Experiments were performed for the study of the influence of impurities on the microstructure and hardness of nanocrystalline Ni films. The samples were prepared by electrodeposition using two basic electrolyte solutions (a sulfate-type bath and a Watts-type bath). The effect of saccharin as organic additive on the microstructure, texture and hardness was studied. It was found that the Watts bath without saccharin yielded a larger grain size compared to its sulfatetype counterpart. For both electrolyte solutions, (220) out-of-plane texture was formed in the saccharin-free films. The additive saccharin eliminated the texture and yielded very fine microstructures with high dislocation densities and twin fault probabilities for both solution types. The influence of saccharin on the defect density was higher for the film prepared from the sulfate-type bath. It was revealed that there is a correlation between the defect density and the grain size. When saccharin was added to the Watts bath, the combined effect of nickelchloride and saccharin led to a bimodal grain size distribution. An additional sample was deposited from an electrolyte containing trisodium citrate to investigate the sodium incorporation in the Ni layers. The correlation between the microstructure and the hardness of the films was discussed in detail.

The purpose of the present study was to provide a reliable value for the specific grain-boundary resistivity ρ SGBR of Ni metal. New results are presented on the room-temperature electrical resistivity of nanocrystalline (nc) Ni metal samples produced by electrodeposition with various grain sizes. These resistivity data were compared with previous reports on nc-Ni and all results were analysed according to the procedure of Andrews [Phys. Lett. 19, 558 (1965)] who found that the resistivity increment due to grain boundaries is proportional to the grain-boundary surface area per unit volume which is, on the other hand, inversely proportional to the grain size. It is pointed out that the grain size directly accessible by transmission electron microscopy imaging is the relevant parameter for the evaluation of ρ SGBR whereas the crystallite size deduced from X-ray diffraction line broadening leads to an underestimation of ρ SGBR because coherency-breaking intragrain defects not contributing significantly to the resistivity also cause a line broadening. From the evaluation of the nc-Ni resistivity data at room temperature, we find that 4.45•10 −16 Ω•m 2 < ρ SGBR (Ni) < 6.2•10 −16 Ω•m 2 and our upper bound agrees exactly with the most recent calculated value in the literature.

The microstructure of electrodeposited Ni films produced without and with organic additives (formic acid and saccharin) was investigated by X-ray diffraction (XRD) line profile analysis and cross-sectional transmission electron microscopy (TEM). Whereas the general effect of these additives on the microstructure (elimination of columnar growth as well as grain refinement) was reproduced, the pronounced intention of this study was to compare the results of various seldom-used high-performance structural characterization methods on identical electrodeposited specimens in order to reveal fine details of structural changes qualitatively not very common in this field. In the film deposited without additives, a columnar structure was observed showing similarities to the T-zone of structure zone models. Both formic acid and saccharin additives resulted in equiaxed grains with reduced size, as well as increased dislocation and twin fault densities in the nanocrystalline films. Moreover, the structure became homogeneous and free of texture within the total film thickness due to the additives. Saccharin yielded smaller grain size and larger defect density than formic acid. A detailed analysis of the grain size and twin boundary spacing distributions was carried out with the complementary application of TEM and XRD, by carefully distinguishing between the TEM and XRD grain sizes.

The room-temperature magnetoresistance (MR) characteristics of nanocrystalline (nc) Ni metal with various grain sizes (between 30 and 100 nm) are investigated in this work for the first time. The nc-Ni foils were produced by electrodeposition and the results are compared with data measured on coarse-grained (bulk) pure Ni metal samples prepared by cold-rolling and annealing. The MR(H) curves measured in magnetic fields up to H 9 kOe are analyzed in detail to determine the anisotropic magnetoresistance (AMR) ratio. The magnitude of the AMR ratio was found to be around 2.5% for bulk Ni and in the range from about 2 to 2.5% for the nc-Ni samples, the latter data not exhibiting a systematic dependence on the grain size. On the other hand, the field-induced resistivity anisotropy splitting ρ AMR in the magnetically saturated state of the nc-Ni series was found to be proportional to the zero-field resistivity of the same samples with different grain sizes. The slope of this proportionality relation provided an AMR ratio of 2.4% for all nc-Ni samples, matching well the value for the bulk Ni samples. Thus, the AMR ratio for polycrystalline Ni metal seems to be fairly independent of the microstructural features. This also means that the AMR ratio is an inherent characteristic of the Ni metal matrix and it remains the same even if the matrix resistivity changes (e.g., by introducing grain boundaries) without noticeably modifying the electronic density of states at least in the vicinity of the Fermi level.

The effect of bath additives on the thermal stability of the microstructure and hardness of nanocrystalline Ni foils processed by electrodeposition was studied. Three samples with a thickness of 20 μ m were prepared: one without any additive and two others with saccharin or trisodium citrate additives. Then, the specimens were heat-treated at different temperatures up to 1000 K. It was found that for the additive-free sample the recovery of the microstructure and the reduction of the hardness started only at temperatures higher than 500 K. At the same time, a decrease of the defect density and hardness was observed even at 400 K for the additive-containing films. This was explained by the higher defect density, which increased the thermodynamic driving force for recovery during annealing. At the highest applied temperature (1000 K), this larger thermodynamic driving force resulted in a recrystallization in the sulfur-containing sample, leading to a very low hardness of about 1000 MPa as compared to the additive-free sample (1300 MPa). On the other hand, the sample deposited with trisodium citrate additive showed a better thermal stability at 1000 K than the additive-free sample: the hardness remained as high as 2000 MPa even at 1000 K.

Carbon quantum dots (CQDs) are a novel family of fluorescent materials that could be employed as non-toxic alternatives to molecular fluorescent dyes in biological research and also in medicine. Four different preparation approaches, including microwave assisted heating and solvent refluxing, were explored. In addition to the widely used microwave assisted methods, a simple convenient new procedure is presented here for the particle synthesis. A detailed X-ray photoelectron spectroscopic (XPS) analysis was employed to characterize the composition, and more importantly, the chemical structure of the CQD samples and the interrelation of the characteristic surface chemical groups with the fluorescence properties and with surface polarity was unambiguously established. In vitro cellular internalization experiments documented their applicability as fluorescence labels while non-toxic properties were also approved. It was demonstrated that the adequate water-dispersibility of the particles plays a crucial role in their biological application. The synthetized CQD samples turned to be promising for cellular imaging applications both in laser illuminated flow cytometric measurements and in fluorescence microscopy.

The tensile and compressive behaviors of 316L stainless steel at room temperature were compared. The differences between the stress–strain responses during tension and compression were explained by the different evolutions of the texture, defect structure, and phase composition. It was found that up to true strain of ~ 25 pct the flow stress during tension was only slightly higher (by ~ 40 MPa) than that during compression, which can be explained by the different textures of the two types of specimens. On the other hand, between the strains of 25 and 50 pct, the strain hardening for tension was much higher, which resulted in a ~ 200 MPa larger flow stress in the tensile-tested specimen at 50 pct strain. It was revealed that the higher flow stress in tension was caused by the harder texture, the higher dislocation density, and the larger fraction of martensite phase.

In a single process run, an amorphous silicon oxynitride layer was grown, which includes the entire transition from oxide to nitride. The variation of the optical properties and the thickness of the layer was characterized by Spectroscopic Ellipsometry (SE) measurements, while the elemental composition was investigated by Energy Dispersive Spectroscopy (EDS). It was revealed that the refractive index of the layer at 632.8 nm is tunable in the 1.48–1.89 range by varying the oxygen partial pressure in the chamber. From the data of the composition of the layer, the typical physical parameters of the process were determined by applying the Berg model valid for reactive sputtering. In our modelling, a new approach was introduced, where the metallic Si target sputtered with a uniform nitrogen and variable oxygen gas flow was considered as an oxygen gas-sputtered SiN target. The layer growth method used in the present work and the revealed correlations between sputtering parameters, layer composition and refractive index, enable both the achievement of the desired optical properties of silicon oxynitride layers and the production of thin films with gradient refractive index for technology applications.