adds rafifinal (Al); Again proceeded alloying smelting 5 minutes to electricity, the Ni of rhenium-containing is processed in charged casting 3Al base alloy bar material.
(3) at the Ni of rhenium-containing 3Use wire cutting method to cut out diameter on the Al base alloy bar material and be 16mm, length equals the cylinder coupon A of 200mm, with cleaning, drying after the polished finish of this cylinder coupon A surface finish, obtains the Ni of rhenium-containing 3Al base alloy coupon.
The 3rd step: prepare the not Ni of rhenium-containing 3Al base alloy seed crystal;
The Ni of common not rhenium-containing 3Al base single crystal alloy raw material (crystalline orientation is (100), and the orientation irrelevance is less than 12 °) is reached the standard grade and cut out diameter is 7mm, and length is the cylinder coupon B of 50mm, after this cylinder coupon B surface economy-combat grinding and polishing optical processing and corrosion treatment, obtains the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is with this Ni of rhenium-containing not 3Al base single crystal alloy seed crystal is enclosed in the ceramic shell mould with alumina slurry, keeps the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is coaxial with ceramic shell mould, and is in the central position of ceramic shell mould, puts into drying baker, in 145 ℃, is incubated 2.5 hours;
The Ni of described common not rhenium-containing 3The composition of Al base single crystal alloy according to weight percent is: the Al of 7.8wt%, and 11% Mo, all the other are Ni.
Described ceramic shell mould is 99 porcelain ceramic shell moulds, and diameter is 20mm, and length equals 250mm; Described polished finish is specially: adopt 400# and 800#SiO successively 2Coated abrasive working, polished finish on polishing machine then; Described corrosion treatment is specially: behind the employing of the sample after polished finish etching reagent corrosion 12min, take out and dry with the clean back of ultrasonic cleaning; Described etching reagent is preferably the mixing liquid of hydrochloric acid and hydrogen peroxide, adds 80ml hydrogen peroxide (concentration is 30%) in every 100ml hydrochloric acid (concentration is 36%); Described alumina slurry is 150 purpose Al by granularity 2O 3The mixed slurry that powder and silica gel are formed, every 100gAl 2O 3Add 52ml silica gel in the powder.
The 4th step: with the Ni of rhenium-containing 3Al base alloy coupon is vertically put into and is had the not Ni of rhenium-containing 3In the ceramic shell mould of Al base alloy seed crystal, will have the Ni of rhenium-containing again 3The Al base alloy coupon and the Ni of rhenium-containing not 3The ceramic shell mould of Al base single crystal alloy seed crystal is put into the oriented monocrystalline stove together;
The 5th step: the vacuum of oriented monocrystalline stove is evacuated to 0.25Pa, regulates in the oriented monocrystalline stove temperature to 1603 ℃, be incubated 6 minutes, treat the Ni of rhenium-containing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal melts fully, makes the Ni of the rhenium-containing of ceramic shell mould, thawing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal moves down in the entering liquid metal cooling tank 1 with the pulling rate of 10mm/min; Behind crystal pulling 25min, crystal pulling finishes, and takes out after cooling to room temperature with the furnace, obtains the Ni of rhenium-containing 3Al base single crystal alloy.
The Ni of the rhenium-containing that obtains 3The density of Al base single crystal alloy is 7.82g/cm 3, crystalline orientation is (100), the orientation irrelevance is less than 12 °.Carry out mechanical property test and find the Ni of this rhenium-containing 3The high-temperature duration life of Al base single crystal alloy under 1100 ℃/130MPa is 247.16h.The Ni of this rhenium-containing 3Al base single crystal alloy unit elongation is 12.3%, and the end face shrinking percentage is 40.0%.
Embodiment 5:
A kind of Ni of rhenium-containing 3The preparation method of Al base single crystal alloy specifically comprises following step:
The first step: preparation liquid-metal-coolant;
Described liquid-metal-coolant is gallium indium alloy or metallic tin.The preparation of said gallium indium alloy: with raw material high purity gallium (Ga) and high purity indium (In); By weight percentage: gallium 20wt%, all the other are indium, take by weighing; Put into beaker be heated to 80 ℃～200 ℃ its reaction is in a liquid state after; Pour in the liquid metal cooling tank 1 as heat-eliminating medium, adopt the vacuum pump oil heating to make the cooling tank temperature maintenance around the liquid metal cooling tank 1, make the gallium indium alloy keep liquid at 20 ℃;
Second step: the Ni of preparation rhenium-containing 3Al base alloy coupon;
(1) will prepare the Ni of rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo), high-purity rhenium (Re), high-purity dysprosium (Dy) and high-purity yttrium (Y) by weight percentage: the Al of 7.6wt%, 11% Mo, 1.5% Re; The Dy of 0.5wt%; The Y of 1wt%, all the other are Ni, take by weighing; And, Ni, Mo, Re, Dy and Y are put into ZGJL-0.025 type vacuum induction furnace with after acetone and the oven dry.
(2) vacuum induction furnace is evacuated to 0.75Pa, 1508 ℃ of feeding temperature-raising to alloying smelting temperature, alloying smelting is after 10 minutes; After being warming up to 1562 ℃; Be incubated 7 minutes, outage is cooled to 1508 ℃, adds rafifinal (Al); Again proceeded alloying smelting 7 minutes to electricity, the Ni of rhenium-containing is processed in charged casting 3Al base alloy bar material.
(3) at the Ni of rhenium-containing 3Use wire cutting method to cut out diameter on the Al base alloy bar material and be 18mm, length equals the cylinder coupon A of 200mm, with cleaning, drying after the polished finish of this cylinder coupon A surface finish, obtains the Ni of rhenium-containing 3Al base alloy coupon.
The 3rd step: prepare the not Ni of rhenium-containing 3Al base alloy seed crystal;
Ni at common not rhenium-containing 3Al base single crystal alloy raw material (crystalline orientation is (111), and the orientation irrelevance is less than 12 °) is reached the standard grade and cut out diameter is 10mm, and length is the cylinder coupon B of 55mm, after this cylinder coupon B surface economy-combat grinding and polishing optical processing and corrosion treatment, obtains the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is with this Ni of rhenium-containing not 3Al base single crystal alloy seed crystal is enclosed in the ceramic shell mould with alumina slurry, keeps the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is coaxial with ceramic shell mould, and is in the central position of ceramic shell mould, puts into drying baker, in 145 ℃, is incubated 3 hours;
The Ni of described common not rhenium-containing 3The composition of Al base single crystal alloy according to weight percent is: all the other are the Al of 7.6wt%, 11% Mo.
Described ceramic shell mould is 99 porcelain ceramic shell moulds, and diameter is 22mm, and length equals 250mm; Described polished finish is specially: adopt 400# and 800#SiO successively 2Coated abrasive working, polished finish on polishing machine then; Described corrosion treatment is specially: behind the employing of the sample after polished finish etching reagent corrosion 12min, take out and dry with the clean back of ultrasonic cleaning; Described etching reagent is preferably the mixing liquid of hydrochloric acid and hydrogen peroxide, adds 90ml hydrogen peroxide (concentration is 30%) in every 100ml hydrochloric acid (concentration is 38%); Described alumina slurry is 200 purpose Al by granularity 2O 3The mixed slurry that powder and silica gel are formed, every 100gAl 2O 3Add 60ml silica gel in the powder.
The 4th step: with the Ni of rhenium-containing 3Al base alloy coupon is vertically put into and is had the not Ni of rhenium-containing 3In the ceramic shell mould of Al base alloy seed crystal, will have the Ni of rhenium-containing again 3The Al base alloy coupon and the Ni of rhenium-containing not 3The ceramic shell mould of Al base single crystal alloy seed crystal is put into the oriented monocrystalline stove together;
The 5th step: the vacuum of oriented monocrystalline stove is evacuated to 0.5Pa, regulates in the oriented monocrystalline stove temperature to 1600 ℃, be incubated 5 minutes, treat the Ni of rhenium-containing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal melts fully, makes the Ni of the rhenium-containing of ceramic shell mould, thawing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal moves down in the entering liquid metal cooling tank 1 with the pulling rate of 3mm/min; Behind crystal pulling 75min, crystal pulling finishes, and takes out after cooling to room temperature with the furnace, obtains the Ni of rhenium-containing 3Al base single crystal alloy.
The Ni of the rhenium-containing that obtains 3The density of Al base single crystal alloy is 7.80g/cm 3, crystalline orientation is (111), the orientation irrelevance is less than 12 °.Carry out mechanical property test and find the Ni of this rhenium-containing 3The high-temperature duration life of Al base single crystal alloy under 1100 ℃/130MPa is 171.12h.The Ni of this rhenium-containing 3Al base single crystal alloy unit elongation is 8.3%, and the end face shrinking percentage is 31.4%.
Embodiment 6:
A kind of Ni of rhenium-containing 3The preparation method of Al base single crystal alloy specifically comprises following step:
The first step: preparation liquid-metal-coolant;
Described liquid-metal-coolant is gallium indium alloy or metallic tin.The preparation of said gallium indium alloy: with raw material high purity gallium (Ga) and high purity indium (In); By weight percentage: gallium 25wt%, all the other are indium, take by weighing; Put into beaker be heated to 80 ℃～200 ℃ its reaction is in a liquid state after; Pour in the liquid metal cooling tank 1 as heat-eliminating medium, adopt the vacuum pump oil heating to make the cooling tank temperature maintenance around the liquid metal cooling tank 1, make the gallium indium alloy keep liquid at 30 ℃;
Second step: the Ni of preparation rhenium-containing 3Al base alloy coupon;
(1) will prepare the Ni of rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo), high-purity rhenium (Re), high-purity dysprosium (Dy) and high-purity yttrium (Y) be the Al of 7.3wt% by weight percentage, 12% Mo, 2% Re; The Dy of 0.3wt%; The Y of 0.3wt%, all the other are Ni, take by weighing; And, Ni, Mo, Re, Dy and Y are put into ZGJL-0.025 type vacuum induction furnace with after acetone and the oven dry.
(2) vacuum induction furnace is evacuated to below the 0.83Pa, 1510 ℃ of feeding temperature-raising to alloying smelting temperature, alloying smelting is after 14 minutes; After being warming up to 1560 ± 10 ℃; Be incubated 10 minutes, outage is cooled to 1510 ℃, adds rafifinal (Al); Again proceeded alloying smelting 10 minutes to electricity, the Ni of rhenium-containing is processed in charged casting 3Al base alloy bar material.
(3) at the Ni of rhenium-containing 3Use wire cutting method to cut out diameter on the Al base alloy bar material and be 20mm, length equals the cylinder coupon A of 200mm, with cleaning, drying after the polished finish of this cylinder coupon A surface finish, obtains the Ni of rhenium-containing 3Al base alloy coupon.
The 3rd step: prepare the not Ni of rhenium-containing 3Al base alloy seed crystal;
Ni at common not rhenium-containing 3Al base single crystal alloy raw material (crystalline orientation is (100), and the orientation irrelevance is less than 12 °) is reached the standard grade and cut out diameter is 6～12mm, and length is the cylinder coupon B of 60mm, after this cylinder coupon B surface economy-combat grinding and polishing optical processing and corrosion treatment, obtains the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is with this Ni of rhenium-containing not 3Al base single crystal alloy seed crystal is enclosed in the ceramic shell mould with alumina slurry, keeps the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is coaxial with ceramic shell mould, and is in the central position of ceramic shell mould, puts into drying baker, in 150 ℃, is incubated 4 hours;
The Ni of described common not rhenium-containing 3The composition of Al base single crystal alloy according to weight percent is: the Al of 7.3wt%, and 12% Mo, all the other are Ni.Described ceramic shell mould is preferably 99 porcelain ceramic shell moulds, and diameter is 22mm, and length equals 250mm; Described polished finish is specially: adopt 400# and 800#SiO successively 2Coated abrasive working, polished finish on polishing machine then; Described corrosion treatment is specially: behind the employing of the sample after polished finish etching reagent corrosion 15min, take out and dry with the clean back of ultrasonic cleaning; Described etching reagent is preferably the mixing liquid of hydrochloric acid and hydrogen peroxide, adds 100ml hydrogen peroxide (concentration is 30%) in every 100ml hydrochloric acid (concentration is 38%); Described alumina slurry is 250 purpose Al by granularity 2O 3The mixed slurry that powder and silica gel are formed, every 100gAl 2O 3Add 60ml silica gel in the powder.
The 4th step: with the Ni of rhenium-containing 3Al base alloy coupon is vertically put into and is had the not Ni of rhenium-containing 3In the ceramic shell mould of Al base alloy seed crystal, will have the Ni of rhenium-containing again 3The Al base alloy coupon and the Ni of rhenium-containing not 3The ceramic shell mould of Al base single crystal alloy seed crystal is put into the oriented monocrystalline stove together;
The 5th step: the vacuum of oriented monocrystalline stove is evacuated to 0.1Pa, regulates in the oriented monocrystalline stove temperature to 1603 ℃, be incubated 10 minutes, treat the Ni of rhenium-containing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal melts fully, makes the Ni of the rhenium-containing of ceramic shell mould, thawing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal moves down in the entering liquid metal cooling tank 1 with the pulling rate of 7mm/min; Behind crystal pulling 30min, crystal pulling finishes, and takes out after cooling to room temperature with the furnace, obtains the Ni of rhenium-containing 3Al base single crystal alloy.
The Ni of the rhenium-containing that obtains 3The density of Al base single crystal alloy is 7.90g/cm 3, crystalline orientation is (100), the orientation irrelevance is less than 12 °.Carry out mechanical property test and find the Ni of this rhenium-containing 3The high-temperature duration life of Al base single crystal alloy under 1100 ℃/130MPa is 255.17h.The Ni of this rhenium-containing 3Al base single crystal alloy unit elongation is 13.1%, and the end face shrinking percentage is 27.1%.
Embodiment 7:
A kind of Ni of rhenium-containing 3The preparation method of Al base single crystal alloy specifically comprises following step:
The first step: preparation liquid-metal-coolant;
Described liquid-metal-coolant is gallium indium alloy or metallic tin.The preparation of said gallium indium alloy: with raw material high purity gallium (Ga) and high purity indium (In); By weight percentage: gallium 10wt%, all the other are indium, take by weighing; Put into beaker be heated to 80 ℃～200 ℃ its reaction is in a liquid state after; Pour in the liquid metal cooling tank 1 as heat-eliminating medium, adopt the vacuum pump oil heating to make the cooling tank temperature maintenance around the liquid metal cooling tank 1, make the gallium indium alloy keep liquid at 15 ℃;
Second step: the Ni of preparation rhenium-containing 3Al base alloy coupon;
(1) will prepare the Ni of rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo), high-purity rhenium (Re), high-purity dysprosium (Dy) and high-purity yttrium (Y) by weight percentage: the Al of 7.4wt%, 13% Mo, 1% Re; The Dy of 0.3wt%; The Y of 0.9wt%, all the other are Ni, take by weighing; And, Ni, Mo, Re, Dy and Y are put into ZGJL-0.025 type vacuum induction furnace with after acetone and the oven dry.
(2) vacuum induction furnace is evacuated to below the 0.6Pa, 1504 ℃ of feeding temperature-raising to alloying smelting temperature, alloying smelting is after 14 minutes; After being warming up to 1560 ℃; Be incubated 5 minutes, outage is cooled to 1504 ℃, adds rafifinal (Al); Again proceeded alloying smelting 5 minutes to electricity, the Ni of rhenium-containing is processed in charged casting 3Al base alloy bar material.
(3) at the Ni of rhenium-containing 3Use wire cutting method to cut out diameter on the Al base alloy bar material and be 18mm, length equals the cylinder coupon A of 200mm, with cleaning, drying after the polished finish of this cylinder coupon A surface finish, obtains the Ni of rhenium-containing 3Al base alloy coupon.
The 3rd step: prepare the not Ni of rhenium-containing 3Al base alloy seed crystal;
Ni at common not rhenium-containing 3Al base single crystal alloy raw material (crystalline orientation preferred (100) or (111); The orientation irrelevance is less than 12 °) to cut out diameter be 12mm to line; Length is the cylinder coupon B of 30mm, after this cylinder coupon B surface economy-combat grinding and polishing optical processing and corrosion treatment, obtains the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is with this Ni of rhenium-containing not 3Al base single crystal alloy seed crystal is enclosed in the ceramic shell mould with alumina slurry, keeps the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is coaxial with ceramic shell mould, and is in the central position of ceramic shell mould, puts into drying baker, in 150 ℃, is incubated 4 hours;
The Ni of described common not rhenium-containing 3The composition of Al base single crystal alloy according to weight percent is: the Al of 7.4wt%, and 13% Mo, all the other are Ni.
It is 22mm that described ceramic shell mould is preferably diameter, and length equals 250mm; Described polished finish is specially: adopt 400# and 800#SiO successively 2Coated abrasive working, polished finish on polishing machine then; Described corrosion treatment is specially: behind the employing of the sample after polished finish etching reagent corrosion 15min, take out and dry with the clean back of ultrasonic cleaning; Described etching reagent is preferably the mixing liquid of hydrochloric acid and hydrogen peroxide, adds 100ml hydrogen peroxide (concentration is 30%) in every 100ml hydrochloric acid (concentration is 36%); Described alumina slurry is 300 purpose Al by granularity 2O 3The mixed slurry that powder and silica gel are formed, every 100gAl 2O 3Add 60ml silica gel in the powder.
The 4th step: with the Ni of rhenium-containing 3Al base alloy coupon is vertically put into and is had the not Ni of rhenium-containing 3In the ceramic shell mould of Al base alloy seed crystal, will have the Ni of rhenium-containing again 3The Al base alloy coupon and the Ni of rhenium-containing not 3The ceramic shell mould of Al base single crystal alloy seed crystal is put into the oriented monocrystalline stove together;
The 5th step: the vacuum of oriented monocrystalline stove is evacuated to 0.17Pa, regulates in the oriented monocrystalline stove temperature to 1603 ℃, be incubated 8 minutes, treat the Ni of rhenium-containing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal melts fully, makes the Ni of the rhenium-containing of ceramic shell mould, thawing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal moves down in the entering liquid metal cooling tank 1 with the pulling rate of 5mm/min; Finish after drawing 40min, take out after cooling to room temperature with the furnace, obtain the Ni of rhenium-containing 3Al base single crystal alloy.
The Ni of the rhenium-containing that obtains 3The density of Al base single crystal alloy is 7.85g/cm 3Carry out mechanical property test and find the Ni of this rhenium-containing 3The high-temperature duration life of Al base single crystal alloy under 1100 ℃/130MPa is 219.31h.The Ni of this rhenium-containing 3Al base single crystal alloy unit elongation is 10.4%, and the end face shrinking percentage is 29.1%.
Embodiment 8:
A kind of Ni of rhenium-containing 3The preparation method of Al base single crystal alloy specifically comprises following step:
The first step: preparation liquid-metal-coolant;
Described liquid-metal-coolant is gallium indium alloy or metallic tin.The preparation of said gallium indium alloy: with raw material high purity gallium (Ga) and high purity indium (In); By weight percentage: gallium 30wt%, all the other are indium, take by weighing; Put into beaker be heated to 80 ℃～200 ℃ its reaction is in a liquid state after; Pour in the liquid metal cooling tank 1 as heat-eliminating medium, adopt the vacuum pump oil heating to make the cooling tank temperature maintenance around the liquid metal cooling tank 1, make the gallium indium alloy keep liquid at 15 ℃;
Second step: the Ni of preparation rhenium-containing 3Al base alloy coupon;
(1) will prepare the Ni of rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo), high-purity rhenium (Re), high-purity dysprosium (Dy) and high-purity yttrium (Y) by weight percentage: the Al of 7.4wt%; 10% Mo, 3% Re, the Dy of 0.06wt%; The Y of 0.5wt%; All the other take by weighing for Ni, and with after acetone and the oven dry, Ni, Mo, Re, Dy and Y are put into ZGJL-0.025 type vacuum induction furnace.
(2) vacuum induction furnace is evacuated to below the 0.7Pa, 1520 ℃ of feeding temperature-raising to alloying smelting temperature, alloying smelting is after 20 minutes; After being warming up to 1550 ℃; Be incubated 5 minutes, outage is cooled to 1520 ℃, adds rafifinal (Al); Again proceeded alloying smelting 6 minutes to electricity, the Ni of rhenium-containing is processed in charged casting 3Al base alloy bar material.
(3) at the Ni of rhenium-containing 3Use wire cutting method to cut out diameter on the Al base alloy bar material and be 20mm, length equals the cylinder coupon A of 200mm, with cleaning, drying after the polished finish of this cylinder coupon A surface finish, obtains the Ni of rhenium-containing 3Al base alloy coupon.
The 3rd step: prepare the not Ni of rhenium-containing 3Al base alloy seed crystal;
Ni at common not rhenium-containing 3Al base single crystal alloy raw material (crystalline orientation is (111), and the orientation irrelevance is less than 12 °) is reached the standard grade and cut out diameter is 12mm, and length is the cylinder coupon B of 60mm, after this cylinder coupon B surface economy-combat grinding and polishing optical processing and corrosion treatment, obtains the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is with this Ni of rhenium-containing not 3Al base single crystal alloy seed crystal is enclosed in the ceramic shell mould with alumina slurry, keeps the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is coaxial with ceramic shell mould, and is in the central position of ceramic shell mould, puts into drying baker, in 150 ℃, is incubated 4 hours;
The Ni of described common not rhenium-containing 3The composition of Al base single crystal alloy according to weight percent is: the Al of 7.4wt%, and 10% Mo, all the other are Ni.
Described ceramic shell mould is preferably 99 porcelain ceramic shell moulds, and diameter is 17mm, and length equals 250mm; Described polished finish is specially: adopt 400# and 800#SiO successively 2Coated abrasive working, polished finish on polishing machine then; Described corrosion treatment is specially: behind the employing of the sample after polished finish etching reagent corrosion 15min, take out and dry with the clean back of ultrasonic cleaning; Described etching reagent is preferably the mixing liquid of hydrochloric acid and hydrogen peroxide, adds 60ml hydrogen peroxide (concentration is 30%) in every 100ml hydrochloric acid (concentration is 38%); Described alumina slurry is 100 purpose Al by granularity 2O 3The mixed slurry that powder and silica gel are formed, every 100gAl 2O 3Add 60ml silica gel in the powder.
The 4th step: with the Ni of rhenium-containing 3Al base alloy coupon is vertically put into and is had the not Ni of rhenium-containing 3In the ceramic shell mould of Al base alloy seed crystal, will have the Ni of rhenium-containing again 3The Al base alloy coupon and the Ni of rhenium-containing not 3The ceramic shell mould of Al base single crystal alloy seed crystal is put into the oriented monocrystalline stove together;
The 5th step: the vacuum of oriented monocrystalline stove is evacuated to 0.17Pa, regulates in the oriented monocrystalline stove temperature to 1603 ℃, be incubated 10 minutes, treat the Ni of rhenium-containing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal melts fully, makes the Ni of the rhenium-containing of ceramic shell mould, thawing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal moves down in the entering liquid metal cooling tank 1 with the pulling rate of 8mm/min; After reaching crystal pulling time 28min, crystal pulling finishes, and takes out after cooling to room temperature with the furnace, obtains the Ni of rhenium-containing 3Al base single crystal alloy.
The Ni of the rhenium-containing that obtains 3The density of Al base single crystal alloy is 8.00g/cm 3, crystalline orientation is (111), the orientation irrelevance is less than 12 °.Carry out mechanical property test and find the Ni of this rhenium-containing 3The high-temperature duration life of Al base single crystal alloy under 1100 ℃/130MPa is 281.25h.The Ni of this rhenium-containing 3Al base single crystal alloy unit elongation is 14.6%, and the end face shrinking percentage is 30.2%.
Embodiment 9:
Basic identical among present embodiment and the embodiment 8, difference only is the Ni of preparation rhenium-containing in the step 2 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo), high-purity rhenium (Re), high-purity dysprosium (Dy) and high-purity yttrium (Y) by weight percentage: the Al of 7wt%; 8% Mo, 0.0005% Re, the Dy of 0.1wt%; The Y of 0.1wt%, all the other are Ni.
Embodiment 10:
Basic identical among present embodiment and the embodiment 8, difference only is the Ni of the preparation rhenium-containing in the step 2 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo), high-purity rhenium (Re), high-purity dysprosium (Dy) and high-purity yttrium (Y) by weight percentage: the Al of 8wt%; 12.5% Mo, 1.5% Re, the Dy of 0.01wt%; The Y of 0.5wt%, all the other are Ni.
Embodiment 11:
A kind of Ni of rhenium-containing 3The preparation method of Al base single crystal alloy comprises following step:
The first step: preparation liquid-metal-coolant;
Described liquid-metal-coolant is the gallium indium alloy.The preparation of said gallium indium alloy: with raw material high purity gallium (Ga) and high purity indium (In); By weight percentage: gallium 10wt%, all the other are indium, take by weighing; Put into beaker be heated to 80 ℃ ℃ its reaction is in a liquid state after; Pour in the liquid metal cooling tank as heat-eliminating medium, adopt the vacuum pump oil heating to make the cooling tank temperature maintenance around the liquid metal cooling tank, make the gallium indium alloy keep liquid at 15 ℃;
Second step: the Ni of preparation rhenium-containing 3Al base alloy coupon;
(1) will prepare the Ni of rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo) and high-purity rhenium (Re) according to weight percent are: the Al of 7～8wt%; 8～13% Mo; 0.0005 the Re of～3wt%; All the other take by weighing for Ni, and with after acetone and the oven dry, Ni, Mo and Re are put into vacuum induction furnace.
(2) vacuum induction furnace is evacuated to 1Pa, 1520 ℃ of feeding temperature-raising to alloying smelting temperature, alloying smelting is after 10 minutes; After being warming up to 1570 ℃; Be incubated 5 minutes, outage is cooled to 1510 ℃, adds rafifinal (Al); Again proceeded alloying smelting 5 minutes to electricity, the Ni of rhenium-containing is processed in charged casting 3Al base alloy bar material.
(3) at the Ni of rhenium-containing 3Use wire cutting method to cut out diameter on the Al base alloy bar material and be 15mm, length equals the cylinder coupon A of 200mm, with cleaning, drying after the polished finish of this cylinder coupon A surface finish, obtains the Ni of rhenium-containing 3Al base alloy coupon.
The 3rd step: prepare the not Ni of rhenium-containing 3Al base alloy seed crystal;
Ni at common not rhenium-containing 3Al base single crystal alloy raw material (crystalline orientation is (100), and the orientation irrelevance is less than 12 °) is reached the standard grade and cut out diameter is 6mm, and length is the cylinder coupon B of 30mm, after this cylinder coupon B surface economy-combat grinding and polishing optical processing and corrosion treatment, obtains the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is with this Ni of rhenium-containing not 3Al base single crystal alloy seed crystal is enclosed in the ceramic shell mould with alumina slurry, keeps the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is coaxial with ceramic shell mould, and is in the central position of ceramic shell mould, puts into drying baker, in 130 ℃, is incubated 2 hours;
The Ni of described common not rhenium-containing 3The composition of Al base single crystal alloy according to weight percent is: the Al of 7wt%, and 8% Mo, all the other are Ni.
Described ceramic shell mould is preferably the round ceramic formwork, and diameter is 17mm, and length equals 250mm; Described polished finish is specially: adopt 400# and 800#SiO successively 2Coated abrasive working, polished finish on polishing machine then; Described corrosion treatment is specially: behind the employing of the sample after polished finish etching reagent corrosion 10min, take out and dry with the clean back of ultrasonic cleaning; Described etching reagent is preferably the mixing liquid of hydrochloric acid and hydrogen peroxide, adds 100ml hydrogen peroxide (concentration is 30%) in every 100ml hydrochloric acid (concentration is 38%); Described alumina slurry is 80 purpose Al by granularity 2O 3The mixed slurry that powder and silica gel are formed, every 100gAl 2O 3Add 50ml silica gel in the powder.
The 4th step: with the Ni of rhenium-containing 3Al base alloy coupon is vertically put into and is had the not Ni of rhenium-containing 3In the ceramic shell mould of Al base alloy seed crystal, will have the Ni of rhenium-containing again 3The Al base alloy coupon and the Ni of rhenium-containing not 3The ceramic shell mould of Al base single crystal alloy seed crystal is put into the oriented monocrystalline stove together;
The 5th step: the vacuum of oriented monocrystalline stove is evacuated to 0.1Pa, regulates in the oriented monocrystalline stove temperature to 1600 ℃, be incubated 5 minutes, treat the Ni of rhenium-containing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal melts fully, makes the Ni of the rhenium-containing of ceramic shell mould, thawing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal moves down in the entering liquid metal cooling tank with the pulling rate of 7.5mm/min; Ni according to rhenium-containing 3The length of Al base alloy coupon and pulling rate are calculated the crystal pulling time, and (the crystal pulling time equals the Ni of rhenium-containing 3The length of Al base alloy coupon is divided by pulling rate), when crystal pulling how long behind the 38min, crystal pulling finishes, and takes out after cooling to room temperature with the furnace, obtains the Ni of rhenium-containing 3Al base single crystal alloy.
Embodiment 12:
A kind of Ni of rhenium-containing 3The preparation method of Al base single crystal alloy comprises following step:
The first step: preparation liquid-metal-coolant;
Described liquid-metal-coolant is a metallic tin.
The preparation of said metallic tin: the raw material high purity tin is heated to melting temperature (232 ℃) it is in a liquid state, pour into then in the liquid metal cooling tank, adopting the vacuum pump oil heating to make the cooling tank temperature around the liquid metal cooling tank is 300 ℃, makes metallic tin keep liquid.
Second step: the Ni of preparation rhenium-containing 3Al base alloy coupon;
(1) will prepare the Ni of rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo) and high-purity rhenium (Re) by weight percentage: the Al of 8wt%, 13% Mo, the Re of 3wt%, all the other take by weighing for Ni, and Ni, Mo and Re are put into vacuum induction furnace.
(2) vacuum induction furnace is evacuated to 1Pa, 1510 ℃ of feeding temperature-raising to alloying smelting temperature, alloying smelting is after 30 minutes; After being warming up to 1550 ℃; Be incubated 10 minutes, outage is cooled to 1500 ℃, adds rafifinal (Al); Again proceeded alloying smelting 10 minutes to electricity, the Ni of rhenium-containing is processed in charged casting 3Al base alloy bar material.
(3) at the Ni of rhenium-containing 3Use wire cutting method to cut out diameter on the Al base alloy bar material and be 20mm, length with cleaning, drying after the polished finish of this cylinder coupon A surface finish, obtains the Ni of rhenium-containing smaller or equal to the cylinder coupon A of 200mm 3Al base alloy coupon.
The 3rd step: prepare the not Ni of rhenium-containing 3Al base alloy seed crystal;
Ni at common not rhenium-containing 3Al base single crystal alloy raw material (crystalline orientation is (111), and the orientation irrelevance is less than 12 °) is reached the standard grade and cut out diameter is 12mm, and length is the cylinder coupon B of 60mm, after this cylinder coupon B surface economy-combat grinding and polishing optical processing and corrosion treatment, obtains the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is with this Ni of rhenium-containing not 3Al base single crystal alloy seed crystal is enclosed in the ceramic shell mould with alumina slurry, keeps the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is coaxial with ceramic shell mould, and is in the central position of ceramic shell mould, puts into drying baker, in 130 ℃, is incubated 4 hours;
The Ni of described common not rhenium-containing 3The composition of Al base single crystal alloy according to weight percent is: the Al of 8wt%, and 13% Mo, all the other are Ni.
Described ceramic shell mould is preferably the round ceramic formwork, and diameter is 22mm, and length is smaller or equal to 250mm; Described polished finish is specially: adopt 400# and 800#SiO successively 2Coated abrasive working, polished finish on polishing machine then; Described corrosion treatment is specially: behind the employing of the sample after polished finish etching reagent corrosion 15min, take out and dry with the clean back of ultrasonic cleaning; Described etching reagent is preferably the mixing liquid of hydrochloric acid and hydrogen peroxide, adds 60ml hydrogen peroxide (concentration is 30%) in every 100ml hydrochloric acid (concentration is 38%); Described alumina slurry is 320 purpose Al by granularity 2O 3The mixed slurry that powder and silica gel are formed, every 100gAl 2O 3Add 60ml silica gel in the powder.
The 4th step: with the Ni of rhenium-containing 3Al base alloy coupon is vertically put into and is had the not Ni of rhenium-containing 3In the ceramic shell mould of Al base alloy seed crystal, will have the Ni of rhenium-containing again 3The Al base alloy coupon and the Ni of rhenium-containing not 3The ceramic shell mould of Al base single crystal alloy seed crystal is put into the oriented monocrystalline stove together;
The 5th step: the vacuum of oriented monocrystalline stove is evacuated to 0.5Pa, regulates in the oriented monocrystalline stove temperature to 1650 ℃, be incubated 10 minutes, treat the Ni of rhenium-containing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal melts fully, makes the Ni of the rhenium-containing of ceramic shell mould, thawing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal moves down in the entering liquid metal cooling tank with the pulling rate of 8mm/min; Ni according to rhenium-containing 3The length of Al base alloy coupon and pulling rate are calculated the crystal pulling time, and (the crystal pulling time equals the Ni of rhenium-containing 3The length of Al base alloy coupon is divided by pulling rate), after reaching crystal pulling time 35min, crystal pulling finishes, and takes out after cooling to room temperature with the furnace, obtains the Ni of rhenium-containing 3Al base single crystal alloy.
Embodiment 13:
The difference of present embodiment and embodiment 1 only was for second step (1): the Ni that will prepare rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo) and high-purity rhenium (Re) be the Al of 7.4wt% by weight percentage; 13% Mo, 0.5% Re, the Y of 0.1wt%; All the other take by weighing for Ni, and Ni, Mo, Y are put into vacuum induction furnace.Its preparation process is identical with the preparation process of embodiment 1.
Embodiment 14:
The difference of present embodiment and embodiment 1 only was for second step (1): the Ni that will prepare rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo) and high-purity rhenium (Re) be the Al of 7.4wt% by weight percentage; 13% Mo, 0.5% Re, the Y of 1wt%; All the other take by weighing for Ni, and Ni, Mo, Y are put into vacuum induction furnace.Its preparation process is identical with the preparation process of embodiment 1.
Embodiment 15:
The difference of present embodiment and embodiment 1 only was for second step (1): the Ni that will prepare rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo) and high-purity rhenium (Re) are the Al of 7.4wt% by weight percentage; 13% Mo, 0.5% Re, the Dy of 0.1wt%; The Y of 1wt%; The Hf of 0.05wt%, all the other take by weighing for Ni, and Ni, Mo, Re, Dy, Y and Hf are put into vacuum induction furnace.Its preparation process is identical with the preparation process of embodiment 1.
Embodiment 16:
The difference of present embodiment and embodiment 1 only was for second step (1): the Ni that will prepare rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo) and high-purity rhenium (Re) are the Al of 7.4wt% by weight percentage; 13% Mo, 0.5% Re, the Dy of 0.1wt%; The Y of 1wt%; The Hf of 0.5wt%, all the other take by weighing for Ni, and Ni, Mo, Re, Dy, Y and Hf are put into vacuum induction furnace.Its preparation process is identical with the preparation process of embodiment 1.

Claims (9)

1. Ni who adopts the liquid metal method of cooling to prepare rhenium-containing 3The method of Al base single crystal alloy is characterized in that: comprise following step:
The first step: the preparation liquid-metal-coolant, liquid-metal-coolant is gallium indium alloy or metallic tin;
Second step: the Ni of preparation rhenium-containing 3Al base alloy coupon;
The 3rd step: prepare the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal, and with this Ni of rhenium-containing not 3Al base single crystal alloy seed crystal is enclosed in the ceramic shell mould with alumina slurry;
The 4th step: with the Ni of rhenium-containing 3Al base alloy coupon is vertically put into and is had the not Ni of rhenium-containing 3In the ceramic shell mould of Al base single crystal alloy seed crystal, will have the Ni of rhenium-containing again 3The Al base alloy coupon and the Ni of rhenium-containing not 3The ceramic shell mould of Al base single crystal alloy seed crystal is put into the oriented monocrystalline stove together;
The 5th step: the vacuum of oriented monocrystalline stove is evacuated to 1 * 10 -1～5 * 10 -1Pa regulates in the oriented monocrystalline stove temperature to 1600 ℃～1650 ℃, is incubated 5～10 minutes, treats the Ni of rhenium-containing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal melts fully, makes the Ni of the rhenium-containing of ceramic shell mould, thawing 3The Al base alloy coupon and the Ni of rhenium-containing not 3Al base single crystal alloy seed crystal moves down in the entering liquid metal cooling tank with the pulling rate of 2～10mm/min; Ni according to rhenium-containing 3The length and the pulling rate of Al base alloy coupon are calculated the crystal pulling time, and after reaching the crystal pulling time, crystal pulling finishes, and take out after cooling to room temperature with the furnace, obtain the Ni of rhenium-containing 3Al base single crystal alloy.
2. a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing according to claim 1 3The method of Al base single crystal alloy; It is characterized in that: when described liquid-metal-coolant was the gallium indium alloy, the preparation method was: with raw material high purity gallium and high purity indium, by weight percentage: gallium 10～30wt%; All the other are indium; Take by weighing, put into beaker be heated to 80～200 ℃ its reaction is in a liquid state after, pour in the liquid metal cooling tank as heat-eliminating medium; Adopt the vacuum pump oil heating to make the cooling tank temperature maintenance around the liquid metal cooling tank, make the gallium indium alloy keep liquid more than 15 ℃.
3. a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing according to claim 1 3The method of Al base single crystal alloy; It is characterized in that: when described liquid-metal-coolant is metallic tin; The preparation method is: the raw material high purity tin is heated to melting temperature it is in a liquid state; Pour into then in the liquid metal cooling tank, adopting the vacuum pump oil heating to make the cooling tank temperature around the liquid metal cooling tank is 250～300 ℃, makes metallic tin keep liquid.
4. according to claim 2 or 3 described a kind of Ni that adopt the liquid metal method of cooling to prepare rhenium-containing 3The method of Al base single crystal alloy, it is characterized in that: described vacuum pump oil is the VM100 vacuum pump oil.
5. a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing according to claim 1 3The method of Al base single crystal alloy is characterized in that: described second step is specially:
(1) will prepare the Ni of rhenium-containing 3Al base alloy materials: high purity nickel (Ni), rafifinal (Al), high-purity molybdenum (Mo) and high-purity rhenium (Re) by weight percentage: the Al of 7～8wt%; 8～13% Mo; 0.0005 the Re of～3wt%, all the other are Ni, take by weighing; And, Ni, Mo and Re are put into vacuum induction furnace with after acetone and the oven dry;
(2) vacuum induction furnace is evacuated to below the 1Pa, 1510 ± 10 ℃ of feeding temperature-raising to alloying smelting temperature, alloying smelting is after 10～30 minutes; After being warming up to 1560 ± 10 ℃; Be incubated 5～10 minutes, outage is cooled to 1500 ± 10 ℃, adds rafifinal (Al); Again proceeded alloying smelting 5～10 minutes to electricity, the Ni of rhenium-containing is processed in charged casting 3Al base alloy bar material;
(3) at the Ni of rhenium-containing 3Using wire cutting method to cut out diameter on the Al base alloy bar material is 15～20mm, and length with cleaning, drying after the polished finish of this cylinder coupon A surface finish, obtains the Ni of rhenium-containing smaller or equal to the cylinder coupon A of 200mm 3Al base alloy coupon.
6. a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing according to claim 5 3The method of Al base single crystal alloy is characterized in that: the Ni of rhenium-containing in the described step (1) 3When containing more than one Dy, Y or Hf in the Al base alloy; Dy, Y or Hf composition are respectively the Dy of 0.05～0.5wt%, the Y of 0.1～1wt% or the Hf of 0.05～0.5wt% by weight percentage; After taking by weighing according to weight percent respectively, more than one Dy, Y or Hf put into vacuum induction furnace with Ni, Mo and Re.
7. a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing according to claim 1 3The method of Al base single crystal alloy is characterized in that: described the 3rd step is specially: at the Ni of common not rhenium-containing 3Al base single crystal alloy raw material is reached the standard grade and cut out diameter is 6～12mm, and length is the cylinder coupon B of 30～60mm, after this cylinder coupon B surface economy-combat grinding and polishing optical processing and corrosion treatment, obtains the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is with this Ni of rhenium-containing not 3Al base single crystal alloy seed crystal is enclosed in the ceramic shell mould with alumina slurry, keeps the not Ni of rhenium-containing 3Al base single crystal alloy seed crystal is coaxial with ceramic shell mould, and is in the central position of ceramic shell mould, puts into drying baker, in 130～150 ℃, is incubated 2～4 hours.
8. a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing according to claim 7 3The method of Al base single crystal alloy is characterized in that: the Ni of described common not rhenium-containing 3The composition of Al base single crystal alloy according to weight percent is: the Al of 7～8wt%, and 8～13% Mo, all the other are Ni.
9. a kind of Ni that adopts the liquid metal method of cooling to prepare rhenium-containing according to claim 1 3The method of Al base single crystal alloy, it is characterized in that: described liquid metal cooling tank is installed on the basetray of oriented monocrystalline stove, and encapsulation process.
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