Vol. 25 No. 1 2023 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. WEB OF SCIENCE
OBRABOTKAMETALLOV Vol. 25 No. 1 2023 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 Affairs, 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. Gerasenko, Director, Scientifi c and Production company “Mashservispribor”, Novosibirsk; Aleksandr N. Korotkov, D.Sc. (Engineering), Professor, Kuzbass State Technical University, Kemerovo; Evgeniy A. Kudryashov, D.Sc. (Engineering), Professor, Southwest State University, Kursk; 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, Institute of Strength Physics and Materials Science, Russian Academy of Sciences (Siberian Branch), Tomsk; Alexander S. Yanyushkin, D.Sc. (Engineering), Professor, I.N. Ulianov Chuvash State University, Cheboksary
Vol. 25 No. 1 2023 5 CONTENTS OBRABOTKAMETALLOV TECHNOLOGY Ryaboshuk S.V., Kovalev P.V. Analysis of the reasons for the formation of defects in the 12-Cr18-Ni10-Ti steel billets and development of recommendations for its elimination............................................................... 6 Lapshin V.P., Moiseev D.V. Determination of the optimal metal processing mode when analyzing the dynamics of cutting control systems................................................................................................................... 16 Gimadeev M.R., Li A.A., Berkun V.O., Stelmakov V.A. Experimental study of the dynamics of the machining process by ball-end mills.................................................................................................................. 44 Bratan S.M., Chasovitina A.S. Simulation of the relationship between input factors and output indicators of the internal grinding process, considering the mutual vibrations of the tool and the workpiece................... 57 EQUIPMENT. INSTRUMENTS Podgornyj Yu.I., KirillovA.V., Skeeba V.Yu., Martynova T.G., Lobanov D.V., Martyushev N.V. Synthesis of the drive mechanism of the continuous production machine......................................................................... 71 Lobanov D.V., Rafanova O.S. Methodology for criteria analysis of multivariant system................................ 85 MATERIAL SCIENCE Sokolov A.G., Bobylyov E.E., Popov R.A. Diffusion coatings formation features, obtained by complex chemical-thermal treatment on the structural steels............................................................................................ 98 Filippov A.V., Khoroshko E.S., Shamarin N.N., Kolubaev E.A., Tarasov S.Yu. Study of the properties of silicon bronze-based alloys printed using electron beam additive manufacturing technology................... 110 Lysykh S.A., Kornopoltsev V.N., Mishigdorzhiyn U.L., Kharaev Yu.P., Tikhonov A.G., Ivancivsky V.V., Vakhrushev N.V. The effect of borocoppering duration on the composition, microstructure and microhardness of the surface of carbon and alloy steels............................................................................................................. 131 EDITORIALMATERIALS 149 FOUNDERS MATERIALS 159 CONTENTS
OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 25 No. 1 2023 Study of the properties of silicon bronze-based alloys printed using electron beam additive manufacturing technology Andrey Filippov а, *, Ekaterina Khoroshko b, Nikolay Shamarin c, Evgeny Kolubaev d, Sergei Tarasov e Institute of Strength Physics and Materials Sciences SB RAS, 2/4, pr. Akademicheskii, Tomsk, 634055, Russian Federation a https://orcid.org/0000-0003-0487-8382, avf@ispms.ru, b https://orcid.org/0000-0001-9078-5662, eskhoroshko@gmail.com, c https://orcid.org/0000-0002-4649-6465, shnn@ispms.ru, d https://orcid.org/0000-0001-7288-3656, eak@ispms.ru, e https://orcid.org/0000-0003-0702-7639, tsy@ispms.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. 2023 vol. 25 no. 1 pp. 110–130 ISSN: 1994-6309 (print) / 2541-819X (online) DOI: 10.17212/1994-6309-2023-25.1-110-130 ART I CLE I NFO Article history: Received: 20 January 2023 Revised: 25 January 2023 Accepted: 01 February 2023 Available online: 15 March 2023 Keywords: Additive technologies Silicon bronze Structure Phase composition Mechanical properties Corrosion Friction Funding This research was funded by Russian Science Foundation project № 21-7900084, https://rscf.ru/project/21-79- 00084/. Acknowledgements Research were conducted at core facility “Structure, mechanical and physical properties of materials”. ABSTRACT Introduction. Additive technologies make it possible to curb material expenses by reducing allowances for the final dimensional machining of workpieces. For such expensive materials as copper and copper alloys, this method is considerably attractive from a perspective of increasing resource efficiency in production. The operational properties of the C65500 alloy manufactured using additive technologies have not been fully studied and require additional research. The aim of the work is to study the structural and phase state, mechanical and operational properties of C65500 bronze specimens printed using electron beam additive manufacturing technology. In the work, specimens made of C65500 wire with different heat input values are studied, some of which were subjected to thermal treatment and mechanical processing, as well as specimens, manufactured using multi-wire technology. The work uses such research methods as the study of corrosion resistance of bronze specimens using a potentiostat, confocal laser scanning microscopy, friction tests and X-ray phase analysis. Results and discussion. Processing of specimens by plastic deformation (compression) and subsequent annealing leads to the most serious structural changes. Based on X-ray phase analysis, it is found that higher silicon content is observed in the case of the addition of silumins to bronze. The study of mechanical properties shows that the specimens, printed using multi-wire technology, have the highest strength properties. During tribological testing, fluctuations in the value of the friction coefficient are revealed, due to the scheme of the experiment and the combined adhesive-oxidative mechanism of specimens’ wear. The addition of 10 wt.% aluminum filament to bronze in the additive manufacturing process is an effective means for increasing the resistance of the material to electrochemical corrosion and increasing its wear resistance. For citation: Filippov A.V., Khoroshko E.S., Shamarin N.N., Kolubaev E.A., Tarasov S.Yu. Study of the properties of silicon bronze-based alloys printed using electron beam additive manufacturing technology. Obrabotka metallov (tekhnologiya, oborudovanie, instrumenty) = Metal Working and Material Science, 2023, vol. 25, no. 1, pp. 110–130. DOI: 10.17212/1994-6309-2023-25.1-110-130. (In Russian). ______ * Corresponding author Filippov Andrey V., Ph.D. (Engineering), Head of Laboratory Institute of Strength Physics and Materials Sciences SB RAS 2/4, pr. Akademicheskii, 634055, Tomsk, Russian Federation Tel.: 8 (999) 178-13-40, e-mail: avf@ispms.ru Introduction Silicon bronzes are rather expensive materials used commonly for the manufacture of products that should possess enhanced corrosion and wear resistance [1]. In connection with this, the development of methods that allow improving the resource usage efficiency is an important scientific and technical task. In this direction, additive manufacturing can provide various options for solving the problem of reducing
OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 25 No. 1 2023 the production costs, due to a significant reduction in allowances for the final dimensional machining of workpieces [2]. At the same time, one of the main problems in the additive manufacturing made of copper and its alloys is the oxidation of interlayer boundaries, which significantly worsens the physical and mechanical properties of printed products. In this regard, three-dimensional printing should be carried out either in a protective gas or in a vacuum [3]. An important advantage of additive technologies is the ability to control the printing modes, which allows varying the melting conditions of the material in a wide temperature range. This is especially important in the manufacture of three-dimensional curved products and non-uniform wall thickness. Indeed, the thickness and height of the wall, as well as the total volume of the printed material, significantly affect the heat removal [4] and, accordingly, the formation of the melt bath. The wire-feed electron-beam additive manufacturing is carried out in a vacuum using a thin wire as a filament. This type of filament is less expensive than powder, which makes this technology less expensive. In addition, this technology allows the use of several wires to feed it into the printing zone in different ratios. As a result, it becomes possible to print new multicomponent alloys with different alloying elements, as well as alloys and composites from dissimilar materials [5–8]. The electron-beam additive manufacturing (EBAM) is used to obtain products from nickel heat-resistant alloys [9–12], intermetallic compounds such as TiAl [13–15], soft magnetic materials based on iron [16], aluminum alloys [17, 18], and magnesium alloys [19], as well as bronze [20, 21]. In the native industry, the silicon bronze grade C65500 is of the most common use. It is used in parts intended to chemical industry, aviation, automotive and shipbuilding industries. At the same time, its analogue is known containing ~7 wt.% Al and ~2 wt.% Si that is produced abroad. This alloy has higher performance characteristics compared to C65500. Therefore, obtaining analogues of this alloy is an urgent task. To solve it a technology of the multiwire electron beam additive manufacturing can be used, which is implemented by feeding two or more wires to the melt bath. In the context of obtaining alloys of the Cu–Al– Si system, it is possible to use an aluminum filament and feed it in the process of printing bronze in a ratio of 10:1, which should provide the required composition of the alloy. Previously, the multiwire electron-beam additive manufacturing was successfully used to obtain specimens from the C65500 alloy [22] and the alloy of the Cu–Al– Si–Mn system [23]. However, in the works known to date, the operational properties of this alloy, obtained using additive technologies, have not been fully investigated. The properties of alloys printed on the basis of silicon bronze with the addition of aluminum filament also remain unexplored. Varying the EBAM heat input, conducting the post-deposition heat and thermomechanical treatments as well as alloying the bronze with Al-Si alloys are in fact three different approaches to the structure modification, which are based on altering cooling rate, recrystallization and constitutional undercooling, respectively. The aim of the work is to study the structural and phase state, mechanical and operational properties of C65500 bronze specimens printed using electron beam additive manufacturing technology. Research methodology The thin-walled specimens were made using the electron-beam additive manufacturing as shown in Figure 1. Two groups of specimens were obtained by EBAM. The first one was made from wire C65500 with different heat inputs: mode 1 – 0.19 kJ/mm, mode 2 – 0.25 kJ/mm, mode 3 – 0.31 kJ/mm. Some of these specimens, with the most coarse-grained structure, were subjected to thermal (annealing at 850 °C) and mechanical treatment (compression deformation by 10 % and subsequent annealing at 850 °C), which made it possible to successfully change its structural state. More detailed information about the processing modes and the structural state of these specimens is given elsewhere [22]. The second part of the specimens was made using the multiwire technology. This approach was used to change the composition of specimens and assess the possibility of controlling its structure and properties, as well as to obtain an alloy of the Cu–Al– Si system with a composition close to foreign analogues (alloy C64200) used in aviation and marine engineering. To do this, two wires were fed into the melt bath so that
OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 25 No. 1 2023 the first one was constantly the C65500 itself while the second was made of an alloy to be intermixed with bronze. Commercially pure aluminum (99% Al) and AK5 (Al-5Si) and AK12 (Al-12Si) alloys were used as such additives. The both wires’ feed rates were adjusted in such a way as to ensure the addition of 10 wt.% of aluminum to the C65500 alloy. As a result, three alloys were obtained: 1) C65500 + 10 wt.% Al, 2) C65500 + 10 wt.% Al-5Si and 3) C65500 + 10 wt.% Al-12Si. The technique for printing specimens is described in more detail elsewhere [23]. Corrosion resistance of bronze specimens was studied by conducting potentiodynamic tests on a threeelectrode circuit and using a potentiostat Electrochemical Instrument P-45X. An aqueous solution of 3.5% NaCl was used as a corrosive medium. As a result, polarization curves were obtained that reflected the changes in potential and corrosion current. The polarization resistance is calculated basing on the ButlerVolmer equation: Rp = (βaβc)/(2.303Icorr(βa + βc)), (1) where βa is the slope of the anode branch, β c is the slope of the cathode branch, icorr is the corrosion current. The weight loss of the specimens was assessed using a Sartorius CP 124 S analytical balance. The surface of bronze specimens after the corrosion resistance test was examined using a confocal laser scanning microscope Olympus OLS-4100. To perform both qualitative and quantitative assessments of the corrosion damage to the surface, optical images were obtained and the roughness was evaluated. Sliding tests were carried out using a Tribotechnic tribometer according to the ball-on-disk scheme under conditions of reciprocating dry sliding friction. Plates cut from printed bronze walls were used as specimens (see Figure 1. pos. 8). Balls made of hardened steel AISI 52100 were used as counterbodies. The study of the surface of bronze specimens and balls after friction, as well as the measurement of the crosssectional profile of the wear tracks, was carried out using a confocal laser scanning microscope Olympus OLS-4100. Microhardness was measured using a Duramin-5 hardness tester at a load of 50 N. The tensile strength characteristics were evaluated on a Testsystem 110 M-10 testing machine. The study of the phase composition of bronze specimens was carried out on a DRON-7 X-ray diffractometer. The elemental composition was determined using Octane Elect energy dispersive spectral (EDS) analysis on a Thermo Fisher Scientific Apreo S LoVac scanning electron microscope. Metallographic studies of the structure of bronze specimens were performed using a confocal laser scanning microscope Olympus OLS -4100. Fig. 1. Scheme of electron beam additive manufacturing and cut-up sketch: 1 – printed material; 2 – substrate; 3 – wire feed direction; 4 – wire feeder; 5 – printing direction; 6 – electron beam; 7 – tensile test specimens; 8 – friction and corrosion resistance test specimen
OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 25 No. 1 2023 Results and discussion Metallographic studies of the structure of specimens Changing the heat input naturally affected the structure of the as-manufactured specimens. As the heat input increases, the grains grow and its shape changes. With minimal heat input (0.19 kJ/mm), a bimodal structure with small elongated and equiaxed grains is observed (Fig. 2, a). The medium and high heat input levels 0.25 kJ/mm and 0.31 kJ/mm resulted in forming zigzag-shaped (Fig. 2, b) and large columnar grains (Fig. 2, c), respectively. Annealing of the columnar grained specimens resulted in forming large nonequiaxed grains with numerous annealing twins (Fig. 2. d). Annealing of the pre-deformed by compression specimens led to the most serious structural changes with formation of small equiaxed grains with a large number of annealing twins (Fig. 2, e). The change in the structural state of the specimens is due to differences in the temperature gradient during printing. With low heat input, the crystallization rate increases and as a result, a finer-grained microstructure is formed. In turn, annealing, as well as deformation and subsequent annealing, lead to recrystallization of the material [24, 25]. As a result of printing of the C65500 alloy with the addition of 10 wt.% Al, a fine-grained structure with almost equiaxed grains 25–125 μm in size was formed (Fig. 3, a). Annealing twins and secondary phase inclusions are also observed. When printing with the addition of alloys Al-5Si and Al-12Si, the structure of the specimens looks different. In both cases, dendritic structure is formed (Figs. 3, b and c). Dendrites’ first order axes are oriented along the direction of wall building, and in the interdendritic space there are interlayers of the secondary phase with a thickness of 3–15 μm. a b c d e Fig. 2. Typical microstructure of specimens printed from C65500. Printing modes 1 (a), 2 (b) and 3 (c). Specimens after annealing (d), as well as after deformation and subsequent annealing (e)
OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 25 No. 1 2023 a b c Fig. 3. Typical microstructure of specimens printed from C65500 with the addition of 10 wt.% Al (a), 10 wt.% Al–5Si (b) and 10 wt.% Al-12Si (c) XRD and EDS analysis phase composition samples It was established from the results of X-ray phase analysis that all the studied specimens were mainly composed of the α-Cu solid solution (Fig. 4). The specimens printed with the addition of aluminum filaments additionally contained iron and particles of silicon silicide that were formed due to the presence of iron in the Al-Si wires. According to the known phase diagrams [26–31], alloys of the Cu–Al–Si system can have two phases, namely, FCC α-Cu phase and HCP γ-phase. In the samples under consideration, it was found using the EDS that the secondary γ-phase contains (copper-balance) ~7 at.% Al, ~(9–10)at. % Si and ~(0.5–0.6) at.% Mn, while the α-phase contains ~10 at.% Al, ~(3.5–5) at.% Si and ~(1.2–1.5) at.% Mn. The higher silicon content is observed obviously in the case of the adding of silumins to the bronze. Fig. 4. X-ray diffraction patterns of specimens printed from C65500 and with the addition of aluminum filament. Printing modes 1 (1), 2 (2) and 3 (3). Specimens after annealing (4), deformation and subsequent annealing (5). Specimens with the addition of 10 wt.% Al (6), 10 wt.% Al–5Si (7) and 10 wt.% Al-12Si (8)
OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 25 No. 1 2023 Ta b l e 1 Mechanical properties of specimens printed from C65500 and with the addition of aluminum filament Specimen designation Offset yield strength, MPa Ultimate strength, MPa Strain-to-fracture, % C65500 (mode 1) 89 242 83 C65500 (mode 2) 93 294 75 C65500 (mode 3) 82 253 114 C65500 (annealing) 92 301 76 C65500 (deformation + annealing) 75 318 91 C65500 (10 wt.% Al) 203 434 21 C65500 (10 wt.% Al–5Si) 150 394 67 C65500 (10 wt.% Al–12Si) 186 448 57 Mechanical properties of specimens Changing the heat input, the use of thermal and mechanical treatments, as well as alloying with aluminum through the use of multiwire technology, made it possible to obtain bronze specimens not only with different structures, but also with modified mechanical properties. It can be seen that the specimens printed using the multiwire technique have the highest strength (Table 1). In addition, these specimens (with the exception of the C65500 alloy with the addition of 10 wt.% Al) are characterized by sufficiently high ductility. Consequently, the two-phase structure of the specimens printed with the addition of Al-5Si and Al-12Si alloys is characterized by high strength and simultaneously high ductility. More detailed study of the strength of the specimens under consideration is presented [22, 23]. Structural modifications have also affected the microhardness of the specimens (Fig. 5). Heat treatment expectedly reduced the microhardness due to the removal of residual stresses. As in the case of strength, specimens with a two-phase structure have a higher hardness compared to that of the single-phase ones. The increase in microhardness was 140–215 %. Corrosion The above-described differences in the structural and phase states of the studied specimens affected not only its mechanical properties, but also its corrosion resistance. Figure 6 shows the potentiodynamic polarization curves that were recorded during the study of the electrochemical corrosion. In all the cases under consideration, the potential changes in the cathode part of the curves are without any significant fluctuations. In the anodic part of the curves, the potential changes similarly to that of the cathodic one, but there is a small region with a slowing growth in the potential, which may indicate passivation of the specimen’s surface. For a specimen, subjected to pre-deformation and annealing, this section is the longest (Fig. 6a). Therefore, this specimen is the most resistant to the action of the corrosive media, which can be caused by more active formation of aluminum and copper oxides, which hinder the anodic dissolution of the specimen. Such an increase in chemical activity may be the result of a refinement of the material structure, accompanied by an increase in the length of grain boundaries. The boundaries serve as a source of active ions that react with the solution in the electrochemical cell and form passive oxide films. In addition, the results obtained indicate the absence of pitting on the surface of all specimens. The parameters of the electrochemical potential of the specimens were established. The corrosion potential (Table 2) for specimens printed with low (mode 1), medium (mode 2) and high (mode 3) heat input are as follows: -178 mV, -210 mV and -202 mV, respectively. The post-manufacture annealing of both as-
OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 25 No. 1 2023 Fig. 5. Microhardness of specimens printed from C65500 and with the addition of aluminum filament. Printing modes 1 (1), 2 (2) and 3 (3). Specimens after annealing (4), deformation and subsequent annealing (5). Specimens with the addition of 10 wt.% Al (6), 10 wt.% Al–5Si (7) and 10 wt.% Al–12Si (8) manufactured and pre-deformed specimens leads to a decrease in the value of the corrosion potential. The corrosion current for this group of specimens does not change significantly (from 5.5 to 5.74 μA). The potentiodynamic polarization curves for the second group of specimens printed with the addition of an aluminum filament are shown in Figure 6, b. By its nature, it is similar to those of the as-printed silicon bronze specimens (Fig. 6, a). An exception is a specimen printed with the addition of Al-12Si alloy. In this case, no surface passivation area is observed, and anodic dissolution begins immediately. For these specimens the corrosion potential ranges from -193 mV to -251 mV, which is generally close in magnitude to that of as-printed silicon, bronze (Table 2). The value of the corrosion current for the specimen C65500 + 10 wt.% Al-5Si is the smallest, and for samples C65500 + 10 wt.% Al and C65500 + 0 wt.% Al-12Si is the largest among those considered in this work. a b Fig. 6. Polarization curves for specimens printed from C65500 (a) and with the addition of aluminum filament (b)
OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 25 No. 1 2023 A quantitative assessment of the corrosion resistance can be obtained by calculating the polarization resistance using equation (1) from the polarization curves. The value of Rp characterizes how resistant the specimen is to oxidation with respect to the applied potential. Based on the data obtained, it follows that the annealing the pre-deformed specimens contributes to an increase in the polarization resistance of specimens printed from silicon bronze. In turn, when printing specimens with the addition of aluminum filaments, the most effective in terms of increasing the polarization resistance is the addition of Al-5Si alloy. For a more detailed assessment of the effect of a corrosive medium on the surface of the specimens, it has been analyzed using a laser scanning microscope. After testing, a micro-topology pattern formed on the surface of the specimens, with clearly distinguishable individual structural elements (grains, annealing twins, etc.). Pitting marks on the surfaces of silicon bronze (Fig. 7) and bronzes printed with the addition of aluminum filament (Fig. 8) were not detected. The boundaries of grains and annealing twins did not undergo any significant dissolution. At the same time, the visually observed surface pattern is not the same in all cases. To quantify these differences, the surface roughness of the specimens under study was evaluated. From the data obtained, it can be seen that the specimens printed from bronze C65500 after testing (Fig. 9) are characterized by the most significant surface roughness. The use of high-temperature annealing contributed to the decrease in the arithmetic mean value of the asperity height (Ra) by 6–12 %. The smallest roughness is observed on the corroded surface of the pre-deformed and annealed specimen (Ra = 0.275 µm). The multiwire approach had its effect on the corroded surface roughness. Based upon the data obtained, the least surface roughness (Ra = 0.296 µm) is exhibited by the specimen printed with the addition of Al-5Si alloy. Based on the data obtained, it follows that the surfaces of the specimens with the lowest roughness are oxidized more uniformly, which may indicate its higher resistance to the electrolyte. Another quantitative characteristic of corrosion resistance of specimens is the loss of mass. To obtain it, the specimens were weighed on an analytical balance before and after testing. As a result, the mass loss was determined for all the studied specimens (Fig. 10). High-temperature annealing, as well as annealing the pre-deformed specimens caused the reduction in mass loss by 15–30% in comparison the that of as-printed silicon bronze specimens. The addition of aluminum filament made it possible to further reduce the weight loss of as-printed specimens by 13–31 % with regard to both as-printed and annealed specimens of bronze C65500. Ta b l e 2 Parameters of Taffel curves according to the data of potentiodynamic tests of specimens printed from C65500 and with the addition of aluminum filament Specimen designation Parameters of polarization curves Ecorr , mV Icorr , μA βa βc Rp, kOhm C65500 (1) –178 5.54 0.030371 –0.02667 1.7 C65500 (3) –210 5.74 0.067731 –0.05687 2.7 C65500 (7) –202 5.6 0.064345 –0.08164 2.4 C65500 (annealing) –229 5.71 0.069095 –0.10014 1.7 C65500 (deformation + annealing) –223 5.5 0.110449 –0.13455 4.8 C65500 (10 wt.% Al) –251 6.6 0.168932 –0.12941 3.6 C65500 (10 wt.% Al–5Si) –239 5.2 0.246156 –0.18557 6.3 C65500 (10 wt.% Al–12Si) –193 8.4 0.116204 –0.13008 5.6
OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 25 No. 1 2023 Fig. 7. The surface of C65500 specimen, printed by the EBAM method, after corrosion tests. Printing modes 1 (a), 2 (b) and 3 (c). Specimen after annealing (d), deformation and subsequent annealing (e) а b c d e a b c Fig. 8. The surface of C65500 specimen with the addition of 10 wt.% Al (a), 10 wt.% Al–5Si (b) and 10 wt.% Al–12Si (c) after corrosion tests All of these results consistently indicate the improved corrosion resistance of the bronze specimens with structures modified due to the use of mechanical and thermal treatments. In turn, the addition of the Al-5Si alloy is the most effective means for modifying the material in order to increase its resistance to electrochemical corrosion.
OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 25 No. 1 2023 Fig. 9. Surface roughness after electrochemical corrosion of the C65500 specimen with the addition of aluminum filament. Printing modes 1 (1), 2 (2) and 3 (3). Samples after annealing (4), deformation and subsequent annealing (5). Samples with the addition of 10 wt.% Al (6), 10 wt.% Al–5Si (7) and 10 wt.% Al–12Si (8) Fig. 10. Mass loss after electrochemical corrosion of the C65500 specimen with the addition of aluminum filament. Printing modes 1 (1), 2 (2) and 3 (3). Samples after annealing (4), deformation and subsequent annealing (5). Samples with the addition of 10 wt.% Al (6), 10 wt.% Al–5Si (7) and 10 wt.% Al–12Si (8)
OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 25 No. 1 2023 Tribological tests The change in the structural and phase state, as well as in the mechanical properties, also affected the results of testing the specimens for friction and wear. From the beginning of testing, the coefficient of friction coefficient (CoF) values are high for bronze C65500 specimens printed with different heat inputs (Fig. 11). Then it decreases by about 20%, after which it begins to increase monotonically until reaching the previous high values. During sliding of a specimen with a structure formed as a result of high-temperature annealing, significant fluctuations in the value of CoF are observed (reach an amplitude of ~0.2) and occupy most of the test time. Sliding of the predeformed and annealed specimen shows the CoF oscillations at the final stage of testing as high as ~0.25. The average CoF values of specimens printed with low (mode 1), medium (mode 2) and high (mode 3) heat input are 0.52, 0.39 and 0.29, respectively. For the specimen after high-temperature annealing, the CoF is 0.3, and for the sequentially deformed and annealed it is 0.34. The high amplitude of the CoF fluctuations is partly due to the test scheme. With reciprocating sliding, the sliding speed is not a constant value in all sections of the friction track. Upon reaching the final section of the friction track, it tends to zero, and then quickly recovers at the start of motion in each new sliding cycle. As a result, a slight change in friction conditions occurs at the extreme sections of the friction track, which affects the magnitude of the friction force. During sliding of specimens printed with the addition of aluminum filament, a different character of the change in the coefficient of friction is observed (Fig. 12). In the beginning, the CoF increases for ~150 seconds, which may correspond to a running-in period, and then stabilizes at a certain level. At the same time, the CoF value significantly decreased in comparison with that of bronzes printed without aluminum additives. The average CoF value is 0.184, 0.28 and 0.191 in the friction of bronze specimens printed with the addition of 10 wt.% Al, Al-5Si and Al-12Si, respectively. To explain the reasons for the CoF fluctuations, the surfaces of wear tracks on bronze specimens (Figs. 13, 15) and the surfaces of steel balls (Figs. 14, 16) were examined. On the surface of the asprinted bronze C65500 specimens, the pronounced wear tracks were formed and the surfaces of these tracks were covered with dark oxides and traces of mechanical damage. On the periphery, traces of deformation of individual sections of the material are also visible; this indicates plastic deformation of the specimens under the action of the counterbody during sliding friction. No signs of wear were found on the surfaces of the steel balls (Fig. 13), which is natural due to its significantly higher hardness compared to those of specimens printed from C65500 bronze. At the same time, Fig. 11. Change in the value of the coefficient of friction during tribological tests of C65500 specimens Fig. 12. Change in the value of the coefficient of friction during tribological tests of C65500 specimens, printed with the addition of aluminum filament
OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 25 No. 1 2023 Fig. 13. Images of the wear surfaces of C65500 bronze specimens, printed according to 1 (a), 3 (b) and 7 (c) EBAM modes, annealed specimen (d), deformed and annealed specimen (e) a b c d e the marks of bronze adhered to balls’ surface are observed. This is due to the adhesive wear mechanism in the considered steel-bronze friction pair. The thickness of these adhesion transferred layers does not exceed 1.5 μm, which was established from measurement of a three-dimensional surface profile using laser scanning microscopy. The surface of wear tracks of bronze specimens (Fig. 15), printed with the addition of aluminum filament, significantly differs from those of the tracks on the surface of as-printed bronze specimens C65500 (Fig. 13). There are no traces of plastic deformation of the material at the periphery of the tracks; there is also no surface oxidation in the form of dark spots. At the same time, on the periphery of the tracks there are areas with material pushed aside as a result of deformation. The surface of the balls (Fig. 16) is covered with a layer of adhesion-transferred bronze, which is significant both in area and in thickness. The thickness of the adhered material is uneven over the entire area and reaches 5–12 µm. This indicates a stronger adhesive interaction between the materials of the friction pair. The experimental data obtained indicate that in the case of dry reciprocating sliding of the specimens, the CoF fluctuations were revealed, which are unavoidable with the use this experimental scheme and the combined adhesive-oxidative wear mechanism.
OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 25 No. 1 2023 Fig. 14. Images of the surface of steel balls after friction in a pair with C65500 bronze specimens, printed according to 1 (a), 3 (b) and 7 (c) EBAM modes, annealed specimen (d), deformed and annealed specimen (e) a b c d e a b c Fig. 15. Images of the wear surfaces of C65500 bronze specimens, printed with the addition of 10 wt.% Al (a), 10 wt.% Al–5Si (b) and 10 wt.% Al–12Si (c) a b c Fig. 16. Images of the surface of steel balls after friction in a pair with C65500 bronze specimens, printed with the addition of 10 wt.% Al (a), 10 wt.% Al–5Si (b) and 10 wt.% Al–12Si (c)
OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 25 No. 1 2023 Quantitative determination of the amount of wear was carried out by determining the cross-sectional profile of wear tracks according to the standard ASTM G133-05 method. To do this, cross-sectional profiles of wear tracks formed on the surfaces of specimens were reconsrtucted for the as-printed bronze C65500 (Fig. 17, a) and bronze with the addition of aluminum filament (Fig. 17, b) using the software. The obtained profiles confirm the presence of the material deformation and its displacement to the periphery of the wear tracks. The key feature of the formation of burrs is the relationship between its height and the mechanical properties of the specimens. The most ductile and least hard specimens are more severely deformed during friction and the highest burrs are formed on its surface. Harder specimens printed with the addition of aluminum filament are less prone to plastic deformation during sliding friction, and the height of the burrs formed on its surface is 2–3 times less (10–15 µm) than for specimens made of bronze (20–30 µm). a b Fig. 17. Cross-section profiles of the wear tracks of specimens, printed from bronze С65500 (a) and with the addition of aluminum filament (b) In accordance with the standard method, the cross-sectional areas of the wear tracks were determined. It can be observed from Figure 18, that the largest cross-sectional area of the wear track was formed during testing of the annealed specimens of bronze C65500 in accordance with its lowest microhardness. As a result, under conditions of microcontact interaction in a friction pair, its material is easier to deform and wear out. In turn, the use of pre-deformation followed by annealing makes it possible to reduce wear by 15–30% for specimens printed from bronze C65500. This is ensured by a fine structure, which more effectively resists plastic deformation due to the presence of a large number of grain and twin boundaries. Among the specimens printed with the addition of aluminum filament, the highest wear resistance was obtained when intermixing the bronze with the Al-5Si alloy. Its wear is 25% less than that of the most wear-resistant specimen of as-printed bronze C65500. This is due to its high microhardness and mechanical strength. The decrease in wear resistance of alloys printed with the addition of aluminum and Al-12Si is due to its mechanical properties and phase composition. In the first case, the alloy has low ductility and subsurface fracture is more feasible during sliding. In the second case, the addition of Al-12Si to C65500 greatly increases the amount of silicides, which adversely affect the properties of the alloy. During sliding, these fine silicides can be pulled out of the matrix and then act on the surface as abrasive particles, increasing the wear of the bronze surface. In addition, alloys printed with the addition of aluminum filament are less prone to the formation of oxide layers. Because of this, the protective function of the oxide layers is not fulfilled and wear occurs mainly due to the adhesive mechanism. As a result, despite high mechanical properties and microhardness, wear reduction is not so significant.
OBRABOTKAMETALLOV MATERIAL SCIENCE Vol. 25 No. 1 2023 Fig. 18. Cross-sectional area of the wear tracks for specimens printed from bronze С65500 and with the addition of aluminum filament. Printing modes 1 (1), 2 (2) and 3 (3). Samples after annealing (4), deformation and subsequent annealing (5). Samples with the addition of 10 wt.% Al (6), 10 wt.% Al–5Si (7) and 10 wt.% Al–12Si (8) Conclusions The paper presents the results of experimental studies of silicon bronze C65500, printed using the technology of electron beam additive manufacturing. Based on the results obtained, the effect of printing conditions and the addition of aluminum filament on the structure, mechanical properties, as well as its relationship with the corrosion resistance and wear resistance of the specimens were established. 1. According to the studies performed, the addition of 10 wt.% aluminum filament leads to the formation of a two-phase structure in printed specimens. In this case, the main phase is the α-Cu solid solution with secondary HCP γ-phase precipitates. The formation of the two-phase structure contributes to improving the strength by ~1.2–1.9 times and microhardness by ~1.4–2.2 times, as well as impairing the ductility by 1.1–5.4 times compared with single-phase specimens. 3. As a result of the study of corrosion resistance, it is shown that corrosion proceeds without the formation of pitting on the surfaces of silicon bronze and bronzes printed with the addition of aluminum filament. 4. High-temperature annealing, as well as plastic deformation by compression followed by annealing, contributed to a reduction in mass loss by 15–30% for specimens printed from silicon bronze. 5. The addition of aluminum filament made it possible to further reduce the weight loss of printed specimens by 13–31%, relative to specimens printed from bronze C65500. 6. The use of deformation followed by annealing makes it possible to reduce wear by 15–30% for specimens printed from bronze C65500. This is ensured by a fine structure, which more effectively resists plastic deformation due to the presence of a large number of grain boundaries. 7. The addition of 10 wt.% alloy Al-5Si in the process of printing bronze contributed to an increase in the wear resistance of the material by 25%, compared with specimens from bronze C65500. The results obtained can be used in the development of technologies for the additive production of products from silicon bronzes.
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