Doktorarbeit / Dissertation, 2022
182 Seiten
The research focused on investigating the use of heterocyclic dithiocarbamate complexes of Ni and Co as single source molecular precursors (SSP) for the fabrication of the corresponding metal sulfide nanoparticles and thin films for application in magnetism and energy.
Chapter 1 introduces the reader to the concepts of nanomaterials and their technological importance. It includes a comprehensive review of the relevant literature related to transition metal sulfides (TMS), particularly nickel sulfide (NixSy) and cobalt sulfide (CoxSy) systems. The chapter also highlights the significance of single-source precursor (SSP) methods for fabricating these nanomaterials and explores the challenges and opportunities related to the energy crisis. The chapter concludes by outlining the research problem, scope, aims, and objectives of the study.
Chapter 2 focuses on the synthesis and characterization of nickel sulfide (NixSy) nanoparticles. The chapter details the synthesis of three heterocyclic dithiocarbamate complexes of nickel, namely bis(piperidinyldithiocarbamato)nickel(II) (1), bis(tetrahydroquinolinyldithiocarbamato)nickel(II) (2), and bis(N'-ethyl-N�piperazinylcarbodithioato-S,S')-Nickel(II) (3), which served as single-source precursors for the fabrication of the corresponding NixSy nanoparticles. The chapter then investigates the effect of various reaction parameters such as temperature, type of capping agent, and the nature of the complex on the morphology, phase purity, and particle size of the NixSy nanoparticles. The chapter further explores the magnetic properties of the synthesized NixSy nanoparticles.
Chapter 3 explores the use of the three heterocyclic dithiocarbamato-nickel(II) complexes (1-3) for the deposition of nickel sulfide thin films via the aerosol-assisted chemical vapour deposition (AACVD) technique. The chapter details the fabrication of NiS thin films with different morphologies by varying the deposition temperature. The chapter also presents a comprehensive analysis of the thin films, using various characterization techniques, including SEM, EDX, powder X-ray diffraction, and UV-Vis spectroscopy. The chapter provides insights into the mechanism of morphological evolution of the NiS thin films.
Chapter 4 reports the synthesis, characterization, and evaluation of a novel cobalt(III) complex, [tris(morpholinodithiocarbamato)cobalt(III)] (4), as a single-source precursor for the preparation of cobalt sulfide nanoplates. The chapter examines the effect of temperature on the morphology and phase purity of the synthesized CoxSy nanoparticles. The chapter further explores the electrochemical and electrocatalytic activities of the prepared cobalt sulfide nanoplates for hydrogen evolution and oxygen evolution reactions and their performance in supercapacitance applications. The chapter highlights the superior performance of the cobalt sulfide nanoplates as bifunctional materials for energy applications.
Chapter 5 examines the effect of cationic disorder in Ni x Co 3−x S 4 thiospinel nanoparticles on their energy generation and storage applications. The chapter focuses on the synthesis of Co or Ni-rich NixCo3-xS4 nanosheets using the corresponding metal complexes of ethyl piperazino-dithiocarbamate as molecular precursors. The study investigates the electrocatalytic performance of the Ni-rich and Co-rich nanosheets in oxygen evolution reaction (OER) and hydrogen evolution reaction (HER). The chapter further explores the supercapacitance performance of the NixCo3-xS4 nanosheets and highlights the superior energy generating and storage efficiency of the Ni-rich NixCo3-xS4 sample.
This work explores the synthesis, characterization, and application of Ni and Co sulfide nanomaterials, primarily for magnetic and energy-related applications. This includes investigating the use of heterocyclic dithiocarbamate complexes as single-source precursors for the fabrication of these nanomaterials. The key themes include the control of phase purity and morphology, the influence of reaction parameters, and the evaluation of the nanomaterials for energy generation through hydrogen and oxygen evolution reactions, as well as energy storage in supercapacitor applications. Important keywords include: single source precursors, dithiocarbamates, nickel sulfide, cobalt sulfide, thiospinel, energy generation, energy storage, supercapacitor, electrocatalysis, hydrogen evolution reaction, oxygen evolution reaction, magnetic properties, and cationic disorder.
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