Structural,microchemical and superconducting properties of ultrathin NbN films on silicon

Structural, chemical and superconducting properties of thin NbN films used for development of fast and sensitive hot‐electron bolometer (HEB) detectors for wide spectra range are reported. The thin NbN films with a thickness between 4 and 10 nm were deposited on the (001)Si substrates by magnetron sputtering. In order to investigate the film morphology and microchemistry, diffraction‐contrast and high‐resolution transmission electron microscopy (TEM) in combination with scanning TEM and electron energy loss spectroscopy (EELS) were performed. In addition, the zero‐resistance critical temperature of the NbN films was measured and correlated to their thickness. The interrelations between fabrication conditions, crystalline and superconducting properties of the differently thick NbN films are discussed. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Superconducting properties of an NbN–SiO2 disordered system obtained by ammonolysis of NbN–SiO2 sol–gel derived coatings

Studies in superconducting properties of NbN–SiO₂ films are reported. The films were obtained through nitridation of sol–gel derived Nb₂O₅–SiO₂ coatings at 1200 °C, a process leading to the formation of disordered structures with NbN metallic grains dispersed in the insulating SiO₂ matrix. Electrical resistivity was measured with the conventional four-terminal method in the temperature range from 5 to 280 K. The samples’ superconducting properties, examined with magnetically modulated microwave absorption (MMMA), depend on the NbN/SiO₂ molar ratio and the film’s thickness.     

Structure and electrical properties of nitrided NbN–TiN sol–gel derived films

The results of investigations of electrical conductivity and the structure of NbN–TiN thin films in a different NbN/TiN molar ratio are presented in this work. Sol–gel derived xNb₂O₅?(100?x)TiO₂ coatings (where x = 100, 90, 80, 70, 60, 50, 40, 0 mol%) were nitrided at 1200 °C to obtain NbN–TiN films. The structural transformations occurring in the films as a result of ammonolysis were studied using X-ray diffraction (XRD), atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The electrical conductivity was measured with a conventional four-terminal method in the temperature range of 5–280 K. The NbN–TiN samples exhibited a negative temperature coefficient of resistivity. The positive temperature coefficient of resistivity was observed only for the x = 0 sample. The results of conductivity versus temperature may be described on the grounds of a model proposed for a weakly disordered system. The film thickness effect on the superconducting properties was studied for x = 80 and x = 100 samples. The superconducting transition was not observed in all samples, the exception was x = 80 sample, 1050 nm in thickness. It is not clear, why all x = 100 samples do not exhibit superconducting transition in resistivity measurements. It seems to be possible, that the Josephson junction formation between NbN grains could be blocked by non-superconducting phases present in these samples.     

Electron Energy-Loss Spectroscopy Study of the Change in the Free-Electron Density in Thin Superconducting NbN Films under Ion-Beam Irradiation

The change in the free-electron density in ultrathin (5 nm) superconducting NbN films in the initial state and after irradiation by O⁺ ions to doses of (0.1–0.9) × 10¹⁷ cm^–2 has been studied by electron energy-loss spectroscopy (EELS). The analysis has been performed on cross section samples prepared by the focused ion beam method, using plasmon oscillations with energies up to 50 eV. The radiation-induced replacement of nitrogen atoms with oxygen atoms in niobium nitride is found to change the electrical properties of the material, which leads to a decrease in the free-electron density with an increase in the irradiation dose.     

Ferroelectric PbTiO3 Powders and Thin Films Derived from Sol-Gel Processing

Lead titanate powders and thin films were prepared by the sol-gel process of metal alkoxide solutions and solvents. From DSC measurements, phase transition temperature of crystallized PbTiO₃ powders was obtained at about 484 °C. From XRD investigation, it was confirmed that the tetragonal phase of polycrystalline PbTiO₃ thin films is formed by coating of concentrated solution on all of the substrates we used after heat treatment above 500 °C. It was found by SEM and ellipsometric analysis that the thin film coated with 0.25 M concentrated solutions once had an average thickness of about 720 Å. Surfaces of thin films were crack-free, uniform, and its average grain size investigated by SEM was 0.6–0.8 μm. Band gap energy of PbTiO₃ thin film coated on the Al₂O₃ (2243) substrate was 3.45 eV, which is assumed to be due to the direct band to band transition. Dielectric constant (ϵ) and dielectric loss (tan δ) of PbTiO₃ thin film amounted to 60–70 and 0.01–0.02 in the region of 10 kHz ∼ 1 MHz at room temperature, respectively, and transition temperature was 486 °C at 1 MHz. From the hysteresis loop of PbTiO₃ thin film, spontaneous polarization of 12 μC/cm² and coercive filed of 45 kV/cm were obtained.     

Study of transport properties co – evaporated lead telluride (PbTe) thin films

Thin films of lead telluride (PbTe) of thicknesses ranging from 1000 Å to 2500 Å have been prepared by co‐evaporation (three temperature) technique, onto precleaned amorphous glass substrates at various temperatures. The deposited samples were annealed and annealed samples were used for characterization. Resistivity of these samples was measured by four‐probe technique as a function of thickness and temperature. Activation energy for charge transport have been evaluated and found in the range of 0.09 to 0.106 eV. Thermoelectric power has been measured and found to be positive indicating that the samples are p‐type semiconducting material. Mobility variation with temperature has been estimated (evaluated) and correlated with scattering mechanism in the entire range of temperature studied. The X‐ray diffraction analysis confirmed that films are polycrystalline having cubic structure cell and lattice parameters are reported.     

Effect of substrate temperature on the properties of reactively sputtered TiN/NbN multilayers

TiN/NbN multilayer coatings were deposited with various substrate temperatures by DC reactive magnetron sputtering method onto Si (111) and glass substrates. The effect of substrate temperature on the structural and optical properties of TiN/NbN multilayers was investigated by X‐ray diffraction, X‐ray photoelectron spectroscopy, Field emission scanning electron microscopy and Photoluminescence measurements. The composition was analyzed by X‐ray photoelectron spectroscopy. X‐ray diffraction results showed that the layers crystallized in cubic structure for TiN and hexagonal structure for NbN. It was found that grain size increased with increase in substrate temperature. The surface morphology of the TiN/NbN thin films showed a dense and smooth surface with substrate temperature upto 200 °C but after 300 °C, the grains became larger and coarse surface was observed. The TiN/NbN multilayer coatings exhibited the characteristic peaks centered at 180, 210 and 560 cm^‐1. Red band emission peaks were observed in the wavelength range of 700‐710 nm. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of boron nitride films on w‐AlN (0001), 4° off‐cut 4H‐SiC (0001), W (110) and Cr (110) substrates by Chemical Vapor Deposition

Boron Nitride is a promising group 13–group 15 compound material that exhibits various interesting properties like wide band gap, chemical stability, attractive mechanical properties and other. The growth behavior of this material has not been investigated in sufficient details to tailor properties of the resulting films. In this work we present the results on the growth of turbostratic boron nitride (t‐BN) thin films at a relatively high growth rate of 3 μm/h with the aim to investigate the potential use of boron trichloride in combination with ammonia as precursors for growth. Deposition experiments were conducted in a vertical cold wall high temperature chemical vapor deposition reactor in the temperature range 1000°C–1700°C depending on the substrate used. Templates of w‐AlN (0001), 4° off‐cut 4H‐SiC (0001), Cr (110) and W (110) were employed as substrates for the BN growth. As‐grown BN layers were characterized by Scanning Electron Microscopy, X‐Ray Diffraction, Electron Diffraction and Raman Spectroscopy. The results indicate that temperature and N/B ratio have a great influence on the crystallinity of the deposited films. For AlN and SiC substrates, a temperature of 1600°C and N/B ratio in range between 3 and 7.5 were identified as the best parameters for the growth of a 2 μm thick t‐BN layer with a spacing between basal planes of about 3.36 Å compare to the 3.33 Å spacing between basal planes of hexagonal or rhombohedral BN (h‐BN or r‐BN). For Cr and W substrates which have a lower mismatch with h‐BN (1 and 8.8 %), layers of t‐BN were deposited at much lower temperature (1000°C–1150°C) with a spacing between basal planes of 3.5 Å and morphology similar to that observed on SiC substrates. We obtained t‐BN layers with in plane strong disorder but out of plane orientation (c‐axis normal to the surface).     

Electronic absorption spectra of lead iodide

Optical absorption studies on gel grown single crystals and vacuum evaporated thin film of lead iodide have been carried out at room temperature and liquid nitrogen temperature. The exciton peak in the case of gel grown crystal was observed at 4940 Å whereas for the film at 4900 Å. The presence of lead colloids in the film was revealed through a broad featureless band around 5500 Å. The absorption tails in the temperature range from 80 to 300 K are found to obey Urbach rule. Examining the various power law dependences of the observed optical density on photon energy, it has been established that the transition is of direct type resulting in a band gap of 2.53 ev.     

Electroluminescence studies of chemically deposited (Zn‐Cd)S:Cu,F films

Electroluminescence (EL) emission has been observed under AC field excitation in chemically deposited (dipping technique) films of (Zn‐Cd)S:Cu,F using substrates of conducting glass plates. Results of XRD, SEM, absorption spectra, transmission spectra, EL emission spectra, voltage, frequency and temperature dependence and brightness waves of EL brightness are presented and discussed. SEM studies show better growth condition in presence of F. X‐ray diffraction studies show diffraction lines due to CdS and ZnS. Both the studies represent average particle sizes of the order of 1Å. Absorption studies show change in band gap due to increasing concentration of ZnS. The observed EL emission (blue‐green region) may be due to Cu, F combination. Results of transmission spectra give band gap similar to those given by absorption spectra. From voltage dependence of EL brightness acceleration‐collision mechanism is found to be effective. Frequency dependence of EL brightness shows first an increase in brightness in the lower frequency range followed by saturation at higher frequencies. Temperature dependence of EL emission shows a maximum at 40°C. Brightness waves consist of primary and secondary waves, which depend on voltage and frequency of excitation & the ambient temperature. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structure of autoepitaxial diamond films

A reflection high energy electron diffraction (RHEED) method has been used to investigate the structural peculiarities of synthetic diamond autoepitaxial films, deposited from a gaseous phase onto natural diamond seed crystal. The diamond films on the (111) and (110) faces usually have internal stresses, which cause the (111) plane microtwinning process at thicknesses of about 1000 Å. The thickness of twin lamellas is about 0.01?1μm. On the (100) face the diamond films do not undergo twinning and have a high structural perfection.     

Optical properties and synthesis of CuInSe2 thin films by selenization of Cu/In layers

In this paper, we report the effect of annealing temperature on the properties of copper indium diselenide (CuInSe₂) thin films. The CuInSe₂ thin films were fabricated at 500 °C for 2 h by annealing Cu‐In layers (as precursors) selenized in a glass tube with pure selenium powder. The structural and morphological properties of the CuInSe₂ thin films were characterized respectively by means of x‐ray diffraction (XRD) and field‐emission scanning electron microscope (FE‐SEM). The type of CuInSe₂ thin film has been identified as direct allowed and the band gap value was determined. The study of UV/Visible/NIR absorption shows that the band gap value of CuInSe₂ thin film is about 1.07 eV, which is within an optimal range for harvesting solar radiation energy. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Solid-phase epitaxy for the formation of superlattices based on A3B5 compounds

To form superlattices based on A³B⁵ compounds, it is suggested to use solid-phase epitaxy (SPE) which includes recystallization of super-thin films of stoichiometric composition deposited by laser evaporation on single-crystal plates or films with the same or close composition. The recrystallization temperature is shown to be reduced considerably for the film grains with its curvature differing significantly from zero and which are in contact with their own single-crystal seed having practically zero curvature. The single-crystal multilayer films GaAs-(Al, Ga)As … GaAs were formed at 300°C. The recrystallization rate at this temperature was 40 Å/min. The autocatalytic action of the single-crystal seed strongly reduced the activation energy of the SPE process, which may be due to diffusion in solid phase.     

Optical properties of thermally evaporated CdS thin films

CdS thin films of varying thicknesses were deposited on cleaned glass substrates at room temperature by thermal evaporation technique in a vacuum of about 2 x 10^‐5 torr. UV‐VIS spectra of the films were studied using the optical transmittance measurements which were taken in the spectral region from 300 nm to 1100 nm. The absorbance and reflectance spectra of the films in the UV‐VIS region were also studied. Optical constants such as optical band gap, extinction coefficient, refractive index, optical conductivity and complex dielectric constant were evaluated from these spectra. All the films were found to exhibit high transmittance (∼ 60 ‐ 93 %), low absorbance and low reflectance in the visible/near infrared region from ∼ 500 nm to 1100 nm. The optical band gap energy was found to be in the range 2.28 – 2.53 eV. All the films annealed at 300°C for 4 hours in vacuum (∼ 10^‐2 torr) showed a decrease in the optical transmittance with its absorption edge shifted towards the longer wavelength, leading to the result that the optical band gap decreases on annealing the films. Also, on annealing crystallinity of the films improves, resulting in decrease in the optical transmittance. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

A Polymorph Crystal Structure of Hexaphenyl Observed in Thin Films

Highly oriented thin films of hexaphenyl — which are used in organic opto‐electronic applications — are characterised in terms of their crystal structures. Two different crystal structures of hexaphenyl (C₃₆H₂₆) are observed when the films are prepared by physical vapour deposition at various substrate temperatures. If the substrate is kept at room temperature, hexaphenyl crystallises within a structure which is already known from single crystal investigations. However, when the thin films are grown at a substrate temperature of 160°C a new crystalline phase appears. This structure was characterised by X‐ray and transmission electron diffraction. Due to the strong preferred orientation of the crystallites within the thin films, the lattice constants as well as main features of the new crystal structure could be determined. The lattice is indexed as monoclinic with: a = 7.98Å, b = 5.54Å, c = 27.64Å and β = 99.8°. The new crystal structure has high similarity to the already known crystal structure: Both structures are built by layers of hexaphenyl molecules, within one layer the aromatic planes of the hexaphenyl molecules are packed in a herringbone pattern. The characteristic feature of the new structure is that the long axes of the hexaphenyl molecules are arranged absolutely perpendicular to the layers, whereas, within the already known structure the long axes show an tilt angle of 17° to the layer normal direction.     

Substrate temperature effect on the optical properties of amorphous Sb2S3 thin films

Sb₂S₃ amorphous thin films were prepared by thermal evaporation of corresponding powder on thoroughly cleaned glass substrates held at temperature in the range 300‐473 K. X‐ray diffraction and atomic force microscopy have been used to order to identify the structure and morphology of surface thin films. The optical constants of the deposition films were obtained from the analysis of the experimental recorded transmission data over the wavelength range 400‐1400 nm. An analysis of the absorption coefficient values revealed an optical indirect transition with the estimation of the corresponding band gap values. It was found that the optical band gap energy decrease with substrate temperature from 1.67 eV at 300 K to 1.48 eV at 473K. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structure analysis of MgSiO3 glass

The structure of MgSiO₃ glass was investigated by a combination of radial distribution function (RDF) analysis with an intensity comparison method on the basis of X-ray diffraction data. There appeared five peaks at 1.63, 2.08, 2.58, 3.25 and 4.2 Å in the RDF curve. The short range structure was found to be similar to that observed in pyroxenes: single chains composed of SiO₄ tetrahedra are linked by Mg²⁺ ions laterally. The Mg²⁺ ion is surrounded by six oxygen atoms on average, four of which form MgO pairs with an average distance of 2.08 Å and the remainder Mg O pairs of 2.5 Å which contribute to the formation of the third peak at 2.58 Å in the RDF curve together with the OO pairs (2.66 Å) in SiO₄ tetrahedra. The calculated intensity curve based on this model was in good agreement with the observed one.     

Luminescence gap in hydrogenated amorphous silicon

The “luminescence gap” is used instead of the thermalization gap and the hopping-gap because the gap is obtained from the luminescence measurement. The luminescence gaps in hydrogenated amorphous silicon (a-Si:H) are observed in the temperature range from 4.2 to 225 K for the films prepared at different substrate temperatures 170 to 300 °C by plasma CVD. It is shown from the temperature dependence of the luminescence gap that the luminescence edges are at the localized band tail states at which the waiting time for the hopping is equal to the life time of the luminescence. The excitation energy dependence of the luminescence peak energy similar to that of the porous Si has been observed.     

Mechanism of condensation of heteroepitaxial A3B5 layers pulse of moderate power

The mechanism of condensation of heteroepitaxial layers in laser deposition was studied on GaAs films on NaCl. Films were deposited in a superhigh vacuum using laser pulses of moderate power. Pulsed deposition proved to be more suitable for nucleation and growth than continuous deposition. However in this case it is important to compare the number of atoms deposited per pulse and the number of preferential adsorption centres in the substrate temperature of 310 °C. The density of dislocations in the films was about 10⁹ cm⁻². The main reasons for the dislocations are the excess of low volatile component and thermal stresses. Using a laser with quantum energy higher than the energy gap of the deposited semiconductor GaAs, which provides congruent evaporation, and making an additional deposition of As, we could reduce dislocations to 10⁷ cm⁻². A mechanism is proposed to explain the reduction of temperature in single crystal growth under laser deposition: high energy ion component of laser plasma gives rise to orienting defects on the substrate surface, and these defects determine epitaxial growth.