Abstract
A new refractory high entropy alloy WMoNbTaV containing Al2O3 was prepared by spark plasma sintering. The effects of sintering temperature on densification behavior, phase structure, microstructure and wear resistance of the alloy were studied. The results show that when sintered at 1800‒1900 °C, the matrix of WMoNbTaV-Al2O3 has a single bcc phase structure, and the average grain size of Al2O3 is 1.15 μm. With the increase in sintering temperature, the grain size of the alloy increases, the density and microhardness also increase, and the hardness reaches 7967.4 MPa when the sintering temperature is 1900 °C. The alloy sintered at 1900 °C has excellent wear resistance, and the wear amount is only half of that of the alloy sintered at 1800 °C. The wear resistance of WMoNbTaV-Al2O3 high entropy alloy is much higher than that of pure W material. When the abrasive particle size is 37.5 μm, the wear mass loss of alloy sintered at 1900 °C is 0.9 mg, and the wear resistance of alloy is 83 times higher than that of pure W material.
Since the proposal of refractory high entropy alloys in 2010, numerous scholars have shown great interest in their properties, making them a significant focal point in the field of high entropy alloy research. Refractory high entropy alloys exhibit exceptional mechanical properties, wear resistance, corrosion resistance, physical properties and high temperature properties (including high temperature strength, high tempe-rature phase stability, high temperature oxidation resistance, etc
Due to the characteristics of fast heating rate, short sintering time, small sintered grains and uniform composition, spark plasma sintering has been increasingly utilized in the preparation of refractory high entropy alloy
The sintering process plays a crucial role in determining the properties of cemented carbide. Sintering temperatur
The addition of α-Al2O3 to the metal can greatly improve the mechanical properties of the material, both at room temperature and high temperature. These improvements in-clude increased tensile strength, yield strength and hardnes
In this work, a new type of high entropy alloy WMoNbTaV containing α-Al2O3 was prepared by spark plasma sintering using mixed metal powder as raw material. The effects of different sintering temperatures (1800, 1850, 1900 °C) on the microstructure, microhardness and wear properties of the WMoNbTaV-Al2O3 high entropy alloy were investigated, and the wear mechanism was discussed. The main objective of this research is to achieve a WMoNbTaV-Al2O3 high entropy alloy with favorable wear properties by controlling the temperature during spark plasma sintering. The experimental findings and theoretical insights provided in this study contribute to the advancement in high performance of high entropy alloy materials via powder metallurgy.
A new high entropy alloy of WMoNbTaV containing Al2O3 was designed. The powders of W, Mo, Nb, Ta, V with a purity of 99.99% and a particle size of approximately 10 μm and Al2O3 powders were selected as raw materials. The powders were mixed in an equal molar ratio of W, Mo, Nb, Ta, V, and 1wt% Al2O3. Tungsten carbide balls were used as the grinding medium, and ball milling was conducted at a speed of 150 r/min for 70 h. The resulting ball milling diagram of the mixed powder is shown in

Fig.1 Schematic diagrams of ball milling mixing (a) and spark plasma sintering (b) for WMoNbTaV-Al2O3 high entropy alloy
To pressurize the WMoNbTaV-Al2O3 high entropy alloy powder mixture, a spark plasma sintering furnace (20T-10) was employed, as depicted in
The crystal structure of the WMoNbTaV-Al2O3 high entropy alloy was analyzed by X-ray diffraction (XRD, Brux-D8). The microstructure and elemental composition of the WMoNbTaV- Al2O3 high entropy alloy were characterized by field emission scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The grain size and orientation of the WMoNbTaV-Al2O3 high entropy alloy were determined by electron backscattered diffraction (EBSD, Oxford C-nano). Square samples of the high entropy alloy measuring 2 mm×5 mm×8 mm were cut and then polished. After ultrasonic cleaning, an argon ion cross-section polishing machine (CP, JEOL IB-19530) was used for ion polishing. The polishing process lasted for 20 min with a voltage of 7.5 kV and a constant current of approximately 120 μA. Finally, EBSD samples were prepared.
The density of sintered samples of WMoNbTaV-Al2O3 high entropy alloy was measured by density measuring instrument (ME203/02). The polished sintered sample was tested by microhardness tester (HVS-1000) under a loading of 4.9 N and a residence time of 10 s. At least 10 different domains of each sample were randomly tested to obtain an average density value.
The wear performance of sintered WMoNbTaV-Al2O3 refractory high entropy alloy samples was evaluated using a wear testing machine (ML-100 model), as shown in

Fig.2 Schematic diagram of abrasive wear test

Fig.3 XRD patterns of WMoNbTaV-Al2O3 high entropy alloy at different sintering temperatures
SEM-EDS analysis of the WMoNbTaV-Al2O3 high entropy alloy microstructure was conducted at various sintering temperatures, as shown in

Fig.4 SEM-EDS results of WMoNbTaV-Al2O3 high entropy alloy at different sintering temperatures: (a) 1800 °C, (b) 1850 °C, and (c) 1900 °C
According to the EDS analysis, when the sintering temperature is 1800 °C, the elements of the high entropy alloy exhibit partial segregation. However, at sintering temperature of 1900 °C, the segregation of elements is greatly weakened, resulting in a more uniform distribution. This improvement is attributed to the higher sintering temperature, which provides sufficient energy for the complete diffusion between the atoms of each elemen

Fig.5 EBSD results of WMoNbTaV-Al2O3 high entropy alloy sintered at different temperatures (a, c, e) and corresponding grain size distributions (b, d, f): (a‒b) 1800 °C, (c‒d) 1850 °C, and (e‒f) 1900 °C
The density of the WMoNbTaV-Al2O3 high entropy alloy is determined by Archimedes drainage method. The relative density (ε) can be calculated by following formula:
(1) |
where ρ is the measured density and ρ0 is the theoretical density which is found to be 12.096 g/c
Sintering temperature/°C | Density/ g·c | Consistency /% | Microhardness, HV/MPa |
---|---|---|---|
1800 | 11.546 | 95.45 | 5478.2 |
1850 | 11.568 | 95.63 | 6095.6 |
1900 | 11.682 | 96.58 | 7967.4 |

Fig.6 Comparison of hardness of different refractory high entropy alloys

Fig.7 Wear test results of WMoNbTaV-Al2O3 high entropy alloy with different abrasive particle sizes and sintering temper- atures: (a) mass loss of abrasive wear and (b) relative wear resistance
Comparing Fig.
This study reveals a positive correlation between the wear resistance of WMoNbTaV-Al2O3 high entropy alloy and the sintering temperature, as well as negative correlation with the abrasive particle size. Specifically, an increase in abrasive particle size leads to an increase in abrasive wear mass loss and a decrease in the wear resistance of WMoNbTaV-Al2O3 high entropy alloy at a constant sintering temperature. Furthermore, under the same particle size, higher sintering temperatures result in smaller abrasive wear mass loss and improved wear resistance of WMoNbTaV-Al2O3 high entropy alloy, which is consistent with the trend observed in microhardness.
The wear morphology of pure W material is examined under different particle sizes, as shown in

Fig.8 Wear morphologies of pure W material with different abra-sive particle sizes: (a) 12.5 μm, (b) 18.75 μm, (c) 37.5 μm, and (d)100 μm

Fig.9 Wear morphologies of WMoNbTaV-Al2O3 high entropy alloy sintered at 1800 °C with different abrasive particle sizes: (a) 12.5 μm, (b) 18.75 μm, (c) 37.5 μm, and (d) 100 μm

Fig.10 Wear morphologies of WMoNbTaV-Al2O3 high entropy alloy sintered at 1850 °C with different abrasive particle sizes: (a) 12.5 μm, (b) 18.75 μm, (c) 37.5 μm, and (d) 100 μm
The results from

Fig.11 Wear morphologies of WMoNbTaV-Al2O3 high entropy alloy sintered at 1900 °C with different abrasive particle sizes: (a) 12.5 μm, (b) 18.75 μm, (c) 37.5 μm, and (d)100 μm
Comparing
(1) The hardness of WMoNbTaV-Al2O3 high entropy alloy is significantly higher than that of pure W material. According to the classic Archard law, higher hardness in alloy translates to better wear resistance.
(2) The presence of Al2O3 phase in WMoNbTaV-Al2O3 high entropy alloy contributes to improved wear resistance. The Al2O3 phase not only exhibits high hardness, but also possesses good toughness. Moreover, the Al2O3 phase is dispersed within the matrix, enabling the alloy to effectively resist abrasion scratches, and providing excellent softening resistanc
(3) The wear mechanism observed in WMoNbTaV-Al2O3 high entropy alloy is primarily abrasive wear, while the wear surface of pure W material exhibits slight plastic deformation alongside abrasive wear. This results in the formation of large-sized abrasive particles, intensifying the wear on the pure W surface. Therefore, it can be concluded that WMoNbTaV-Al2O3 high entropy alloy demonstrates exceptional wear resistance based on the wear morphology observed.
1) The spark plasma sintered WMoNbTaV-Al2O3 high entropy alloy matrix consists of a single bcc phase. As the sintering temperature increases, average grain size, density and microhardness of the alloy also increase. At a sintering temperature of 1900 °C, the alloy exhibits an average grain size of 8.95 μm, a density of 96.58%, and a microhardness of 7967.4 MPa.
2) When subjected to the same wear conditions, the WMoNbTaV-Al2O3 high entropy alloy demonstrates signifi-cantly higher wear resistance than pure W material. At an abrasive particle size of 37.5 μm, the alloy experiences a wear mass loss of 0.9 mg at 1900 °C, which is 83 times higher than that of pure W material. The wear mechanism of pure W material involves abrasive wear accompanied by slight
plastic deformation, whereas the wear mechanism of the WMoNbTaV-Al2O3 high entropy alloy is primarily abrasive wear.
3) The wear resistance of the WMoNbTaV-Al2O3 high entropy alloy exhibits a positive correlation with sintering temperature and a negative correlation with wear particle size. With increasing the sintering temperature, the hardness is improved and the abrasive wear mass loss decreases, resulting in improved wear resistance of the WMoNbTaV-Al2O3 high entropy alloy. The alloys sintered at 1800 and 1850 °C are suitable for fine abrasive wear conditions, while the alloy sintered at 1900 °C is appropriate for medium abrasive wear conditions.
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