CN113528926A - Oriented FeAl-based alloy and preparation method thereof - Google Patents

Oriented FeAl-based alloy and preparation method thereof Download PDF

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Publication number
CN113528926A
CN113528926A CN202110653471.2A CN202110653471A CN113528926A CN 113528926 A CN113528926 A CN 113528926A CN 202110653471 A CN202110653471 A CN 202110653471A CN 113528926 A CN113528926 A CN 113528926A
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feal
alloy
equal
based alloy
oriented
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陈�光
彭海鑫
郑功
侯锐
周冰
黄腾达
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Nanjing University of Science and Technology
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Nanjing University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/04—Making ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • 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
    • 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
    • C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
    • 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
    • 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
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C30B29/605—Products containing multiple oriented crystallites, e.g. columnar crystallites

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a preparation method of oriented FeAl-based alloy, wherein the FeAl alloy comprises the following components by atomic percent as FeaAlbWherein a is more than or equal to 37 and less than or equal to 45, b is more than or equal to 55 and less than or equal to 63, and a + b =100, and the structure is columnar crystal; the method comprises the following steps: selecting proper components according to a phase diagram of a FeAl binary alloy system; preparing a cylindrical rod master alloy by adopting a water-cooled copper crucible and a vacuum non-consumable arc melting furnace; directionally solidifying the master alloy rod by adopting a Bridgman crystal growth device to obtain the alloy rod with the orientationA columnar-grain FeAl-based alloy. Compared with the isometric FeAl-based alloy, the oriented FeAl-based alloy prepared by the invention has more excellent comprehensive mechanical properties.

Description

Oriented FeAl-based alloy and preparation method thereof
Technical Field
The invention belongs to the technical field of directional solidification, and particularly relates to a preparation method of a directional FeAl-based alloy.
Background
FeAl alloy is one of the most promising aluminum-containing intermetallic compounds. Like other aluminum-containing alloys, FeAl alloy has the excellent characteristics of high specific strength, high thermal stability, corrosion resistance, oxidation resistance, good high-temperature mechanical properties and the like. In addition, because the high-temperature alloy takes two basic industrial elements of Fe and Al as main raw materials, compared with other high-temperature alloys, the high-temperature alloy has more advantages in cost and has great application potential in the aspects of high-temperature corrosion resistance, oxidation resistance, high-temperature structural materials and the like. Over the last twenty years, much progress has been made in the study of FeAl alloys. FeAl alloys have been successfully used in many applications, such as replacing FeCrAl heating elements for heating rods in textile dyeing machines; the thermocouple protective sleeve is used instead of stainless steel; a fluidized bed boiler bottom feed nozzle; a double-acting slide valve guide rail of the catalytic cracking device; heat exchange tubes and walls, etc. The FeAl alloy has high magnetic permeability and good wear resistance, and can be used as a magnetic head material.
Although the FeAl alloy has the advantages, the FeAl alloy has the defects of high brittleness, poor plasticity and toughness, low tensile strength and the like, so that the FeAl alloy is difficult to machine and form and is not suitable for important structural parts and high-precision complex parts. The specific reasons are as follows: the complex crystal structure and special atomic bond mode of FeAl alloy determine that the FeAl alloy has high elastic modulus and hardness, the performance of high-hardness materials is quite sensitive to the structure, and the tiny structural defects can cause brittle fracture of the materials. And defects in the material are usually formed on the grain boundaries, and the environmental hydrogen embrittlement also acts through the grain boundaries, where a vaporization reaction of hydrogen embrittlement occurs. Therefore, the brittleness of the FeAl alloy is mostly originated from the grain boundary, and the problem of brittleness of the intermetallic compound is solved by solving the brittleness problem of the grain boundary.
Disclosure of Invention
The invention aims to provide a preparation method of an oriented FeAl-based alloy.
The technical solution for realizing the purpose of the invention is as follows: preparation method of oriented FeAl-based alloy, wherein expression of oriented FeAl-based alloy is FeaAlbWherein a is more than or equal to 37 and less than or equal to 45, b is more than or equal to 55 and less than or equal to 63, and a + b =100, the method comprises the following steps:
(1) weighing raw materials according to the target FeAl alloy components;
(2) smelting and casting to obtain a FeAl alloy rod;
(3) under the protection of argon, a Bridgman crystal growth device is adopted to carry out directional solidification on the cylindrical rod alloy, the heating temperature is 1200-1900 ℃, the heat preservation time is 1-60 min, and the drawing speed is 0.1-1000 mu m/s, so that the FeAl column crystal is obtained.
Preferably, in the step (2), a water-cooled copper crucible suspension smelting furnace or a vacuum non-consumable arc smelting furnace is adopted to repeatedly smelt the raw materials for at least 4 times, and then the raw materials are cast by the vacuum non-consumable arc smelting furnace to obtain the FeAl alloy round rod with the diameter of 8-10 mm.
Preferably, in the step (3), the heating temperature is 1300-1600 ℃, the heat preservation time is 20-60 min, and the drawing speed is 5-500 μm/s.
Preferably, in the step (3), FeAl columnar crystals with the diameter of 8-10 mm and the length of 6-13 cm are obtained through directional solidification.
Compared with the prior art, the invention has the following remarkable advantages:
(1) the FeAl alloy prepared by the invention has a columnar crystal structure, eliminates a transverse crystal boundary, improves the comprehensive mechanical property of the alloy, and effectively solves the problems of poor plasticity and toughness, low strength and the like of the alloy.
(2) The method utilizes the unique characteristics of the Bridgman directional solidification device to prepare the FeAl alloy with the columnar crystal structure in one step, and has simple preparation method and lower process cost.
Drawings
FIG. 1 is a binary system phase diagram of FeAl alloy.
FIG. 2 is a scanning microstructure of a directionally solidified FeAl alloy sheet of example 1 (a is a scanning image, and b is a table of the midpoint scanning compositions in a).
FIG. 3 is a micrograph and optical micrograph of a directionally solidified FeAl alloy of example 1 (a is the as-cast region, b is the competing region, c is the stable region, and d is the magnified region in c).
FIG. 4 is a graph showing the quasi-static compression of example 1 with as-cast FeAl alloy.
FIG. 5 is a micrograph of a directionally solidified FeAl alloy of example 2.
FIG. 6 is a micrograph of a directionally solidified FeAl alloy of example 3.
FIG. 7 is a micrograph of a directionally solidified FeAl alloy of example 3.
FIG. 8 is a micrograph of a directionally solidified FeAl alloy of comparative example 1.
FIG. 9 is a micrograph of a directionally solidified FeAl alloy of comparative example 2.
FIG. 10 is a micrograph of a directionally solidified FeAl alloy of comparative example 3.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
Example 1
(1) According to a binary system phase diagram of the FeAl alloy shown in figure 1, the proportioning component is Fe40Al60The alloy of (1).
(2) Repeatedly smelting the raw materials for at least 4 times by using a water-cooled copper crucible suspension smelting furnace, and then casting by using a vacuum non-consumable arc smelting furnace to obtain a FeAl alloy round rod with the diameter of 8 mm;
(3) under the protection of argon, a Bridgman directional solidification device is adopted to directionally solidify the cylindrical rod master alloy, the heating temperature is 1380 ℃, the heat preservation time is 20min, the drawing speed is 100 mu m/s, and finally the FeAl column crystal with the diameter of 8mm and the length of 6cm is obtained.
Point scanning is carried out on the selected area of the microscopic morphology, and the black structure is FeAl phase, and the white structure is FeAl phase2And (4) phase(s). As is clear from FIG. 1 and FIG. 2, around 1102 ℃ ε → FeAl + FeAl occurs2Phase change, epsilon phase generation of FeAl + FeAl2And (4) lamellar organization. The specific structure is shown in FIG. 3, and thus a FeAl alloy having a columnar crystal structure can be obtained. As can be seen from FIG. 4, the compression properties of the FeAl alloy having the columnar structure are higher than those of the FeAl alloy in the as-cast stateThe elongation is about 3 times higher and the elongation is about 1 time higher.
Example 2
Adopts the component Fe45Al55The other steps are the same as in example 1, except that: during directional solidification, the heating temperature is 1600 ℃, the holding time is 60min, and the drawing speed is 300 mu m/s, so that the FeAl alloy with the columnar crystal structure as shown in example 1 can still be obtained, and the micrograph thereof is shown in FIG. 5. The compression performance of the alloy is about 2 times higher than that of cast FeAl alloy, and the elongation is about 1 time higher.
Example 3
Adopts the component Fe37Al63The other steps are the same as in example 1, except that: during directional solidification, the heating temperature is 1500 ℃, the holding time is 40min, the drawing speed is 500 μm/s, and the FeAl alloy with the columnar crystal structure as described in example 1 can still be obtained, and the micrograph thereof is shown in FIG. 6. The compression performance of the alloy is about 2 times higher than that of cast FeAl alloy, and the elongation is about 1 time higher.
Example 4
Adopts the component Fe40Al60The other steps are the same as in example 1, except that: the holding time for directional solidification is 30min, the drawing rate is 5 μm/s, and the FeAl alloy with the columnar crystal structure as described in example 1 can still be obtained, and the micrograph thereof is shown in FIG. 7. The compression performance of the alloy is about 3 times higher than that of cast FeAl alloy, and the elongation is about 1 time higher.
Comparative example 1
Adopts the component Fe35Al65The other steps are the same as those of example 1, and a stable-section FeAl alloy without columnar crystal structure is obtained, and a micrograph thereof is shown in FIG. 8.
Comparative example 2
Adopts the component Fe47Al53The other steps are the same as those of example 1, and a stable-section FeAl alloy without columnar crystal structure is obtained, and a micrograph thereof is shown in FIG. 9.
Comparative example 3
Adopts the component Fe40Al60Under the growth rate of 1100 μm/s, and other conditionsIn the same manner as in example 1, a FeAl alloy having a stable-stage columnar-crystal-free structure was obtained, and its micrograph is shown in FIG. 10.

Claims (5)

1. The preparation method of the directional FeAl-based alloy is characterized in that the expression is FeaAlbWherein a is more than or equal to 37 and less than or equal to 45, b is more than or equal to 55 and less than or equal to 63, and a + b =100, the method comprises the following steps:
(1) weighing raw materials according to the target FeAl alloy components;
(2) smelting and casting to obtain a FeAl alloy rod;
(3) under the protection of argon, a Bridgman crystal growth device is adopted to carry out directional solidification on the cylindrical rod alloy, the heating temperature is 1200-1900 ℃, the heat preservation time is 1-60 min, and the drawing speed is 0.1-1000 mu m/s, so that the FeAl columnar crystal is obtained.
2. The method of claim 1, wherein in the step (2), the raw materials are repeatedly smelted by a water-cooled copper crucible suspension smelting furnace or a vacuum non-consumable arc smelting furnace for at least 4 times, and then the raw materials are cast by the vacuum non-consumable arc smelting furnace to obtain the FeAl alloy round rod with the diameter of 8-10 mm.
3. The method according to claim 1, wherein in the step (3), the heating temperature is 1300-1600 ℃, the holding time is 20-60 min, and the drawing rate is 5-500 μm/s.
4. The method of claim 1, wherein in the step (3), the FeAl columnar crystals with the diameter of 8-10 mm and the length of 6-13 cm are obtained by directional solidification.
5. An oriented FeAl-based alloy prepared according to the method of claims 1-4.
CN202110653471.2A 2021-06-11 2021-06-11 Oriented FeAl-based alloy and preparation method thereof Pending CN113528926A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114433823A (en) * 2022-01-19 2022-05-06 南京理工大学 Oriented ZrCr-based alloy and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0465686A1 (en) * 1990-07-07 1992-01-15 Asea Brown Boveri Ag Oxidation- and corrosion resistant alloy for parts subjected to medium high temperatures and based on doped iron trialuminide Fe3Al
CN103789598A (en) * 2014-02-28 2014-05-14 南京理工大学 Directional TiAl-based alloy and preparation method thereof
CN105821470A (en) * 2016-04-14 2016-08-03 南京理工大学 Dual-structure titanium aluminum (TiAl) alloy and preparation method thereof
CN110090942A (en) * 2019-06-06 2019-08-06 西安建筑科技大学 The method that the multifunctional integrated material of Fe-Al-Ta is prepared using Bridgman directional solidification technique

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0465686A1 (en) * 1990-07-07 1992-01-15 Asea Brown Boveri Ag Oxidation- and corrosion resistant alloy for parts subjected to medium high temperatures and based on doped iron trialuminide Fe3Al
CN103789598A (en) * 2014-02-28 2014-05-14 南京理工大学 Directional TiAl-based alloy and preparation method thereof
CN105821470A (en) * 2016-04-14 2016-08-03 南京理工大学 Dual-structure titanium aluminum (TiAl) alloy and preparation method thereof
CN110090942A (en) * 2019-06-06 2019-08-06 西安建筑科技大学 The method that the multifunctional integrated material of Fe-Al-Ta is prepared using Bridgman directional solidification technique

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
A.SCHERF ET AL.: "Orientation relationship of eutectoid FeAl and FeAl2", 《JOURNAL OF APPLIED CRYSTALLOGRAPHY》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114433823A (en) * 2022-01-19 2022-05-06 南京理工大学 Oriented ZrCr-based alloy and preparation method thereof

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