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Microstructure and Thermoelectric Characterization of Composite www.nature.com/scientificreports OPEN Microstructure and Thermoelectric Characterization of Composite Nanofber Webs Derived from Polyacrylonitrile and Sodium Cobalt Oxide Precursors Kyoung Moon Ryu1, Young Hun Kang2, Song Yun Cho2, Sang Hoon Lee1, Young Chul Choi1, Min Su Kim1 & Young Gyu Jeong1 ✉ We report the microstructure and thermoelectric properties of composite nanofber webs, which were fabricated by dual-electrospinning of polyacrylonitrile (PAN) and sodium cobalt oxide (NaCo2O4) precursor solutions with diferent input compositions and following heat-treatment at 600–900 °C for simultaneous carbonation and calcination. The SEM and EDS mapping images revealed that PAN- derived carbon nanofbers (CNFs) and NaCo2O4-based ceramic nanofbers coexisted in the composite nanofber webs and that their relative contents could be controlled by the input compositions. The Seebeck coefcient increased from ~26.77 to ~73.28 μV/K and from ~14.83 to ~40.56 μV/K with increasing the relative content of NaCo2O4 nanofbers in the composite nanofber webs fabricated at 700 and 800 °C, respectively. On the other hand, the electrical conductivity of the composite nanofber webs increased with the decrement of the relative content of NaCo2O4 nanofbers as well as the increment of the heat-treatment temperature. Owing to the opposite contributions of NaCo2O4 nanofbers and CNFs to the Seebeck coefcient, electrical conductivity and thermal conductivity, a 2 maximum power factor of ~5.79 μW/mK and a fgure of merit of ~0.01 were attained for CNF/NaCo2O4- based composite nanofber webs fabricated at 45 wt% input composition of NaCo2O4 and at heat- treatment of 700 °C. Termoelectric materials and devices have a lot of potential because they have the advantage of using eco-friendly methods to generate electrical energy using the waste heat from the industry and human or the heat in nature1. Tose materials and devices are based on the thermoelectric efect, which is the reversible conversion between electrical energy and thermal energy. Te performance of the thermoelectric materials can be evaluated as a thermoelectric fgure of merit, ZT = S2σT/κ, S is the Seebeck coefcient, σ is the electrical conductivity, κ is the thermal conductivity and T is the absolute temperature2–5. Terefore, high electrical conductivity, large Seebeck coefcient and low thermal conductivity are required for high performance thermoelectric materials. Especially, nanostructured materials are considered to be efective than bulk materials in enhancing ther- moelectric fgure of merit through phonon scattering at grain boundaries and interfaces. Termoelectric mate- rials are divided into organic and inorganic materials. For organic thermoelectric materials, many researchers have investigated by using electrically conductive polymers, such as polypyrrole, polyaniline and poly(3 ,4-ethylenedioxythiophene):poly(styrene sulfonate) (PEDOT/PSS)6–10. Te conductive polymers exhibited cost efectiveness, high fexibility, low intrinsic thermal conductivity and outstanding potential for use on the human body and bent part. However, electrically conductive polymer-based thermoelectric materials are difcult to use as thermoelectric energy harvesters because of their low power factor (S2σ), high contact resistance with metal electrodes and very low thickness11–13. In order to achieve high output power density, the use of inorganic thermoelectric materials is inevitable. Among transition metal oxide-based inorganic thermoelectric materials, 1Department of Advanced Organic Materials and Textile System Engineering, Chungnam National University, Daejeon, 34134, Republic of Korea. 2Division of Advanced Materials, Korea Research Institute of Chemical Technology, Daejeon, 34114, Republic of Korea. ✉e-mail: [email protected] SCIENTIFIC REPORTS | (2020) 10:9633 | https://doi.org/10.1038/s41598-020-66667-6 1 www.nature.com/scientificreports/ www.nature.com/scientificreports sodium cobalt oxide (NaCo2O4) is known to have high Seebeck coefcient of ~100 μV/K and ZT value of ~1.2 at 800 K14–18, in addition to non-toxicity, high thermal and chemical stability. However, the inorganic thermoelectric materials are typically expensive and brittle, which renders their application in large areas difcult. In this study, to overcome the disadvantages of each organic and inorganic thermoelectric materials, we have fabricated a series of composite nanofber webs composed of NaCo2O4-based ceramic nanofbers and polyacry- lonitrile (PAN)-derived carbon nanofbers (CNFs), and have investigated their microstructure and thermoelectric performance by considering the relative compositions of NaCo2O4 and CNFs as well as fabrication temperature. For the purpose, NaCo2O4 precursor and PAN were dissolved in a solvent, independently, and two solutions were spun simultaneously into single nanofber web by using dual-electrospinning technique. Ten, the as-spun nano- fber webs were heat-treated at diferent temperatures of 600–900 °C for calcination and carbonization to develop both NaCo2O4-based nanofbers and PAN-derived carbon nanofbers (CNFs) in the fnal nanofber webs. Te morphology and microstructures of the as-spun and heat-treated composite nanofber webs were characterized by using electron microscopy, energy dispersive spectroscopy, and X-ray difraction technique. Te electrical conductivity, thermal conductivity, Seebeck coefcient and thermoelectric power factor of the composite nano- fber webs were investigated by considering the compositions and microstructural features developed at diferent heat-treatment temperatures. Experimental Materials. Polyacrylonirile (PAN, Mw = 150,000 g/mol, Sigma Aldrich Com.) and N,N-dimethylformamide (DMF, 99.0%, Samchun Com.) were used for the preparation of CNF precursor solution. Poly(vinyl pyrroli- done) (PVP, Mw = 1,300,000 g/mol, Sigma Aldrich Com.), methanol (99.5%, Samchun Com.), sodium acetate trihydrate (99.0%, Alfa Aesar Com.) and cobalt(II) acetate tetrahydrate (98.0%, Alfa Aesar Com.) were used for preparing NaCo2O4 precursor solution for the electrospinning. All the chemicals and materials were used without further purifcation. Fabrication of composite nanofber webs. A series of composite nanofber webs, which are composed of NaCo2O4 nanofbers and PAN-derived CNFs, was fabricated, as shown schematically in Fig. 1. First, three diferent NaCo2O4 precursor solutions for electrospinning were prepared by dissolving sodium acetate trihy- drate, cobalt (II) acetate tetrahydrate, and PVP in methanol. Here, the mole ratio of sodium acetate trihydrate and cobalt (II) acetate tetrahydrate as NaCo2O4 precursors was controlled to be 1.1:2.0 and the concentrations of NaCo2O4 precursors in methanol were set to be 17.3, 32.0 and 44.0 wt%. Afer stirring those solutions at 20 °C for 30 min, PVP was added into each NaCo2O4 precursor solutions, which were then stirred until homogene- ous solutions were obtained. A PAN solution for electrospinning was also prepared by dissolving PAN in DMF. Te concentration of PAN in the solution was adjusted to be 6.0 wt%. To prepare precursor nanofber webs via 19–21 dual-electrospinning , the PAN solution and a NaCo2O4 precursor solution, which were put in diferent syringes of 25 mL, were electrospun simultaneously into a rotating metal collector through a 23 gauge needle at the condition of a feeding rate of 0.5 mL/h, electric potential of 25 kV, and distance between the syringe metal tips and the collector of 30 cm. Te as-spun nanofber webs were dried at 60 °C for 2 h to remove any residual solvent and then transferred into a tubular furnace for two-step heat-treatment, which was associated with the stabili- zation/carbonization of PAN nanofbers as well as the calcination of NaCo2O4 precursor nanofbers. Te frst heat-treatment was carried out at 260 °C for 1 h under air condition for thermal stabilization of PAN nanofber component in the dual-electrospun nanofbers. For the calcination to form NaCo2O4 ceramic nanofbers as well as for the carbonization of thermally-stabilized PAN nanofbers, the second heat-treatment was performed by heating the thermally stabilized nanofbers to diferent temperatures of 600–900 °C at a heating rate of 10 °C/min and holding at each fnal temperature for 1 h under argon gas atmosphere. Te fnal CNF/NaCo2O4 composite nanofber webs manufactured at diferent input compositions and heat-treatment temperatures were named as TMx-y, where x and y denote the content of NaCo2O4 nanofbers by wt% and the calcination/carbonization tem- peratures of 600–900 °C, respectively, as listed in Table 1. Characterization of composite nanofber webs. Te temperature-dependent thermal decomposition behavior of the components for fabricating CNF/NaCo2O4-based composite nanofber webs was analyzed by using a thermogravimetric analyzer (TGA 4000, Perkin Elmer Inc.). TGA experiments were carried out under nitrogen gas condition from room temperature to 800 °C at a heating rate of 10 °C/min. Te morphological features and elemental composition of the as-spun and heat-treated composite nanofber webs were examined by a scanning electron microscope (SEM, JSM-7000F, JEOL) equipped with an energy dis- persive X-ray spectrometer (EDS). For the SEM experiment, all the nanofber samples were coated with platinum to prevent any surface charging. Te elemental composition of the composite nanofber webs fabricated at difer- ent heat-treatment temperatures of 600–900 °C was analyzed by using EDS data. Te crystalline features of the composite nanofber webs were identifed by a high resolution X-ray
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