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In this paper, a new synthesis of carbon nanofibers (CNFs)/carbon nanowalls (CNWs) was performed to improve the characteristics of anode materials of lithium-ion batteries by using the advantages offered by CNWs and CNFs. Among the carbon-based nanomaterials, CNWs provide low resistance and high specific surface area. CNFs have the advantage of being stretchable and durable. The CNWs were grown using a microwave plasma-enhanced chemical vapor deposition (PECVD) system with a mixture of methane (CH₄) and hydrogen (H₂) gases. Polyacrylonitrile (PAN) and N,N-Dimethyl Formamide (DMF) were stirred to prepare a solution and then nanofibers were fabricated using an electrospinning method. Heat treatment in air was then performed using a hot plate for stabilization. In addition, heat treatment was performed at 800 °C for 2 h using rapid thermal annealing (RTA) to produce CNFs. A field emission scanning electron microscope (FE-SEM) was used to confirm surface and cross-sectional images of the CNFs/CNWs anode materials. Raman spectroscopy was used to examine structural characteristics and defects. Cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and constant current charge/discharge tests were performed to analyze the electrical characteristics. The synthesized CNFs/CNWs anode material had a CV value in which oxidation and reduction reactions were easily performed, and a low Rct value of 93 Ω was confirmed.