Preparation of Ceramic Phase-Reinforced High-Entropic Alloy Composite Coatings: History
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Contributor:
Haoran Zhang
,
Yaowei Yong
,
Fuwei Wang
,
Yuan Liang
,
Lin Liu
,
Hong Liu
,
Yang Gao

The production of ceramic phase-reinforced high-entropy alloy composite coatings with excellent mechanical properties, high-temperature oxidation resistance, and corrosion resistance via laser cladding is a new hotspot in the field of surface engineering. However, as high-entropy alloys have a wide range of constituent systems and different kinds of ceramic particles are introduced in different ways that give the coatings unique microscopic organization, structure, and synthesized performance, it is necessary to review the methods of preparing ceramic phase-reinforced high-entropy alloys composite coatings via laser cladding.

  • laser cladding
  • surface modification
  • ceramic reinforcement
  • protective coatings

1. In Situ Generation Method

The in situ generation method refers to the in situ generation of the ceramic phase during the preparation of composite coatings and is based on the reaction between the raw materials or between the raw materials and the surrounding gases in the plasma. It is based on the original method of the in situ generation of metal/ceramic composite coatings, high-entropic alloy as a metal base, in situ generation of ceramic phase to improve the mechanics of high-entropic alloy composite coatings, and other comprehensive achievements. Preparing in situ-generated ceramic phase high-entropy alloy-based composite coatings using laser cladding is an effective method to solve the problem of poor interfacial bonding between ceramic particles and the metal matrix [1]. This method prepares the composite coatings with a simple process and a high deposition rate, and the matrix and composite ceramic phase possess good bonding properties and wettability. The ceramic particles generated in situ by the chemical reaction are disposed uniformly in the metal matrix, which reduces the influence between the interfaces and improves the overall performance and service life of the coating. Some researchers, including Feng et al. [2], Yang et al. [3], and Lin et al. [4], used the in situ generation of ceramic particles such as borides and carbides to significantly elevate the properties of entropy alloy coatings in terms of hardness, wear resistance, and corrosion resistance.
Guo et al. [5] successfully fabricated in situ-generated TiC ceramic-reinforced CoCrCuFeNiSi0.2 coatings on 304 stainless steel via laser cladding. The experimental results show that with the increase of Ti and C, the composite coating CoCrCuFeNiSi0.2 (Ti, C)x change from a single FCC solid-solution structure to an FCC Solid-solution structure. With the addition of Ti and C, the in situ TiC ceramics are mainly distributed at the grain boundaries. It can be observed that the coating has a typical dendritic structure at (Ti, C)0, and as the (Ti, C)x content increases, white particles gradually appear in the grain boundaries, and the size of the white particles gradually increases. The white particles are in situ-generated TiC particles. The in situ-generated TiC particles perform solid-solution strengthening and diffusion strengthening on the high-entropy coating, which significantly increases the hardness and wear resistance of the coating. With a maximum hardness of 517.2 HV0.2
and an average microhardness of 498.5 HV0.2, the (Ti, C)1.0 coating has the highest hardness, nearly 2 points higher than the HEA coatings without Ti and C. The hardness of the (Ti, C)1.5 coating is lower than that of the (Ti, C)1.0 coating, but as the content of Ti and C increases, the size of the TiC particles generated in situ in the coating increases as well, weakening the reinforcing effect. (Ti, C)1.0 has the best wear performance; the gradual increase in TiC ceramic produced in situ lowers the coefficient of friction of the CoCrCuFeNiSi0.2HEA coatings and significantly improves the coating’s resistance to abrasion. During the wear process, (Ti, C)1.5 large ceramic particles exert a plowing effect on the coating, making wear grooves on the surface more noticeable.
The performance of high-entropic alloy composite coatings is strongly influenced by the size of in situ-generated ceramic particles. Liu et al. [6] produced AlCoCrFeNiTix reinforced with TiC particles in situ that were authigenic using laser cladding on the surface of AISI 1045 steel. In contrast to that, Guo et al. [7] used the laser thinning effect to extract the high-entropic Fe and C elements in the coatings from the AISI 1045 steel matrix. Two BCC phases, Fe-Cr and Al-Ni, along with a trace amount of in situ TiC phase in the form of micro- and nanoparticle-sized particles, made up the coatings. The composite coatings of CoCrCuFeNiTi1.0 HEA with the highest average microhardness (860.1 HV0.3) exhibited a direct correlation with the increased volume fraction of the TiC particle phase (2.6%). The three-dimensional morphological characteristics and height analysis curves of the wear of the CTi0 coating and the CTi1.0 coating at high-temperature conditions are provided. The wear mechanism of this coating at high-temperature coating is mainly oxidative and adhesive wear. Compared with the wear characteristics under ambient conditions, the wear under high-temperature conditions exhibits bumps caused by plastic deformation rather than obvious furrows. According to the results of the height analysis, the height variation in the wear region of the CTi1.0 coating is significantly smaller than that of the CTi0 coating. These results suggest the existence of oxidative wear during the wear process, especially at high temperatures, which is usually associated with frictional heat. The micro- and nano-sized TiC particles improve the coating hardness and high-temperature friction resistance via solid-solution strengthening, diffusion strengthening, and grain refinement, demonstrating that oxidative and adhesive wear are the primary mechanisms of the coating’s wear at high temperatures. Compared to high-entropy alloy coatings, different ceramics have different mechanisms and reinforcing effects. Zhou et al. [8] examined the effects of two ceramic particles, B4C and SiC, on the mechanical properties and microstructure of CoCrMoNbTi high-entropy alloy coatings. The findings indicated that B4C had the strongest strengthening effect on the high-entropy alloy coating’s properties. The coating’s microhardness increased from 666.2 HV0.5 to 886.9 HV0.5, which was attributed to the in situ generation of TiC during the melting process from C and Ti elements in the TC4 substrate, which served as a role in precipitation reinforcement and grain refining on the coating. Additionally, the alloy’s room temperature abrasion resistance was improved, and the coefficient of friction and wear rate were significantly decreased.
Refractory alloying components (e.g., G., Nb, Ta, W, Mo, and V) cause HEA coatings to exhibit lattice distortion, obstruct dislocation motion, and encourage the development of BCC phases, thereby fortifying the coatings with the solid solution. Additionally, their larger atomic radius typically results in an increase in the solid solution’s lattice constant [7], enhancing the coatings’ mechanical qualities and wear resistance. Recent studies by Chang et al. [9], Xiang et al. [10], Liu et al. [11], and Li et al. [12] examined the effects of refractory alloying elements on the characteristics of high-entropy alloy coatings. Based on how well strength, plasticity, and density match, refractory alloy elements can be broadly categorized into three groups. The first group is made up of high-density W and Mo alloys as well as other elements from the fifth and sixth subgroups. The second group is made up of low-density, high-plasticity, and high-entropy refractory alloys that contain elements from the fourth subgroup with lower density, like B, Ti, Zr, and Hf. The third category consists of elements from the third period that are added to the previously listed elements, like Al and Si. The third category combines refractory alloys with high entropy, modified strength, and toughness with third-cycle elements like Al and Si. The coordinated action of ceramic phases and refractory alloy elements is studied in high-entropy alloy composite coatings to generate new research ideas for coatings with high abrasion resistance and excellent mechanical properties. In their study, Zhao et al. [13] investigated the synergistic effect of Mo and in situ TiC on AlCoCrFeNi HEA coatings. They found that the grain size of the coating was only 1/24 of that of the AlCoCrFeNi coatings. Additionally, the hardness of the coating increased by 69.3%, and the wear resistance improved by 5.77 times due to the synergistic effect of Mo and in situ TiC.
TiB and TiC are ceramic-reinforced particles known for their excellent performance. TiB exhibits exceptional physical and thermomechanical properties [14], boasting a remarkable hardness of up to 27 GPa. On the other hand, TiC possesses a high modulus of elasticity, high hardness, low coefficient of friction, excellent chemical stability, and good wettability with the metal substrate. Additionally, coatings containing an excess of elemental Ti in solid-solution form not only significantly enhance the base material’s mechanical properties and wear resistance [15] but also act as a solid lubricant, thereby reducing the coating wear rate. These properties make it a promising candidate for improving high-entropy alloy coatings. However, the in situ generation of single TiB2 ceramic particles for high-entropy alloy coatings exhibits poor high-temperature oxidation properties and low fracture toughness. To overcome these limitations, incorporating two or more ceramic-reinforcing phases has been explored to enhance the thermal stability of high-entropy alloy coatings and achieve coating grain refinement. The resulting high-entropy alloy composite coatings exhibit high hardness, high wear resistance, and high-temperature oxidation resistance [16][17][18]. He et al. [19] conducted a study on the preparation of CoCrMoNbTi high-entropy alloy coatings by adding B4C on a titanium alloy substrate using a laser melting technique. The researchers observed that as the B4C content increased, the solid phase in the coating underwent three stages: BCC1 + BCC2 → BCC1 + BCC2 + TiC → BCC1 + BCC2 + TiC + TiB. In addition, two ceramic-reinforced phases, TiC and TiB, were generated in situ. These ceramic particles were found to be diffusely distributed in the coating and exhibited different morphologies. The presence of these particles inhibited grain growth and resulted in grain refinement, leading to a submicron grain size. The hardness of the coating increased from 666.26 HV0.5 to 954.11 HV0.5, and Young’s modulus increased from 168.88 GPa to 240.35 GPa. These enhancements significantly improved the hardness and tensile strength of the coating. Yan et al. [20] successfully prepared in situ Ti (C, N)-reinforced AlCoCrFeNiSi high-entropy alloy coatings with a functional gradient bilayer structure on an H13 steel substrate. The involvement of nitrogen in the coating reaction resulted in the in situ generation of Ti (C, N) ceramic particles. The first layer is an FCC solid solution, and the second layer is a mixture of disordered BCC phase (Fe-Cr) and ordered B2 phase (Al-Ni-Ti). It has a high content of Ti (C, N) ceramic particles and TiSi2 speckled between grain boundaries in the microstructure. The high hardness of the second layer is attributed to the diffuse reinforcement induced by the ceramic particles. The in situ-generated Ti (C, N) ceramic particles, as non-deformable particles, effectively enhance the surface hardness of the HEA gradient coating. Additionally, the reticular TiSi2 distribution along the body-centered cubic grain boundaries impedes grain boundary migration and contributes to the microstructure refinement, further enhancing the high hardness of the second layer. The main wear mechanisms of the coating are oxidative wear and a small amount of abrasive wear. The strong interfacial bonding between the in situ-generated Ti (C, N) particles and the HEA substrate provides the coating with high surface hardness and resistance to plastic deformation. Similar to Yan et al., Liu et al. [21] utilized high-purity nitrogen as a protective gas to melt-coat FeCoNiCrMnTix (atomic ratio x = 0, 0.5, 1.0, and 1.5) HEA-coated high-entropy alloy coatings onto the surface of 304 stainless steel in order to produce high-quality, defect-free coatings. This process resulted in the in situ formation of TiN particles. The coating is composed of the FCC phase, TiN phase, and Laves phase. As the Ti content (x = 0, 0.5, 1.0, and 1.5) increases, a stepped crystalline morphology gradually forms, and the amount of TiN particles in the coating increases, thereby enhancing the wear resistance of the coating. However, when the Ti content exceeds 1.0 reduced defects in coatings.
Currently, laser cladding primarily utilizes various in situ generation methods to enhance the ceramic phase. These methods include in situ single generation, in situ single generation with high melting point element doping, in situ double generation, in situ multi-gradient generation, and others. Research has shown that ceramic particles generated in situ from some elements in the matrix are concentrated in the submicron or micro-nanometer level and exhibit uniform distribution. Increasing the ceramic particle content effectively enhances the composite coating’s hardness, wear resistance, and high-temperature abrasion resistance. However, the overall content of ceramic particles in the composite coatings is relatively low. Alternatively, content generated in situ are added to the elements to obtain a relatively high ceramic content in the entropy alloy composite coatings. In that case, the size of the ceramic particles will gradually increase with the increase in element content. Once the ceramic particles reach a certain size, the comprehensive performance of the composite coatings will decrease. Therefore, it is necessary to investigate the optimal content ratio of the elements to obtain excellent performance of the coatings when using this method to obtain ceramic particles. The in situ generation of single-phase ceramic phases is a straightforward process, allowing for the easy prediction and analysis of the phase composition of the composite coating after fusion coating. The combined action of high melting point elements and ceramic phases can further refine the grains and enhance composite coatings’ wear resistance and mechanical properties compared to the generation of single ceramic phases. However, the high melting point elements come at a higher cost. The in situ generation of dual ceramic phases compensates for the single ceramic phase’s limitations in terms of high-temperature oxidation and other properties. Building on this, in situ multi-ceramic phase gradient generation solves the issue of poor toughness in the coating. It can yield composite coatings with good hardness and plastic properties by increasing the ceramic content. Nevertheless, the method of coating preparation becomes more complex, and controlling the composition of the coating phase in each layer and the overall ceramic content is challenging. Each method has its advantages and disadvantages. However, different in situ generation methods can yield different phases and unique microstructures, further enhancing the hardness, abrasion resistance, high-temperature oxidation resistance, and corrosion resistance of high-entropy alloy coatings. These methods provide new design ideas for obtaining high-quality, high-entropy alloy coatings.

2. Addition Method

The additive method involves mixing ceramic powder and high-entropy alloy powder according to a certain proportion, ball milling the mixture, and pre-positioning it on the surface of the substrate. Alternatively, synchronous powder delivery can be used under the protection of inert gas or in a vacuum environment using a laser heat source to melt the pre-positioned coatings or spray powder, so that the powder into the metal substrate surface to form a ceramic phase reinforced by the high-entropy alloy coatings. The pre-positioning method is commonly used in experimental protocols where the powder particles are on the nano-scale, and the simultaneous powder feeding is mostly used for mixed powders of tens of microns or more.
The external addition method allows for the accurate control of the size and content of ceramic particles in high-entropy alloy composite coatings compared to the in situ generation method. Wang et al. [22], Li et al. [23], and Xi et al. [24] discovered that a small number of small-sized ceramic particles can greatly refine the grain size of the target material and effectively enhance its mechanical properties. Cai et al. [25] conducted an investigation on the laser fusion coating of FeMnCrNiCo + x(TiC) (x = 0, 5, 10, 15 wt%) coatings. The experiments involved adding a mixture of TiC ceramic particles with particle sizes ranging from 10 μm to 20 μm. The average grain size in the CoCrNiMn fusion cladding layer is 75.881 μm. However, with the addition of x = 0, 5, 10, 15 wt% TiC ceramic particles, the average grain size decreases to 36.061 μm, 29.714 μm, and 25.706 μm, respectively. This grain refinement significantly improves the resistance to plastic deformation of the fusion cladding layer. It is important to note that the plastic deformation resistance of the fusion-coated layer is significantly improved. However, as the ceramic content increases, coating cracks tend to extend along the grain direction. Additionally, excessive ceramic content during the friction process can accelerate the detachment of ceramic particles from the surface of the coating. Li et al. [26], in order to further improve the hardness and abrasion resistance of the AlCoCrFeNi high-entropy alloy, investigated the effect of different ceramic contents on the performance of the high-entropy coatings. Experiments in the AlCoCrFeNi high-entropy alloy with different mass fractions (10%, 20%, 30%) of NbC ceramic particles were added, and the coatings were prepared using the laser cladding method to study the organizational evolution and mechanical behaviors of the composite coatings with different contents of NbC particles. NbC particles are mainly distributed in the grain boundaries of the high-entropy alloys, and the NbC particles have a strong pinch effect, which has unique advantages in inhibiting the growth of high-entropy alloys’ grains. NbC particles have a strong pinch effect, which has a unique advantage in inhibiting the grain growth of high-entropy alloys, and the FCC phase in the coating decreases as the content of NbC particles increases. When the mass fraction of NbC particles is 20%, the alloy has the highest hardness (525 HV), the best wear resistance with an average coefficient of friction value of 1.023, and a mass loss of 1.05 mg. The additive method allows for a flexible selection of ceramic particles, overcoming the limitations of the in situ generation method. SiC is an excellent ceramic reinforcement because of its high hardness, excellent wear resistance, superior thermal conductivity, and high-temperature oxidation resistance; it is often selected as the reinforcing phase for metallic materials. Xu et al. [27] prepared SiC particle-reinforced CoCrFeNiCu composite coatings on the surface of 316 L stainless steel using the laser melting technique. The CoCrFeNiCu (SiC)x HEA coating is a face-centered cubic structure, and a second phase consisting of Cr7C3 is formed at the grain boundaries. Grain boundary strengthening improves the hardness, wear resistance, and corrosion resistance. For the CoCrFeNiCu (SiC)15 HEA coating, the microhardness, wear, and friction coefficients were 568.4 HV, 0.9 mg, and 0.35, respectively. With the increase of SiC content, the corrosion resistance of CoCrFeNiCu (SiC)x HEA coatings in 3.5% NaCl solution increases. The corrosion performance of the CoCrFeNiCu (SiC)1.0 coatings is better than the other coatings, and the wear resistance, tribological properties, and corrosion resistance of CoCrFeNiCu high-entropy alloy with the addition of SiC ceramic phase are significant. The wear resistance, tribological properties, and corrosion resistance of CoCrFeNiCu high-entropy alloy with SiC ceramic phase are significantly improved. In the high-entropy alloy composite coatings with added ceramics, changes in the atomic ratio of certain constituent elements in the high-entropy alloy base will cause a phase change in the coating and thus improve the coating properties and the effect of changes in the atomic ratio in the high-entropy coatings on the properties of the composite coatings can be conveniently realized by the additive method. Xu et al. [28] investigated the effect of the content of Al and Ti on the properties of the AlCoCrFeNiTi HEA coatings reinforced by SiC particles under laser melting conditions. The influence of Al and Ti element content on the characteristics of AlCoCrFeNiTi coatings reinforced with SiC particles under laser melting conditions was examined. The microstructures, phase compositions, mechanical properties, and corrosion resistance of the coatings with and without SiC particles were analyzed and compared, offering novel research to elucidate the advancement of high-strength and high-wear-resistant high-entropy alloy coatings. The results show that SiC particles decompose into Si and C during liquid phase deposition. The cubic phase L21 in the Al0.5 alloy coatings precipitates out of the disordered BCC matrix and transforms into the coarse lath-like organization composed of the L21 and FCC matrix in the Al0.5/SiC coatings. Meanwhile, the braided network structure in the Al0.8/SiC alloy coatings was more refined with the increase of the volume fraction of the B2 phase. The hardness of the Al0.8/SiC alloy coatings increased from 637 HV0.2 to 718 HV0.2, and the coefficient of friction was reduced from 0.40 to 0.31. The presence of SiC particles exerted a detrimental impact on the microhardness of the Al0.5/SiC alloy coating, leading to a decrease from 743 HV0.2 to 679 HV0.2. This was attributed to the coarsening of the microstructure and an increased fraction of the supple FCC solid solution. The formation of a fine cubic L21 phase in the disordered BCC matrix in the Al0.5 alloy coatings was replaced by a lath-like coupled organization consisting of FCC and L21 phases. As a result, the coating microhardness shows a decreasing trend.
High-content ceramic particles reinforced laser fusion composite coatings are brittle and generate huge thermal stresses during the laser fusion process, which often leads to the presence of cracks. The selection and design of metal matrix materials is an effective way to solve the cracking problem of metal–ceramic composite coatings. Due to the special composition design, high-entropy alloys (HEAs) have excellent wear resistance, corrosion resistance, and high-temperature softening resistance. In particular, HEAs with face-centered cubic (FCC) single solid-phase structures exhibit good toughness and corrosion resistance but low hardness and strength. Combining FCC HEAs with ceramic particles can obtain composite coatings with high strength and toughness. Ma et al. [29] successfully prepared a crack-free 60 wt% WC particle-reinforced FeCoNiCr high-entropy alloy composite coating. The composite coating consists of a face-centered cubic (FCC) solid-solution phase, WC, W2C, and Co4W2C. The composite coating consists of dendrites, massive precipitated phases, and herringbone-like precipitated phases distributed around the WC particles. The composite coating has no obvious weaving structure. The average microhardness of the composite coatings was 506 HV0.05. The average coefficient of friction and wear volume loss were 0.474 and 0.041 mm3, respectively, significantly improving the coatings’ hardness and wear resistance.
When the physical properties of the ceramic particles and the alloy matrix are different, increasing residual stresses within the coating as the ceramic addition increases can lead to cracks within the coating. According to studies [30][31][32][33][34], the best option to reduce residual stresses and enhance wear and corrosion performance is to use gradient coatings with continuous compositional content variations. Functional gradient coatings on ceramic and metallic materials lead to coatings with continuous gradient behavior in terms of organization and properties. These coatings meet the specific performance requirements at different locations of the part and address the defects associated with poor bond strength and rapid changes in properties at the metal/ceramic interface. Wang et al. [35] and Chen et al. [36] showed that gradient coatings improve the performance of ceramic composite coatings to a large extent and provide new ideas for surface modification and repair of parts. Zhang et al. [37] explored a new method of ceramic-reinforced CoCrFeNiMo0.2 high-entropy alloy composite gradient coating in order to strengthen the high-entropy alloy with a face-centered cubic structure, and the design of the coating on the substrate surface. SiC was not added to the first layer of material to improve the bonding strength between the coating and the matrix, and the SiC content was increased layer by layer. Process optimization parameters were used, and each layer was cooled for three minutes after fusion coating to reduce heat accumulation. When a high-power laser melts, silicon carbide mainly decomposes into graphite and silicon vapor. Some carbon atoms dissolve in the solid solution, while others combine with other alloying elements to form carbides. Excessive decomposition of silicon carbide leads to an excess of elemental carbon. In a high-temperature melt pool, the carbon adsorbs to each other and covers the gaseous material, slowing down the release of the gas. The melt pool solidifies rapidly, and the gases have no time to escape. As a result of the pressure, a structure with large pores on the coating and small pores underneath is eventually formed. The gradient coatings prepared using this method possessed good frictional and mechanical properties, with the second, third, and fourth layers exhibiting significantly higher average hardnesses, measured at 594 HV, 722 HV, and 788 HV, respectively, which can be attributed to the presence of a body-centered cubic structure, carbides, and grain-boundary strengthening effects. The hardness of these layers is three to four times higher than that of the first layer. The wear mechanism changes from adhesive wear to abrasive wear as the number of coating layers increases. The wear rates of the second, third, and fourth layers were all reduced by at least 87% compared to the first layer. However, different forms of abrasive wear were observed between these layers.
The additive method is currently focused on the high-entropy alloy to add a ceramic phase, high-entropy alloy of certain elements in the change on the addition of ceramic phase after the coating performance, gradient composite coatings, and other research methods, each method of ceramic particles added to the content and size of the different will have an impact on the coating organization and thus affecting the performance of the coating. Compared to the in situ generation method, the additive method can flexibly control the size and content of ceramic particles in the coating. Although the coating obtained via the additive method is easy to produce micro-cracks along the direction of the ceramic particles, via the control of the ceramic content, particle size, and process parameters, it can effectively control the cracks produced by the coating to obtain excellent performance.

This entry is adapted from the peer-reviewed paper 10.3390/coatings14010127

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