CN110257684B - A preparation process of FeCrCoMnNi high-entropy alloy matrix composites - Google Patents
A preparation process of FeCrCoMnNi high-entropy alloy matrix composites Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 70
- 239000002131 composite material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000011159 matrix material Substances 0.000 title claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 23
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 16
- 238000011068 loading method Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 5
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- 239000010439 graphite Substances 0.000 claims description 95
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- 238000005516 engineering process Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 238000005728 strengthening Methods 0.000 abstract description 7
- 239000006185 dispersion Substances 0.000 abstract description 3
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
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- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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Abstract
本发明公开了一种FeCrCoMnNi高熵合金基复合材料的制备工艺，由FeCrCoMnNi粉末及纳米TiC粉末经放电等离子烧结工艺制备而成，原料配比按质量百分比构成为：FeCrCoMnNi 91‑97％，TiC 3‑9％。本发明在烧结温度1000℃，加载压力50MPa，保温时间5min，TiC添加量为7％时，放电等离子烧结的FeCrCoMnNi高熵合金基复合材料性能较优，硬度、室温屈服强度和600℃高温屈服强度分别为1092.4HV，979.7MPa，563.6MPa。TiC及反应形成的M23C6强化相均匀分布在FeCrCoMnNi高熵合金基体中，起到弥散强化的作用。
The invention discloses a preparation process of a FeCrCoMnNi high-entropy alloy-based composite material, which is prepared from FeCrCoMnNi powder and nano-TiC powder through a spark plasma sintering process. -9%. When the sintering temperature is 1000°C, the loading pressure is 50MPa, the holding time is 5min, and the TiC addition amount is 7%, the FeCrCoMnNi high-entropy alloy matrix composite material by spark plasma sintering has better performance, hardness, room temperature yield strength and 600°C high temperature yield strength. They are 1092.4HV, 979.7MPa and 563.6MPa respectively. TiC and the M 23 C 6 strengthening phase formed by the reaction are uniformly distributed in the FeCrCoMnNi high-entropy alloy matrix and play the role of dispersion strengthening.
Description
Technical Field
The invention relates to a preparation process of a FeCrCoMnNi high-entropy alloy-based composite material, belonging to the field of preparation of high-entropy alloy-based composite materials.
Background
The design of the multi-principal-element high-entropy alloy breaks through the design limitation of the traditional metal material, and the high-entropy alloy material with excellent performances such as high hardness, high strength, corrosion resistance and the like can be obtained through reasonable component design. Of all the high entropy alloy systems currently under investigation, the most commonly of interest to researchers are FeCrCoMnNi high entropy alloys with a stable single phase face centered cubic structure (FCC). The FeCrCoMnNi high-entropy alloy shows high plasticity under the conditions of room temperature and low temperature, has small change of mechanical property along with the temperature under the condition of high temperature, and has high-temperature stability. However, the FeCrCoMnNi high-entropy alloy has low hardness and strength, and how to improve the hardness and strength of the FeCrCoMnNi high-entropy alloy has important practical significance for the practical application of the high-entropy alloy under the condition of not reducing the plasticity or reducing the degree to a smaller degree.
In order to further improve the performance of the high-entropy alloy, a high-entropy alloy-based composite material is developed on the basis of the high-entropy alloy-based composite material, and the high-entropy alloy-based composite material integrates the performance of a reinforcing phaseThe alloy has the characteristics of high strength, high hardness, high-entropy alloy matrix, high temperature resistance and the like, and has high scientific research value and wide application prospect. The high-entropy alloy-based composite material prepared by powder metallurgy has certain prospect due to the characteristics of low cost, simple preparation process, easy realization of large-scale mass production and the like. Fine grain size and size reduction to the nano-scale (<100nm) to a large extent contribute to the strength of the material through the hallepatch relationship and grain boundary strengthening. Al (Al)2O3As a typical ceramic particle reinforcement, the composite material has high elastic modulus, high potential theoretical strength, excellent heat resistance and chemical stability, low density, wide source, good interface bonding with an aluminum matrix and no harmful interface reaction, and is considered to be a good reinforcement of an aluminum matrix composite material. But Al2O3Poor wettability with iron-based materials, Al is added in a general manner2O3The two phases are separated at the interface when combined with Fe, cracks are easily generated at the interface under the action of external load to cause fracture, and the two phases are not matched in high-temperature thermodynamics, so that the Fe-based composite material with excellent performance is difficult to prepare. SiC is used as a particle reinforcement for preparing the iron-based composite material due to the excellent properties of high strength, high modulus, wear resistance, heat resistance, high temperature resistance and the like. However, the Fe-based material and SiC particles undergo a severe chemical reaction at the interface to form a more brittle silicide. With Al2O3Compared with SiC ceramic particles, the TiC-Fe-based material has good wettability and does not generate interfacial chemical reaction at high temperature, and has inherent advantage in the aspect of preparing Fe-based composite materials with excellent performance because the TiC particles are commonly used as a reinforcing phase and widely applied to the preparation of the composite materials. The existing high-entropy alloy-based composite material is mainly prepared by adopting a fusion casting method, namely, a high-entropy alloy matrix is melted in advance, and reinforcing body particles are directly formed or directly added with fibers through in-situ reaction in a melt. The preparation of the high-entropy alloy-based composite material by using the high-entropy alloy powder as a raw material and adopting a spark plasma sintering method is rarely reported at present. The high-entropy alloy-based composite material prepared by adopting the mechanical alloying technology and the spark plasma sintering technology has the following main advantages: enhancementThe size of the body is small, and the distribution is dispersed; the nano-scale reinforcing phase is beneficial to improving the strength of the composite material; the powder system has high storage energy and is beneficial to reducing the densification temperature.
Disclosure of Invention
In order to avoid the defects in the prior art, the invention aims to provide a preparation process of a FeCrCoMnNi high-entropy alloy-based composite material.
The preparation process of the FeCrCoMnNi high-entropy alloy-based composite material comprises the following steps of:
step 1: preparation of the Mixed powder
Weighing FeCrCoMnNi powder and nano TiC powder according to the proportion, pouring the powder into a stainless steel ball milling tank, and adding hard alloy balls, wherein the ball-to-material ratio is 10: 1, vacuumizing a ball milling tank and then filling argon, ball milling at the rotation speed of 300-400rpm for 15-25h until the materials are completely and uniformly mixed, and obtaining sintered mixed powder;
step 2: assembly
Preparing a graphite mold, two matched graphite pressure heads, two graphite gaskets and graphite paper in advance; cutting the graphite paper into two circular graphite papers with the diameter the same as the inner diameter of the graphite mould and a rectangular graphite paper capable of covering the inner wall of the graphite mould; sticking rectangular graphite paper on the inner wall of a graphite mould, and assembling according to the sequence of a graphite pressure head/a graphite gasket/the graphite paper/mixed powder to be sintered/the graphite paper/the graphite gasket/the graphite pressure head;
and step 3: spark plasma sintering
And placing the assembled graphite mold into a discharge plasma sintering furnace, vacuumizing the sintering furnace to below 20Pa at room temperature, heating to the sintering temperature of 950-1100 ℃ and preserving the heat for 5-15min, wherein the loading pressure is 40-50MPa, cooling and unloading after the heat preservation is finished, and cooling along with the furnace to obtain the FeCrCoMnNi high-entropy alloy-based composite material.
In the step 1, the FeCrCoMnNi high-entropy alloy-based composite material is prepared from the following raw materials in percentage by mass: 91-97% of FeCrCoMnNi and 3-9% of TiC.
In step 1, the particle size of the FeCrCoMnNi powder is 20-50 μm, and the purity is more than or equal to 99%; the grain size of the TiC powder is 20-40nm, and the purity is more than or equal to 99%.
In step 3, the heating rate is 50 ℃/min; the loading rate was 50 MPa/min.
In step 3, the unloading mode is that the unloading speed is reduced to 0MPa at 50 MPa/min.
The FeCrCoMnNi high-entropy alloy-based composite material is prepared by using a discharge plasma sintering process (sintering temperature: 950-1100 ℃, heat preservation time: 5-15min, pressure: 40-50MPa), wherein the FeCrCoMnNi high-entropy alloy-based composite material with better performance is obtained when sintering temperature is 1000 ℃, heat preservation time is 5min, loading pressure is 50MPa, and 7 wt% of TiC is added, and the hardness, the room-temperature yield strength and the 600 ℃ high-temperature yield strength are 1092.4HV, 979.7MPa and 563.56MPa respectively, so that the FeCrCoMnNi high-entropy alloy-based composite material has better application value.
Compared with the prior art, the invention has the beneficial effects that:
1. the FeCrCoMnNi high-entropy alloy-based composite material has a simple structure, and takes an FCC phase matrix as a main component, TiC and M formed by reaction23C6The particles are uniformly distributed in the matrix to play a role in dispersion strengthening.
2. The alloy has the highest hardness of 1092.4HV, the room-temperature yield strength of 979.7MPa, the compressive strain rate of more than 10 percent, high strength, high plasticity and higher hardness, and has wide application prospect.
3. The yield strength of the FeCrCoMnNi high-entropy alloy-based composite material at the high temperature of 600 ℃ can reach 563.56MPa, which is far higher than that of a typical FeCrCoMnNi high-entropy alloy.
Drawings
Fig. 1 is an X-ray diffraction (XRD) spectrum of FeCrCoMnNi high entropy alloy and FeCrCoMnNi high entropy alloy based composite with different mass fractions of TiC added. FIG. 1 shows that after TiC is added, the phase structure of FeCrCoMnNi high-entropy alloy-based composite material consists of FCC, TiC and M23C6And (4) forming.
Fig. 2 is a Scanning Electron Microscope (SEM) photograph of FeCrCoMnNi high entropy alloy and FeCrCoMnNi high entropy alloy based composite with different mass fractions of TiC added. From FIG. 2, it can be seen that the FeCrCoMnNi high-entropy alloy-based composite material is mainly composed of FCC phase, M23C6And TiC strengthening phase is dispersed in the matrix.
Fig. 3 is the room temperature compressive stress strain curve of FeCrCoMnNi high entropy alloy and FeCrCoMnNi high entropy alloy based composite with different TiC content, and it can be seen from fig. 3 that the compressive plasticity of all materials is more than 9%.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1:
the process for preparing the FeCrCoMnNi high-entropy alloy-based composite material by spark plasma sintering in the embodiment comprises the following steps:
1. preparation of the Mixed powder
Weighing 3 wt% of nano TiC powder and 97 wt% of FeCrCoMnNi high-entropy alloy powder, pouring the two kinds of powder into a stainless steel ball-milling tank, and adding a hard alloy ball, wherein the ball-material ratio is 10: 1, vacuumizing a ball milling tank, filling argon, and ball milling for 20 hours until the materials are completely and uniformly mixed to obtain reaction sintering mixed powder;
2. assembly
Preparing a graphite die with the inner diameter of 20mm, two matched graphite pressure heads, two graphite gaskets and graphite paper in advance; cutting the graphite paper into two circular graphite papers with the diameter of 20mm and a rectangular graphite paper which just covers the inner wall of the graphite mould; sticking rectangular graphite paper on the inner wall of a graphite mould, and assembling according to the sequence of a graphite pressure head/a graphite gasket/the graphite paper/mixed powder to be sintered/the graphite paper/the graphite gasket/the graphite pressure head;
3. spark plasma sintering
And placing the assembled graphite mold into a discharge plasma sintering furnace, vacuumizing the sintering furnace to below 20Pa at room temperature, heating to 1000 ℃, keeping the temperature at 1000 ℃ for 5min at 50MPa, cooling along with the furnace, and reducing the unloading speed to 0MPa at 50 MPa/min.
The hardness, room-temperature yield strength and high-temperature yield strength at 600 ℃ obtained in this example were 881.2HV, 825.4MPa and 389.8MPa, respectively.
Experimental example 2:
the process for preparing the FeCrCoMnNi high-entropy alloy-based composite material by spark plasma sintering in the embodiment comprises the following steps:
1. preparation of the Mixed powder
Weighing 5 wt% of nano TiC powder and 95 wt% of FeCrCoMnNi high-entropy alloy powder, pouring the two kinds of powder into a stainless steel ball-milling tank, and adding a hard alloy ball, wherein the ball-material ratio is 10: 1, vacuumizing a ball milling tank, filling argon, and ball milling for 20 hours until the materials are completely and uniformly mixed to obtain reaction sintering mixed powder;
2. assembly
Preparing a graphite die with the inner diameter of 20mm, two matched graphite pressure heads, two graphite gaskets and graphite paper in advance; cutting the graphite paper into two circular graphite papers with the diameter of 20mm and a rectangular graphite paper which just covers the inner wall of the graphite mould; sticking rectangular graphite paper on the inner wall of a graphite mould, and assembling according to the sequence of a graphite pressure head/a graphite gasket/the graphite paper/mixed powder to be sintered/the graphite paper/the graphite gasket/the graphite pressure head;
3. spark plasma sintering
And placing the assembled graphite mold into a discharge plasma sintering furnace, vacuumizing the sintering furnace to below 20Pa at room temperature, heating to 1000 ℃, keeping the temperature at 1000 ℃ for 5min at 50MPa, cooling along with the furnace, and reducing the unloading speed to 0MPa at 50 MPa/min.
The hardness, room-temperature compressive yield strength and 600 ℃ high-temperature yield strength obtained in this example were 911.6HV, 912.6MPa and 488.4MPa, respectively.
Example 3:
the process for preparing the FeCrCoMnNi high-entropy alloy-based composite material by spark plasma sintering in the embodiment comprises the following steps:
1. preparation of the Mixed powder
Weighing 7 wt% of nano TiC powder and 93 wt% of FeCrCoMnNi high-entropy alloy powder, pouring the two powders into a stainless steel ball-milling tank, and adding a hard alloy ball, wherein the ball-material ratio is 10: 1, vacuumizing a ball milling tank, filling argon, and ball milling for 20 hours until the materials are completely and uniformly mixed to obtain reaction sintering mixed powder;
2. assembly
Preparing a graphite die with the inner diameter of 20mm, two matched graphite pressure heads, two graphite gaskets and graphite paper in advance; cutting the graphite paper into two circular graphite papers with the diameter of 20mm and a rectangular graphite paper which just covers the inner wall of the graphite mould; sticking rectangular graphite paper on the inner wall of a graphite mould, and assembling according to the sequence of a graphite pressure head/a graphite gasket/the graphite paper/mixed powder to be sintered/the graphite paper/the graphite gasket/the graphite pressure head;
3. spark plasma sintering
And placing the assembled graphite mold into a discharge plasma sintering furnace, vacuumizing the sintering furnace to below 20Pa at room temperature, heating to 1000 ℃, keeping the temperature at 1000 ℃ for 5min at 50MPa, cooling along with the furnace, and reducing the unloading speed to 0MPa at 50 MPa/min.
The hardness, room-temperature yield strength and high-temperature yield strength at 600 ℃ obtained in this example were 1092.4HV, 979.7MPa and 563.6MPa, respectively.
Example 4:
the process for preparing the FeCrCoMnNi high-entropy alloy-based composite material by spark plasma sintering in the embodiment comprises the following steps:
1. preparation of the Mixed powder
Weighing 9 wt% of nano TiC powder and 91 wt% of FeCrCoMnNi high-entropy alloy powder, pouring the two kinds of powder into a stainless steel ball-milling tank, and adding a hard alloy ball, wherein the ball-material ratio is 10: 1, vacuumizing a ball milling tank, filling argon, and ball milling for 20 hours until the materials are completely and uniformly mixed to obtain reaction sintering mixed powder;
2. assembly
Preparing a graphite die with the inner diameter of 20mm, two matched graphite pressure heads, two graphite gaskets and graphite paper in advance; cutting the graphite paper into two circular graphite papers with the diameter of 20mm and a rectangular graphite paper which just covers the inner wall of the graphite mould; sticking rectangular graphite paper on the inner wall of a graphite mould, and assembling according to the sequence of a graphite pressure head/a graphite gasket/the graphite paper/mixed powder to be sintered/the graphite paper/the graphite gasket/the graphite pressure head;
3. spark plasma sintering
And placing the assembled graphite mold into a discharge plasma sintering furnace, vacuumizing the sintering furnace to below 20Pa at room temperature, heating to 1000 ℃, keeping the temperature at 1000 ℃ for 5min at 50MPa, cooling along with the furnace, and reducing the unloading speed to 0MPa at 50 MPa/min.
The hardness, room-temperature yield strength and high-temperature yield strength at 600 ℃ obtained in this example were 902.9HV, 846.2MPa and 441.6MPa, respectively.
Table 1 shows the hardness and yield strength at 600 ℃ of FeCrCoMnNi high-entropy alloy-based composite materials of FeCrCoMnNi high-entropy alloy and TiC with different mass fractions, and the hardness and yield strength at high temperature of the materials show the trend of increasing and then decreasing along with the increase of the mass fraction of the TiC, and the FeCrCoMnNi high-entropy alloy-based composite materials have the best performance when 7 wt% of TiC is added.
TABLE 1
Example results summary:
the invention utilizes the discharge plasma sintering technology to prepare the FeCrCoMnNi high-entropy alloy-based composite material with good comprehensive mechanical property. The invention utilizes TiC and M formed by reaction23C6The strengthening phase is uniformly distributed in the high-entropy alloy FeCrCoMnNi matrix, so that the dispersion strengthening effect is achieved, and the comprehensive mechanical property of the material is improved. The FeCrCoMnNi high-entropy alloy-based composite material still has higher yield strength at high temperature. When 7 wt% of TiC powder and 93 wt% of FeCrCoMnNi high-entropy alloy powder are preferably added, the comprehensive mechanical property of the composite material is higher when the discharge plasma sintering temperature is 1000 ℃, the loading pressure is 50MPa, and the heat preservation time is 5 min. The invention can prepare FeCrCoMnNi high-entropy alloy-based composite material with excellent comprehensive mechanical properties.
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| JP7471078B2 (en) * | 2019-12-24 | 2024-04-19 | 山陽特殊製鋼株式会社 | A multi-component alloy with excellent resistance to softening, balance of strength and elongation, and excellent wear resistance. |
| CN111218603B (en) * | 2020-03-10 | 2022-03-29 | 中国科学院兰州化学物理研究所 | Preparation method of high-entropy alloy-based high-temperature solid lubricating composite material |
| CN112063894B (en) * | 2020-08-13 | 2022-02-01 | 中南大学 | Method for preparing precipitation-strengthened high-entropy alloy by spark plasma sintering |
| CN114411008A (en) * | 2020-10-28 | 2022-04-29 | 中国科学院理化技术研究所 | A kind of preparation method of high entropy alloy composite material |
| FR3121374A1 (en) * | 2021-03-31 | 2022-10-07 | Sintermat | Process for manufacturing metal parts and metal parts obtained based on SPS sintering |
| CN113816747A (en) * | 2021-08-27 | 2021-12-21 | 合肥工业大学 | TiC enhanced MAX phase high-entropy ceramic matrix composite material and preparation method thereof |
| CN113816746A (en) * | 2021-08-27 | 2021-12-21 | 合肥工业大学 | MAX-phase high-entropy ceramic matrix composite material and preparation method thereof |
| CN114807725B (en) * | 2022-05-31 | 2023-04-07 | 中国矿业大学 | High-entropy alloy-based nano superhard composite material enhanced by inlaid particles and preparation method thereof |
| CN115747610B (en) * | 2022-11-18 | 2024-08-02 | 陕西理工大学 | SiC-doped high-entropy alloy and preparation method and application thereof |
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