Deposition conditions in tailoring the morphology of highly porous reticular films prepared by electrostatic spray deposition (ESD) technique

Spongy-like reticular structure is a unique morphology fabricated by electrostatic spray deposition (ESD) technique. The effects of solvent, substrate temperature, precursor feeding rate, static electric field strength, and deposition time on tailoring the reticular structure were investigated. Scanning electron microscopy was used to observe the film morphology. MnO_x or LiMn₂O₄ were selected as the model materials. It is found that in addition to the conventional solvent butyl carbitol, other kinds of solvents such as ethylene glycol and propylene glycol can also be used to obtain reticular films at a suitable substrate temperature. Porous films with a low cross-linking degree pore structure can be prepared by increasing precursor feeding rate or decreasing substrate temperature. Increasing the deposition time or the electric field strength helps to obtain reticular films with more homogeneous pore size distribution. In addition, the addition of a high boiling-point solvent in mixed alcohol solvent results in the increase of proper substrate temperature. It is concluded that the fluidity of the spray droplets on the surface of a hot substrate is an important factor to form a reticular film.     

The study of exchange coupling in NiFe/Cu/IrMn trilayer structures by MOKE and FMR measurements

The exchange coupling strength of NiFe/Cu/IrMn trilayer films was examined with both a new magneto optical Kerr effect (MOKE) method developed for the exchange coupling field determination and ferromagnetic resonance (FMR) measurements. We found that the value for exchange coupling field obtained by the MOKE technique coincided with FMR result with high accuracy. Other peculiarities of FMR measurements due to interlayer exchange coupling such as angular dependence of resonance field on Cu spacer thickness are also shown in the article.     

Scanning probe microscopy studies of PbS surfaces oxidized in air and etched in aqueous acid solutions

Natural n-type PbS single crystals have been studied using AFM, STM and STS after long-term oxidation in air at ambient temperatures and extensive etching in aqueous acid solutions, in contrast to previous work devoted to initial corrosion of fresh surfaces. The exposure of PbS to atmosphere at high relative humidity for several days yields widespread loose oxidation products; the process is much slower at low humidity. Surface morphologies diverge after the treatment in 1 M perchloric and hydrochloric acid solutions at room temperature and become widely different at elevated temperatures, displaying commonly etch pits up to several micrometers in size and depth along with rather uniformly distributed 20-100 nm protrusions of PbS phase. The changes both in topography and semiconducting properties of PbS found by tunneling spectroscopy have been explained in terms of the non-uniform distribution of donor- and acceptor-type defects D⁺/D⁻ in the metal depleted surface layer, which are generated by chemical reactions and, in turn, determine the rates of the PbS corrosion. In particular, the D⁻ centers exhibit a self-catalyzing effect on the non-oxidative local dissolution of PbS in HCl media, resulting in the deep etch pits.     

Properties of Josephson junctions in the inhomogeneous magnetic field of a system of ferromagnetic particles

The effect of an array of ferromagnetic nanoparticles on the field-dependent critical current of the short overlap Josephson junction is experimentally studied. Large reversible variations of the maximum critical current are observed depending on the magnetic state of the particles. The pronounced commensurability effects are detected which are proved by the additional peaks of magnetic field induced diffraction pattern.     

Hydrolytic degradation and thermal stability of poly(naphthylimides) based on naphthalene-1,4,5,8-tetracarboxylic dianhydride and bis(naphthalic anhydrides)

The molecular properties of a number of new poly(naphthylimides) derived from naphthalene-1,4,5,8-tetracarboxylic dianhydride and bis(naphthalic anhydrides) have been studied. On the basis of hydrodynamic studies of the polymers at various stages of their thermal degradation in 96% H₂SO₄ and thermogravimetric measurements, the hydrolytic stability and thermooxidative resistance of the polymers have been compared. A correlation between the experimental data and the chemical structure of molecular chains has been established.     

Elastic instability of the nano-structured state as an intrinsic probe to study the early formation stages of sol–gel derived (Pb<Subscript>1-x</Subscript>Ca<Subscript>x</Subscript>)TiO<Subscript>3</Subscript> thin films

A novel method to investigate the early formation stages of polycrystalline (Pb_1-xCa_x)TiO₃ (PCT) perovskite films by means of traditional Brillouin and micro-Brillouin spectroscopy (BS, mBS) is described in the present work. The films were prepared by chemical solution deposition (CSD) onto oxidized (100)Si substrates and treated at temperatures between 350–650 °C by rapid thermal processing (RTP). The elastic instability observed by Brillouin spectroscopy at the nano-structured state of the PCT films was used here to determine their crystallization temperatures. Coexistence of different nanocrystalline phases (e.g., pyrochlore, perovskite) in the films could also be detected by this technique. The reliability of these results is demonstrated by complementary information obtained by X-ray diffraction (XRD) and scanning force microscopy (SFM). The effects of the annealing temperature and of the Ca²⁺ content on the crystallization process of these films are also discussed. PACS 78.35.+c; 77.84.-s; 61.82.Rx     

Studying high-spin ferric heme proteins by pulsed EPR spectroscopy: Analysis of the ferric form of the E7Q mutant of human neuroglobin

In this work, the high-spin ferric form of the E7Q mutant of human neuroglobin (E7Q-NGB) is studied by X-band continuous-wave electron paramagnetic resonance (CW EPR) and hyperfine sublevel correlation (HYSCORE) spectroscopy. It is shown that the use of matched pulses in the HYSCORE experiment is essential to observe the nitrogen spectral contributions. The validity of approximating the high-spin Fe(III) system (S=5/2) as an effectiveS=1/2 system is tested and the consequences for the HYSCORE simulations are highlighted. Comparative HYSCORE experiments combined with deuterium exchange experiments for aquometmyoglobin and ferric E7Q-NGB clearly show that the heme iron of the latter protein is pentacoordinated, lacking the distal water. Furthermore, CW EPR experiments show that, at high pH, the E10K residue is coordinating to the heme iron in this globin. These observations are corroborated by resonance Raman experiments and could also be reproduced for other E7 mutants of human and mouse neuroglobin. Finally, the proton and nitrogen hyperfine and nuclear quadrupole parameters obtained for ferric E7Q-NGB are discussed in detail.     

Strong temperature effect on X-ray photo-etching of polytetrafluoroethylene using a 10 Hz laser-plasma radiation source based on a gas puff target

The first results of experiments on direct photo-etching of heated PTFE using a 10 Hz X-ray source based on a laser-irradiated gas puff target are presented. X-ray radiation in the wavelength range from 6 to 20 nm was produced as a result of irradiation of a double-stream gas puff target with Nd:YAG laser pulses of energy 0.8 J and time duration 3 ns. The resulting X-ray pulses with energy of about 100–200 mJ were used to irradiate samples of PTFE to create microstructures by direct photo-etching. Strong enhancement of the photo-etching process was observed for samples heated up to 300 °C. PACS 52.38.Ph; 81.65.Cf; 61.82.Pv     

Investigation on hexamethyldisilazane vapor treatment of plasma-damaged nanoporous organosilicate films

Hexamethyldisilazane (HMDS) vapor treatment of plasma-damaged nanoporous organosilicate thin films has been studied as a function of treatment temperature in this work. Although, the HMDS vapor treatment facilitated incorporation of methyl (CH₃) groups subsequent to the removal of free hydroxyl (OH) groups in the damaged films at treatment temperature as low as 55 °C, the bonded OH groups were not removed. More significantly, detailed analysis of the results reveals that HMDS vapor modified only the surface of the plasma-damaged samples and not the entire film as expected. This is attributed to the formation of a thin solid layer on the surface, which effectively prevents penetration of HMDS vapors into the bulk. The Fourier transform-infrared (FT-IR) absorption and dielectric constant measurements confirm that the vapor treatment assists only partial curing of the plasma-damaged films. Alternative processes of curing the films with HMDS dissolved in supercritical carbon dioxide (SCCO₂) as a medium of reaction in static and pulsed modes were also attempted and the results are presented in this paper.