Structural features and tribological properties of multilayer high-temperature plasma coatings

Vol. 26 No. 3 2024 3 EDITORIAL COUNCIL EDITORIAL BOARD EDITOR-IN-CHIEF: Anatoliy A. Bataev, D.Sc. (Engineering), Professor, Rector, Novosibirsk State Technical University, Novosibirsk, Russian Federation DEPUTIES EDITOR-IN-CHIEF: Vladimir V. Ivancivsky, D.Sc. (Engineering), Associate Professor, Department of Industrial Machinery Design, Novosibirsk State Technical University, Novosibirsk, Russian Federation Vadim Y. Skeeba, Ph.D. (Engineering), Associate Professor, Department of Industrial Machinery Design, Novosibirsk State Technical University, Novosibirsk, Russian Federation Editor of the English translation: Elena A. Lozhkina, Ph.D. (Engineering), Department of Material Science in Mechanical Engineering, Novosibirsk State Technical University, Novosibirsk, Russian Federation The journal is issued since 1999 Publication frequency – 4 numbers a year Data on the journal are published in «Ulrich's Periodical Directory» Journal “Obrabotka Metallov” (“Metal Working and Material Science”) has been Indexed in Clarivate Analytics Services. Novosibirsk State Technical University, Prospekt K. Marksa, 20, Novosibirsk, 630073, Russia Tel.: +7 (383) 346-17-75 http://journals.nstu.ru/obrabotka_metallov E-mail: metal_working@mail.ru; metal_working@corp.nstu.ru Journal “Obrabotka Metallov – Metal Working and Material Science” is indexed in the world's largest abstracting bibliographic and scientometric databases Web of Science and Scopus. Journal “Obrabotka Metallov” (“Metal Working & Material Science”) has entered into an electronic licensing relationship with EBSCO Publishing, the world's leading aggregator of full text journals, magazines and eBooks. The full text of JOURNAL can be found in the EBSCOhost™ databases.

OBRABOTKAMETALLOV Vol. 26 No. 3 2024 4 EDITORIAL COUNCIL EDITORIAL COUNCIL CHAIRMAN: Nikolai V. Pustovoy, D.Sc. (Engineering), Professor, President, Novosibirsk State Technical University, Novosibirsk, Russian Federation MEMBERS: The Federative Republic of Brazil: Alberto Moreira Jorge Junior, Dr.-Ing., Full Professor; Federal University of São Carlos, São Carlos The Federal Republic of Germany: Moniko Greif, Dr.-Ing., Professor, Hochschule RheinMain University of Applied Sciences, Russelsheim Florian Nürnberger, Dr.-Ing., Chief Engineer and Head of the Department “Technology of Materials”, Leibniz Universität Hannover, Garbsen; Thomas Hassel, Dr.-Ing., Head of Underwater Technology Center Hanover, Leibniz Universität Hannover, Garbsen The Spain: Andrey L. Chuvilin, Ph.D. (Physics and Mathematics), Ikerbasque Research Professor, Head of Electron Microscopy Laboratory “CIC nanoGUNE”, San Sebastian The Republic of Belarus: Fyodor I. Panteleenko, D.Sc. (Engineering), Professor, First Vice-Rector, Corresponding Member of National Academy of Sciences of Belarus, Belarusian National Technical University, Minsk The Ukraine: Sergiy V. Kovalevskyy, D.Sc. (Engineering), Professor, Vice Rector for Research and Academic Aff airs, Donbass State Engineering Academy, Kramatorsk The Russian Federation: Vladimir G. Atapin, D.Sc. (Engineering), Professor, Novosibirsk State Technical University, Novosibirsk; Victor P. Balkov, Deputy general director, Research and Development Tooling Institute “VNIIINSTRUMENT”, Moscow; Vladimir A. Bataev, D.Sc. (Engineering), Professor, Novosibirsk State Technical University, Novosibirsk; Vladimir G. Burov, D.Sc. (Engineering), Professor, Novosibirsk State Technical University, Novosibirsk; Aleksandr N. Korotkov, D.Sc. (Engineering), Professor, Kuzbass State Technical University, Kemerovo; Dmitry V. Lobanov, D.Sc. (Engineering), Associate Professor, I.N. Ulianov Chuvash State University, Cheboksary; Aleksey V. Makarov, D.Sc. (Engineering), Corresponding Member of RAS, Head of division, Head of laboratory (Laboratory of Mechanical Properties) M.N. Miheev Institute of Metal Physics, Russian Academy of Sciences (Ural Branch), Yekaterinburg; Aleksandr G. Ovcharenko, D.Sc. (Engineering), Professor, Biysk Technological Institute, Biysk; Yuriy N. Saraev, D.Sc. (Engineering), Professor, V.P. Larionov Institute of the Physical-Technical Problems of the North of the Siberian Branch of the RAS, Yakutsk; Alexander S. Yanyushkin, D.Sc. (Engineering), Professor, I.N. Ulianov Chuvash State University, Cheboksary

Vol. 26 No. 3 2024 5 CONTENTS OBRABOTKAMETALLOV TECHNOLOGY Sukhov A.V., Sundukov S.K., Fatyukhin D.S. Assembly of threaded and adhesive-threaded joints with the application of ultrasonic vibrations...................................................................................................................................... 6 Baraboshkin K.A., Adigamov R.R., Yusupov V.S., Kozhevnikova I.A., Karlina A.I. Thermomechanical rolling in well casing production (research review)......................................................................................................................... 24 Dwivedi R., Somatkar A., Chinchanikar S. Modeling and optimization of roller burnishing of Al6061-T6 process for minimum surface roughness, better microhardness and roundness................................................................................ 52 Ilinykh A.S., Pikalov A.S., Miloradovich V.K., Galay M.S. Experimental studies of rail grinding modes using a new high-speed electric drive...................................................................................................................................................... 66 Karlina Yu.I., Konyukhov V.Yu., Oparina T.A. Assessment of the possibility of resistance butt welding of pipes made of heat-resistant steel 0.15C-5Cr-Mo................................................................................................................................... 79 Gimadeev M.R., Stelmakov V.A., Shelenok E.A. Product life cycle: machining processes monitoring and vibroacoustic signals fi lterings.................................................................................................................................................................... 94 EQUIPMENT. INSTRUMENTS Zakovorotny V.L., Gvindjiliya V.E., Kislov K.V. Information properties of frequency characteristics of dynamic cutting systems in the diagnosis of tool wear....................................................................................................................... 114 Ablyaz T.R., Blokhin V.B., Shlykov E.S., Muratov K.R., Osinnikov I.V. Features of the use of tool electrodes manufactured by additive technologies in electrical discharge machining of products....................................................... 135 Sidorov E.A., GrinenkoA.V., ChumaevskyA.V., Panfi lovA.O., Knyazhev E.O., NikolaevaA.V., CheremnovA.M., Rubtsov V.E., Utyaganova V.R., Osipovich K.S., Kolubaev E.A. Patterns of reverse-polarity plasma torches wear during cutting of thick rolled sheets..................................................................................................................................... 149 MATERIAL SCIENCE Semin V.O., Panfi lov A.O., Utyaganova V.R., Vorontsov A.V., Zykova A.P. Corrosion properties of CuAl9Mn2/ER 321 composites formed by dual-wire-feed electron beam additive manufacturing................................ 163 Dewangan R., Sharma B.P., Sharma S.S. Investigation of hardness behavior in aluminum matrix composites reinforced with coconut shell ash and red mud using Taguchi analysis............................................................................ 179 Saprykina N.А., Saprykin A.А., Sharkeev Y.P., Ibragimov E.А. The eff ect of technological parameters on the microstructure and properties of the AlSiMg alloy obtained by selective laser melting......................................................... 192 Burdilov A.A., Dovzhenko G.D., Bataev I.A., Bataev A.A. Methods of synchrotron radiation monochromatization (research review).................................................................................................................................................................. 208 Burkov A.A., Dvornik M.A., Kulik M.A., Bytsura A.Yu. Wear resistance and corrosion behavior of Cu-Ti coatings in SBF solution..................................................................................................................................................................... 234 Pugacheva N.B., Bykova T.M., Sirosh V.A., MakarovA.V. Structural features and tribological properties of multilayer high-temperature plasma coatings........................................................................................................................................ 250 Sharma B.P., Dewangan R., Sharma S.S. Characterizing the mechanical behavior of eco-friendly hybrid polymer composites with jute and Sida cordifolia fi bers.................................................................................................................... 267 Kornienko E.E., Gulyaev I.P., Smirnov A.I., Plotnikova N.V., Kuzmin V.I., Golovakhin V., Tambovtsev A.S., Tyryshkin P.A., Sergachev D.V. Fine structure features of Ni-Al coatings obtained by high velocity atmospheric plasma spraying.................................................................................................................................................................... 286 EDITORIALMATERIALS 298 FOUNDERS MATERIALS 307 CONTENTS

OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 26 No. 3 2024 Structural features and tribological properties of multilayer high-temperature plasma coatings Natalia Pugacheva 1, 2, a, Tatyana Bykova 1, 2, b, *, Vitaly Sirosh 3, c, Alexey Makarov 3, d 1 Institute of Engineering Science Ural Branch, Russian Academy of Sciences, 34 Komsomolskaya str., Yekaterinburg, 620049, Russian Federation 2 Ural Federal University named after the first President of Russia B.N. Yeltsin, 19 Mira str., Ekaterinburg, 620002, Russian Federation 3 M.N. Miheev Institute of Metal Physics, Ural Branch of the Russian Academy of Sciences, 18 S. Kovalevskoy str., Ekaterinburg, 620108, Russian Federation a https://orcid.org/0000-0001-8015-8120, nata5-4@yandex.ru; b https://orcid.org/0000-0002-8888-6410, tatiana_8801@mail.ru; c https://orcid.org/0000-0002-8180-9543, sirosh.imp@yandex.ru; d https://orcid.org/0000-0002-2228-0643, av-mak@yandex.ru Obrabotka metallov - Metal Working and Material Science Journal homepage: http://journals.nstu.ru/obrabotka_metallov Obrabotka metallov (tekhnologiya, oborudovanie, instrumenty) = Metal Working and Material Science. 2024 vol. 26 no. 3 pp. 250–266 ISSN: 1994-6309 (print) / 2541-819X (online) DOI: 10.17212/1994-6309-2024-26.3-250-266 ART I CLE I NFO Article history: Received: 31 May 2024 Revised: 22 June 2024 Accepted: 08 July 2024 Available online: 15 September 2024 Keywords: Plasma spraying Multilayer coating Iron oxide Strengthening phases Micromechanical properties Friction coefficient Wear resistance Funding The work was carried out within the framework of the state assignment of the IMASH Ural Branch of the Russian Academy of Sciences on topic No. 124020700063-3 on the equipment of the Center for Shared Use “Plastometry”. The work was carried out within the framework of the state assignment of the Institute of Physics and Mathematics, Ural Branch of the Russian Academy of Sciences on the topic “Structure” No. 122021000033-2. ABSTRACT Introduction. Multilayer high-temperature coatings obtained using plasma spraying, are studied. The combination of layers of different chemical and phase compositions made it possible to increase wear resistance by 1.5–2.0 times. The purpose of this work is to study the influence of the chemical composition of sprayed coatings on the phase composition, structure, micromechanical and tribological characteristics under conditions of dry sliding friction of surface layers. Materials and methods of research. Coatings A and B consist of sequentially sprayed layers. The first and second layers were sprayed in a reducing atmosphere: the first layer was a heat-resistant selffluxing powder of two systems: 1 – Fe-Cr-Si-Mn-B-C for coating A and 2 – Fe-Ni-Si-Mn-B-C for coating B; the second layer was a mixture of self-fluxing powder with iron powder in a 1:1 ratio. The third layer was obtained by spraying iron powder in an oxidizing atmosphere to form a metal oxide coating. To create a layer of scale on the surface, coated specimens were subjected to high-temperature annealing at a temperature of 1,000 ℃. The chemical composition and nature of the distribution of elements over the thickness of the coatings were determined by micro-X-ray spectral analysis using a TWSCAN scanning electron microscope with an Oxford energy-dispersive attachment. Microhardness and micromechanical properties were studied using an instrumental microhardness tester of the Fischerscope HM2000 XYm system at a load of 0.980 N. Determination of tribological properties was carried out on a laboratory installation using the “finger-disc” scheme at loads of 30, 75, 100 and 130 N. To measure roughness parameters and obtain 3-D profilometry of surfaces after testing, a non-contact profilometer-profiler Optical profiling system Veeco WYKO NT 1100 was used. Results and discussion. Metallographic studies have shown that the formed multilayer coatings consist of an internal metal layer and an external oxide layer with a total thickness of the entire coating up to 800–850 μm. It is established that the first sprayed layer has the highest level of microhardness, which is due to the high-volume fraction of the strengthening phases contained in it (~ 95 %). It is shown that the coating A has increased wear resistance, which is expressed by minimal weight loss (~ 1.5 times less than that of the coating of the coatimg B), the friction coefficient was f = 0.3 for coating A and f = 0.4 for coating B. The study of wear surfaces has shown that for all selected test loads under sliding friction conditions, the coating of both compositions was preserved, even at a maximum load of 130 N. For citation: Pugacheva N.B., Bykova T.M., Sirosh V.A., Makarov A.V. Structural features and tribological properties of multilayer high-temperature plasma coatings. Obrabotka metallov (tekhnologiya, oborudovanie, instrumenty) = Metal Working and Material Science, 2024, vol. 26, no. 3, pp. 250–266. DOI: 10.17212/1994-6309-2024-26.3-250-266. (In Russian). ______ * Corresponding author Bykova Tatiana M., Ph.D. (Engineering), Senior Researcher Institute of Engineering Science Ural UB RAS, 34 Komsomolskaya str., 620049, Yekaterinburg, Russian Federation Tel.: +7 343 362-30-43, e-mail: tatiana_8801@mail.ru Introduction Increasing the durability of high-temperature multilayer coatings for parts operating in wear conditions at high operating temperatures in various industrial areas is a relevant objective for the following reasons: firstly, the resulting coatings should have high temperature and oxidation resistance; secondly, it should retain adhesion to the base material; thirdly, it should have high corrosion resistance [1]. The choice of

OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 26 No. 3 2024 the composition of coatings and the method of its formation on the surface of the part is determined by the operating conditions, which leads to the need for an individual approach to the formation of multilayer coatings of different chemical composition [2–3]. The application of multilayer high-temperature coatings for piercing tools in the production of seamless hot-rolled steel pipes, which are used as structural pipes in construction, mechanical engineering, and oil industry, is promising [4]. The piercing mandrel is used in the production of hollow billets, from which a seamless pipe is produced in subsequent rolling, rolling, reducing, straightening and calibrating mills [5]. The mandrel is exposed to both high temperatures and abrasive wear during operation [6, 7]. To improve the strength and wear resistance, as well as to avoid sticking on the mandrel, its surface is subjected to hardening treatment, by applying a protective high-temperature coating on its toe and spherical surface, followed by an oxidized layer on the outer surface of the material. To form high-temperature coatings resistant to abrasive wear at high sliding speeds, various self-fluxing high and medium-carbon iron-based alloys alloyed with chromium, nickel, vanadium and manganese are used [8–10]. Iron powder is used to form an oxidized layer on the outer surface, which is applied in an oxidizing atmosphere. Applying an oxide outer layer has a number of advantages: firstly, the oxide layer prevents material from sticking to the mandrel during operation; secondly, at high operating temperatures it creates additional thermal resistance, increasing the thermal resistance of the coating itself; thirdly, at high operating temperatures, scale softens, and it begins to work as a lubricant with the contacted surface [11–15]. Thus, the purpose of the work is to study the influence of the chemical composition of sprayed coatings on the phase composition, structure, micromechanical and tribological characteristics under conditions of dry sliding friction of surface layers. Materials and research methods In this work, multilayer coatings of two different compositions consisting of three successively applied layers were investigated. The difference in the composition of the obtained coatings is the first layer, for the formation of which heat-resistant self-fluxing iron-based powders were used (Table 1). To obtain the first layer of coating of composition 1, Fe-Cr-Si-Mn-B-C powder with a particle size of 50–90 μm was used (Fig. 1 a). The first coating layer of composition 2 is Fe-Ni-Si-Mn-B-C powder with a particle size of 60–100 μm (Fig. 1 b). A mixture of Fe powder with self-fluxing powder in ratio (1:1) was used to form the second layer of both coatings and the third layer was obtained from Fe powder with particle size of 40–100 µm (Fig. 1 c). All layers of the studied coatings were obtained by plasma-powder spraying technology with contact excitation of arc discharge UPN-60KM TSP2017, manufacturer LLC “NPP TSP” (Ekaterinburg). The first (metal) layer, which chemical composition shown in Table 1, due to its high hardness and wear resistance protects the mandrel material from destruction in case of wear of the upper layers during operation. The second (transition) layer is obtained by spraying a mixture of self-fluxing powder with Fe powder. It is designed for a smooth change of properties as well as for better adhesion of the outer layer to Ta b l e 1 Composition of sprayed powders Powder Content of chemical elements, mass. % Ni Cr Si B C Mn Fe Composition 1 (powder Fe-Cr-Si-Mn-B-C) – 3.8 2.3 3.6 1.2 1.0 base Composition 2 (powder Fe-Ni-Si-Mn-B-C) 9.0 – 1.2 2.7 0.5 4.0 base

OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 26 No. 3 2024 а b c Fig. 1. Morphology of powder particles for obtaining a multilayer coating: а – powder of composition 1; b – powder of composition 2; c – Fe powder the inner layer. In order to create a surface scale layer, and to equalize the chemical composition of all layers and increase its adhesion, the coated specimens were subjected to high-temperature annealing at 1,000 ℃. The coating containing the first layer with chromium (composition 1 in Table 1) will be conventionally designated as coating A, and the coating with nickel-containing inner layer (composition 2 in Table 1) will be conventionally designated as coating B. Microstructure, chemical composition, structure features and thickness of the obtained coatings were studied on cross cuts by means of a TESCAN VEGAII XMU scanning electron microscope with an energy dispersive attachment of OXFORD HKLNordlysF+ at 100 to 800-fold magnification. By the microindentation method, using a Fischerscope HM2000 XYm measuring system with a Vickers indenter and WIN-HCU software at a maximum load of 0.980 N, the characteristics that reflect the features of the mechanical behavior of the studied coatings under elastic-plastic deformation were determined [16]. Strength indices (microhardness HV, HIT, HM and contact modulus of elasticity (E*)) and plasticity indices (elastic recovery (Re), work of plastic deformation (φ) and creep (CIT) during indentation) were determined. The values of Re, φ and CIT were calculated according to the formulas: max max 100% p h h h − = ⋅ Re ; (1) 1 100 % We Wt   ϕ = − ⋅     ; (2) max 1 1 100% h h CIT h − = ⋅ . (3) where We is a work of elastic deformation during indentation, released at removal of the applied load; Wt is a total mechanical work during indentation; h1 is a depth of indenter insertion; hmax is a maximum depth of indenter insertion. Investigation of tribological properties was carried out on a laboratory setup using the “pin-on-disc” scheme according to Fig. 2. The friction speed was 5 m/s at loads of 30, 75, 100 and 130 N. In each test, the sliding distance was 5,000 m. The “pin” specimens were made of A-coated and B-coated steel. The “disc” specimen was a disc made of 12 Cr-Mo steel. The tests measured the friction force using a leaf spring with resistance strain gauges glued on it. The heating of the friction surfaces occurred due to the friction itself; external heating sources were not used. The heating temperature of the friction surface was measured using a thermocouple mounted on a “pin” specimen near the friction surface.

OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 26 No. 3 2024 To measure the roughness parameters and obtain 3-D profilometry of the surfaces of the coated specimens in the initial state and after testing, a non-contact profilometer-profilograph Optical profiling system Veeco WYKO NT 1100 was used. Results and discussion Determination of the structure and phase composition of coatings The results of metallographic studies showed that the formed multilayer coatings consist of sequentially applied layers with the total thickness of the entire coating up to 800–850 μm. Figure 3 shows the microstructure and distribution of elements in the obtained coatings. Previously performed phase X-ray diffraction analysis [17] showed that the first (metal) layer of coating A of composition 1 (denoted by number 1 in Fig. 3 a) consists of a solid solution of Cr, Si and Mn in α-Fe with strengthening phases in the form of carbides and silicides of chromium and manganese (Cr23C6, Cr5Si3, CrSi, Cr3Si and Mn5Si3) and iron borides FeB (Fe2B). The metal layer of coating B of composition 2 (denoted by number 1 in Fig. 3 b) consists of two solid solutions of ferrite (α-Fe) and austenite (γ-Fe). The strengthening phases are dispersion carbides, silicides and borides (NiSi2, Ni3Si2, Mn5Si3, Fe5Si3, Fe2B). The second (transition) layer and the outer (oxide) layer (denoted by numbers 2 and 3 in Fig. 3 a and b) on both coatings consist of an α-solid solution based on Fe and oxides FeO, Fe2O3 and Fe3O4. Determination of micromechanical properties of sprayed coatings Based on the results of instrumental microindentation, it was found that the highest level of microhardness was possessed by the first metal layer (1) for coating A the microhardness was 1,030 HV 0.1. The first (metal) layer (1) in coating B was characterized by a microhardness of 745 HV 0.1. The increased hardness of the metal layer of coating A is associated with a high content of strengthening phases in it. The microhardness of the transition layer (2) is 650 HV 0.1 for coating A and 580 HV 0.1 for coating B. The microhardness of the outer oxide layer (3) for both coatings is 290 HV 0.1. The variation of microhardness in related areas reaches ~ 350–380 HV 0.1 for coating A and ~ 150–300 HV 0.1 for coating B, which is explained by a decrease in the volume fraction of the strengthening phase (Tables 2 and 4). The strengthening phases in the coatings reduce the values of maximum and residual indentation depths hmax and hp, which leads to an increase in the values of indentation hardness at maximum load HIT (meaning an increase in resistance to permanent deformation) and Martens hardness HM, which takes into account both plastic and elastic deformation, the indentation elastic modulus E* of both coatings changes insignificantly (Fig. 4 a and 5 a in Tables 2 and 4). In earlier studies [18, 19] it was shown that such parameters as elastic recovery Re, (characterizes the share of elastic deformation in the total deformation during indentation), and indices of the plastic component of work φ and creep CIT are used to assess the resistance of surface layers to mechanical action. Specimen Fig. 2. Tribological loading scheme “pin-on-disc”

OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 26 No. 3 2024 а b Fig. 3. Microstructure and distribution of elements in the coatings: а – coating A; b – coating B As can be seen from Tables 3 and 5 and Figures 4 b and 5 b in the transition and oxide layer (2) and (3), the creep parameters CIT and the plastic component of the work φ have maximum values in contrast to the metallic layer (1) this is explained by the increased plasticity of these layers, the purpose of which is to act as a lubricant under high operating loads. The maximum values of the Re index are characterized for the metal layer (1), which indicates the ability of this layer to resist mechanical action without plastic deformation in the elastic region.

OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 26 No. 3 2024 Ta b l e 2 Results of instrumented microindentation of coating A at a maximum load on the indenter of 980 mN (100 g) Areas of analysis HM, GPa (±34) HIT, GPa (±43) HV (±41) E*, GPa (±10.7) hmax, μm (±0.34) hp, μm (±0.31) h1, μm (±0.34) Metal layer (1) 722.6 1090.0 1030 208.8 2.3 1.5 2.2 Transition layer (2) 500.6 686.7 650 173.7 2.8 1.9 2.6 Oxide layer (3) 258.3 305.7 290 150.5 3.9 3.3 3.6 Ta b l e 3 Plasticity parameters for coating A Areas of analysis Rе, % φ, % CIT, % Metal layer (1) 35 65 4.5 Transition layer (2) 31 67 6.5 Oxide layer (3) 15 84 8.4 Ta b l e 4 Results of instrumented microindentation of coating B at a maximum load on the indenter of 980 mN (100 g) Areas of analysis HM, GPa (±34) HIT, GPa (±43) HV (±41) E*, GPa (±10.7) hmax, μm (±0.34) hp, μm (±0.31) h1, μm (±0.34) Metal layer (1) 579.7 787.6 745 199.0 2.7 1.5 2.4 Transition layer (2) 477.2 616.4 580 164.5 2.9 1.6 2.7 Oxide layer (3) 264.2 306.5 290 140.0 3.9 2.7 3.5 Ta b l e 5 Plasticity parameters for coating B Areas of analysis Rе, % φ, % CIT, % Metal layer (1) 44 70 6.6 Transition layer (2) 43 73 7.4 Oxide layer (3) 28 81 8.9 Determination of tribological properties under sliding friction conditions The most important requirement for the coatings analyzed in this work is resistance under wear conditions. Tests under sliding friction conditions made it possible to identify general regularities in the behavior of specimens under external loading and form recommendations for its application in real operating conditions [20–22].

OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 26 No. 3 2024 a b Fig. 4. Average values of strength (a) and ductility (b) of coating A: 1 – Oxide layer; 2 – Transition layer; 3 – Metal layer a b Fig. 5. Average values of strength (a) and ductility (b) of coating B: 1 – Oxide layer; 2 – Transition layer; 3 – Metal layer The results of tribological tests of coatings under sliding friction conditions are presented in Figs. 6 and 7. It is shown that the coating of composition A has increased wear resistance compared to the coating of composition B, which also agrees with the data obtained on the values of microhardness and micromechanical properties (see Tables 2–5) [23]. Coating A is characterized by minimum mass loss (~ 1.5 times less than that of coating B) and maximum coefficient of friction (f ~ 0.3). At the initial stage of friction at a load of 30 N there is a run-in period characterized by the highest wear rates (mass loss) and friction coefficients f ~ 0.6 for both coatings. Further, at a load of 75 N, the frictional heating temperature of the friction surface increases, which leads to softening of the scale layer and to a decrease in the friction coefficient f ~ 0.4 for both coatings, which provides an accelerated transition to steady-state wear. At a load of 100–130 N, the steady-state wear on the sliding distance is characterized by almost the same change in mass loss (Fig. 6), as well as close levels of friction coefficient f ~ 0.3–0.4 for coating A and f ~ 0.4 for coating B (Fig. 7 It is worth noting that the temperature of frictional heating of friction surfaces in the case of coating B is lower. It is especially noticeable at friction with loads of 30 and 75 N. The study of wear surfaces of coatings A and B showed that after sliding friction tests at loads of 30 and 75 N, setting processes characterized by detachment of outer coating particles develop (Fig. 8 a, b and

OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 26 No. 3 2024 Fig. 6. Weight loss of specimens after testing under sliding friction conditions Fig. 7. Friction coefficient f and temperature T (℃) near sliding friction surfaces: a – coating A; b – coating B а b

OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 26 No. 3 2024 Fig. 8. Coating A surfaces after sliding friction tests: a – load 30 N; b – load 75 N; c – load 100 N; d – load 130 N а b c d Fig. 9 a, b). With increasing load (100 and 130 N), when the oxide layer is almost completely worn out, the metal layer of the coatings of compositions A and B provides the transition to wear by the mechanism of plastic displacement (Fig. 8 c, d and Fig. 9 c, d), which corresponds to a decrease in the magnitude of wear. The study of the chemical composition of the wear surfaces showed that at all selected test loads under sliding friction conditions the inner layers of both compositions were preserved at a maximum load of 130 N (Tables 6 and 7). This confirms the purpose of these layers to prevent tool fracture, which allows timely restoration of wearied outer layers. The results of studies of surface roughness of coatings A and B showed that after sliding friction tests there is a smoothing of the initial surface roughness and a decrease in the value of the arithmetic mean deviation of the profile Ra. The minimum values of the arithmetic mean deviation of the Ra profile are observed after a load of 30 N (Ra = 0.434 μm for coating A and Ra = 0.99 μm for coating B), where the wear of the surface oxide layer, which plays the role of lubrication, occurs. As the sliding friction load increases from 75 N to 130 N, the average Ra value increases (see Fig. 10 c–e and Fig. 11 c–e). Analysis of the surface micro-profile taken during 3D profilometry showed that after friction with 30 and 75 N load, isolated depressions related to the setting processes were observed (Fig. 10 b, c and Fig. 11 b, c shown by arrows). The surfaces after friction with a load of 100 and 130 N (Fig. 10 d, e and Fig. 11 d, e) are characterized by the presence of unidirectional protrusions and depressions. Higher values of roughness parameter Ra for coating B after sliding friction tests are characterized by the presence of more oxides on the surface (see Tables 6 and 7). As a result of the research, it was found that the tribological properties of the studied coatings depend on the chemical composition of the sprayed material and the resulting strengthening phases.

OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 26 No. 3 2024 Fig. 9. Coating B surfaces after sliding friction tests: a – load 30 N; b – load 75 N; c – load 100 N; d – load 130 N a b c d Ta b l e 6 Chemical composition of the wear surface of the coating А, at. % Load Fe O Cr Mn Si B C 30 N 56.30 4.87 0.23 0.11 0.14 7.15 4.87 75 N 47.45 4.63 0.72 0.24 0.54 7.41 4.63 100 N 63.03 9.63 2.42 1.15 1.84 11.40 8.00 130 N 57.63 13.23 2.74 1.30 1.87 13.24 6.87 Ta b l e 7 Chemical composition of the wear surface of the coating B, at. % Load Fe O Ni Mn Si B C 30 N 60.59 38.02 0.13 0.20 0.17 0.00 0.00 75 N 61.67 29.34 3.91 1.94 1.47 2.19 1.07 100 N 61.06 28.25 4.80 2.17 1.76 2.46 1.48 130 N 59.36 28.13 6.28 2.28 1.72 4.07 1.00

OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 26 No. 3 2024 a b c d e Fig. 10. 3-D profilograms of the coated specimen A: a – in the initial state; b – after a wear test at a load of 30 N; c – 75 N; d – 100 N; e – 130 N a b c d e Fig. 11. 3-D profilograms of the coated specimen B: a – in the initial state; b – after a wear test at a load of 30 N; c – 75 N; d – 100 N; e –130 N The strengthening phases formed in the process of plasma spraying contribute to an increase in the microhardness and wear resistance of the materials under study, as well as a decrease in the intensity of wear under conditions of dry sliding friction.

OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 26 No. 3 2024 Conclusion High-temperature coatings obtained by plasma spraying consist of successively applied layers: the first inner (metal) layer is obtained by spraying self-fluxing powders of two different compositions of Fe-CrSi-Mn-B-C system (composition 1) and Fe-Ni-Si-Mn-B-C system (composition 2); the second layer is a transitional layer obtained by spraying a mixture of high-temperature powders of compositions 1 or 2, with Fe powder in the ratio of 50:50 and the outer (metal-oxide) layer is obtained by spraying Fe powder in an oxidizing atmosphere to form an oxide layer consisting of a mixture of iron oxides (FeO + Fe2O3 + Fe3O4) on the surface. The total thickness of the obtained coatings is 800–850 µm. The inner (metal) layer is characterized by high hardness (up to 1,030 HV 0.1 for coating composition 1 and 745 HV 0.1 for coating composition 2) and Re values, which indicates the ability of this layer to resist mechanical stress without plastic deformation in the elastic region. High plasticity indices of outer layers (creep CIT and plastic component of work φ) are established, the purpose of which is to act as a lubricant under high operating loads. Under conditions of dry sliding friction, it is shown that coating A has increased wear resistance compared to coating B; the friction coefficient for coating A is f = 0.3, the friction coefficient for coating B is f = 0.4. The study of the wear surfaces showed that on the surface of the obtained coatings after sliding friction tests at the load of 30 and 75 N the processes of seizure develop, and at increasing the load to 100 N and 130 N there is a transition to wear by the mechanism of plastic displacement, which corresponds to a decrease in the magnitude of wear. Under all selected test loads under conditions of dry sliding friction, high-temperature layers of coatings of both compositions are preserved at the maximum load of 130 N. After the sliding friction tests, a significant surface smoothing and a reduction in the arithmetic mean deviation of the Ra profile are recorded. References 1. Guzanov B.N., Kositsyn S.V., Pugacheva N.B. Uprochnyayushchie zashchitnye pokrytiya v mashinostroenii [Reinforcing protective coatings in engineering industry]. Ekaterinburg, UrO RAN Publ., 2003. 244 p. ISBN 5-76911405-3. 2. Serin K., Pehle H.J. Improved service life for hot forming tools in seamless tube plants. Stahl und Eisen, 2014, vol. 134 (11), pp. 161–174. 3. Sivakumar R., Mordike B.L. High temperature coatings for gas turbine blades: a review. Surface and Coatings Technology, 1989, vol. 37 (2), pp. 139–160. DOI: 10.1016/0257-8972(89)90099-6. 4. Podshivalkin S.A., Torbeev A.N. Struktura i svoistva oksidirovannykh pokrytii [Structure and properties of oxidized coatings]. Master’s Journal, 2012, no. 2, pp. 91–98. (In Russian). 5. Fomin A.A., Steinhauer A.B., Lyasnikov V.N., Wenig S.B., Zakharevich A.M. Nanocrystalline structure of the surface layer of plasma-sprayed hydroxyapatite coatings obtained upon preliminary induction heat treatment of metal base. Technical Physics Letters, 2012, vol. 38 (5), pp. 481–483. DOI: 10.1134/S1063785012050227. 6. Sazonenko I.O., Zemuov V.A., Yurchak A.N. K voprosu povysheniya stoikosti opravok proshivnykh stanov [To the matter of stabilization of saddles of punch mills]. Lit’e i metallurgiya = Foundry Production and Metallurgy, 2012, no. 4, pp. 135–138. (In Russian). 7. Pukhov E.V., Zagoruyko K.V. Rezul’taty eksperimental’nykh issledovanii iznosostoikosti poverkhnosti kolenchatogo vala, vosstanovlennoi metodom gazoplamennogo naneseniya samoflyusuyushchikhsya poroshkov [The results of experimental studies of the wear resistance of the surface of the crankshaft restored by the method of flame application of self-fluxing powders]. Mezhdunarodnyi tekhniko-ekonomicheskii zhurnal = The International Technical-Economic Journal, 2020, no. 4, pp. 45–52. DOI: 10.34286/1995-4646-2020-73-4-45-52. (In Russian). 8. Manoilo E.D., Radchenko A.A., Shardakov S.N. [Continuous gas-flame coating of self-fluxing alloy powders on rod couplings of oil pumps]. Poroshkovaya metallurgiya: inzheneriya poverkhnosti, novye poroshkovye kompozitsionnye materialy. Svarka [Powder metallurgy: surface engineering, new powder composite materials. Welding]. Collection of reports of the 13th International Symposium. Pt. 2. Minsk, 2023, pp. 171–186. (In Russian).

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