WO2023193451A1 - 一种提升FeCrAl基电阻合金力学和电阻性能的方法及FeCrAl基电阻合金 - Google Patents

一种提升FeCrAl基电阻合金力学和电阻性能的方法及FeCrAl基电阻合金 Download PDF

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WO2023193451A1
WO2023193451A1 PCT/CN2022/134252 CN2022134252W WO2023193451A1 WO 2023193451 A1 WO2023193451 A1 WO 2023193451A1 CN 2022134252 W CN2022134252 W CN 2022134252W WO 2023193451 A1 WO2023193451 A1 WO 2023193451A1
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alloy
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李志明
朱书亚
甘科夫
严定舜
张勇
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Central South University
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    • 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
    • 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
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/28—Ferrous alloys, e.g. steel alloys containing chromium with titanium or zirconium
    • 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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/34—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of silicon

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  • the invention belongs to the technical field of metal material preparation, and specifically relates to a method for improving the mechanical and resistance properties of FeCrAl-based resistance alloys and FeCrAl-based resistance alloys.
  • Resistance alloys with high resistivity (>100 ⁇ cm) and low temperature coefficient of resistivity (TCR) ( ⁇ 100ppm/K) are used in many key areas such as high-precision electronic measurement systems, GPS positioning systems, data storage, thermoelectric devices, and temperature Aspects such as control sensors play a vital role.
  • Iron-chromium-aluminum (FeCrAl)-based alloys are used as resistance alloys because of their advantages such as high resistivity, high strength, excellent high-temperature oxidation resistance, and low cost.
  • the growing industrial development requires low-cost resistance alloys with high strength, high deformability, high resistivity, and low temperature coefficient of resistivity to further improve processability, sensitivity, and promote the miniaturization and integration of electronic equipment. develop.
  • the following factors limit the further development and practical application of traditional FeCrAl-based alloys with low-cost advantages as resistive materials.
  • the traditional method to improve the strength and resistivity of Fe-Cr-A1 alloy is to increase the Cr and Al content.
  • high Cr and Al content can easily lead to stress concentration and aggravate brittle fracture, resulting in poor processability, that is, high strength and high machinability. It is difficult to have both deformability and deformability.
  • adjusting the ratio of Fe, Cr, and Al can adjust the temperature coefficient of resistivity, but it is often difficult to achieve both high resistivity and low resistivity temperature coefficient.
  • the present invention provides a method for improving the mechanical and resistance properties of FeCrAl-based resistance alloys and a FeCrAl-based resistance alloy to solve the problem of high resistivity and low resistivity temperature coefficient of traditional FeCrAl resistance alloys.
  • Technical problems include poor synergy between high strength and high deformability.
  • One of the objects of the present invention is to provide a FeCrAl-based resistance alloy that can achieve excellent comprehensive properties of high strength, high deformability, high resistivity, and low resistivity temperature coefficient in a wide temperature range.
  • the "wide temperature range” referred to in the present invention refers to a wide temperature range below 673K.
  • the "high strength” referred to in the present invention refers to the characteristics of the alloy material obtained by the present invention having a compressive yield strength of 600-1400MPa and a compressive strength of 900-2200MPa.
  • the “high deformability” referred to in the present invention refers to the characteristic that the alloy material obtained by the present invention has a compressive strain of more than 10%.
  • the “high resistivity” referred to in the present invention refers to the characteristics of the alloy material obtained by the present invention having a resistivity of 140 to 230 ⁇ .cm.
  • the “low temperature coefficient of resistivity” referred to in the present invention refers to the characteristic that the alloy material obtained by the present invention has a temperature coefficient of resistivity of -200 to 100 ppm/K.
  • the invention provides the following technical solution: a FeCrAl-based resistance alloy, which is composed of the following components in atomic percentage: Fe 52 ⁇ 59%, Cr 25 ⁇ 29%, Al 11 ⁇ 15%, Ti 2.5 ⁇ 5% and Si 1.5 ⁇ 3%;
  • the sum of the atomic percentages of Fe, Cr, and Al is ⁇ 92% and ⁇ 96%
  • the sum of the atomic percentages of Ti and Si is ⁇ 8% and ⁇ 4%
  • the sum of the atomic percentages of each component is 100%.
  • the composition of the alloy of the present invention in terms of atomic percentages may be, but is not limited to, 54% Fe, 27% Cr, 13.5% Al, 4% Ti, 1.5% Si; or 55% Fe, 28% Cr, 12% Al, 3 %Ti, 2%Si; or 52%Fe, 29%Cr, 14%Al, 2%Ti, 3%Si; or 59%Fe, 26%Cr, 11%Al, 2.5%Ti, 1.5%Si; or 56% Fe, 25% Cr, 13% Al, 3.5% Ti, 2.5% Si, etc.
  • Another object of the present invention is to provide a method for improving the mechanical and resistance properties of FeCrAl-based resistance alloys by introducing alloying elements Ti and Si into the FeCrAl alloy to induce the formation of a multi-component nanodispersed phase that is consistent with the BCC matrix of the FeCrAl alloy. ;
  • the sum of the atomic percentages of Ti and Si accounts for 4 to 8% of the total.
  • the "BCC matrix” referred to in the present invention refers to a body-centered cubic matrix.
  • dispersed phase in the present invention refers to the fine, dispersed solid phase formed by precipitation from a supersaturated solid solution.
  • the sum of the atomic percentages of Ti accounts for 2.5 to 5% of the total;
  • the total atomic percentage of Si accounts for 1.5 to 3% of the total.
  • the FeCrAl alloy is composed of Fe, Cr, and Al, and the sum of the atomic percentages of Fe accounts for 52 to 59% of the total, and Cr
  • the sum of the atomic percentages of Al accounts for 25 to 29% of the total, and the sum of the atomic percentages of Al accounts for 11 to 15% of the total.
  • the raw materials of each component are prepared according to the atomic ratio of each component of the alloy, and are smelted and poured under vacuum or inert gas protection conditions to obtain Alloy materials.
  • Melting refers to a pyrometallurgical process in which metal materials are put into a heating furnace to be melted to produce crude metal, which can be carried out using existing equipment such as suspension furnaces, induction furnaces, blast furnaces, reverberatory furnaces, and electric arc furnaces.
  • the melting is performed under vacuum conditions and the vacuum degree in the furnace is maintained at 1 to 0.0001 Pa.
  • the melting is carried out under inert gas protection conditions, and the inert gas pressure in the furnace is maintained at 0.000001 to 5 MPa.
  • the melting temperature is 1623-2473K and the temperature is maintained for 0.01-1 hour.
  • the raw materials for each component are pure metal element particles or blocks with a purity higher than 99wt.%, and are repeatedly smelted 3 to 8 times. .
  • the obtained alloy material has a compressive yield strength of 600-1400MPa, a compressive strength of 900-2200MPa, and a compressive strain of more than 10%;
  • the alloy has a resistivity of 140-230 ⁇ .cm in a wide temperature range below 673K; the temperature coefficient of resistivity is -200-100ppm/K.
  • the present invention has the following beneficial effects:
  • the present invention provides a new method, which is to induce the formation of a multi-component nanodispersed phase consistent with the BCC matrix by introducing appropriate amounts of alloying elements Ti and Si.
  • the multi-component L2 1 nanoparticle phase significantly increases the compressive strength of the alloy, enhances its deformability, increases the resistivity, reduces the temperature coefficient of resistivity, and shows an overall improvement in mechanical and resistive properties.
  • the method provided by the invention has a simple preparation process, does not require cumbersome heat treatment, and can obtain excellent performance in the casting state. This is expected to provide a new method to solve the problems of traditional FeCrAl resistance alloys such as difficulty in combining high resistivity and low resistivity temperature coefficient, and poor synergy between high strength and high deformability.
  • Figure 1 is an XRD spectrum of the FeCrAl-based resistance alloy obtained in Example 1 of the present invention.
  • Figure 2 shows the EBSD phase distribution diagram and inverse polar figure (IPF) of the FeCrAl-based resistance alloy obtained in Example 1 of the present invention.
  • Figure 3 is a scanning electron microscope morphology diagram of the microstructure of the FeCrAl-based resistance alloy obtained in Example 1 of the present invention.
  • Figure 4 is a high-angle annular dark field image (HAADF) and selected area electron diffraction spectrum of the FeCrAl-based resistance alloy obtained in Example 1 of the present invention under a transmission electron microscope.
  • HAADF high-angle annular dark field image
  • Figure 5 is a HAADF image under a transmission electron microscope of the FeCrAl-based resistance alloy obtained in Example 1 of the present invention and its corresponding energy spectrum surface distribution image.
  • Figure 6 is a resistivity-temperature curve of the FeCrAl-based resistance alloy obtained in Example 1 of the present invention.
  • Figure 7 is a compressive engineering stress-strain diagram at room temperature of the FeCrAl-based resistance alloy obtained in Example 1 of the present invention.
  • Figure 8 is a compressive engineering stress-strain diagram of the FeCrAl-based resistance alloy obtained in Example 1 of the present invention at 673K.
  • Figure 9 is a scanning electron microscope morphology diagram of the microstructure of the FeCrAl-based resistance alloy obtained in Example 2 of the present invention.
  • Figure 10 is a resistivity-temperature curve of the FeCrAl-based resistance alloy obtained in Example 2 of the present invention.
  • Figure 11 is a scanning electron microscope morphology of the microstructure of the FeCrAl-based resistance alloy obtained in Example 3 of the present invention.
  • Figure 12 is a resistivity-temperature curve of the FeCrAl-based resistance alloy obtained in Example 3 of the present invention.
  • Figure 13 is a room temperature compression engineering stress-strain diagram of the FeCrAl-based resistance alloy obtained in Example 3 of the present invention.
  • Figure 14 is a scanning electron microscope morphology diagram of the microstructure of the alloy obtained in Comparative Example 1 of the present invention.
  • Figure 15 is a resistivity-temperature curve diagram of the alloy obtained in Comparative Example 1 of the present invention.
  • Figure 16 is a room temperature compression engineering stress-strain diagram of the alloy obtained in Comparative Example 1 of the present invention.
  • Figure 17 is a scanning electron microscope morphology diagram of the microstructure of the alloy obtained in Comparative Example 2 of the present invention.
  • Figure 18 is a resistivity-temperature curve diagram of the alloy obtained in Comparative Example 2 of the present invention.
  • Figure 19 is a room temperature compression engineering stress-strain diagram of the alloy obtained in Comparative Example 2 of the present invention.
  • Figure 20 is an XRD spectrum of the alloy material provided in Comparative Example 3 of the present invention.
  • Figure 21 is the EBSD phase distribution diagram and inverse polar figure (IPF) of the alloy material provided in Comparative Example 3 of the present invention.
  • Figure 22 is a scanning electron microscope morphology diagram of the microstructure of the alloy material provided in Comparative Example 3 of the present invention.
  • Figure 23 is a scanning electron microscope backscattered electron image of the alloy material provided in Comparative Example 3 of the present invention and its corresponding energy spectrum surface distribution image.
  • Figure 24 is a resistivity-temperature curve diagram of the alloy material provided in Comparative Example 3 of the present invention.
  • Figure 25 is a compressive engineering stress-strain diagram at room temperature of the alloy material provided in Comparative Example 3 of the present invention.
  • Figure 26 is a scanning electron microscope morphology diagram of the microstructure of the alloy material provided in Comparative Example 4 of the present invention.
  • Figure 27 is a resistivity-temperature curve diagram of the alloy material provided in Comparative Example 4 of the present invention.
  • Figure 28 is a compressive engineering stress-strain diagram at room temperature of the alloy material provided in Comparative Example 4 of the present invention.
  • references herein to "one embodiment” or “an embodiment” refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. "In one embodiment” appearing in different places in this specification does not all refer to the same embodiment, nor is it a separate or selective embodiment that is mutually exclusive with other embodiments.
  • Ingredients are made according to the chemical formula Fe 55 Cr 28 Al 12 Ti 3 Si 2 (atomic percentage).
  • the raw materials use blocks corresponding to each pure element; suspension smelting is used to smelt under an inert gas protective atmosphere, and the smelting is repeated 4 times; the smelting is carried out in a vacuum After the temperature was raised to 0.001 Pa, argon gas was poured in until the pressure was slightly positive, the melting temperature was 1873K, the temperature was maintained for 5 minutes, and cast into a rectangular parallelepiped shape to obtain the FeCrAl-based resistance alloy of Example 1.
  • the main phase of the FeCrAl-based resistance alloy obtained in Example 1 is a BCC solid solution structure.
  • the nanodispersed particles in the FeCrAl-based resistance alloy obtained in Example 1 exhibit an L2 1 structure and have a completely coherent relationship with the BCC matrix.
  • the particle size is 45 ⁇ 11nm and the area percentage is 33% ⁇ 4%.
  • the dispersed L2 1 structure nanophases in the FeCrAl-based resistance alloy obtained in Example 1 are enriched in Al, Ti and Si elements and poor in Fe and Cr elements.
  • the room temperature resistivity of the FeCrAl-based resistance alloy obtained in Example 1 can be as high as ⁇ 183 ⁇ .cm, and it still remains at ⁇ 181 ⁇ .cm when the temperature is raised to 673K.
  • the temperature coefficient of resistivity in the temperature range from room temperature to 673K is as low as -35 ⁇ 10ppm/K.
  • the FeCrAl-based resistance alloy obtained in Example 1 has a compressive yield strength at room temperature of approximately 1096 MPa, a compressive strength of approximately 1694 MPa, and a compressive strain of approximately 20%.
  • the FeCrAl-based resistance alloy obtained in Example 1 has a compressive yield strength of about 1055MPa at 673K, a compressive strength of up to 1980MPa, and a compressive strain of up to 35%.
  • Ingredients are made according to the chemical formula Fe 55 Cr 28 Al 12 Ti 3 Si 2 (atomic percentage).
  • the raw materials use blocks corresponding to each pure element; suspension smelting is used to smelt under an inert gas protective atmosphere, and the smelting is repeated 4 times; the smelting is carried out in a vacuum After the temperature is pumped to 0.001 Pa, argon gas is injected until the pressure is slightly positive. The melting temperature is 1873K. Hold the heat for 5 minutes. Cast it into a rectangular shape. The alloy is raised from room temperature to 673K at a heating rate of 4K/min and then quickly quenched. That is The FeCrAl-based resistance alloy of Example 2 was obtained.
  • Ingredients are made according to the chemical formula Fe 54 Cr 27 Al 13.5 Ti 4 Si 1.5 (atomic percentage).
  • the raw materials use blocks corresponding to each pure element; arc melting is used to smelt under an inert gas protective atmosphere, and the smelting is repeated 4 times; smelting is carried out in a vacuum
  • the temperature was raised to 0.001 Pa, and then argon gas was poured in until the pressure was slightly positive.
  • the melting temperature was 1873K, and the FeCrAl-based resistance alloy of Example 3 was obtained.
  • the nanoparticles are dispersedly distributed in the FeCrAl-based resistance alloy obtained in Example 3.
  • the room temperature resistivity of the FeCrAl-based resistance alloy obtained in Example 3 can be as high as ⁇ 184 ⁇ .cm, and it still remains at ⁇ 180 ⁇ .cm when the temperature is raised to 673K.
  • the temperature coefficient of resistivity in the temperature range from room temperature to 673K is as low as -58ppm/K.
  • the FeCrAl-based resistance alloy obtained in Example 3 has a compressive yield strength of approximately 1243MPa, a compressive strength of approximately 1823MPa, and a compressive strain of approximately 17%.
  • Ingredients are made according to the chemical formula Fe 58 Cr 22 Al 15 Ti 1 Si 4 (atomic percentage).
  • the raw materials use blocks corresponding to each pure element; arc melting is used to smelt under an inert gas protective atmosphere, and the smelting is repeated 4 times; vacuum is used during smelting. After pumping the temperature to 0.001 Pa, argon gas was injected until the pressure was slightly positive. The melting temperature was 1873K, and the alloy in Comparative Example 1 was obtained.
  • the alloy obtained in Comparative Example 1 has signs of the presence of nanoparticles. It can be seen from Figure 15 that the room temperature resistivity of the alloy obtained in Comparative Example 1 is approximately 204 ⁇ .cm. The temperature coefficient of resistivity in the temperature range from room temperature to 673K is approximately -159ppm/K. It can be seen from Figure 16 that the compressive yield strength of the alloy obtained in Comparative Example 1 is about 850MPa, the compressive strength is about 1878MPa, and the compressive strain is about 30%.
  • Ingredients are made according to the chemical formula Fe 56 Cr 25 Al 14 Ti 2 Si 3 (atomic percentage).
  • the raw materials use blocks corresponding to each pure element; arc melting is used to smelt under an inert gas protective atmosphere, and the smelting is repeated 4 times; smelting is carried out in a vacuum After pumping the temperature to 0.001 Pa, argon gas was injected until the pressure was slightly positive. The melting temperature was 1873K, and the alloy in Comparative Example 2 was obtained.
  • the alloy obtained in Comparative Example 2 has dispersed nanoparticles. It can be seen from Figure 18 that the room temperature resistivity of the alloy obtained in Comparative Example 2 is approximately 197 ⁇ .cm. The temperature coefficient of resistivity in the temperature range from room temperature to 673K is approximately -171ppm/K. It can be seen from Figure 19 that the compressive yield strength of the alloy obtained in Comparative Example 2 is about 980MPa, the compressive strength is about 2026MPa, and the compressive strain is about 30%.
  • Ingredients are made according to the chemical formula Fe 55 Cr 28 Al 12 Ti 3 Si 2 (atomic percentage).
  • the raw materials use blocks corresponding to each pure element; suspension smelting is used to smelt under an inert gas protective atmosphere, and the smelting is repeated 4 times; the smelting is carried out in a vacuum
  • argon gas is injected until the pressure is slightly positive, the melting temperature is 1873K, the temperature is maintained for 5 minutes, and the shape is cast into a rectangular parallelepiped; then high-temperature homogenization treatment is performed under an argon protective atmosphere (argon pressure is 10Pa).
  • the temperature is 1573K, the homogenization treatment time is 3 hours and then oil quenched, and the alloy of Comparative Example 3 is obtained.
  • Ingredients are made according to the chemical formula Fe 55 Cr 29 Al 16 (atomic percentage).
  • the raw materials use blocks corresponding to each pure element; arc melting is used to smelt under an inert gas protective atmosphere, and the smelting is repeated 4 times; the vacuum is pumped to 0.001 during smelting. After the sealing, argon gas was injected until the pressure was slightly positive, and the melting temperature was 1873K, thus obtaining the alloy of Comparative Example 4.
  • Comparing Example 1 and Comparative Example 3 it can be seen that the compressive strength, compressive strain and resistance of the alloy that does not contain the multi-component L2 1 nanodispersed phase that is completely consistent with the BCC matrix provided by the method of the present invention, that is, the alloy of Comparative Example 3
  • the temperature stability is worse than that of Example 1.
  • Comparing Example 1 and Comparative Example 4 it can be seen that the compressive yield strength of the alloy without introducing Ti and Si elements is much lower than the yield strength of the alloy obtained after optimization of the present invention, and the resistivity temperature stability is poor.
  • the present invention introduces appropriate amounts of alloying elements Ti and Si to induce the formation of a multi-component nano-dispersed phase multi-component L2 1 nano-dispersed phase that is consistent with the body-centered cubic (BCC) matrix, which can effectively improve the deformability and deformability within 673K.
  • BCC body-centered cubic
  • Resistivity-Temperature Stability Comparing Example 1 and Comparative Example 5, it can be seen that the alloy obtained by the method of the present invention has both high resistivity and low temperature coefficient of resistivity.
  • the present invention provides a method for improving the mechanical and resistance properties of FeCrAl-based resistance alloys, that is, by introducing appropriate amounts of alloying elements Ti and Si to induce the formation of a multi-component nanodispersed phase consistent with the BCC matrix. It has the following characteristics: first, the alloying elements Ti and Si are introduced in appropriate amounts to induce the formation of a multi-component nanodispersed phase that is completely consistent with the BCC matrix. This coherent multi-component nanodispersed phase maintains high strength while improving work hardening ability, thereby increasing compressive strength and compressive strain. Secondly, the existence of the multi-component coherent nanodispersed phase reduces the temperature coefficient of resistivity.
  • the atomic radii of the added alloy elements Ti and Si are quite different from the atomic radii of Fe and Cr elements, resulting in large lattice distortion, effectively improving the solid solution strengthening effect and lattice scattering effect in the alloy, and thus Improves strength and resistivity.
  • this alloy does not contain rare metal elements and can be developed into an environmentally friendly resistance alloy. That is to say, through the technical measures provided by this invention, excellent comprehensive characteristics of high strength, high deformability, high resistivity, and low temperature coefficient of resistivity can be achieved in a wide temperature range.

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Abstract

本发明公开了一种提升FeCrAl基电阻合金力学和电阻性能的方法及FeCrAl基电阻合金，本发明通过向FeCrAl合金中引入合金元素Ti和Si诱导形成与FeCrAl合金的BCC基体共格的多组分纳米弥散相；优化后的合金化学组成为：Fe 52～59％，Cr 25～29％，Al 11～15％，Ti 2.5～5％，Si 1.5～3％。本发明方法获得的合金基体呈现BCC结构组织特征，基体中弥散分布着具有L2 1结构的多组分纳米颗粒，纳米颗粒与BCC基体保持完全共格的取向关系，使得合金压缩强度显著提升，可变形能力增强，并且提高了电阻率，降低了电阻率温度系数，表现出力学和电阻性能的全面提升。

Description

一种提升FeCrAl基电阻合金力学和电阻性能的方法及FeCrAl基电阻合金 技术领域
本发明属于金属材料制备技术领域，具体涉及到一种提升FeCrAl基电阻合金力学和电阻性能的方法及FeCrAl基电阻合金。
背景技术
具有高电阻率(＞100μΩ·cm)和低电阻率温度系数(TCR)(<100ppm/K)的电阻合金在许多关键领域如高精密电子测量系统、GPS定位系统、数据存储、热电设备以及温度控制传感器等方面起着至关重要的作用。铁铬铝(FeCrAl)基合金因具备高电阻率、高强度、优异的抗高温氧化性和低成本等优势而作为电阻合金使用。
日益增长的工业发展，需要兼具高强度、高可变形性、高电阻率、低电阻率温度系数的低成本电阻合金，以进一步提高可加工性、灵敏度以及推动电子设备的小型化、集成化发展。然而，以下因素限制了具备低成本优势的传统FeCrAl基合金作为电阻材料的进一步发展和实际应用。首先，提高Fe-Cr-A1合金强度和电阻率的传统方法是增加Cr和Al含量，但高Cr和Al含量容易导致应力集中而加剧脆性断裂，致使可加工能力差，即高强度和高可变形性难以兼具。其次，调整Fe、Cr、Al的比例可以调节电阻率温度系数，但高电阻率和低电阻率温度系数往往难以兼具。
发明内容
本部分的目的在于概述本发明的实施例的一些方面以及简要介绍一些较佳实施例。在本部分以及本申请的说明书摘要和发明名称中可能会做些简化或省略以避免使本部分、说明书摘要和发明名称的目的模糊，而这种简化或省略不能用于限制本发明的范围。
鉴于上述和/或现有技术中存在的不足，本发明提供一种提升FeCrAl基电阻合金力学和电阻性能的方法及FeCrAl基电阻合金，解决传统FeCrAl电阻合金高电阻率与低电阻率温度系数难以兼具、高强度与高可变形性协同能力差等技术问题。
本发明的其中一个目的是提供一种FeCrAl基电阻合金，其可实现宽温域内兼具高强度、高可变形性、高电阻率、低电阻率温度系数的优异综合特性。
在此，本发明所称的“宽温域”是指673K以下的宽温域。本发明所称的 “高强度”是指本发明所得合金材料具有压缩屈服强度在600～1400MPa，抗压强度在900～2200MPa的特性。本发明所称的“高可变形性”是指本发明所得合金材料具有压缩应变在10％以上的特性。本发明所称的“高电阻率”是指本发明所得合金材料具有电阻率为140～230μΩ.cm的特性。本发明所称的“低电阻率温度系数”是指本发明所得合金材料具有电阻率温度系数为-200～100ppm/K的特性。
本发明提供了如下技术方案：一种FeCrAl基电阻合金，由下述组分按原子百分比组成：Fe 52～59％、Cr 25～29％、Al 11～15％、Ti 2.5～5％和Si 1.5～3％；
其中，Fe、Cr、Al的原子百分比之和≥92％且≤96％，Ti、Si的原子百分比之和≤8％且≥4％，各组分原子百分比之和为100％。
例如，本发明的合金按原子百分比组成可以是，但不限于54％Fe、27％Cr、13.5％Al、4％Ti、1.5％Si；或55％Fe、28％Cr、12％Al、3％Ti、2％Si；或52％Fe、29％Cr、14％Al、2％Ti、3％Si；或59％Fe、26％Cr、11％Al、2.5％Ti、1.5％Si；或56％Fe、25％Cr、13％Al、3.5％Ti、2.5％Si等。
本发明的另一个目的是提供一种提升FeCrAl基电阻合金力学和电阻性能的方法，通过向FeCrAl合金中引入合金元素Ti和Si诱导形成与FeCrAl合金的BCC基体共格的多组分纳米弥散相；
其中，Ti、Si的原子百分比之和占总体的4～8％。
在此处，本发明所称“BCC基体”是指体心立方基体。
本发明所称“弥散相”是指从过饱和固溶体中析出形成的细小、弥散分布的固相。
作为本发明提升FeCrAl基电阻合金力学和电阻性能的方法的一种优选方案，其中：所述Ti的原子百分比之和占总体的2.5～5％；
所述Si的原子百分比之和占总体的1.5～3％。
作为本发明提升FeCrAl基电阻合金力学和电阻性能的方法的一种优选方案，其中：所述FeCrAl合金，由Fe、Cr、Al组成，Fe的原子百分比之和占总体的52～59％，Cr的原子百分比之和占总体的25～29％，Al的原子百分比之和占总体的11～15％。
作为本发明提升FeCrAl基电阻合金力学和电阻性能的方法的一种优选方案，其中：按合金各组元原子配比配取各组分原料，在真空或惰性气体保护条 件下熔炼，浇注，得合金材料。
本发明所称“熔炼”是指，将金属材料投入加热炉熔化产出粗金属的火法冶金过程，可以采用悬浮炉、感应炉、鼓风炉、反射炉、电弧炉等现有设备进行。
作为本发明提升FeCrAl基电阻合金力学和电阻性能的方法的一种优选方案，其中：所述在真空条件下熔炼，维持炉内真空度在1～0.0001帕。
作为本发明提升FeCrAl基电阻合金力学和电阻性能的方法的一种优选方案，其中：所述在惰性气体保护条件下熔炼，维持炉内惰性气体压力在0.000001～5兆帕。
作为本发明提升FeCrAl基电阻合金力学和电阻性能的方法的一种优选方案，其中：所述熔炼，熔炼温度为1623～2473K，并保温0.01～1h。
作为本发明提升FeCrAl基电阻合金力学和电阻性能的方法的一种优选方案，其中：所述各组分原料采用纯度高于99wt.％的纯金属元素颗粒或块体，反复熔炼3～8次。
作为本发明提升FeCrAl基电阻合金力学和电阻性能的方法的一种优选方案，其中：所得合金材料，具有压缩屈服强度在600～1400MPa，抗压强度在900～2200MPa，压缩应变在10％以上；合金在673K以下的宽温域内，电阻率为140～230μΩ.cm；电阻率温度系数为-200～100ppm/K的特性。
与现有技术相比，本发明具有如下有益效果：
本发明提供一种新方法，即通过引入适量合金元素Ti和Si诱导形成与BCC基体共格的多组分纳米弥散相。该多组分L2 1纳米颗粒相使得合金压缩强度显著提升，可变形能力增强，并且提高了电阻率，降低了电阻率温度系数，表现出力学和电阻性能的全面提升。本发明所提供的方法制备工艺简单、无需进行繁琐的热处理，铸造状态下即可获得优异性能。这有望为解决传统FeCrAl电阻合金高电阻率与低电阻率温度系数难以兼具、高强度与高可变形性协同能力差等问题提供新方法。
附图说明
为了更清楚地说明本实用新型实施例的技术方案，下面将对实施例描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本实用新型的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动性 的前提下，还可以根据这些附图获得其它的附图。其中：
图1为本发明实施例1所得FeCrAl基电阻合金的XRD谱图。
图2为本发明实施例1所得FeCrAl基电阻合金的EBSD相分布图及反极图(IPF)。
图3为本发明实施例1所得FeCrAl基电阻合金的微观组织的扫描电镜形貌图。
图4为本发明实施例1所得FeCrAl基电阻合金透射电镜下的高角环形暗场像(HAADF)及选区电子衍射谱图。
图5为本发明实施例1所得FeCrAl基电阻合金透射电镜下的HAADF图像及其对应的能谱面分布图像。
图6为本发明实施例1所得FeCrAl基电阻合金的电阻率-温度曲线图。
图7为本发明实施例1所得FeCrAl基电阻合金室温下的压缩工程应力-应变图。
图8为本发明实施例1所得FeCrAl基电阻合金在673K下的压缩工程应力-应变图。
图9为本发明实施例2所得FeCrAl基电阻合金的微观组织的扫描电镜形貌图。
图10为本发明实施例2所得FeCrAl基电阻合金的电阻率-温度曲线图。
图11为本发明实施例3所得FeCrAl基电阻合金的微观组织的扫描电镜形貌图。
图12为本发明实施例3所得FeCrAl基电阻合金的电阻率-温度曲线图。
图13为本发明实施例3所得FeCrAl基电阻合金的室温压缩工程应力-应变图。
图14为本发明对比例1所得合金的微观组织的扫描电镜形貌图。
图15为本发明对比例1所得合金的电阻率-温度曲线图。
图16为本发明对比例1所得合金的室温压缩工程应力-应变图。
图17为本发明对比例2所得合金的微观组织的扫描电镜形貌图。
图18为本发明对比例2所得合金的电阻率-温度曲线图。
图19为本发明对比例2所得合金的室温压缩工程应力-应变图。
图20为本发明对比例3提供的合金材料的XRD谱图。
图21为本发明对比例3提供的合金材料的EBSD相分布图及反极图(IPF)。
图22为本发明对比例3提供的合金材料的微观组织的扫描电镜形貌图。
图23为本发明对比例3提供的合金材料的扫描电镜背散射电子图像及其对应的能谱面分布图像。
图24为本发明对比例3提供的合金材料的电阻率-温度曲线图。
图25为本发明对比例3提供的合金材料室温下的压缩工程应力-应变图。
图26为本发明对比例4提供的合金材料的微观组织的扫描电镜形貌图。
图27为本发明对比例4提供的合金材料的电阻率-温度曲线图。
图28为本发明对比例4提供的合金材料室温下的压缩工程应力-应变图。
具体实施方式
为使本发明的上述目的、特征和优点能够更加明显易懂，下面结合说明书实施例对本发明的具体实施方式做详细的说明。
在下面的描述中阐述了很多具体细节以便于充分理解本发明，但是本发明还可以采用其他不同于在此描述的其它方式来实施，本领域技术人员可以在不违背本发明内涵的情况下做类似推广，因此本发明不受下面公开的具体实施例的限制。
其次，此处所称的“一个实施例”或“实施例”是指可包含于本发明至少一个实现方式中的特定特征、结构或特性。在本说明书中不同地方出现的“在一个实施例中”并非均指同一个实施例，也不是单独的或选择性的与其他实施例互相排斥的实施例。
实施例1
按照化学式Fe 55Cr 28Al 12Ti 3Si 2(原子百分数)进行配料，原料使用各纯元素对应的块体；采用悬浮熔炼，在惰性气体保护气氛下进行熔炼，反复熔炼4次；熔炼时真空度抽至0.001帕后冲入氩气至气压微正，熔炼温度为1873K，保温5min，浇铸成长方体形状，即得实施例1的FeCrAl基电阻合金。
由图1和图2可见，实施例1所得FeCrAl基电阻合金主相为BCC固溶体结构。由图3可见，实施例1所得FeCrAl基电阻合金中存在弥散分布的纳米颗粒。由图4可见，实施例1所得FeCrAl基电阻合金中的纳米弥散颗粒呈现L2 1结构，且与BCC基体呈现完全共格关系，颗粒尺寸为45±11nm，面积百分比为33％±4％。由图5可见，实施例1所得FeCrAl基电阻合金中弥散分布 的L2 1结构的纳米相同时富集Al、Ti和Si元素，贫瘠Fe和Cr元素。从图6可见，实施例1所得FeCrAl基电阻合金的室温电阻率可高达～183μΩ.cm，在升温至673K时依然维持在～181μΩ.cm。室温至673K温度范围内的电阻率温度系数低至-35±10ppm/K。从图7可见，实施例1所得FeCrAl基电阻合金在室温下的压缩屈服强度约为1096MPa，抗压强度约为1694MPa，压缩应变约为20％。从图8可见，实施例1所得FeCrAl基电阻合金在673K下的压缩屈服强度约为1055MPa，抗压强度可高达1980MPa，压缩应变可高达35％。
实施例2
按照化学式Fe 55Cr 28Al 12Ti 3Si 2(原子百分数)进行配料，原料使用各纯元素对应的块体；采用悬浮熔炼，在惰性气体保护气氛下进行熔炼，反复熔炼4次；熔炼时真空度抽至0.001帕后冲入氩气至气压微正，熔炼温度为1873K，保温5min，浇铸成长方体形状，将合金经历以4K/min的升温速率由室温升至673K后快速淬火之后，即得实施例2的FeCrAl基电阻合金。
从图9和10可见，实施例2所得FeCrAl基电阻合金中的L2 1结构的纳米弥散相在673K温度下依然稳定存在，决定室温至673K温度范围内的低电阻率温度系数(-46ppm/K)。
实施例3
按照化学式Fe 54Cr 27Al 13.5Ti 4Si 1.5(原子百分数)进行配料，原料使用各纯元素对应的块体；采用电弧熔炼，在惰性气体保护气氛下进行熔炼，反复熔炼4次；熔炼时真空度抽至0.001帕后冲入氩气至气压微正，熔炼温度为1873K，即得实施例3的FeCrAl基电阻合金。
从图11可见，实施例3所得FeCrAl基电阻合金中在弥散分布的纳米颗粒。由图12可见，实施例3所得FeCrAl基电阻合金的室温电阻率可高达～184μΩ.cm，在升温至673K时依然维持在～180μΩ.cm。室温至673K温度范围内的电阻率温度系数低至-58ppm/K。从图13可见，实施例3所得FeCrAl基电阻合金的压缩屈服强度约为1243MPa，抗压强度约为1823MPa，压缩应变约为17％。
对比例1
按照化学式Fe 58Cr 22Al 15Ti 1Si 4(原子百分数)进行配料，原料使用各纯元素对应的块体；采用电弧熔炼，在惰性气体保护气氛下进行熔炼，反复熔炼4次； 熔炼时真空度抽至0.001帕后冲入氩气至气压微正，熔炼温度为1873K，即得对比例1中的合金。
由图14可见对比例1所得合金有存在纳米颗粒的迹象。由图15可见对比例1所得合金的室温电阻率约为204μΩ.cm。室温至673K温度范围内的电阻率温度系数约为-159ppm/K。由图16可见对比例1所得合金的压缩屈服强度约为850MPa，抗压强度约为1878MPa，压缩应变约为30％。
对比例2
按照化学式Fe 56Cr 25Al 14Ti 2Si 3(原子百分数)进行配料，原料使用各纯元素对应的块体；采用电弧熔炼，在惰性气体保护气氛下进行熔炼，反复熔炼4次；熔炼时真空度抽至0.001帕后冲入氩气至气压微正，熔炼温度为1873K，即得对比例2中的合金。
由图17可见对比例2所得合金的存在弥散纳米颗粒。由图18可见对比例2所得合金的室温电阻率约为197μΩ.cm。室温至673K温度范围内的电阻率温度系数约为-171ppm/K。由图19可见对比例2所得合金的压缩屈服强度约为980MPa，抗压强度约为2026MPa，压缩应变约为30％。
对比例3
按照化学式Fe 55Cr 28Al 12Ti 3Si 2(原子百分数)进行配料，原料使用各纯元素对应的块体；采用悬浮熔炼，在惰性气体保护气氛下进行熔炼，反复熔炼4次；熔炼时真空度抽至0.001帕后冲入氩气至气压微正，熔炼温度为1873K，保温5min，浇铸成长方体形状；然后进行高温均匀化处理，在氩气保护氛围下进行(氩气压力为10Pa)，温度为1573K，均匀化处理时间为3小时后油淬，即得对比例3的合金。
从图20和21可见，对比例3所得合金呈现单相BCC结构。附图22和23进一步证实对比例3所得合金不存在弥散分布的纳米颗粒。从图24可见，对比例3所得合金室温至673K温度范围内的电阻率温度系数为-163±10ppm/K。从图25可见，对比例3所得合金的压缩屈服强度约为1191MPa，抗压强度仅为1254MPa，压缩应变仅为8％。
对比例4
按照化学式Fe 55Cr 29Al 16(原子百分数)进行配料，原料使用各纯元素对应的块体；采用电弧熔炼，在惰性气体保护气氛下进行熔炼，反复熔炼4次；熔 炼时真空度抽至0.001帕后冲入氩气至气压微正，熔炼温度为1873K，即得对比例4的合金。
从图26可见，对比例4所得合金为单相BCC结构。从图27可见，对比例4所得合金室温至673K温度范围内的电阻率温度系数约为-146ppm/K。从图28可见，对比例4所得合金的压缩屈服强度远低于实施例1或2的强度。
对比例5
根据公开文献Metallurgical transactions A的记载[T.Naohara,A.Inoue,T.Minemura,T.Masumoto,K.Kumada,Metallurgical transactions A 13(1982)337-343]，传统Fe 65Cr 20Al 15、Fe 60Cr 20Al 20、Fe 50Cr 30Al 20合金的室温电阻率分别为156μΩ.cm,180μΩ.cm和186μΩ.cm；室温至673K范围内的电阻率温度系数分别为-17ppm/K、-73ppm/K和-85ppm/K。即高电阻率与低电阻率温度系数难以兼具。
比较实施例1、2和3可知：经本发明提供的方法优化后的合金中存在的与BCC基体完全共格的多组分L2 1纳米弥散相可以在673K下稳定存在，优化后的合金具备优异的中温力学性能、同时保持了高电阻率和673K以内的电阻率-温度稳定性。
比较实施例1和对比例1、2可知，所引入的Ti、Si元素含量不在我方发明范围内时所得合金，电阻率温度稳定性明显比实施例1差。
比较实施例1和对比例3可知，不含本发明方法所提供的与BCC基体完全共格的多组分L2 1纳米弥散相的合金，即对比例3合金，抗压强度、压缩应变及电阻率温度稳定性均比实施例1差。比较实施例1和对比例4可知，不引入Ti和Si元素的合金的压缩屈服强度远低于本发明优化后所得合金的屈服强度，且电阻率温度稳定性差。即本发明通过引入适量合金元素Ti和Si诱导形成与体心立方(BCC)基体共格的多组分纳米弥散相多组分L2 1纳米弥散相，能够有效地提升可变形能力和673K以内的电阻率-温度稳定性。比较实施例1和对比例5可知，本发明方法所获取的合金兼具高电阻率和低电阻率温度系数。
本发明提供一种提升FeCrAl基电阻合金力学和电阻性能的方法，即通过引入适量合金元素Ti和Si诱导形成与BCC基体共格的多组分纳米弥散相。具有以下特点：首先，适量引入合金元素Ti和Si，诱导形成与BCC基体完全共格的多组分纳米弥散相。该共格多组分纳米弥散相维持高强度的同时提高了加 工硬化能力进而提升抗压强度和压缩应变。其次，该多组分共格纳米弥散相的存在降低了电阻率温度系数。再者，所添加的合金元素Ti和Si的原子半径与Fe和Cr元素的原子半径相差较大，产生较大的晶格畸变，有效提高合金中的固溶强化效应以及晶格散射作用，进而提升强度和电阻率。此外，该合金与传统FeCrAl合金相比，不含有稀有金属元素可发展为环境友好型电阻合金。即通过该发明提供的技术措施，可实现宽温域内兼具高强度、高可变形性、高电阻率、低电阻率温度系数的优异综合特性。
应说明的是，以上实施例仅用以说明本发明的技术方案而非限制，尽管参照较佳实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的精神和范围，其均应涵盖在本发明的权利要求范围当中。

Claims (10)

  1. 一种FeCrAl基电阻合金，其特征在于：由下述组分按原子百分比组成：Fe 52～59％、Cr 25～29％、Al 11～15％、Ti 2.5～5％和Si 1.5～3％；
    其中，Fe、Cr、Al的原子百分比之和≥92％且≤96％，Ti、Si的原子百分比之和≤8％且≥4％，各组分原子百分比之和为100％。
  2. 一种提升FeCrAl基电阻合金力学和电阻性能的方法，其特征在于：通过向FeCrAl合金中引入合金元素Ti和Si诱导形成与FeCrAl合金的BCC基体共格的多组分纳米弥散相；
    其中，Ti、Si的原子百分比之和占总体的4～8％。
  3. 如权利要求2所述的提升FeCrAl基电阻合金力学和电阻性能的方法，其特征在于：所述Ti的原子百分比之和占总体的2.5～5％；
    所述Si的原子百分比之和占总体的1.5～3％。
  4. 如权利要求2或3所述的提升FeCrAl基电阻合金力学和电阻性能的方法，其特征在于：所述FeCrAl合金，由Fe、Cr、Al组成，Fe的原子百分比之和占总体的52～59％，Cr的原子百分比之和占总体的25～29％，Al的原子百分比之和占总体的11～15％。
  5. 如权利要求4所述的提升FeCrAl基电阻合金力学和电阻性能的方法，其特征在于：按合金各组元原子配比配取各组分原料，在真空或惰性气体保护条件下熔炼，得合金材料。
  6. 如权利要求5所述的提升FeCrAl基电阻合金力学和电阻性能的方法，其特征在于：所述在真空条件下熔炼，维持炉内真空度在1～0.0001帕。
  7. 如权利要求5所述的提升FeCrAl基电阻合金力学和电阻性能的方法，其特征在于：所述在惰性气体保护条件下熔炼，维持炉内惰性气体压力在0.000001～5兆帕。
  8. 如权利要求5～7中任一项所述的提升FeCrAl基电阻合金力学和电阻性能的方法，其特征在于：所述熔炼，熔炼温度为1623～2473K，并保温0.01～1h。
  9. 如权利要求8所述的提升FeCrAl基电阻合金力学和电阻性能的方法，其特征在于：所述各组分原料采用纯度高于99wt.％的纯金属元素颗粒或块体，反复熔炼3～8次。
  10. 如权利要求2、3、5～7、9中任一项所述的提升FeCrAl基电阻合金力学和电阻性能的方法，其特征在于：所得合金材料，具有压缩屈服强度在600～1400 MPa，抗压强度在900～2200MPa，压缩应变在10％以上；合金在673K以下的宽温域内，电阻率为140～230μΩ.cm；电阻率温度系数为-200～100ppm/K的特性。
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