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 ...
In this study, we present the detailed investigation of the influence of the etching medium (acidic or basic Piranha solutions) and the etching time on the morphology and surface relief of ultrafine grained (UFG) and coarse grained (CG) titanium. The surface relief and morphology have been studied by means of scanning electron microscopy (SEM), atomic force microscopy (AFM), and the spectral ellipsometry. The composition of the samples has been determined by X-ray fluorescence analysis (XRF) and X-ray Photoelectron Spectroscopy (XPS). Significant difference in the etching behavior of UFG and CG titanium has been found. UFG titanium exhibits higher etching activity independently of the etching medium. Formed structures possess higher homogeneity. The variation of the etching medium and time leads to micro-, nano-, or hierarchical micro/nanostructures on the surface. Significant difference has been found between surface composition for UFG titanium etched in basic and acidic Piranha solution. Based on the experimental data, the possible reasons and mechanisms are considered for the formation of nano- and microstructures. The prospects of etched UFG titanium as the material for implants are discussed.
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.
In this work, we study the influence of the surface properties of ultrafine grained (UFG) and coarse grained (CG) titanium on the morphology, viability, proliferation and differentiation of osteoblast-like MG-63 cells. Wet chemical etching in H2SO4/H2O2 and NH4OH/H2O2 solutions was used for producing surfaces with varying morphology, topography, composition and wettability. The topography and morphology have been studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The composition was determined by time of flight mass-spectrometry (TOF-SIMS) and X-ray photoelectron spectroscopy (XPS). The results showed that it is possible to obtain samples with different compositions, hydrophilicity, topography and nanoscale or/and microscale structures by changing the etching time and the type of etching solution. It was found that developed topography and morphology can improve spreading and proliferation rate of MG-63 cells. A significant advantage of the samples of the UFG series in comparison with CG in adhesion, proliferation at later stages of cultivation (7 days), higher alkaline phosphatase (ALP) activity and faster achievement of its maximum values was found. However, there is no clear benefit of the UFG series on osteopontin (OPN) expression. All studied samples showed no cytotoxicity towards MG-63 cells and promoted their osteogenic differentiation.
Three-dimensional printed nitinol (NiTi) alloys have broad prospects for application in medicine due to their unique mechanical properties (shape memory effect and superplasticity) and the possibilities of additive technologies. However, in addition to mechanical properties, specific physicochemical characteristics of the surface are necessary for successful medical applications. In this work, a comparative study of additively manufactured (AM) NiTi samples etched in H2SO4/H2O2, HCl/H2SO4, and NH4OH/H2O2 mixtures was performed. The morphology, topography, wettability, free surface energy, and chemical composition of the surface were studied in detail. It was found that etching in H2SO4/H2O2 practically does not change the surface morphology, while HCl/H2SO4 treatment leads to the formation of a developed morphology and topography. In addition, exposure of nitinol to H2SO4/H2O2 and HCl/H2SO4 contaminated its surface with sulfur and made the surface wettability unstable in air. Etching in NH4OH/H2O2 results in surface cracking and formation of flat plates (10–20 microns) due to the dissolution of titanium, but clearly increases the hydrophilicity of the surface (values of water contact angles are 32–58°). The etch duration (30 min or 120 min) significantly affects the morphology, topography, wettability and free surface energy for the HCl/H2SO4 and NH4OH/H2O2 etched samples, but has almost no effect on surface composition.
Original 1CP powder was studied and it was founded that powder material partially consists of the amorphous phase, in which crystallization begins at 450 °C and ends at 575 °C. Selective laser melting parameters were investigated through the track study, and more suitable ones were found: laser power P = 90, 120 W; scanning speed V = 1200 mm/s. Crack-free columnar elements were obtained. The sample obtained with P = 90 W, contains a small amount of amorphous phase. X-ray diffraction of samples shows the presence of α-Fe(Si) and Fe2B. SEM-image analysis shows the presence of ordered Fe3Si in both samples. Annealed samples show 40% less microhardness; an annealed sample containing amorphous phase shows higher soft-magnetic properties: 2.5% higher saturation magnetization, 35% higher residual magnetization and 30% higher rectangularity coefficient.
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