Temperature-Driven Optimization of LiCoO2 Thin-Film Cathodes via Pulsed Laser Deposition: Structural and Morphological Control
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Keywords:
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Cathode, LiCoO2 Thin Film, PLD, Substrate Temperature, Morphology
Abstract
Thin LiCoO2 film cathodes were fabricated on silicon substrate by Pulsed Laser Deposition (PLD). The microstructural properties were investigated as a function of the substrate temperature (Ts), which varied between 750◦C, 850 ◦C and 900 ◦C. The deposition was performed using Nd:YAG laser (266 nm, 100 mJ) under an oxygen partial pressure of 200 mTorr. X-ray Diffraction (XRD) analysis revealed that films consist of HT-LiCoO2 and a small amount of Co3O4 precipitates. The highest crystallinity was obtained for the thin film deposited at Ts = 900 ◦C, whereas the Atomic Force Microscopy (AFM) indicated uniform grain size distributions of the film deposited at Ts = 850 ◦C with an approximate surface roughness of 18 nm. The increase of surface roughness at higher Ts was attributed to non-uniform grain distribution, highlighting the importance of substrate temperature control in minimizing interfacial defects for improved electrochemical performance. This study provides key insights into the interplay between PLD parameters and film microstructure, offering a pathway for optimizing LiCoO2 cathodes for thin-film batteries and advanced solid-state energy storage devices.
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Bates, J. B., N. J. Dudney, B. J. Neudecker, F. X. Hart, H. P. Jun, and S. A. Hackney (2000). Preferred Orientation of Polycrystalline LiCoO2 Films. Journal of The Electrochemical Society, 147(1); 59
Chaudhary, D. and P. C. Sharma (2022). An Overview of Internet of Things Related Protocols, Technologies, Challenges and Application. In Ambient Intelligence and Internet of Things. John Wiley & Sons, Ltd, pages 33–52
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Delluva, A. A., J. Dudoff, G. Teeter, and A. Holewinski (2020). Cathode Interface Compatibility of Amorphous LiMn2O4 (LMO) and Li7La3Zr2O12 (LLZO) Characterized With Thin-Film Solid-State Electrochemical Cells. ACS Applied Materials & Interfaces, 12(22); 24992–24999
Donders, M.E., W.M.Arnoldbik, H.C.M.Knoops, W.M.M. Kessels, and P. H. L. Notten (2013). Atomic Layer Deposition of LiCoO2 Thin-Film Electrodes for All-Solid-State Li-Ion Microbatteries. Journal of The Electrochemical Society, 160(5); A3066
Dupre, N., M. Cuisinier, Y. Zheng, V. Fernandez, J. Hamon, M. Hirayama, and D. Guyomard (2018). Evolution of LiFePO4 Thin Films Interphase With Electrolyte. Journal of Power Sources, 382; 45–55
Fenech, M. and N. Sharma (2020). Pulsed Laser Deposition Based Thin Film Microbatteries. Chemistry– An Asian Journal, 15(12); 1829–1847
Ganesh, K. S., B. P. Reddy, P. J. Kumar, and O. Hussain (2018). Influence of Zr Dopant on Microstructural and Electrochemical Properties of LiCoO2 Thin Film Cathodes by RF Sputtering. Journal of Electroanalytical Chemistry, 828; 71–79
Goodenough, J. B. and Y. Kim (2010). Challenges for Rechargeable Li Batteries. Chemistry of Materials, 22(3); 587–603
Hirayama, M., K. Suzuki, R. Kanno, T. Masuda, and K. Tamura (2021). Characterization of Cathode/Sulfide Electrolyte Interface Using a Thin-Film Model Battery. In K. Kanamura, editor, Next Generation Batteries: Realization of High Energy Density Rechargeable Batteries. Springer Singapore, Singapore, pages 167–178
Hsueh, T.-H., C.-H. Tsai, S.-E. Liu, M.-C. Wang, S.-M. Chang, A. Shiue, and K.-Y. Chin (2022). LiCoO2 Battery Electrode Fabricated by High Deposition-Rate Atmospheric Plasma Spraying for Lithium Battery. Journal of The Electrochemical Society, 169(10); 100506
Jaguemont, J. and F. Bardé (2023). A Critical Review of Lithium-Ion Battery Safety Testing and Standards. Applied Thermal Engineering, 231; 121014
Jung, K.-T., G.-B. Cho, K.-W. Kim, T.-H. Nam, H.-M. Jeong, S.-C. Huh, and J.-P. Noh (2013). Influence of the Substrate Texture on the Structural and Electrochemical Properties of Sputtered LiCoO2 Thin Films. Thin Solid Films, 546; 414–417. The Proceedings of International Union of The Materials Research Society- International Conference in Asia 2012 (IUMRS-ICA 2012)
Kadhem, S. J. (2023). Preparation of Al2O3/PVA Nanocomposite Thin Films by a Plasma Jet Method. Science and Technology Indonesia, 8(3); 471–478
Kawashima, K., T. Ohnishi, and K. Takada (2020). High Rate Capability of LiCoO2 Cathodes. ACS Applied Energy Materials, 3(12); 11803–11810
Kurbatov, S. V., A. S. Rudy, V. V. Naumov, A. A. Mironenko, O. V. Savenko, M. A. Smirnova, and D. E. Pukhov (2024). A Comprehensive Study of Nonuniformity Properties of The LiCoO2 Thin-Film Cathode Fabricated by RF Sputtering. Russian Microelectronics, 53(3); 202–216
Kwon, T., T. Ohnishi, K. Mitsuishi, T. C. Ozawa, and K. Takada (2015). Synthesis of LiCoO2 Epitaxial Thin Films Using a Sol–Gel Method. Journal of Power Sources, 274; 417–423
Lin, C. and S. Lin (2022). Issues, Developments, and Computation Analyses of Interfacial Stability in All-Solid-State Li Batteries. JOM, 74(12); 4654–4663
Lu, W., J. Zhang, J. Xu, X. Wu, and L. Chen (2017). In Situ Visualized Cathode Electrolyte Interphase on LiCoO2 in High Voltage Cycling. ACS Applied Materials & Interfaces, 9(22); 19313–19318
Lyu, Y., X. Wu, K. Wang, Z. Feng, T. Cheng, Y. Liu, and B. Guo (2021). An Overview on The Advances of LiCoO2 Cathodes for Lithium-Ion Batteries. Advanced Energy Materials, 11(2); 2000982
Maruno, M., F. Nakayama, Y. Suzuki, M. Sakakura, T. Ohnishi, Y. Nomura, and Y. Iriyama (2025). Chemical Design Rules for Low-Resistivity Electrode–Electrolyte Interfaces in All-Solid-State Lithium Batteries. Communications Materials, 6(1); 144
Maruyama, S., O. Kubokawa, K. Nanbu, K. Fujimoto, and Y. Matsumoto (2016). Combinatorial Synthesis of Epitaxial LiCoO2 Thin Films on SrTiO3(001) Via On-Substrate Sintering of Li2CO3 and CoO by Pulsed Laser Deposition. ACS Combinatorial Science, 18(6); 343–348
Matsuda, Y., N. Kuwata, and J. Kawamura (2018). Thin-Film Lithium Batteries With 0.3–30 um Thick LiCoO2 Films Fabricated by High-Rate Pulsed Laser Deposition. Solid State Ionics, 320; 38–44
Matsuda, Y., N. Kuwata, T. Okawa, A. Dorai, O. Kamishima, and J. Kawamura (2019). In Situ Raman Spectroscopy of LixCoO2 Cathode in Li/Li3PO4/LiCoO2 All-Solid-State Thin-Film Lithium Battery. Solid State Ionics, 335; 7–14
Moazzen, E., J. Mujtaba, B. Buchholz, D. Isheim, N. S. Luu, D. Rowell, and S. A. Barnett (2024). Atom Probe Tomography of the LiFePO4-Electrolyte Interface Enabled by Thin Film Electrodes. Journal of The Electrochemical Society, 171(7); 070527
Morozov, A. V., H. Paik, A. O. Boev, D. A. Aksyonov, S. A. Lipovskikh, K. J. Stevenson, and A. M. Abakumov (2022). Thermodynamics As a Driving Factor of LiCoO2 Grain Growth on Nanocrystalline Ta-LLZO Thin Films for All Solid-State Batteries. ACS Applied Materials & Interfaces, 14(35); 39907–39916
Nishio, K., T. Ohnishi, M. Osada, N. Ohta, K. Watanabe, and K. Takada (2016). Influences of High Deposition Rate on LiCoO2 Epitaxial Films Prepared by Pulsed Laser Deposition. Solid State Ionics, 285; 91–95. The 40th Symposium on Solid State Ionics in Japan
Ohnishi, T. (2024). Fabrication of Thin-Film Batteries Composed of LiCoO2, Li3PO4, and Li Layers. Journal of Solid State Electrochemistry, 28(12); 4355–4366
Ohnishi, T., K. Mitsuishi, and K. Takada (2021). In Situ X-Ray Diffraction of LiCoO2 in Thin-Film Batteries Under High-Voltage Charging. ACS Applied Energy Materials, 4(12); 14372–14379
Ohnishi, T., K. Nishio, and K. Takada (2015). Composition Controlled LiCoO2 Epitaxial Thin Film Growth by Pulsed Laser Deposition. In F. H. Teherani, D. C. Look, and D. J. Rogers, editors, Oxide-Based Materials and Devices VI, volume 9364. SPIE, page 93640L
Ohnishi, T. and K. Takada (2024). Thin Film Battery With Epitaxial LiCoO2 Cathode. In Y. Iriyama, K. Amezawa, Y. Tateyama, and N. Yabuuchi, editors, Interface Ionics: For All-Solid-State Batteries and Solid State Ionics Devices. Springer Nature Singapore, Singapore, pages 21–31
Otoyama, M., Y. Ito, A. Hayashi, and M. Tatsumisago (2016). Raman Imaging for LiCoO2 Composite Positive Electrodes in All-Solid-State Lithium Batteries Using Li2S–P2S5 Solid Electrolytes. Journal of Power Sources, 302; 419–425
Ozcan, P., N. Esen, A. Cantas, L. Ozyuzer, M. Ozdemir, K. Kosiel, and G. Aygun (2025). Investigation of LiCoO2 Thin Films Grown Under Relatively Low Substrate Temperature for All Solid State Lithium Ion Battery Applications. Vacuum, 239; 114439
Pegoretti, V., P. Dixini, P. Smecellato, S. Biaggio, and M. Freitas (2017). Thermal Synthesis, Characterization and Electrochemical Study of High-Temperature (HT) LiCoO2 Obtained from Co(OH)2 Recycled of Spent Lithium Ion Batteries. Materials Research Bulletin, 86; 5–9
Perkins, J. D., C. S. Bahn, J. M. McGraw, P. A. Parilla, and D. S. Ginley (2001). Pulsed Laser Deposition and Characterization of Crystalline Lithium Cobalt Dioxide (LiCoO2) Thin Films. Journal of The Electrochemical Society, 148(12); A1302
Porthault, H., F. LeCras, J.-M. Duffault, and S. Franger (2016). Fast Deposition of Conformal LiCoO2 Thin Film Electrodes for High Capacity 3D Batteries. Materials Science and Engineering: B, 213; 163–168
Porthault, H., F. Le Cras, and S. Franger (2010). Synthesis of LiCoO2 Thin Films by Sol/Gel Process. Journal of Power Sources, 195(19); 6262–6267
Qiu, J., H. Li, T. Wu, Y. He, R. Xu, Y. Hua, and Y. Cui (2025). Construction of Longitudinal (003) Textured Low-Strain Diffusion Channel in 4.6 V LiCoO2-Based All-Solid-State Thin Film Battery for Microelectronic Systems. ACS Energy Letters, 20(7); 3249–3258
Rao, M. (2010). Growth and Microstructural Features of Laser Ablated LiCoO2 Thin Films. Journal of Crystal Growth, 312(19); 2799–2803
Schneider, C. A., W. S. Rasband, and K. W. Eliceiri (2012). NIH Image to ImageJ: 25 Years of Image Analysis. Nature Methods, 9(7); 671–675
Takeuchi, S., H. Tan, K. K. Bharathi, G. R. Stafford, J. Shin, S. Yasui, and L. A. Bendersky (2015). Epitaxial LiCoO2 Films as a Model System for Fundamental Electrochemical Studies of Positive Electrodes. ACS Applied Materials & Interfaces, 7(15); 7901–7911
Tang, S., M. Lai, and L. Lu (2006). Effects of Oxygen Pressure on LiCoO2 Thin Film Cathodes and Their Electrochemical Properties Grown by Pulsed Laser Deposition. Journal of Alloys and Compounds, 424(1); 342–346
Tintignac, S., R. Baddour-Hadjean, J. Pereira-Ramos, and R. Salot (2014). High Rate Bias Sputtered LiCoO2 Thin Films as Positive Electrode for All-Solid-State Lithium Microbatteries. Electrochimica Acta, 146; 472–476
Usai, L., J. J. Lamb, E. Hertwich, O. S. Burheim, and A. H. Strømman (2022). Analysis of the Li-Ion Battery Industry in Light of the Global Transition to Electric Passenger Light Duty Vehicles Until 2050. Environmental Research: Infrastructure and Sustainability, 2(1); 011002
Whittingham, M. S. (2004). Lithium Batteries and Cathode Materials. Chemical Reviews, 104(10); 4271–4302
Wu, T., Y. Zhao, X. Zhang, S. Ma, K. Wei, Y. Wei, and Y. Cui (2022). Improved Solid Interfacial Kinetics and Electrochemical Performance for LiCoO2 (110) Textured Thin Film Lithium Batteries. Applied Surface Science, 591; 153174
Xia, H. and L. Lu (2007). Texture Effect on the Electrochemical Properties of LiCoO2 Thin Films Prepared by PLD. Electrochimica Acta, 52(24); 7014–7021
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Authors
Ayu, N. I. P., Rivai, A. K., & Evvy, K. (2025). Temperature-Driven Optimization of LiCoO2 Thin-Film Cathodes via Pulsed Laser Deposition: Structural and Morphological Control. Science and Technology Indonesia, 10(4), 1215–1224. https://doi.org/10.26554/sti.2025.10.4.1215-1224
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