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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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
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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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/04Making ferrous alloys by melting
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/06Ferrous alloys, e.g. steel alloys containing aluminium
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    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
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    • C30B28/00Production of homogeneous polycrystalline material with defined structure
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    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
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Abstract

本发明公开了一种定向FeAl基合金的制备方法,所述的FeAl合金成分按原子百分比记为FeaAlb,其中37≤a≤45,55≤b≤63,a+b=100,其组织为柱状晶;其步骤为:根据FeAl二元合金体系相图选择合适成分;采用水冷铜坩埚和真空非自耗电弧熔炼炉制备圆柱棒母合金;采用Bridgman晶体生长装置对母合金棒进行定向凝固,得到所述具有定向柱状晶组织的FeAl基合金。对比等轴晶的FeAl基合金,本发明制备的定向FeAl基合金拥有更加优异的综合力学性能。

Figure 202110653471

The invention discloses a preparation method of an oriented FeAl-based alloy. The FeAl alloy composition is recorded as Fe a Al b in atomic percentage, wherein 37≤a≤45, 55≤b≤63, a+b=100, and The structure is columnar crystal; the steps are: select appropriate components according to the phase diagram of the FeAl binary alloy system; use a water-cooled copper crucible and a vacuum non-consumable arc melting furnace to prepare a cylindrical rod master alloy; use a Bridgman crystal growth device to process the master alloy rod. Directional solidification is carried out to obtain the FeAl-based alloy with directional columnar crystal structure. Compared with the equiaxed FeAl-based alloy, the oriented FeAl-based alloy prepared by the present invention has more excellent comprehensive mechanical properties.

Figure 202110653471

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)

1.一种定向FeAl基合金的制备方法,其特征在于,其表达式为FeaAlb,其中,37≤a≤45,55≤b≤63 ,a+b=100,包括以下步骤:1. A preparation method of an oriented FeAl-based alloy, characterized in that its expression is Fe a Al b , wherein 37≤a≤45, 55≤b≤63, a+b=100, comprising the following steps: (1)根据目标FeAl合金成分称配原料;(1) Weigh the raw materials according to the target FeAl alloy composition; (2)熔炼、浇铸得到FeAl合金棒;(2) Smelting and casting to obtain FeAl alloy rods; (3)氩气保护下,采用Bridgman晶体生长装置对圆柱棒合金进行定向凝固,加热温度为1200~1900℃,保温时间为1~60min,抽拉速率为0.1~1000μm/s,得到FeAl柱状晶。(3) Under the protection of argon, the Bridgman crystal growth device was used to directional solidify the cylindrical rod alloy. The heating temperature was 1200-1900 °C, the holding time was 1-60 min, and the pulling rate was 0.1-1000 μm/s to obtain FeAl columnar crystals. . 2.如权利要求1所述的方法,其特征在于,步骤(2)中,采用水冷铜坩埚悬浮熔炼炉或真空非自耗电弧熔炼炉反复熔炼至少4次原料,然后采用真空非自耗电弧熔炼炉浇铸得到直径为8~10mm的FeAl合金圆棒。2. The method of claim 1, wherein in step (2), a water-cooled copper crucible suspension smelting furnace or a vacuum non-consumable arc smelting furnace is used to repeatedly smelt the raw materials for at least 4 times, and then the vacuum non-consumable is used to smelt the raw materials. FeAl alloy round rods with diameters of 8-10 mm are obtained by casting in an arc melting furnace. 3.如权利要求1所述的方法,其特征在于,步骤(3)中,加热温度为1300~1600℃,保温时间为20~60min,抽拉速率为5~500μm/s。3 . The method of claim 1 , wherein, in step (3), the heating temperature is 1300-1600° C., the holding time is 20-60 min, and the pulling rate is 5-500 μm/s. 4 . 4.如权利要求1所述的方法,其特征在于,步骤(3)中,定向凝固得到直径8~10mm,长度为6~13cm的FeAl柱状晶。4. The method of claim 1, wherein in step (3), FeAl columnar crystals with a diameter of 8-10 mm and a length of 6-13 cm are obtained by directional solidification. 5.如权利要求1-4所述的方法制备的定向FeAl基合金。5. The oriented FeAl-based alloy prepared by the method of claims 1-4.
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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

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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
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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

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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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