{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2025,10,12]],"date-time":"2025-10-12T03:12:16Z","timestamp":1760238736971,"version":"build-2065373602"},"reference-count":49,"publisher":"MDPI AG","issue":"12","license":[{"start":{"date-parts":[[2022,6,9]],"date-time":"2022-06-09T00:00:00Z","timestamp":1654732800000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"funder":[{"DOI":"10.13039\/501100001871","name":"FEDER National funds FCT","doi-asserted-by":"publisher","award":["POCI-01-0145-FEDER-031807","UIDB\/00285\/2020","POCI-01-0247-FEDER-024521","LA\/P\/0112\/2020","POCI-01-0145-FEDER-030446"],"award-info":[{"award-number":["POCI-01-0145-FEDER-031807","UIDB\/00285\/2020","POCI-01-0247-FEDER-024521","LA\/P\/0112\/2020","POCI-01-0145-FEDER-030446"]}],"id":[{"id":"10.13039\/501100001871","id-type":"DOI","asserted-by":"publisher"}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Materials"],"abstract":"<jats:p>Alloyed-transition metal dichalcogenide (TMD) coatings have been under investigation as multi-environment lubricants for the past few decades. These coatings display very low coefficient of friction properties at elevated temperatures. Studies on the annealing of these low-friction coatings are missing in the literature. For the first time, in this study, the annealing of the W-S-N dry lubricant coatings was carried out to study its effects on the composition, morphology, crystal structure and hardness of the coatings. The W-S-N coatings were deposited by direct current (DC) reactive magnetron sputtering. The analysis was carried out for as-deposited, 200 \u00b0C and 400 \u00b0C annealed coatings. The as-deposited coatings have N content in the range of 0\u201325.5 at. %. The coatings are compact and the densification increased with the increase in N-alloying. All the coatings are crystalline except the highest N-alloyed coating which is X-ray amorphous. A maximum hardness of 8.0 GPa was measured for the coating alloyed with 23 at. % N. Annealing did not affect the composition and morphology of the coatings, while some variations were observed in their crystal structure and hardness. The maximum hardness increased from 8 GPa to 9.2 GPa after 400 \u00b0C annealing of the 23 at. % N-alloyed coating.<\/jats:p>","DOI":"10.3390\/ma15124088","type":"journal-article","created":{"date-parts":[[2022,6,12]],"date-time":"2022-06-12T09:26:48Z","timestamp":1655026008000},"page":"4088","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Effect of Annealing Heat Treatment on the Composition, Morphology, Structure and Mechanical Properties of the W-S-N Coatings"],"prefix":"10.3390","volume":"15","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-5598-8322","authenticated-orcid":false,"given":"Talha Bin","family":"Yaqub","sequence":"first","affiliation":[{"name":"CEMMPRE-Centre for Mechanical Engineering Materials and Processes, University of Coimbra, Rua Lu\u00eds Reis Santos, 3030-788 Coimbra, Portugal"},{"name":"Laboratory of Tests, Wear and Materials, IPN-LED & MAT-Instituto Pedro Nunes, Rua Pedro Nunes, 3030-199 Coimbra, Portugal"},{"name":"School of Chemical and Materials Engineering (SCME), National University of Sciences and Technology (NUST), H-12, Islamabad 44000, Pakistan"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1466-3353","authenticated-orcid":false,"given":"Abbas","family":"Al-Rjoub","sequence":"additional","affiliation":[{"name":"CEMMPRE-Centre for Mechanical Engineering Materials and Processes, University of Coimbra, Rua Lu\u00eds Reis Santos, 3030-788 Coimbra, Portugal"}]},{"given":"Hafiza Ayesha","family":"Khalid","sequence":"additional","affiliation":[{"name":"CEMMPRE-Centre for Mechanical Engineering Materials and Processes, University of Coimbra, Rua Lu\u00eds Reis Santos, 3030-788 Coimbra, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4208-9018","authenticated-orcid":false,"given":"Khurram","family":"Yaqoob","sequence":"additional","affiliation":[{"name":"School of Chemical and Materials Engineering (SCME), National University of Sciences and Technology (NUST), H-12, Islamabad 44000, Pakistan"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4035-3241","authenticated-orcid":false,"given":"Filipe","family":"Fernandes","sequence":"additional","affiliation":[{"name":"CEMMPRE-Centre for Mechanical Engineering Materials and Processes, University of Coimbra, Rua Lu\u00eds Reis Santos, 3030-788 Coimbra, Portugal"},{"name":"ISEP\u2014School of Engineering, Polytechnic of Porto, Rua Dr. Antonio Bernardino de Almeida 431, 4200-072 Porto, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8251-5099","authenticated-orcid":false,"given":"Albano","family":"Cavaleiro","sequence":"additional","affiliation":[{"name":"CEMMPRE-Centre for Mechanical Engineering Materials and Processes, University of Coimbra, Rua Lu\u00eds Reis Santos, 3030-788 Coimbra, Portugal"},{"name":"Laboratory of Tests, Wear and Materials, IPN-LED & MAT-Instituto Pedro Nunes, Rua Pedro Nunes, 3030-199 Coimbra, Portugal"}]}],"member":"1968","published-online":{"date-parts":[[2022,6,9]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"1412","DOI":"10.1016\/j.matdes.2007.09.005","article-title":"Improving Hardness of Electroless Ni\u2013B Coatings Using Optimized Deposition Conditions and Annealing","volume":"29","author":"Oraon","year":"2008","journal-title":"Mater. Des."},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"106265","DOI":"10.1016\/j.triboint.2020.106265","article-title":"Significantly Enhanced Mechanical and Tribological Properties of Co-Based Alloy Coatings by Annealing Treatment","volume":"146","author":"Tang","year":"2020","journal-title":"Tribol. Int."},{"key":"ref_3","doi-asserted-by":"crossref","first-page":"549","DOI":"10.1016\/S1359-6462(99)00394-2","article-title":"Quantification of Age Hardening in Maraging Steels and an Ni-Base Superalloy","volume":"42","author":"Sha","year":"2000","journal-title":"Scr. Mater."},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"1475","DOI":"10.1016\/S1359-6462(97)00294-7","article-title":"Precipitation Hardening of Mg-Ca(-Zn) Alloys","volume":"37","author":"Nie","year":"1997","journal-title":"Scr. Mater."},{"key":"ref_5","doi-asserted-by":"crossref","unstructured":"Fernandes, F., Al-rjoub, A., Cavaleiro, D., Polcar, T., and Cavaleiro, A. (2020). Room and High Temperature Tribological Performance of Multilayered TiSiN\/TiN and TiSiN\/TiN(Ag) Coatings Deposited by Sputtering. Coatings, 10.","DOI":"10.3390\/coatings10121191"},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"127767","DOI":"10.1016\/j.surfcoat.2021.127767","article-title":"Influence of Ag Additions on the Structure, Mechanical Properties and Oxidation Behaviour of CrAlNAg Coatings Deposited by Sputtering","volume":"426","author":"Rajput","year":"2021","journal-title":"Surf. Coat. Technol."},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"108703","DOI":"10.1016\/j.matdes.2020.108703","article-title":"Influence of Ag Alloying on the Morphology, Structure, Mechanical Properties, Thermal Stability and Oxidation Resistance of Multilayered TiSiN\/Ti(Ag)N Films","volume":"192","author":"Cavaleiro","year":"2020","journal-title":"Mater. Des."},{"key":"ref_8","doi-asserted-by":"crossref","first-page":"167","DOI":"10.1016\/j.surfcoat.2018.02.025","article-title":"Influence of Ag Additions on the Structure, Mechanical Properties and Oxidation Behaviour of Cr-O Coatings Deposited by HiPIMS","volume":"339","author":"Fernandes","year":"2018","journal-title":"Surf. Coat. Technol."},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"36","DOI":"10.1016\/S0257-8972(99)00228-5","article-title":"Nanocomposite Tribological Coatings for Aerospace Applications","volume":"116\u2013119","author":"Voevodin","year":"1999","journal-title":"Surf. Coat. Technol."},{"key":"ref_10","first-page":"741","article-title":"Nanocomposite and Nanostructured Tribological Materials for Space Applications","volume":"65","author":"Voevodin","year":"2005","journal-title":"Compos. Sci. Technol."},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"128035","DOI":"10.1016\/j.matlet.2020.128035","article-title":"Molybdenum Diselenide Coatings as Universal Dry Lubricants for Terrestrial and Aerospace Applications","volume":"275","author":"Yaqub","year":"2020","journal-title":"Mater. Lett."},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"10583","DOI":"10.1103\/PhysRevB.48.10583","article-title":"Superlubricity of Molybdenum Disulphide","volume":"48","author":"Martin","year":"1993","journal-title":"Phys. Rev. B"},{"key":"ref_13","unstructured":"Yaqub, T.B. (2020). Optimization of Sputtered Mo-Se-C Coatings for Efficient Self-Adaptation during Sliding in Diverse Environments, Universidade De Coimbra."},{"key":"ref_14","doi-asserted-by":"crossref","unstructured":"Vazirisereshk, M.R., Martini, A., Strubbe, D.A., and Baykara, M.Z. (2019). Solid Lubrication with MoS2: A Review. Lubricants, 7.","DOI":"10.3390\/lubricants7070057"},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"686","DOI":"10.1016\/j.surfcoat.2011.03.004","article-title":"Review on Self-Lubricant Transition Metal Dichalcogenide Nanocomposite Coatings Alloyed with Carbon","volume":"206","author":"Polcar","year":"2011","journal-title":"Surf. Coat. Technol."},{"key":"ref_16","doi-asserted-by":"crossref","first-page":"67","DOI":"10.1016\/S0257-8972(01)01108-2","article-title":"Advantages of Using Self-Lubricating, Hard, Wear-Resistant MoS2-Based Coatings","volume":"142\u2013144","author":"Renevier","year":"2001","journal-title":"Surf. Coat. Technol."},{"key":"ref_17","doi-asserted-by":"crossref","first-page":"137","DOI":"10.1016\/j.tsf.2005.04.078","article-title":"Effects of Temperature on the Chemistry and Tribology of Co-Sputtered MoSx -Ti Composite Thin Films","volume":"489","author":"Savan","year":"2007","journal-title":"Thin Solid Films"},{"key":"ref_18","doi-asserted-by":"crossref","first-page":"1302","DOI":"10.1021\/acsanm.8b02184","article-title":"Mo-S-Ti-C Nanocomposite Films for Solid-State Lubrication","volume":"2","author":"Duan","year":"2019","journal-title":"ACS Appl. Nano Mater."},{"key":"ref_19","doi-asserted-by":"crossref","first-page":"5666","DOI":"10.1016\/j.tsf.2009.02.103","article-title":"Growth, Structure and Friction Behavior of Titanium Doped Tungsten Disulphide (Ti-WS2) Nanocomposite Thin Films","volume":"517","author":"Scharf","year":"2009","journal-title":"Thin Solid Films"},{"key":"ref_20","doi-asserted-by":"crossref","first-page":"7532","DOI":"10.1016\/j.tsf.2010.05.040","article-title":"Tribological Behaviour of MoS2\/Au Coatings","volume":"518","author":"Chien","year":"2010","journal-title":"Thin Solid Films"},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"175","DOI":"10.1016\/S0043-1648(99)00100-3","article-title":"Wear Behavior of Pb-Mo-S Solid Lubricating Coatings","volume":"230","author":"Wahl","year":"1999","journal-title":"Wear"},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"140","DOI":"10.1016\/j.apsusc.2016.01.163","article-title":"Microstructure and Tribological Properties of MoS2 + Zr Composite Coatings in High Humidity Environment","volume":"367","author":"Ye","year":"2016","journal-title":"Appl. Surf. Sci."},{"key":"ref_23","doi-asserted-by":"crossref","first-page":"565","DOI":"10.1016\/j.surfcoat.2010.07.050","article-title":"Structure, Morphology and Chemical Composition of Sputter Deposited Nanostructured Cr-WS2 Solid Lubricant Coatings","volume":"205","author":"Deepthi","year":"2010","journal-title":"Surf. Coat. Technol."},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"41","DOI":"10.1016\/j.surfcoat.2018.04.040","article-title":"On the S\/W Stoichiometry and Triboperformance of WSx C(H) Coatings Deposited by Magnetron Sputtering","volume":"365","author":"Cao","year":"2019","journal-title":"Surf. Coat. Technol."},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"103","DOI":"10.1080\/21663831.2018.1561538","article-title":"Self-Healing of a Pre-Notched WS2\/a-C Coating","volume":"7","author":"Cao","year":"2019","journal-title":"Mater. Res. Lett."},{"key":"ref_26","doi-asserted-by":"crossref","first-page":"1","DOI":"10.1016\/j.apsusc.2019.03.294","article-title":"Structure, Mechanical and Tribological Properties of Mo-S-N Solid Lubricant Coatings","volume":"486","author":"Hudec","year":"2019","journal-title":"Appl. Surf. Sci."},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"124992","DOI":"10.1016\/j.surfcoat.2019.124992","article-title":"DCMS Mo-Se-C Solid Lubricant Coatings\u2014Synthesis, Structural, Mechanical and Tribological Property Investigation","volume":"378","author":"Yaqub","year":"2019","journal-title":"Surf. Coat. Technol."},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"126536","DOI":"10.1016\/j.surfcoat.2020.126536","article-title":"Structure, Mechanical and Tribological Properties of MoSe2 and Mo-Se-N Solid Lubricant Coatings Tom\u00e1\u0161","volume":"405","author":"Hudec","year":"2021","journal-title":"Surf. Coat. Technol."},{"key":"ref_29","doi-asserted-by":"crossref","first-page":"126722","DOI":"10.1016\/j.surfcoat.2020.126722","article-title":"Tribological Behaviour of Mo-S-N Solid Lubricant Coatings in Vacuum, Nitrogen Gas and Elevated Temperatures","volume":"405","author":"Hudec","year":"2021","journal-title":"Surf. Coat. Technol."},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"106363","DOI":"10.1016\/j.triboint.2020.106363","article-title":"Synthesis, Microstructure and Mechanical Properties of W\u2013S\u2013C Self-Lubricant Thin Films Deposited by Magnetron Sputtering","volume":"150","author":"Vuchkov","year":"2020","journal-title":"Tribol. Int."},{"key":"ref_31","doi-asserted-by":"crossref","first-page":"125481","DOI":"10.1016\/j.surfcoat.2020.125481","article-title":"The Effect of Substrate Location on the Composition, Microstructure and Mechano-Tribological Properties of W-S-C Coatings Deposited by Magnetron Sputtering","volume":"386","author":"Vuchkov","year":"2020","journal-title":"Surf. Coat. Technol."},{"key":"ref_32","doi-asserted-by":"crossref","unstructured":"Vuchkov, T., Yaqub, T.B., Evaristo, M., and Cavaleiro, A. (2020). Synthesis, Microstructural, and Mechano-Tribological Properties of Self-Lubricating W-s-C(H) Thin Films Deposited by Different RF Magnetron Sputtering Procedures. Coatings, 10.","DOI":"10.3390\/coatings10030272"},{"key":"ref_33","doi-asserted-by":"crossref","unstructured":"Yaqub, T.B., Vuchkov, T., Sanguino, P., Polcar, T., and Cavaleiro, A. (2020). Comparative Study of DC and RF Sputtered MoSe2 Coatings Containing Carbon\u2014An Approach to Optimize Stoichiometry, Microstructure, Crystallinity and Hardness. Coatings, 10.","DOI":"10.3390\/coatings10020133"},{"key":"ref_34","doi-asserted-by":"crossref","first-page":"126360","DOI":"10.1016\/j.surfcoat.2020.126360","article-title":"Insights into the Wear Track Evolution with Sliding Cycles of Carbon-Alloyed Transition Metal Dichalcogenide Coatings","volume":"403","author":"Yaqub","year":"2020","journal-title":"Surf. Coat. Technol."},{"key":"ref_35","doi-asserted-by":"crossref","first-page":"126651","DOI":"10.1016\/j.surfcoat.2020.126651","article-title":"Elevated-Temperature Super-Lubrication Performance Analysis of Dispersion-Strengthened WSN Coatings: Experimental Research and First-Principles Calculation","volume":"406","author":"Zhu","year":"2021","journal-title":"Surf. Coat. Technol."},{"key":"ref_36","doi-asserted-by":"crossref","first-page":"230","DOI":"10.1016\/j.surfcoat.2004.08.146","article-title":"Temperature Dependence of Tribological Properties of MoS2 and MoSe2 Coatings","volume":"193","author":"Kubart","year":"2005","journal-title":"Surf. Coat. Technol."},{"key":"ref_37","doi-asserted-by":"crossref","first-page":"547","DOI":"10.1016\/j.jmrt.2022.02.116","article-title":"Exploring the Industrial Implementation of W-S-N Coatings: A Detailed Study of the Synthesis, Compositional, Structural, Mechanical and Multi-Environment Lubrication Properties","volume":"18","author":"Yaqub","year":"2022","journal-title":"J. Mater. Res. Technol."},{"key":"ref_38","doi-asserted-by":"crossref","first-page":"1564","DOI":"10.1557\/JMR.1992.1564","article-title":"An Improved Technique for Determining Hardness and Elastic Modulus Using Load and Displacement Sensing Indentation Experiments","volume":"7","author":"Oliver","year":"1992","journal-title":"J. Mater. Res."},{"key":"ref_39","unstructured":"Martin, P.M. (2009). Martin Handbook of Deposition Technologies for Films and Coatings: Science, Applications and Technology, Elsevier Inc."},{"key":"ref_40","first-page":"69","article-title":"The Foundations of Vacuum Coating Technology","volume":"156","author":"Mattox","year":"2003","journal-title":"Coating"},{"key":"ref_41","doi-asserted-by":"crossref","first-page":"125996","DOI":"10.1016\/j.surfcoat.2020.125996","article-title":"Low Peak Power Deposition Regime in HiPIMS: Deposition of Hard and Dense Nanocomposite Ti-Si-N Fi Lms by DOMS without the Need of Energetic Bombardment","volume":"397","author":"Fernandes","year":"2020","journal-title":"Surf. Coat. Technol."},{"key":"ref_42","doi-asserted-by":"crossref","first-page":"83","DOI":"10.1016\/j.mattod.2016.10.004","article-title":"Interlayer-Expanded MoS2","volume":"20","author":"Rasamani","year":"2017","journal-title":"Mater. Today"},{"key":"ref_43","first-page":"671214","article-title":"Aqueous Medium Synthesis Route for Randomly Stacked Molybdenum Disulfide","volume":"2013","author":"Panigrahi","year":"2013","journal-title":"J. Nanopart."},{"key":"ref_44","doi-asserted-by":"crossref","first-page":"7","DOI":"10.1016\/j.surfcoat.2014.11.074","article-title":"Structure, Mechanical and Tribological Properties of Self-Lubricant W-S-N Coatings","volume":"261","author":"Mutafov","year":"2015","journal-title":"Surf. Coat. Technol."},{"key":"ref_45","doi-asserted-by":"crossref","first-page":"552","DOI":"10.1016\/S0257-8972(02)00622-9","article-title":"Mechanical Behaviour of W\u2013S\u2013N and W\u2013S\u2013C Sputtered Coatings Deposited with a Ti Interlayer","volume":"164","author":"Nossa","year":"2003","journal-title":"Surf. Coat. Technol."},{"key":"ref_46","doi-asserted-by":"crossref","first-page":"185","DOI":"10.1016\/j.surfcoat.2016.04.040","article-title":"Structural, Mechanical and Tribological Properties of Mo-S-N Solid Lubricant Films","volume":"296","author":"Zhang","year":"2016","journal-title":"Surf. Coat. Technol."},{"key":"ref_47","doi-asserted-by":"crossref","first-page":"142","DOI":"10.1016\/j.surfcoat.2017.06.087","article-title":"Effect of Carbon Concentration and Argon Flow Rate on the Microstructure and Triboperformance of Magnetron Sputtered WS2\/a-C Coatings","volume":"332","author":"Cao","year":"2017","journal-title":"Surf. Coat. Technol."},{"key":"ref_48","doi-asserted-by":"crossref","unstructured":"Mathew, S., Abraham, A.R., Chintalapati, S., Sarkar, S., Joseph, B., and Venkatesan, T. (2020). Temperature Dependent Structural Evolution of WSe2: A Synchrotron X-Ray Diffraction Study. Condens. Matter, 5.","DOI":"10.3390\/condmat5040076"},{"key":"ref_49","doi-asserted-by":"crossref","first-page":"35154","DOI":"10.1038\/srep35154","article-title":"Substrate Sensitivity of Monolayer WS2","volume":"6","author":"Mccreary","year":"2016","journal-title":"Sci. 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