CN113862542B - Nano-scale silicide and Laves phase reinforced refractory high-entropy alloy material and preparation method thereof - Google Patents

Nano-scale silicide and Laves phase reinforced refractory high-entropy alloy material and preparation method thereof Download PDF

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CN113862542B
CN113862542B CN202111096394.1A CN202111096394A CN113862542B CN 113862542 B CN113862542 B CN 113862542B CN 202111096394 A CN202111096394 A CN 202111096394A CN 113862542 B CN113862542 B CN 113862542B
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马兆龙
刘宸毓
徐子祁
程兴旺
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Beijing Institute of Technology BIT
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Abstract

The invention relates to a nanoscale silicide and Laves phase reinforced refractory high-entropy alloy material and a preparation method thereof, belonging to the field of high-entropy alloys. The novel alloy is composed of Nb, ti, ta, cr, al, V, si, mo and other elements, the alloy is of a single-phase BCC structure under the as-cast condition, and the alloy is processed by cold deformation and a subsequent heat treatment method to obtain a large amount of nano-scale M5Si3 phase and Laves phase which are dispersed and distributed. The density of the alloy is less than or equal to 8g/cm 3 The composite material has high tensile yield strength and elongation at break, and excellent mechanical properties. The yield strength can reach more than 850MPa, and the elongation at break is more than 10%. Meanwhile, the alloy has good oxidation resistance at high temperature.

Description

Nano-scale silicide and Laves phase reinforced refractory high-entropy alloy material and preparation method thereof
Technical Field
The invention relates to a nanoscale silicide and Laves phase reinforced refractory high-entropy alloy material and a preparation method thereof, belonging to the field of high-entropy alloys.
Background
The high-entropy alloy is a brand-new alloy material formed by a plurality of metal elements according to an equal atomic ratio or a nearly equal atomic ratio. Different from the design concept of the traditional alloy, the high-entropy alloy realizes that the thermodynamics 'entropy' is taken as the main control factor of the alloy structure through the multi-component mixed design. Thus, the high-entropy alloy has important performances of high strength, high hardness and corrosion resistance, and shows different performance characteristics due to flexible and changeable component proportion regulation of alloy components. The refractory high-entropy alloy (RHAS) is a multi-component alloy composed of W, mo, nb, ta, V, ti, zr, hf and other refractory metal elements. Due to the characteristics of high melting point and solid solution strengthening, many refractory high-entropy alloys show remarkably excellent high-temperature strength at high temperature, and are expected to become a new-generation high-temperature alloy.
However, the application of the high-entropy alloy is severely limited by the problems of high density, poor plasticity, poor high-temperature oxidation resistance and the like. Some refractory high-entropy alloy systems with better plasticity, such as hfnbtatzr and the like, have a single-phase structure and show lower strength at high temperature. The addition of Al, cr, si and other elements on the tough matrix can introduce a second phase, effectively improve the strength and improve the high-temperature oxidation resistance. However, the distribution and morphology of the second phase can greatly reduce the plastic deformability of the alloy. Therefore, at present, no refractory high-entropy alloy has an alloy with low density, oxidation resistance and strong plasticity matching, which is one of the problems to be solved in the research of the refractory high-entropy alloy. The invention provides a nano-scale silicide and Laves phase reinforced refractory high-entropy alloy material and a preparation method thereof, aiming at solving the defects of the refractory high-entropy alloy, the invention obviously reduces the alloy density through component regulation and control, improves the oxidation resistance of an alloy matrix at high temperature, introduces nano-scale particles of the silicide and the Laves phase through a subsequent processing technology, and simultaneously ensures higher strength and plasticity.
Disclosure of Invention
The invention aims to solve the problems that the high-entropy refractory alloy has high density and cannot simultaneously give consideration to strong plasticity and high-temperature oxidation resistance, and provides a nanoscale silicide and Laves phase reinforced high-entropy refractory alloy material and a preparation method thereof.
In order to achieve the above purpose, the invention is realized by the following technical scheme.
A nanometer silicide and Laves phase enhanced refractory high-entropy alloy comprises an NbTiTaCrAlVSiMo series alloy composed of eight elements such as Nb, ti, ta, cr, al, V, si, mo and the like, wherein the atomic percentage ranges of the elements are respectively as follows: nb is more than or equal to 30 percent and less than or equal to 50 percent, ti is more than or equal to 25 percent and less than or equal to 35 percent, ta is more than 0 and less than or equal to 20 percent, al and Cr are more than 5 percent and less than or equal to 15 percent, si is more than 0 and less than or equal to 5 percent, and V and Mo are more than 0 and less than or equal to 10 percent. The NbTiTaCrAlVSiMo alloy shows a single-phase BCC structure under the as-cast condition. After rolling and heat treatment, the alloy consists of BCC phase with fine crystalline structure, nanometer M5Si3 phase and Laves phase.
The design principle of the alloy components is as follows: the phase formation of the alloy matrix is mainly determined by the entropy of mixing (Δ S) mix ) Enthalpy of mixing (Δ H) mix ) The atomic size difference (δ) and the Valence Electron Concentration (VEC) are used to determine the phase formation of the high-entropy alloy. These parameters are expressed as follows:
Figure BDA0003265031750000021
Figure BDA0003265031750000022
Figure BDA0003265031750000023
VEC＝∑c i VEC i
wherein c is i Is the mole fraction of the i element, H ij Is the enthalpy of mixing between the i and j elements, r i Is the atomic radius of the i element,
Figure BDA0003265031750000024
is the average size of the alloy system, VEC i Is the valence electron concentration of the i element, the lower the VEC, the better the plasticity of the alloy as a whole. This patent requires the formation of a unique structure with two nano-precipitated phases, thus requiring the alloy to be able to form a single-phase structure at high temperature, while being able to precipitate a second phase at moderate temperature, thus requiring the alloy to have a single-phase forming ability that is neither too good nor too poor. Thus, the parameters, delta, Δ H, associated with the ability of the alloy to form a single phase mix 、ΔS mix The following requirements should be met: delta is more than or equal to 4.5 and less than or equal to 5.7, delta H is more than or equal to-15 mix ≤-5kJ/mol，11.3≤ΔS mix ≤14.2J/K.mol，VCE≤4.8。
With Nb 38 Ti 33 Ta 12 Cr 5 Al 3 V 5 Si 2 Mo 2 For example, δ =5.1%, Δ H is calculated mix ＝7.46kJ/mol，ΔS mix =12.88J/k.mol, VEC =4.66, satisfactory.
A nanometer silicide and Laves phase reinforced refractory high-entropy alloy material comprises the following steps:
the method comprises the following steps: and cutting the as-cast high-entropy alloy into long strips with the length of l mm, the width of w mm and the thickness of h mm, and then rolling by using a cold rolling mill to obtain the alloy with the deformation of x. Wherein l is more than or equal to 5,w and more than or equal to 5,h and more than or equal to 5; x is more than or equal to 50 percent and less than or equal to 95 percent.
Step two: sealing the rolled high-entropy alloy by using a quartz tube filled with argon;
step three: the high-entropy alloy is heated for 10 to 50 hours at the temperature of 900 to 1100 ℃ and then cooled by water to obtain the high-strength high-toughness refractory high-entropy alloy with the nanoscale M5Si3 phase and the nanoscale Laves phase.
Advantageous effects
1. The invention relates to a nano-scale silicide and Laves phase reinforced refractory high-entropy alloy material which is mainly composed of eight elements such as Nb, ti, ta, cr, al, V, si, mo and the like, and a BCC phase matrix with a fine crystal structure, nano-scale M5Si3 silicide and Laves phases are obtained through cold rolling and subsequent heat treatment processes.
2. The density of the nano-scale silicide and Laves phase reinforced refractory high-entropy alloy material is less than or equal to 8g/cm 3 The high-strength oxidation-resistant composite material has excellent oxidation resistance at high temperature, simultaneously has good strong plasticity matching, the tensile yield strength can reach more than 850Mpa at room temperature, the tensile fracture elongation reaches more than 10 percent, and the weight gain per unit area is less than 2mg/cm after long-time oxidation at 650 DEG C 2 Is obviously superior to other most refractory high-entropy alloy systems.
Drawings
FIG. 1 is Nb after treatment 38 Ti 33 Ta 12 Cr 5 Al 3 V 5 Si 2 Mo 2 A back-scattered electron image of the alloy;
FIG. 2 is a processed Nb 38 Ti 33 Ta 12 Cr 5 Al 3 V 5 Si 2 Mo 2 The mechanical property curve of the alloy;
FIG. 3 is Nb 38 Ti 33 Ta 12 Cr 5 Al 3 V 5 Si 2 Mo 2 Oxidation kinetics after 50h oxidation in air at 650 ℃.
Detailed Description
The invention is further described with reference to the following figures and examples.
Example 1
The embodiment is a nano-scale silicide and Laves phase reinforced refractory high-entropy alloy, which comprises a BCC phase with a fine crystalline structure and a nano-scale M5Si3 phase and a Laves phase. The nano-scale silicide and Laves phase reinforced refractory high-entropy alloy consists of eight elements of Nb, ti, ta, cr, al, V, si, mo and the like, and the components of the alloy are Nb 38 Ti 33 Ta 12 Cr 5 Al 3 V 5 Si 2 Mo 2 In the as-cast condition, the alloy has a single-phase BCC structure.
The nano-scale silicide and Laves phase reinforced refractory high-entropy alloy comprises the following specific steps:
the method comprises the following steps: the as-cast high-entropy alloy was cut into a strip having a length of 30mm, a width of 10mm and a thickness of 10mm, and then rolled by a cold rolling mill to obtain a strain amount of 80%.
Step two: sealing the rolled high-entropy alloy by using a quartz tube filled with argon;
step three: the high-entropy alloy is heated for 20 hours at the temperature of 950 ℃ and then is cooled by water to obtain the high-strength high-toughness refractory high-entropy alloy with the nanometer M5Si3 phase and the Laves phase.
For Nb after rolling 38 Ti 33 Ta 12 Cr 5 Al 3 V 5 Si 2 Mo 2 The alloy was subjected to structural analysis by scanning electron microscopy as shown in FIG. 1. The results show that the alloy phase composition comprises a BCC phase, an M5Si3 phase and a Laves phase. Wherein the BCC phase is a fine crystalline structure, the M5Si3 phase and the Laves phase are dispersed and distributed on the BCC matrix, and the size of the matrix is about 300 nm. Enhancing Nb for the treated M5Si3 phase and the Laves phase 38 Ti 33 Ta 12 Cr 5 Al 3 V 5 Si 2 Mo 2 The alloy is subjected to room temperature tensile mechanical property test, and the tensile yield strength of the alloy is 870MPa, the tensile elongation at break of the alloy is about 11%, and the alloy shows excellent mechanical properties, as shown in figure 2. Meanwhile, the oxidation weight gain per unit area is 0.91mg/cm within 50h at 650 DEG C 2 As shown in FIG. 3, the materialThe appearance and the appearance are almost not changed, and the high-temperature oxidation resistance is shown.
Example 2
The embodiment is a nano-scale silicide and Laves phase reinforced refractory high-entropy alloy, which comprises a BCC phase with a fine crystalline structure and a nano-scale M5Si3 phase and a Laves phase. The nano-scale silicide and Laves phase reinforced refractory high-entropy alloy consists of eight elements of Nb, ti, ta, cr, al, V, si, mo and the like, and the components of the alloy are Nb 42 Ti 32 Ta 10 Cr 6 Al 2 V 4 Si 3 Mo 1 In the as-cast condition, the alloy has a single-phase BCC structure.
The nano-scale silicide and Laves phase reinforced refractory high-entropy alloy comprises the following specific steps:
the method comprises the following steps: the as-cast high-entropy alloy was cut into a strip having a length of 30mm, a width of 10mm and a thickness of 10mm, and then rolled by a cold rolling mill to obtain a strain amount of 85%.
Step two: sealing the rolled high-entropy alloy by using a quartz tube filled with argon;
step three: and (3) heating the high-entropy alloy at 950 ℃ for 10h at the same temperature, and then cooling with water to obtain the high-strength high-toughness refractory high-entropy alloy with the nanometer M5Si3 phase and the Laves phase.
For Nb after rolling 42 Ti 32 Ta 10 Cr 6 Al 2 V 4 Si 3 Mo 1 The alloy was subjected to structural analysis. The results show that the alloy phase composition comprises a BCC phase, an M5Si3 phase and a Laves phase. Wherein the BCC phase is a fine crystal structure, the M5Si3 phase and the Laves phase are dispersed and distributed on the BCC matrix, and the size of the matrix is about 250 nm. Strengthening Nb for the treated M5Si3 phase and the Laves phase 42 Ti 32 Ta 10 Cr 6 Al 2 V 4 Si 3 Mo 1 The alloy is subjected to room temperature tensile mechanical property test, and the tensile yield strength is about 900MPa, the tensile elongation at break is about 13%, and the alloy shows excellent mechanical property. Meanwhile, the oxidation weight gain per unit area is 1.2mg/cm within 50h at 650 DEG C 2 The appearance of the material is almost not changed, andshowing excellent high-temperature oxidation resistance.
Example 3
The embodiment is a nano-scale silicide and Laves phase reinforced refractory high-entropy alloy which comprises a BCC phase with a fine crystalline structure and a nano-scale M5Si3 phase and a Laves phase. The nano-scale silicide and Laves phase reinforced refractory high-entropy alloy consists of eight elements of Nb, ti, ta, cr, al, V, si, mo and the like, and the components of the alloy are Nb 39 Ti 30 Ta 15 Cr 4 Al 6 V 2 Si 4 Mo 2 In the as-cast condition, the alloy has a single-phase BCC structure.
The nanometer silicide and Laves phase reinforced refractory high-entropy alloy comprises the following specific steps:
the method comprises the following steps: the as-cast high-entropy alloy was cut into a strip having a length of 30mm, a width of 10mm and a thickness of 10mm, and then rolled by a cold rolling mill to obtain a strain amount of 80%.
Step two: sealing the rolled high-entropy alloy by using a quartz tube filled with argon;
step three: and (3) heating the high-entropy alloy at 950 ℃ for 20h at the same temperature, and then cooling with water to obtain the high-strength high-toughness refractory high-entropy alloy with the nanometer M5Si3 phase and the Laves phase.
For Nb after rolling 39 Ti 30 Ta 15 Cr 4 Al 6 V 2 Si 4 Mo 2 The alloy was subjected to structural analysis. The results show that the alloy phase composition comprises a BCC phase, an M5Si3 phase and a Laves phase. Wherein the BCC phase is a fine crystalline structure, the M5Si3 phase and the Laves phase are dispersed and distributed on the BCC matrix, and the size of the matrix is about 350 nm. Strengthening Nb for the treated M5Si3 phase and the Laves phase 39 Ti 30 Ta 15 Cr 4 Al 6 V 2 Si 4 Mo 2 The alloy is subjected to room temperature tensile mechanical property test, and the tensile yield strength is about 930MPa, the tensile elongation at break is about 12%, and the alloy shows excellent mechanical property. Meanwhile, the oxidation weight gain per unit area is 1.1mg/cm within 50h at 650 DEG C 2 The appearance of the material is almost unchanged, and the material shows excellent high-temperature oxidation resistance.
The foregoing is a description of the preferred embodiments of the present invention. It should be noted that the present invention is not limited to the above embodiments, and any modifications, equivalent replacements, or improvements that can be made to the present invention are included in the protection scope of the present invention when the scope of the claims, the summary of the invention, and the accompanying drawings are satisfied.

Claims (1)

1. A nanometer silicide and Laves phase reinforced refractory high-entropy alloy is characterized in that: the NbTiTaCrAlVSiMo alloy with the tensile fracture elongation at room temperature of more than 10 percent consists of eight elements of Nb, ti, ta, cr, al, V, si and Mo, and the atomic percent ranges of the elements are respectively as follows: nb is more than or equal to 30% and less than or equal to 50%, ti is more than or equal to 25% and less than or equal to 35%, ta is more than 0 and less than or equal to 20%, al and Cr are more than or equal to 5% and less than or equal to 15%, si is more than 0 and less than or equal to 5%, V and Mo are more than 0 and less than or equal to 10%; under the as-cast condition, the NbTiTaCrAlVSiMo alloy shows a single-phase BCC structure; after rolling and heat treatment, the alloy consists of a BCC phase with a fine grain structure, a nanoscale M5Si3 phase and a nanoscale Laves phase;
the method for preparing the nano-scale silicide and Laves phase reinforced refractory high-entropy alloy comprises the following steps:
the method comprises the following steps: cutting the as-cast high-entropy alloy into long strips with the length of l mm, the width of w mm and the thickness of h mm, and then rolling by using a cold rolling mill to obtain the deformation of x; wherein l is more than or equal to 5,w and more than or equal to 5,h and more than or equal to 5; x is more than or equal to 50% and less than or equal to 95%;
step two: sealing the rolled high-entropy alloy by using a quartz tube filled with argon;
step three: and (3) heating the high-entropy alloy at 900-1100 ℃ for 10-50h, and then cooling with water to obtain the high-strength high-toughness refractory high-entropy alloy with the nanoscale M5Si3 phase and the nanoscale Laves phase.
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