CN109082710A - A kind of preparation method of the nickel-base high-temperature single crystal alloy coupon of chemical component continuous gradient distribution - Google Patents
A kind of preparation method of the nickel-base high-temperature single crystal alloy coupon of chemical component continuous gradient distribution Download PDFInfo
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- CN109082710A CN109082710A CN201811079655.7A CN201811079655A CN109082710A CN 109082710 A CN109082710 A CN 109082710A CN 201811079655 A CN201811079655 A CN 201811079655A CN 109082710 A CN109082710 A CN 109082710A
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- single crystal
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/52—Alloys
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/14—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method characterised by the seed, e.g. its crystallographic orientation
Abstract
The invention discloses a kind of preparation methods of the nickel-base high-temperature single crystal alloy coupon of chemical component continuous gradient distribution, belong to technical field of metal material preparation.This method realizes crystal growth by directional solidification processes using the high-melting-point single crystal alloy for being placed on formwork lower end as seed crystal.In the case where two kinds of alloys are completely melt state, two kinds of aluminium alloys are mutually mixed by convection current or diffusion, to change alloying component, generate component gradient.This method can be realized the other component gradient distribution of Centimeter Level in nickel-based monocrystal sample, can satisfy the demand of the macro-mechanical properties such as lasting, creep research.
Description
Technical field
The present invention relates to technical field of metal material preparation, and in particular to a kind of distribution of chemical component continuous gradient it is Ni-based
The preparation method of single crystal super alloy coupon.
Background technique
In June, 2011, US President Barack Obama Carnegie Mellon University make with " advanced manufacturing industry partnership "
" material genome plan " (Materials Genome Initiative, MGI) is proposed in the speech being the theme, and is clearly referred to
Its general objective is to utilize the breakthrough for calculating, obtaining in terms of high-throughput experiment and data mining in material simulation in recent years out, will be new
Speed of the material from discovery to application at least doubles, and cost at least reduces half.MGI presents the following advanced material exploitation
Brand-new mode.In recent years, domestic " the material genome plan " for also starting Chinese version, greatly develops material genome skill
Art.High Throughput Preparation as one of material genome-based technologies achieves more significant development.The high pass of metal material
Measure preparation method there are many, including combinatorial material chip approach, powder metallurgy process, 3D printing method, based on common melting cast
Make new equipment, the polynary section method of diffusion etc. of exploitation.Wherein, combinatorial material chip approach is not particularly suited for high temperature alloy neck
Domain；The methods of powder metallurgy, 3D printing and new equipment based on the exploitation of common melting and casting are all by controlling raw material powder
The accurate change of gradient matched to realize material composition of ingredient, the material of acquisition is polycrystalline alloy；Spread polynary section method
Although capableing of the monocrystalline sample of prepared composition gradient distribution, the distribution distance of gradient components is very narrow (about 200 μm), Bu Nengman
The demand of sufficient macro-mechanical property (such as lasting, creep) research.Currently, being suitable for the high-throughput preparation of nickel-base high-temperature single crystal alloy
Method has not been reported.
Summary of the invention
The purpose of the present invention is to provide a kind of nickel-base high-temperature single crystal alloy coupons of chemical component continuous gradient distribution
Preparation method can be realized the other component gradient distribution of Centimeter Level in nickel-based monocrystal sample, can satisfy the macroscopic views such as lasting, creep
The demand of mechanical property research.
To achieve the above object, the technical solution adopted in the present invention is as follows:
A kind of preparation method of the nickel-base high-temperature single crystal alloy coupon of chemical component continuous gradient distribution, the chemical component
Continuous gradient distribution nickel-base high-temperature single crystal alloy refer to, the element A content distribution gradient in alloy composition, except nickel with
Then content remains unchanged outer other elements；The preparation method of the nickel-base high-temperature single crystal alloy coupon the following steps are included:
(1) prepared by formwork: the formwork includes formwork chassis and the oxidation for installing nickel-base high-temperature single crystal alloy coupon
Aluminum pipe drills on the formwork chassis, and alumina tube is inserted into the hole on formwork chassis and fixed (coating can be used to fix)；
(2) alloy bar material prepares: according to the distribution of element A content in subject alloy coupon, preparing element A respectively and contains
The alloy bar material that the alloy bar material and element A content that amount is a1 are a2, wherein the relatively high alloying component of fusing point is prepared into monocrystalline
The alloy bar material of state, it is low-melting, it does not require；The diameter of alloy bar material is slightly less than the internal diameter of alumina tube on formwork；Together
When, for the monocrystalline state alloy bar material of high-melting-point ingredient as seed crystal, length is greater than 3cm；Two bars are placed in aluminium oxide after being connected to each other
Guan Zhong；
(3) it the nickel-base high-temperature single crystal alloy coupon of preparation chemical component continuous gradient distribution: uses high speed freezing method (HRS)
Formwork, is fixed on aqueous cold plate by preparation first, is placed in holding furnace；The temperature and smelting time of holding furnace are needed according to two kinds
The contact surface type of ingredient coupon determines that vacuum degree≤1Pa in furnace, the withdrawing rate of directional solidification is 3~6mm/min.
In above-mentioned steps (1), the formwork chassis is prepared using conventional method, is wrapped by coating to collar plate shape wax-pattern
Wrap up in, air-dry, dewaxing, polish after obtain；The material of the alumina tube is high purity aluminium oxide, according to required coupon size selection oxygen
Change the internal diameter of aluminum pipe, the quantity of alumina tube is determined according to experiment demand.
In above-mentioned steps (2), the element A refers to any host element in nickel-base high-temperature single crystal alloy in addition to nickel；
The distribution of element A weight percentage is a1%~a2% in subject alloy coupon, and (a1 is content lower limit to a1 < a2, and a2 is
Upper content limit).
In above-mentioned steps (2), the high-melting-point bar as seed crystal is placed on alumina tube lower part, and another bar is placed on aluminium oxide
The top of pipe, the contact surface of two bars guarantee clean, fitting.
In above-mentioned steps (2), when two bars are connected to each other, contact surface is flat face or lozenges；The flat face refers to
Contact surface is perpendicular to alumina tube axial direction, and the lozenges refers to contact surface and alumina tube axial direction angulation is 0 °~90 °
Between.
In above-mentioned steps (2), when two bars dock, the selection principle of contact surface are as follows: when the density of high-melting-point bar is small
When low melting point bar, contact surface is flat face；When the density of high-melting-point bar is greater than low melting point bar, then contact surface is wedge
Shape face；The height of lozenges is depending on the length of required gradient components.
In above-mentioned steps (3), the selection principle of furnace temperature and smelting time is kept the temperature are as follows: when contact surface is flat face, protect
Warm furnace temperature should be higher than that 50~100 DEG C of lower end high-melting-point bar fusing point, 20~40min of smelting time；When contact surface is lozenges
When, heat preservation furnace temperature should be higher than that 100~150 DEG C of lower end high-melting-point bar fusing point, 2~4h of smelting time.
The principle of the present invention is as follows:
Using high-melting-point single crystal alloy as seed crystal, crystal growth is realized by directional solidification processes.It is complete in two kinds of alloys
Under running down state, two kinds of aluminium alloys are mutually mixed by convection current or diffusion, to change alloying component, generate ingredient ladder
Degree.When the density of upper end low-melting alloy is greater than lower end high-melting-point alloy, convection current can occur for two kinds of aluminium alloys, be mutually mixed,
To change alloying component, component gradient is generated.At this point, the contact surface of two kinds of alloys is flat face, kept the temperature by reducing
Furnace temperature shortens the speed and distance of smelting time control aluminium alloy convection current.And under the density of upper end low-melting alloy is less than
When holding high-melting-point alloy, convection current does not occur for aluminium alloy, and the contact surface that two kinds of alloys are arranged is lozenges, by element in aluminium alloy
In diffusion realize two kinds of alloy fusions in the radial direction.In the wedge contact section of two kinds of alloys, two kinds of any one cross section
Specific gravity shared by alloy is different from, to generate component gradient.Since the diffusion rate of element is slower, heat preservation is improved
Furnace temperature increases smelting time, to ensure the adequacy of radial diffusion.
Beneficial effects of the present invention are as follows:
(1) the preparation side of the nickel-base high-temperature single crystal alloy coupon of a kind of chemical component continuous gradient distribution provided by the invention
Method can disposably prepare the single crystal samples of Multiple components gradient distribution, greatly improve the system of experiment single crystal samples
Standby efficiency, reduces experimental cost, belongs to a kind of high-throughput preparation method.
(2) formwork structure that the present invention uses is simple, easily prepares, and can adjust the diameter of monocrystalline coupon according to actual needs
And radical, there is great flexibility.
(3) in Crystal Nickel-based Superalloy coupon prepared by the present invention, the distribution distance of gradient components can reach a centimetre rank,
The processing that can be used for the samples such as lasting, creep, the iron-enriched yeast for mechanical property are studied.
Detailed description of the invention
Fig. 1 is the flow diagram of preparation method of the present invention；In figure: 1- alumina tube, 2- formwork chassis, 3- aqueous cold plate,
4- calandria, 5- high-melting-point alloy bar, 6- low-melting alloy bar.
Fig. 2 is the composition analysis result of 1 tantalum content change of gradient monocrystalline coupon of the embodiment of the present invention.
Fig. 3 is the composition analysis result of 2 chromium content change of gradient monocrystalline coupon of the embodiment of the present invention.
Specific embodiment
It elaborates below with reference to embodiment to the present invention, but protection scope of the present invention is not limited only to following implementations
Example.
Embodiment 1:
The present embodiment is the preparation of the nickel-base high-temperature single crystal alloy coupon of tantalum (Ta) content continuous gradient distribution, specific steps
Are as follows:
(1) prepared by formwork: the preparation of formwork chassis 2 uses conventional method, is wrapped up by coating collar plate shape wax-pattern, wind
Do, dewax, polish after obtain.The high purity aluminium oxide pipe that the formwork of monocrystalline coupon is 10mm using internal diameter is installed, length is
150mm, radical are 4.Formwork chassis is drilled, is inserted into alumina tube 1, and fixed with coating.
(2) alloy bar material prepares: according to the change of gradient range (5~9wt%) of designed Ta content, preparing respectively
The alloy of two kinds of ingredients of 5wt%Ta and 9wt%Ta, specific ingredient are as shown in table 1.Alloy melting point containing 5wt%Ta is high, is prepared into
The monocrystalline coupon of diameter 16mm；Alloy smelting containing 9wt%Ta is at alloy pig.Two kinds of alloys are processed into the stick of diameter 9.8mm
Material, length are 6cm, and contact surface is processed into flat face.Two kinds of alloy bar materials are fitted on formwork in alumina tube, 5wt% is contained
The high-melting-point alloy bar 5 of Ta is placed on lower end, and the low-melting alloy bar 6 containing 9wt%Ta is placed on upper end, the contact of two kinds of coupons
Face guarantees clean, fitting.
The chemical component (wt%) of two kinds of alloys used in 1 embodiment 1 of table
| Alloy | Cr | Co | W | Mo | Ta | Al | Re | Ru | Ni |
| 5Ta | 3.5% | 8% | 6% | 1.5% | 5% | 6% | 5% | 3% | It is remaining |
| 9Ta | 3.5% | 8% | 6% | 1.5% | 9% | 6% | 5% | 3% | It is remaining |
(3) gradient components monocrystalline coupon gradient components coupon directional solidification: is prepared using high speed freezing method (HRS).By mould
Shell is fixed on aqueous cold plate 3, is risen up into holding furnace, and calandria 4 heats formwork in holding furnace.Keeping the temperature furnace temperature is 1480
DEG C, smelting time 30min, vacuum degree≤1Pa in furnace.After melting, using the withdrawing rate of 3mm/min by formwork from heat preservation
It is pulled out in furnace, that is, the nickel-base high-temperature single crystal alloy coupon of the distribution of Ta content continuous gradient needed for obtaining.
Constituent analysis is carried out to the longitudinal section of Ta concentration gradients variation monocrystalline coupon using the power spectrum of scanning electron microscope, as a result such as
Shown in Fig. 2.It can be seen from the figure that the distance of Ta concentration gradients variation is about 25mm, variation range substantially 5~
8.5wt%.
Embodiment 2:
The present embodiment is the preparation of the nickel-base high-temperature single crystal alloy coupon of chromium (Cr) content continuous gradient distribution, specific steps
Are as follows:
(1) prepared by formwork: the preparation of formwork chassis uses conventional method, is wrapped up by coating collar plate shape wax-pattern, wind
Do, dewax, polish after obtain.The formwork for installing monocrystalline coupon uses internal diameter for the high purity aluminium oxide pipe of 6mm, length 150mm,
Radical is 4.Formwork chassis is drilled, is inserted into alumina tube, and fixed with coating.
(2) alloy bar material prepares: according to the change of gradient range (2.5~6wt%) of Cr content, preparing 2.5wt% respectively
The alloy of two kinds of ingredients of Cr and 6wt%Cr, specific ingredient are as shown in table 2.2.5wt%Cr alloy melting point is high, is prepared into diameter
The monocrystalline coupon of 16mm；6wt%Cr alloy smelting is at alloy pig.Two kinds of alloys are processed into the coupon of diameter 5.8mm, length is equal
For 6cm, contact surface is processed into lozenges, lozenges height 25mm.Two kinds of alloy coupons are fitted into formwork, 2.5wt%Cr examination
Stick is placed on lower end, and 6wt%Cr coupon is placed on upper end, and the contact surface of two kinds of coupons guarantees clean, fitting.
The chemical component (wt%) of two kinds of alloys used in 2 embodiment 2 of table
| Alloy | Cr | Co | W | Mo | Ta | Al | Re | Ru | Ni |
| 2.5Cr | 2.5% | 8% | 5% | 1% | 8% | 6% | 5% | 3% | It is remaining |
| 6Cr | 6% | 8% | 5% | 1% | 8% | 6% | 5% | 3% | It is remaining |
(3) gradient components monocrystalline coupon gradient components coupon directional solidification: is prepared using high speed freezing method (HRS).By mould
Shell is fixed on aqueous cold plate, is risen up into holding furnace.Keeping the temperature furnace temperature is 1550 DEG C, smelting time 2h, vacuum degree≤1Pa in furnace.
After melting, formwork is pulled out out of holding furnace using the withdrawing rate of 5mm/min, that is, Cr content continuous gradient needed for obtaining
The nickel-base high-temperature single crystal alloy coupon of distribution.
Constituent analysis is carried out to the longitudinal section of Cr concentration gradients variation monocrystalline coupon using the power spectrum of scanning electron microscope, as a result such as
Shown in Fig. 3.It can be seen from the figure that the distance of Cr concentration gradients variation is about 20mm, variation range substantially 2.5~
6wt%.
Claims (7)
1. a kind of preparation method of the nickel-base high-temperature single crystal alloy coupon of chemical component continuous gradient distribution, it is characterised in that: institute
The nickel-base high-temperature single crystal alloy for stating the distribution of chemical component continuous gradient refers to that the element A content in alloy composition is in gradient
Distribution, then content remains unchanged the other elements in addition to nickel；The preparation method of the nickel-base high-temperature single crystal alloy coupon include with
Lower step:
(1) prepared by formwork: the formwork includes formwork chassis and the alumina tube for installing nickel-base high-temperature single crystal alloy coupon,
It drills on the formwork chassis, alumina tube is inserted into the hole on formwork chassis and fixed；
(2) alloy bar material prepares: according to the distribution of element A content in subject alloy coupon, preparing element A content respectively is
The alloy bar material and element A content of a1 is the alloy bar material of a2, and wherein the relatively high alloying component of fusing point is prepared into monocrystalline state
Alloy bar material, it is low-melting, it does not require；Meanwhile the monocrystalline state alloy bar material of high-melting-point ingredient, as seed crystal, length is greater than
3cm；Two bars are placed in alumina tube after being connected to each other；
(3) it the nickel-base high-temperature single crystal alloy coupon of preparation chemical component continuous gradient distribution: is made using high speed freezing method (HRS)
It is standby, formwork is fixed on aqueous cold plate first, is placed in holding furnace；The temperature and smelting time of holding furnace need according to two kinds at
The contact surface type of coupon is divided to determine, vacuum degree≤1Pa in furnace, the withdrawing rate of directional solidification is 3~6mm/min.
2. the preparation side of the nickel-base high-temperature single crystal alloy coupon of chemical component continuous gradient distribution according to claim 1
Method, it is characterised in that: in step (1), the formwork chassis is prepared using conventional method, is carried out by coating to collar plate shape wax-pattern
Wrap up, air-dry, dewaxing, polish after obtain；The material of the alumina tube is high purity aluminium oxide, according to required coupon size selection
The quantity of the internal diameter of alumina tube, alumina tube is determined according to experiment demand.
3. the preparation side of the nickel-base high-temperature single crystal alloy coupon of chemical component continuous gradient distribution according to claim 1
Method, it is characterised in that: in step (2), the element A refers to any pivot in nickel-base high-temperature single crystal alloy in addition to nickel
Element；The distribution of element A weight percentage is a1%~a2%, a1 < a2 in subject alloy coupon.
4. the preparation side of the nickel-base high-temperature single crystal alloy coupon of chemical component continuous gradient distribution according to claim 1
Method, it is characterised in that: in step (2), the high-melting-point bar as seed crystal is placed on alumina tube lower part, and another bar is placed on oxidation
The top of aluminum pipe, the contact surface of two bars guarantee clean, fitting；The diameter of alloy bar material is slightly less than alumina tube on formwork
Internal diameter.
5. the preparation side of the nickel-base high-temperature single crystal alloy coupon of chemical component continuous gradient distribution according to claim 1
Method, it is characterised in that: in step (2), when two bars are connected to each other, contact surface is flat face or lozenges；The flat face is
Abutment face perpendicular to alumina tube axial direction, the lozenges refer to contact surface and alumina tube axial direction angulation be 0 °~
Between 90 °.
6. the preparation side of the nickel-base high-temperature single crystal alloy coupon of chemical component continuous gradient distribution according to claim 5
Method, it is characterised in that: in step (2), when two bars dock, the selection principle of contact surface are as follows: when the density of high-melting-point bar
When less than low melting point bar, contact surface is flat face；When the density of high-melting-point bar is greater than low melting point bar, then contact surface is
Lozenges；The height of lozenges is depending on the length of required gradient components.
7. the preparation side of the nickel-base high-temperature single crystal alloy coupon of chemical component continuous gradient distribution according to claim 1
Method, it is characterised in that: in step (3), keep the temperature the selection principle of furnace temperature and smelting time are as follows: when contact surface is flat face,
Heat preservation furnace temperature should be higher than that 50~100 DEG C of lower end high-melting-point bar fusing point, 20~40min of smelting time；When contact surface is wedge shape
When face, heat preservation furnace temperature should be higher than that 100~150 DEG C of lower end high-melting-point bar fusing point, 2~4h of smelting time.
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| CN109811405A (en) * | 2019-03-28 | 2019-05-28 | 西北工业大学 | A kind of preparation method of Nb-Si based ultra-high temperature alloying component gradient test specimen |
| CN111979582A (en) * | 2020-08-21 | 2020-11-24 | 西北工业大学 | Preparation method of single crystal superalloy with gradient structure |
| WO2021196713A1 (en) * | 2020-03-30 | 2021-10-07 | 上海交通大学 | Substrate-triggered directional solidification process for single crystal superalloy |
| CN114346180A (en) * | 2022-01-07 | 2022-04-15 | 西安交通大学 | Method for controlling mosaic defects of single crystal high-temperature alloy blade |
| CN114934312A (en) * | 2022-05-18 | 2022-08-23 | 中南大学 | Device and method for manufacturing high-throughput sample and gradient functional material |
| CN117760813B (en) * | 2023-12-27 | 2024-05-14 | 烟台大学 | Nickel-based superalloy high-flux sample with continuously-changed element content and preparation method thereof |
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|---|---|---|---|---|
| CN109811405A (en) * | 2019-03-28 | 2019-05-28 | 西北工业大学 | A kind of preparation method of Nb-Si based ultra-high temperature alloying component gradient test specimen |
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| CN114346180B (en) * | 2022-01-07 | 2023-02-24 | 西安交通大学 | Method for controlling mosaic defects of single crystal high-temperature alloy blade |
| CN114934312A (en) * | 2022-05-18 | 2022-08-23 | 中南大学 | Device and method for manufacturing high-throughput sample and gradient functional material |
| CN117760813B (en) * | 2023-12-27 | 2024-05-14 | 烟台大学 | Nickel-based superalloy high-flux sample with continuously-changed element content and preparation method thereof |
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