Atomic layer deposition (ALD) provides a promising route for depositing uniform thin-film electrodes for Li-ion batteries. In this work, bis(methylcyclopentadienyl) nickel(II) (Ni(MeCp) 2 ) and bis(cyclopentadienyl) nickel(II) (NiCp 2 ) were used as precursors for NiO ALD. Oxygen plasma was used as a counter-reactant. The films were studied by spectroscopic ellipsometry, scanning electron microscopy, atomic force microscopy, X-ray diffraction, X-ray reflectometry, and X-ray photoelectron spectroscopy. The results show that the optimal temperature for the deposition for NiCp 2 was 200-300 • C, but the optimal Ni(MeCp) 2 growth per ALD cycle was 0.011-0.012 nm for both precursors at 250-300 • C. The films deposited using NiCp 2 and oxygen plasma at 300 • C using optimal ALD condition consisted mainly of stoichiometric polycrystalline NiO with high density (6.6 g/cm 3 ) and low roughness (0.34 nm). However, the films contain carbon impurities. The NiO films (thickness 28-30 nm) deposited on stainless steel showed a specific capacity above 1300 mAh/g, which is significantly more than the theoretical capacity of bulk NiO (718 mAh/g) because it includes the capacity of the NiO film and the pseudo-capacity of the gel-like solid electrolyte interface film. The presence of pseudo-capacity and its increase during cycling is discussed based on a detailed analysis of cyclic voltammograms and charge-discharge curves (U(C)).NiO nanofilms are produced using various methods [12] such as thermal spraying, pulsed laser deposition, sol-gel, spin-coating, dip-coating, chemical vapor deposition, and atomic layer deposition (ALD). ALD is the most promising technology because it provides control over the thickness and purity of coatings with high precision, and can deposit uniform surface coatings on of complex shape and even porous and high aspect ratio substrates [13][14][15]. This method could be a crucial factor for transition from 2D to 3D solid-state batteries (SSB), which are structured on 3D substrates with high aspect ratio instead of planar substrates. It could increase the energy density of SSB with the same thickness of the electrode to maintain the required conductivity of the layers [16]. ALD is based on a realization of the sequence of chemical reactions between gaseous reagents and the surface species of the substrate, separated in time by purges with an inert gas to prevent uncontrolled reactions between the reactants and the reaction products. Because of the self-limiting nature, this method allows the deposition of films in a layer-by-layer fashion and the control of the thickness with high precision [13].When selecting the deposition conditions via ALD, it is necessary to consider the stability and reactivity of the precursors. Many precursors have been tested for ALD NiO so far, but the most frequently used are shown in Table 1: nickel(II) acetylacetonate (Ni(acac) 2 ), bis(2,2,6,6-tetramethylheptane-3,5dionate)nickel(II) (Ni(thd) 2 ), bis(cyclopentadienyl) nickel(II) (NiCp 2 ), and NiCp 2 -based compounds such as ...
Lithium nickelate (LiNiO2) and materials based on it are attractive positive electrode materials for lithium-ion batteries, owing to their large capacity. In this paper, the results of atomic layer deposition (ALD) of lithium–nickel–silicon oxide thin films using lithium hexamethyldisilazide (LiHMDS) and bis(cyclopentadienyl) nickel (II) (NiCp2) as precursors and remote oxygen plasma as a counter-reagent are reported. Two approaches were studied: ALD using supercycles and ALD of the multilayered structure of lithium oxide, lithium nickel oxide, and nickel oxides followed by annealing. The prepared films were studied by scanning electron microscopy, spectral ellipsometry, X-ray diffraction, X-ray reflectivity, X-ray photoelectron spectroscopy, time-of-flight secondary ion mass spectrometry, energy-dispersive X-ray spectroscopy, transmission electron microscopy, and selected-area electron diffraction. The pulse ratio of LiHMDS/Ni(Cp)2 precursors in one supercycle ranged from 1/1 to 1/10. Silicon was observed in the deposited films, and after annealing, crystalline Li2SiO3 and Li2Si2O5 were formed at 800 °C. Annealing of the multilayered sample caused the partial formation of LiNiO2. The obtained cathode materials possessed electrochemical activity comparable with the results for other thin-film cathodes.
The combination of titania nanofilms and silver nanoparticles (NPs) is a very promising material, with antibacterial and osseointegration-induced properties for titanium implant coatings. In this work, we successfully prepared TiO2 nanolayer/Ag NP structures on titanium disks using atomic layer deposition (ALD). The samples were studied by scanning electron microscopy (SEM), X-ray diffraction, X-ray photoelectron spectroscopy (XPS), contact angle measurements, and SEM-EDS. Antibacterial activity was tested against Staphylococcus aureus. The in vitro cytological response of MG-63 osteosarcoma and human fetal mesenchymal stem cells (FetMSCs) was examined using SEM study of their morphology, MTT test of viability and differentiation using alkaline phosphatase and osteopontin with and without medium-induced differentiation in the osteogenic direction. The samples with TiO2 nanolayers, Ag NPs, and a TiO2/Ag combination showed high antibacterial activity, differentiation in the osteogenic direction, and non-cytotoxicity. The medium for differentiation significantly improved osteogenic differentiation, but the ALD coatings also stimulated differentiation in the absence of the medium. The TiO2/Ag samples showed the best antibacterial ability and differentiation in the osteogenic direction, indicating the success of the combining of TiO2 and Ag to produce a multifunctional biocompatible and bactericidal material.
Nanostructured metal oxides (MOs) demonstrate good electrochemical properties and are regarded as promising anode materials for high-performance lithium-ion batteries (LIBs). The capacity of nickel-cobalt oxides-based materials is among the highest for binary transition metals oxide (TMOs). In the present paper, we report the investigation of Ni-Co-O (NCO) thin films obtained by atomic layer deposition (ALD) using nickel and cobalt metallocenes in a combination with oxygen plasma. The formation of NCO films with different ratios of Ni and Co was provided by ALD cycles leading to the formation of nickel oxide (a) and cobalt oxide (b) in one supercycle (linear combination of a and b cycles). The film thickness was set by the number of supercycles. The synthesized films had a uniform chemical composition over the depth with an admixture of metallic nickel and carbon up to 4 at.%. All samples were characterized by a single NixCo1-xO phase with a cubic face-centered lattice and a uniform density. The surface of the NCO films was uniform, with rare inclusions of nanoparticles 15–30 nm in diameter. The growth rates of all films on steel were higher than those on silicon substrates, and this difference increased with increasing cobalt concentration in the films. In this paper, we propose a method for processing cyclic voltammetry curves for revealing the influence of individual components (nickel oxide, cobalt oxide and solid electrolyte interface—SEI) on the electrochemical capacity. The initial capacity of NCO films was augmented with an increase of nickel oxide content.
Lithium-oxygen thin films were deposited by atomic layer deposition (ALD) on the surface of silicon and stainless-steel using lithium bis (trimethylsilyl) amide (LiHMDS) and different counter-reagents (water, ozone, oxygen plasma). The deposited films were non-stable at storage in the air atmosphere. Results of scanning electron microscopy showed that films show a tendency to crystallization and peeling from the substrate surface. X-ray photoelectron spectroscopy and time-of-flight secondary ion mass spectroscopy revealed that films mainly consist of LiOH/Li2CO3. Coating the surface of lithium-oxygen films with an aluminum oxide layer using the ALD trimethylaluminum (TMA) and water as precursors did not lead to a significant improvement in stability. Nevertheless, the stable films can be obtained using ALD supercycles consisting of sequential pulsing of LiHMDS-water-TMA-water at 250°C.
Titanium oxide nanocoatings were synthesized on the surface of monocrystalline silicon and ultra-fine-grained titanium by atomic layer deposition (ALD) using titanium tetrachloride (TiCl4) and titanium tetraisopropoxide (TTIP). The morphology of the samples was studied by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The structure and composition were studied by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), contact angle measurements, and energy-dispersive spectroscopy (EDS). The cytological response of osteosarcoma MG-63 and human fetal mesenchymal stem cells (FetMSCs) were studied by analyzing their morphology, viability, and alkaline phosphatase activity with and without the use of medium-induced differentiation in the osteogenic direction. A significant influence of the precursor type and ALD temperature on the crystal structure, morphology, composition, and surface free energy of TiO2 nanocoatings was found. The biocompatibility of amorphous non-stoichiometric and partially crystalline stoichiometric TiO2 coatings was compared. Both types of cells showed faster adhesion and improved spreading on the surface for the samples from TTIP compared to those from TiCl4 at the early stages of cultivation (2 h) due to the difference in composition and higher surface free energy. No cytotoxic effect was found on both types of coatings, nor was there a noticeable difference in cell differentiation. All ALD coatings provided excellent biocompatibility and osteoconductive properties.
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