Edelweiss Applied Science and Technology ISSN: 2576-8484 Vol. 8, No. 5, 598-607 2024 Publisher: Learning Gate DOI: 10.55214/25768484.v8i5.1720 © 2024 by the authors; licensee Learning Gate © 2024 by the authors; licensee Learning Gate * Correspondence: mgrigor@rocketmail.com Solar technology for the production of Bi/Pb superconducting ceramics and its properties D. Gulamova1, Т. Gulamov2, G. Mamniashvili3*, G. Donadze4, V. Peikrishvili5 1Materials Science Institute, SPA “Physics-Sun”, Academy of Sciences, 700084, Tashkent, Uzbekistan., Tashkent, Uzbekistan. 2Almalyk branch of National University of Science and Technology “MISIS”, Almalyk, A. Temurst., 56, Uzbekistan. 3,4Andronikashvili Institute of Physics at Tbilisi State University, 6 Tamarashvili St., 0177, Tbilisi, Georgia; mgrigor@rocketmail.com (G.M) 5F. Tavadze Institute of Metallurgy and Materials Science, 10, E.Mindeli St. 0186, Tbilisi, Georgia. Abstract: Based on the experience of isostoichiometric and isostructural oxides production using solar energy, the prospects for synthesizing of Bi/Pb superconducting ceramics are shown. The principle of technology in the Large Solar Furnace (Parkent), the influence of gradient conditions on the formation of the oriented structure of crystallites-nuclei, and the connection of the innate properties of precursors with the lamellar morphology and phase composition of massive ceramics are described. The homophase composition of Bi/Pb ceramics was determined. Graphs of resistance and voltage of BSCCO in the temperature range 80-320K are presented. Anomalous of resistance and magnetic susceptibility in bismuth cuprates synthesized by solar energy were observed. Experimental graphs in resistance and magnetic susceptibility changes represent dependencies characteristic of the potential superconducting transitions. The manifestation of the Meissner effect at room temperature and normal atmospheric pressure and daylight, and under the influence of light is shown. The properties of Bi/Pb ceramics are explained by the connection with the innate properties of precursors obtained by concentrated solar energy. Keywords: BSCCO, Homophase composition, Intergrain boundaries, Morphology, Precursors, Ceramic, Resistance, Solar technology, Synthesis, Voltage, XRD. 1. Introduction Promising examples of “nitrogenous” superconductors practical use in various fields of human life activities force us to continue experimental and theoretical research on the way to searching technologies for creating room-temperature massive superconducting materials, which are necessary for high current energetics and massive products. Results of the using various technologies show the importance of the principle process and conditions influencing the critical characteristics of target superconductors [1-16]. Current parameters direct the dependence on the microstructure perfection and force to search for technologies and conditions that allow the formation of a massive oriented crystalline structure of superconducting ceramics. Application of known texturizing technologies with directed impact of the gradient heat flow led to positive results concerning the thin superconducting films, but it is a very challengingly difficult technology process to create the oriented microstructure in massive ceramics with congenital misoriented microstructure. In comparison with technologies based on “solid state reaction” the melting technologies, based on the principle of growing up monocrystals with oriented crystallization of melt, allows for the creation of a high texture [17]. However, the necessity of maintaining a flat crystallization front for implementation of peritectic equilibrium, a low crystallization process speed, high energy consumption, an inert crucible problem, and the complicated technological equipment confine the wide practical application of these technologies. Developed in 599 Edelweiss Applied Science and Technology ISSN: 2576-8484 Vol. 8, No. 5: 598-607, 2024 DOI: 10.55214/25768484.v8i5.1720 © 2024 by the authors; licensee Learning Gate recent years the nontrivial energy-saving, green “Super Fast Alloys Quenching–T” (“SFAQ”) technology of superconducting cuprates synthesis is founded on using solar energy for melting and hardening in sharp temperature gradient conditions. [18-23]. The positive results, reached by using this method, raise expectations of progress in obtaining massive high-temperature superconducting ceramics by solar energy. The article presents the features of solar technology and the results of studies of precursors and ceramics of Bi/Pb cuprates to present experimental data to expand the practical applications of solar technologies in the materials science of bismuth superconductors. 2. Synthesis Methods Results and Discussions Mixtures for bismuth cuprates synthesis by solar energy were prepared from compounds of Bi2O3, PbO, SrO, CaO, CuO powders according to formula Bi1.7Pb0.3Sr2Ca(n-1)Cu(n)Oy, n=3-30. Before the synthesis in a large Solar Furnace (LSF) (Parkent), the analysis of optical-energy parameters meeting the requirements for melting and hardening was carried out. These parameters provide the directed microstructure, the eutectic phase amorphization, and the average productivity of ≈20kg/sunny day for the above pointed mixture composition above [24]. The directed growth of crystallite-nuclei is accomplished through a sharp temperature gradient in molten bath and remains at firing it. This is one of the most valuable advantages of solar gradient technology, which is very complicated or impossible to implement by the most known processes. To implement the “solar” technological process of obtaining material by melting or heat treatment it is necessary to arrange the initial powder (mixture) into a melting area (or heat treatment one) so that excludes the way out of the focal the zone and the dropping of drops the mixture from the water-cooled substrate. In the case of the inclined arrangement of a water-cooled substrate, it is necessary to define optimal tilt angle of a substrate and the density of falling concentrated solar flux on the material substrate to direct crystallite growth in a direction of solar flux vector. In this way, the sustainable implement of the molten bath position during the melting of mixtures and the orientation of formed in the melt crystallites in a direction of heat source is reached. The appropriate density of solar flux needed for the melting of mixtures of the superconducting cuprates is approximately defined from the ionization energy of oxides included in the formula of Bi1.7Pb0.3Sr2Ca(n-1)Cu(n)Oy, n=3-30, and data on the energy of formation of bismuth cuprates [25]. The substrate was inclined at an angle of about 30 degrees to the optical axis of LSF (Parkent). Solar flux density in the focal zone of the substrate was calculated [26]: Sc=S0 ′·cosi (Sc– direct radiation, i– angle of incidence of solar flux). 1) 4=∡70o, i=∡0o S4=S0cosi S4=7.45 wt/cm2cos0=7.45 Wt/cm2 2) 3=∡52.5o, i=∡17.5o S3=S0cosi S3=30.29 wt/cm2cos17.5=28.88 Wt/cm2 Allowing for errors in LSF optical system due to inaccuracies of mirror adjustment and dust on their surface, the solar flux density was not less than 400 wt/sm2. The substrate position scheme in the Bi/Pb synthesis process and the positions of the mixture and melt on the water-cooled base in LSF are shown in Figure 1а,b,с. 600 Edelweiss Applied Science and Technology ISSN: 2576-8484 Vol. 8, No. 5: 598-607, 2024 DOI: 10.55214/25768484.v8i5.1720 © 2024 by the authors; licensee Learning Gate Figure 1. Water-cooled substrate position scheme of the molten melt (mixture) bath in the technological process of synthesis in Large Solar Furnace (a), prepared mixture charge for melting (b), the synthesis process in a melt on the water-cooled base, inclined at an angle ≈30о to the optical axis of Large Solar Furnace (Parkent). The technological process of synthesis of Bi/Pb superconductors was preceded by the analysis of previously performed technologies of synthesis of materials of different composition: Al2O3, Al2TiO5, ZrO2-Al2O3 (eutectic), SrTiO3, BaTiO3, CaTiO3, Bi/Pb (BSCCO), partly presented in Fig. 2 [26]. Figure 2. Materials, obtained by melting and hardening in the LSF (Parkent) according to the scheme with the slope angle of the water-cooled substrate ≈ 30о. For the synthesis of materials with different properties, the concentrated solar flux with a power which appropriating to their melting temperatures, color, and bulk density was required. A similar method of the parameter optimization of the LSF optical-energy system was used in the technology of the Bi/Pb synthesis. Before the melting a mixture is heated in the solar flux densities interval 150 – 300wt/cm2. At a solar flux density of ~ 460wt/cm2, after the melt bath was formed, the melt was formed, the melt was hardened in a dispersant [20-23]. In Fig. 1с it could be imagined the parameters of melt which is discharged by a thin jet onto the dispersant. The melted charge on which the melt is located is a garnish fragment which is represented in Fig. 3a, which is the support for the melt. Plate precursors are shown in Fig. 3b. Figure 3. Chipped pieces of garnish (а); plate-precursors, obtained by hardening melt in dispersant (b). 601 Edelweiss Applied Science and Technology ISSN: 2576-8484 Vol. 8, No. 5: 598-607, 2024 DOI: 10.55214/25768484.v8i5.1720 © 2024 by the authors; licensee Learning Gate Plate precursors` microstructure is represented by oriented nanocrystallites surrounded by an amorphous phase. ХRD patterns show crystalline and traces of the X-ray amorphous phases (Fig. 4 a, b, с). Figure 4. Oriented nano crystallite nuclei, surrounded by amorphous phase (а, b, c); ХRD patterns of precursor with nominal composition Bi1.7Pb0.3Sr2Ca(n-1)Cu(n)Oy, n=20 (d). The structure of a ceramics, which is made of glass precursors, consists of mutually disassembled block plates, showed in Fig. 5a. The unit block comprises layers-plates separated by nano-dimensional inter-grain boundaries (Fig. 5b). Such morphology is formed based on the oriented layered structure of crystallite germs shown in Fig. 4 a, b. Figure 5. Disoriented ceramic chip microstructure (a); Laminated unit microstructure with nano-dimensional grain boundaries (b). The phase ceramic composition of ceramics represented by homologous phases of a series Bi1.7Pb0.3Sr2Ca(n-1)Cu(n)Oy, n=20. For example, in Fig. 6 the diffractogram of ceramics of nominal composition "n=20" is shown with fragments representing a series of reflexes with close values 2Ɵ, indicated in the phase homologs assumption. The parameters of the phase homolog elementary cell given in Table 1 are calculated by extreme and middle reflexes. 602 Edelweiss Applied Science and Technology ISSN: 2576-8484 Vol. 8, No. 5: 598-607, 2024 DOI: 10.55214/25768484.v8i5.1720 © 2024 by the authors; licensee Learning Gate Figure 6. Diffractogram of ceramics with nominal composition Bi1.7Pb0.3Sr2Ca(n-1)Cu(n)Oy, n=20 with fragments of phase-homologs. Table 1. Parameters of the elementary cell of phase homologs of series Bi1.7Pb0.3Sr2Ca(n-1)Cu(n)Oy, n=20, calculated from a low angle, large angle, and mean reflexes. Compo sition Parameters of a unit cell according to the extreme small-angle reflection Parameters of a unit cell according to the average reflection Parameters of a unit cell according to the extreme high angle reflection 2223 аav.=3,8609 c/а=9,6578 c/b=9,8064 аav.=3,8424 c/а=9,6277 c/b=9,7485 аav.=3,8180 c/а=9,6324 c/b=9,7338 bav.=3,8024 bav.=3,7948 bav.=3,7782 c=37,2877 c=36,9936 c=36,7764 2245 аav.=3,8955 c/а=12,7294 c/b=12,9718 аav.=3,8396 c/а=12,8605 c/b=12,9897 аav.=3,8250 c/а=12,8163 c/b=12,8752 bav.=3,8227 bav.=3,8014 bav.=3,8075 c=49,5872 c=49,3792 c=49,0224 2267 аav.=3,8523 c/а=16,0723 c/b=16,0150 аav.=3,8375 c/а=16,0014 c/b=16,0311 аav.=3,8022 cav.=61,1119 c/а=16,0728 c/b=16,0550 cav.=61,9267 cav.=61,4054 2289 аav.=3,8549 c/а=19,3456 c/b=19,4455 аav.=3,8293 c/а=19,3489 c/b=19,3930 аav.=3,8262 c/а=19,1375 c/b=19,3689 bav.=3,8351 bav.=3,8206 bav.=3,7805 c=74,5755 c=74,0928 c=73,2240 221112 аav.=3,8512 c/а=24,0560 c/b=24,4988 аav.=3,8140 c/а=24,1960 c/b=24,3460 аav.=3,7667 c/а=24,3633 c/b=24,0240 bav.=3,7816 bav.=3,7905 bav.=3,8199 cav.=92,6445 cav.=92,2837 cav=91,7694 221415 аav.=3,8824 c/а=28,6791 c/b=29,0297 аav.=3,8583 c/а=28,6918 c/b=29,0326 аav.=3,8311 c/а=28,7372 c/b=28,9548 bav.=3,8355 bav.=3,8130 bav.=3,8023 cav.=111,3436 cav.=110,7014 cav.=110,0950 221920 аav.=3,8382 c/а=37,1070 c/b=36,7461 аav.=3,8264 c/а=37,0890 c/b=36,9230 аav.=3,7731 c/а=37,2553 c/b=36,5796 bav.=3,8759 bav.=3,8436 bav.=3,8428 cav.=142,4241 cav.=141,9174 cav.=140,5681 222425 аav.=3,8657 c/а=36,6408 c/b=37,1161 аav.=3,8287 c/а=36,7605 c/b=36,5838 аav.=3,8032 c/а=36,8315 c/b=36,6504 b=3,8162 b=3,8472 b=3,8220 cav.=141,6423 cav.=140,7450 cav.=140,0777 222930 аav.=3,8584 c/а=36,6082 c/b=36,7119 аav.=3,8439 c/а=36,6106 c/b=36,7607 аav.=3,8090 c/а=36,8552 c/b=36,7001 bav.=3,8475 bav.=3,8282 bav.=3,8251 cav.=141,2492 cav.=140,7273 cav.=140,3816 603 Edelweiss Applied Science and Technology ISSN: 2576-8484 Vol. 8, No. 5: 598-607, 2024 DOI: 10.55214/25768484.v8i5.1720 © 2024 by the authors; licensee Learning Gate The resistance and voltage of ceramics of all nominal formulations is affected by the temperature- time firing mode at normal atmospheric pressure. The electrophysical properties were studied using resistive 4-pin [28] and magnetic inductance [29] methods. These methods determined voltage, current, and resistance with a Rigol DM3058E multimeter. The temperature is determined by chromel-copel and chromel-alumel thermocouples, graduated in boiling water and ice. When a sample is placed within of sensing coils of an ac susceptometer [29] the voltage balance is disturbed and measured voltage U is proportional to the susceptibility of the sample. In the graphs of resistance R and voltage U, measured on the same samples, the anomalous effects are repeated in similar temperature intervals of 280-300 K (Figs. 7-10). The resistance of ceramics obtained in a temperature range of 840-850оС, by firing during less than 10 hours, represents a resistance drop characteristic of a semiconductor with a temperature increase in the range of 80-320 K (Fig. 7a). After increasing the firing time at 18 hours, the smooth dependence of R(Ω)- ToC (Fig. 7a) is broken, the effects of resistance drop in the temperature range 220-240 K and increased resistance at 310 K (Fig. 7b) appear. The anomalous effect at 310 K may be due to the influence of the superconducting phase. A Figure. 7. Dependences of resistances (a, b) and voltage (c) on temperature of cuprate ceramics of nominal composition Bi1.7Pb0.3Sr2Ca(n-1)Cu(n)Oy, n=20, obtained at a temperature of 840-846oC, at firing ≈10 h.(a) and ≈18 h (b, c). The resistance and voltage tension of ceramics obtained by firing for 30-48 hours represents almost constant dependence with weak abnormal deviations near 310K (Fig. 8 a, b). Figure 8. Dependence of resistance (a) and voltage (b) on the temperature of ceramic cuprates of nominal composition Bi1.7Pb0.3Sr2Ca(n-1)Cu(n)Oy, n=20, obtained at a temperature of 840-846оС and firing time ≈30-48 hours [27]. Almost a full-volume content of phases with Tc=120-152 K is obtained in ceramics, fired during 115 h (Fig. 9 a, b). Deviations from the linear relationship occur in a temperature range of 300-320 K 604 Edelweiss Applied Science and Technology ISSN: 2576-8484 Vol. 8, No. 5: 598-607, 2024 DOI: 10.55214/25768484.v8i5.1720 © 2024 by the authors; licensee Learning Gate Figure 9. Dependence of resistance (a) and voltage (b) on the temperature of ceramic cuprates of nominal composition Bi1.7Pb0.3Sr2Ca(n-1)Cu(n)Oy, n=20, obtained at temperatures 840- 846oC, 115 hours. In firing mode 843-847oC, 20-24 hours ceramic samples with anomalies above 260K in high temperature area were obtained. The resistance and voltage dependences on temperature are shown in Fig. 10 a, b indicating effects near 270 K and 300 K. These anomalies consist of the torsion oscillation determined of superconducting phase at Tc=295 K [23]. A resistance other than zero could be related to the percolation effects, i.e. the microstructure of the ceramic ship (Fig. 4a) shows a violation of strictly oriented microstructure. Figure 10. Resistance (a) and voltage (b) of ceramic made in 843-847oC mode, 20-24 h. Confirmation of the formation by the superconductive phases in a temperature range above 280 K may be a sample ejection effect at room temperature and normal atmospheric pressure (Meissner effect) shown in Fig. 11 a, b, c. Figure 11. 605 Edelweiss Applied Science and Technology ISSN: 2576-8484 Vol. 8, No. 5: 598-607, 2024 DOI: 10.55214/25768484.v8i5.1720 © 2024 by the authors; licensee Learning Gate Ejection of the magnet by a ceramic sample of nominal composition Bi1.7Pb0.3Sr2Ca(n-1)Cu(n)Oy, n=20 at room temperature, normal atmospheric pressure, under the influence of light (a), (b), (c) [23]. The new result is the ejection effect of the magnet from the ceramic of all nominal of the Bi1.7Pb0.3Sr2Ca(n-1)Cu(n)Oy, n=3-20 range at room temperature and normal ambient pressure, daylight (Fig. 11a,b,c) and white light source. Ceramics exhibit no ferromagnetic properties, so the effects of ejection of the magnet from the samples (Meissner effect) in comparison with anomalies on graphs R(Ohm)-T(K) at room temperature and normal pressure could be explained by the assumption of superconducting phases. 3. Conclusion Depending on the reaction of the formation of the material of a given composition by the variation of the density of the solar flux in the focal zone of the LSF (Parkent), materials with different melting temperatures, formed according to different types of reactions - congruent or incongruent can be synthesized. The properties of isostructural and isostochiometric oxide groups of different compositions showed certain advantages of solar technologies: completeness of synthesis, purity of process, suppression of peritectic reaction, etc. On the example of Bi/Pb cuprate, the possibility and advantages of green "sun" technology for the production of Bi/Pb superconducting cuprate ceramics have been determined. The developed "SFAQ" gradient technology allows us to obtain positive results, namely to synthesize full- volume superconducting ceramics with Tc=110 K and to obtain room-temperature superconducting phases with Tc 280-317 K. The Bi/Pb cuprate synthesis requires of the peritectic interaction between the initial components. Optimum solar technology meets the important requirement of superconducting materials - the formation of oriented crystallites-embryos that are the innate basis of the nano-dimensional plate- oriented ceramic microstructure and the "freezing" of the amorphous eutectic involved in the superconducting phase formation reaction. For the first time, the microstructure of ceramics represented by superconducting homologous phases was obtained by solar technology. Different stoichiometry of phase homology determines the potential difference and, accordingly, the charge concentration at the inter-grain boundaries. In the case of such a process, it is possible an assumption about the negative influence compensation by crystal lattice on conduction electrons. The increase in charge density is directly related to the increase in the Cooper pairs density and critical properties. The mobility and advantages of "green" technology make it possible to offer solar technologies for both the research and synthesis of experimental and industrial batches of materials of a given composition. The use of "solar" technology for the synthesis of materials used in the film technology is advisable, since the average productivity of LSF (Parkent), ranging from 20-30 kg/solar day, can provide raw material for the industrial production of film equipment, chips, etc. Acknowledgments: The authors express gratitude to the technical staff of the LSF (Parkent) for assistance in the conduct of melting processes and to Bobokulov S.H. and Eshonkulov E.B. for the conduct of measurements. This work was supported by grants: MRB-2021-533; FR-22-8346 and the Shota Rustaveli National Science Foundation of Georgia (SRNSFG) [STEM-22-1030]. Copyright: © 2024 by the authors. 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