CN107254716B - A kind of electro-beam floating zone domain melting directional solidifying method for preparing of Fe-Al-Ta composite material - Google Patents
A kind of electro-beam floating zone domain melting directional solidifying method for preparing of Fe-Al-Ta composite material Download PDFInfo
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- CN107254716B CN107254716B CN201710438831.0A CN201710438831A CN107254716B CN 107254716 B CN107254716 B CN 107254716B CN 201710438831 A CN201710438831 A CN 201710438831A CN 107254716 B CN107254716 B CN 107254716B
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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
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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
- C30B21/00—Unidirectional solidification of eutectic materials
- C30B21/04—Unidirectional solidification of eutectic materials by zone-melting
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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
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/08—Production of homogeneous polycrystalline material with defined structure from liquids by zone-melting
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Abstract
A kind of electro-beam floating zone domain melting directional solidifying method for preparing of Fe-Al-Ta composite material, the micro refractory metal Ta with strong ductility is added in metallic compound between Fe-Al, eutectic alloy or eutectic alloy are prepared, Fe (Al, Ta)/Fe is obtained by eutectic reaction2Ta (Al) eutectic composites or the eutectic composite material of Fe-Al-Ta, Laves phase Fe therein2Ta (Al) has six side C14 structures (1700 DEG C of fusing point >), has very high intensity, matrix phase Fe (Al, Ta) and Laves phase Fe when temperature is higher than 1000 DEG C2Ta (Al) symbiosis simultaneously from melt is compound, so as to improve material brittleness and improve the strength of materials, the present invention is not only the design of Laves phase alloy ingredient and the research and development of high temperature structural material provide theoretical foundation, and has important learning value to the application for expanding electron-beam zone melting directional solidification technique.
Description
Technical field
The invention belongs to metallurgical technology field, be related to the brittle improvement of Fe-Al intermetallic compound, in particular to it is a kind of
The electro-beam floating zone domain melting directional solidifying method for preparing of Fe-Al-Ta composite material.
Background technique
Intermetallic compound is other than metallic bond, some covalent bond, has the preferable plasticity and ceramics of metal concurrently
Good elevated temperature strength is the high-temperature structural material of a kind of great potential.Fe-Al intermetallic compound (Fe3Al、FeAl、FeAl2、
Fe2Al5And FeAl3) it is one of the most typically to represent, raw material use two kinds of basic native elements of Fe and Al, and price is low
It is honest and clean；In addition crystal structure of the metallic compound with long-range order, the interatomic existing metallic bond of combination between Fe-Al, and have altogether
Valence link and ionic bond, unique more bonding structures determine its special performance: having lower density, inoxidizability better than not
Steel, heat and corrosion resistant become rusty better than nickel-base alloy, higher elevated temperature strength and creep-resistant property, high temperature corrosion and wear resistance, high resistance etc..
However, the stretch percentage elongation of the material only has 2%-3%, far below common high-temperature structural materials such as stainless steel, heat resisting steel, and
Processability is poor, hinders its large-scale application as high-temperature structural material in the industrial production.
Bridgman method (Bridgman) is a kind of common crystal growth, and Bridgman method has technology maturation, knot
The steady feature of brilliant process, but the solidification rate of Bridgman technology is 2-15cm/h, relatively low, this allows for solidified structure
It can not further refine；The temperature gradient of Bridgman technology is relatively low, about 45K/cm, and lower temperature gradient is also seriously made
About organizational controls and performance improve.
Summary of the invention
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of Fe-Al-Ta composite materials
Melting directional solidifying method for preparing in electro-beam floating zone domain is made by improving the temperature gradient in directional solidification solid liquid interface forward position
It keeps planar interface within the scope of wider solidification rate, to obtain, structure refinement, directional effect are good and what is had excellent performance is total to
Brilliant in-situ composite.Specifically, aiming at the problem that brittleness improving environment of metallic compound between Fe-Al relatively lags,
By adding micro Ta element, using the electron-beam zone melting directional solidification technique of high-temperature gradient, process of setting is controlled, is produced
Microstructure ultra-fining treatment is mutually uniformly distributed, is orientated orderly Laves phase Fe with high accuracy2Fe (Al, Ta)/Fe that Ta (Al) strengthens2Ta
(Al) composite material, so that the comprehensive mechanical property of material be made to improve, the performance for effectively overcoming metallic compound between Fe-Al is lacked
Fall into the problem with preparation method deficiency.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of electro-beam floating zone domain melting directional solidifying method for preparing of Fe-Al-Ta composite material, it is golden between Fe-Al
Belong in compound and be added the micro refractory metal Ta (7at.%~9at.%) with strong ductility, preparation eutectic alloy or
Eutectic alloy obtains Fe (Al, Ta)/Fe by eutectic reaction2Ta (Al) eutectic composites or Fe-Al-Ta are eutectic
Composite material, Laves phase Fe therein2Ta (Al) has six side C14 structures (fusing point > 1700 DEG C), is higher than 1000 DEG C in temperature
When have very high intensity, matrix phase Fe (Al, Ta) and Laves phase Fe2Ta (Al) symbiosis simultaneously from melt is compound, so as to improve
The brittleness of material simultaneously improves the strength of materials.
Above-mentioned Fe (Al, Ta)/Fe2Ta (Al) eutectic composites or the eutectic composite material of Fe-Al-Ta belong to
Target product Fe-Al-Ta composite material of the present invention.
The present invention improves the brittleness of Fe-Al intermetallic compound by the measure of alloying, crystal grain refinement, will be micro
Fe-Al alloy is added in high-melting-point Ta, is prepared using the method for electro-beam floating zone domain melting by the control to process of setting
High performance Fe-Al-Ta eutectic autogenous composite material
The adding manner of the Ta: according to Fe-Al-Ta phasor, by 99.9% pure Fe, 99.999% pure Al and 99.95%
Ta is mixed, molten homogeneous, using process for vacuum induction smelting in vacuum (1.0 × 10-2Pa eutectic alloy casting is prepared in)
Ingot or eutectic alloy cast ingot.
According to the eutectic point of Fe-Al-Ta phasor, eutectic alloy or eutectic alloy are prepared.For example, the eutectic alloy
In, the ratio between atomicity percentage composition of Fe:Ta:Al is 85:7:8；In the eutectic alloy, the atomicity percentage of Fe:Ta:Al
The ratio between content is 84:9:7, or, 82:11:7.
Eutectic reaction includes two parts:
A, by eutectic alloy or eutectic alloy, melting generates eutectic alloy in the vaccum sensitive stove of high-purity Ar atmosphere
Ingot or eutectic alloy pig, occur eutectic reaction in process of setting；
Eutectic alloy ingot or eutectic alloy pig are carried out electro-beam floating zone domain melting directional solidification by b, obtain Fe
(Al,Ta)/Fe2Eutectic occurs in process of setting for Ta (Al) eutectic composites or the eutectic composite material of Fe-Al-Ta anti-
It answers.
The electro-beam floating zone domain melting directional solidification carries out under high-temperature gradient.
The smelting temperature of the electro-beam floating zone domain melting directional solidification is 1580~1680 DEG C, temperature gradient 350
~450K/cm, solidification rate 0.5mm/min, 1mm/min, 2mm/min or 4mm/min, electron gun rated power are 500KW,
Conduction ratio is 30%, and acceleration voltage is 8.5~9.2kV, and emission current is 11~13mA, and vacuum degree is 1.4~1.6 × 10- 4mbar。
Compared with prior art, the present invention uses the electro-beam floating zone domain melting directional solidification technique handle of high-temperature gradient
High-melting-point Ta is added Fe-Al alloy and produces microstructure ultra-fining treatment, volume fraction by accurately controlling and optimizing directional solidification process
Adjustable and orientation Laves phase with high accuracy strengthens Fe (Al, Ta)/Fe2Ta (Al) eutectic autogenous composite material, proposes its ductility
Height arrive about 13%, and as high-temperature structural material in the industrial production can large-scale application, to expand Fe-Al intermetallic
The application of object.The present invention is not only that the design of Laves phase alloy ingredient and the research and development of high temperature structural material provide theoretical foundation,
And there is important learning value to the application for expanding electron-beam zone melting directional solidification technique.
Detailed description of the invention
Fig. 1 is electron beam zone melting schematic diagram of the present invention.
Fig. 2 is electron gun schematic diagram.
Specific embodiment
The embodiment that the present invention will be described in detail with reference to the accompanying drawings and examples.
A kind of electro-beam floating zone domain melting directional solidifying method for preparing of Fe-Al-Ta composite material of the present invention, in Fe-
The micro metal Ta hard to tolerate with strong ductility is added between Al in metallic compound, prepares eutectic alloy or eutectic conjunction
Gold, melting generates eutectic alloy ingot or eutectic alloy pig in the vaccum sensitive stove of high-purity Ar atmosphere, by eutectic alloy ingot or
Eutectic alloy pig carries out electro-beam floating zone domain melting directional solidification, obtains Fe (Al, Ta)/Fe2Ta (Al) eutectic composite wood
Material or the eutectic composite material of Fe-Al-Ta.
Laves phase Fe therein2Ta (Al) has six side C14 structures (fusing point > 1700 DEG C), when temperature is higher than 1000 DEG C
There are very high intensity, matrix phase Fe (Al, Ta) and Laves phase Fe2Ta (Al) symbiosis simultaneously from melt is compound, so as to improve material
The brittleness of material simultaneously improves the strength of materials.
The technological parameter of electro-beam floating zone domain melting directional solidification is as follows:
Smelting temperature: 1580~1680, DEG C temperature gradient: 350~450K/cm, solidification rate: 0.5mm/min, 1mm/
Min, 2mm/min or 4mm/min, electron gun rated power: 500KW, conduction ratio: 30%, acceleration voltage: 8.5~9.2kV, hair
Radio stream: 11~13mA, vacuum degree: 1.4~1.6 × 10-4mbar。
Due to being heated using electron beam, beam bombardment sample is inevitably generated convection current in fusion process, right
Under the conditions of stream coupon solidified since one end normally result in ingredient along solidification directional spreding it is uneven, for solidification after sample
Reversely, secondary beam magnetostrictive properties are carried out, being uniformly distributed for ingredient can also be effectively realized.Herein on basis,
By further Orthogonal Optimization Test, it is as follows to obtain optimal directional solidification processes parameter:
(1) eutectic alloy
Smelting temperature: 1600 DEG C
Temperature gradient: 380K/cm, 390K/cm, 410K/cm, 440K/cm
Solidification rate: 0.5mm/min, 1mm/min, 2mm/min, 4mm/min
Conduction ratio: 30%
Acceleration voltage: 8.7kV
Emission current: 11mA
Vacuum degree: 1.4~1.6 × 10-4mbar
(2) hypoeutectic alloy
Smelting temperature: 1620 DEG C
Temperature gradient: 380K/cm, 390K/cm, 410K/cm, 440K/cm
Solidification rate: 0.5mm/min, 1mm/min, 2mm/min, 4mm/min
Conduction ratio: 30%
Acceleration voltage: 8.9kV
Emission current: 12mA
Vacuum degree: 1.4~1.6 × 10-4mbar
(3) hypereutectic alloy
Smelting temperature: 1640 DEG C
Temperature gradient: 380K/cm, 390K/cm, 410K/cm, 440K/cm
Solidification rate: 0.5mm/min, 1mm/min, 2mm/min, 4mm/min
Conduction ratio: 30%
Acceleration voltage: 9.2kV
Emission current: 13mA
Vacuum degree: 1.4~1.6 × 10-4mbar
Case study on implementation 1
1) according to the eutectic point of Fe-Al-Ta phasor, Fe85/Ta7/Al8 (at%) eutectic alloy is prepared.In high-purity Ar gas
Melting in the vaccum sensitive stove of atmosphere, doubling are cut intoCoupon.
2) it will be cut intoCoupon, vacuum degree be 1.4~1.6 × 10-4Mbar, conduction ratio are
30%, electron beam zone melting (1600 DEG C) are carried out in the furnace that acceleration voltage 8.7KV, emission current are 11mA, makes coupon area
Domain fusing.(coupon is melted using ring-type electron gun and is formed on narrow melting zone, melting zone is maintained at former by surface tension
Expect and stick and solidified between charge bar, when coupon slowly moves along the vertical direction behind melting zone directional solidification, thus along whole
The vertical direction of a charge bar is grown.)
3) sample melts in lesser range, passes through directional solidification from bottom to top, the temperature gradient control of solid liquid interface
For system in 380K/cm, the solidification rate of coupon is 0.5mm/min to be oriented solidification, optimizes eutectic alloy tissue, and improve it
Performance.
Case study on implementation 2
1) according to the eutectic point of Fe-Al-Ta phasor, Fe85/Ta7/Al8 (at%) eutectic alloy is prepared.In high-purity Ar gas
Melting in the vaccum sensitive stove of atmosphere, doubling are cut intoCoupon.
2) it will be cut intoCoupon, vacuum degree be 1.4~1.6 × 10-4Mbar, conduction ratio are
30%, electron beam zone melting (1600 DEG C) are carried out in the furnace that acceleration voltage 8.7KV, emission current are 11mA, makes coupon area
Domain fusing.
3) sample melts in lesser range, passes through directional solidification from bottom to top, the temperature gradient control of solid liquid interface
For system in 390K/cm, the solidification rate of coupon is 1mm/min to be oriented solidification, optimizes eutectic alloy tissue, and improve its property
Energy.
Case study on implementation 3
1) according to the eutectic point of Fe-Al-Ta phasor, Fe85/Ta7/Al8 (at%) eutectic alloy is prepared.In high-purity Ar gas
Melting in the vaccum sensitive stove of atmosphere, doubling are cut intoCoupon.
2) it will be cut intoCoupon, vacuum degree be 1.4~1.6 × 10-4Mbar, conduction ratio are
30%, electron beam zone melting (1600 DEG C) are carried out in the furnace that acceleration voltage 8.7KV, emission current are 11mA, makes coupon area
Domain fusing.
3) sample melts in lesser range, passes through directional solidification from bottom to top, the temperature gradient control of solid liquid interface
For system in 410K/cm, the solidification rate of coupon is 2mm/min to be oriented solidification, optimizes eutectic alloy tissue, and improve its property
Energy.
Case study on implementation 4
1) according to the eutectic point of Fe-Al-Ta phasor, Fe85/Ta7/Al8 (at%) eutectic alloy is prepared.In high-purity Ar gas
Melting in the vaccum sensitive stove of atmosphere, doubling are cut intoCoupon.
2) it will be cut intoCoupon, vacuum degree be 1.4~1.6 × 10-4Mbar, conduction ratio are
30%, electron beam zone melting (1600 DEG C) are carried out in the furnace that acceleration voltage 8.7KV, emission current are 11mA, makes coupon area
Domain fusing.
3) sample melts in lesser range, passes through directional solidification from bottom to top, the temperature gradient control of solid liquid interface
For system in 440K/cm, the solidification rate of coupon is 4mm/min to be oriented solidification, optimizes eutectic alloy tissue, and improve its property
Energy.
Case study on implementation 5
1) according to the eutectic point of Fe-Al-Ta phasor, Fe84/Ta9/Al7 (at.%) hypoeutectic alloy is configured.High-purity
Melting in the vaccum sensitive stove of Ar atmosphere, doubling are cut intoCoupon.
2) it will be cut intoCoupon, vacuum degree be 1.4~1.6 × 10-4Mbar, conduction ratio are
30%, electron beam zone melting (1620 DEG C) are carried out in the furnace that acceleration voltage 8.9KV, emission current are 12mA, makes coupon area
Domain fusing.
3) sample melts in lesser range, passes through directional solidification from bottom to top, the temperature gradient control of solid liquid interface
For system in 380K/cm, the solidification rate of coupon is that 0.5mm/min is oriented solidification, optimizes hypoeutectic alloy tissue, and improve it
Performance.
Case study on implementation 6
1) according to the eutectic point of Fe-Al-Ta phasor, Fe84/Ta9/Al7 (at.%) hypoeutectic alloy is configured.High-purity
Melting in the vaccum sensitive stove of Ar atmosphere, doubling are cut intoCoupon.
2) it will be cut intoCoupon, vacuum degree be 1.4~1.6 × 10-4Mbar, conduction ratio are
30%, electron beam zone melting (1620 DEG C) are carried out in the furnace that acceleration voltage 8.9KV, emission current are 12mA, makes coupon area
Domain fusing.
3) sample melts in lesser range, passes through directional solidification from bottom to top, the temperature gradient control of solid liquid interface
For system in 390K/cm, the solidification rate of coupon is that 1mm/min is oriented solidification, optimizes hypoeutectic alloy tissue, and improve its property
Energy.
Case study on implementation 7
1) according to the eutectic point of Fe-Al-Ta phasor, Fe84/Ta9/Al7 (at.%) hypoeutectic alloy is configured.High-purity
Melting in the vaccum sensitive stove of Ar atmosphere, doubling are cut intoCoupon.
2) it will be cut intoCoupon, vacuum degree be 1.4~1.6 × 10-4Mbar, conduction ratio are
30%, electron beam zone melting (1620 DEG C) are carried out in the furnace that acceleration voltage 8.9KV, emission current are 12mA, makes coupon area
Domain fusing.
3) sample melts in lesser range, passes through directional solidification from bottom to top, the temperature gradient control of solid liquid interface
For system in 410K/cm, the solidification rate of coupon is that 2mm/min is oriented solidification, optimizes hypoeutectic alloy tissue, and improve its property
Energy.
Case study on implementation 8
1) according to the eutectic point of Fe-Al-Ta phasor, Fe84/Ta9/Al7 (at%) hypoeutectic alloy is configured.High-purity
Melting in the vaccum sensitive stove of Ar atmosphere, doubling are cut intoCoupon.
2) it will be cut intoCoupon, vacuum degree be 1.4~1.6 × 10-4Mbar, conduction ratio are
30%, electron beam zone melting (1620 DEG C) are carried out in the furnace that acceleration voltage 8.9KV, emission current are 12mA, makes coupon area
Domain fusing.
3) sample melts in lesser range, passes through directional solidification from bottom to top, the temperature gradient control of solid liquid interface
For system in 440K/cm, the solidification rate of coupon is that 4mm/min is oriented solidification, optimizes hypoeutectic alloy tissue, and improve its property
Energy.
Case study on implementation 9
1) according to the eutectic point of Fe-Al-Ta phasor, Fe82/Ta11/Al7 (at%) hypereutectic alloy is configured.High-purity
Melting in the vaccum sensitive stove of Ar atmosphere, doubling are cut intoCoupon.
2) it will be cut intoCoupon, vacuum degree be 1.4~1.6 × 10-4Mbar, conduction ratio are
30%, electron beam zone melting (1640 DEG C) are carried out in the furnace that acceleration voltage 9.2KV, emission current are 13mA, makes coupon area
Domain fusing.
3) sample melts in lesser range, passes through directional solidification from bottom to top, the temperature gradient control of solid liquid interface
For system in 380K/cm, the solidification rate of coupon is that 0.5mm/min is oriented solidification, optimizes hypereutectic alloy tissue, and improve it
Performance.
Case study on implementation 10
1) according to the eutectic point of Fe-Al-Ta phasor, Fe82/Ta11/Al7 (at%) hypereutectic alloy is configured.High-purity
Melting in the vaccum sensitive stove of Ar atmosphere, doubling are cut intoCoupon.
2) it will be cut intoCoupon, vacuum degree be 1.4~1.6 × 10-4Mbar, conduction ratio are
30%, electron beam zone melting (1640 DEG C) are carried out in the furnace that acceleration voltage 9.2KV, emission current are 13mA, makes coupon area
Domain fusing.
3) sample melts in lesser range, passes through directional solidification from bottom to top, the temperature gradient control of solid liquid interface
For system in 390K/cm, the solidification rate of coupon is that 1mm/min is oriented solidification, optimizes hypereutectic alloy tissue, and improve its property
Energy.
Case study on implementation 11
1) according to the eutectic point of Fe-Al-Ta phasor, Fe82/Ta11/Al7 (at%) hypereutectic alloy is configured.High-purity
Melting in the vaccum sensitive stove of Ar atmosphere, doubling are cut intoCoupon.
2) it will be cut intoCoupon, vacuum degree be 1.4~1.6 × 10-4Mbar, conduction ratio are
30%, electron beam zone melting (1640 DEG C) are carried out in the furnace that acceleration voltage 9.2KV, emission current are 13mA, makes coupon area
Domain fusing.
3) sample melts in lesser range, passes through directional solidification from bottom to top, the temperature gradient control of solid liquid interface
For system in 410K/cm, the solidification rate of coupon is that 2mm/min is oriented solidification, optimizes hypereutectic alloy tissue, and improve its property
Energy.
Case study on implementation 12
1) according to the eutectic point of Fe-Al-Ta phasor, Fe82/Ta11/Al7 (at%) hypereutectic alloy is configured.High-purity
Melting in the vaccum sensitive stove of Ar atmosphere, doubling are cut intoCoupon.
2) it will be cut intoCoupon, vacuum degree be 1.4~1.6 × 10-4Mbar, conduction ratio are
30%, electron beam zone melting (1640 DEG C) are carried out in the furnace that acceleration voltage 9.2KV, emission current are 13mA, makes coupon area
Domain fusing.
3) sample melts in lesser range, passes through directional solidification from bottom to top, the temperature gradient control of solid liquid interface
For system in 440K/cm, the solidification rate of coupon is that 4mm/min is oriented solidification, optimizes hypereutectic alloy tissue, and improve its property
Energy.
Properties of product description:
The Fe-Al-Ta composite material prepared by electron beam zone melting, by accurately controlling and optimizing directional solidification mistake
Journey, produces that microstructure ultra-fining treatment, volume fraction are adjustable and orientation Laves phase with high accuracy strengthens Fe (Al, Ta)/Fe2Ta (Al) is altogether
Brilliant in-situ composite makes its ductility improve ((elongation about 13%)).
Experimental method:
By the various moderns analysis and testing technology such as scanning electron microscope, X-ray, different component, different solidification rates are investigated
The coagulating properties such as solidification structure, phase composition, the interphase structure of Fe-Al-Ta alloy.And Fe (Al, Ta)/Fe2Ta (Al)
Composite processing tests the mechanical property such as its hardness, fracture toughness at standard specimen, using equipment such as microhardness testers, stretchings
Can, specify the relationship between Solidification Parameters-solidified structure-material property.
In the present invention, by expanding the composition range of constituent element, improving the temperature gradient in directional solidification solid liquid interface forward position
(350~450K/cm) makes its within the scope of wider solidification rate (0.5~4.0mm/min) to keep planar interface, to obtain
Structure refinement, directional effect be good and the eutectic autogenous composite material that has excellent performance.
Fig. 1 is electron beam zone melting schematic diagram, and electron beam zone refining furnace is an extremely complex system.Working principle
Are as follows: electron gun 11 launches electronics, and electronics is accelerated under the action of electric field, makes beam bombardment surface of material, will high speed
The kinetic energy of moving electron is converted to thermal energy, makes material zone melting.
Fe-Al-Ta blank stick 14 is to be vertically mounted in the clamp structure with upper clamp and lower clamp, and melting zone 13 is it
On narrow zone, lower clamp can make sample in a certain range left and right up and down adjustment, hollow cathode can be by means of driver
Structure is moved up and down with the speed of 0~± 23mm/min along sample.When high voltage power supply is connected, the electronics that electron gun is launched passes through
Electric field action is accelerated, bombards sample, and kinetic energy is converted into thermal energy.If the energy of electron beam is sufficiently high, coupon is heated to
It is white-hot and melt, it is grown under the induction of grain of crystallization 12.
Fig. 2 is electron gun schematic diagram, and electron gun is the device of vacuum electron beam zone refining furnace most critical.The work of electron gun
Make principle are as follows: emit a large amount of thermoelectrons after filament heating power to incandescent state, accelerating field uses negative high voltage, plus earth,
Electronics accelerates under the action of high voltage electric field.Due to accelerating field, the effect of shielding, electronics is enable to assemble to anode.
The ring-type electron gun is mainly by electron gun gun body 24, upper auxiliary electrode 21, lower auxiliary electrode 23, filament and bunching electrode
25 4 parts form, and electron gun gun body is water-cooling structure, are divide into upper part and lower part, and upper auxiliary electrode is housed on gun body top
21, bunching electrode 25 and filament (cathode 22) are equipped with lower interpole 23 in gun body lower part.In the electron gun, gun body, up and down auxiliary
Pole and interpole connect negative high voltage, need to carry out the molten bar ground connection in area, as anode 26.
The foregoing is merely a kind of embodiment of material of the invention, it is not all of or the embodiment of sole material,
Any equivalent transformation that those of ordinary skill in the art take technical solution of the present invention by reading description of the invention,
All are covered by the claims of the invention.
Claims (4)
1. a kind of electro-beam floating zone domain melting directional solidifying method for preparing of Fe-Al-Ta composite material, it is characterised in that:
Ta, 7at.%~9at.% of the additional amount of Ta metallic compound total amount between Fe-Al is added between Fe-Al in metallic compound,
Eutectic alloy or eutectic alloy are prepared, Fe (Al, Ta)/Fe is obtained by eutectic reaction2Ta (Al) eutectic composites or
The eutectic composite material of Fe-Al-Ta, Laves phase Fe therein2Ta (Al) has six side's C14 structures, matrix phase Fe (Al, Ta)
With Laves phase Fe2Ta (Al) symbiosis simultaneously from melt is compound, wherein the eutectic reaction includes:
A, by eutectic alloy or eutectic alloy, in the vaccum sensitive stove of high-purity Ar atmosphere melting generate eutectic alloy ingot or
Eutectic alloy pig, occurs eutectic reaction in process of setting；
Eutectic alloy ingot or eutectic alloy pig it is solidifying to be carried out electro-beam floating zone domain melting orientation by b under high-temperature gradient
Gu obtaining Fe (Al, Ta)/Fe2Ta (Al) eutectic composites or the eutectic composite material of Fe-Al-Ta, send out in process of setting
Raw eutectic reaction；The smelting temperature of the electro-beam floating zone domain melting directional solidification is 1580~1680 DEG C, and temperature gradient is
350~450K/cm, solidification rate 0.5mm/min, 1mm/min, 2mm/min or 4mm/min, electron gun rated power are
500KW, conduction ratio 30%, acceleration voltage be 8.5~9.2kV, emission current be 11~13mA, vacuum degree be 1.4~1.6 ×
10-4mbar。
2. the electro-beam floating zone domain melting directional solidifying method for preparing of Fe-Al-Ta composite material according to claim 1,
The adding manner of the Ta: according to Fe-Al-Ta phasor, Fe, Al and Ta are mixed, molten homogeneous uses vacuum induction
Melting technique prepares eutectic alloy ingot casting or eutectic alloy cast ingot in a vacuum.
3. the electro-beam floating zone domain melting directional solidifying method for preparing of Fe-Al-Ta composite material according to claim 1,
It is characterized in that, preparing eutectic alloy or eutectic alloy according to the eutectic point of Fe-Al-Ta phasor.
4. the electro-beam floating zone domain melting directional solidifying method for preparing of Fe-Al-Ta composite material according to claim 3,
It is characterized in that,
In the eutectic alloy, the ratio between atomicity percentage composition of Fe:Ta:Al is 85:7:8；
In the eutectic alloy, the ratio between atomicity percentage composition of Fe:Ta:Al is 84:9:7, or, 82:11:7.
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