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Article

Microstructure and Wear Resistance of FeCuNiTiAl High-Entropy Alloy Coating on Ti6Al4V Substrate Fabricated by Laser Metal Deposition

by
Dongqi Zhang
,
Dong Du
,
Guan Liu
,
Ze Pu
,
Shuai Xue
and
Baohua Chang
*
State Key Laboratory of Tribology, Department of Mechanical Engineering, Tsinghua University, Beijing 100084, China
*
Author to whom correspondence should be addressed.
Lubricants 2022, 10(10), 263; https://doi.org/10.3390/lubricants10100263
Submission received: 26 September 2022 / Revised: 14 October 2022 / Accepted: 17 October 2022 / Published: 18 October 2022
(This article belongs to the Special Issue Assessment of Abrasive Wear)
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Versions Notes

Abstract

:
In order to improve the hardness and wear resistance of titanium alloys, an equimolar ratio high-entropy alloy (HEA) FeCuNiTiAl coating was fabricated on the surface of titanium alloy Ti6Al4V by means of laser metal deposition for the first time. The microstructure and composition of the HEA coating and the transition zone were observed by scanning electron microscopy (SEM) and energy dispersive spectrometer (EDS). The results show that HEA coating and Ti6Al4V have suitable metallurgical bonding, and no defects, such as cracks, are found at the interface. The hardness of the HEA coating is between 450 and 500 HV0.5, which is about 1.5 times that of the Ti6Al4V substrate. Wear tests show that the wear rate of HEA coating is 0.89 × 10−5 mm3/(N·m), while that of Ti6Al4V reaches 53.97 × 10−5 mm3/(N·m), and the wear resistance of substrate is increased 60 times by the HEA coating. The wear mechanism of the Ti6Al4V substrate is mainly abrasive wear, and the wear mechanism of FeCuNiTiAl HEA coating is mainly adhesive wear, accompanied by slight oxidation wear and abrasive wear.

1. Introduction

Titanium and its alloys are often used in aerospace [1,2], automotive [3,4], medical apparatus [5,6], and other fields due to their suitable mechanical strength, biocompatibility, and corrosion resistance. Among them, Ti6Al4V alloy is the most widely used. However, the poor tribological properties of titanium alloys severely limit their application in severe wear and friction conditions [7]. Therefore, the surface of titanium alloy needs to be treated to improve its wear resistance. In recent years, many surface modification techniques, such as plasma spraying [8,9], physical vapor deposition (PVD) [10], chemical vapor deposition (CVD) [11], ion implantation [12], nitriding [13] and laser cladding (also known as laser metal deposition, (LMD)) [14,15] have been used to solve this problem. Among them, LMD can deposit thick and dense protective coatings having strong metallurgical bonding with substrates and rapid preparation efficiency. Therefore, LMD has attracted wide attention in recent years [14,15,16,17].
High-entropy alloys (HEAs) were first proposed in 2004 and have received extensive attention and research in the past decade [18,19,20]. Unlike traditional alloys with only one or two main elements, HEAs usually contains five or more main elements in equal or near-equal molar percentages [21,22,23]. HEAs have unique properties, including a high-entropy effect, hysteresis diffusion effect, lattice distortion, and cocktail effect [24]. HEAs generally have a variety of ideal properties, such as low-temperature ductility and toughness, high hardness and strength, excellent corrosion resistance, and wear resistance [25,26,27,28]. It has great potential applications in aerospace, transportation, energy, electronics, biomedical, molds, and tools sectors [29]. In view of the suitable wear resistance of HEAs, they are often used as wear-resistant coating materials. The TiAlNiSiV HEA coating with a near-equal molar ratio was fabricated on Ti6Al4V alloy by Zhang et al. [30]. Compared with the Ti6Al4V substrate, the hardness and wear resistance of the TiAlNiSiV HEA coating were greatly improved. They found that the wear resistance of the TiAlNiSiV HEA coating is 5 times that of the Ti6Al4V substrate. The content of a certain element can affect the microstructure and wear resistance of HEAs. Xiang et al. [31] studied the CoCrFeNiNbx HEA coatings prepared on pure titanium sheets by pulsed laser cladding. After adding 1 at. % Nb, Cr2Nb Laves phase with C15-type cubic structure appeared in the interdendritic region, in addition to the BCC solid-solution phase and the Cr2Ti Laves phase. The hardness also increased by 218 HV. Zhao et al. [32] investigated the AlNbTaZrx HEA coatings prepared on Ti6Al4V substrate by laser cladding. The results showed that when the x increased from 0.2 to 1.0, the average microhardness of the HEA coatings increased by about 17%. The wear mechanism and the high-temperature oxidation resistance changed with the content of the Zr element.
The performance of HEAs is closely related to the composition and content of elements, and most studies are based on the analysis of HEAs with equimolar ratios. To our knowledge, the FeCuNiTiAl HEA powders have not previously been used in laser metal deposition. In this paper, the FeCuNiTiAl HEA coating was fabricated on a Ti6Al4V substrate by LMD technology for the first time. The interface metallurgy between the HEA coating and the substrate was analyzed, and the microstructure, hardness, and wear resistance of the HEA coating were studied.

2. Experimental

2.1. Material and LMD Process

The pre-alloyed FeCuNiTiAl HEA powders (Beijing Gaoke New Material Technology Co., Ltd., Beijing, China) used in this work were prepared by gas atomization. The size (diameter) of the FeCuNiTiAl HEA powders is 50–150 μm, and the average powder size (d50) is 73.39 μm. The scanning electron microscope (SEM) (Zeiss, Oberkochen, Germany) image of the powders is shown in Figure 1. The elemental composition of the HEA powders is shown in Table 1. Before the experiment, the Ti6Al4V substrate was polished with 400#, 800#, and 1200# silicon carbide sandpapers and then cleaned with acetone three times to remove the oxides and contaminants on the surface of the Ti6Al4V substrate. The powders were dried in a vacuum drying furnace at 120 °C for 2 h before use.
A self-built LMD system was used in the experiment, which was equipped with a 4000 W continuous fiber laser and a coaxial powder feed cladding head with a four-stream nozzle. A 6-dof robot was used to move the laser processing head according to the set deposition paths. The schematic of the experiment is shown in Figure 2. To avoid damage to optical fiber caused by laser reflection, the vertical direction of the laser beam was tilted by 5°.
To obtain the optimal process parameters in the LMD experiment, the process parameters have been studied with the laser power ranging from 400 to 800 W and the scanning speed ranging from 10 to 20 mm/s. With the optimized parameters, a uniform coating can be obtained, and the metallurgical bonding of the coating/substrate interface is suitable. All of the experimental parameters of the LMD experiment are listed in Table 2.

2.2. Materials Characterization

The samples for cross-section analysis were prepared by wire cutting and polished first with 400#–2000# sandpapers and then with the 1–2 μm diamond polishing compounds. The cross sections were etched with the solution (HF:HNO3:H2O = 1:1:7) for 20 s and then rinsed with alcohol. The microstructure and morphology of the coating were observed by SEM. The element distributions were analyzed by the energy dispersive spectrometer (EDS). The porosity of the HEA coating was calculated by Image-Pro Plus software (Media Cybernetics, Rockville, MD, USA) according to the SEM image of the cross-section.

2.3. Microhardness and Wear Tests

The microhardness test was carried out using a Vickers hardness tester (FM-800, FUTURE-TECH Corporation, Tokyo, Japan), and the test parameters were set as the load of 500 g and the duration time of 10 s. After the LMD experiment, the specimens for wear test were cut from the Ti6Al4V substrate and the laser deposition samples using wire cutting. The wear surface size of the specimens is 15 mm × 6 mm. Due to the wear test must be carried out on a flat surface, the HEA coating was sanded with sandpapers in advance to obtain a smooth HEA surface. The surface of the Ti6Al4V substrate also needs to be polished smooth with 1200# sandpapers.
The wear tests were performed using a ball-to-block device (UMT5, Bruker, Billerica, MA, USA) at a humidity of 62% and an ambient temperature of 24.7 °C. The friction ball is a Si3N4 ceramic ball with a diameter of 4 mm. The wear test adopts the linear reciprocating mode, the linear distance is 5 mm, and the total sliding time is 30 min. The normal constant load is 5 N, and the frequency is 5 Hz.
The three-dimensional white light interference surface topography instrument (Zygo Corporation, Middlefield, CT, USA) was used to measure the wear profiles and wear volumes. The wear rate (δ) is often used to characterize the wear resistance of the material, and the calculation formula of the wear rate is as follows [33]:
δ = V l o s s F   ·   L
where Vloss is the total wear volume, F is the normal constant load, and L is the total reciprocating distance.

3. Results and Discussion

3.1. Microstructure

The cross-sectional morphology of the single-track laser deposition HEA coating shown in Figure 3a,b is the local enlargement of the microstructure of area B in Figure 3a. It can be observed that the HEA deposition layer has a maximum thickness of about 800 μm. A few pores of different sizes exist in the HEA coating, which is related to the fact that the laser metal deposition is carried out in the air, resulting in a 0.2% porosity content of the HEA coating. Figure 3c is the magnified observation of the transition area C between the coating and the substrate in Figure 3b. It can be observed that the bottom is a columnar crystal region grown from the substrate, indicating that the HEA coating and the Ti6Al4V substrate form a suitable metallurgical bond, and no cracks are found. Figure 3d is an enlarged view of the middle area D of the HEA coating in Figure 3b. It is found that this part of the coating is composed of equiaxed crystals. Both dendrite region (DR) (dark phase) and interdendritic region (IR) (white phase) are visible [31,34]. X-ray diffraction is often used to analyze phase formation [35], and we will further analyze the composition of DR and IR in the future.
Figure 4 is the EDS mapping results of Figure 3c. Due to the difference in the composition and content of elements between the coating and the substrate, a transition zone is formed at the interface between the HEA coating and the substrate, and the columnar crystal structure is rich in Ti. This is because the Ti element in the Ti6Al4V substrate enters into the molten HEA and metallurgical bonding occurs at the interface, resulting in the content of the Ti element at the interface being much higher than that of the HEA coating. Figure 5 is the EDS mapping results of Figure 3d. It can be found that Cu and Fe elements are mainly concentrated in the IR, and Ti, Al, Ni, V, and other elements are enriched in the DR.
Figure 6 shows the EDS line scanning results along the thickness direction, and the elemental changes from the substrate to the HEA coating can be seen. The change of Ti and Al elements in the transition zone is very obvious. The high content of the Ti element is due to the fusion of Ti6Al4V into the HEA coating, while the Al element comes from the diffusion of the HEA coating to the Ti6Al4V substrate side. What is more, the distribution of Cu elements in the HEA coating fluctuates greatly in Figure 6. This is because the Cu element is mainly distributed in the IR, as shown in Figure 5.

3.2. Microhardness

The microhardness result of the sample in the thickness direction is shown in Figure 7. The hardness of the HEA coating is significantly higher than that of the Ti6Al4V substrate, which is about 1.5 times that of the substrate. The hardness of the HEA coating with a thickness of 0–600 μm is about 450–500 HV0.5, and the hardness of the transition zone is the highest, reaching 650 HV0.5. The hardness of the heat-affected zone (HAZ) is around 350 HV0.5, slightly higher than that of the substrate. The hardness of the Ti6Al4V substrate is the lowest, all below 300 HV0.5.
As shown in Figure 6, there is an obvious transition zone of about 100 μm thickness between the coating layer and the substrate, which has an elongated columnar crystal structure, as shown in Figure 3c. This transition zone is rich in Ti element from the substrate, which may form some brittle phase, resulting in different coating hardness. This phenomenon has also been observed in some studies [36,37]. The increase in the hardness in HAZ is mainly due to the strengthening effect of α’ martensite that formed during fast cooling of the LMD process. The closer the HAZ is to the substrate/coating interface, the greater the thermal gradient and the higher the content of α’ martensite and the corresponding hardness [38,39,40].

3.3. Wear Resistance

The difference in hardness between HEA coating and Ti6Al4V substrate means the difference in wear resistance. Figure 8 shows the three-dimensional surface profiles of the wear tracks of the Ti6Al4V substrate and HEA coating. Figure 9 exhibits the surface profiles of the two samples, and it can be clearly seen that the wear resistance of the two materials is very different. The wear track width of the Ti6Al4V substrate is about 1100 μm, and the maximum depth is about 70 μm, while the wear track width of HEA coating is about 450 μm, and the maximum depth is about 5 μm.
The wear rate results calculated according to Equation (1) are shown in Figure 10. The wear rate of HEA coating is very low, and its value is 0.89 × 10−5 mm3/(N·m). The wear rate of the Ti6Al4V substrate is 60 times that of HEA coating, reaching 53.97 × 10−5 mm3/(N·m). It implies that the FeCuNiTiAl HEA exhibits excellent wear resistance. The wear rates of different HEAs coatings are compared, as shown in Table 3, and find that the wear resistance of the FeCuNiTiAl HEA is above the middle level.
Figure 11a,b presented the worn surface morphologies of the Ti6Al4V substrate and FeCuNiTiAl HEA coating after the wear tests. It can be seen that due to the low hardness of the Ti6Al4V substrate, there are obvious wide and deep parallel grooves in the sliding direction on the surface, which are the typical abrasive wear mechanism [37]. In addition, a large amount of debris can be found on the friction surface, and the EDS mapping scanning results show that the debris contained a large amount of Si and O elements. This is because in the process of wear, the long-term reciprocating friction of the Si3N4 ceramic ball will shed a small number of wear debris, and the O element indicates that a small amount of oxides are formed during the friction process. Therefore, the wear mechanism of the Ti6Al4V substrate is mainly abrasive wear [30,32].
The wear morphology of the HEA coating is shown in Figure 11b. Due to the high hardness of HEA, the wear surface is relatively smooth. Spalling pits are formed by the shedding of metal particles along the sliding direction, and some oxides (darker regions) can also be found. The EDS mapping results show that the spalling pits contain a large number of O elements and a small amount of Si elements. This is probably because the constituent elements such as Ti, Al, Fe, and Cu in the HEA coating generate a large amount of oxides under the condition of frictional heat. When the Si3N4 ceramic ball leaves, a tear pit is formed due to adhesion. Therefore, the wear mechanism of HEA coating is mainly adhesive wear, accompanied by oxidative wear and abrasive wear [45,46].

4. Conclusions

FeCuNiTiAl HEA coating was fabricated on the surface of the Ti6Al4V substrate by laser metal deposition technology. The microstructure and mechanical properties were studied, and the wear resistance was analyzed. The conclusions are as follows:
  • FeCuNiTiAl HEA coating and Ti6Al4V substrate have suitable metallurgical bonding. No cracks, pores, or other defects are found at the interface;
  • FeCuNiTiAl HEA can be used as the wear-resistant coating material of Ti6Al4V, greatly improving the wear resistance of Ti6Al4V. The hardness of HEA coating is 1.5 times that of Ti6Al4V substrate, and its wear resistance is 60 times that of Ti6Al4V;
  • The wear mechanism of the Ti6Al4V substrate is mainly abrasive wear, and the wear mechanism of FeCuNiTiAl HEA coating is mainly adhesive wear, accompanied by slight oxidation wear and abrasive wear.

Author Contributions

Conceptualization, D.Z., G.L. and B.C.; Data curation, D.Z., G.L. and S.X.; Formal analysis, D.Z. and S.X.; Funding acquisition, B.C.; Investigation, D.Z., G.L. and Z.P.; Resources, D.Z., Z.P. and S.X.; Software, D.Z. and Z.P.; Supervision, D.D. and B.C.; Validation, D.Z.; Writing—original draft, D.Z. and B.C.; Writing—review and editing, D.Z., D.D. and B.C. All authors have read and agreed to the published version of the manuscript.

Funding

The authors appreciate the financial support of this work from the Tribology Science Fund of the State Key Laboratory of Tribology (SKLT2022C20).

Data Availability Statement

Not applicable.

Conflicts of Interest

The authors declare no conflict of interest.

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Figure 1. SEM image of the FeCuNiTiAl HEA powders.
Figure 1. SEM image of the FeCuNiTiAl HEA powders.
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Figure 2. Schematic of the LMD experiment.
Figure 2. Schematic of the LMD experiment.
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Figure 3. The microstructures of the HEA coating: (a) overall view; (b) magnified observation of area B in (a); (c) magnified observation of area C in (b), and (d) magnified observation of area D in (b).
Figure 3. The microstructures of the HEA coating: (a) overall view; (b) magnified observation of area B in (a); (c) magnified observation of area C in (b), and (d) magnified observation of area D in (b).
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Figure 4. Element distributions of Figure 3c.
Figure 4. Element distributions of Figure 3c.
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Figure 5. Element distributions of Figure 3d.
Figure 5. Element distributions of Figure 3d.
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Figure 6. EDS line scanning results.
Figure 6. EDS line scanning results.
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Figure 7. Microhardness distribution along the thickness of the specimen.
Figure 7. Microhardness distribution along the thickness of the specimen.
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Figure 8. Three-dimensional surface profiles after wear tests: (a) Ti6Al4V substrate and (b) HEA coating.
Figure 8. Three-dimensional surface profiles after wear tests: (a) Ti6Al4V substrate and (b) HEA coating.
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Figure 9. Typical cross-sectional profiles of the wear tracks.
Figure 9. Typical cross-sectional profiles of the wear tracks.
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Figure 10. The wear rate of Ti6Al4V substrate and HEA coating.
Figure 10. The wear rate of Ti6Al4V substrate and HEA coating.
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Figure 11. SEM morphologies and corresponding oxygen and silicon elemental EDS mappings of wear tracks after dry sliding wear: (a) substrate and (b) HEA coating.
Figure 11. SEM morphologies and corresponding oxygen and silicon elemental EDS mappings of wear tracks after dry sliding wear: (a) substrate and (b) HEA coating.
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Table
Table 1. The elemental composition of the HEA powders.
Table 1. The elemental composition of the HEA powders.
ElementsFeCuNiTiAlElse
wt.%22.0825.1223.2118.9310.4350.225
Table
Table 2. Experimental parameters of the LMD experiment.
Table 2. Experimental parameters of the LMD experiment.
Laser power (W)400
Laser spot diameter (mm)3
Scanning speed (mm/s)12.5
Powder feed rate (g/min)6.5
Carrier gas flow rate (L/min)10
Table
Table 3. The wear rates of different HEAs coatings.
Table 3. The wear rates of different HEAs coatings.
MaterialsFriction PairWear Rate/mm3/(N·m)References
AlCoCrFe2.5NiSi3N41.09 × 10−3[41]
AlCoCrFeNiZrO25.18 × 10−4[42]
CrFeCoNiCuGCr152.26 × 10−4[43]
AlNbTaZr0.8Si3N41.16 × 10−4[32]
TiVCrAlSiGCr152.52 × 10−5[25]
FeCuNiTiAlSi3N48.90 × 10−6Our work
Fe25Co25Ni25(B0.7Si0.3)25GCr153.64 × 10−6[44]
Al1.5CrFeCoNiCuGCr156.64 × 10−7[43]
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Zhang, D.; Du, D.; Liu, G.; Pu, Z.; Xue, S.; Chang, B. Microstructure and Wear Resistance of FeCuNiTiAl High-Entropy Alloy Coating on Ti6Al4V Substrate Fabricated by Laser Metal Deposition. Lubricants 2022, 10, 263. https://doi.org/10.3390/lubricants10100263

AMA Style

Zhang D, Du D, Liu G, Pu Z, Xue S, Chang B. Microstructure and Wear Resistance of FeCuNiTiAl High-Entropy Alloy Coating on Ti6Al4V Substrate Fabricated by Laser Metal Deposition. Lubricants. 2022; 10(10):263. https://doi.org/10.3390/lubricants10100263

Chicago/Turabian Style

Zhang, Dongqi, Dong Du, Guan Liu, Ze Pu, Shuai Xue, and Baohua Chang. 2022. "Microstructure and Wear Resistance of FeCuNiTiAl High-Entropy Alloy Coating on Ti6Al4V Substrate Fabricated by Laser Metal Deposition" Lubricants 10, no. 10: 263. https://doi.org/10.3390/lubricants10100263

APA Style

Zhang, D., Du, D., Liu, G., Pu, Z., Xue, S., & Chang, B. (2022). Microstructure and Wear Resistance of FeCuNiTiAl High-Entropy Alloy Coating on Ti6Al4V Substrate Fabricated by Laser Metal Deposition. Lubricants, 10(10), 263. https://doi.org/10.3390/lubricants10100263

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