CN113564497A - A kind of Fe-based amorphous alloy and its preparation method and application - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
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- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000010936 titanium Substances 0.000 claims abstract description 3
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 3
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- 230000001681 protective effect Effects 0.000 claims description 9
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0611—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
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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
- C22C33/003—Making ferrous alloys making amorphous alloys
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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
- C22C33/06—Making ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/123—Spraying molten metal
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Abstract
The invention relates to the technical field of amorphous alloys, in particular to a Fe-based amorphous alloy and a preparation method and application thereof. The invention adopts industrial pure Fe, Cr, Mo, C, W, Y and prealloy FeB to carry out electric arc melting in argon atmosphere with deoxidization of sponge titanium to prepare an alloy ingot of Fe-based alloy, and adopts a single-roller melting and strip-spinning method or a thermal spraying technology to prepare a Fe-based amorphous alloy sample. The Fe-based amorphous alloy prepared by the method has extremely low corrosion rate of liquid lead-bismuth alloy under the condition of simulating the lead-cold fast reactor working condition.
Description
Technical Field
The invention relates to the technical field of amorphous alloys, in particular to a Fe-based amorphous alloy and a preparation method and application thereof.
Background
Nuclear power is taken as a clean energy source capable of replacing fossil fuels in a large scale and plays an important role in the current world energy structure, but the current thermal neutron reactor applied in a large scale has the problems of low resource utilization rate, radioactive waste accumulation and potential nuclear safety. With the increase of nuclear energy demand, experts and scholars at home and abroad focus on researching and developing a cleaner, efficient and safe nuclear energy system. Among the many developing fourth generation nuclear power reactor types, Lead-cooled fast reactors (LFRs) are considered to have the most potential for application. The reactor coolant in the LFR is liquid lead-bismuth eutectic alloy which has good thermophysical property, neutron property, thermal stability, radiation resistance and higher chemical inertness, and the excellent characteristics of the LBE alloy coolant greatly improve the safety of the LFR. LFR also has significant advantages in nuclear fuel proliferation and nuclear waste disposal (cn201810809190. x). The coolant flowing in the LFR reactor internal thermal circulation loop is an LBE alloy. At present, materials of key structural components such as a container, a pipeline, a circulating pump and the like in the heat circulation convection loop are generally made of structural steel materials such as T91, 316L and the like. There is a material compatibility problem between the solid steel structure material and the LBE alloy, i.e., the LBE alloy has a strong Liquid Metal Corrosion (LMC) effect on the steel. Corrosion of liquid metals can be carried out by dissolution, oxidation, carburization, formation of intermetallic compounds, and the like. Therefore, the corrosion problem of the LBE alloy to the structural material seriously affects the safety and service life of the LFR (CN201410217256.8), the material compatibility problem is one of the major bottleneck problems of the practical engineering application of the LFR, the research on the corrosion resistance and protection of the structural material in the LBE alloy, and the development of a novel protective material resistant to the corrosion of the LBE alloy is a hot point problem at the forefront of the world nuclear engineering field.
The most studied protective materials resisting corrosion of the LBE alloy at present are crystal structure materials (such as ODS steel, FeCrAl alloy and T91 steel cn201610810661.x, and the like), and although some materials already show good corrosion resistance, in a low-oxygen-concentration LBE alloy environment, corrosion of the materials can cause serious grain boundary corrosion besides dissolution corrosion, and the grain boundary corrosion can also cause a liquid metal grain boundary embrittlement problem, so that the mechanical properties of the structural materials are reduced.
Disclosure of Invention
At present, the protective material which is researched more and resists LBE alloy corrosion can generate dissolution corrosion and serious grain boundary corrosion in a low-oxygen-concentration LBE alloy environment, the grain boundary corrosion can also cause the problem of liquid metal grain boundary embrittlement, the mechanical property of the structural material is reduced, the safety and the service life of LFR are seriously influenced, and the application cost of the lead-cooled fast reactor is further improved.
In view of the above problems, the present invention provides an Fe-based amorphous alloy, and a preparation method and an application thereof, so as to enhance the corrosion resistance of the Fe-based amorphous alloy and make the Fe-based amorphous alloy a candidate material for LFR corrosion protection.
The purpose of the invention can be realized by the following technical scheme:
the invention provides a Fe-based amorphous alloy, the nominal component of which is FeCrMoWxCBY，0≤x≤8。
The invention also provides a preparation method of the Fe-based amorphous alloy, which comprises the following steps:
(1) carrying out arc melting on industrial pure Fe, Cr, Mo, C, W, Y and prealloy FeB in an anoxic state to prepare an alloy ingot of the Fe-based alloy;
(2) preparing a Fe-based amorphous alloy sample by adopting a single-roller melting strip-spinning method or a thermal spraying technology, wherein the nominal component of the Fe-based amorphous alloy is FeCrMoWxCBY，0≤x≤8。
In one embodiment of the present invention, the anoxic state in step (1) means: excess oxygen was removed in an argon atmosphere with titanium sponge.
In one embodiment of the present invention, in the step (1), the mixture ratio of each component includes: 99.7 wt.% Fe, 99.98 wt.% Cr, 99.9 wt.% Mo, 99.999 wt.% C, 99.5 wt.% W, 99.6 wt.% Y, 99.38 wt.% prealloyed FeB.
In one embodiment of the invention, the Fe-based alloy ingot obtained in the step (1) is remelted at least four times to obtain a melt with uniform components, the obtained melt is dropped into a copper mold to prepare a rod-shaped sample, and the rod-shaped sample is prepared into the Fe-based amorphous alloy sample by a single-roller melting and strip-spinning method or a thermal spraying technology.
In one embodiment of the present invention, in the step (2), the preparation of the Fe-based amorphous alloy sample by the single-roll melt-spinning method or by the thermal spraying technique is performed under a protective gas atmosphere.
In one embodiment of the present invention, in step (2), the shielding gas includes, but is not limited to, high purity argon.
In one embodiment of the present invention, in the step (2), the Fe-based amorphous alloy ribbon with a thickness of 30-50 μm is prepared by the method for preparing the Fe-based amorphous alloy at a rotation speed of 20-40 m/s. Preferably, the width of the Fe-based amorphous alloy strip is 1mm to 1.5 mm.
In one embodiment of the present invention, in the step (2), the process conditions of the thermal spraying technique are: the spraying distance is 150-180mm, the powder feeding speed is 40-50g/min, the propane pressure is 0.4-0.6MPa, the air pressure is 0.5-0.7MPa, and N is2Pressure of 0.2-0.4Mpa, H2The pressure is 0.05-0.1 MPa.
The invention also provides an application of the Fe-based amorphous alloy obtained based on the method, and the Fe-based amorphous alloy is used as a corrosion protection candidate material for lead-cooled fast reactors.
The invention adopts amorphous alloy as LBE alloy corrosion protective material, the amorphous alloy is also called as metal glass, because of the unique structural characteristics of long-range disorder and short-range order, the amorphous alloy generally has high strength and hardness, high elastic limit, excellent corrosion resistance and wear resistance, etc. The amorphous alloy has uniform component distribution on the macro and micro, and has no crystal structure defects (dislocation and grain boundary) of the traditional material, and the characteristics enable the amorphous alloy to have more excellent LBE corrosion resistance, and can reduce local corrosion caused by non-uniform components and the problems of grain boundary corrosion and embrittlement caused by the grain boundary. Meanwhile, although the Fe-based amorphous alloy has a series of excellent properties, the Fe-based amorphous alloy is difficult to be used as a large-scale structural member due to the limitations of glass forming capability and the critical dimension of the amorphous alloy, the size problem of the amorphous alloy can be solved by a thermal spraying technology, and the Fe-based amorphous alloy coating prepared by the thermal spraying technology (such as High Velocity Air furnace, HVAF) can be applied to parts such as nuclear waste storage tanks, water turbine blades and the like.
Compared with the prior art, the novel Fe-based amorphous alloy prepared by the invention has the following advantages and beneficial effects:
(1) the Fe-based amorphous alloy has the unique excellent performances (high strength, high hardness and excellent corrosion resistance) of the amorphous alloy, also has excellent oxidation resistance and has obvious advantages in the aspect of large-scale industrial application.
(3) The Fe-based amorphous alloy coating material also has high hardness (>1000Hv) and high thermal stability (crystallization temperature T)x>550 ℃), corrosion resistance, wear resistance and the like, and is a potential LFR corrosion protection candidate material.
Drawings
FIG. 1 is an X-ray diffraction pattern of a Fe-based amorphous alloy sample prepared in example 1 of the present invention.
FIG. 2 is a comparison of the corrosion interface of the Fe-based amorphous alloy sample prepared in example 1 of the present invention and the corrosion interface of CG9Cr + AlSi other materials.
FIG. 3 is a graph comparing the corrosion rates of Fe-based amorphous alloy prepared in example 1 of the present invention and other materials.
FIG. 4 is a corrosion interface diagram of the Fe-based amorphous alloy sample prepared in example 2 of the present invention.
FIG. 5 is a graph of TiC coating corrosion interface compared to the Fe-based amorphous alloy sample prepared in example 2 of the present invention.
FIG. 6 is a graph comparing the corrosion rates of Fe-based amorphous alloy prepared in example 2 of the present invention and other materials.
Detailed Description
The invention provides a Fe-based amorphous alloy, the nominal component of which is FeCrMoWxCBY，0≤x≤8。
The invention also provides a preparation method of the Fe-based amorphous alloy, which comprises the following steps:
(1) carrying out arc melting on industrial pure Fe, Cr, Mo, C, W, Y and prealloy FeB in an argon atmosphere with deoxidization of sponge titanium to prepare an alloy ingot of Fe-based alloy;
(2) remelting the Fe-based alloy ingot obtained in the step (1) at least four times to obtain a melt with uniform components;
(3) dripping the melt obtained in the step (2) into a copper mold to prepare a rod-shaped sample;
(4) under the protective gas atmosphere, preparing Fe-based amorphous alloy strips by adopting a single-roller melting strip-spinning method or preparing Fe-based amorphous alloy strips by adopting a thermal spraying technologyThe Fe-based amorphous alloy coating comprises a nominal component of FeCrMoWxCBY，0≤x≤8。
In one embodiment of the present invention, in the step (1), the mixture ratio of each component includes: 99.7 wt.% Fe, 99.98 wt.% Cr, 99.9 wt.% Mo, 99.999 wt.% C, 99.5 wt.% W, 99.6 wt.% Y, 99.38 wt.% prealloyed FeB.
In one embodiment of the present invention, in step (4), the shielding gas includes, but is not limited to, high purity argon.
In one embodiment of the present invention, in the step (4), the Fe-based amorphous alloy ribbon with a width of 1mm to 1.5mm and a thickness of 30 μm to 50 μm is prepared at a rotation speed of 20 m/s to 40 m/s.
In one embodiment of the present invention, in the step (4), the process conditions of the thermal spraying technique are: the spraying distance is 150-180mm, the powder feeding speed is 40-50g/min, the propane pressure is 0.4-0.6MPa, the air pressure is 0.5-0.7MPa, and N is2Pressure of 0.2-0.4Mpa, H2The pressure is 0.05-0.1 MPa.
The invention also provides an application of the Fe-based amorphous alloy obtained based on the method, and the Fe-based amorphous alloy is used as a corrosion protection candidate material for lead-cooled fast reactors.
The invention adopts amorphous alloy as LBE alloy corrosion protective material, the amorphous alloy is also called as metal glass, because of the unique structural characteristics of long-range disorder and short-range order, the amorphous alloy generally has high strength and hardness, high elastic limit, excellent corrosion resistance and wear resistance, etc. The amorphous alloy has uniform component distribution on the macro and micro, and has no crystal structure defects (dislocation and grain boundary) of the traditional material, and the characteristics enable the amorphous alloy to have more excellent LBE corrosion resistance, and can reduce local corrosion caused by non-uniform components and the problems of grain boundary corrosion and embrittlement caused by the grain boundary. Meanwhile, although the Fe-based amorphous alloy has a series of excellent properties, the Fe-based amorphous alloy is difficult to be used as a large-scale structural member due to the limitations of glass forming capability and the critical dimension of the amorphous alloy, the size problem of the amorphous alloy can be solved by a thermal spraying technology, and the Fe-based amorphous alloy coating prepared by the thermal spraying technology (such as High Velocity Air furnace, HVAF) can be applied to parts such as nuclear waste storage tanks, water turbine blades and the like.
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
The present example provides four Fe-based amorphous alloys FeCrMoCBY (denoted as W0) and FeCrMoW2CBY (noted as W2), FeCrMoW4CBY (noted as W4), FeCrMoW6The preparation method of CBY (marked as W6) (Fe + W is a fixed value, and other contents are unchanged) comprises the following steps:
four Fe-based alloy ingots were prepared by arc melting of commercially pure Fe (99.7 wt.%), Cr (99.98 wt.%), Mo (99.9 wt.%), C (99.999 wt.%), W (99.5 wt.%), Y (99.6 wt.%) and prealloyed FeB (99.38 wt.%) in a titanium-getter argon atmosphere, each ingot being remelted at least four times to obtain compositional homogeneity; dripping the melt into a copper mold to prepare a rod-shaped sample; four Fe-based amorphous alloy strip samples with the width of 1.2mm and the thickness of about 40 mu m are prepared by adopting a single-roller melting and strip-spinning method under the argon atmosphere and at the rotating speed of 35 m/s. The X-ray diffraction patterns of four different Fe-based amorphous alloy strip samples are shown in figure 1. From fig. 1, it is concluded that the four different compositions of Fe-based alloys are amorphous.
Statically soaking the prepared sample W6 in an LBE alloy with oxygen saturation at 500 ℃ for 500h to obtain a W6 Fe-based amorphous alloy corrosion interface as shown in figure 2 (a); the comparative material was statically immersed in oxygen-saturated LBE alloy at 500 ℃ for 500 hours to obtain a CG9Cr + AlSi corrosion interface of other steel materials as shown in FIG. 2(b), and an oxide layer and ODZ were generated between the substrate and Pb-Bi. From fig. 2, it is concluded that W6 has a thickness of the etched interface less than CG9Cr + AlSi.
The graph comparing the corrosion rate of the W6 Fe-based amorphous alloy with other materials is shown in FIG. 3, and the conclusion is that the corrosion rate of the W6 Fe-based amorphous alloy is < SMRT 9Cr + AlSi <410SS < CG9Cr2WVTa < CLAM.
Example 2
This example provides a preparation method of four Fe-based amorphous alloys, fecrmobby (denoted as W0), FeCrMoW2CBY (denoted as W2), FeCrMoW4CBY (denoted as W4), and FeCrMoW6CBY (denoted as W6).
The preparation method is the same as that of example 1.
Four samples of W0, W2, W4 and W6 Fe-based amorphous alloys were statically immersed in 500 ℃ vacuum LBE alloy for 1000h, and the corrosion interface and EDS element line scan are shown in FIG. 4, and the EDS element line scan is used for calculating the thickness of the corrosion interface.
The TiC coating of the comparative material was statically immersed in a vacuum LBE alloy at 500 ℃ for 1000h, the corrosion-prone interface of which is shown in fig. 5. The conclusion is that the thickness of the corrosion interface of the W0, W2, W4 and W6 Fe-based amorphous alloy is less than that of the TiC coating.
The results of the etching rate are shown in FIG. 6
The corrosion rate of the above prepared samples W0, W2, W4 and W6 Fe-based amorphous alloy compared with other materials is shown in fig. 6, and it is concluded that the corrosion rate of W4 < W2< W0< W6< TiC coating < clamp.
Example 3
This example provides a Fe-based amorphous alloy as Fe47-xCr20Mo10WxC15B6Y2(x is 0 to 8 at.%).
The preparation method is the same as that of example 1. Mixing Fe47-xCr20Mo10WxC15B6Y2(x 0-8 at.%) the sample was statically soaked in oxygen-controlled LBE alloy at 500 ℃ for 500-1000 h.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
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| JPH01247555A (en) * | 1988-03-30 | 1989-10-03 | Hitachi Metals Ltd | Hyperfine-crystal fe-base alloy excellent in corrosion resistance and its production |
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| CN107513673A (en) * | 2017-07-18 | 2017-12-26 | 同济大学 | A kind of block Fe-based amorphous alloy and preparation method thereof |
| CN111020411A (en) * | 2019-12-11 | 2020-04-17 | 深圳大学 | Amorphous alloy net, preparation method thereof and application thereof in sewage treatment |
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Patent Citations (4)
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|---|---|---|---|---|
| JPH01247555A (en) * | 1988-03-30 | 1989-10-03 | Hitachi Metals Ltd | Hyperfine-crystal fe-base alloy excellent in corrosion resistance and its production |
| CN101323951A (en) * | 2007-06-13 | 2008-12-17 | 中国科学院金属研究所 | A kind of preparation method of non-magnetic high corrosion resistance wear-resistant amorphous steel coating |
| CN107513673A (en) * | 2017-07-18 | 2017-12-26 | 同济大学 | A kind of block Fe-based amorphous alloy and preparation method thereof |
| CN111020411A (en) * | 2019-12-11 | 2020-04-17 | 深圳大学 | Amorphous alloy net, preparation method thereof and application thereof in sewage treatment |
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| CN114717489A (en) * | 2022-03-23 | 2022-07-08 | 同济大学 | Liquid lead-bismuth alloy corrosion-resistant aluminum-containing iron-based amorphous alloy |
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