Annealing Effect on Mechanical and Tribological behaviour of Nanoscale Mechanics of Thin Layer Metallic Glasses for Engineering Material Applications

Annealing Effect on Mechanical and Tribological behaviour of Nanoscale Mechanics of Thin Layer Metallic Glasses for Engineering Material Applications | 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 Annealing Effect on Mechanical and Tribological behaviour of Nanoscale Mechanics of Thin Layer Metallic Glasses for Engineering Material Applications Adem Ali Muhabie, Wubshet Mekonnen Girma This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-3109079/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract A new and unique alloy formulation design strategies has been developed in order to fabricate thin layered metallic glasses (TFMG) with superior fracture resistance and low coefficient of friction (COF) during nano-scraching test. Due to the outstanding properties, TFMG could be applied for different uses uch as surface coating, biomedical, bio implant, electronic devices, spacecraft and railway, all of which need surface fracture resistance. The fabricated Zr-based metallic glass having the composition of Zr60Cu25Al5Ag5Ni5 (at.%) was annealed for 10, 30, and 60 min below the glass transition temperature. Nanoindentation and nanoscratch tests were used to investigate mechanical and nanotribological properties. Atomic force microscopy (AFM) was used to examine the surface morphology and microstructures. The annealing effect and applied forces change over the chemical structure and stability, morphological change, elastic modulus, hardness, wear rate, and coefficient of friction of the samples were systematically investigated. The nano-indentation data indicated that the hardness and average elastic modulus of the samples increased with increasing annealing time, compared with those of the as-cast MG. More intriguingly, the coefficient of friction and wear rate decreases when the annealing time increases compared to as-cast MG. Furthermore, the continuous wear process, wear depth, wear track volume, and contact area decreases with increasing annealing time, as a result of the improvement of the mechanical and tribological properties of the thin-layered MGs. This study can be a reference to the design protocol to prepare novel a-MGs, which have outstanding mechanical and tribological behavior for engineering material applications. Atomic force microscopy (AFM) annealing coefficient of friction wear rate nanoscratch thin layer metallic glass. Figures Figure 1 Figure 2 Figure 3 Figure 4 1. Introduction Bulk metallic glasses (BMGs) are the focus of a demanding research areas for researchers around the world. 1 BMGs are structurally amorphous metallic alloys, and their compositions are mixed to avoid crystallization during cooling from the melt. 2 BMGs exhibit extraordinary outstanding properties such as high elasticity, 3 high hardness, appreciable toughness, good tribology prosperity 4 and superior corrosion resistance. 5 In addition, due to the lack of long-range atomic order in BMGs offers them exceptional mechanical and physic-chemical properties, 6 related to conventional crystalline metallic materials, making them a promising class of engineering materials. MGs are also novel wear-resistant 7 and low friction materials with high intensive demand in tribological applications. 8 Zr-based MGs display a smaller friction coefficient than other metals during dry sliding conditions. 9 In previous work we reported that the wear resistance of CuZr-based MG materials is comparable to classical tribological ceramics but superior to that of high-performance steel 10 . Metallic glasses can be formed thermoplastically in the supercooled liquid regime. These special properties of MGs make them a perfect candidates for multipurpose application, such as microgears, media-storage devices, 11 building construction, bio-implant, 12 electrode materials, 13 energy conversion/storage 14 and sensors. 15 Developing a proper alloy composition determines both structural and chemical homogeneities, nanometer-sized ductile dendrite homogeneities as a result of annealing have proven their value in increasing plasticity compared to the as-cast MG. Presence of such homogeneities promotes the plastic formability because they increase nucleation and branching. 16 At the macroscale the tribological mechanisms are complex and involve a combination of plasticity, 17 transformation and structural relaxations with structural changes. 18 19 There is no clear and unique correlation between the hardness/modulus and the tribological behavior of metallic glasses has been established so far. Hence, the contributions of hardness, elastic modulus, and thermal treatment on wear resistance and nanoscale friction of thin MG compared to bulk and as-cast counterpart should be studied. 20 Furthermore, improper alloy composition of crystallites, rough surface, and surface reaction structural relations are the cause for their high friction, poor wear resistance, and poor plasticity limit the long-term performance of metallic glasses at ambient temperature. 21 In addition, localized and inhomogeneous decomposition at ambient temperature, free volume, and accompanied with strain lead to early failure of deformation, which still limits the long-term service of MGs for structural applications. 22 To avoid this catastrophic failure, this investigation aims to study mechanical properties like elastic moduli or hardness, inhomogeneous, and microstructure of metallic glasses in addition to thermal treatment play a great role to provide information about the interrelation mechanism with that of nanoscale friction and nanoscale wear rate. In this, we design a proper alloy composition, characterize the structure, mechanical and tribological properties of thin layer amorphous Zr60Cu25Al5Ag5Ni5 by annealing at various length times ( 10,30 and 60 minutes) and we report and discuss the load dependence of friction and wear resistance of metallic glasses. 2. Experimental section Sample preparation and characterization methods A Zr 60 Cu 25 Al 5 Ag 5 Ni 5 metallic glass was prepared as follows. The inorganic alloys of metals such Zr, Al,Cu,Ni,Ag above 99.9 Wt % in purity were mixed and cast on Zr-gettered. The cast alloys were placed on a copper cruisers compressed with a quartz tubes at a temperature of 825 ± 25°C. In order to insure the homogeneous metals in the metallic glass, melting of the alloy should be repeated for five times. 200 mm ribbons of MG were prepared from large melt spinning copper wheel ejection argon gas. 200 nm MG were coated on silicon wafer by sputtering method from the ribbon. The samples were annealed for 10 min, 30 min, and 60 min at 450 o C, and then cooled the samples at ambient temperature in a vacuum place. For comparison, with one non-annealed sample representing as-prepared or as-cast samples. Nanoindentation experiments were operated using Hysitron Triboindenter TI-750 L (Hysitron, Inc., Minneapolis, MN USA) for 0.9 and 4 µN at a constant loading/unloading rate of 0.1µN/s. four indentations were performed to prove the accuracy of data from the same sample. Nano-scratch tests were performed at a velocity of µm s – 1 with applied force of 0.9 and 4 µN as a function of displacement to evaluate the wear rate, wear depth, coefficient of friction, and contact area. Nano-scratch tests were repeated for three times. 3. Results and Discussion 3.1. Microstructure and mechanical properties Annealing thin layer metallic glass at various length times (10, 30, and 60 minutes) was selected as test parameters because of their differences in microstructure, mechanical and tribological properties of Zr60Cu25Al5Ag5Ni5 MG. In order to explore the annealing effect on microstructure and surface morphology, the atomic force spectroscopy (AFM) has been used. The AFM images in Fig. 1 (a) and (b) clearly show the presence of nanoparticles with sizes of around 5.96 nm and 5.05 nm for the specimens annealed for 30 and 60, respectively. The images show the nanoscale inhomogeneity indicating chemical relaxation, with the evolution of atomic scale upon annealing below the glass transition temperature. The AFM topography results are in line with previously reported results. 23 These local compositional fluctuations or random arrangements of atoms influence the plasticity of MGs, without high loss of strength or hardness. Arrangement of atoms can affect atomic transport, hardness, elastic modulus, magnetic, wear rate, friction and electrochemical properties. 7 , 24 Annealing results for chemical reordering leads to phase transition of MG, depending on the interatomic distance of atoms and improved plasticity of MG. Short interatomic distance between transition metals in the alloy composition may be existed only in the metallic glass. 25 Representative indentations on the BMG and TLMG of load-displacement curves are shown in Fig. 1 b. The surface indentation profiles show that the indented depth of TLMG is shallow compared to BMG, indicating lower material loss and higher wear resistance compared to the bulk MG. The depth dependence of the mechanical properties, the Hardness (H), and elastic modulus ( E) values of the MGs were determined for samples which were annealed for different times. The average hardness of metallic glasses increased from 9.75 to 13.4 GPa (Fig. 1 d) as the annealing time rose from zero to 60 min, as result of atomic reordering and structural relaxation that occurred at longer annealing times. Atomic chemical ordering in the glassy phase is smaller than in the crystalline phase, which indicates the improvement of mechanical and tribological properties. 26 The elastic modulus improved from 142.49 to 162.64 with increasing annealing time (figure S2). With respect to elastic behavior, describing the metallic glasses properties not only by hardness and modulus, but by using a hardness/ modulus (H/E) ratio indicating the elastic strain to failure. 2 The average H/E ratio was also increased as the annealing time increases as shown Figure S 3 . The H/E ratio indicates the plasticity of sample deformation. Materials with higher H/E ratio may reveal a structural transition from elastic to plastic behavior at higher stress levels compared to those with lower H/E ratio. H/E is a strong pointer of a good wear resistance of material. The large H/E value indicating material has high resist plastic deformation and the most durable MGs can be used for many applications, which were annealed at different times individually to obtain heat-dependent surface properties. The mechanical properties observed in this research are comparable to the previously works. 2 , 27 3.2 Tribological properties 3.2.1 Coefficient of friction Figure 2 displays the behavior of friction of thin film metallic glasses surface as a function of displacement, annealing time, and number of wear cycles. Friction coefficients of bulk and thin layer metallic glass as a function of sliding displacement were shown in Fig. 2 a. The coefficient of friction is larger in bulk Mg than thin film MG. The saw-tooth appearance of bulk MG is revealed, indicating shear banding and plow formation as the indenter deformed the matrix as a result of the absence of elastic plasticity. It might be difficult for the movement atom in all direction while the indenter scratching the surface due to the presence or some extent of crystallinity. As the annealing time increases, reducing the grain size, annealing-induced embrittlement of metallic glasses a result in a lower friction coefficient and excellent wear resistance. Figure 2 b demonstrates that for all annealed MGs, the reduction of friction force was observed as a function of sliding distance under load 4 µN. The value of friction force dropped gradually when the annealing time increases from zero to 60 min. The friction force of highly annealed MGs is much lower than that of the cast- MG. The graph of friction force for a cast MG revealed sawtooth, many small peaks, indicating the rough surface, deformation of surface matrix and weak wear resistance performance, whereas the graph of highly annealed MG showed a smooth peak as increasing the annealing time indicating the laminated surface, mechanical and tribology properties were successfully improved. 6 , 28 The coefficient of friction as a function of the number of scratch cycles after annealing for different time is shown in Fig. 2 c under applied load of 0.9 µN. The coefficient of friction initially seems increases with the number of wear cycles and then reaches a steady value at for all samples. The increase in the coefficient of friction during the initial wear cycle is related to a larger plowing depth, as reported previously. 29 In addition, the coefficient of friction of the thin film MGs slightly decreases with increasing temperature aging time. The effects of annealing time on the coefficient of friction of thin film MGs has been observed in Fig. 2 d under 0.9 µN and 4 µN applied force. The mean coefficient of friction value was similar for both test conditions. It is clear that the value of friction coefficient is about 0.062 for the non-annealed, while for the MG annealed for 60 min, the coefficient of friction slightly decreased (< 0.03) under 0.9 µN applied force. The friction coefficient decreases with increasing annealing time in both conditions, in line with previous reports, 30 demonstrating the possibility of reduction of friction coefficient by tuning the surface patterning with aging temperature. 7 It is reported that most of frictional work during the wear process create heat energy which modifies the tribological behaviors of Nano-scratched surfaces such as forming delocalized free metal ions for chemical reordering or even heating interfacial contact materials. 31 3.2.2 Nanowear depth Nano-scratch test was conducted on the TLMGs which were annealed at different time individually to obtain heat-dependent surface properties. Figure 3 shows the AFM images of the wear track surface of three MGs after nanoscratch test using normal forces, 4 µN. The nanoscratched MGs surface of AFM images at normal force FN = 0.9 µN is shown in figure S 3 . All nanoscratches wear track images display different features in both loads. AFM images demonstrate different wear depth and contact area of MGs for different annealing times. Wide and deep grooves were shown (Fig. 3 a) for non-annealed MG but a shallow scratch tracks were observed for highly annealed MGs (Fig. 3 c). The wear debris has been seen for as-cast which are material accumulation on the lateral sides, which indicates the serious plastic deformation during friction. The wear rate and volume loss for 4 µN were significantly higher than 0.9 µN test condition, in line with previously reported. 31a The nanoscratch wear track images of the three thin film MGs at normal forces, 0.9 µN were shown Figures S4. The wear depth of each scratch sample was determined and shown in Fig. 3 d. The values of the wear depth decrease from 201.56 nm for the non-annealed to 148.43, 37.32, and 25.27 nm for the TLMG annealed for 10, 30 and 60 min, respectively in line with previous reports. The wear depth is equivalent to both the height of the accumulated material and the depth of the scratch. It can be seen that the thin layer MG which is annealed for a long period of time that revealed a shallow wear track, indicating there is clearly elastic recovery behind the indenter and exhibited excellent wear resistance performance and very low coefficient of friction. 32 Wear resistance improved with annealing time increases, as a result of good hardness and elastic modulus of materials which lead to too much reduction of friction while plowing the MG layer on an indenter. 33 During annealing, anti-wear and coefficient of friction in all conditions improved on surface of the film, there might be dangling bonds (immobilized free radical), therefore, annealing needs to be satisfied this bond by surface reconstruction, by charge transfer, by chemical absorption. 34 23, 35 3.2.3. Wear rate The variations of wear rate as a function of displacement for each annealed sample at a normal force of 0.9 and 4µN load are shown in figures (4a &4b). It is found that for all samples, the wear rate first decreases, and then steady-state wear is observed as a function of the sliding distance under both loads and all annealing time. The wear rate dropped continuously with increasing annealing time and for both test conditions. The wear rates for 4 µN were meaningfully higher than 0.9 N test conditions, in line with previous work. 36 More importantly, the wear rate of the highly annealed MGs is much lower than that of the non-annealed MG. Figure 4 c shows the contact area as a function of annealing time for 0.9 and 4 µN. As can be seen, the scratch contact area decreases with increasing the annealing time for both loads. Contact areas for 4 µN were meaningfully higher than 0.9 N test conditions, in line with previous work. This behavior of the contact area is depending on the mechanical properties (hardness and elastic modulus) and the microstructure of the film. 37 Figure 4 d shows the wear volume of the scratched area of samples for normal force, 4µN. As it is found that the wear volume decreases with increasing annealing time as a result of improved elastic modulus or high H/E ratio and low friction coefficient. This will be the reason for the high wear resistance of materials. 38 Researchers regarded that the real area of contact and material properties such as microstructure, surface topography, and mechanical properties are the key factors that govern the wear rate. 39 4. Conclusions In summary, we have studied the surface morphology and microstructure by atomic force microscope, mechanical properties by nano-indentation experiment, and tribological properties by Nano-scratch experiment of MG films annealed for various lengths of time. The hardness value, the average elastic modulus of the samples increased with increasing the annealing time, the annealed samples revealed better properties than as-cast MG. The H/E ratio of all samples increased with increasing annealing time. The nanoscratch results indicate that annealing at different time significantly reduces friction and improves wear resistance performance. In addition, the decrease of wear depth, wear volume, and contact area under annealing effect appeared in the continuous wear process, resulting in a lower coefficient of friction and good wear prevention performance, making MGs a promising material for applications in tribological materials, electrode materials, energy storage and sensor applications. Declarations Acknowledgments The authors thank Woldiya University for facilitating the experimental works and funding only chemicals. Author contributions Muhabie Adema Ali designed the research, performed all experiments and wrote the paper. Girma Wubshet Mekonnen edited and revised the paper. All authors discussed about the results and commented on the paper. Conflict of interest The authors declare no competing of interest. Data and code availability All data obtained or discussed during this study are included in this article. Ethical approval No experiments have been conducted on animal and human tissue. Supplementary Materials Figure S 1 shows the images of MGs (before and after annealing) obtained by AFM. Image of the MG which is annealed for 60 minutes reveals the laminated structure whereas the MG which is not annealed revealed high roughness. Figure S 2 , showing the elastic modulus, E values of the MGs annealed at 10, 30, and 60 min. The average elastic modulus of metallic glass was increased as a result of the annealing time rise from 10 to 60 min. The H/E ratios of all samples were shown in Figures S3 and increased with increasing annealing time. Figure S4 shows AFM images of the three thin film MGs after scratch test at normal forces, 0.9 μN. The images demonstrate the appearances of different features of the wear track such as different wear depth and wear volume for as-cast and MG and annealed for 30 min. Shallow groove depths were seen for MGs but no scratch track was observed for MG annealed for 60 minutes. References Zhao, X.; Sun, J.; Yu, M.; Zhang, M.; Liu, F.; Zhang, Y.; Liu, L., Effects of heat treatment on the thermal, mechanical and corrosion properties of deformed Zr-based bulk metallic glasses. Materials Chemistry and Physics 2020, 256 , 123705. Li, M.-f.; Wang, D.-p.; Malomo, B.; Yang, L., Microstructural mechanisms of tuning the deformation behaviors in annealed metallic glasses. Journal of Alloys and Compounds 2021, 876 , 160029. 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Journal of Non-Crystalline Solids 2023, 601 , 122047; (b) Wang, W.; Mraied, H.; Diyatmika, W.; Chu, J. P.; Li, L.; Cai, W., Effects of nanoscale chemical heterogeneity on the wear, corrosion, and tribocorrosion resistance of Zr-based thin film metallic glasses. Surface and Coatings Technology 2020, 402 , 126324. Additional Declarations No competing interests reported. Supplementary Files supplementalfiles.docx Cite Share Download PDF Status: Posted Version 1 posted 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. We do this by developing innovative software and high quality services for the global research community. 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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-3109079","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":215265623,"identity":"4c105258-7bd7-442f-9922-905d6193d148","order_by":0,"name":"Adem Ali Muhabie","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA/ElEQVRIiWNgGAWjYDACdsYGBiBKYGBvbDj4oQIowszcgF8LM0wLz+GDjyXOQEXwawFisBaJtGQD3jYGCBcf4G9mbt3wcYddHj9DjpmE5LzaaP52oJYfFdtwapE4zNh2c+aZ5GLJhjNmEoXbjufOOMzYwNhz5jZua4BabvO2MSduONgDtGXbsdwGoBZmoCBOHfIQLfWJ+w/zmEnwzjmWO5+QFgOIlsOJG9jYgN5vqMndQEiLIdgvbceLJc4wAwP52IHcjUAtB/H5Re54+7MbH9uq8/jnPwRGZU1d7rzzhw8++FGBx/to4DCYPEC0eiCoI0XxKBgFo2AUjBAAAO9tZB+MUMLfAAAAAElFTkSuQmCC","orcid":"","institution":"Woldia University","correspondingAuthor":true,"submittingAuthor":false,"prefix":"","firstName":"Adem","middleName":"Ali","lastName":"Muhabie","suffix":""},{"id":215265625,"identity":"c516f100-09b4-409e-b7c6-19040ef7a853","order_by":1,"name":"Wubshet Mekonnen Girma","email":"","orcid":"","institution":"Wollo University","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Wubshet","middleName":"Mekonnen","lastName":"Girma","suffix":""}],"badges":[],"createdAt":"2023-06-26 06:29:32","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-3109079/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-3109079/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":39587341,"identity":"fd964e9d-c6b9-4a21-a88f-ba6fa7ecb5fa","added_by":"auto","created_at":"2023-07-05 15:24:38","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":144287,"visible":true,"origin":"","legend":"\u003cp\u003eAFM image showing the microstructure of MG at annealing time 30(a) and 60min (b). (c) Indentation profile of TLMG and BMG. (d) Hardness of TLMGs for annealing times of 10, 30, and 60 minutes.\u003c/p\u003e","description":"","filename":"1.png","url":"https://assets-eu.researchsquare.com/files/rs-3109079/v1/01ce4b77bb4f284b0f660039.png"},{"id":39587342,"identity":"be4ceebf-fc6f-4ceb-b4aa-c87c65690b7f","added_by":"auto","created_at":"2023-07-05 15:24:38","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":76741,"visible":true,"origin":"","legend":"\u003cp\u003e(a) coefficient of friction for BMG and TLMG with displacement. (b) Friction force of TLMG at different annealing times. Coefficient of friction as a function of the number of scan cycles (c) and annealing time (d).\u003c/p\u003e","description":"","filename":"2.png","url":"https://assets-eu.researchsquare.com/files/rs-3109079/v1/94f1b8734aba330cf42d8655.png"},{"id":39588911,"identity":"5a8a72a5-84db-48fa-8433-f3819d4d8aaf","added_by":"auto","created_at":"2023-07-05 15:32:38","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":207545,"visible":true,"origin":"","legend":"\u003cp\u003eAFM images after nanoscratch tests over (a) the as-cast TLMG and after annealing for (b) 30 and (c) 60 min at normal force of 4 μN and the corresponding (d) wear depth of each sample at a load of 4μN.\u003c/p\u003e","description":"","filename":"3.png","url":"https://assets-eu.researchsquare.com/files/rs-3109079/v1/3fdd1cd95c8959c5686cbef2.png"},{"id":39587344,"identity":"f312a1fd-1007-4056-a391-ca64d9f7a098","added_by":"auto","created_at":"2023-07-05 15:24:38","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":77111,"visible":true,"origin":"","legend":"\u003cp\u003eshows the wear rate as a function of annealing time for (a) 4 μN and (b) 0.9 μN. (c) contact area as a function of annealing time for 0.9 and 4 μN.(d) wear volume for each sample as a function of sliding displacement for 4 μN.\u003c/p\u003e","description":"","filename":"4.png","url":"https://assets-eu.researchsquare.com/files/rs-3109079/v1/baa3c1050264376c3369b4f6.png"},{"id":39737887,"identity":"4b56ae40-708c-4a4d-9f88-3693a96aa9f9","added_by":"auto","created_at":"2023-07-08 15:59:31","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":962047,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-3109079/v1/7c1596a8-fbcd-4b7f-9dfe-8f3edea286c8.pdf"},{"id":39587345,"identity":"dd6f07d4-3e9f-4a1a-97a6-8b7323a89027","added_by":"auto","created_at":"2023-07-05 15:24:38","extension":"docx","order_by":1,"title":"","display":"","copyAsset":false,"role":"supplement","size":649750,"visible":true,"origin":"","legend":"","description":"","filename":"supplementalfiles.docx","url":"https://assets-eu.researchsquare.com/files/rs-3109079/v1/a014868d9c4ffc046c359a89.docx"}],"financialInterests":"No competing interests reported.","formattedTitle":"Annealing Effect on Mechanical and Tribological behaviour of Nanoscale Mechanics of Thin Layer Metallic Glasses for Engineering Material Applications","fulltext":[{"header":"1. Introduction","content":"\u003cp\u003eBulk metallic glasses (BMGs) are the focus of a demanding research areas for researchers around the world.\u003csup\u003e\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e\u003c/sup\u003e BMGs are structurally amorphous metallic alloys, and their compositions are mixed to avoid crystallization during cooling from the melt.\u003csup\u003e\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e\u003c/sup\u003e BMGs exhibit extraordinary outstanding properties such as high elasticity,\u003csup\u003e\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e\u003c/sup\u003e high hardness, appreciable toughness, good tribology prosperity\u003csup\u003e\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e\u003c/sup\u003e and superior corrosion resistance.\u003csup\u003e\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e\u003c/sup\u003e In addition, due to the lack of long-range atomic order in BMGs offers them exceptional mechanical and physic-chemical properties,\u003csup\u003e\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e\u003c/sup\u003e related to conventional crystalline metallic materials, making them a promising class of engineering materials. MGs are also novel wear-resistant\u003csup\u003e\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e\u003c/sup\u003e and low friction materials with high intensive demand in tribological applications.\u003csup\u003e\u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e\u003c/sup\u003e Zr-based MGs display a smaller friction coefficient than other metals during dry sliding conditions.\u003csup\u003e\u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e\u003c/sup\u003e In previous work we reported that the wear resistance of CuZr-based MG materials is comparable to classical tribological ceramics but superior to that of high-performance steel\u003csup\u003e\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e\u003c/sup\u003e. Metallic glasses can be formed thermoplastically in the supercooled liquid regime. These special properties of MGs make them a perfect candidates for multipurpose application, such as microgears, media-storage devices,\u003csup\u003e\u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e\u003c/sup\u003e building construction, bio-implant,\u003csup\u003e\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e\u003c/sup\u003e electrode materials,\u003csup\u003e\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e\u003c/sup\u003e energy conversion/storage\u003csup\u003e14\u003c/sup\u003e and sensors.\u003csup\u003e\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e\u003c/sup\u003e Developing a proper alloy composition determines both structural and chemical homogeneities, nanometer-sized ductile dendrite homogeneities as a result of annealing have proven their value in increasing plasticity compared to the as-cast MG. Presence of such homogeneities promotes the plastic formability because they increase nucleation and branching.\u003csup\u003e\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e\u003c/sup\u003e At the macroscale the tribological mechanisms are complex and involve a combination of plasticity,\u003csup\u003e\u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e\u003c/sup\u003e transformation and structural relaxations with structural changes.\u003csup\u003e\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e 19\u003c/sup\u003e There is no clear and unique correlation between the hardness/modulus and the tribological behavior of metallic glasses has been established so far. Hence, the contributions of hardness, elastic modulus, and thermal treatment on wear resistance and nanoscale friction of thin MG compared to bulk and as-cast counterpart should be studied.\u003csup\u003e\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e\u003c/sup\u003e Furthermore, improper alloy composition of crystallites, rough surface, and surface reaction structural relations are the cause for their high friction, poor wear resistance, and poor plasticity limit the long-term performance of metallic glasses at ambient temperature.\u003csup\u003e\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e\u003c/sup\u003e In addition, localized and inhomogeneous decomposition at ambient temperature, free volume, and accompanied with strain lead to early failure of deformation, which still limits the long-term service of MGs for structural applications. \u003csup\u003e\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e\u003c/sup\u003e To avoid this catastrophic failure, this investigation aims to study mechanical properties like elastic moduli or hardness, inhomogeneous, and microstructure of metallic glasses in addition to thermal treatment play a great role to provide information about the interrelation mechanism with that of nanoscale friction and nanoscale wear rate. In this, we design a proper alloy composition, characterize the structure, mechanical and tribological properties of thin layer amorphous Zr60Cu25Al5Ag5Ni5 by annealing at various length times ( 10,30 and 60 minutes) and we report and discuss the load dependence of friction and wear resistance of metallic glasses.\u003c/p\u003e"},{"header":"2. Experimental section","content":"\u003cp\u003e \u003cb\u003eSample preparation and characterization methods\u003c/b\u003e \u003c/p\u003e \u003cp\u003eA Zr\u003csub\u003e60\u003c/sub\u003eCu\u003csub\u003e25\u003c/sub\u003eAl\u003csub\u003e5\u003c/sub\u003eAg\u003csub\u003e5\u003c/sub\u003eNi\u003csub\u003e5\u003c/sub\u003e metallic glass was prepared as follows. The inorganic alloys of metals such Zr, Al,Cu,Ni,Ag above 99.9 Wt % in purity were mixed and cast on Zr-gettered. The cast alloys were placed on a copper cruisers compressed with a quartz tubes at a temperature of 825\u0026thinsp;\u0026plusmn;\u0026thinsp;25\u0026deg;C. In order to insure the homogeneous metals in the metallic glass, melting of the alloy should be repeated for five times. 200 mm ribbons of MG were prepared from large melt spinning copper wheel ejection argon gas. 200 nm MG were coated on silicon wafer by sputtering method from the ribbon. The samples were annealed for 10 min, 30 min, and 60 min at 450 \u003csup\u003eo\u003c/sup\u003eC, and then cooled the samples at ambient temperature in a vacuum place. For comparison, with one non-annealed sample representing as-prepared or as-cast samples. Nanoindentation experiments were operated using Hysitron Triboindenter TI-750 L (Hysitron, Inc., Minneapolis, MN USA) for 0.9 and 4 \u0026micro;N at a constant loading/unloading rate of 0.1\u0026micro;N/s. four indentations were performed to prove the accuracy of data from the same sample. Nano-scratch tests were performed at a velocity of \u0026micro;m s\u003csup\u003e\u0026ndash;\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e\u003c/sup\u003e with applied force of 0.9 and 4 \u0026micro;N as a function of displacement to evaluate the wear rate, wear depth, coefficient of friction, and contact area. Nano-scratch tests were repeated for three times.\u003c/p\u003e"},{"header":"3. Results and Discussion","content":"\u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003e3.1. Microstructure and mechanical properties\u003c/h2\u003e \u003cp\u003eAnnealing thin layer metallic glass at various length times (10, 30, and 60 minutes) was selected as test parameters because of their differences in microstructure, mechanical and tribological properties of Zr60Cu25Al5Ag5Ni5 MG. In order to explore the annealing effect on microstructure and surface morphology, the atomic force spectroscopy (AFM) has been used. The AFM images in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e (a) and (b) clearly show the presence of nanoparticles with sizes of around 5.96 nm and 5.05 nm for the specimens annealed for 30 and 60, respectively. The images show the nanoscale inhomogeneity indicating chemical relaxation, with the evolution of atomic scale upon annealing below the glass transition temperature. The AFM topography results are in line with previously reported results.\u003csup\u003e\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e\u003c/sup\u003e These local compositional fluctuations or random arrangements of atoms influence the plasticity of MGs, without high loss of strength or hardness. Arrangement of atoms can affect atomic transport, hardness, elastic modulus, magnetic, wear rate, friction and electrochemical properties.\u003csup\u003e\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e, \u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e\u003c/sup\u003e Annealing results for chemical reordering leads to phase transition of MG, depending on the interatomic distance of atoms and improved plasticity of MG. Short interatomic distance between transition metals in the alloy composition may be existed only in the metallic glass.\u003csup\u003e\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e\u003c/sup\u003e Representative indentations on the BMG and TLMG of load-displacement curves are shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003eb. The surface indentation profiles show that the indented depth of TLMG is shallow compared to BMG, indicating lower material loss and higher wear resistance compared to the bulk MG.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe depth dependence of the mechanical properties, the Hardness (H), and elastic modulus (\u003cem\u003eE)\u003c/em\u003e values of the MGs were determined for samples which were annealed for different times. The average hardness of metallic glasses increased from 9.75 to 13.4 GPa (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ed) as the annealing time rose from zero to 60 min, as result of atomic reordering and structural relaxation that occurred at longer annealing times. Atomic chemical ordering in the glassy phase is smaller than in the crystalline phase, which indicates the improvement of mechanical and tribological properties.\u003csup\u003e\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e\u003c/sup\u003e The elastic modulus improved from 142.49 to 162.64 with increasing annealing time (figure S2). With respect to elastic behavior, describing the metallic glasses properties not only by hardness and modulus, but by using a hardness/ modulus (H/E) ratio indicating the elastic strain to failure.\u003csup\u003e\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e\u003c/sup\u003e The average H/E ratio was also increased as the annealing time increases as shown Figure S\u003csub\u003e3\u003c/sub\u003e. The H/E ratio indicates the plasticity of sample deformation. Materials with higher H/E ratio may reveal a structural transition from elastic to plastic behavior at higher stress levels compared to those with lower H/E ratio. H/E is a strong pointer of a good wear resistance of material. The large H/E value indicating material has high resist plastic deformation and the most durable MGs can be used for many applications, which were annealed at different times individually to obtain heat-dependent surface properties. The mechanical properties observed in this research are comparable to the previously works.\u003csup\u003e\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e, \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e3.2 Tribological properties\u003c/h2\u003e \u003cdiv id=\"Sec6\" class=\"Section3\"\u003e \u003ch2\u003e\u003cb\u003e3.2.1 Coefficient of friction\u003c/b\u003e\u003c/h2\u003e \u003cp\u003eFigure \u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e displays the behavior of friction of thin film metallic glasses surface as a function of displacement, annealing time, and number of wear cycles. Friction coefficients of bulk and thin layer metallic glass as a function of sliding displacement were shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003ea. The coefficient of friction is larger in bulk Mg than thin film MG. The saw-tooth appearance of bulk MG is revealed, indicating shear banding and plow formation as the indenter deformed the matrix as a result of the absence of elastic plasticity. It might be difficult for the movement atom in all direction while the indenter scratching the surface due to the presence or some extent of crystallinity. As the annealing time increases, reducing the grain size, annealing-induced embrittlement of metallic glasses a result in a lower friction coefficient and excellent wear resistance. Figure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003eb demonstrates that for all annealed MGs, the reduction of friction force was observed as a function of sliding distance under load 4 \u0026micro;N. The value of friction force dropped gradually when the annealing time increases from zero to 60 min. The friction force of highly annealed MGs is much lower than that of the cast- MG. The graph of friction force for a cast MG revealed sawtooth, many small peaks, indicating the rough surface, deformation of surface matrix and weak wear resistance performance, whereas the graph of highly annealed MG showed a smooth peak as increasing the annealing time indicating the laminated surface, mechanical and tribology properties were successfully improved.\u003csup\u003e\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e, \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e\u003c/sup\u003e The coefficient of friction as a function of the number of scratch cycles after annealing for different time is shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003ec under applied load of 0.9 \u0026micro;N. The coefficient of friction initially seems increases with the number of wear cycles and then reaches a steady value at for all samples. The increase in the coefficient of friction during the initial wear cycle is related to a larger plowing depth, as reported previously.\u003csup\u003e\u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e\u003c/sup\u003e In addition, the coefficient of friction of the thin film MGs slightly decreases with increasing temperature aging time. The effects of annealing time on the coefficient of friction of thin film MGs has been observed in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003ed under 0.9 \u0026micro;N and 4 \u0026micro;N applied force. The mean coefficient of friction value was similar for both test conditions. It is clear that the value of friction coefficient is about 0.062 for the non-annealed, while for the MG annealed for 60 min, the coefficient of friction slightly decreased (\u0026lt;\u0026thinsp;0.03) under 0.9 \u0026micro;N applied force. The friction coefficient decreases with increasing annealing time in both conditions, in line with previous reports,\u003csup\u003e\u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e\u003c/sup\u003e demonstrating the possibility of reduction of friction coefficient by tuning the surface patterning with aging temperature.\u003csup\u003e\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e\u003c/sup\u003e It is reported that most of frictional work during the wear process create heat energy which modifies the tribological behaviors of Nano-scratched surfaces such as forming delocalized free metal ions for chemical reordering or even heating interfacial contact materials.\u003csup\u003e\u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec7\" class=\"Section3\"\u003e \u003ch2\u003e3.2.2 Nanowear depth\u003c/h2\u003e \u003cp\u003eNano-scratch test was conducted on the TLMGs which were annealed at different time individually to obtain heat-dependent surface properties. Figure\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e shows the AFM images of the wear track surface of three MGs after nanoscratch test using normal forces, 4 \u0026micro;N. The nanoscratched MGs surface of AFM images at normal force FN\u0026thinsp;=\u0026thinsp;0.9 \u0026micro;N is shown in figure S\u003csub\u003e3\u003c/sub\u003e. All nanoscratches wear track images display different features in both loads. AFM images demonstrate different wear depth and contact area of MGs for different annealing times. Wide and deep grooves were shown (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ea) for non-annealed MG but a shallow scratch tracks were observed for highly annealed MGs (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ec). The wear debris has been seen for as-cast which are material accumulation on the lateral sides, which indicates the serious plastic deformation during friction. The wear rate and volume loss for 4 \u0026micro;N were significantly higher than 0.9 \u0026micro;N test condition, in line with previously reported.\u003csup\u003e31a\u003c/sup\u003e The nanoscratch wear track images of the three thin film MGs at normal forces, 0.9 \u0026micro;N were shown Figures S4. The wear depth of each scratch sample was determined and shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ed. The values of the wear depth decrease from 201.56 nm for the non-annealed to 148.43, 37.32, and 25.27 nm for the TLMG annealed for 10, 30 and 60 min, respectively in line with previous reports. The wear depth is equivalent to both the height of the accumulated material and the depth of the scratch. It can be seen that the thin layer MG which is annealed for a long period of time that revealed a shallow wear track, indicating there is clearly elastic recovery behind the indenter and exhibited excellent wear resistance performance and very low coefficient of friction. \u003csup\u003e\u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e32\u003c/span\u003e\u003c/sup\u003e Wear resistance improved with annealing time increases, as a result of good hardness and elastic modulus of materials which lead to too much reduction of friction while plowing the MG layer on an indenter.\u003csup\u003e\u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e33\u003c/span\u003e\u003c/sup\u003e During annealing, anti-wear and coefficient of friction in all conditions improved on surface of the film, there might be dangling bonds (immobilized free radical), therefore, annealing needs to be satisfied this bond by surface reconstruction, by charge transfer, by chemical absorption. \u003csup\u003e\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e 23, 35\u003c/sup\u003e\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec8\" class=\"Section3\"\u003e \u003ch2\u003e3.2.3. Wear rate\u003c/h2\u003e \u003cp\u003eThe variations of wear rate as a function of displacement for each annealed sample at a normal force of 0.9 and 4\u0026micro;N load are shown in figures (4a \u0026amp;4b). It is found that for all samples, the wear rate first decreases, and then steady-state wear is observed as a function of the sliding distance under both loads and all annealing time. The wear rate dropped continuously with increasing annealing time and for both test conditions. The wear rates for 4 \u0026micro;N were meaningfully higher than 0.9 N test conditions, in line with previous work.\u003csup\u003e\u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e\u003c/sup\u003e More importantly, the wear rate of the highly annealed MGs is much lower than that of the non-annealed MG. Figure\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ec shows the contact area as a function of annealing time for 0.9 and 4 \u0026micro;N. As can be seen, the scratch contact area decreases with increasing the annealing time for both loads. Contact areas for 4 \u0026micro;N were meaningfully higher than 0.9 N test conditions, in line with previous work. This behavior of the contact area is depending on the mechanical properties (hardness and elastic modulus) and the microstructure of the film.\u003csup\u003e\u003cspan citationid=\"CR37\" class=\"CitationRef\"\u003e37\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eFigure \u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ed shows the wear volume of the scratched area of samples for normal force, 4\u0026micro;N. As it is found that the wear volume decreases with increasing annealing time as a result of improved elastic modulus or high H/E ratio and low friction coefficient. This will be the reason for the high wear resistance of materials.\u003csup\u003e\u003cspan citationid=\"CR38\" class=\"CitationRef\"\u003e38\u003c/span\u003e\u003c/sup\u003e Researchers regarded that the real area of contact and material properties such as microstructure, surface topography, and mechanical properties are the key factors that govern the wear rate.\u003csup\u003e\u003cspan citationid=\"CR39\" class=\"CitationRef\"\u003e39\u003c/span\u003e\u003c/sup\u003e\u003c/p\u003e \u003c/div\u003e \u003c/div\u003e"},{"header":"4. Conclusions","content":"\u003cp\u003eIn summary, we have studied the surface morphology and microstructure by atomic force microscope, mechanical properties by nano-indentation experiment, and tribological properties by Nano-scratch experiment of MG films annealed for various lengths of time. The hardness value, the average elastic modulus of the samples increased with increasing the annealing time, the annealed samples revealed better properties than as-cast MG. The H/E ratio of all samples increased with increasing annealing time. The nanoscratch results indicate that annealing at different time significantly reduces friction and improves wear resistance performance. In addition, the decrease of wear depth, wear volume, and contact area under annealing effect appeared in the continuous wear process, resulting in a lower coefficient of friction and good wear prevention performance, making MGs a promising material for applications in tribological materials, electrode materials, energy storage and sensor applications.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eAcknowledgments\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors\u003cstrong\u003e\u0026nbsp;\u003c/strong\u003ethank Woldiya University for facilitating the experimental works and funding only chemicals.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAuthor contributions\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eMuhabie Adema Ali designed the research, performed all experiments and wrote the paper. Girma Wubshet Mekonnen edited and revised the paper. All authors discussed about the results and commented on the paper.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eConflict of interest\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors declare no competing of interest.\u0026nbsp;\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eData and code availability\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eAll data\u0026nbsp;obtained or discussed during this study\u0026nbsp;are included in this article.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eEthical approval\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eNo experiments have been conducted on animal and human tissue.\u0026nbsp;\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eSupplementary Materials\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eFigure S\u003csub\u003e1\u003c/sub\u003e shows the images of MGs (before and after annealing) obtained by AFM. Image of the MG which is annealed for 60 minutes reveals the laminated structure whereas the MG which is not annealed revealed high roughness. \u0026nbsp;Figure\u0026nbsp;S\u003csub\u003e2\u003c/sub\u003e, showing the elastic modulus, \u003cem\u003eE\u0026nbsp;\u003c/em\u003evalues of the MGs annealed at 10, 30, and 60 min. The average elastic modulus of metallic glass was increased as a result of the annealing time rise from 10 to 60 min. \u0026nbsp; The H/E ratios of all samples were shown in Figures S3 and increased with increasing annealing time. Figure S4 shows AFM images of the three thin film MGs after scratch test at normal forces, 0.9 \u0026mu;N. The images demonstrate the appearances of different features of the wear track such as different wear depth and wear volume for as-cast and MG and annealed for 30 min. Shallow groove depths were seen for MGs but no scratch track was observed for MG annealed for 60 minutes.\u0026nbsp;\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n\u003cli\u003eZhao, X.; Sun, J.; Yu, M.; Zhang, M.; Liu, F.; Zhang, Y.; Liu, L., Effects of heat treatment on the thermal, mechanical and corrosion properties of deformed Zr-based bulk metallic glasses. \u003cem\u003eMaterials Chemistry and Physics \u003c/em\u003e\u003cstrong\u003e2020,\u003c/strong\u003e \u003cem\u003e256\u003c/em\u003e, 123705.\u003c/li\u003e\n\u003cli\u003eLi, M.-f.; Wang, D.-p.; Malomo, B.; Yang, L., Microstructural mechanisms of tuning the deformation behaviors in annealed metallic glasses. \u003cem\u003eJournal of Alloys and Compounds \u003c/em\u003e\u003cstrong\u003e2021,\u003c/strong\u003e \u003cem\u003e876\u003c/em\u003e, 160029.\u003c/li\u003e\n\u003cli\u003eMeylan, C.; Papparotto, F.; Nachum, S.; Orava, J.; Miglierini, M.; Basykh, V.; Ferenc, J.; Kulik, T.; Greer, A., Stimulation of shear-transformation zones in metallic glasses by cryogenic thermal cycling. \u003cem\u003eJournal of Non-Crystalline Solids \u003c/em\u003e\u003cstrong\u003e2020,\u003c/strong\u003e \u003cem\u003e548\u003c/em\u003e, 120299.\u003c/li\u003e\n\u003cli\u003eZhou, Q.; Du, Y.; Ren, Y.; Kuang, W.; Han, W.; Wang, H.; Huang, P.; Wang, F.; Wang, J., Investigation into nanoscratching mechanical performance of metallic glass multilayers with improved nano-tribological properties. \u003cem\u003eJournal of Alloys and Compounds \u003c/em\u003e\u003cstrong\u003e2019,\u003c/strong\u003e \u003cem\u003e776\u003c/em\u003e, 447-459.\u003c/li\u003e\n\u003cli\u003eLiang, D.; Tseng, J.-C.; Liu, X.; Cai, Y.; Xu, G.; Shen, J., Investigation of the structural heterogeneity and corrosion performance of the annealed Fe-based metallic glasses. \u003cem\u003eMaterials \u003c/em\u003e\u003cstrong\u003e2021,\u003c/strong\u003e \u003cem\u003e14\u003c/em\u003e (4), 929.\u003c/li\u003e\n\u003cli\u003eSalehan, R.; Shahverdi, H. 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P.; Li, L.; Cai, W., Effects of nanoscale chemical heterogeneity on the wear, corrosion, and tribocorrosion resistance of Zr-based thin film metallic glasses. \u003cem\u003eSurface and Coatings Technology \u003c/em\u003e\u003cstrong\u003e2020,\u003c/strong\u003e \u003cem\u003e402\u003c/em\u003e, 126324.\u003c/li\u003e\n\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":false,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"Atomic force microscopy (AFM), annealing, coefficient of friction, wear rate, nanoscratch, thin layer metallic glass.","lastPublishedDoi":"10.21203/rs.3.rs-3109079/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-3109079/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eA new and unique alloy formulation design strategies has been developed in order to fabricate thin layered metallic glasses (TFMG) with superior fracture resistance and low coefficient of friction (COF) during nano-scraching test. Due to the outstanding properties, TFMG could be applied for different uses uch as surface coating, biomedical, bio implant, electronic devices, spacecraft and railway, all of which need surface fracture resistance. The fabricated Zr-based metallic glass having the composition of Zr60Cu25Al5Ag5Ni5 (at.%) was annealed for 10, 30, and 60 min below the glass transition temperature. Nanoindentation and nanoscratch tests were used to investigate mechanical and nanotribological properties. Atomic force microscopy (AFM) was used to examine the surface morphology and microstructures. The annealing effect and applied forces change over the chemical structure and stability, morphological change, elastic modulus, hardness, wear rate, and coefficient of friction of the samples were systematically investigated. The nano-indentation data indicated that the hardness and average elastic modulus of the samples increased with increasing annealing time, compared with those of the as-cast MG. More intriguingly, the coefficient of friction and wear rate decreases when the annealing time increases compared to as-cast MG. Furthermore, the continuous wear process, wear depth, wear track volume, and contact area decreases with increasing annealing time, as a result of the improvement of the mechanical and tribological properties of the thin-layered MGs. This study can be a reference to the design protocol to prepare novel a-MGs, which have outstanding mechanical and tribological behavior for engineering material applications.\u003c/p\u003e","manuscriptTitle":"Annealing Effect on Mechanical and Tribological behaviour of Nanoscale Mechanics of Thin Layer Metallic Glasses for Engineering Material Applications","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2023-07-05 15:24:33","doi":"10.21203/rs.3.rs-3109079/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"ade2ff50-416c-49f9-8419-355db11f1401","owner":[],"postedDate":"July 5th, 2023","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2023-07-08T15:59:19+00:00","versionOfRecord":[],"versionCreatedAt":"2023-07-05 15:24:33","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-3109079","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-3109079","identity":"rs-3109079","version":["v1"]},"buildId":"7rjqhiLT3MXkJMwkYKINL","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}