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Article

Investigation of Tensile and Fatigue Behavior of Cr/CrN/TiCrN/TiCrCN Multilayer Films Coated on AA6063 and AZ91 Alloys by Closed-Field Unbalanced Magnetron Sputtering Process

by
Ruhi Yeşildal
1,
Sadberk Sezer
1 and
Filiz Karabudak
2,*
1
Engineering Faculty, Atatürk University, 25240 Erzurum, Turkey
2
Faculty of Engineering and Natural Sciences, Gümüşhane University, 29100 Gümüşhane, Turkey
*
Author to whom correspondence should be addressed.
Appl. Sci. 2025, 15(7), 3525; https://doi.org/10.3390/app15073525
Submission received: 14 February 2025 / Revised: 14 March 2025 / Accepted: 17 March 2025 / Published: 24 March 2025
(This article belongs to the Section Mechanical Engineering)
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Abstract

:
Despite the widespread use of Mg and Al alloys among light metals in the automobile and aviation industries, they have low tensile and fatigue strength. Therefore, in the present work, AZ91 Mg and AA6063 Al alloys were coated with a multilayer transition metal nitride film (Cr/CrN/TiCrN/TiCrCN) to increase fatigue and tensile strength. Films with Cr/CrN/TiCrN/TiCrCN microstructure architecture were synthesized on the surfaces of AZ91 Mg and AA6063 Al alloys using the CFUBMS (closed-field unbalanced magnetron sputtering) system, one of the PVD (physical vapor deposition) techniques. Films’ structural properties were analyzed by XRD, SEM, and EDAX, whereas mechanical properties were investigated using tensile and rotary bending fatigue testing machines. According to the SEM examination, the Cr, CrN, TiCrN, and TiCrCN multilayer nitride films on the two alloys have a columnar and dense microstructure. The XRD analysis detected Cr (211), CrN (111) and (200), TiN (111), (200) and (222), and TiCN (200) and (311) diffraction peaks. The Cr/CrN/TiCrN/TiCrCN multilayer coating increased the fatigue limit value of AZ91 by 11.22% from 70.26 MPa to 78.15 MPa. The fatigue limit value of AA6063 decreased by 9.79% from 79.71 MPa to 71.9 MPa. After coating, the tensile strength value of AZ91 increased from 137.89 MPa to 139.65 MPa, while the tensile strength of AA6063 decreased from 129.35 MPa to 118.16 MPa.

1. Introduction

Magnesium, aluminum, and their alloys are lightweight engineering materials that draw attention with their low densities [1,2]. They have a significant potential for use in industrial applications because of their advantages, including good thermal conductivity, high processability and superior strength/weight ratio. Due to their lightness, they stand out among metallic materials and alloys in the aerospace, automotive, and aviation industries [3,4,5]. These metals and alloys are not suitable for various structural machinery applications due to their inadequate resistance to erosion, corrosion, tribochemical wear, and fatigue under certain conditions, which limits their use [6,7,8,9]. These properties, which are related to the near-surface regions, expand the application area of metals and alloys by changing the composition and microstructure without changing the risky properties. Despite widespread industrial use, various surface coating techniques are used to increase mechanical properties such as low tensile and fatigue strength [1,2]. Numerous surface modifications have been developed for magnesium alloys to eliminate the mentioned weaknesses and increase their performance. These modifications include electroless coating [10], plasma electrolytic oxidation [11], PVD coating [12], thermal spraying [13], chemical vapor deposition (CVD), and magnetron sputtering (MS) methods [10,14,15]. In particular, the most used MS method increases homogeneity and efficiency by controlling the magnetic fields [16]. With this method, hard coatings based on titanium carbonitride (TiCN) with wear resistance are produced. In order to increase the tribological and corrosion properties of these coatings, Nb, Si, Zr, Cr, and Ag alloying can be carried out with Al and O because with this method, it is possible to obtain properties with different structures and morphologies depending on the coating conditions [15].
Light materials and their alloys including magnesium and aluminum, can also be coated with different nitride coatings, e.g., TiN, TiVN, TiCrN, TiAlN, and TiNbN, using the MS system [5,13].
Single and multiphase nitride films are used to produce wear-resistant protective coatings by depositing them on materials used for cutting and shaping tools [17,18,19,20,21]. TiN films, which provide high wear resistance and hardness, are the most commonly used industrial hard coatings to enhance mechanical properties [4,16]. The transition metal coating chromium nitride (CrN) has good corrosion and wear resistance and high hardness [22,23]. Ti–Zr–N [24], Cr–Ti–N [25], Cr–Al–N [26], Cr–W–N [27], and Cr–Si–N [28] have been developed with the objective of enhancing the chemical and mechanical features of binary films such as CrN and TiN, and numerous articles have reported superior structural, mechanical (tensile and fatigue), and tribological properties.
Guu and Hocheng (2001) examined the impacts of PVD and TiN coating on the fatigue life of AISI D2 tool steel under diverse processing parameters, including impulse current and impulse duration. The study in which surface hardness, roughness, and tensile and fatigue strength were measured determined that fatigue life increased due to increased hardness, better surface quality, and reduced superficial tensile residual stress [29]. Puchi-Cabrera et al. (2004) studied the fatigue properties of TiN coating on AISI 316L. It was found that nitride coating significantly increased both fatigue life and limit [30]. Baldissera et al. (2010) studied the fatigue behavior of AISI 302. The CrN coating considerably enhanced the base material’s fatigue resistance [31]. In their study, Baragetti et al. (2005) evaluated the fatigue strength of diverse CrN-PVD-coated specimens produced from H11 tool steel or 6082 aluminum alloy. The researchers observed a 15% improvement in fatigue limits of the coated steel samples. A decrease in fatigue limit was observed in coated aluminum samples [32]. Oskouei and Ibrahim (2011) investigated the effects of heat treatment on improving the low fatigue properties of PVD-coated 7075-T6 Al alloy. It has been found that the PVD process carried out at a high operating temperature of 450 °C significantly reduces the fatigue and tensile strength of the substrate coating system. After the final heat treatment was applied, the results of fatigue and tensile tests showed significant improvements, approaching the initial properties of the uncoated 7075-T6 [33]. Very few studies have been conducted in the literature on multilayer PVD nitride coating to improve the tribological and mechanical properties of metals and alloys. TiNbVN quaternary system multilayer nitride coating was also encountered in a recent study [13], which evaluated the mechanical and tribological properties of the Al-2024 alloy. Another study assessed the tensile and fatigue behaviors of the Ti/TiN/Ti/TiVN coating deposited on AZ91 and it was observed that the tensile and fatigue limit increased due to the nitride coating [34].
In light of the studies reviewed in the literature, it is emphasized that there is no previous study that comparatively evaluated the tensile and fatigue tests on AZ91 and AA6063 base materials coated with Cr/CrN/TiCrN/TiCrCN multilayer coating using the CFUBMS system, thus highlighting the original contribution of this study. Since it is a study aimed at increasing the strength of lightweight materials that have significant potential use in industrial applications, it is thought that it will provide innovation and guide the advanced material technologies sector.

2. Materials and Methods

2.1. Coating Production

Fatigue and tensile specimens were prepared by cutting AZ91 Mg and AA6063 Al alloys whose chemical compositions are given in Table 1. The mechanical characteristics are shown in Table 2.
Cr/CrN/TiCrN/TiCrCN multilayer nitride coatings (Figure 1) were coated by a CFUBMS system. A titanium target (99.95% pure) and a chromium target (99.95% pure), connected to a pulsed DC power supply, were used in the process of multilayer nitride coating. An ion cleaning procedure was initially performed on AZ91 and AA6063 materials at a negative voltage of 800 V for 40 min. After the above-mentioned procedure, a chromium interlayer was added to increase the adhesion between the base materials and the coating. At this stage, the base material’s negative voltage was kept at 250 V, whereas a current of 2.5 A was applied to the chromium target for 10 min. Afterward, the current applied to the chromium target was set to 3 A and the CrN layer was proceeded to. During this 15 min stage, N2 gas was supplied to ensure that the nitride phase was formed. The N2 gas flow was kept constant at 7 sccm. Then, a current of 3 A was applied to the titanium targets for 15 min. For the TiCrN layer, a current of 3 A was applied to the titanium and chromium targets during the 15 min procedure. Finally, the TiCrCN layer was proceeded to. A current of 3 A was applied to the titanium and chromium targets, while a current of 1.5 A was applied to the carbon. The constant negative voltage applied to the base materials was 50 V. During the entire coating procedure, the operating pressure was kept at 2.5 × 10−3 torr, the frequency was kept at 100 kHz, the impulse duration was adjusted at 2 μs, and the duty cycle was set at 20%.
The films’ structural properties and post-damage surface images were obtained using XRD, SEM, and EDS. Energy dispersive spectrometry (EDAX) determined the chemical composition of the Cr/CrN/TiCrN/TiCrCN multilayer nitride films. The SEM analyses of the morphology of fatigue-tensile fracture surfaces were conducted on an FEI QUANTA FEG 450 model scanning electron microscope. XRD measurements were made using a PANALYTICAL EMPYREAN model diffractometer equipped with CuKα (λ = 1.5404) at a scanning range of 20–90° and a 2°/min scanning speed. A Mahr surface profilometer determined surface roughness (Ra) values.

2.2. Fatigue and Tensile Tests of the Test Specimens

At room temperature, tensile tests were performed with a Shimadzu AGS-X universal machine at a 1.0 mm/min speed. Fatigue tests were conducted on an R.R. Moore-type rotary bending fatigue machine with a rotation speed of 3000 rpm. At least three fatigue tests were performed according to the ASTM STP 91 [35] standard at each stress level (Figure 2a). Six specimens were prepared from each of the AZ91 and AA6063 base and coated specimens in line with the ASTM E8 [36] standard (Figure 2b).

3. Research Results and Discussion

3.1. SEM and XRD Analyses

Figure 3 shows the cross-sectional morphology and topography of Cr, CrN, TiCrN, and TiCrCN multilayer nitride coatings obtained from Si glass. Figure 3 shows the synthesized multilayer coating has a columnar and dense microstructure [5,13]. The thickness of the coating acquired from the cross-sectional SEM image is 1.085 μm. The coating’s average surface roughness was measured to be Ra = 1.327 μm. The maximum roughness value was measured to be Rz = 6.43 μm.
Upon examining Figure 4, the tables presenting the EDAX values of AA6063 Al and AZ91 Mg alloys in the Cr/CrN/TiCrN/TiCrCN-coated and uncoated conditions are observed. Considering the Al and Mg alloys used in Figure 4, AA6063 alloy with deposited coating contains 5.87% C, 2.99% N, 1.64% O, 7.61% Al, 6.21% Ti, 73.9% Cr, and 1.77% Mn by weight. Coated AZ91 contains 16.21% C, 15.09% N, 13.01% O, 22.28% Cr, 25.9% Mg, 0.98% Al, and 6.53% Ti by weight.
When AZ91 Mg alloy’s XRD diffraction peaks are examined in the 2θ = 20–90° scattering range, it is seen that the diffraction peaks from interdendritic eutectic β phase (Mg17Al12) and α-Mg dendrites (matrix) are the prominent compositions [37,38,39]. XRD patterns confirm that α-Al (111), AlFeSi (222), Mg2Si (011) and (004), and CuAl2 (002) diffraction peaks were prominent compositions for AA6063 Al alloy [40,41,42,43,44]. For AA6063 and AZ91, in Cr, CrN, TiCrN, and TiCrCN multilayer nitride coatings, high-intensity diffraction peaks (211) were detected for Cr, (111) and (200) diffraction peaks were detected for CrN coating, (111), (200) and (222) diffraction peaks were detected for TiN, and (200) and (311) diffraction peaks were detected for TiCN [15,45,46,47,48,49] (Figure 5).

3.2. Fatigue Test

The increase in fatigue life with CFUBMS coating varies depending on the coating parameters, type of coating, coating layer, and even thickness. Additionally, it is possible to reduce residual stresses induced by CAD with the coating interlayer’s optimized design. The relationship between surface roughness and fatigue damage is also directly related to the initiation of cracks under fatigue conditions. In the case of fatigue, the crack begins with a burr, a notch, or a scratch on the surface. Therefore, fatigue damage is directly related to surface roughness [50,51]. The aim of the PVD system is to increase the tensile and fatigue strength of TiN, CrN, ZrN, TiAlN, TiCrN, and TiZrN-coated metals and alloys. At the same time, it is possible to further improve the mechanical properties and adhesion strength of the coatings by adding intermediate layers [52].
In that respect, scientific research has attempted to obtain better fatigue strength by improving the roughness using different methods, especially Alibeyoğlu et al. (2024), who considerably increased the fatigue strength of AZ91 with multilayer Ti/TiN/Ti/TiVN coating in their research [34].
Upon reviewing the studies in which single-layer or multilayer PVD coatings displayed different behaviors in terms of fatigue strength, TiN coatings increased fatigue life in some materials while reducing it in others. The study by Guu and Hocheng (2001) stressed that the fatigue limit increased with a significant increase in hardness, a better surface quality, and a decrease in superficial tensile residual stress in TiN-coated AISI D2 [29]. Baldissera et al. (2010) assumed that the possible surface residual stresses arising in the CrN grown by the PVD procedure, which significantly improved the fatigue resistance of AISI 302, mainly contributed to the improvement [31]. CrN coatings significantly increased fatigue life [31,32]. Nevertheless, some studies have shown that TiN and CrN coatings have reduced fatigue strength in aluminum alloys.
In their study, Baragetti et al. (2005) evaluated the fatigue strength of different CrN-coated-with-PVD specimens produced from H11 or 6082 alloys. The fatigue limit of steel-coated specimens improved in comparison with uncoated ones, and an increase of 15% was observed. However, for coated aluminum specimens, no improvement was determined in the fatigue limit compared to uncoated ones; on the contrary, a decrease was observed [32]. In the study conducted by Oskouei and Ibrahim (2011), a significant reduction of 94% in fatigue life was recorded for TiN coated on 7075-T6 alloy by PVD compared to the base material [33].
Figure 6 shows the comparative logarithmic S-N curves of AA606 and AZ91 materials and coated specimens. The load was added until the specimens broke or until 1.0 × 107 cycles were completed. The curves demonstrated a sharp decrease in the 90–70 MPa range. The fatigue strength of uncoated AZ91 was 70.26 MPa, but after nitride coating it increased to 78.15 MPa. The coating increased the fatigue limit value and life by approximately 11.22%. The fatigue strength of AA 6063 decreased from 79.71 MPa to 71.9 MPa with the Cr/CrN/TiCrN/TiCrCN coating. The nitride coating reduced the fatigue limit value by 9.79%.
In light of the studies in the literature [34], it can be resulted that the fatigue strength and life may have increased with the considerable improvement in strength and adhesion strength in AZ91 Mg alloy with the reduced surface roughness in our multilayer nitride coating. Although the present study did not measure residual stresses, it is thought that the gain in the fatigue limit of the coating substrate system originates from compressive residual stresses in the coating that prevent the propagation of fatigue cracks.
The studies by [32,33] showed that the fatigue limit was reduced when TiN and CrN single-layer coatings were applied separately. In our study, as a solution to this problem, multilayer Cr/CrN/TiCrN/TiCrCN coating was grown on the AA6063 Al alloy. However, contrary to the expected increase in fatigue, it reduced the fatigue limit. The decrease in the tensile strength of the AA6063 Al alloy with the coating in the current study is also supported by literature information. Although an adhesion investigation was not performed in our research, it is thought that the coating surface adhesion may be low. It is predicted that the crack that starts in the coating progresses rapidly and results in fracture since it is thought that there is a coating/substrate incompatibility in the ductile AA6063 material and the relatively more brittle Cr and high-strength Ti-based coating.

3.3. Fatigue Fracture Surfaces

Figure 7 shows the fracture surface images of uncoated and film-coated samples of AA6063 Al and AZ91 Mg alloys after fatigue testing. A fractographic study was carried out for uncoated and multilayered Cr/CrN/TiCrN/TiCrCN nitride-coated AZ91 and AA6063 specimens with the objective of determining the fatigue life behavior in Figure 7. In literature, fatigue cracks started in cracks, surface/subsurface defects, and notches on the specimen surface in uncoated specimens and were merged with secondary cracks as the crack progressed [37,53,54].
Mayer et al. reported similar results on the beginnings of cracks for AZ91 materials [55]. At very low cycle counts, pores act as a fatigue initiation point. The increased number of cycles controls crack beginnings at low strain amplitude values. Roughness adversely impacts fatigue life in both cases [56]. When the literature is examined, Goodenberger and Stephens (1993) concluded that fatigue cracks in AZ91-T6 alloy began from surface defects [57]. Puchi-Cabrera et al. (2004) observed that fatigue beginning in TiN-coated 316L steel nucleated from surface cracks and propagated along the coating–substrate interface. They emphasized that the fracture of the substrate was dominated by the nitride coating since the fatigue cracks began at the coating surface. It was emphasized that the increased fatigue strength of the substrate in most of the max. alternating strain range was mainly due to the residual compressive stresses in the coating and the good adhesion of the coating to the substrate. It was concluded that TiN coating on 316L effectively improves corrosion, rust and wear as well as fatigue properties [30].
Since the Cr/CrN/TiCrN/TiCrCN multilayer nitride coating displayed a columnar and dense microstructure, the fatigue limit value and strength were better in comparison with uncoated AZ91 materials because there were fewer cracks, notches, and defects on the surface that could lead to crack initiation in SEM image results. It was revealed that the fatigue fracture of the substrate coating composite was dominated by the fracture of the Cr/CrN/TiCrN/TiCrCN coating because fatigue cracks first formed on the coating’s surface and then propagated toward the substrate [30]. Additionally, the lower value of surface roughness supports the said result.
The studies by [32,33], in which TiN and CrN single-layer coatings were applied separately to Al alloys, showed that the fatigue limit decreased.
In the current study, Cr/CrN/TiCrN/TiCrCN multilayer nitride coating was applied to increase the fatigue strength of the AA603 Al alloy. Nevertheless, contrary to expectations, fatigue strength decreased with combined TiN and CrN coating. Assuming that fatigue cracks nucleate on the coating surface and rapidly propagate toward the substrate after consuming the full coating thickness provides metallographic support for the reason for the reduced fatigue strength, whereas the presence of Ti and Cr and the production of multilayer coating led to the increased fatigue strength of AZ91, causing a reduction in AA6063.

3.4. Tensile Test

Figure 8 displays the tensile test curves of the AA6063 and AZ91 multilayer coated specimens. The tensile strength and strain (mm) of the multilayer coated specimens increased in comparison with the AZ91 base material. With the coating, the tensile strength of the AZ91 alloy increased from 137.89 MPa to 139.65 MPa. When the coated and uncoated AZ91 samples were compared, the coating increased the tensile strength from 137.89 MPa to 139.65 Mpa (Table 3). The good adhesion, homogeneity, columnar, dense, and high-strength properties of the coating ensured that the coating maintained its integrity for a long time during the tensile test, resulting in an increase in tensile strength parallel to fatigue. The extended initiation time of cracks in the base material resulted in delayed plastic deformation, delayed crack initiation, nucleation, and propagation, allowing the tensile strength to increase. Consequently, it was evaluated that applying Cr/CrN/TiCrN/TiCrCN thin hard-coating film increased the tensile strength of the AZ91 Mg alloy and prolonged the crack initiation time. The above-mentioned findings show that coating applications represent an effective method to enhance the mechanical characteristics of materials such as the AZ91 Mg alloy. The said findings support similar research in the literature [34,58].
Upon reviewing the literature, in the study by [32,33], the yield and tensile strength of the aluminum alloy 7075-T6 substrate coated with 3-μm-thick TiN using PVD decreased significantly by 78% and 54%, respectively. It was thought that the high operating temperature during the deposition procedure led to a reduction in the tensile properties of coated Al 7075-T6 [32,33]. The Cr/CrN/TiCrN/TiCrCN multilayer coating reduced the maximum tensile strength value of AA6063 Al alloy from 129.35 MPa to 118.16 MPa. The presence of Ti and Cr and the production of the multilayer coating increased the fatigue and tensile strength of AZ91 in parallel while reducing them in AA6063.

3.5. Tensile Fracture Surfaces

Figure 9 displays the tensile fracture surface images of the AZ91 Mg and AA6063 Al specimens and the SEM images of the Cr/CrN/TiCrN/TiCrCN multilayer nitride coating after the tensile test fracture damage. Tensile test SEM damage images show that the tensile crack initiation starts from the coating surface in the nitride-coated AZ91 alloy. Tensile crack propagation can be characterized by more randomly oriented line-like features combined with tear ridges and secondary cracks along the interfaces. In AA6063, cracks started from the coating surface, and damage occurred with their spread toward the center of the Al layer after the coating was finished. It is thought that the reason for this is that the adhesion between the coating and the AA6063 substrate is low, and the coating peels off from the surface very quickly, initiating and accelerating the crack.

4. Conclusions

The coating thickness in multilayer nitride was measured as 1.085 μm, surface roughness as Ra = 1.327 μm, and maximum roughness value as Rz = 6.43 μm.
For AA6063 and AZ91, in the Cr, CrN, TiCrN, and TiCrCN multilayer nitride coating, high-intensity diffraction peaks (211) were detected for Cr, (111) and (200) diffraction peaks were detected for CrN coating, (111), (200), and (222) diffraction peaks were detected for TiN, and (200) and (311) diffraction peaks were detected for TiCN.
For the AZ91 base material, tensile and fatigue cracks started in notches, voids, or cracks on the surface. Cracks started from surface roughness in nitride coatings and spread and progressed in a similar way to the base material. With the multilayer hard nitride coating that fills the defects, notches, and gaps on the surface of the base material with low surface roughness, the tensile strength also increased in parallel with the fatigue strength. The fatigue limit value of the AZ91 base material increased from 69.09 MPa to 92.47 MPa. The multilayer nitride coating increased the tensile strength value of the base material from 137.89 MPa to 139.65 MPa.
In the tensile and fatigue tests of the multilayer AA6063 nitride-coated AA6063 alloy, the crack initiation probably started from the coating–aluminum layer interface due to low adhesion and spread rapidly towards the aluminum layer after consuming the coating. With the nitride coating, the fatigue strength value of the AA6063 base material decreased from 79.71 MPa to 71.9 MPa and the tensile strength value from 129.35 MPa to 118.16 MPa.
Consequently, although the Cr/CrN/TiCrN/TiCrCN multilayer coating increased the tensile and fatigue strength of the AZ91 Mg alloy, it reduced the tensile and fatigue strength of the AA6063 Al alloy. For the AZ91 alloy, multilayer nitride coatings represent an appropriate method to increase tensile and fatigue strength.

Author Contributions

Methodology, S.S. and F.K.; Investigation, R.Y. and F.K.; Resources, S.S.; Writing—original draft, R.Y.; Writing—review & editing, S.S. and F.K.; Supervision, R.Y. All authors have read and agreed to the published version of the manuscript.

Funding

This research received no external funding.

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

The original contributions presented in the study are included in the article, further inquiries can be directed to the corresponding author.

Conflicts of Interest

The authors declare no conflict of interest.

References

  1. Shaha, S.K.; Dayani, S.B.; Xue, Y.; Pang, X.; Jahed, H. Improving corrosion and corrosion-fatigue resistance of AZ31B Cast Mg alloy using combined cold spray and top coatings. Coatings 2018, 8, 443. [Google Scholar] [CrossRef]
  2. Kiryukhantsev-Korneev, P.V.; Amankeldina, Z.S.; Levashov, E.A. Effects of boron addition on the structure and properties of Cr–Al–Ti–Ncoatings obtained using the CFUBMS system. Phys. Met. Metallogr. 2020, 121, 575–581. [Google Scholar]
  3. Wuhrer, R.; Yeung, W.; Phillips, M.; McCredie, G. Study on d.c. magnetron sputter deposition of titanium aluminium nitride thin films: Effect of aluminium content on coating. Thin Solid Films 1996, 290–291, 339–342. [Google Scholar] [CrossRef]
  4. Ramadoss, R.; Kumar, N.; Pandian, R.; Dash, S.; Ravindran, T.; Arivuoli, D.; Tyagi, A. Tribological properties and deformation mechanism of TiAlN coating sliding with various counterbodies. Tribol. Int. 2013, 66, 143–149. [Google Scholar] [CrossRef]
  5. Keleş, A.; Çiçek, H.; Baran, Ö.; Totik, Y.; Efeoğlu, İ. Determining the critical loads of V and Nb doped ternary TiN-based coatings deposited using CFUBMS on steels. Surf. Coat. Technol. 2017, 332, 168–173. [Google Scholar] [CrossRef]
  6. Richman, R.; McNaughton, W. Correlation of cavitation erosion behavior with mechanical properties of metals. Wear 1990, 140, 63–82. [Google Scholar] [CrossRef]
  7. Monaghan, D.; Arnell, R. Novel PVD films by unbalanced magnetron sputtering. Vacuum 1992, 43, 77–81. [Google Scholar] [CrossRef]
  8. Altun, H.; Sen, S. The effect of DC magnetron sputtering AlN coatings on the corrosion behaviour of magnesium alloys. Surf. Coat. Technol. 2005, 197, 193–200. [Google Scholar] [CrossRef]
  9. Kalita, S.J. Microstructure and corrosion properties of diode laser melted friction stir weld of aluminum alloy 2024 T351. Appl. Surf. Sci. 2011, 257, 3985–3997. [Google Scholar] [CrossRef]
  10. Myung, H.S.; Park, Y.S.; Jung, M.J.; Hong, B.; Han, J.G. Synthesis and mechanical properties of amorphous carbon films by closed-field unbalanced magnetron sputtering. Mater. Lett. 2004, 58, 1513–1516. [Google Scholar] [CrossRef]
  11. Altun, H.; Sinici, H. Corrosion behaviour of magnesium alloys coated with TiN by cathodic arc deposition in NaCl and Na2SO4 solutions. Mater. Charact. 2008, 59, 266–270. [Google Scholar] [CrossRef]
  12. Liang, C.-L.; Cheng, G.-A.; Zheng, R.-T.; Liu, H.-P. Fabrication and performance of TiN/TiAlN nanometer modulated coatings. Thin Solid Films 2011, 520, 813–817. [Google Scholar] [CrossRef]
  13. Baran, Ö.; Keleş, A.; Çiçek, H.; Totik, Y.; Efeoğlu, İ. The mechanical and tribological properties of Ti [Nb, V] N films on the Al-2024 alloy. Surf. Coat. Technol. 2017, 332, 312–318. [Google Scholar]
  14. Hoche, H.; Groß, S.; Oechsner, M. Development of new PVD coatings for magnesium alloys with improved corrosion properties. Surf. Coat. Technol. 2014, 259, 102–108. [Google Scholar] [CrossRef]
  15. Kenzhegulov, A.; Mamaeva, A.; Panichkin, A.; Alibekov, Z.; Kshibekova, B.; Bakhytuly, N.; Wieleba, W. Comparative study of tribological and corrosion characteristics of TiCN, TiCrCN, and TiZrCN coatings. Coatings 2022, 12, 564. [Google Scholar] [CrossRef]
  16. Mattox, D.M. Handbook of Physical Vapor Deposition (PVD) Processing; Elsevier: Amsterdam, The Netherlands, 2010. [Google Scholar]
  17. Park, M.; Leyland, A.; Matthews, A. Corrosion performance of layered coatings produced by physical vapour deposition. Surf. Coat. Technol. 1990, 43–44, 481–492. [Google Scholar] [CrossRef]
  18. Parameswaran, V.R.; Immarigeon, J.P.; Nagy, D. Tribological behaviour of ion deposited ZrN coatings on mild steel substrate. Surf. Coat. Technol. 1992, 13, 251. [Google Scholar]
  19. Jehn, H. Improvement of the corrosion resistance of PVD hard coating–substrate systems. Surf. Coat. Technol. 2000, 125, 212–217. [Google Scholar] [CrossRef]
  20. Kim, G.; Lee, S.; Hahn, J.; Lee, B.; Han, J.; Lee, J. Effects of the thickness of Ti buffer layer on the mechanical properties of TiN coatings. Surf. Coat. Technol. 2003, 171, 83–90. [Google Scholar] [CrossRef]
  21. Gorokhovsky, V.; Bowman, C.; Gannon, P.; VanVorous, D.; Voevodin, A.; Rutkowski, A.; Muratore, C.; Smith, R.; Kayani, A.; Gelles, D.; et al. Tribological performance of hybrid filtered arc-magnetron coatings: Part I: Coating deposition process and basic coating properties characterization. Surf. Coat. Technol. 2006, 201, 3732–3747. [Google Scholar] [CrossRef]
  22. Vetter, J.; Knaup, R.; Dweletzki, H.; Schneider, E.; Vogler, S. Hard coatings for lubrication reduction in metal forming. Surf. Coat. Technol. 1996, 86–87, 739–747. [Google Scholar] [CrossRef]
  23. Smith. Handbook of Thin-Film Deposition Processes and Techniques; Noyes Publications: Ridg, NJ, USA, 2001; p. 629. [Google Scholar]
  24. Ramana, J.V.; Kumar, S.; David, C.; Raju, V.S. Structure, composition and microhardness of (Ti, Zr) N and (Ti, Al) N coatings prepared by DC magnetron sputtering. Mater. Lett. 2004, 58, 2553–2558. [Google Scholar]
  25. Uchida, M.; Nihira, N.; Mitsuo, A.; Toyoda, K.; Kubota, K.; Aizawa, T. Friction and wear properties of CrAlN and CrVN films deposited by cathodic arc ion plating method. Surf. Coat. Technol. 2004, 177–178, 627–630. [Google Scholar] [CrossRef]
  26. Hones, P.; Diserens, M.; Sanjinés, R.; Lévy, F. Electronic structure and mechanical properties of hard coatings from the chromium–tungsten nitride system. J. Vac. Sci. Technol. B Microelectron. Nanometer Struct. Process. Meas. Phenom. 2000, 18, 2851–2856. [Google Scholar] [CrossRef]
  27. Musil, J.; Vlček, J. Magnetron sputtering of hard nanocomposite coatings and their properties. Surf. Coat. Technol. 2001, 142–144, 557–566. [Google Scholar] [CrossRef]
  28. Barna, P.B.; Adamik, M. Growth mechanisms of polycrystalline thin films. In Science and Technology of Thin Films; World Scientific: Singapore, 1995; pp. 1–28. [Google Scholar]
  29. Guu, Y.; Hocheng, H. Improvement of fatigue life of electrical discharge machined AISI D2 tool steel by TiN coating. Mater. Sci. Eng. A 2001, 318, 155–162. [Google Scholar] [CrossRef]
  30. Puchi-Cabrera, E.S.; Matínez, F.; Herrera, I.; Berríos, J.A.; Dixit, S.; Bhat, D. On the fatigue behavior of an AISI 316L stainless steel coated with a PVD TiN deposit. Surf. Coat. Technol. 2004, 182, 276–286. [Google Scholar]
  31. Baldissera, P.; Cavalleri, S.; Marcassoli, P.; Tordini, F. Study of the effect of DCT and PVD treatments on the fatigue behaviour of AISI 302 stainless steel. Key Eng. Mater. 2010, 417–418, 49–52. [Google Scholar] [CrossRef]
  32. Baragetti, S.; Lavecchia, G.; Terranova, A. Variables affecting the fatigue resistance of PVD-coated components. Int. J. Fatigue 2005, 27, 1541–1550. [Google Scholar] [CrossRef]
  33. Oskouei, R.H.; Ibrahim, R.N. The effect of a heat treatment on improving the fatigue properties of aluminium alloy 7075-T6 coated with TiN by PVD. Procedia Eng. 2011, 10, 1936–1942. [Google Scholar] [CrossRef]
  34. Alibeyoğlu, F.; Karabudak, F.; Yeşildal, R.; Balcı, A.; Efeoğlu, İ.; Ateş, O.K. Fatigue and Tensile Behaviour of Ti + TiN + Ti + TiVN Multilayer Nitride Films Coated on AZ91 Magnesium Alloy by Closed Field Unbalanced Magnetron Sputtering. Mater. Res. Express 2024, 11, 066520. [Google Scholar] [CrossRef]
  35. ASTM STP 91; Handbook of Fatigue Testing. ASTM Committee E-9 on Fatigue. ASTM International: West Conshohocken, PA, USA, 1974; p. 566.
  36. ASTM E8/E8M-16a; Standard Test Methods for Tension Testing of Metallic Materials. ASTM International: West Conshohocken, PA, USA, 2016.
  37. Rettberg, L.H.; Jordon, J.B.; Horstemeyer, M.F.; Jones, J.W. Low-cycle fatigue behavior of die-cast mg alloys AZ91 and AM60. Met. Mater. Trans. A 2012, 43, 2260–2274. [Google Scholar] [CrossRef]
  38. Mokhtarishirazabad, M.; Boutorabi, S.; Azadi, M.; Nikravan, M. Effect of rare earth elements on high cycle fatigue behavior of AZ91 alloy. Mater. Sci. Eng. A 2013, 587, 179–184. [Google Scholar] [CrossRef]
  39. Pu, D.; Wu, S.; Yang, H.; Chen, X.; Li, J.; Feng, X.; Zheng, K.; Pan, F. Effect of Ti particles on microstructure and mechanical properties of TiP/AZ91 composites. J. Mater. Res. Technol. 2023, 22, 1362–1374. [Google Scholar] [CrossRef]
  40. Totik, Y.; Sadeler, R.; Kaymaz, I.; Gavgali, M. The effect of homogenisation treatment on cold deformations of AA 2014 and AA 6063 alloys. J. Mech. Work. Technol. 2004, 147, 60–64. [Google Scholar] [CrossRef]
  41. Leszczyńska-Madej, B.; Richert, M.; Wąsik, A.; Szafron, A. Analysis of the microstructure and selected properties of the aluminium alloys used in automotive air-conditioning systems. Metals 2017, 8, 10. [Google Scholar] [CrossRef]
  42. Thangapandian, N.; Prabu, S.B.; Padmanabhan, K.A. Effect of temperature on grain size in AA6063 aluminum alloy subjected to repetitive corrugation and straightening. Acta Metall. Sin. 2019, 32, 835–844. [Google Scholar] [CrossRef]
  43. Ali, L.F.; Kuppuswamy, N.; Soundararajan, R.; Ramkumar, K.; Sivasankaran, S. Microstructural evolutions and mechanical properties enhancement of AA 6063 alloy reinforced with Tungsten (W) nanoparticles processed by friction stir processing. Mater. Charact. 2021, 172, 110903. [Google Scholar] [CrossRef]
  44. Wang, D.S.; Wei, W.; Wei, K.X.; Alexandrov, I.V.; An, X.L.; Wang, D.D.; Liu, X.K. Grain Refinement and Mechanical Properties of Photovoltaic Frame 6063 Al Alloy with an Addition of ECAP-ed Al-5%Ti-1%B Master Alloy. JOM 2024, 76, 2027–2042. [Google Scholar] [CrossRef]
  45. Voevodin, A.; Rebholz, C.; Schneider, J.; Stevenson, P.; Matthews, A. Wear resistant composite coatings deposited by electron enhanced closed field unbalanced magnetron sputtering. Surf. Coat. Technol. 1995, 73, 185–197. [Google Scholar] [CrossRef]
  46. Aouadi, S.M.; Chladek, J.A.; Namavar, F.; Finnegan, N.; Rohde, S.L. Characterization of Ti-based nanocrystalline ternary nitride films. J. Vac. Sci. Technol. B Microelectron. Nanometer Struct. Process. Meas. Phenom. 2002, 20, 1967–1973. [Google Scholar] [CrossRef]
  47. Leonov, A.A.; Denisova, Y.A.; Denisov, V.V.; Syrtanov, M.S.; Shmakov, A.N.; Savostikov, V.M.; Teresov, A.D. Structure and properties of CrN/TiN multi-layer coatings obtained by vacuum-arc plasma-assisted deposition method. Coatings 2023, 13, 351. [Google Scholar] [CrossRef]
  48. Lyu, Y.; Zhang, Q.; Liu, Y.; Deng, X.; Sun, H.; Mo, M. Effect of Microstructure of TiN/TiCN Layer on the Structural, Mechanical and Tribological Properties of the Ti/TiN/TiCN Films. Lubricants 2023, 11, 21. [Google Scholar] [CrossRef]
  49. Sala, N.; de Figueiredo, M.R.; Franz, R.; Kainz, C.; Sánchez-López, J.; Rojas, T.; Reyes, D.F.d.L.; Colominas, C.; Abad, M.D. Microstructural and mechanical properties of TiN/CrN and TiSiN/CrN multilayer coatings deposited in an industrial-scale HiPIMS system: Effect of the Si incorporation. Surf. Coat. Technol. 2024, 494, 131461. [Google Scholar] [CrossRef]
  50. Uslu, M.E.; Onel, A.C.; Ekinci, G.; Toydemir, B.; Durdu, S.; Usta, M.; Arslan, L.C. Investigation of (Ti, V) N and TiN/VN coatings on AZ91D Mg alloys. Surf. Coat. Technol. 2015, 284, 252–257. [Google Scholar]
  51. Fattah-Alhosseini, A.; Chaharmahali, R.; Babaei, K. Effect of particles addition to solution of plasma electrolytic oxidation (PEO) on the properties of PEO coatings formed on magnesium and its alloys: A review. J. Magnes. Alloys 2020, 8, 799–818. [Google Scholar] [CrossRef]
  52. Chang, Y.-Y.; Feng, H.-Q.; Chen, C.-C. Effect of CrMoN addition on the thermal stability and cyclic impact resistance of TiVN coatings. Surf. Coat. Technol. 2023, 473, 129963. [Google Scholar] [CrossRef]
  53. Xue, Y.; Horstemeyer, M.; McDowell, D.; Elkadiri, H.; Fan, J. Microstructure-based multistage fatigue modeling of a cast AE44 magnesium alloy. Int. J. Fatigue 2004, 29, 666–676. [Google Scholar] [CrossRef]
  54. Azadi, M.; Farrahi, G.H.; Winter, G.; Eichlseder, W. Fatigue lifetime of AZ91 magnesium alloy subjected to cyclic thermal and mechanical loadings. Mater. Des. 2014, 53, 639–644. [Google Scholar] [CrossRef]
  55. Mayer, H.; Papakyriacou, M.; Zettl, B.; Stanzl-Tschegg, S. Influence of porosity on the fatigue limit of die cast magnesium and aluminium alloys. Int. J. Fatigue 2003, 25, 245–256. [Google Scholar] [CrossRef]
  56. Stanzl-Tschegg, S.; Mayer, H.; Beste, A.; Kroll, S. Fatigue and fatigue crack propagation in AlSi7Mg cast alloys under in-service loading conditions. Int. J. Fatigue 1995, 17, 149–155. [Google Scholar] [CrossRef]
  57. Goodenberger, D.L.; Stephens, R.I. Fatigue of AZ91E-T6 cast magnesium alloy. J. Eng. Mater. Technol. 1993, 115, 391–397. [Google Scholar] [CrossRef]
  58. Shugurov, A.R.; Kuzminov, E.D. The effect of multilayer architecture and Ta alloying on the mechanical performance of Ti-Al-N coatings under scratching and uniaxial tension. Metals 2021, 11, 1307. [Google Scholar] [CrossRef]
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Figure 1. Schematic image of multilayer Cr/CrN/TiCrN/TiCrCN film on AZ91 Mg and AA6063 Al alloys.
Figure 1. Schematic image of multilayer Cr/CrN/TiCrN/TiCrCN film on AZ91 Mg and AA6063 Al alloys.
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Figure 2. (a) Fatigue, (b) tensile specimens (dimensions in mm).
Figure 2. (a) Fatigue, (b) tensile specimens (dimensions in mm).
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Figure 3. Cross-sectional SEM images of multilayer Cr/CrN/TiCrN/TiCrCN films.
Figure 3. Cross-sectional SEM images of multilayer Cr/CrN/TiCrN/TiCrCN films.
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Figure 4. EDAX graphs of multilayer Cr/CrN/TiCrN/TiCrCN nitride films coated on AZ91 and AA6063.
Figure 4. EDAX graphs of multilayer Cr/CrN/TiCrN/TiCrCN nitride films coated on AZ91 and AA6063.
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Figure 5. XRD graphs of multilayer Cr/CrN/TiCrN/TiCrCN nitride films coated on AA6063 and AZ91.
Figure 5. XRD graphs of multilayer Cr/CrN/TiCrN/TiCrCN nitride films coated on AA6063 and AZ91.
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Figure 6. Specimens’ S-N curves.
Figure 6. Specimens’ S-N curves.
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Figure 7. Fatigue fracture surface images of the specimens.
Figure 7. Fatigue fracture surface images of the specimens.
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Figure 8. Specimens’ tensile curves.
Figure 8. Specimens’ tensile curves.
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Figure 9. Tensile fracture surface images of the specimens.
Figure 9. Tensile fracture surface images of the specimens.
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Table 1. Chemical composition of AZ91 and AA6063 alloys.
Table 1. Chemical composition of AZ91 and AA6063 alloys.
AlloysAlZnMnSiCuFeCrOthersTiMg
AZ918.840.610.180.020.005--- Balance
AA6063Balance0.10.10.2–0.60.10.350.10.150.10.45–0.9
Table 2. Mechanical characteristics of AZ91 and AA6063 alloys.
Table 2. Mechanical characteristics of AZ91 and AA6063 alloys.
Mechanical Characteristics/AlloysAZ91AA6063 (T6)
Modulus of Elasticity (GPa)4568
Tensile Strength (MPa)230205–245
Yield Strength (MPa)150170–210
Hardness (Brinell)6375
Elongation (%)3–712
Poisson ratio0.350.33
Table 3. Summary table of the specimens’ tensile curves.
Table 3. Summary table of the specimens’ tensile curves.
AA6063 BaseAA6063 CoatedAZ91 BaseAZ91 Coated
Stress
(Mpa)		Strain
(%)		Stress
(Mpa)		Strain
(%)		Stress
(Mpa)		Strain
(%)		Stress
(Mpa)		Strain
(%)
Average129.358.18118.167.50137.8912.83139.6512.74
Deviation5.120.353.520.144.410.454.040.36
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Yeşildal, R.; Sezer, S.; Karabudak, F. Investigation of Tensile and Fatigue Behavior of Cr/CrN/TiCrN/TiCrCN Multilayer Films Coated on AA6063 and AZ91 Alloys by Closed-Field Unbalanced Magnetron Sputtering Process. Appl. Sci. 2025, 15, 3525. https://doi.org/10.3390/app15073525

AMA Style

Yeşildal R, Sezer S, Karabudak F. Investigation of Tensile and Fatigue Behavior of Cr/CrN/TiCrN/TiCrCN Multilayer Films Coated on AA6063 and AZ91 Alloys by Closed-Field Unbalanced Magnetron Sputtering Process. Applied Sciences. 2025; 15(7):3525. https://doi.org/10.3390/app15073525

Chicago/Turabian Style

Yeşildal, Ruhi, Sadberk Sezer, and Filiz Karabudak. 2025. "Investigation of Tensile and Fatigue Behavior of Cr/CrN/TiCrN/TiCrCN Multilayer Films Coated on AA6063 and AZ91 Alloys by Closed-Field Unbalanced Magnetron Sputtering Process" Applied Sciences 15, no. 7: 3525. https://doi.org/10.3390/app15073525

APA Style

Yeşildal, R., Sezer, S., & Karabudak, F. (2025). Investigation of Tensile and Fatigue Behavior of Cr/CrN/TiCrN/TiCrCN Multilayer Films Coated on AA6063 and AZ91 Alloys by Closed-Field Unbalanced Magnetron Sputtering Process. Applied Sciences, 15(7), 3525. https://doi.org/10.3390/app15073525

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