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Article

Effect of Modulation Period on the Microstructure and Tribological Properties of AlCrTiVNbN/TiSiN Nano Multilayer Films

School of Mechanical and Materials Engineering, North China University of Technology, Beijing 100144, China
*
Author to whom correspondence should be addressed.
Coatings 2025, 15(7), 839; https://doi.org/10.3390/coatings15070839
Submission received: 24 June 2025 / Revised: 13 July 2025 / Accepted: 15 July 2025 / Published: 17 July 2025
(This article belongs to the Special Issue Surface Protection for Metal Materials)

Abstract

The impact of modulation periods on the microstructure, as well as the tribological and mechanical characteristics of the AlCrTiVNbN/TiSiN nano multilayer films, was investigated. The films were prepared with modulation periods ranging from 4 nm to 7 nm, and their properties were explored using X-ray diffraction (XRD), scanning electron microscope (SEM), nanoindentation, and a tribological tester. All nano multilayer films revealed a face-centered cubic (FCC) structure with a preferred planar direction of (200). As the modulation period increased, the XRD peak moved to higher angles, and the interplanar distance decreased. Also, the mechanical properties deteriorated, and the COF rose monotonically as a result. The nano multilayer film with a modulation period equal to 4 nm exhibited a smooth surface with minimal small particles, the highest hardness of 15.51 ± 0.16 GPa and elastic modulus of 182.89 ± 2.38 GPa, the highest values for the ratios of H/E and H3/E2, the lowest average friction coefficient of 0.73, and a wear rate equal to (8.2 9 ± 0.18) × 10−8 mm3·N−1·m−1. The improvement in the properties of the film was ascribed to the coherent growth and alternating stress field between the AlCrTiVNbN and TiSiN layers.

1. Introduction

Friction and wear are some of the main parameters responsible for the failure of mechanical components [1,2]. The coating is a very effective method to enhance the tribological behaviors of the parts [3,4]. Nano multilayer films are capable of combining the beneficial properties of two different materials, leading to improvements in the hardness, elastic modulus [5,6,7], tribological properties, corrosion resistance [8,9], thermal stability [10,11], and thermoelectrical properties [12] of the films. The contents and modulation period λ of elements affect the microstructure and properties of the films [13,14,15]. The hardness of CrN/TiN nano multilayer films ranges from 26 to 29 GPa when λ ranges from 6 to 16.5 nm. The CrN/TiN nano multilayer film featuring a λ value of 8.4 nm demonstrates the lowest wear rate [16]. The CrAlN/TiSiN film with λ = 19 nm shows a superior resistance to impact wear compared to the one with λ = 455 nm [17]. Moreover, the structure of the AlN layer transforms into a c-AlN pseudocrystal structure due to the “template effect” introduced by TaN. Enhanced oxidation resistance is observed in the TaN/AlN nano multilayer film when lAlN = 0.4 nm, as the AlN layers operate as an effective barrier preventing the oxidation of TaN layers [18]. The TiC/Ti nano multilayer with a thickness of 1.5 nm for the Ti sublayer has a higher hardness and fracture toughness than the film with 8 nm due to the FCC-TiC(111)/FCC-Ti(111) coherent interface [19]. High-entropy nitrides (HENs) were selected as a material of the nano multilayer film because of their outstanding properties, such as their higher hardness, higher thermal hardness, better cavitation erosion resistance, better corrosion resistance, and tribological properties [20,21]. The TiN/(CrVTaTiW)Nx coating has an FCC structure. It is reported that the HEN layer thickness exhibited a positive correlation with both the elastic modulus and hardness of the multilayer films, with the highest values appearing for a layer thickness equal to 4.8 nm [22]. The (AlCrTiZrMo)N/ZrO2 film displayed the highest values of elastic modulus and hardness for a ZrO2 layer thickness equal to 0.6 nm. This observation may be attributed to the formation of an epitaxial growth interface that strengthens the film structure [23]. The (AlCrTiZrV)N/SiC nano multilayer film develops a crystalline structure when the SiC layer thickness reaches 0.5 nm, influenced by the templating effects of the (AlCrTiZrV)N layer. At this thickness, the film achieves its peak hardness [24]. The literature review indicates that HENs possess significant potential for advanced applications. Based on these findings, an investigation was conducted on the cavitation erosion resistance of TiSiN/NiTiAlCoCrN nano multilayer films with various λ values. The results reveal that as λ increases, the mass loss from cavitation erosion initially declines and subsequently rises. The optimal cavitation erosion resistance is achieved in the TiSiN/NiTiAlCoCrN nano multilayer film with λ = 11 nm [25]. Therefore, the one layer or λ has a critical influence on the characteristics of multilayer thin films.
AlCrTiVNbN/TiSiN nano multilayer films with various λ values were synthesized using a multi-target magnetron sputtering system. The surface morphologies and phase structure of the films were examined through SEM and XRD techniques. Moreover, their tribological and mechanical characteristics were evaluated.

2. Experimental Details

2.1. Film Deposition

The substrates made of 304 stainless steels with dimensions of Φ20 mm × 3 mm were used. These substrates first underwent ultrasonic cleaning for 20 min in an acetone solution and then in an anhydrous ethanol solution. The targets were Ti, TiSi, and AlCrTiVNb, each with dimensions of Φ50.8 mm × 4 mm. The TiSi target contained 10% Si, while the AlCrTiVNb target consisted of equimolar proportions of all constituent elements. All targets had a purity level of 99.99%.
JCP-350M2 (Techno Company, Beijing, China) was utilized to synthesize the AlCrTiVNbN/TiSiN nano multilayer films. The vacuum level inside the chamber was 3 × 10−3 Pa. Argon was introduced as the working gas. The targets underwent pre-sputtering for 10 min, while the substrates were etched with Ar ions for 10 min to eliminate surface impurities and oxides. Nitrogen was introduced as the reactive gas, maintaining an Ni−Ar flow rate ratio of 1:1. The film deposition was carried out at room temperature. The substrate was not preheated. A TiN transition layer was deposited for 60 min to enhance film−substrate adhesion. The AlCrTiVNb target was controlled using DC power of 110 W, resulting in a deposition speed equal to 0.09 nm·s−1. The TiSi target was controlled by RF power at 100 W, producing a deposition rate equal to 0.045 nm·s−1. The AlCrTiVNb and TiSi targets were alternatively activated to fabricate the AlCrTiVNbN/TiSiN nano multilayer film. Figure 1 shows the nano mutilayer structure. The thickness of the AlCrTiVNbN layer was kept at 3 nm, while the TiSiN layer thicknesses were set at 1, 2, 3, and 4 nm, resulting in λ values of 4, 5, 6, and 7 nm, respectively. The detailed parameters are outlined in Table 1.

2.2. Characterization of Film Properties

The phase structures of the films were examined via an Ultima IV XRD(Rigaku, Tokyo, Japan) system, coupled with a Cu target (Cu−Kα). The Cu−Kα wavelength was 0.15406 nm, with an operating current equal to 40 mA and a voltage equaling 40 kV. The scanning was performed at a speed of 8°/s, with a step size of 0.02°, covering a 2θ range from 10° to 80°. The surface morphology, cross-sectional structure, and wear track images were captured using a Sigma-300 SEM (Carl Zeiss AG, Oberkochen, Germany) system. Elemental compositions on the film structure and within wear tracks were analyzed using an EDS (Oxford Instruments, Oxfordshire, UK). It should be indicated that the hardness and elastic modulus were measured via an nano-indenter (Anton Paar GmbH, Graz, Austria), equipped with a Berkovich tip. The unloading and loading rates were set to 20 mN·min−1, with a maximum applied load equal to 20 mN. For each sample, five measurement points were selected, and the average of these values was explored as the final result. The tribological performance was analyzed using a CFT-I (Zhongke Co., Lanzhou, China) material surface performance tester. A GCr15 ball with a diameter equal to 6 mm served as the counter material. The applied load (F) was 100 g, and the reciprocating frequency (f) was 200 C·min−1, the reciprocating sliding distance was 5 mm, and the total test duration was 20 min. Each friction test was performed three times for every sample. The wear track volume (V) was quantified utilizing a laser scanning confocal microscope(Olympus Corporation, Tokyo, Japan), whereas the wear rate was determined mathematically as follows:
W = V F d
where F denotes the normal force and d is the sliding distance.

3. Results and Discussion

3.1. Microstructure

Figure 2 illustrates the XRD patterns, which show an FCC structure with a preferred planar direction of (200). Table 2 presents the diffraction angle 2θ, interplanar distance and the full width at half maximum (FWHM), revealing a positive correlation between λ and 2θ, while the interplanar distance shows a negative correlation.
The 2θ value corresponding to the (200) plane of the AlCrTiVNbN monolayer film is lower than those observed for all AlCrTiVNbN/TiSiN nano multilayer films. As λ increases, both the 2θ values and the FWHM increase for the (200) plane, while the interplanar distance decreases. Further analysis using Scherrer’s formula reveals that the increase in FWHM values indicates a reduction in interplanar distance and crystallinity [26]. This is consistent with the 2θ results for the (200) plane. Based on the template effect [27], the TiSiN layer adopts the coherent lattice structure of the AlCrTiVNbN layer during the deposition process. As the lattice constant of the TiSiN layer is smaller than that of the AlCrTiVNbN layer, the TiSiN layer experiences tensile stress while the AlCrTiVNbN layer undergoes compressive stress. This results in the formation of alternating tensile and compressive stress field within the AlCrTiVNbN/TiSiN nano multilayer films, thereby enhancing their overall structural characteristics.
The surface and cross-sectional images of the AlCrTiVNbN/TiSiN nano multilayer films presented in Figure 3 reveal a columnar crystal, oriented perpendicular to the substrate surface. The total film thickness decreases from 944 nm to 659 nm with increasing λ. According to the relationship between the deposition cycles, modulation period λ, and the nano multilayer film, the λ values for M4 to M7 were calculated as 3.78 nm, 4.41 nm, 5.03 nm, and 5.51 nm, respectively. The measured λ values of the films are lower than the designed values in Table 1 because manual control of target switching induces deposition time errors. From top to bottom, the film structure consists of the AlCrTiVNbN/TiSiN nano multilayer film, transition layer TiN, and substrate. The interfaces formed between the layers can be seen clearly in the obtained images. With increasing λ, the thickness of the AlCrTiVNbN/TiSiN nano multilayer films is reduced because the cycles decrease. The surfaces of the films have a cauliflower-like morphology and contain cracks. With increasing λ, the particles on the surface grow larger, and the number of cracks also increases. The reason is that the particles easily grow because the atoms diffuse less readily at the low deposition speed during the process. The cracks form because of the residual stress between the particles during the deposition process [28].
Figure 4 and Figure 5 depict the 3D morphologies and surface roughness of the AlCrTiVNbN/TiSiN nano multilayer films measured by AFM, respectively. The smallest particle size is seen on the surface of the M4 film. As λ increases, the size of the particles becomes bigger. The size of the particles is the largest on the surface of the M7 film, which coincides with the SEM image in Figure 3. As λ increases, the surface roughness of the films increases. As λ increases, the speed of deposition decreases and the atoms do not easily diffuse, which leads to the atoms forming “island” shapes and grow into bigger particles during deposition.

3.2. Mechanical Properties

Figure 6 and Table 3 depict the hardness, elastic modulus, H/E, and H3/E2 of the nano multilayer films. The hardness of the M4 film is higher than that of the AlCrTiVNbN film and the other nano multilayer films, reaching 15.51 ± 0.16 GPa; simultaneously, the elastic modulus of M4 peaks at 182.89 ± 2.38 GPa, representing the maximum value observed across all of the samples. As λ increases, the hardness, elastic modulus, H/E, and H3/E2 decrease. For the M7 film, the hardness and elastic modulus drop to 9.472 ± 0.39 GPa and 163.35 ± 3.69 GPa, respectively, along with the lowest H/E and H3/E2 ratios.
H/E reflects the fracture toughness of the films and H3/E2 represents the resistance ability to the plastic deformation of the films [29]. Higher H/E and H3/E2 values indicate better tribological properties of the films. M4 has the highest H/E and H3/E2, which tends to improve the tribological properties of films [30,31].
The enhancement in mechanical properties can be attributed to the alternating stress field between the AlCrTiVNbN and TiSiN layers, as well as to solution strengthening. Firstly, when λ < 4 nm, the TiSiN layer grows epitaxially along the AlCrTiVNbN layer, enhancing the mutual layer growth. The interfaces between the TiSiN and AlCrTiVNbN layers inhibit dislocation motion, and an alternating stress field forms between the layers. Secondly, the AlCrTiVNbN layer undergoes solution strengthening due to its composition of seven elements, similar to HEAS.

3.3. Tribological Characteristics

The friction curve and mean COF values of the films are depicted in Figure 7. The friction enters a stable friction stage after 3 min, and the friction curve exhibits minimal fluctuation. The average COF increases as λ increases. The M4 film exhibits the lowest friction coefficient of 0.73, which is bigger than that of the AlCrTiVNbN monolayer. There are four reasons for the improvement in tribological properties. Firstly, the M4 film has the highest hardness. Secondly, it also has the highest H/E and H3/E2 values, which enhance the fracture toughness of the films. Thirdly, the M4 film has the smoothest surface, which reduces shear forces during friction. An alternating stress field and numerous interfaces exist within the nano multilayer film. These interfaces significantly restrict crack propagation and reduce the formation of wear debris.
The wear track morphologies of the AlCrTiVNbN/TiSiN nano multilayer films are depicted in Figure 8. Furrows ar visible on wear tracks surfaces, and the width of the wear tracks increases with increasing λ. Wear debris appears on all surfaces of the wear tracks, and tearing marks appear on the surfaces of M6 and M7 films. Thus, abrasive wear is the primary wear mechanism in the M4 and M5 films, while a combination of adhesive and abrasive wear is responsible for the wear behavior observed within the M6 and M7 films.
The wear rate and wear volume of the films, as presented in Figure 9, indicate a positive correlation with λ. The M4 film exhibits the lowest wear volume of 3.32 × 10−3 mm3 and the lowest wear rate, equal to (8.29 ± 0.18) × 10−8 mm3∙N−1∙m−1. The M5 film and M6 film displayed similar wear rates and wear volumes. The M7 exhibit the highest wear rate, equal to 11.9 × 10−8 mm3∙N−1∙m−1.
Figure 10 depicts the element distribution images of the M4 film. The elements Al, Ti, V, Nb, N disappear from the wear track, while the concentration of O is significantly higher in the wear track than on the undeformed surface of the M4 film. This indicates that oxidation takes place during the friction process. The oxidation products generated play a dual role: they not only decrease surface abrasion and spalling, but also form protective layers that act as solid lubricants, like Magnéli phases, to reduce adhesion [32]. During the friction process, oxides such as Al2O3, Cr2O3, TiO2, and V2O5 are formed. Al2O3 and Cr2O3 exhibit high hardness, whereas TiO2 and V2O5, which are associated with Magnéli phases, provide self-lubricating properties, thus enhancing the tribological characteristics of the films [33]. The increased Cr content on the wear track compared to the deposition surface suggests that the M4 film has worn through to the substrate.

4. Conclusions

The AlCrTiVNbN/TiSiN nano multilayer films were produced using a magnetron sputtering system. The structural characteristics were investigated comprehensively.
(1)
All prepared films displayed an FCC structure with a preferred planar direction of (200). As λ increased, the interplanar distance decreased and the surface roughness increased.
(2)
The nano multilayer film with λ = 4 nm (M4) showed a smooth surface with small particles. It also demonstrated the highest hardness of 15.51 ± 0.16 GPa and elastic modulus of 182.89 ± 2.38 GPa, along with the peak H/E (0.084) and H3/E2 (0.111) ratios. As λ increased, the hardness and elastic modulus of the films declined. This was ascribed to the solution strengthening and the formation of a compression and tensile alternating stress field between the TiSiN and AlCrTiVNbN layers.
(3)
As λ increased, the COF of the films and the wear rate of the films increased. The film with λ = 4 nm (M4) showed the lowest COF of 0.73 and the wear rate equal to (8.29 ± 0.18) × 10−8 mm3∙N−1∙m−1. The oxidation products decreased surface abrasion and displayed self-lubrication during the tribological process. The wear mechanism included abrasive wear, adhesive wear, and oxidation wear.

Author Contributions

Conceptualization, H.Y., Z.D. and F.L.; methodology, H.Y.; validation, H.Y., H.W. and X.L.; formal analysis, H.Y.; investigation, H.W.; resources, F.L.; data curation, H.W.; writing—original draft preparation, H.W.; writing—review and editing, H.Y.; visualization, H.Y.; supervision, F.L.; project administration, F.L. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by Joint Funds of the National Natural Science Foundation of China, grant number “U23A2025” and The APC was funded by Yuyou Team of North China University of Technology (Grant No. 22XN746).

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

All obtained data have been included in the article.

Acknowledgments

Thanks Liu for his guidance during the experiment and for his valuable suggestions in the data analysis.

Conflicts of Interest

The authors declare no conflicting interests.

References

  1. Luo, D.; Zhou, Q.; Huang, Z.; Li, Y.; Liu, Y.; Li, Q.; He, Y.; Wang, H. Tribological Behavior of High Entropy Alloy Coatings: A Review. Coatings 2022, 12, 1428. [Google Scholar] [CrossRef]
  2. Xu, Y.; Li, G.; Xia, Y. Synthesis and characterization of super-hard AlCrTiVZr high-entropy alloy nitride films deposited by HiPIMS. Appl. Surf. Sci. 2020, 523, 146529. [Google Scholar] [CrossRef]
  3. Zhang, X.; Pelenovich, V.; Liu, Y.; Ke, X.; Zhang, J.; Yang, B.; Ma, G.; Li, M.; Wang, X. Effect of bias voltages on microstructure and properties of (TiVCrNbSiTaBY)N high entropy alloy nitride coatings deposited by RF magnetron sputtering. Vacuum 2022, 195, 110710. [Google Scholar] [CrossRef]
  4. Zhao, Y.Q.; Mu, Y.T.; Liu, M. Mechanical properties and friction-wear characteristics of VN/Ag multilayer coatings with heterogeneous and transition interfaces. Trans. Nonferrous Met. Soc. China 2020, 30, 472–483. [Google Scholar] [CrossRef]
  5. Ren, B.; Zhao, R.F.; Zhang, G.P.; Liu, Z.X.; Cai, B.; Jiang, A.Y. Microstructure and properties of the AlCrMoZrTi/(AlCrMoZrTi)N multilayer high-entropy nitride ceramics films deposited by reactive RF sputtering. Ceram. Int. 2022, 48, 16901–16911. [Google Scholar] [CrossRef]
  6. Wang, L.P.; Qi, J.L.; Cao, Y.Q.; Zhang, K.; Wen, M. N-rich Zr3N4 nanolayers-dependent superhard effect and fracture behavior in TiAlN/Zr3N4 nanomultilayer films. Ceram. Int. 2020, 46, 19111–19120. [Google Scholar] [CrossRef]
  7. Zhang, Y.T.; He, X.; Wang, N.; Wang, L.P.; Pang, H.P.; Hao, J.; Wen, M.; Qi, J. Insight into deformation modes of bcc-Nb/fcc-Cantor nanomultilayer film. Surf. Coat. Technol. 2025, 497, 131751. [Google Scholar] [CrossRef]
  8. Yang, M.; Fan, X.; Ren, S.; Wang, L. Enhanced environmental adaptability of sandwich-like MoS2/Ag/WC nanomultilayer films via Ag nanoparticle diffusion-dominated defect repair. Mater. Horiz. 2024, 11, 5230–5243. [Google Scholar] [CrossRef]
  9. Zhang, Z.; Jin, P.; Chen, Y.H.; Zhang, T.F.; Gyawali, G.; Zhu, X.Z.; Li, G.F.; Zhang, S.H. Enhanced corrosion and tribo-corrosion resistance of self-organized nano-multilayer oxynitride coatings on tungsten copper alloy. Corros. Sci. 2025, 246, 112740. [Google Scholar] [CrossRef]
  10. Lu, X.; Zeng, L.F.; Zhang, J.H.; Li, S.Y.; Jiang, P.G. Significant enhancement in the strength and thermal stability of Cu/Nb nano-multilayer via a minor Ag doping. J. Alloys Compd. 2025, 1022, 180035. [Google Scholar] [CrossRef]
  11. Yeom, J.; Lorenzin, G.; Claudia, C.; Jolanta, J.-R. The thermal stability and degradation mechanism of Cu/Mo nanomultilayers. Sci. Technol. Adv. Mater. 2024, 25, 2357536. [Google Scholar] [CrossRef]
  12. Kim, T.; Han, S.; Lee, J.; Na, Y.; Jung, J.; Park, Y.C.; Oh, J.; Yang, C.; Kim, H.Y. Development and Characterization of Low Temperature Wafer-Level Vacuum Packaging Using Cu-Sn Bonding and Nanomultilayer Getter. Micromachines 2023, 14, 448. [Google Scholar] [CrossRef]
  13. Wang, Y.X.; Wang, D. Effects of yttrium doping on high-temperature oxidation, friction, and wear properties of CrAlN films. Mater. Res. Express 2024, 11, 016402. [Google Scholar] [CrossRef]
  14. Wang, Y.X.; Lou, B.Y. Microstructure and High-Temperature Friction and Wear Properties of CrAlMoN Film. Oxid. Met. 2021, 95, 239–250. [Google Scholar] [CrossRef]
  15. Wang, Y.X.; Ji, Y. Influence of Mo Doping on the Microstructure, Friction, and Wear Properties of CrAlN Films. J. Mater. Eng. Perform. 2021, 30, 1938–1944. [Google Scholar] [CrossRef]
  16. Petkov, N.; Bakalova, T.; Bahchedzhiev, H.; Krafka, M.; Lemberk, L. Modulation period effect on the CrN/TiN coating properties. J. Nano Res. 2023, 79, 37–48. [Google Scholar] [CrossRef]
  17. Luo, Y.; Dong, Y.; Xiao, C.; Wang, X.; Peng, H. Impact Abrasive Wear Property of CrAlN/TiSiN Multilayer Coating at Elevated Temperatures. Materials 2022, 15, 2214. [Google Scholar] [CrossRef]
  18. Qi, J.L.; Wang, L.P.; Zhang, Y.; Guo, X.; Yu, W.Q.; Wang, Q.H.; Zhang, K.; Ren, P.; Wen, M. Amorphous AlN nanolayer thickness dependent toughness, thermal stability and oxidation resistance in TaN/AlN nanomultilayer films. Surf. Coat. Technol. 2021, 405, 126724. [Google Scholar] [CrossRef]
  19. Hao, J.; Wang, L.P.; Zhao, C.; Zhang, K.; Qi, J.L.; Pang, H.P.; Ren, P.; Wen, M. Effects of interface configurations on strengthening-toughening and tribological behaviors of TiC/Ti nano-multilayers. Surf. Coat. Technol. 2025, 497, 131726. [Google Scholar] [CrossRef]
  20. Zaid, H.; Tanaka, K.; Ciobanu, C.V.; Yang, J.M.; Kodambaka, S.; Kindlund, H. Growth of elastically-stiff, nanostructured, high-entropy alloy nitride, (VNbTaMoW)N/Al2O3(0001) thin film. Scr. Mater. 2021, 197, 113813. [Google Scholar] [CrossRef]
  21. Yuan, Y.; Xiao, Y.L.; Yu, C.T.; Xuan, L.; Azfar, H.; Jiao, L.Z.; Jun, J.L.; Chao, Y.; Hui, C.; Rui, L. Characterization of interface properties and enhancement of thermal hardness in TiN/(CrVTaTiW)Nx multilayered structures: Investigating diverse crystallization templates. J. Alloys Compd. 2025, 1020, 179440. [Google Scholar] [CrossRef]
  22. Tu, Y.; Li, J.; Yuan, Y.; Zhao, J.; Hameed, A.; Yan, C.; Chen, H.; Lan, R.; Cheng, B.; Wang, P.; et al. Thickness modulation influenced mechanical properties of TiN/(CrVTaTiW)Nx multilayer coatings. Ceram. Int. 2024, 50, 53007–53014. [Google Scholar] [CrossRef]
  23. Zhai, Q.; Li, W.; Liu, P.; Cheng, W.; Zhang, K.; Ma, F.; Chen, X.; Feng, R.; Liaw, P.K. Mechanical Behavior and Thermal Stability of (AlCrTiZrMo)N/ZrO2 Nano-Multilayered High-Entropy Alloy Film Prepared by Magnetron Sputtering. Crystals 2022, 12, 232. [Google Scholar] [CrossRef]
  24. Wang, Y.; Hao, E.; An, Y.; Chen, J.; Zhou, H. Effects of microstructure and mechanical properties on cavitation erosion resistance of NiCrWMoCuCBFe coatings. Appl. Surf. Sci. 2021, 547, 149125. [Google Scholar] [CrossRef]
  25. Li, B.H.; Ma, X.; Li, W.; Zhai, Q.Q.; Liu, P.; Zhang, K.; Ma, F.C.; Wang, J.J. Effect of SiC thickness on microstructure and mechanical properties of (AlCrTiZrV)N/SiC nano-multilayers film synthesized by reactive magnetron sputtering. Thin Solid Film. 2021, 730, 138724. [Google Scholar] [CrossRef]
  26. Yan, H.; Si, L.; Dou, Z.; Yang, Y.; Li, H.; Liu, F. Cavitation Erosion Resistance of TiSiN/NiTiAlCoCrN Nanomultilayer Films with Different Modulation Periods. Coatings 2023, 13, 1431. [Google Scholar] [CrossRef]
  27. Cheng, W.J.; Liu, P.; Zhu, X.F.; Meng, Y.; Lu, H.M.; Li, W. Effects of modulation layer thickness on microstructures and mechanical behavior of VN/TiN-Ni nano-multilayered films. Trans. Nonferrous Met. Soc. China 2025, 24. Available online: https://link.cnki.net/urlid/43.1239.tg.20250318.1056.011 (accessed on 1 March 2025).
  28. Yong, Q.F.; Fei, Z.; Qian, Z.W.; Mao, D.Z.; Zhi, F.Z.; Li, L.K.Y. The influence of Mo target current on the microstructure, mechanical and tribological properties of CrMoSiCN coatings in artificial seawater. J. Alloys Compd. 2019, 791, 800–813. [Google Scholar]
  29. Li, C.; Wang, L.; Shang, L.; Cao, X.Q.; Zhang, G.; Yu, Y.; Li, W.S.; Zhang, S.Z.; Hu, H.T. Mechanical and high-temperature tribological properties of CrAlN/TiSiN multilayer coating deposited by PVD. Ceram. Int. 2021, 47, 29285–29294. [Google Scholar] [CrossRef]
  30. Chen, Z.L.; Lou, M.; Geng, D.S.; Xu, Y.X.; Wang, Q.M.; Zheng, J.; Zhu, R.Y.; Chen, Y.B.; Kim, K.H. Effect of the modulation geometry on mechanical and tribological properties of TiSiN/TiAlN nano-multilayer coatings. Surf. Coat. Technol. 2021, 423, 127586. [Google Scholar] [CrossRef]
  31. Zhu, S.; Zhang, B.S.; Tao, X.W.; Yu, Y.Q.; Zhang, Z.J.; Wang, Z.; Lu, B. Microstructure and Tribology Performance of Plasma-Clad Intermetallic-Reinforced CoCrFeMnNi-Based High-Entropy Alloy Composite Coatings. Tribol. Trans. 2020, 64, 264–274. [Google Scholar] [CrossRef]
  32. Chen, X.; Ma, Y.; Yang, Y.; Meng, A.; Han, Z.X.; Han, Z.; Zhao, Y.H. Revealing tribo–oxidation mechanisms of the copper–WC system under high tribological loading. Scr. Mater. 2021, 204, 114142. [Google Scholar] [CrossRef]
  33. Bolelli, G.; Steduto, D.; Kiilakoski, J.; Varis, T.; Lusvarghi, L.; Vuoristo, P. Tribological properties of plasma sprayed Cr2O3, Cr2O3–TiO2, Cr2O3–Al2O3 and Cr2O3–ZrO2 coatings. Wear 2021, 480–481, 203931. [Google Scholar] [CrossRef]
Figure 1. Schematic diagram of the AlCrTiVNbN/TiSiN nano multilayer film.
Figure 1. Schematic diagram of the AlCrTiVNbN/TiSiN nano multilayer film.
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Figure 2. XRD patterns of AlCrTiVNbN/TiSiN nano multilayer films.
Figure 2. XRD patterns of AlCrTiVNbN/TiSiN nano multilayer films.
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Figure 3. Surface and cross-sectional images obtained for the AlCrTiVNbN/TiSiN nano multilayer films: (a) 4 nm, (b) 5 nm, (c) 6 nm, and (d) 7 nm.
Figure 3. Surface and cross-sectional images obtained for the AlCrTiVNbN/TiSiN nano multilayer films: (a) 4 nm, (b) 5 nm, (c) 6 nm, and (d) 7 nm.
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Figure 4. Three-dimension images of AlCrTiVNbN/TiSiN nano multilayer films: (a) 4 nm, (b) 5 nm, (c) 6 nm, (d) 7 nm, and (e) 0 nm.
Figure 4. Three-dimension images of AlCrTiVNbN/TiSiN nano multilayer films: (a) 4 nm, (b) 5 nm, (c) 6 nm, (d) 7 nm, and (e) 0 nm.
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Figure 5. Surface roughness of AlCrTiVNbN/TiSiN nano multilayer films.
Figure 5. Surface roughness of AlCrTiVNbN/TiSiN nano multilayer films.
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Figure 6. Mechanical properties of AlCrTiVNbN/TiSiN nano multilayer films: (a) hardness and elastic modulus values; (b) H/E and H3/E2..
Figure 6. Mechanical properties of AlCrTiVNbN/TiSiN nano multilayer films: (a) hardness and elastic modulus values; (b) H/E and H3/E2..
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Figure 7. (a) Friction curve and (b) average coefficient of friction of AlCrTiVNbN/TiSiN nano multilayer films.
Figure 7. (a) Friction curve and (b) average coefficient of friction of AlCrTiVNbN/TiSiN nano multilayer films.
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Figure 8. Wear track morphologies of AlCrTiVNbN/TiSiN nano multilayer films: (a) 4 nm, (b) 5 nm, (c) 6 nm, and (d) 7 nm.
Figure 8. Wear track morphologies of AlCrTiVNbN/TiSiN nano multilayer films: (a) 4 nm, (b) 5 nm, (c) 6 nm, and (d) 7 nm.
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Figure 9. Plots of wear rate and wear volume obtained for the AlCrTiVNbN/TiSiN nano multilayer films.
Figure 9. Plots of wear rate and wear volume obtained for the AlCrTiVNbN/TiSiN nano multilayer films.
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Figure 10. Element distribution on wear tracks of the AlCrTiVNbN/TiSiN nano multilayer film with λ = 4 nm: (a) Al, (b) Ti, (c) V, (d) Nb, (e) N, (f) Si, (g) Cr, and (h) O.
Figure 10. Element distribution on wear tracks of the AlCrTiVNbN/TiSiN nano multilayer film with λ = 4 nm: (a) Al, (b) Ti, (c) V, (d) Nb, (e) N, (f) Si, (g) Cr, and (h) O.
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Table 1. Deposition parameters of the TiSiN layers.
Table 1. Deposition parameters of the TiSiN layers.
Abbr.Thickness of TiSiN Layer/nmDeposition Time/sλ/nmCycles/N
M41234250
M52465200
M63696146
M74927123
Table 2. The values of 2θ, interplanar distance, and FWMH were obtained for the films.
Table 2. The values of 2θ, interplanar distance, and FWMH were obtained for the films.
Abbr.λ/nm2θ/(°)Interplanar Distance/nmFWHM/rad
043.7950.20660.1875
M4443.9780.20570.1902
M5544.1100.20510.1913
M6644.2410.20450.1920
M7744.4250.20380.2292
Table 3. Mechanical properties of the films.
Table 3. Mechanical properties of the films.
Abbr.λ/nmAverage Hardness/GPaElastic Modulus/GPa
014.264169.796
M4415.510182.895
M5513.440176.811
M6612.345170.586
M779.4723163.350
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Yan, H.; Wang, H.; Li, X.; Dou, Z.; Liu, F. Effect of Modulation Period on the Microstructure and Tribological Properties of AlCrTiVNbN/TiSiN Nano Multilayer Films. Coatings 2025, 15, 839. https://doi.org/10.3390/coatings15070839

AMA Style

Yan H, Wang H, Li X, Dou Z, Liu F. Effect of Modulation Period on the Microstructure and Tribological Properties of AlCrTiVNbN/TiSiN Nano Multilayer Films. Coatings. 2025; 15(7):839. https://doi.org/10.3390/coatings15070839

Chicago/Turabian Style

Yan, Hongjuan, Haoran Wang, Xiaona Li, Zhaoliang Dou, and Fengbin Liu. 2025. "Effect of Modulation Period on the Microstructure and Tribological Properties of AlCrTiVNbN/TiSiN Nano Multilayer Films" Coatings 15, no. 7: 839. https://doi.org/10.3390/coatings15070839

APA Style

Yan, H., Wang, H., Li, X., Dou, Z., & Liu, F. (2025). Effect of Modulation Period on the Microstructure and Tribological Properties of AlCrTiVNbN/TiSiN Nano Multilayer Films. Coatings, 15(7), 839. https://doi.org/10.3390/coatings15070839

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