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CN109898005A - A kind of WVTaZrHf infusibility high-entropy alloy of high intensity and preparation method thereof - Google Patents

A kind of WVTaZrHf infusibility high-entropy alloy of high intensity and preparation method thereof Download PDF

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CN109898005A
CN109898005A CN201910347837.6A CN201910347837A CN109898005A CN 109898005 A CN109898005 A CN 109898005A CN 201910347837 A CN201910347837 A CN 201910347837A CN 109898005 A CN109898005 A CN 109898005A
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entropy alloy
particle size
wvtazrhf
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CN109898005B (en
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吴玉程
侯庆庆
罗来马
傅铭麒
谭晓月
昝祥
朱晓勇
刘东光
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Hefei University of Technology
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Abstract

The invention discloses WVTaZrHf infusibility high-entropy alloys of a kind of high intensity and preparation method thereof, wherein the constituent element of WVTaZrHf infusibility high-entropy alloy includes W, V, Ta, Zr, Hf, each component is constituted by atomic percent are as follows: W 22.5~23.5%, V 22.5~23.5%, Ta 22.5~23.5%, Zr 6-10%, Hf 22.5~23.5%.The present invention usually improves the structure of alloy by adding Zr, Hf member, prepares the infusibility high entropy alloy material with close-packed hexagonal structure by discharge plasma sintering, and then improve the hardness and strength of infusibility high-entropy alloy.

Description

A kind of WVTaZrHf infusibility high-entropy alloy of high intensity and preparation method thereof
Technical field
The present invention relates to a kind of infusibility high-entropy alloy and preparation method thereof, specifically a kind of WVTaZrHf of high intensity Infusibility high-entropy alloy and preparation method thereof.
Background technique
Due to being influenced by lanthanide contract, the atomic radius of hafnium is almost equal with zirconium, therefore the property extremely phase of hafnium and zirconium Seemingly.The crystal structure of hafnium and zirconium is all close-packed hexagonal structure.Hafnium has the stronger ability for absorbing neutron, and can slow down nucleon The rate of chain reaction inhibits " flame " of atomic reaction.Meanwhile with stronger high-temperature-resistant and anti-corrosion performance, and form Material has the characteristics such as the strong, easy processing of plasticity, therefore becomes one of the important materials of atomic energy industry, is now widely used for Manufacture the control rod and protective device of nuclear reactor.Zirconium have excellent corrosion resistance, high fusing point, superelevation hardness and The characteristics such as intensity are widely used in aerospace, military project, nuclear reaction, atomic energy field.Zirconium can be used as " the dimension of metallurgical industry Raw element ", plays its strong deoxidation, denitrogenates, the effect of desulfuration.
High-entropy alloy, the alloy of the alloy being made of a variety of essential elements, especially five yuan or more, and it is each main Element atomic percentage with higher, generally between 5% to 35%, therefore can without a kind of atomic percent of element More than 50%, and then become alloy with a kind of alloy material of element essential element.Research is found by high entropy effect It influences, and the possessed mixing of when entropy of mixing of the more high-entropy alloy of element number often is much higher than to form intermetallic compound Entropy, this effect can make intermetallic compound be difficult to occur, thus the formation for being easy to that there is the solid solution of simple structure, by a variety of The randomness of the alloy system of metallic element composition is very big, and the alloy system entropy of mixing is larger at this time, then system is more stable, to have Conducive to effective mixing between various elements so that each constituent element No- L aw Order and form simple crystalline phase, i.e. the generation center of area Cubic crystal, body centred cubic crystal or Patterns for Close-Packed Hexagonal Crystal inhibit the formation of intermetallic compound brittlement phase.
Summary of the invention
The present invention provides WVTaZrHf infusibility high-entropy alloy of a kind of high intensity and preparation method thereof, by addition Zr, Hf member usually improves the structure of alloy, and the infusibility high-entropy alloy with close-packed hexagonal structure is prepared by discharge plasma sintering Material, and then improve the hardness and strength of infusibility high-entropy alloy.
Discharge plasma sintering is with heating rate is fast, sintering time is short, even tissue, the natural shape for being able to maintain raw material The high feature of state, sintered body consistency is a kind of high-efficient, simple process preparation method.The present invention is using powder mixing machine Method obtains composite granule, then prepares the good WVTaZrHf of the comprehensive performances such as hardness, intensity by discharge plasma sintering Single-phase infusibility high entropy alloy material.
High-intensitive WVTaZrHf infusibility high-entropy alloy of the invention, constituent element include W, V, Ta, Zr, Hf, and each component is by original Sub- percentage is constituted are as follows: and W22.5~23.5%, V22.5~23.5%, Ta22.5~23.5%, Zr6-10%, Hf22.5~ 23.5%.
The preparation method of high-intensitive WVTaZrHf infusibility high-entropy alloy of the invention, includes the following steps:
Step 1: mixed powder
Five kinds of metal powders of W, V, Ta, Zr, Hf are measured according to the ratio and is placed in mechanical mixture in barrel mixer and obtains W-V-Ta- Zr-Hf composite powder;
In step 1, Particle Sizes are as follows: W Powder Particle Size is 2 μm, and V Powder Particle Size is 25 μm, and Ta Powder Particle Size is 25 μm, Zr powder Granularity is 28 μm, and Hf Powder Particle Size is 38 μm.(W fusing point: 3410 DEG C;V fusing point: 1890 DEG C, boiling point: 3000 DEG C;Ta fusing point: 2996 DEG C, boiling point: 5425 DEG C;Zr fusing point: 1852 DEG C, boiling point: 4377 DEG C, Hf fusing point: 2227 DEG C, boiling point: 4602 DEG C)
Step 2: sintering
W-V-Ta-Zr-Hf composite powder is packed into graphite jig, then mold is put into discharge plasma sintering furnace, it is right It is sintered stove evacuation, then 800 DEG C is warming up to 100 DEG C/min and keeps the temperature 10 minutes, control pressure is no more than 25MPa;Then with 100 DEG C/min is warming up to 1500 DEG C and keeps the temperature 5 minutes, and pressure is controlled in sintering and is no more than 50MPa, is down to room temperature after heat preservation, Room temperature is down to get W-V-Ta-Zr-Hf high entropy alloy material is arrived with 100 DEG C/min after heat preservation.
The beneficial effects of the present invention are embodied in:
The addition of Zr, Hf of the present invention improve the structure of alloy, are prepared by discharge plasma sintering with solid matter six The infusibility high entropy alloy material of square structure, significantly improves the hardness and strength of infusibility high-entropy alloy.The difficulty that the present invention prepares The close-packed hexagonal structure that molten high entropy alloy material tissue is, microscopic structure is uniform, and relative density is up to 99.9% or more, microhardness 576.3~600.2Hv of value is better than pure tungsten material (320~360Hv of microhardness).Compressive strength at room temperature 1207.6~ 1439.4MPa。
Detailed description of the invention
Fig. 1 shows the X-ray diffractogram of the single-phase infusibility high-entropy alloy of W-V-Ta-Zr-Hf of the preparation of the embodiment of the present invention 2 Spectrum, showing that the present invention prepares alloy structure is that close-packed hexagonal is single-phase.
Fig. 2 shows the scanning electron of the single-phase infusibility high-entropy alloy of W-V-Ta-Zr-Hf of the preparation of the embodiment of the present invention 2 is aobvious Micro mirror figure.
Fig. 3 shows the buckling resistant of the single-phase infusibility high-entropy alloy room temperature of W-V-Ta-Zr-Hf of the preparation of the embodiment of the present invention 2 Line.The intensity of material is significantly improved, and compression strength is 1439.4MPa, fracture elongation 8% at room temperature.
Specific embodiment
Technical solution of the present invention is described in further detail with specific embodiment with reference to the accompanying drawing.
Embodiment 1:
The single-phase infusibility high-entropy alloy of WVTaZrHf in the present embodiment, constituent element W, V, Ta, Zr, Hf, wherein each component is by original Sub- percentage is constituted are as follows: W22.5%, V22.5%, Ta22.5%, Zr10%, Hf22.5%.
Particle Sizes are as follows: W Powder Particle Size is 2 μm, and V Powder Particle Size is 25 μm, and Ta Powder Particle Size is 25 μm, and Zr Powder Particle Size is 28 μm, Hf Powder Particle Size is 38 μm.
The preparation method of the single-phase infusibility high-entropy alloy of WVTaZrHf, includes the following steps: in the present embodiment
Step 1: mixed powder
Five kinds of metal powders of W, V, Ta, Zr, Hf are measured according to the ratio and is placed in mechanical mixture in barrel mixer and obtains W-V-Ta- Zr-Hf composite powder;
Step 2: sintering
W-V-Ta-Zr-Hf composite powder is packed into graphite jig, then mold is put into discharge plasma sintering furnace, it is right It is sintered stove evacuation, then 800 DEG C is warming up to 100 DEG C/min and keeps the temperature 10 minutes, control pressure is no more than 25MPa;Then with 100 DEG C/min is warming up to 1500 DEG C and keeps the temperature 5 minutes, and pressure is controlled in sintering and is no more than 50MPa, is down to room temperature after heat preservation, Room temperature is down to get W-V-Ta-Zr-Hf high entropy alloy material is arrived with 100 DEG C/min after heat preservation.
The close-packed hexagonal structure that the crystal structure of high-entropy alloy is after sintering, tissue topography is more uniform, and relative density is reachable 99.1% or more of theoretical density, hardness and intensity with higher.Hardness mean value 581.2Hv is (micro- hard better than pure tungsten material Spend 320~360Hv), the intensity of material is significantly improved, and compression strength is 1207.6MPa at room temperature.
Embodiment 2:
The single-phase infusibility high-entropy alloy of WVTaZrHf in the present embodiment, constituent element W, V, Ta, Zr, Hf, wherein each component is by original Sub- percentage is constituted are as follows: W23%, V23%, Ta23%, Zr8%, Hf23%.
Particle Sizes are as follows: W Powder Particle Size is 2 μm, and V Powder Particle Size is 25 μm, and Ta Powder Particle Size is 25 μm, and Zr Powder Particle Size is 28 μm, Hf Powder Particle Size is 38 μm.
The preparation method of the single-phase infusibility high-entropy alloy of WVTaZrHf, includes the following steps: in the present embodiment
Step 1: mixed powder
Five kinds of metal powders of W, V, Ta, Zr, Hf are placed in mechanical mixture in barrel mixer according to a certain percentage and obtain W- V-Ta-Zr-Hf composite powder;
Step 2: sintering
W-V-Ta-Zr-Hf composite granule is packed into graphite jig, then mold is put into discharge plasma sintering furnace, it is right It is sintered stove evacuation, then 800 DEG C is warming up to 100 DEG C/min and keeps the temperature 10 minutes, control pressure is no more than 25MPa;Then with 100 DEG C/min is warming up to 1500 DEG C and keeps the temperature 5 minutes, and pressure is controlled in sintering and is no more than 50MPa, is down to room temperature after heat preservation, Room temperature is down to get W-V-Ta-Zr-Hf high entropy alloy material is arrived with 100 DEG C/min after heat preservation.
The close-packed hexagonal structure that the crystal structure of high-entropy alloy is after sintering, even tissue, without obvious stomata, relative density 99.9% or more of accessibility theory density has high hardness and intensity.Hardness mean value 600.2Hv, it is (micro- better than pure tungsten material 320~360Hv of hardness), the intensity of material is significantly improved, and compression strength is 1439.4MPa at room temperature, and fracture elongation is 8%.
Embodiment 3:
The single-phase infusibility high-entropy alloy of WVTaZrHf in the present embodiment, constituent element W, V, Ta, Zr, Hf, wherein each component is by original Sub- percentage is constituted are as follows: W23.5%, V23.5%, Ta23.5%, Zr6%, Hf23.5%.
Particle Sizes are as follows: W Powder Particle Size is 2 μm, and V Powder Particle Size is 25 μm, and Ta Powder Particle Size is 25 μm, and Zr Powder Particle Size is 28 μm, Hf Powder Particle Size is 38 μm.
The preparation method of the single-phase infusibility high-entropy alloy of WVTaZrHf, includes the following steps: in the present embodiment
Step 1: mixed powder
Five kinds of metal powders of W, V, Ta, Zr, Hf are placed in mechanical mixture in barrel mixer according to a certain percentage and obtain W- V-Ta-Zr-Hf composite powder;
Step 2: sintering
W-V-Ta-Zr-Hf composite granule is packed into graphite jig, then mold is put into discharge plasma sintering furnace, it is right It is sintered stove evacuation, then 800 DEG C is warming up to 100 DEG C/min and keeps the temperature 10 minutes, control pressure is no more than 25MPa;Then with 100 DEG C/min is warming up to 1500 DEG C and keeps the temperature 5 minutes, and pressure is controlled in sintering and is no more than 50MPa, is down to room temperature after heat preservation, Room temperature is down to get W-V-Ta-Zr-Hf high entropy alloy material is arrived with 100 DEG C/min after heat preservation.
The close-packed hexagonal structure that the crystal structure of high-entropy alloy is after sintering organizes relatively uniform, coarse grains, without obvious Stomata, 99.6% or more of relative density accessibility theory density, hardness and intensity with higher.Hardness mean value 576.3Hv, it is excellent In pure tungsten material (320~360Hv of microhardness), the intensity of material is significantly improved, and compression strength is at room temperature 1327.3MPa。

Claims (4)

1.一种高强度的WVTaZrHf难熔高熵合金,其特征在于:1. a high-strength WVTaZrHf refractory high-entropy alloy is characterized in that: 所述WVTaZrHf难熔高熵合金的组元包括W、V、Ta、Zr、Hf,各组分按原子百分比构成为:W22.5~23.5%,V 22.5~23.5%,Ta 22.5~23.5%,Zr 6-10%,Hf 22.5~23.5%。The components of the WVTaZrHf refractory high-entropy alloy include W, V, Ta, Zr, and Hf. Zr 6-10%, Hf 22.5-23.5%. 2.一种权利要求1所述的WVTaZrHf难熔高熵合金的制备方法,其特征在于包括如下步骤:2. a preparation method of WVTaZrHf refractory high-entropy alloy according to claim 1, is characterized in that comprising the steps: 步骤1:混粉Step 1: Mix the Powder 将W、V、Ta、Zr、Hf五种金属粉按配比量置于滚筒式混合机中机械混合得到W-V-Ta-Zr-Hf复合粉末;The five metal powders of W, V, Ta, Zr and Hf are placed in a drum mixer according to the proportion and mechanically mixed to obtain the W-V-Ta-Zr-Hf composite powder; 步骤2:烧结Step 2: Sintering 将W-V-Ta-Zr-Hf复合粉末装入石墨模具,再将模具放入放电等离子烧结炉中,对烧结炉抽真空,随后升温至800℃保温10分钟,控制压强不超过25MPa;随后升温至1500℃保温5分钟,烧结中控制压强不超过50MPa,保温结束后降至室温,即得到W-V-Ta-Zr-Hf高熵合金材料。Put the W-V-Ta-Zr-Hf composite powder into the graphite mold, then put the mold into the spark plasma sintering furnace, vacuum the sintering furnace, and then heat up to 800 ℃ for 10 minutes, and control the pressure not to exceed 25MPa; then heat up to Hold the temperature at 1500°C for 5 minutes, control the pressure during sintering not to exceed 50 MPa, and then drop to room temperature after the heat preservation to obtain the W-V-Ta-Zr-Hf high-entropy alloy material. 3.根据权利要求2所述的制备方法,其特征在于:3. preparation method according to claim 2, is characterized in that: 步骤1中,原始粉末粒度为:W粉粒度为2μm,V粉粒度为25μm,Ta粉粒度为25μm,Zr粉粒度为28μm,Hf粉粒度为38μm。In step 1, the original powder particle size is: W powder particle size is 2 μm, V powder particle size is 25 μm, Ta powder particle size is 25 μm, Zr powder particle size is 28 μm, and Hf powder particle size is 38 μm. 4.根据权利要求2所述的制备方法,其特征在于:4. preparation method according to claim 2, is characterized in that: 步骤2中,升温速率控制为100℃/min;保温结束后的降温速率为100℃/min。In step 2, the heating rate is controlled to be 100°C/min; the cooling rate after the heat preservation is completed is 100°C/min.
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CN110343932A (en) * 2019-08-28 2019-10-18 合肥工业大学 A kind of WVTaZrSc infusibility high-entropy alloy and preparation method thereof with high intensity
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CN113652595A (en) * 2021-08-23 2021-11-16 太原理工大学 A kind of high-strength and high-toughness TiZrHfNbTaWx refractory high-entropy alloy and preparation method thereof
CN114941099A (en) * 2022-05-26 2022-08-26 合肥工业大学 A kind of high-strength and high-hardness W-Ta-V-Zr system refractory high-entropy alloy and preparation method thereof

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110343932A (en) * 2019-08-28 2019-10-18 合肥工业大学 A kind of WVTaZrSc infusibility high-entropy alloy and preparation method thereof with high intensity
CN110538945A (en) * 2019-09-19 2019-12-06 中国人民解放军陆军装甲兵学院 Refractory high-entropy alloy stranded wire material, application and preparation method thereof
CN110538945B (en) * 2019-09-19 2021-04-13 中国人民解放军陆军装甲兵学院 Refractory high-entropy alloy stranded wire material, application and preparation method thereof
CN113652595A (en) * 2021-08-23 2021-11-16 太原理工大学 A kind of high-strength and high-toughness TiZrHfNbTaWx refractory high-entropy alloy and preparation method thereof
CN114941099A (en) * 2022-05-26 2022-08-26 合肥工业大学 A kind of high-strength and high-hardness W-Ta-V-Zr system refractory high-entropy alloy and preparation method thereof

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