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Article

Synthesis and Characterization of Titanium Layer with Fiber-like Morphology on HDPE by Plasma Treatment

by
Erick Yair Vargas-Oliva
1,
Carolina Hernández-Navarro
2,
Violeta Guzman-Ayon
3,
María del Pilar Jadige Ceballos-Muez
3,
Ernesto David García-Bustos
4,*,
Marco Antonio Doñu-Ruiz
5,
Noé López-Perrusquia
5,*,
Martin Flores-Martínez
6 and
Stephen Muhl-Saunders
7
1
Doctorado en Ciencia de Materiales, Universidad Politécnica del Valle de México, Tultitlán 54910, Estado de México, Mexico
2
División de Estudios de Posgrado e Investigación, Tecnológico Nacional de México, Instituto Tecnológico de Roque, Carretera Celaya, Celaya 38110, Guanajuato, Mexico
3
Instituto Tecnológico y de Estudios Superiores de Occidente, Tlaquepaque 45520, Jalisco, Mexico
4
SECIHTI, Universidad Politécnica del Valle de México, Tultitlán 54910, Estado de México, Mexico
5
División de Ingeniería Industrial, Grupo de Ciencia e Ingeniería de Materiales, Universidad Politécnica del Valle de México, Tultitlán 54910, Estado de México, Mexico
6
Departamento de Ingeniería de Proyectos, Centro Universitario de Ciencias Exactas e Ingenierías (CUCEI), Universidad de Guadalajara, Guadalajara 44430, Jalisco, Mexico
7
Departamento de Instituto de Investigaciones en Materiales, Universidad Nacional Autónoma de México, Ciudad de México 04510, Mexico
*
Authors to whom correspondence should be addressed.
Coatings 2025, 15(9), 995; https://doi.org/10.3390/coatings15090995
Submission received: 8 August 2025 / Revised: 19 August 2025 / Accepted: 21 August 2025 / Published: 27 August 2025
(This article belongs to the Special Issue Mechanical Properties and Tribological Behavior of Alloy/Coatings, 2nd Edition)
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Abstract

High-density polyethylene (HDPE) is widely used for different applications, but its low resistance to ultraviolet radiation, plastic deformation, chemical stability, and wear re-sistance limits its use in high-demand work environments. Modifying of the surface characteristics could improve the work efficiency of the parts exposed to an aggressive environment. Plasma treatments change the surface characteristics with deposition of a coating or by modifying the surface’s energy, varying the surface properties. This study presents the mechanical and tribological properties of a titanium (Ti) layer with fiber-like morphology produced on HDPE surfaces by plasma treatment involving plasma etching and the deposition of Ti atoms, through DC magnetron sputtering. On the HDPE substrates grew up Ti layer with fibers-like morphology with a diameter of 1.6 ± 0.44 μm. These fibers were elemental composed by 91.5 ± 0.9% Ti and 8.5 ± 0.6% O with α-Ti phase combined with HDPE crystalline structure. The Ti coating increased the hardness of the substrate and showed a good adhesion to HDPE surface. During the sliding test, the Ti layer with fiber-like morphology exhibited plastic deformation and debris accumulation, leading to the formation of a tribolayer without layer detachment. Notably, no detachment of the layer was observed, effectively protected the polymer surface, and enhanced its performance for tribological applications.

Graphical Abstract

1. Introduction

The Polyethylene-based materials, such as high-density polyethylene (HDPE) and ultra-high molecular weight polyethylene (UHMWPE), are commonly used in several applications. Although UHMWPE offers superior mechanical and tribological properties compared to HDPE, it poses challenges in production through injection molding or extrusion [1,2,3]. Consequently, HDPE remains continuously employed in packing, food, pipet, medical, automotive among other industry fields [4,5,6]. The sliding wear performance of thermoplastic polymers is typically correlate with their low coefficient of friction (CoF), self-lubrication property and beneficial thermomechanical properties, among many experimental factors such as surface roughness and applied surface pressure [7]. In order to overcome the intrinsic mechanical and tribological shortcomings of HDPE, improvements can be achieved either by embedding reinforcing particles or fibers during the injection molding process [8,9,10,11], and by modifying its surface characteristics through various post-processing techniques. These approaches are intended to improve the material’s surface behavior under high-performance or demanding operational environments. On this regard, improvements in the mechanical, electrical, catalytic, and tribological properties of the HDPE surfaces directly impact the life-time of the parts, work environment, and human health, especially when these are exposed to a high-demand work environment, causing fractures of the system parts due to the polymer degradation [12].
Surface morphology plays a critical role in the performance of polymers in tribosystems, where interactions with the environment depend on factors such as roughness, porosity, geometry, and effective surface area. Modifying the surface properties of HDPE is achieved by altering and controlling the surface characteristics, which can change the chemical stability, electric resistance, plastic deformation, wear rate, particle liberation and coefficient of friction properties, improving its efficiency of a high demand operation. Plasma processes modify the surfaces characteristics bombarding the surfaces of the substrate, to variety the surfaces energy, or a target of specific material to liberate atoms that despite on the substrate in a controlled atmosphere produces a coating with specific characteristics, changing the surface properties [13,14,15]. The surface morphology is an important factor for the efficiency of the polymer in a tribosystem due to the relation between the environment and the surfaces, which is a function of the roughness, porosity, geometry, area, and other surface factors. For that, the surfaces treatments used to modify the mechanical, electrical, tribological and biomedical properties of the parts includes the study, modification, and application of the surfaces morphology [13,14,16]. Among plasma treatments, etching and deposition of a thin-film on the substrate are the most common methods for modifying polymer the surfaces characteristics. These characteristics depend on various plasma operation factors, such as energy, density, ion-ized and neutral species of the plasma and the characteristics of the polymer itself, such as molecular size, polymer chain length, elemental composition, density, and others [17,18,19,20,21,22].
However, although the deposition of metallic layer on a polymer surfaces is complicated due to their inherently low surface polarity, causing a low addition of the metallic layers, the etching process increased the surfaces energy of the polymer substrate, improving the adhesion of the layers [23,24,25,26]. Titanium (Ti) and its alloys are well-established materials used for a wide range of applications, due to their inertness and the spontaneous formation of a stable titanium oxide (TiO2) layer, which imparts excellent mechanical and tribological [27,28,29]. The deposition of Ti layers can thus improve the protection, adhesion, optical, catalytic, electrical, biomedical, mechanical and tribological properties of the polymeric substrates. Moreover, Ti nano- and microstructures have been utilized to produce anatase and rutile phases of TiO2 via post-deposition treatments for use in solar cells, biomedical devices, hydrogen fuel cells, and other advanced technologies [29,30,31,32,33]. For that some Ti fiber applications have been reported: Liu et al. [34] reported the use of Ti fiber in polymer electrolyte membrane (PEM) water electrolyzes for power-to-gas applications, Takizawa et al. [35] employed Ti fibers as a support, forming a scaffold-like morphology, and Kotha et al. [36] reported the use of Ti fibers in the Acrylic bone cements reinforcement to be used in total joint arthroplasties, among other applications.
In this regard, this work presents initial findings on the morphology, elemental and crystalline structure characteristics of the Ti fiber-like morphology produced by a DC-magnetron sputtering plasma process on HDPE surfaces, as well as the resulting and its mechanical and tribological properties. The plasma treatment involved an initial surface etching operation of the HDPE surfaces, followed by the deposition of Ti atoms, leading to Ti layer formation with a fiber-like morphology on the HDPE surface. The formation of a Ti layer with a fiber-like morphology could increase the use of HDPE in the osseointegration and catalytic application.

2. Materials and Methods

The HDPE samples, with dimensions of 38.1 mm (1.5 inches) in diameter and 5 mm in thickness, were polished with sandpaper ranging from 150 to 1500 grit sizes. Prior to plasma treatment, the HDPE surfaces were cleaned using an ultrasonic bath containing industrial soap, distilled water, and isopropyl alcohol for 10 min each sample. The plasma processing of both Si and HDPE substrates was conducted simultaneously in a DC magnetron sputtering system, applying 40 W to the Ti target under a base pressure of 6 × 10−4 Pa and a working pressure of 0.8 Pa using argon (Ar) as the working gas with a flow rate of 10 sccm.
Before the Ti deposition step, a DC plasma etching of 5 min on the substrate surfaces were performed using the same parameters as in the sputtering process. The samples were structurally, elementally, and morphologically characterized using X-ray diffraction (XRD with an Empyrean Panalytical diffractometer Enigma Business Park. Grovewood Road, Malvern, UK), energy-dispersive X-ray spectroscopy (EDS-Bruker, 40 Mann ing Rd, Billerica, MA, USA), and scanning electron microscopy (SEM-Tescan, Zum Lonnenhohl 46, Dortmund, Germany). For the morphological analysis of untreated HDPE surfaces, a thin gold (Au) coating was applied via DC sputtering for 20 s to prevent charging during SEM imaging.
The variation in the electrical resistivity of the treated and untreated polymer surfaces was measured using two points technique with two points of three size pyramid covered with gold layer at 2 mm of distance. The hardness was determinate using Shore D (Hilitand) on treated and untreated HDPE surfaces according to ASTM D2240, the hardness test has carried out 4 time on different coated and uncoated zones. Scratch resistance was evaluated using a scratch tester (Millennium-Tribotechnic, 4 rue Valiton, Clichy, France) with loads ranging from 0 to 10 and 40 N, creating tracks of 5 mm length over 1 min, using an Al2O3 ball with a diameter of 3 mm (based in ASTM D7027-CETR-UMT2, Center for Tribology, Campell, CA, USA), the scratch test was repeated 3 time on different coated zones. The tribological properties were examined using sliding tests configuration with a linear stroke length of 10 mm at 30 RPM of the motion motor, producing 1 go-back reciprocating motion cycle each 2 s, applying loads of 1, 2, and 3 N for 1800 s with a spherical pin of ZrO2 measuring 5 mm in diameter according to ASTM G133. Each wear tests were repeated three time on different coated zones. The friction force was recorded in real-time, and wear tracks were characterized using an optical profilometer (Nexview-Zygo, Laurel Brook Road, Middlefield, CT, USA) and SEM for wear track on HDPE treated surfaces and optical microscopy for the wear track on spherical pin of ZrO2.

3. Results

3.1. Surface Characteristics

Figure 1a shows the secondary electron (SE) micrograph of the cross-section of the Si substrate after plasma treatment and Ti deposition process. The micrograph reveals a columnar morphology with a 0.76 ± 0.01 μm thickness of the Ti layer. The Ti layers exhibited a crystalline structure with (200) plane and elemental composition of 91.5 ± 0.9% Ti and 8.5 ± 0.6% O, that are typical of the Ti film deposition by DC-magnetron sputtering process [33,37]. Figure 1b presents the morphology of untreated HDPE surfaces before and after sputtering plasma treatment with Ti deposition. Untreated HDPE displayed a nodule-like morphology with interconnected fibers. After plasma treatment, the HDPE surface exhibited a fiber-like morphology, measuring 1.66 ± 0.4 μm in diameter. This fiber-like structure is attributed to the surface polarization of the HDPE surface induced by the Ar+ ions bombarding during the etching operation, followed by the deposition of Ti atoms on the HDPE surfaces that were expelled from the Ti target by the sputtering process during plasma treatment, leading to fiber formation. The elemental composition of fiber-like morphology was determined to be 90 ± 0.9% Ti and 10 ± 0.6% O. Similar fiber-like morphology have been reported by Yakovlev et al. [21], who produced nanostructures via RF-magnetron sputtering of Pt and CeO2 on membrane surfaces. Other studies also indicate the formation of fiber-like morphologies using sputtering plasma processes, especially sputtering-etching on polymer surfaces such as Polyethylene Terephthalate (PET), Polymethyl methacrylate (PMMA), Polytetrafluoroeth-ylene (PTFE), and other polymeric surfaces [38,39,40]. This surface topography is known to enhance the surface area, thereby improving properties such as catalytic activity, hydrophobicity, and cellular proliferation. Figure 1c displays the X-ray diffraction (XRD) patterns of the silicon (Si) and high-density polyethylene (HDPE) substrates after plasma treatment [18,20,21,41,42,43,44]. Both patterns show a diffraction peak at 36.6° corresponding to the (100) plane of the α-Ti phase (reference card 00-044-1288) on both the Si and HDPE substrates. Additionally, peaks at 21.5° and 23.9° are present, corresponding to the (110) and (200) planes of the orthorhombic structure of HDPE (reference card 00-040-1995).

3.2. Mechanical Properties

The surface hardness measurements of the polymer surfaces increased with the Ti fiber layer, showing values 61 ± 3 for the untreated HDPE and 67 ± 2 for the treated surfaces. Figure 2 presents the scratch test results on the treated HDPE surfaces, showcasing depth penetration, tangential forces, and representative scratch tracks generated under applied loads of 0 to 10 N and 0 to 40 N. The width profiles of the scratch tracks produced during the test from 0 to 10 N loads, shows deformation in the center of the wear track. In contrast, for 0–40 N loads, the central zone exhibited a softer worn region, as stresses exceeded the plastic limit of the Ti fibers, causing fracture. In the same way, both width profiles have not plastic defamation on the racetrack borders, common in the racetrack produced on untreated HDPE, demonstrating that the Ti fiber layer improve the stresses support transmitted from the scratch operation to the borders of the wear track [45,46,47,48]. For loads ranging from 0 to 10 N, although there was a consistent increase in both deep penetration and tangential force, at 3.2 N of applied load (1.6 mm of racetrack), the slap of the penetration reduced due to the load was supported by the HDPE substrate rather than solely by the Ti fibers, reducing the plastic deformation. However, for the 0 to 40 N tests, a decrease in tangential force was noted at approximately 29.6 N applied load (3.7 mm position), while penetration depth continued to increase. This penetration suggests that the load applied during the test exceeded the load capacity of the treated surfaces. Notably, the scratch tracks did not exhibit spallation zones, indicating a high plastic deformation of the Ti fibers layer. In the same way, the tangential force shows a linear increment during the test from 0 to 10 N, with average slope value of 0.54 ± 0.04. The tangential force produced during the tests from 0 to 40 N shows a semi-liner increment with the increment of the applied load to obtain a load value of 29.6 N, where an instant decrement of the tangential force was observed. This performance of the tangential force before of the instant decrement was caused by the change of the elastic deformation of the surfaces that increased due to the stresses produced during the sliding contact to overcome the Yield stress that caused a high deformation of the surfaces in fort of the indenter [45,46,47,48]. However, the treated surfaces did not present detachment or plastic deformation on the worn borders, demonstrating a good adhesion and load-bearing capacity.

3.3. Tribological Properties

The wear tracks produced on the treated HDPE surfaces at applied loads of 1 N, 2 N, and 3 N are shown in Figure 3. While the stresses from the sliding operation led to the plastic deformation and fracture of the fibers (designated as ff), generating debris (d) that accumulated between the fibers. Despite this, the fibers remained attached to the surfaces, providing continued protection. A tribolayer (tl), composed of polymer material from the HDPE substrate and fiber debris, was formed in different areas of the wear tracks. The wear track area that was cover for the tribolayer increased with the applied load, covering most of the wear tracks during the 3 N test. This layer was a protective barrier, reducing contact between the pin and the treated surfaces. However, due to the fatigue from the cyclic reciprocating sliding operation, the tribolayer experienced plastic deformation and brittle fractures (bf), particularly during the tests at 3 N. The formation of the tribolayer and the variation in the area that this layer covers produced a similar wear rate during the sliding tests for the three applied loads, because the wear track was formed by the Ti fiber deformation, and the pin did not touch the HDPE substrate. The contact areas on the pin surfaces showed no significant wear due to the pin hardness was higher than the Ti fibers, and they were covered with a tribolayer formed from transferred material (tm) originating from the wear track of the treated surfaces, along with debris accumulation around the contact area.
Increasing the applied load led to a greater extent of fiber fractures and elastoplastic deformation on the treated surfaces, which improved the adhesion force between the sliding pin and the Ti fiber layer, as well as the accumulating material in front of the pin during the sliding operation. This effects contributed to increase the friction force (FF) with the increment of the applied load during the sliding tests, as shown in Figure 4a. Additionally, the progressive damage exposed more of the substrate, enhancing the formation of a tribolayer in the worn zone that acted as a protective layer during the sliding operation, particularly during the tests at 2 N and 3 N. The FF behavior produced during the sliding tests on the treated HDPE surfaces is exhibited in Figure 4. The FF behavior produced during the tribological test at 1 N was stable, without variations, which indicates a homogenous contact surface. The FF behavior shows a decrement at the end of the tests due to the fracture of the fibers, and the substrate material produces a tribolayer that decreases the FF value. The coefficient of friction (CoF) increases with the increment of applied load, showing CoF values of 0.33 ± 0.04, 0.35 ± 0.05 and 0.38 ± 0.03 for the test at 1, 2 and 3 N, respectively. The increment in the CoF is attributed to the increment in the elastic deformation of the surfaces in front of the indenter during the rubbing operation. While, the wear rate (K) presented a lower value produced by the tests at 2 and 3 N tests than at 1 N, with K values of 6.3 ± 0.8, 4.9 ± 0.7 and 5.6 ± 0.7 × 10−13 m3N−1m−1 respectively.

4. Discussion

Although High-density polyethylene (HDPE) is widely employed across industrial applications, its long-term performance is often compromised under aggressive condi-tions due to limited resistance to oxidation, fracture and wear. To overcome these draw-baks, strategies that improve the surface integrity of HDPE are essential, enabling compo-nents to operate reliably and with extended service life demanding. Consequently, surface modification of the HDPE components is required to enhance their performance and ex-tend their service life under selective working conditions.
Ti is a material that has an excellent protection in several work environments that improve the chemical stability, optical radiation, and tolerance to frictional stresses, thereby improving the life-time of components. The plasma treatments are widely used to modify the surfaces characteristics changing the surfaces energy or depositing a layer with specific characteristics. In this study, the plasma treatment was composed by an etching operation with Ar+ ion bombarding in DC sputtering process of the HDPE surfaces and the deposition of the Ti atoms that were produced for the Ar+ bombarding of Ti target in a DC sputtering operation. The etching process fractures the polymer fibers and activates molecules that increase the polarity of the HDPE surface. This enhancement occurs without a chemical reaction, as etching is performed in an argon or non-reactive environment. Both material fracture and thermal phenomena contribute to the improved polarity of the HDPE substrate [19,22,26,49]. The titanium (Ti) atoms deposited, resulting in a layer with columnar morphology on the silicon substrate [27,29,33]. While the increment of the polarity of the HDPE surfaces increased adhesion of Ti atoms to the polymer surfaces, combined with their low mobility, allows for the development of a fiber-like morphology of Ti [19,22,24,26,49].
The mechanical tests demonstrated that the Ti fiber-like layer improve the resistance to the plastic deformation, exhibiting a higher hardness compared with the untreated HDPE surface. The Ti fiber layer exhibited a good adhesion to the HDPE surfaces, revealing fractures and deformation of the fibers, but without detachment and good load-bearing support, reducing the surfaces deformation and the wear of the polymeric substrate [45,46,47,48].
Tribological tests demonstrated that the wear tracks were characterized by fiber fractures and plastic deformation. However, at an applied load of 1 N, the worn zone exhibited fractured fibers with minimal polymer material remaining. The combination of fiber debris and remaining polymer material contributed to the formation of a protecting tribolayer on some areas of the wear track that increase with increment of the load, being denser and cover a more contact area for the tests at 2 and 3 N than at 1 N tests. The plastic deformation of the Ti layer and the formation of the tribolayer on the worn surfaces indicates that plasma treatment effectively improves surface protection, distributing stress across the fibers and reducing the wear of the surfaces during the sliding operation.

5. Conclusions

  • The plasma treatment successfully combined the etching effect on the HDPE that polarized the polymer surfaces, facilitating the the titanium (Ti) deposition, forming a layer with fibers-like morphology with the α-Ti phase crystalline structure.
  • The Ti coating with fiber-like morphology had a good adhesion to the HDPE surfaces and load-bearing capacity, reducing the plastic deformation around the worn zones.
  • The plasma treatment provided effective surface protection for the HDPE substrate by enabling plastic deformation and fiber fracture without layer detachment, leading to the formation of a tribolayer that contributed to reducing surface wear during sliding operations.

Author Contributions

Conceptualization, E.Y.V.-O.; writing—original draft preparation, C.H.-N.; formal analysis, V.G.-A.; Conceptualization M.d.P.J.C.-M.; investigation, M.A.D.-R.; data curation methodology, N.L.-P.; writing—review and editing, E.D.G.-B.; visualization, S.M.-S.; supervision and validation, M.F.-M. All authors have read and agreed to the published version of the manuscript.

Funding

This research received no external funding.

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

Data are contained within the article.

Acknowledgments

Laboratory for Surface Studies, Modification, and Application (LEMAS)-Polytechnic University of the Valley of Mexico in the project CIR/0022/2022 of the program “Researchers for Mexico” of SECIHTI.

Conflicts of Interest

The authors declare no conflict of interest.

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Coatings 15 00995 g001
Figure 1. SEM micrographs of (a) Ti film on Si substrate, (b) fiber-like morphology on HDPE substrate and (c) XRD patterns of untreated HDPE substrate, Ti coating on Si substrate and HDPE surface.
Figure 1. SEM micrographs of (a) Ti film on Si substrate, (b) fiber-like morphology on HDPE substrate and (c) XRD patterns of untreated HDPE substrate, Ti coating on Si substrate and HDPE surface.
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Figure 2. (a) Transversal profile at 5 mm of scratch track, (b) longitudinal and Tangential force profile produced during the scratch tests from 0 to 10 and 40 N applied load, and (c) representative of the racetrack of the scratch test from 0 to 40 N test on treated HDPE surfaces.
Figure 2. (a) Transversal profile at 5 mm of scratch track, (b) longitudinal and Tangential force profile produced during the scratch tests from 0 to 10 and 40 N applied load, and (c) representative of the racetrack of the scratch test from 0 to 40 N test on treated HDPE surfaces.
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Figure 3. SEM micrographs and optical images of the wear track produced by sliding tests at applied load of 1 N, 2 N, and 3 N on the treated HDPE surfaces.
Figure 3. SEM micrographs and optical images of the wear track produced by sliding tests at applied load of 1 N, 2 N, and 3 N on the treated HDPE surfaces.
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Figure 4. (a) Friction force performance and (b) Coefficient of friction (CoF) and wear rate produced by sliding tests at 1 N, 2 N, and 3 N on the treated HDPE surfaces.
Figure 4. (a) Friction force performance and (b) Coefficient of friction (CoF) and wear rate produced by sliding tests at 1 N, 2 N, and 3 N on the treated HDPE surfaces.
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MDPI and ACS Style

Vargas-Oliva, E.Y.; Hernández-Navarro, C.; Guzman-Ayon, V.; Ceballos-Muez, M.d.P.J.; García-Bustos, E.D.; Doñu-Ruiz, M.A.; López-Perrusquia, N.; Flores-Martínez, M.; Muhl-Saunders, S. Synthesis and Characterization of Titanium Layer with Fiber-like Morphology on HDPE by Plasma Treatment. Coatings 2025, 15, 995. https://doi.org/10.3390/coatings15090995

AMA Style

Vargas-Oliva EY, Hernández-Navarro C, Guzman-Ayon V, Ceballos-Muez MdPJ, García-Bustos ED, Doñu-Ruiz MA, López-Perrusquia N, Flores-Martínez M, Muhl-Saunders S. Synthesis and Characterization of Titanium Layer with Fiber-like Morphology on HDPE by Plasma Treatment. Coatings. 2025; 15(9):995. https://doi.org/10.3390/coatings15090995

Chicago/Turabian Style

Vargas-Oliva, Erick Yair, Carolina Hernández-Navarro, Violeta Guzman-Ayon, María del Pilar Jadige Ceballos-Muez, Ernesto David García-Bustos, Marco Antonio Doñu-Ruiz, Noé López-Perrusquia, Martin Flores-Martínez, and Stephen Muhl-Saunders. 2025. "Synthesis and Characterization of Titanium Layer with Fiber-like Morphology on HDPE by Plasma Treatment" Coatings 15, no. 9: 995. https://doi.org/10.3390/coatings15090995

APA Style

Vargas-Oliva, E. Y., Hernández-Navarro, C., Guzman-Ayon, V., Ceballos-Muez, M. d. P. J., García-Bustos, E. D., Doñu-Ruiz, M. A., López-Perrusquia, N., Flores-Martínez, M., & Muhl-Saunders, S. (2025). Synthesis and Characterization of Titanium Layer with Fiber-like Morphology on HDPE by Plasma Treatment. Coatings, 15(9), 995. https://doi.org/10.3390/coatings15090995

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