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Article

The Mechanical Performance Enhancement of the CrN/TiAlCN Coating on GCr15 Bearing Steel by Controlling the Nitrogen Flow Rate in the Transition Layer

by
Yuchuan Cheng
,
Junxiang Li
,
Fang Liu
,
Hongjun Li
and
Nu Yan
*
School of Mechanical Engineering and Automation, Wuhan Textile University, Wuhan 430200, China
*
Author to whom correspondence should be addressed.
Coatings 2025, 15(3), 254; https://doi.org/10.3390/coatings15030254
Submission received: 21 January 2025 / Revised: 18 February 2025 / Accepted: 18 February 2025 / Published: 20 February 2025
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Abstract

:
The main focus of this work is the successful deposition of hard and wear-resistant TiAlCN coating on the surface of GCr15 bearing steel by means of magnetron sputtering technology. The phase composition of the chromium nitride transition layer was monitored by precisely controlling the nitrogen (N2) flow rate to strengthen the bonding between the TiAlCN coating and the GCr15 bearing steel surface. It was found that coating performance reached the optimal state at a N2 flow rate of 40 sccm, yielding a hardness of 23.3 GPa, a friction coefficient of only 0.27, and a wear rate of 0.19 × 10−8 mm3/N·m.

1. Introduction

GCr15 bearing steel, as a typical structural material, finds extensive utilization in the Mechanical Manufacturing, Energy and Power, and Transportation fields [1]; however, insufficient surface hardness and abrasion resistance greatly limit its wide application [2]. Hence, the enhancement of hard coatings has emerged as a commonly utilized and highly effective solution for enhancing the durability and wear durability of GCr15 bearing steel [3].
PVD and CVD are commonly employed to deposit multi-element composite coatings on substrate surfaces to compensate for their shortcomings, such as low hardness and poor durability due to corrosion and friction failure [4,5,6]. Titanium nitride (TiN)-based coatings are generally applied in industrial practice [7,8], and their performance can be further enhanced by incorporating a variety of alloying elements. Aluminum (Al) has been added to target the enhancement of coating hardness and oxidation resistance [9,10,11]; however, it increases the friction coefficient and reduces the toughness of coatings [12]. Zhang et al. [13] prepared a high-quality TiAlN coating with a hardness of 34.31 GPa based on filter cathode vacuum arc technology. Hussein et al. [14] have demonstrated that based on the arc deposition of TiAlN ceramic coating, the deposited TiAlN film presented an elastic modulus of 419.9 GPa, a surface hardness of 44.4 GPa, and an improved plastic deformation resistance in comparison to the uncoated alloy. Zeng et al. [15] have also made significant progress in preparing superhard TiAlCN coatings using the RF magnetron sputtering method. TiAlCN coatings with optimized carbon and nitrogen content display outstanding hardness that exceeds 40 GPa, which greatly broadens the potential applications of these coatings in various industrial scenarios where high hardness and wear durability are crucial requirements. The aforesaid research efforts provide valuable guidance for the development of more advanced coating technologies to meet the ever-increasing demands of modern industries.
However, due to the poor adherence of coatings to substrates, coatings easily fall off of substrates, thus greatly affecting their service life [16,17].
In order to solve this problem, multilayered nanocoatings have been developed. Multilayered nanocoatings involve the alternate deposition of at least two nanoscale materials on substrates [18,19,20], and this unique multilayered structural design can alleviate the conflict that exists between the superhard properties and the weak toughness and adhesion of coatings. When these multilayered nanocoatings come in contact with materials that possess good mutual solubility, they readily form solid solutions at the coating interface, and consequently, a composite interface is created, which is characterized by high adhesion among the constituent layers within the coating structure, and this high-adhesion interface can well assist in bettering the overall performance and durability of multilayer nanocoatings in different applications [21,22]. The adhesion between coatings and substrates is one of the pivotal assessment indexes for the performance and service life of coatings [23], and enhanced adhesion can yield the effective enhancement of coatings’ tribological and corrosion properties [24,25]. Zhang et al. [13] prepared TiAlN/TiAl multilayer coatings using filter cathode vacuum arc technology, and the coatings had a maximum adhesion strength of 89.56 N and exhibited excellent wear resistance in an oil-lubricated environment. Luo et al. [26] prepared multilayered CrN/W DLC/DLC (diamond-like carbon) coatings with improved stability and reliability and enhanced adhesion through magnetron sputtering.
Based on the above research results, the present work selected GCr15 bearing steel as the substrate to prepare a multilayered TiAlCN/CrN coating by magnetron sputtering. Chromium nitride (CrN) coatings exhibit outstanding wear and corrosion resistance [27], extremely strong adhesion, and the lowest friction coefficient [28,29]. Therefore, a CrN transition layer was first prepared on the substrate surface, and subsequently, a layer of TiAlCN was deposited on the transition layer.
XRD and SEM were used for coating microstructure detection. This study paid attention to how nitrogen content affected the coatings’ microstructure and physical properties, with the objective of examining the correlations between the surface morphology, interface structure, and hardness as well as fracture toughness. The determination of mechanical properties relied on the nanoindentation technique [30,31,32].

2. Experimental Methods

2.1. Coating Deposition

Multilayered CrN/TiAlCN coatings were deposited on the GCr15 bearing steel substrate at different N2 flow rates on a JGP-450A magnetron sputtering device (Shenyang Scientific Instrument of the Chinese Academy of Sciences, Shenyang, China).
Before the deposition process, the GCr15 bearing steel substrate (diameter = 10 mm; thickness = 1 mm) was ground flat with sandpapers of 100, 240, 800 and 1500 grade and subsequently polished with emery paste to reduce its surface roughness. The substrate was then ultrasonically decontaminated with ethanol and deionized water for 30 min to remove any debris or contaminants from the substrate surface. Finally, the substrate was dried in clean air.
The CrN buffer layer and the TiAlCN layer were both fabricated through magnetron sputtering. TiAl targets (diameter = 76.2 mm; purity = 99.9%), Cr targets (diameter = 76.2 mm; purity = 99.95%), and graphite targets (purity = 99.999%) were used as sputtering cathodes.
Before the TiAlCN coating was deposited, a CrN buffer layer approximately 500 nm in thickness was pre-deposited on the substrate. In the CrN/TiAlCN composite coating, the main function of the CrN transition layer is to increase the bonding strength between the substrate and the surface coating. The substrate was placed on a rotating base which was 10 cm away from the target. Meanwhile, two targets were both aimed at the substrate at an angle of 45 obliquely. During deposition, the rotating speed of the substrate was maintained at 5 rpm. When the vacuum was pumped down to 7 × 10−4 Pa after evacuation, an ion source was used to etch the substrate in an argon atmosphere for 5 min. This etching process removed impurities and contaminants from the substrate surface. The DC (direct current) power of the Cr target and the sputtering time were set to 200 W and 5 min, respectively, for CrN buffer layer deposition. The argon flow rate was 80 sccm, and the sputtering pressure in the vacuum chamber was kept at 0.5 Pa. Moreover, for buffer layer deposition, different N2 flow rates of 10 sccm, 20 sccm, 30 sccm, 40 sccm, and 50 sccm were used.
After the deposition of the CrN buffer layer, the sample was placed back on the rotating base. The DC powers of the TiAl target and the C target were set to 300 W and 200 W, respectively, for TiAlCN layer deposition. The flow rates of nitrogen and argon were set to 40 sccm and 80 sccm, respectively, and the working time was 90 min. After the completion of the sputtering process, the gas flow and the power were turned off. The sample was then left in the vacuum chamber to cool down gradually to room temperature. This cooling process in the vacuum environment ensured the stability and quality of the coating.

2.2. Coating Characterization

The crystal structures of the as-prepared coatings were determined using an X-ray diffractometer (PANalytical, Empyrean, The Netherlands) at 40 kV and 40 mA under Cu-Kα radiation (λ = 1.541874 Å) in a scanning range of 30°–80° with a step of 0.02° and a speed of 5°/min. The morphological characteristics of the substrate and the coatings were examined on The Carl Zeiss Sigma 500 field emission scanning electron microscope is produced by Carl Zeiss AG in Oberkochen, Germany.

2.3. Nanoindentation and Scratch Test

A nanoindenter device (Keysight G200, Santa Rosa, CA, USA) was used to examine the coatings’ hardness and Young’s modulus. The hardness results were evaluated within the range of 10%–15% of the total coating thickness, with the aim of evading the influence of such an index. Each experiment was repeated three times, and relevant calculations were conducted using the Oliver and Pharr method [33].
Scratch tests were also conducted on the Keysight G200 nanoindentation device (Santa Rosa, CA, USA) to evaluate the adhesion strengths of the TiAlCN/CrN coatings in dry environments. A Berkovich diamond tip of 20 nm in radius (MicroStar Technology, Huntsville, TX, USA) was used in the scratch test.

2.4. Sliding Friction Test

Friction experiments were performed on an MDZ-1GL high- and low-temperature friction testing machine (Jinan Yihua, Jinan, China). Si3N4 balls of 3 mm in diameter were used to achieve ball–disk friction pairs. Si3N4 balls and samples were cleaned in an ultrasonic bath with alcohol before the friction test. The friction test was carried out under a loading force of 1 N, with a duration of 5 min and a speed of 2 mm/s. After the experiment was completed, the width and depth of the scratches were obtained. The equation below explains the wear rates [34].
W S = V F × L
where WS represents the sliding wear rate (mm3/N·m), V indicates the wear volume of the coating (mm3) (V = Cross-sectional area × the scratch distance), F is the normal load (N), and L is the total friction distance (m). The scratched morphologies of the coatings were spotted with the assistance of a conventional optical microscope.

3. Results and Discussion

3.1. Coating Surface Morphology

Figure 1 illustrates the XRD patterns of the CrN coatings deposited at N2 flow rates of 10–50 sccm, revealing the XRD peak of CrN deposited on the GCr15 bearing steel surface. The major diffraction peaks at 37.600°, 43.92°, and 76.154° originated from the (1 1 1), (2 0 0), and (2 2 2) planes of the CrN coating, respectively (PDF#76-2494). The diffraction peaks at 44.386° and 64.578° appeared from the (1 1 0) and (2 0 0) planes of the substrate (Cr), respectively. With the N2 flow rate rising from 10 sccm to 30 sccm, no prominent XRD peak of CrN appeared; however, at 40 sccm, the XRD peak of the CrN phase exhibited a strong (1 1 1) orientation. Meanwhile, compared with the situation at 50 sccm, the XRD peaks shifted to the left. Through comparison with the PDF card, it was observed that the Cr2N phase had formed. At this time, the CrN and Cr2N phases coexisted. When the flow rate was further increased to 50 sccm, the diffraction peak of CrN shifted to the left and the light intensity decreased.
Figure 2 demonstrates the phase structures of the CrN/TiAlCN coatings deposited at N2 flow rates of 10–50 sccm. Due to the structural similarity between TiN and TiC, C atoms can replace some N atoms in TiN to form TiCN, and when Al/(Ti + Al) < 60%, Al atoms are capable of replacing some Ti atoms to form fcc-TiAlCN [12]. The as-deposited coatings possessed a B1-NaCl crystal structure and manifested multiple (1 1 1) and (3 1 1) orientations. When the N2 flow rate was 40 sccm, the (1 1 1) peak was the strongest and clearest and had the highest crystallinity. As TiC (PDF#05-0693) and TiN (PDF#06-0642) possess an identical crystallographic structure and similar lattice parameters, their XRD patterns were hardly distinguishable. The positions of the (1 1 1) and (3 1 1) peaks were detected between the XRD peaks of TiC and TiN, revealing the formation of a solid solution of (Ti, Al) (C, N).
The above XRD results indicate the successful deposition of the CrN and TiAlCN coatings on the GCr15 steel matrix.
Figure 3a–e display top-view SEM micrographs of CrN coatings deposited at different N2 flow rates. In the N2 flow rate range of 10–30 sccm, the coatings possessed a sheet structure, which was attached to the substrate and contained numerous white particles. This situation occurred because during the DC sputtering process, atoms continuously escaped from the target material and directly attached to the surface of the substrate without participating in the reaction. When the N2 flow rate further increased, a dense accumulation of nanoparticles occurred, the coating contained a dense columnar structure with a smooth surface, and the grain size decreased. The EDS spectrum elucidates the coatings’ chemical composition and content (Figure 3(a1–e1)). As the N2 flow continued to increase, the N content in the layer increased from 10.19 to 43.1, and when the N2 flow was 40 sccm, the N content in the layer reached the maximum value. Upon an additional increase in the N2 flow rate, the N content was reduced to 40.01, negatively affecting the coating composition (Table 1). It is noticeable in Figure 1 that Cr2N and CrN phases coexist in the coating when the N2 flow rate is 40 sccm; however, at 50 sccm, the intensity of the Cr2N peak starts to decrease. Due to the existence of Cr in both the CrN transition layer and the substrate, it was difficult to determine the Ti:N atomic ratio in the coating.
Figure 4 presents the SEM image and elemental composition of the TiAlCN coating. The TiAlCN coating deposited on the CrN transition layer has a dense structure with a smooth surface; however, white particles are not uniformly distributed in the coating, because in the DC sputtering process, the sputtered particles directly form the film. Jing et al. [35] asserted that when there are impurities in the coating, they can inhibit the growth of grains and also make the grains re-aggregate and nucleate, thus resulting in a more compact structure. Hence, the as-prepared CrN/TiAlCN coating with good surface topography can effectively eliminate surface defects that cannot be avoided by traditional surface treatments.

3.2. The Nanomechanical Characterization of the Coatings

3.2.1. Nanohardness Measurement

The hardness and elastic modulus of the nanocomposite coatings were measured by using a nanoindenter. As CrN exhibits high hardness, the depth ratio of the indenter into CrN determined the coating hardness. During the nanoindentation experiments, the depth under the maximum load was 15% of the coating depth. Figure 5 shows that the thicknesses of the CrN coating and the TiAlCN coating are 489.2 nm and 1779.4 nm, respectively, so the indentation depth selected is approximately 300 nm. Moreover, in order to acquire a more accurate hardness and elastic modulus, five different indentation points were measured on each sample, and their average was considered the final value [36]. Figure 6a gives the average values of nanohardness and the elastic modulus. With the increase in N2 content, the nanohardness first rises from 21.2 GPa (n = 10) to 23.3 GPa (n = 40), followed by a decrease to 19 GPa (n = 50), and the average elastic modulus shows a gradual increase from 238.8 GPa to 293.7 GPa. Cr2N exhibits a higher hardness versus CrN coatings. During the continuous rise in the N2 flow rate, Cr2N and CrN phases were continuously formed. When the N2 flow rate was 40 sccm, Cr2N and CrN phases coexisted in the coating; thus, the coating microstructure became dense, the residual compressive stress increased, and the grain size decreased, resulting in the highest hardness. When N2 flow continues to increase, the strength and hardness of Cr2N and CrN peaks decrease [37,38].
Figure 6b reveals the hardness and elastic modulus of the multilayered CrN/TiAlCN coatings deposited at different N2 flow rates. With the continuous rise in the N2 flow rate, both the nanohardness and the average elastic modulus gradually increased from 1.33 GPa to 5.23 GPa and from 23.4 GPa to 83.6 GPa, respectively. The change in coating hardness might result from the difference in the phase content and composition of the CrN transition layer.

3.2.2. The Scratch Behavior of the Coatings

Coating adhesion is a pivotal influencing factor in the corrosion resistance of solid particles [39]. The adhesion of the prepared CrN/TiAlCN composite coating on the GCr15 bearing steel substrate was tested by means of scratch experiments. It is noticeable from Figure 7 that a large area of the single-layered TiAlCN coating was spalling due to cracking or delamination, whereas an accumulation of the outer edge of the scratched track occurred in the multilayered CrN/TiAlCN coating. The crystal structure of the TiAlCN coating contained fcc—(Ti, Al) (C, N) (Figure 2). The huge difference in atomic size and the difference in crystal structure led to lattice mismatch and asynchronism in the crystal morphology, resulting in low film–substrate bonding strength [40]. However, there was no interface mismatch problem between the nanocrystal structure and the transition layer, which significantly increased the film–substrate bonding strength, and the transition layer served as a buffer between them. The Cr atoms in the CrN transition layer form metallic bonds with the Ti atoms and Al atoms in the TiAlCN coating. The existence of these chemical bonds can further enhance the bonding strength between the coatings and improve the overall performance of the coatings. The relatively stable transition of the lattice structure reduces lattice mismatch, improves the compatibility, and thus enhances coating–matrix binding. A similar result has also been reported in the Chinese literature [41].
Figure 7b–f demonstrate the scratch test results for the CrN transition layer at different N2 flow rates. With the gradual rise in the N2 flow rate, the scratched morphology tended to be smooth without large area shedding. This happened because the increased nitride content in the transition layer improved the matching degree between the TiAlCN coating and the substrate lattice. At a N2 flow rate of 40 sccm, the peak intensity and content of Cr2N and CrN phases in the transition layer were strongest and highest, respectively (Figure 1), indicating that coating adhesion under this condition was strongest. Moreover, at 40 sccm, the scratches were clear and complete, and no spalling and corrosion spots were detected near the scratches (Figure 7e). Also, higher hardness more effectively protects the coating from mechanical damage during frictional corrosion, a result found by Hassani et al. [42]. A study by Kato [43] propounded that high hardness could sufficiently ensure the realization of excellent wear resistance.

3.3. The Tribological Characterization of the Coatings

Figure 8 presents the frictional forces and friction coefficients of the CrN/TiAlCN coatings deposited at different N2 flow rates. The frictional force fluctuated slightly in the preliminary stage owing to the coating surface cracking, strong roughness, and the accumulation of wear debris generated from the deformation and adhesion resistance in the friction-sliding process. The friction force tended to be stable as the sliding time increased. With the rise in the N2 flow rate in the CrN transition layer, the fluctuation range of friction and the friction coefficient both gradually decreased. When the N2 flow rate was 40 sccm, the fluctuation range of friction was smallest and the friction coefficient was lowest (0.27). It can be inferred that during the friction process, adding Cr2N and CrN hard phase particles in the transition layer and embedding the coating into the softer coating increase the material’s plastic deformation, and the deformation and damage of the coating do not make the friction curve fluctuate significantly, thus reducing the coating’s friction coefficient.
According to Figure 9, which illustrates the wear rate of CrN/TiAlCN multilayer coatings under various N2 flow rates, the single-layer TiAlCN coating has the highest wear rate, while that of the multilayer coating declines as the nitride content increases in the transition layer. The N2 flow rate decreases to the lowest at 40 sccm and tends to be stable at 0.187 × 10−7 mm3/N·m, because the coating will exhibit a higher hardness upon the flow rate of the transition layer exceeding 40 sccm. The coefficient of friction is the most stable. At the same time, this also proves that the addition of the transition layer excels in reducing the coating’s wear rate.

4. Conclusions

This study aimed for successful multilayered CrN/TAlCN coating deposition on the GCr15 bearing steel surface through magnetron sputtering. The impacts of different N2 flow rates in the CrN transition layer on the crystal structures, constituent components, and mechanical and tribological properties of the coating were probed. The key findings of this work are presented below.
(1)
The addition of the CrN transition layer between the TiAlCN coating and the substrate effectively strengthened the physical properties of the composite coating.
(2)
As the N2 flow rate increased, the hardness and elastic modulus of the coating initially rose and then gradually declined. The hardness peaked at 23.3 GPa when the N2 flow rate reached 40 sccm.
(3)
The continuous rise in the N2 flow rate increased the nitride content in the CrN transition layer, making the TiAlCN coating quite compatible with the substrate.
(4)
The friction coefficient and wear rate of the CrN/TiAlCN coating decreased with the continuous rise in the N2 flow rate, and the values reached 0.27 and 0.19 × 10−7 mm3/N·m, respectively, at a N2 flow rate of 40 sccm, yielding the best performance.
The results of this experiment can be used to optimize the process parameters of magnetron sputtering, strengthen the physical properties of GCr15 bearing steel, and improve the service life of bearings.

Author Contributions

Y.C.: Investigation, Supervision, Conceptualization, Writing—original draft. J.L.: Investigation. F.L. and H.L.: Investigation, Software, Formal analysis. N.Y.: Supervision, Writing—review & editing. All authors have read and agreed to the published version of the manuscript.

Funding

This work was supported by the National Natural Science Foundation of China (no. 12402142), Natural Science Foundation of Hubei Province (no. 2024AFB235), and Hubei Provincial Department of Education Science and Technology Research Project (no. Q20221714).

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

Data are contained within the article.

Conflicts of Interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

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Figure 1. XRD patterns of CrN coatings deposited at different N2 flow rates.
Figure 1. XRD patterns of CrN coatings deposited at different N2 flow rates.
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Figure 2. XRD patterns of multilayered CrN/TiAlCN coatings deposited at different N2 flow rates.
Figure 2. XRD patterns of multilayered CrN/TiAlCN coatings deposited at different N2 flow rates.
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Figure 3. (a–e) SEM images and (a1–e1) corresponding EDS elemental mapping of CrN coatings deposited at different N2 flow rates: (a,a1) 100 sccm, (b,b1) 20 sccm, (c,c1) 30 sccm, (d,d1) 40 sccm, and (e,e1) 50 sccm.
Figure 3. (a–e) SEM images and (a1–e1) corresponding EDS elemental mapping of CrN coatings deposited at different N2 flow rates: (a,a1) 100 sccm, (b,b1) 20 sccm, (c,c1) 30 sccm, (d,d1) 40 sccm, and (e,e1) 50 sccm.
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Figure 4. (a) SEM images and (b) corresponding EDS elemental mapping of TiAlCN coatings deposited.
Figure 4. (a) SEM images and (b) corresponding EDS elemental mapping of TiAlCN coatings deposited.
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Figure 5. The thickness of the CrN coating (a) and TiAlCN coating (b).
Figure 5. The thickness of the CrN coating (a) and TiAlCN coating (b).
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Figure 6. Hardness and elastic modulus of (a) CrN and (b) CrN/TiAlCN coatings at different N2 flow rates.
Figure 6. Hardness and elastic modulus of (a) CrN and (b) CrN/TiAlCN coatings at different N2 flow rates.
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Figure 7. (a) Scratch test results for the TiAlCN coating. (b–f) Scratch test results for the multilayered CrN/TiAlCN coating.
Figure 7. (a) Scratch test results for the TiAlCN coating. (b–f) Scratch test results for the multilayered CrN/TiAlCN coating.
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Figure 8. (a) Frictional force and (b) friction coefficient of multilayered CrN/TiAlCN coatings deposited at different N2 flow rates.
Figure 8. (a) Frictional force and (b) friction coefficient of multilayered CrN/TiAlCN coatings deposited at different N2 flow rates.
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Figure 9. Wear rates of multilayered CrN/TiAlCN coatings deposited at different N2 flow rates.
Figure 9. Wear rates of multilayered CrN/TiAlCN coatings deposited at different N2 flow rates.
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Table 1. Relative contents of CrN coating elements at different N2 flow rates.
Table 1. Relative contents of CrN coating elements at different N2 flow rates.
SampleCr (at%)N (at%)
10 sccm89.8110.19
20 sccm75.3324.67
30 sccm70.6829.32
40 sccm56.943.1
50 sccm59.9940.01
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MDPI and ACS Style

Cheng, Y.; Li, J.; Liu, F.; Li, H.; Yan, N. The Mechanical Performance Enhancement of the CrN/TiAlCN Coating on GCr15 Bearing Steel by Controlling the Nitrogen Flow Rate in the Transition Layer. Coatings 2025, 15, 254. https://doi.org/10.3390/coatings15030254

AMA Style

Cheng Y, Li J, Liu F, Li H, Yan N. The Mechanical Performance Enhancement of the CrN/TiAlCN Coating on GCr15 Bearing Steel by Controlling the Nitrogen Flow Rate in the Transition Layer. Coatings. 2025; 15(3):254. https://doi.org/10.3390/coatings15030254

Chicago/Turabian Style

Cheng, Yuchuan, Junxiang Li, Fang Liu, Hongjun Li, and Nu Yan. 2025. "The Mechanical Performance Enhancement of the CrN/TiAlCN Coating on GCr15 Bearing Steel by Controlling the Nitrogen Flow Rate in the Transition Layer" Coatings 15, no. 3: 254. https://doi.org/10.3390/coatings15030254

APA Style

Cheng, Y., Li, J., Liu, F., Li, H., & Yan, N. (2025). The Mechanical Performance Enhancement of the CrN/TiAlCN Coating on GCr15 Bearing Steel by Controlling the Nitrogen Flow Rate in the Transition Layer. Coatings, 15(3), 254. https://doi.org/10.3390/coatings15030254

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