Synergistic Enhancement of Wear Resistance in Zirconium Alloys via Combined Laser Texturing and Thermal Oxidation

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Abstract Zirconium (Zr)-based alloys have great potential for orthopedic implants due to their excellent mechanical properties, corrosion resistance, and biocompatibility. However, untreated Zr-based alloys exhibit inadequate wear resistance, which limits their service life as joint prostheses. This study employed a combined surface texturing and thermal oxidation approach to enhance wear resistance. Biomimetic micro-textures were fabricated on the alloy surface via laser processing, followed by high-temperature oxidation to produce a textured ceramic coating. The influence of micro-texture diameter on anti-friction performance was systematically investigated. Results demonstrated significant improvements in hardness and wettability. Rotary friction tests were performed using a pin-on-disc tribometer. Tests revealed that ceramic-textured specimens outperformed smooth surfaces in terms of friction reduction and wear resistance. Specifically, the friction coefficient was reduced by 25.24%, with a maximum wear reduction rate of 27.7%. This study provides a novel strategy for improving the surface properties of Zr-based alloys.
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Synergistic Enhancement of Wear Resistance in Zirconium Alloys via Combined Laser Texturing and Thermal Oxidation | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Synergistic Enhancement of Wear Resistance in Zirconium Alloys via Combined Laser Texturing and Thermal Oxidation Qingchun Zheng, Jiachen Zhang, Zhitao Cao, Jiali Hao, Ya Chen, and 2 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-6869786/v1 This work is licensed under a CC BY 4.0 License Status: Under Review Version 1 posted 12 You are reading this latest preprint version Abstract Zirconium (Zr)-based alloys have great potential for orthopedic implants due to their excellent mechanical properties, corrosion resistance, and biocompatibility. However, untreated Zr-based alloys exhibit inadequate wear resistance, which limits their service life as joint prostheses. This study employed a combined surface texturing and thermal oxidation approach to enhance wear resistance. Biomimetic micro-textures were fabricated on the alloy surface via laser processing, followed by high-temperature oxidation to produce a textured ceramic coating. The influence of micro-texture diameter on anti-friction performance was systematically investigated. Results demonstrated significant improvements in hardness and wettability. Rotary friction tests were performed using a pin-on-disc tribometer. Tests revealed that ceramic-textured specimens outperformed smooth surfaces in terms of friction reduction and wear resistance. Specifically, the friction coefficient was reduced by 25.24%, with a maximum wear reduction rate of 27.7%. This study provides a novel strategy for improving the surface properties of Zr-based alloys. Laser surface texturing Zircaloy High-temperature oxidation Coefficient of friction Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 Figure 11 Introduction The hip joint is one of the most critical joints in the human body, as it supports body weight and dynamic loads while enabling a wide range of movements during daily activities (Garcia, et al.2024; Ghosh et al.2016; Gao et al.2022). A major factor limiting the lifespan of hip joint implants is the generation of wear particles due to the long-term wear of artificial materials (Revell et al.2008). The wear resistance of the friction pair materials in the joint significantly influences the in vivo service life of artificial joint prostheses after replacement. Commonly used materials for joint pairs include cobalt-chromium alloys, titanium alloys, and zirconium (Zr) alloys. Among these, as novel implant materials, Zr alloys exhibit superior biocompatibility and corrosion resistance, which helps reduce the risk of bone resorption. Additionally, incorporating elements such as niobium into Zr alloys enhances their mechanical properties and brings their elastic modulus closer to that of natural bone. However, Zr alloys have relatively low hardness, necessitating high-temperature surface oxidation treatment to improve their hardness before they can be utilized as implant materials (Nyakundi et al.2024; Toker et al.2012; Kam et al.2021; Behnam et al.2024). Meanwhile, Zr-based alloy joint pairs function as metal-on-metal prostheses, resembling “hard-on-hard” or “ceramic-on-ceramic” combinations, which exhibit excellent strength and wear resistance. Despite these advantages, reducing friction at the material interface remains a significant challenge requiring further investigation (Girija et al.2025; Chen et al.2019; Zhang Z et al.2020, Yang et al.2018; Scholes et al.2000). As evidenced by numerous scholarly studies, micro-texturing has been shown to enhance lubrication effects and reduce surface wear significantly. Surface micro-texturing is now recognized as one of the key research directions in surface engineering, with broad applications in improving the tribological properties, lubrication performance, and biocompatibility of materials. For instance, using laser surface texturing technology, Bao, Y et al. successfully fabricated biomimetic vein-like micro-textures on Al 2 O 3 /TiC ceramic surfaces (Bao et al.2023; Liang et al.2023). Their findings demonstrated that these biomimetic textures not only markedly improved the wettability of the substrate but also substantially influenced the tribological behavior of deposited coatings, leading to a significant reduction in friction coefficient compared to smooth surfaces. Similarly, Qin(2023) investigated the synergistic effects of biomimetic shark skin textures and air plasma treatment on stick-slip friction. The results confirmed that air plasma treatment and biomimetic textures effectively reduced friction forces. In another study, Oeffner et al. (2012) developed “shark skin-like” swimsuit fabrics and dynamically tested their performance. They found that this specially structured fabric could enhance swimming speed while reducing drag resistance (Zheng et al.2024; Wang et al.2024). The oxide layer formed through thermal oxidation is typically denser than that produced by anodic or plasma electrolytic oxidation, enhancing its protective capabilities. Moreover, by precisely controlling the oxidation temperature and duration, the thickness of the oxide layer can be tailored to meet specific application requirements. To develop dental implant screw materials with low elastic modulus, excellent wear resistance, high corrosion resistance, and stability, researchers have applied high-temperature oxidation treatment to medical-grade Zr-20Nb alloys, resulting in a smooth and dense oxide layer. The findings indicate that the pitting corrosion resistance of the oxidized Zr-Nb-Ti alloy is significantly superior to that of the untreated alloy. Regarding the nitriding of Zr and Zr-based alloys, experimental studies have demonstrated that pure Zr metal samples treated with gradient nitriding exhibit hardness values ranging from 492 to 1365 HV. Notably, samples treated at 800°C for 6 h demonstrate the best in vitro corrosion and wear resistance, reducing corrosion rates by 93% compared to untreated pure Zr (Xiong et al.2023; Muthuchamy et al.2020). In previous experimental studies, scholars have rarely investigated Zr-based alloys for use as orthopedic implants. Consequently, this paper proposes the combined treatment method of laser micro-texturing and high-temperature oxidation to improve the surface wear resistance of Zr alloys. This approach provides theoretical guidance for the future application of Zr-based alloys. Materials and methods Design of Micro-textures For self-protection, beetles have developed unique shell structures, with the circular pit-like surface structure exhibiting notable drag-reducing and wear-resistant properties. This study employs the circular pit structure of the beetle shell as a bionic design prototype for the design and fabrication of surface micro-textures. The microscopic morphology of the beetle shell is presented in Fig. 1 (Li et al.2023). The impact of micro-texture size on the surface performance of materials is substantial. When the diameter exceeds 1000 µm, the texture may compromise the uniformity of the lubricating film, resulting in reduced lubrication efficiency, elevated temperature, increased friction, and consequently accelerated wear and shortened service life. Conversely, when the diameter is less than 100 µm, the texture struggles to establish effective oil film load-bearing capacity, thereby diminishing lubrication performance (Liu et al. 2022 ). Therefore, appropriately selecting the micro-texture size is essential for achieving efficient lubrication and enhancing wear resistance. The design parameters of micro-textures are presented in Table 1 . To standardize variables for analysis, the texture area ratio is defined as S p , as follows: S p =S t /S (1) where S t is the single texture area, and S is the texture unit area. Table 1 Dimensional parameters of microtomography Sample Texture type Texture diameter(µm) Depth(µm) Density(%) 1 Smooth surface 0 0 0 2 Micro-textured surface 200、300、400、450、500、550、600 10 25% 3 Oxide micro-textured surface 200、300、400、450、500、550、600 10 25% Laser surface texturing The initial surface was polished to achieve a roughness value below 10 nm (without texture), which meets the ISO 7206-2 standard for articulating surfaces of metallic implants (ISO.2011).Laser processing achieves micron-level precision via non-contact etching, thereby fulfilling surface accuracy requirements (Lee et al.2016; Schmidt et al.2018). As illustrated in Fig. 3 , the energy distribution of the laser beam conforms to a Gaussian profile (Xu et al.2019; Krása et al.2013), with peak energy concentrated in the central region and gradually decreasing toward the edges. In the experiment, a YLP-F20 fiber laser marking machine was employed with the following fixed parameters: 20 marking cycles, a speed of 100 mm/s, a Q-switching frequency of 20 kHz, and an output power of 4 W. Thermal oxidation process Pre-treated Zr-based alloy samples were carefully arranged in a hot isostatic pressing (HIP) furnace, maintaining a precise distance between each sample. Subsequently, an inert gas with a predetermined oxygen concentration was introduced into the furnace at atmospheric pressure. The samples were heated at a controlled rate to approximately 600°C and held at this temperature for approximately 30 minutes. They were then cooled at a rate of 0.7°C/min to approximately 450°C, followed by natural cooling to below 200°C before removal. As a result, the Zr-based alloy material with an oxide layer on its surface was successfully synthesized (Agustianingrum et al.2020; Kumar et al.2019), as depicted in Fig. 4 . Contact angle and tribology tests Measured using the model JC2000DM contact angle measuring instrument, in order to reduce the experimental error, the measurement results are taken as the average value of the contact angle obtained from three different measurement areas. The friction tests of textured surfaces were performed using the vertical universal friction and wear testing machine MVF-1A manufactured by Jinan Hengxu Testing Machine Technology Co., Ltd. The configuration and operating principle of the testing equipment are illustrated in Fig. 5 . In the test setup, the disc sample was securely mounted in a fixture, and friction was induced between the disc and a Zr-based alloy sample via the rotational motion of a cylindrical pin. The applied load was precisely controlled through feedback from a force sensor integrated into the control system. Before each test, the disc sample was cleaned with deionized water for 5 min to ensure surface purity. Each set of experiments was repeated three times under identical conditions to guarantee the reliability and reproducibility of the data. For the friction and wear testing of artificial hip joints, bovine serum albumin (BSA) solution was chosen as the lubricant due to its composition being analogous to human body fluids and its adjustable concentration, enabling a more accurate simulation of the in vivo lubrication environment. In accordance with the YY/T 0651.1–2016 standard, the lubricant concentration was set at 30 mg/mL, prepared by mixing bovine serum albumin powder with deionized water. The test conditions are detailed in Table 2 . Table 2 Test condition parameters for oxidized specimens operating condition Specific parameters upper specimen zircaloy bottom specimen zircaloy unit area load 30.2Mpa rotation speed 60r/min running time 60min lubricant 30mg/ml bovine serum lubricant The specimens were weighed before and after the test. After the friction and wear test, the surfaces of the worn specimens were ultrasonically cleaned to remove bovine serum albumin residues and wear debris, followed by immersion in anhydrous ethanol for 15 min of ultrasonic cleaning. After cleaning, the specimens were dried and individually reweighed to determine the weight loss due to surface wear. The wear severity was assessed based on the difference in weight change, and the wear rate was subsequently calculated. For microscopic characterization of the specimens, this study primarily employed scanning electron microscopy (SEM) and a 3D surface profilometer for observation. Both instruments provided effective support across different observation scales. Results and discussion Oxidized-specimen surface hardness analysis Figure 6 illustrates the effect of laser processing on the surface hardness of the specimens. The hardness of the smooth surface is measured at 181.3HV. After laser processing, the hardness of the textured surface increases slightly, with an enhancement ranging from 5–20%. This increase in hardness can primarily be attributed to the following mechanisms: Laser processing induces rapid heating, melting, and re-solidification of the material’s surface layer. The rapid thermal cycle alters the microstructure by refining the grains and inducing residual stress, thereby improving compressive strength and wear resistance. However, due to the limited processing time and a relatively low laser power setting aimed at maintaining surface quality, the improvement in surface hardness remains modest. According to the measurement results of the surface hardness of the oxidized materials, it is evident that the surface hardness of the oxidized specimens has significantly increased, with values ranging from 1000 to 1200 HV. The primary reasons for the enhanced hardness of the oxide layer formed during the high-temperature oxidation of Zr alloys are as follows: The structural characteristics of oxides, Zr oxide, and Zr nitride, formed through the high-temperature oxidation of Zr, exhibit high hardness and excellent wear resistance. The corresponding reaction formulas are as follows: $$\:\begin{array}{c}\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:Zr+{O}_{2}=Zr{O}_{2}\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:(1)\end{array}$$ $$\:\begin{array}{c}\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:2Zr+{N}_{2}=2ZrN\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:\:(2)\end{array}$$ The crystal structure of zirconia, such as the tetragonal or monoclinic phase, is critical in enhancing the material’s hardness. Additionally, the oxide layer generally exhibits high compactness, enabling it to resist deformation under external pressure better and thus improve its hardness. At elevated temperatures, Zr oxide may undergo phase transformation, particularly from the monoclinic phase to the tetragonal phase. This transformation induces an increase in internal stress, which further contributes to the enhanced hardness of the oxide layer (Ito et al.2020; Wu et al.2020). The EDS energy spectrum analysis results for the specimen surface, conducted using a scanning electron microscope, are presented in Fig. 7 : The EDS energy spectrum analysis indicates that, following high-temperature oxidation, the atomic percentage of oxygen on the sample surface increases from 21–46%. Nitrogen rises from an undetectable level (0%) to 5%. These changes are attributed to the chemical reactions between Zr and oxygen (forming ZrO₂) and between Zr and nitrogen (forming ZrN). Both reaction products contribute to enhancing the wear resistance of Zr alloys. Furthermore, the analysis demonstrates that the atomic composition consists of 27% Zr, 46% O, and 5% N, which aligns precisely with the stoichiometric requirements for forming ZrO₂ and ZrN. In addition, the microstructural refinement during high-temperature oxidation further enhances the material’s hardness. Fine oxide and nitride particles effectively hinder dislocation motion and suppress plastic deformation, thereby contributing to the increased hardness of the material. Partial zirconia condenses on the surface to form a porous oxide layer, while some particles are dispersed within the surrounding matrix. This distribution leads to a substantial increase in the oxygen content on the surface following oxidation(Li et al.2020). Surface characteristics of oxidized microtextured specimens: roughness and wettability analysis Researchers have found that the roughness was closely related with tribological properties. To evaluate the surface roughness of textured Zr-based alloys, the indenter was carried out on the space between the micro-textures. The test data analysis of texture parameters ranging from 200 to 600 µm revealed that laser processing increased the material’s surface roughness (Ra value) from 0.05 µm to 3–4 µm. The Ra value exhibited a trend of initially increasing and subsequently decreasing, reaching its maximum value of 3.9 µm at 400 µm. Figure 8 demonstrates that the contact angle of the smooth surface is 66.07°, whereas the contact angle on the micro-textured sample surface decreases significantly, enhancing its hydrophilicity. Specifically, when the diameter of the micro-texture is 400 µm, the contact angle reaches its minimum value of 29.31°, which indicates that the micro-scale structure improves surface wettability by reducing the contact angle. Moreover, after surface oxidation treatment, the contact angle decreases further to 24.6°, significantly enhancing hydrophilicity. During the laser texturing process, finer needle-like microstructures form on the internal walls of the micro-textures. This composite morphology creates regular concave-convex structures, thereby significantly increasing surface roughness. When the texture size exceeds 400 µm (e.g., 500 and 600 µm), the surface morphology tends to become smoother. This phenomenon can be attributed to the “filling effect”, where larger structural gaps are filled or integrated, reducing microscopic irregularities and consequently decreasing surface roughness. The enhanced wettability is primarily due to the capillary force generated by the micro-pit structures, which facilitates liquid being drawn into the micro-pits, accelerating droplet spreading and reducing the contact angle. As the texture spacing increases, the droplet’s surface tension causes the liquid-gas interface to shift downward, enabling the liquid to penetrate the texture gaps more easily. This leads to a transition from the Cassie state to the Wenzel state, accompanied by a reduction in the contact angle. Experimental results of frictional wear on oxidized and textured surfaces Experimental analysis of friction coefficient This section used the pin-on-disk friction test to measure and analyze the friction coefficients resulting from relative motion. Figure 9 illustrates the friction coefficient data for both the smooth sample and the micro-textured surface. Figure 9 indicates that the smooth surface exhibits a higher and more fluctuating friction coefficient, with an average value of approximately 0.2502. The micro-textured surface demonstrates a lower and more stable friction coefficient. Specifically, when the micro-texture diameter is 400 µm, the friction coefficient reaches its minimum value of 0.1869, representing a 25.24% reduction compared to the smooth surface. This significant decrease can be attributed to the forming of a continuous fluid film under lubrication conditions, which effectively isolates the two sliding surfaces and supports the load, thereby minimizing direct metal-to-metal contact. Generally, a smaller contact angle of liquid droplets on the sliding surface correlates with better lubrication performance and a lower friction coefficient. The smooth surface has a larger contact angle and reduced hydrophilicity, leading to poorer lubricating film stability and a higher friction coefficient. From a microscopic perspective, the initial contact during the friction process occurs between the rough peaks of the upper and lower friction surfaces. As friction progresses, these rough peaks gradually wear off and accumulate on the surface, leading to scratches on the smooth surface. Furthermore, the actual contact area between the rough peaks is extremely limited, resulting in high contact stress and severe wear. When the alloy surface undergoes micro-texturing, the enhanced hydrophilicity ensures that all surface cavities are filled with liquid, forming a continuous, stable lubricating film with low shear strength. This lubricating film effectively converts solid-solid friction into solid-liquid friction, thereby improving the friction environment and reducing the friction coefficient. Additionally, the surface microstructures serve as a reservoir for the lubricant, providing timely replenishment “secondary lubrication”, capturing wear debris, and preventing three-body wear. Micro-textured surface weight loss under oxidation treatment As shown in Fig. 10 , compared to the untreated smooth surface, the mass loss after friction is significantly reduced for samples subjected to texturing and oxidation treatments. Specifically, the unprocessed smooth specimen exhibited a mass loss of 0.106 g after testing, whereas the oxidized specimen demonstrated a markedly lower mass loss of only 0.018 g. For surfaces treated solely with texturing, the mass loss ranged between 0.025 g and 0.032 g, corresponding to a wear reduction rate of 76.5%, indicating stable surface performance. Notably, specimens that underwent both texturing and oxidation treatment exhibited even lower wear mass losses, ranging from 0.013 g to 0.017 g. Several factors can account for the significant reduction in the wear volume of textured and oxidized samples. First, high-temperature oxidation generates a dense and hard ceramic oxide layer, substantially increasing surface hardness and markedly enhancing wear resistance. This robust ceramic layer is an effective wear-resistant barrier, minimizing material loss during friction. Secondly, surface micro-texturing significantly reduces wear by modifying the contact mechanics between friction pairs. Micro-textures facilitate the capture and retention of wear debris, thereby mitigating the abrasive effects of these particles on the surface. Moreover, the micro-pits created through micro-texturing serve as effective reservoirs for debris and lubricants, enabling the maintenance of a stable lubricating film during the friction process and consequently reducing wear. The tribological properties were investigated by analyzing the morphological features of surface scratches. A 3D Surface Profiler was employed to conduct precise measurements of the profile of individual wear scars, thereby enabling a deeper understanding of the wear mechanisms. As illustrated in Fig. 11 , the wear morphology of the sample surface after the friction and wear test is presented. Figure 11 presents the three-dimensional topography of the smooth Zr-based alloy surface and the micro-textured ceramic surface after the friction test. As depicted in Fig. 11 (a), extensive scratches have formed on the smooth surface due to prolonged reciprocating friction, leading to a significant degradation in surface quality. The wear marks exhibit groove-like features along the sliding direction, with the large worn area indicating severe wear. In contrast, as shown in Fig. 11 (b), the micro-textured ceramic surface exhibits no apparent wear morphology and remains relatively smooth. Furthermore, by comparing the two-dimensional profiles in Fig. 11 (a) and 11(b), it is evident that the wear depth on the micro-textured ceramic surface is considerably less than that on the smooth surface. This phenomenon can be attributed to the fact that ductile metallic materials’ adhesive and frictional properties are heavily influenced by their surface characteristics, such as hardness, chemical activity, and metallurgical compatibility. Zirconium demonstrates good metallurgical compatibility with most metals, which results in adhesive wear when Zr slides against a metal surface. However, forming oxide and nitride layers through high-temperature oxidation offers an effective solution to mitigate this issue by significantly enhancing surface hardness and reducing metallurgical compatibility with the substrate. After ceramization, the originally soft Zr alloy surface transforms into a hard ceramic layer with superior wear resistance. These findings suggest that the wear mechanism on the oxidized surface is predominantly mild abrasive wear. Conclusions In this study, a biomimetic micro-texture was designed on the surface of Zr-based alloys, and a ceramic oxide layer was formed via high-temperature oxidation to enhance their wear resistance. The main findings can be summarized as follows: 1. Bionic micro-textures in the form of circular pits were designed and fabricated on Zr-based alloy discs. After optimizing the micro-texture parameters (diameter, depth, and area ratio), fluid polishing was performed to refine the pits’ surface and interior. Subsequently, high-temperature oxidation treatment was applied, successfully forming a ZrO 2 -ZrN composite ceramic oxide layer on the textured specimen surfaces. 2. The samples’ hardness significantly increased after oxidation treatment. EDS analysis confirmed that the oxide layer primarily consisted of ZrO₂ and ZrN. The surface hardness of the textured samples increased from 200HV to a maximum of 1229HV. After laser processing, the surface roughness increased from 0.05 of the smooth surface to about 3.9. Contact angle measurements revealed that increasing the diameter of the biomimetic circular textures markedly enhanced the surface hydrophilicity, with the contact angle decreasing from 66.07° for the smooth surface to 29.21° for the textured surface and further to 24.6° after high-temperature oxidation. These findings indicate that reasonable micro-textures can achieve hydrophilic surfaces conforming to the Wenzel wetting model. 3. The effects of oxidation treatment and micro-texture parameters on anti-friction performance was examined under wet lubrication conditions using pin-on-disc friction and wear tests. The results demonstrated that the biomimetic micro-textures significantly improved the wear resistance of Zr-based alloys. Before oxidation, the friction coefficient of the textured samples ( a = 400µm, h p =10µm, S p =25%) decreased by up to 34.4% compared to the smooth samples, while the wear reduction rate increased by up to 76.4%. After oxidation, due to the enhanced hardness, the friction coefficient of the textured samples decreased by 25.24% compared to the smooth samples, and the wear reduction rate increased by up to 27.7%. Furthermore, the friction coefficient was significantly reduced after oxidation, and no obvious scratches were observed on the surface. This study proved that the proposed bionic micro-texture design, in combination with a high-temperature oxidation treatment, markedly enhanced the surface hardness, wettability, and wear resistance of the Zr-based alloy under study. These findings offer valuable insights and serve as a critical reference for material surface engineering. Declarations Data Availability Statement Datasets generated and analyzed during the current study may be obtained from the corresponding authors upon reasonable request. Declaration of Competing 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. Author Contribution Qingchun Zheng: Conceptional; Methodology; In vestigation; Supervision; Writing - Review & Editing. Jiachen Zhang: Methodology; Investigation; Data Curation ;Writing-Original draft. Zhitao Cao: Investigation; Methodology. Jiali Hao: Investigation; Methodology. 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Xu, X., Yang, X., Li, J., Pan, S., Bi, Y., Gao, Y.: Influence of laser energy distribution on laser surface microstructure processing. Optik 199, Article 163244 (2019). Krása, J.: Gaussian energy distribution of fast ions emitted by laser-produced plasmas. Appl. Surf. Sci. 272, 46–49 (2013). Agustianingrum, M.P., Lee, U., Park, N.: High-temperature oxidation behaviour of CoCrNi medium-entropy alloy. Corros. Sci. 173, Article 108755 (2020). Kumar, N.K., Das, J., Mitra, R.: Effect of Zr addition on microstructure, hardness and oxidation behavior of arc-melted and spark plasma sintered multiphase Mo-Si-B alloys. Metall. Mater. Trans. A 1–20 (2019). Ito, S., Takahashi, K., Sasaki, S.: Generation mechanism of friction anisotropy by surface texturing under boundary lubrication. Tribol. Int. 149, Article 105598 (2020). Wu, K., Yao, H., Cheng, X., Hu, J., Cao, G., Yuan, G.: Oxidation behavior and chemical evolution of architecturally arranged Zr/Si multilayer at high temperature. Surf. Coat. Technol. 399 (2020). Li, C., Chengbao, L., Hao, W., Haichao, Z., Feixiong, M., Liping, W.: A mussel-inspired delivery system for enhancing self-healing property of epoxy coatings. J. Mater. Sci. Technol. 80, Prepublish (2020). Additional Declarations No competing interests reported. Cite Share Download PDF Status: Under Review Version 1 posted Editorial decision: Revision requested 21 Sep, 2025 Reviews received at journal 29 Aug, 2025 Reviewers agreed at journal 17 Aug, 2025 Reviews received at journal 17 Aug, 2025 Reviewers agreed at journal 17 Aug, 2025 Reviews received at journal 29 Jun, 2025 Reviewers agreed at journal 29 Jun, 2025 Reviewers agreed at journal 22 Jun, 2025 Reviewers invited by journal 19 Jun, 2025 Editor assigned by journal 12 Jun, 2025 Submission checks completed at journal 12 Jun, 2025 First submitted to journal 11 Jun, 2025 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-6869786","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":474793663,"identity":"9f0793a5-e133-42a2-a662-bbab993a2ed7","order_by":0,"name":"Qingchun Zheng","email":"","orcid":"","institution":"TianjinTianjin Key Laboratory for Advanced Mechatronic System Design and Intelligent Control","correspondingAuthor":false,"prefix":"","firstName":"Qingchun","middleName":"","lastName":"Zheng","suffix":""},{"id":474793664,"identity":"9a5df30b-5c46-41dd-bc93-183d3ee0bfec","order_by":1,"name":"Jiachen Zhang","email":"","orcid":"","institution":"TianjinTianjin Key Laboratory for Advanced Mechatronic System Design and Intelligent Control","correspondingAuthor":false,"prefix":"","firstName":"Jiachen","middleName":"","lastName":"Zhang","suffix":""},{"id":474793665,"identity":"d8bc9a56-a0af-4a5b-8e94-2cee5b15cf64","order_by":2,"name":"Zhitao Cao","email":"","orcid":"","institution":"TianjinTianjin Key Laboratory for Advanced Mechatronic System Design and Intelligent Control","correspondingAuthor":false,"prefix":"","firstName":"Zhitao","middleName":"","lastName":"Cao","suffix":""},{"id":474793666,"identity":"c69fd11a-f41e-471c-9491-ed90b96da8aa","order_by":3,"name":"Jiali Hao","email":"","orcid":"","institution":"TianjinTianjin Key Laboratory for Advanced Mechatronic System Design and Intelligent Control","correspondingAuthor":false,"prefix":"","firstName":"Jiali","middleName":"","lastName":"Hao","suffix":""},{"id":474793667,"identity":"7fe5ae13-0239-409e-b597-8af0bcac3078","order_by":4,"name":"Ya Chen","email":"","orcid":"","institution":"Tianjin Bone Implant Interface Functionalization and Personalization Research Enterprise Key Laboratory","correspondingAuthor":false,"prefix":"","firstName":"Ya","middleName":"","lastName":"Chen","suffix":""},{"id":474793668,"identity":"56a731e0-b0be-47fa-860d-1bbe3c0567fd","order_by":5,"name":"Chunqiu Zhang","email":"","orcid":"","institution":"TianjinTianjin Key Laboratory for Advanced Mechatronic System Design and Intelligent Control","correspondingAuthor":false,"prefix":"","firstName":"Chunqiu","middleName":"","lastName":"Zhang","suffix":""},{"id":474793669,"identity":"9ff59b60-97d7-4c3b-b6fa-73f4f9d56028","order_by":6,"name":"Yahui Hu","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAAxUlEQVRIiWNgGAWjYBACAyBmZmCQYGBsb2x8+IEULRKMPYebjSVI0AK0RiK9TYCHGC3mEjmGnwvbLOqYZz5sA2q0k9NtIKDFckaOsfTMNqDDZie2PShgSDY2O0DIYTdyDKR5IVraDSQYDiRuI0KL8W+wlpkH2yR4iNRiBrFlBiOxWs48K7PmOSch2diTCAxkA2L8cjx5822esjp+w/bjDx9+qLCTI6iFgYHDAEwZNoBNIKgcBNgfgCl5ohSPglEwCkbBiAQA4Rk+bQV2PV8AAAAASUVORK5CYII=","orcid":"","institution":"TianjinTianjin Key Laboratory for Advanced Mechatronic System Design and Intelligent Control","correspondingAuthor":true,"prefix":"","firstName":"Yahui","middleName":"","lastName":"Hu","suffix":""}],"badges":[],"createdAt":"2025-06-11 08:53:31","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-6869786/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-6869786/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":85216856,"identity":"ae1ae958-2869-41e6-8b4e-041c24fbdb10","added_by":"auto","created_at":"2025-06-23 13:34:24","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":152998,"visible":true,"origin":"","legend":"\u003cp\u003eBeetle shell\u003c/p\u003e","description":"","filename":"image1.png","url":"https://assets-eu.researchsquare.com/files/rs-6869786/v1/d95a49142d0f1bdb8bc6c57a.png"},{"id":85218073,"identity":"4190c01d-17dc-4c97-94d4-f04741647e57","added_by":"auto","created_at":"2025-06-23 13:42:25","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":88289,"visible":true,"origin":"","legend":"\u003cp\u003eDesign of circular pit structure\u003c/p\u003e","description":"","filename":"image2.png","url":"https://assets-eu.researchsquare.com/files/rs-6869786/v1/3d803ad195986bf5b7ac11ff.png"},{"id":85216869,"identity":"75aa3b1b-9acb-4cec-bcb0-5c8096bdbebd","added_by":"auto","created_at":"2025-06-23 13:34:25","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":191663,"visible":true,"origin":"","legend":"\u003cp\u003eLaser processing principles\u003c/p\u003e","description":"","filename":"image3.png","url":"https://assets-eu.researchsquare.com/files/rs-6869786/v1/dfbc07af4b92e1b83162fbb9.png"},{"id":85216857,"identity":"f0e3a2ef-d995-48fe-bee4-54475c87dc00","added_by":"auto","created_at":"2025-06-23 13:34:24","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":332763,"visible":true,"origin":"","legend":"\u003cp\u003eSchematic illustration of the high-temperature oxidation process\u003c/p\u003e","description":"","filename":"image4.png","url":"https://assets-eu.researchsquare.com/files/rs-6869786/v1/edad569d3d331a7c6b66d517.png"},{"id":85218071,"identity":"dd164503-0006-46e6-af76-10e0b15e1ecf","added_by":"auto","created_at":"2025-06-23 13:42:24","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":155578,"visible":true,"origin":"","legend":"\u003cp\u003eSchematic diagram of contact angle measurement experiment (a) and friction experiment(b)\u003c/p\u003e","description":"","filename":"image5.png","url":"https://assets-eu.researchsquare.com/files/rs-6869786/v1/3de7739bcd8f3b5a977a9b18.png"},{"id":85216860,"identity":"46292521-3bf1-466d-bf2e-1b8998b4617c","added_by":"auto","created_at":"2025-06-23 13:34:24","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":683258,"visible":true,"origin":"","legend":"\u003cp\u003eHardness. measurement results of specimens before and after oxidation\u003c/p\u003e","description":"","filename":"image6.png","url":"https://assets-eu.researchsquare.com/files/rs-6869786/v1/4c9d4e4c2282a53eec950f44.png"},{"id":85216851,"identity":"df1a8844-ce05-45ad-af6b-84f5e15c85ed","added_by":"auto","created_at":"2025-06-23 13:34:24","extension":"png","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":190182,"visible":true,"origin":"","legend":"\u003cp\u003eEDS results on elemental content (a) and atomic percentage vs. elemental content (b) on the surface of three specimens.\u003c/p\u003e","description":"","filename":"image7.png","url":"https://assets-eu.researchsquare.com/files/rs-6869786/v1/520a2514f157e855da87eb3e.png"},{"id":85218424,"identity":"d066936e-f4e1-4eef-893d-fd6ff8808249","added_by":"auto","created_at":"2025-06-23 13:50:25","extension":"png","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":46420,"visible":true,"origin":"","legend":"\u003cp\u003eThe contact angle and surface roughness measurements for Schematic illustration(a) and analysis(b).\u003c/p\u003e","description":"","filename":"image8.png","url":"https://assets-eu.researchsquare.com/files/rs-6869786/v1/79c86014ca04049d0cc16532.png"},{"id":85216853,"identity":"f25d02aa-130d-4e83-b072-f6363c1a618e","added_by":"auto","created_at":"2025-06-23 13:34:24","extension":"png","order_by":9,"title":"Figure 9","display":"","copyAsset":false,"role":"figure","size":672043,"visible":true,"origin":"","legend":"\u003cp\u003eThe friction coefficient curves of oxidized specimens with different micro-texture geometric parameters\u003c/p\u003e","description":"","filename":"image9.png","url":"https://assets-eu.researchsquare.com/files/rs-6869786/v1/d7da61cb27509417bdcc2450.png"},{"id":85216859,"identity":"3f1b13d8-9fde-47c3-a45b-2214557a82af","added_by":"auto","created_at":"2025-06-23 13:34:24","extension":"png","order_by":10,"title":"Figure 10","display":"","copyAsset":false,"role":"figure","size":980730,"visible":true,"origin":"","legend":"\u003cp\u003eWeight loss of different micro-texture geometric parameters\u003c/p\u003e","description":"","filename":"image10.png","url":"https://assets-eu.researchsquare.com/files/rs-6869786/v1/b90bec06dadb65acb7f42f31.png"},{"id":85216909,"identity":"d7db70cf-64d8-41eb-a187-58b183baecab","added_by":"auto","created_at":"2025-06-23 13:34:26","extension":"png","order_by":11,"title":"Figure 11","display":"","copyAsset":false,"role":"figure","size":299128,"visible":true,"origin":"","legend":"\u003cp\u003ePost-friction morphology of oxidized textured surfaces: (a) wear pattern on smooth surfaces; (b) wear pattern on textured specimens with a 450μm diameter.\u003c/p\u003e","description":"","filename":"image11.png","url":"https://assets-eu.researchsquare.com/files/rs-6869786/v1/05eea01597a4f03aa82f2382.png"},{"id":85219772,"identity":"365c9fd5-885b-408b-8e63-dbe4b1c825ec","added_by":"auto","created_at":"2025-06-23 13:58:26","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":4460882,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-6869786/v1/4336854c-a5d4-4d58-a00c-c0b49989bcaa.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Synergistic Enhancement of Wear Resistance in Zirconium Alloys via Combined Laser Texturing and Thermal Oxidation","fulltext":[{"header":"Introduction","content":"\u003cp\u003eThe hip joint is one of the most critical joints in the human body, as it supports body weight and dynamic loads while enabling a wide range of movements during daily activities (Garcia, et al.2024; Ghosh et al.2016; Gao et al.2022). A major factor limiting the lifespan of hip joint implants is the generation of wear particles due to the long-term wear of artificial materials (Revell et al.2008). The wear resistance of the friction pair materials in the joint significantly influences the in vivo service life of artificial joint prostheses after replacement. Commonly used materials for joint pairs include cobalt-chromium alloys, titanium alloys, and zirconium (Zr) alloys. Among these, as novel implant materials, Zr alloys exhibit superior biocompatibility and corrosion resistance, which helps reduce the risk of bone resorption. Additionally, incorporating elements such as niobium into Zr alloys enhances their mechanical properties and brings their elastic modulus closer to that of natural bone. However, Zr alloys have relatively low hardness, necessitating high-temperature surface oxidation treatment to improve their hardness before they can be utilized as implant materials (Nyakundi et al.2024; Toker et al.2012; Kam et al.2021; Behnam et al.2024). Meanwhile, Zr-based alloy joint pairs function as metal-on-metal prostheses, resembling \u0026ldquo;hard-on-hard\u0026rdquo; or \u0026ldquo;ceramic-on-ceramic\u0026rdquo; combinations, which exhibit excellent strength and wear resistance. Despite these advantages, reducing friction at the material interface remains a significant challenge requiring further investigation (Girija et al.2025; Chen et al.2019; Zhang Z et al.2020, Yang et al.2018; Scholes et al.2000).\u003c/p\u003e \u003cp\u003eAs evidenced by numerous scholarly studies, micro-texturing has been shown to enhance lubrication effects and reduce surface wear significantly. Surface micro-texturing is now recognized as one of the key research directions in surface engineering, with broad applications in improving the tribological properties, lubrication performance, and biocompatibility of materials. For instance, using laser surface texturing technology, Bao, Y et al. successfully fabricated biomimetic vein-like micro-textures on Al\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e/TiC ceramic surfaces (Bao et al.2023; Liang et al.2023). Their findings demonstrated that these biomimetic textures not only markedly improved the wettability of the substrate but also substantially influenced the tribological behavior of deposited coatings, leading to a significant reduction in friction coefficient compared to smooth surfaces. Similarly, Qin(2023) investigated the synergistic effects of biomimetic shark skin textures and air plasma treatment on stick-slip friction. The results confirmed that air plasma treatment and biomimetic textures effectively reduced friction forces. In another study, Oeffner et al. (2012) developed \u0026ldquo;shark skin-like\u0026rdquo; swimsuit fabrics and dynamically tested their performance. They found that this specially structured fabric could enhance swimming speed while reducing drag resistance (Zheng et al.2024; Wang et al.2024).\u003c/p\u003e \u003cp\u003eThe oxide layer formed through thermal oxidation is typically denser than that produced by anodic or plasma electrolytic oxidation, enhancing its protective capabilities. Moreover, by precisely controlling the oxidation temperature and duration, the thickness of the oxide layer can be tailored to meet specific application requirements. To develop dental implant screw materials with low elastic modulus, excellent wear resistance, high corrosion resistance, and stability, researchers have applied high-temperature oxidation treatment to medical-grade Zr-20Nb alloys, resulting in a smooth and dense oxide layer. The findings indicate that the pitting corrosion resistance of the oxidized Zr-Nb-Ti alloy is significantly superior to that of the untreated alloy. Regarding the nitriding of Zr and Zr-based alloys, experimental studies have demonstrated that pure Zr metal samples treated with gradient nitriding exhibit hardness values ranging from 492 to 1365 HV. Notably, samples treated at 800\u0026deg;C for 6 h demonstrate the best in vitro corrosion and wear resistance, reducing corrosion rates by 93% compared to untreated pure Zr (Xiong et al.2023; Muthuchamy et al.2020).\u003c/p\u003e \u003cp\u003eIn previous experimental studies, scholars have rarely investigated Zr-based alloys for use as orthopedic implants. Consequently, this paper proposes the combined treatment method of laser micro-texturing and high-temperature oxidation to improve the surface wear resistance of Zr alloys. This approach provides theoretical guidance for the future application of Zr-based alloys.\u003c/p\u003e"},{"header":"Materials and methods","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003eDesign of Micro-textures\u003c/h2\u003e \u003cp\u003eFor self-protection, beetles have developed unique shell structures, with the circular pit-like surface structure exhibiting notable drag-reducing and wear-resistant properties. This study employs the circular pit structure of the beetle shell as a bionic design prototype for the design and fabrication of surface micro-textures. The microscopic morphology of the beetle shell is presented in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e(Li et al.2023).\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe impact of micro-texture size on the surface performance of materials is substantial. When the diameter exceeds 1000 \u0026micro;m, the texture may compromise the uniformity of the lubricating film, resulting in reduced lubrication efficiency, elevated temperature, increased friction, and consequently accelerated wear and shortened service life. Conversely, when the diameter is less than 100 \u0026micro;m, the texture struggles to establish effective oil film load-bearing capacity, thereby diminishing lubrication performance (Liu et al. \u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e2022\u003c/span\u003e). Therefore, appropriately selecting the micro-texture size is essential for achieving efficient lubrication and enhancing wear resistance. The design parameters of micro-textures are presented in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e. To standardize variables for analysis, the texture area ratio is defined as S\u003csub\u003ep\u003c/sub\u003e, as follows:\u003c/p\u003e \u003cp\u003eS\u003csub\u003ep\u003c/sub\u003e=S\u003csub\u003et\u003c/sub\u003e/S (1)\u003c/p\u003e \u003cp\u003ewhere S\u003csub\u003e\u003cem\u003et\u003c/em\u003e\u003c/sub\u003e is the single texture area, and S is the texture unit area.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eDimensional parameters of microtomography\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"5\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"char\" char=\".\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSample\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eTexture type\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eTexture diameter(\u0026micro;m)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003eDepth(\u0026micro;m)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003eDensity(%)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e1\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eSmooth surface\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e0\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e0\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e0\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e2\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eMicro-textured surface\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e200、300、400、450、500、550、600\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e10\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e25%\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eOxide micro-textured surface\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e200、300、400、450、500、550、600\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"char\" char=\".\" colname=\"c4\"\u003e \u003cp\u003e10\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e25%\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003c/div\u003e\n\u003ch3\u003eLaser surface texturing\u003c/h3\u003e\n\u003cp\u003eThe initial surface was polished to achieve a roughness value below 10 nm (without texture), which meets the ISO 7206-2 standard for articulating surfaces of metallic implants (ISO.2011).Laser processing achieves micron-level precision via non-contact etching, thereby fulfilling surface accuracy requirements (Lee et al.2016; Schmidt et al.2018). As illustrated in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e, the energy distribution of the laser beam conforms to a Gaussian profile (Xu et al.2019; Kr\u0026aacute;sa et al.2013), with peak energy concentrated in the central region and gradually decreasing toward the edges. In the experiment, a YLP-F20 fiber laser marking machine was employed with the following fixed parameters: 20 marking cycles, a speed of 100 mm/s, a Q-switching frequency of 20 kHz, and an output power of 4 W.\u003c/p\u003e \n\u003ch3\u003eThermal oxidation process\u003c/h3\u003e\n\u003cp\u003ePre-treated Zr-based alloy samples were carefully arranged in a hot isostatic pressing (HIP) furnace, maintaining a precise distance between each sample. Subsequently, an inert gas with a predetermined oxygen concentration was introduced into the furnace at atmospheric pressure. The samples were heated at a controlled rate to approximately 600\u0026deg;C and held at this temperature for approximately 30 minutes. They were then cooled at a rate of 0.7\u0026deg;C/min to approximately 450\u0026deg;C, followed by natural cooling to below 200\u0026deg;C before removal. As a result, the Zr-based alloy material with an oxide layer on its surface was successfully synthesized (Agustianingrum et al.2020; Kumar et al.2019), as depicted in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e.\u003c/p\u003e\n\u003ch3\u003eContact angle and tribology tests\u003c/h3\u003e\n\u003cp\u003eMeasured using the model JC2000DM contact angle measuring instrument, in order to reduce the experimental error, the measurement results are taken as the average value of the contact angle obtained from three different measurement areas.\u003c/p\u003e\u003cp\u003eThe friction tests of textured surfaces were performed using the vertical universal friction and wear testing machine MVF-1A manufactured by Jinan Hengxu Testing Machine Technology Co., Ltd. The configuration and operating principle of the testing equipment are illustrated in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e. In the test setup, the disc sample was securely mounted in a fixture, and friction was induced between the disc and a Zr-based alloy sample via the rotational motion of a cylindrical pin. The applied load was precisely controlled through feedback from a force sensor integrated into the control system. Before each test, the disc sample was cleaned with deionized water for 5 min to ensure surface purity. Each set of experiments was repeated three times under identical conditions to guarantee the reliability and reproducibility of the data.\u003c/p\u003e \u003cp\u003eFor the friction and wear testing of artificial hip joints, bovine serum albumin (BSA) solution was chosen as the lubricant due to its composition being analogous to human body fluids and its adjustable concentration, enabling a more accurate simulation of the in vivo lubrication environment. In accordance with the YY/T 0651.1\u0026ndash;2016 standard, the lubricant concentration was set at 30 mg/mL, prepared by mixing bovine serum albumin powder with deionized water. The test conditions are detailed in Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab2\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 2\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eTest condition parameters for oxidized specimens\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"2\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eoperating condition\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eSpecific parameters\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eupper specimen\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003ezircaloy\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003ebottom specimen\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003ezircaloy\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eunit area load\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e30.2Mpa\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003erotation speed\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e60r/min\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003erunning time\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e60min\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003elubricant\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e30mg/ml bovine serum lubricant\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003eThe specimens were weighed before and after the test. After the friction and wear test, the surfaces of the worn specimens were ultrasonically cleaned to remove bovine serum albumin residues and wear debris, followed by immersion in anhydrous ethanol for 15 min of ultrasonic cleaning. After cleaning, the specimens were dried and individually reweighed to determine the weight loss due to surface wear. The wear severity was assessed based on the difference in weight change, and the wear rate was subsequently calculated. For microscopic characterization of the specimens, this study primarily employed scanning electron microscopy (SEM) and a 3D surface profilometer for observation. Both instruments provided effective support across different observation scales.\u003c/p\u003e"},{"header":"Results and discussion","content":"\u003cdiv id=\"Sec8\" class=\"Section2\"\u003e \u003ch2\u003eOxidized-specimen surface hardness analysis\u003c/h2\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e illustrates the effect of laser processing on the surface hardness of the specimens. The hardness of the smooth surface is measured at 181.3HV. After laser processing, the hardness of the textured surface increases slightly, with an enhancement ranging from 5\u0026ndash;20%. This increase in hardness can primarily be attributed to the following mechanisms: Laser processing induces rapid heating, melting, and re-solidification of the material\u0026rsquo;s surface layer. The rapid thermal cycle alters the microstructure by refining the grains and inducing residual stress, thereby improving compressive strength and wear resistance. However, due to the limited processing time and a relatively low laser power setting aimed at maintaining surface quality, the improvement in surface hardness remains modest.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eAccording to the measurement results of the surface hardness of the oxidized materials, it is evident that the surface hardness of the oxidized specimens has significantly increased, with values ranging from 1000 to 1200 HV. The primary reasons for the enhanced hardness of the oxide layer formed during the high-temperature oxidation of Zr alloys are as follows:\u003c/p\u003e \u003cp\u003eThe structural characteristics of oxides, Zr oxide, and Zr nitride, formed through the high-temperature oxidation of Zr, exhibit high hardness and excellent wear resistance. The corresponding reaction formulas are as follows:\u003cdiv id=\"Equa\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equa\" name=\"EquationSource\"\u003e\n$$\\:\\begin{array}{c}\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:Zr+{O}_{2}=Zr{O}_{2}\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:(1)\\end{array}$$\u003c/div\u003e\u003c/div\u003e\u003cdiv id=\"Equb\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equb\" name=\"EquationSource\"\u003e\n$$\\:\\begin{array}{c}\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:2Zr+{N}_{2}=2ZrN\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:\\:(2)\\end{array}$$\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eThe crystal structure of zirconia, such as the tetragonal or monoclinic phase, is critical in enhancing the material\u0026rsquo;s hardness. Additionally, the oxide layer generally exhibits high compactness, enabling it to resist deformation under external pressure better and thus improve its hardness. At elevated temperatures, Zr oxide may undergo phase transformation, particularly from the monoclinic phase to the tetragonal phase. This transformation induces an increase in internal stress, which further contributes to the enhanced hardness of the oxide layer (Ito et al.2020; Wu et al.2020).\u003c/p\u003e \u003cp\u003eThe EDS energy spectrum analysis results for the specimen surface, conducted using a scanning electron microscope, are presented in Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e:\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe EDS energy spectrum analysis indicates that, following high-temperature oxidation, the atomic percentage of oxygen on the sample surface increases from 21\u0026ndash;46%. Nitrogen rises from an undetectable level (0%) to 5%. These changes are attributed to the chemical reactions between Zr and oxygen (forming ZrO₂) and between Zr and nitrogen (forming ZrN). Both reaction products contribute to enhancing the wear resistance of Zr alloys. Furthermore, the analysis demonstrates that the atomic composition consists of 27% Zr, 46% O, and 5% N, which aligns precisely with the stoichiometric requirements for forming ZrO₂ and ZrN.\u003c/p\u003e \u003cp\u003eIn addition, the microstructural refinement during high-temperature oxidation further enhances the material\u0026rsquo;s hardness. Fine oxide and nitride particles effectively hinder dislocation motion and suppress plastic deformation, thereby contributing to the increased hardness of the material. Partial zirconia condenses on the surface to form a porous oxide layer, while some particles are dispersed within the surrounding matrix. This distribution leads to a substantial increase in the oxygen content on the surface following oxidation(Li et al.2020).\u003c/p\u003e \u003c/div\u003e\n\u003ch3\u003eSurface characteristics of oxidized microtextured specimens: roughness and wettability analysis\u003c/h3\u003e\n\u003cp\u003eResearchers have found that the roughness was closely related with tribological properties. To evaluate the surface roughness of textured Zr-based alloys, the indenter was carried out on the space between the micro-textures. The test data analysis of texture parameters ranging from 200 to 600 \u0026micro;m revealed that laser processing increased the material\u0026rsquo;s surface roughness (Ra value) from 0.05 \u0026micro;m to 3\u0026ndash;4 \u0026micro;m. The Ra value exhibited a trend of initially increasing and subsequently decreasing, reaching its maximum value of 3.9 \u0026micro;m at 400 \u0026micro;m.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003e demonstrates that the contact angle of the smooth surface is 66.07\u0026deg;, whereas the contact angle on the micro-textured sample surface decreases significantly, enhancing its hydrophilicity. Specifically, when the diameter of the micro-texture is 400 \u0026micro;m, the contact angle reaches its minimum value of 29.31\u0026deg;, which indicates that the micro-scale structure improves surface wettability by reducing the contact angle. Moreover, after surface oxidation treatment, the contact angle decreases further to 24.6\u0026deg;, significantly enhancing hydrophilicity.\u003c/p\u003e \u003cp\u003eDuring the laser texturing process, finer needle-like microstructures form on the internal walls of the micro-textures. This composite morphology creates regular concave-convex structures, thereby significantly increasing surface roughness. When the texture size exceeds 400 \u0026micro;m (e.g., 500 and 600 \u0026micro;m), the surface morphology tends to become smoother. This phenomenon can be attributed to the \u0026ldquo;filling effect\u0026rdquo;, where larger structural gaps are filled or integrated, reducing microscopic irregularities and consequently decreasing surface roughness. The enhanced wettability is primarily due to the capillary force generated by the micro-pit structures, which facilitates liquid being drawn into the micro-pits, accelerating droplet spreading and reducing the contact angle. As the texture spacing increases, the droplet\u0026rsquo;s surface tension causes the liquid-gas interface to shift downward, enabling the liquid to penetrate the texture gaps more easily. This leads to a transition from the Cassie state to the Wenzel state, accompanied by a reduction in the contact angle.\u003c/p\u003e\n\u003ch3\u003eExperimental results of frictional wear on oxidized and textured surfaces\u003c/h3\u003e\n\u003cdiv id=\"Sec11\" class=\"Section2\"\u003e \u003ch2\u003eExperimental analysis of friction coefficient\u003c/h2\u003e \u003cp\u003eThis section used the pin-on-disk friction test to measure and analyze the friction coefficients resulting from relative motion. Figure\u0026nbsp;\u003cspan refid=\"Fig9\" class=\"InternalRef\"\u003e9\u003c/span\u003e illustrates the friction coefficient data for both the smooth sample and the micro-textured surface.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig9\" class=\"InternalRef\"\u003e9\u003c/span\u003e indicates that the smooth surface exhibits a higher and more fluctuating friction coefficient, with an average value of approximately 0.2502. The micro-textured surface demonstrates a lower and more stable friction coefficient. Specifically, when the micro-texture diameter is 400 \u0026micro;m, the friction coefficient reaches its minimum value of 0.1869, representing a 25.24% reduction compared to the smooth surface. This significant decrease can be attributed to the forming of a continuous fluid film under lubrication conditions, which effectively isolates the two sliding surfaces and supports the load, thereby minimizing direct metal-to-metal contact. Generally, a smaller contact angle of liquid droplets on the sliding surface correlates with better lubrication performance and a lower friction coefficient. The smooth surface has a larger contact angle and reduced hydrophilicity, leading to poorer lubricating film stability and a higher friction coefficient.\u003c/p\u003e \u003cp\u003eFrom a microscopic perspective, the initial contact during the friction process occurs between the rough peaks of the upper and lower friction surfaces. As friction progresses, these rough peaks gradually wear off and accumulate on the surface, leading to scratches on the smooth surface. Furthermore, the actual contact area between the rough peaks is extremely limited, resulting in high contact stress and severe wear. When the alloy surface undergoes micro-texturing, the enhanced hydrophilicity ensures that all surface cavities are filled with liquid, forming a continuous, stable lubricating film with low shear strength. This lubricating film effectively converts solid-solid friction into solid-liquid friction, thereby improving the friction environment and reducing the friction coefficient. Additionally, the surface microstructures serve as a reservoir for the lubricant, providing timely replenishment \u0026ldquo;secondary lubrication\u0026rdquo;, capturing wear debris, and preventing three-body wear.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec12\" class=\"Section2\"\u003e \u003ch2\u003eMicro-textured surface weight loss under oxidation treatment\u003c/h2\u003e \u003cp\u003eAs shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig10\" class=\"InternalRef\"\u003e10\u003c/span\u003e, compared to the untreated smooth surface, the mass loss after friction is significantly reduced for samples subjected to texturing and oxidation treatments. Specifically, the unprocessed smooth specimen exhibited a mass loss of 0.106 g after testing, whereas the oxidized specimen demonstrated a markedly lower mass loss of only 0.018 g. For surfaces treated solely with texturing, the mass loss ranged between 0.025 g and 0.032 g, corresponding to a wear reduction rate of 76.5%, indicating stable surface performance. Notably, specimens that underwent both texturing and oxidation treatment exhibited even lower wear mass losses, ranging from 0.013 g to 0.017 g.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eSeveral factors can account for the significant reduction in the wear volume of textured and oxidized samples. First, high-temperature oxidation generates a dense and hard ceramic oxide layer, substantially increasing surface hardness and markedly enhancing wear resistance. This robust ceramic layer is an effective wear-resistant barrier, minimizing material loss during friction.\u003c/p\u003e \u003cp\u003eSecondly, surface micro-texturing significantly reduces wear by modifying the contact mechanics between friction pairs. Micro-textures facilitate the capture and retention of wear debris, thereby mitigating the abrasive effects of these particles on the surface. Moreover, the micro-pits created through micro-texturing serve as effective reservoirs for debris and lubricants, enabling the maintenance of a stable lubricating film during the friction process and consequently reducing wear.\u003c/p\u003e \u003cp\u003eThe tribological properties were investigated by analyzing the morphological features of surface scratches. A 3D Surface Profiler was employed to conduct precise measurements of the profile of individual wear scars, thereby enabling a deeper understanding of the wear mechanisms. As illustrated in Fig.\u0026nbsp;\u003cspan refid=\"Fig11\" class=\"InternalRef\"\u003e11\u003c/span\u003e, the wear morphology of the sample surface after the friction and wear test is presented.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig11\" class=\"InternalRef\"\u003e11\u003c/span\u003e presents the three-dimensional topography of the smooth Zr-based alloy surface and the micro-textured ceramic surface after the friction test. As depicted in Fig.\u0026nbsp;\u003cspan refid=\"Fig11\" class=\"InternalRef\"\u003e11\u003c/span\u003e(a), extensive scratches have formed on the smooth surface due to prolonged reciprocating friction, leading to a significant degradation in surface quality. The wear marks exhibit groove-like features along the sliding direction, with the large worn area indicating severe wear. In contrast, as shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig11\" class=\"InternalRef\"\u003e11\u003c/span\u003e(b), the micro-textured ceramic surface exhibits no apparent wear morphology and remains relatively smooth. Furthermore, by comparing the two-dimensional profiles in Fig.\u0026nbsp;\u003cspan refid=\"Fig11\" class=\"InternalRef\"\u003e11\u003c/span\u003e(a) and 11(b), it is evident that the wear depth on the micro-textured ceramic surface is considerably less than that on the smooth surface. This phenomenon can be attributed to the fact that ductile metallic materials\u0026rsquo; adhesive and frictional properties are heavily influenced by their surface characteristics, such as hardness, chemical activity, and metallurgical compatibility. Zirconium demonstrates good metallurgical compatibility with most metals, which results in adhesive wear when Zr slides against a metal surface. However, forming oxide and nitride layers through high-temperature oxidation offers an effective solution to mitigate this issue by significantly enhancing surface hardness and reducing metallurgical compatibility with the substrate. After ceramization, the originally soft Zr alloy surface transforms into a hard ceramic layer with superior wear resistance. These findings suggest that the wear mechanism on the oxidized surface is predominantly mild abrasive wear.\u003c/p\u003e \u003c/div\u003e"},{"header":"Conclusions","content":"\u003cp\u003eIn this study, a biomimetic micro-texture was designed on the surface of Zr-based alloys, and a ceramic oxide layer was formed via high-temperature oxidation to enhance their wear resistance. The main findings can be summarized as follows:\u003c/p\u003e \u003cp\u003e1. Bionic micro-textures in the form of circular pits were designed and fabricated on Zr-based alloy discs. After optimizing the micro-texture parameters (diameter, depth, and area ratio), fluid polishing was performed to refine the pits\u0026rsquo; surface and interior. Subsequently, high-temperature oxidation treatment was applied, successfully forming a ZrO\u003csub\u003e2\u003c/sub\u003e-ZrN composite ceramic oxide layer on the textured specimen surfaces.\u003c/p\u003e\u003cp\u003e2. The samples\u0026rsquo; hardness significantly increased after oxidation treatment. EDS analysis confirmed that the oxide layer primarily consisted of ZrO₂ and ZrN. The surface hardness of the textured samples increased from 200HV to a maximum of 1229HV. After laser processing, the surface roughness increased from 0.05 of the smooth surface to about 3.9. Contact angle measurements revealed that increasing the diameter of the biomimetic circular textures markedly enhanced the surface hydrophilicity, with the contact angle decreasing from 66.07\u0026deg; for the smooth surface to 29.21\u0026deg; for the textured surface and further to 24.6\u0026deg; after high-temperature oxidation. These findings indicate that reasonable micro-textures can achieve hydrophilic surfaces conforming to the Wenzel wetting model.\u003c/p\u003e \u003cp\u003e3. The effects of oxidation treatment and micro-texture parameters on anti-friction performance was examined under wet lubrication conditions using pin-on-disc friction and wear tests. The results demonstrated that the biomimetic micro-textures significantly improved the wear resistance of Zr-based alloys. Before oxidation, the friction coefficient of the textured samples (\u003cem\u003ea\u003c/em\u003e\u0026thinsp;=\u0026thinsp;400\u0026micro;m, \u003cem\u003eh\u003c/em\u003e\u003csub\u003e\u003cem\u003ep\u003c/em\u003e\u003c/sub\u003e=10\u0026micro;m, \u003cem\u003eS\u003c/em\u003e\u003csub\u003e\u003cem\u003ep\u003c/em\u003e\u003c/sub\u003e=25%) decreased by up to 34.4% compared to the smooth samples, while the wear reduction rate increased by up to 76.4%. After oxidation, due to the enhanced hardness, the friction coefficient of the textured samples decreased by 25.24% compared to the smooth samples, and the wear reduction rate increased by up to 27.7%. Furthermore, the friction coefficient was significantly reduced after oxidation, and no obvious scratches were observed on the surface.\u003c/p\u003e\u003cp\u003eThis study proved that the proposed bionic micro-texture design, in combination with a high-temperature oxidation treatment, markedly enhanced the surface hardness, wettability, and wear resistance of the Zr-based alloy under study. These findings offer valuable insights and serve as a critical reference for material surface engineering.\u003c/p\u003e"},{"header":"Declarations","content":"\u003ch2\u003eData Availability Statement \u003c/h2\u003e\n\u003cp\u003eDatasets generated and analyzed during the current study may be obtained from the corresponding authors upon reasonable request.\u003c/p\u003e\n\u003ch2\u003eDeclaration of Competing Interest\u003c/h2\u003e\n\u003cp\u003eThe 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.\u003c/p\u003e\u003ch2\u003eAuthor Contribution\u003c/h2\u003e\u003cp\u003eQingchun Zheng: Conceptional; Methodology; In vestigation; Supervision; Writing - Review \u0026amp; Editing. Jiachen Zhang: Methodology; Investigation; Data Curation ;Writing-Original draft. Zhitao Cao: Investigation; Methodology. Jiali Hao: Investigation; Methodology. Ya Chen:Investigation. Chunqiu Zhang: Investigation; Methodology. Yahui Hu: Methodology; Formal analysis; Data Curation; Writing - Re view \u0026amp; Editing.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n\u003cli\u003eVelasquez Garcia, A., Bukowiec, L.G., Yang, L., Nishikawa, H., Fitzsimmons, J.S., Larson, A.N., Wyles, C.C.: Artificial intelligence-based three-dimensional templating for total joint arthroplasty planning: a scoping review. Int. Orthop. 48(3), 997\u0026ndash;1010 (2024)\u003c/li\u003e\n\u003cli\u003eGhosh, S., Abanteriba, S.: Status of surface modification techniques for artificial hip implants. Sci. Technol. Adv. Mater. 17, 715\u0026ndash;735 (2016).\u003c/li\u003e\n\u003cli\u003eGao, L., Lu, X., Zhang, X., Meng, Q., Jin, Z.: Lubrication modelling of artificial joint replacements: current status and future challenges. 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Heat Mass Transf. 170, 120936 (2021).\u003c/li\u003e\n\u003cli\u003eBehnam, D., Fangzhou, S., Alberto, T., et al.: Plasma defect-engineering of bulk oxygen-deficient zirconia. Acta Mater. 262, (2024).\u003c/li\u003e\n\u003cli\u003eGirija, M., Kumar, S.T.: Characterization of akermanite (AKT) and zirconia-infused PMMA bone cement composite with superior physicochemical, mechanical, and bioactive properties for enhanced orthopaedic performance. Compos. Interfaces 32(6), 817\u0026ndash;841 (2025). \u003c/li\u003e\n\u003cli\u003eChen, K., Zeng, L., Li, Z., Chai, L., Wang, Y., Chen, L.-Y., Yu, H.: Effects of laser surface alloying with Cr on microstructure and hardness of commercial purity Zr. J. Alloys Compd. 784, 1106\u0026ndash;1112 (2019).\u003c/li\u003e\n\u003cli\u003eZhang, Z., Zhang, Y., Li, X., Alexander, J., Dong, H.: An enhanced ceramic conversion treatment of Ti6Al4V alloy surface by a pre-deposited thin gold layer. J. Alloys Compd. 844, 155867 (2020).\u003c/li\u003e\n\u003cli\u003eYang, L., Ding, Y., Cheng, B., He, J., Wang, G., Wang, Y.: Investigations on femtosecond laser modified micro-textured surface with anti-friction property on bearing steel GCr15. Appl. Surf. Sci. 434, 831\u0026ndash;842 (2018)\u003c/li\u003e\n\u003cli\u003eScholes, S.C., Unsworth, A., Hall, R.M., Scott, R.: The effects of material combination and lubricant on the friction of total hip prostheses. Wear 241, 209\u0026ndash;213 (2000).\u003c/li\u003e\n\u003cli\u003eBao,Y.,Deng,J.,Wang, J.,Wang, R., Sun, Q., Wu, J.: Tribological Properties of Bi2S3/MoS2 Composite Coatings Deposited on Biomimetic Leaf Vein Textured Surfaces. Tribol Lett 71, 97 (2023).\u003c/li\u003e\n\u003cli\u003eLiang, Y., Wang, W., Zhang, Z., Xing, H., Wang, C., Zhang, Z., Gao, D.: Effect of material selection and surface texture on tribological properties of key friction pairs in water hydraulic axial piston pumps: A review. 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Sci. 141, 27 (2024).\u003c/li\u003e\n\u003cli\u003eWang, Y., Cheng, D., Ye, X., Liu, K., Yang, J., Yang, C., Hu, N.: Interfacial construction and interlayer properties of fiber metal laminates-based bionic micro\u0026ndash;nano composite structure inspired by the toe-end morphology of tree frogs. Thin-Walled Struct. 205, 112515 (2024).\u003c/li\u003e\n\u003cli\u003eXiong, X., Li, X., James, A., Zhang, Z., Dong, H.: A novel catalytic ceramic conversion treatment of Zr702 to combat wear. Materials 16(5), Article 1763 (2023).\u003c/li\u003e\n\u003cli\u003eMuthuchamy, A., Boggupalli, L.P., Yadav, D.R., Kumar, N.N., Agrawal, D.K., Annamalai, A.R.: Particulate-reinforced tungsten heavy alloy/yttria-stabilized zirconia composites sintered through spark plasma sintering. Arab. J. Sci. Eng. 45(11), 1\u0026ndash;9 (2020).\u003c/li\u003e\n\u003cli\u003eLi, X., Gao, K., Zhao, Y., Xie, X., L\u0026uuml;, X., Zhang, C., Ai, H.: Wear resistance study of bionic pitted Ni cladding layer on 7075 aluminum alloy drill pipe surface. Coatings 13(10), Article 1768 (2023).\u003c/li\u003e\n\u003cli\u003eLiu, S., Sai, Q., Wang, S., Williams, J.: Effects of laser surface texturing and lubrication on the vibrational and tribological performance of sliding contact. Lubricants 10(1), Article 10 (2022).\u003c/li\u003e\n\u003cli\u003eISO: ISO 7206\u0026ndash;2 I: Implants for Surgery\u0026mdash;Partial and Total Hip Joint Prostheses Part 2: Articulating Surfaces Made of Metallic, Ceramic and Plastics Materials, p. 5. ISO, Geneva (2011)\u003c/li\u003e\n\u003cli\u003eLee, C.-M., Woo, W.-S., Kim, D.-H., Oh, W.-J., Oh, N.-S.: Laser-assisted hybrid processes: A review. Int. J. Precis. Eng. Manuf. 17(2), 257\u0026ndash;267 (2016).\u003c/li\u003e\n\u003cli\u003eSchmidt, M., Z\u0026auml;h, M., Li, L., Duflou, J., Overmeyer, L., Vollertsen, F.: Advances in macro-scale laser processing. CIRP Ann. Manuf. Technol. 67(2), 719\u0026ndash;742 (2018).\u003c/li\u003e\n\u003cli\u003eXu, X., Yang, X., Li, J., Pan, S., Bi, Y., Gao, Y.: Influence of laser energy distribution on laser surface microstructure processing. Optik 199, Article 163244 (2019).\u003c/li\u003e\n\u003cli\u003eKr\u0026aacute;sa, J.: Gaussian energy distribution of fast ions emitted by laser-produced plasmas. Appl. Surf. Sci. 272, 46\u0026ndash;49 (2013).\u003c/li\u003e\n\u003cli\u003eAgustianingrum, M.P., Lee, U., Park, N.: High-temperature oxidation behaviour of CoCrNi medium-entropy alloy. Corros. Sci. 173, Article 108755 (2020).\u003c/li\u003e\n\u003cli\u003eKumar, N.K., Das, J., Mitra, R.: Effect of Zr addition on microstructure, hardness and oxidation behavior of arc-melted and spark plasma sintered multiphase Mo-Si-B alloys. Metall. Mater. Trans. A 1\u0026ndash;20 (2019).\u003c/li\u003e\n\u003cli\u003eIto, S., Takahashi, K., Sasaki, S.: Generation mechanism of friction anisotropy by surface texturing under boundary lubrication. Tribol. Int. 149, Article 105598 (2020).\u003c/li\u003e\n\u003cli\u003eWu, K., Yao, H., Cheng, X., Hu, J., Cao, G., Yuan, G.: Oxidation behavior and chemical evolution of architecturally arranged Zr/Si multilayer at high temperature. Surf. Coat. Technol. 399 (2020).\u003c/li\u003e\n\u003cli\u003eLi, C., Chengbao, L., Hao, W., Haichao, Z., Feixiong, M., Liping, W.: A mussel-inspired delivery system for enhancing self-healing property of epoxy coatings. J. Mater. Sci. Technol. 80, Prepublish (2020).\u003c/li\u003e\n\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"international-journal-of-mechanics-and-materials-in-design","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"","sideBox":"Learn more about [International Journal of Mechanics and Materials in Design](https://link.springer.com/journal/10999)","snPcode":"10999","submissionUrl":"https://submission.springernature.com/new-submission/10999/3","title":"International Journal of Mechanics and Materials in Design","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"Laser surface texturing, Zircaloy, High-temperature oxidation, Coefficient of friction","lastPublishedDoi":"10.21203/rs.3.rs-6869786/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-6869786/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eZirconium (Zr)-based alloys have great potential for orthopedic implants due to their excellent mechanical properties, corrosion resistance, and biocompatibility. However, untreated Zr-based alloys exhibit inadequate wear resistance, which limits their service life as joint prostheses. This study employed a combined surface texturing and thermal oxidation approach to enhance wear resistance. Biomimetic micro-textures were fabricated on the alloy surface via laser processing, followed by high-temperature oxidation to produce a textured ceramic coating. The influence of micro-texture diameter on anti-friction performance was systematically investigated. Results demonstrated significant improvements in hardness and wettability. Rotary friction tests were performed using a pin-on-disc tribometer. Tests revealed that ceramic-textured specimens outperformed smooth surfaces in terms of friction reduction and wear resistance. Specifically, the friction coefficient was reduced by 25.24%, with a maximum wear reduction rate of 27.7%. This study provides a novel strategy for improving the surface properties of Zr-based alloys.\u003c/p\u003e","manuscriptTitle":"Synergistic Enhancement of Wear Resistance in Zirconium Alloys via Combined Laser Texturing and Thermal Oxidation","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-06-23 13:34:19","doi":"10.21203/rs.3.rs-6869786/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2025-09-21T13:50:53+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-08-29T08:41:40+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"299429117656947991678861594181066362535","date":"2025-08-17T21:20:32+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-08-17T18:53:37+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"111957638687752412640148699257742332805","date":"2025-08-17T16:24:43+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2025-06-29T07:40:35+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"94183685044067013038280811813781762520","date":"2025-06-29T06:19:52+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"324949697155694000287471637179283287296","date":"2025-06-22T23:23:27+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2025-06-19T12:50:48+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2025-06-12T13:27:07+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2025-06-12T13:25:45+00:00","index":"","fulltext":""},{"type":"submitted","content":"International Journal of Mechanics and Materials in Design","date":"2025-06-11T08:39:09+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"international-journal-of-mechanics-and-materials-in-design","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"","sideBox":"Learn more about [International Journal of Mechanics and Materials in Design](https://link.springer.com/journal/10999)","snPcode":"10999","submissionUrl":"https://submission.springernature.com/new-submission/10999/3","title":"International Journal of Mechanics and Materials in Design","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"2b5c9f49-e0b5-472f-8e47-396009fb825a","owner":[],"postedDate":"June 23rd, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"under-review","subjectAreas":[],"tags":[],"updatedAt":"2025-11-20T20:38:14+00:00","versionOfRecord":[],"versionCreatedAt":"2025-06-23 13:34:19","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-6869786","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-6869786","identity":"rs-6869786","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}

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