Eugeniusz Łągiewka

Crystallite Size Determination of MgO Nanopowder from X-Ray Diffraction Patterns Registered in GIXD Technique

The problem of the crystallite size determination for nanomaterials from X-ray diffraction data obtained in asymmetrical GIXD geometry was analyzed. The studies were performed on nanocrystalline MgO powder prepared by sol-gel synthesis. The nanopowder was preliminary characterized from X-ray diffraction pattern registered in classical Bragg-Brentano geometry and electron microscope observation. The estimated crystallite size, calculated form Williamson-Hall method, equals to 5 nm whereas the lattice distortion is negligible (0.1%). The X-ray diffraction patterns were registered in 30-135º 2θ range using tunnel GIXD technique for the incident α angle: 0.25; 0.5; 1; 2.5 and 5 degrees, respectively. Additional broadening of diffraction lines originated from applied geometry was observed. The calculated crystallite size deviate significantly in comparison to results obtained from classical Bragg-Brentano data. Corrections for additional line broadening were determined, which should be applied for accurate crystallite size calculation in studies of thin nanocrystalline layers using GIXD technique.

Lattice and Peak Profile Parameters in GIXD Technique

Grazing incident X-ray diffraction technique was applied to determine the influence of incident beam angle (α angle) on structural parameters as well as peak profile. X-ray diffraction patterns were registered in asymmetrical geometry, in which a parallel beam was formed by Soller and divergence slits. Lowering of the α angle results in accuracy decrease of lattice parameters as well as in significant broadening of a half-width of X-ray diffraction line.

Electrolytical obtaining of Ni-Mo coatings with polypyrrole

Electrolytic coatings Ni-Mo with PPy were obtained by electrodeposition and electropolymerization from a galvanic bath containing Ni2+, MoO4 2–, ClO4 – ions and pyrrole (Py). The cyclic chronovoltamperommetric curve was used to determine the potential and current density of electrodeposition process. As the electropolymerization is anodic process while the electrodeposition is cathodic one, the electrode was working alternately as anode and cathode. The process was conducted under alternating potentiostatic or galvanostatic conditions. Comparative tests were carried out for Ni-Mo alloy. The results of structural investigation of the obtained coatings by the X-ray diffraction method show, the Ni-Mo layers are nanocrystalline solid solution of molybdenum in nickel (α phase), whereas the Ni-Mo+PPy coatings are characterized by decreased peaks coming from Ni-Mo base. Surface morphology of obtained Ni-Mo+PPy and Ni-Mo coatings was investigated by scanning microscope. It was stated, that the coatings obtained by alternating potentiostatic method exhibit multilayer character, whereas the coatings obtained under alternating galvanostatic conditions are characterized by the presence of Ni-Mo nanoagglomerates plated on polymer surface.

The Influence of Sodium Molybdate on the Properties of Zn-Ni Layers Obtained by Electrolytic Deposition

This study was undertaken in the aim to try the limit of extraction of Zn from Zn-Ni system. The aim was realized by the addition of MoO42- ions into the galvanic bath containing Ni2+ and Zn2+ ions. Zn-Ni-Mo layers were deposited under galvanostatic conditions on (OH18N9) austenitic steel substrate. The influence of Na2MoO4 concentration in a bath on the surface morphology, chemical and phase composition and the corrosion resistance of obtained layers, was investigated. The properties of Zn-Ni-Mo layers were compared to the properties of electrolytic Zn-Ni layer. Structural investigations were performed by the X-ray diffraction (XRD) method. The surface morphology and chemical composition and surface chemical elements distribution of deposited layers were studied using a scanning electron microscope. Electrochemical corrosion resistance investigations were done by classical Stern method and electrochemical impedance spectroscopy. The potentiodynamic curves in the range of  0.05V to the potential of open circuit, were obtained. On the base of these curves the parameters like corrosion potential- Ecor, corrosion current density- icor and the polarization resistance- Rp were determined. These values served as a measure of the corrosion resistance of obtained layers. Results of impedance investigations were presented on the Nyquist Z”= f (Z’) and the Bode log Z = f (log) and  = f (log), diagrams. On the basis on this research, it was exhibited that surface morphology, chemical composition of Zn-Ni-Mo layers are dependent on Mo contents. The optimal content of Na2MoO4 in the bath for the sake of corrosion resistance in 5% NaCl, is found to be 1.2 gdm-3.

Studies on Electrodeposited Ni-Mo Nanocrystalline Alloy

The studies on structure of electrodeposited Ni-Mo nanocrystalline lloys are the subject of this paper. The contents of molybdenum in alloys was growing with the change of current density and they were in a range from 3.5 to 23 [at.%]. X-ray diff raction was performed using a Philips Diffractometer PW1130 with cooper radiation ( λ = 1.5418 Å) and graphite monochromator on the diffracted beam. The structure analysis was prepared b y Rietveld Refinement using DBWS 1988 RR version program. The received accuracy parameters: Rp and Rwp were in a ran ge from 2.3 to 8.3 % and goodness of fit was in a range from 1.17 to 2.9 %. Based on the Rietveld refinement results, the change of lattice parameters – a (from 3.50 to 3.58 Å), the crysta lline ize – D (from 3 to 22 nm), and the lattice strain – a a ∆ (from 3.4 to 16.5 x 10 ) were also studied.

Electrochemical Characterization of Nickel-Phosphorus Based Coatings Containing Cobalt

The Ni-P, Ni-Co-P and Ni-P+Co coatings were obtained in galvanostatic conditions at the current density of jdep= -200 mA cm-2. A stereoscopic microscope was used for surface morphology characterization of the coatings. The X-ray diffraction (XRD) method was used to determine phase composition of the coatings and the atomic absorption spectrometry (AAS) was applied to specify their chemical composition. The behavior of the obtained coatings was investigated in the process of hydrogen evolution reaction (HER) from 5 M KOH using steady-state polarization and electrochemical impedance spectroscopy (EIS) methods. It was found that introduction into Ni-P amorphous matrix powder of cobalt produced porous electrode materials which could be used for the HER.

Influence of thermal treatment on the corrosion resistance of electrolytic Zn–Ni+Ni composite coatings

This study was undertaken in order to obtain and characterize the corrosion resistance of Zn–Ni+Ni composite coatings. The influence of thermal treatment on surface morphology, phase composition, and corrosion resistance of Zn–Ni+Ni coating was investigated. The Zn–Ni+Ni coating was deposited under galvanostatic conditions (j = 40 mA cm−2). Thermal treatment was carried out in argon atmosphere. The surface morphology of Zn–Ni+Ni coatings was carried using a scanning electron microscope (JEOL JSM-6480) and the surface chemical composition was determined by the EDS method. Structural investigations were conducted by X-ray diffraction method. The studies of electrochemical corrosion resistance were carried out in a 5% NaCl solution, using potentiodynamic and scanning vibrating electrode (SVET) methods. On the grounds of corrosion investigations, it was stated that thermal treatment improves both total and localized corrosion resistance of Zn–Ni+Ni coating in a 5% NaCl water solution. The higher corrosion resistance of the thermally treated Zn–Ni+Ni coating could be attributed to the increase in the amount of zinc bonded to nickel in the form of Ni2Zn11 and Ni5Zn21 intermetallic phases. The SVET analysis indicated that thermal treatment of Zn–Ni+Ni coating causes a decrease in the number of corrosion centers on their surface area.

Cini-Sawatzky's Model in Studies of Electrodeposited Ni-Mo Alloys with Polymers

Electronic structures of electrodeposited Ni-Mo layers with polyethylene, polytiophene and polypyrrole were studied by Auger electron spectroscopy using the Cini-Sawatzkys model. Comparison of the theoretical and experimental lines was carried out using the asymmetry parameter of the spectral lines. It is pointed out that the changes of the spectral main lines Ni and Mo are connected with the ways of polymerization. It has been also shown that the application of the Cini-Sawaztky model to the experimental spectral lines can be used to explain the distortion appearing in the materials. Model parameters, i.e., intra-atomic correlation and bandwidth were determined.

Influence of thermal treatment on the corrosion resistance of electrolytic Zn-Ni coatings

This study was undertaken in order to obtain and characterize the corrosion resistance of Zn-Ni coating. The process was carried out under galvanostatic conditions (j = 50 mA·cm−2) chosen on the ground of an analysis of the deposition process in the Hull’s cell. The Zn-Ni coatings were deposited on austenitic (OH18N9) steel substrate from the ammonia bath. Thermal treatment of Zn-Ni coating was carried out in argon atmosphere. Structural investigations were conducted by X-ray diffraction method. Surface morphology of the obtained coatings was determined using a scanning electron microscope (JEOL JSM-6480) with EDS attachment. The electrochemical corrosion resistance of the prepared Zn-Ni coatings, austenitic (OH18N9) and (St3S) steels, was defined. The studies of electrochemical corrosion resistance were carried out in 5 % NaCl, using potentiodynamic and electrochemical impedance spectroscopy (EIS) methods. Examinations of localized corrosion resistance were conducted using scanning vibrating electrode technique (SVET). On the grounds of these investigations it was found that Zn-Ni coating after thermal treatment was more corrosion resistant than the Zn-Ni coating before thermal treatment. The relatively good corrosion resistance of Zn-Ni coatings is not as high as the resistance of (OH18N9) steel substrate, but higher compared to (St3S) steel. Therefore, the Zn-Ni coatings may be regarded as a protective coating for St3S steel.

The Characteristic of the Multilayer Thin Films by X-Ray Reflectometry Method

The X-ray reflectometry (XR), as a non-destructive method, is a powerful tool in obtaining information about parameters of thin films such as thickness, average density and interface roughness. In this paper Cu/Au, Au/Cu and Cu/Ag multilayer thin films (where the total thickness is less then 1000Å) are presented. The multilayer films are obtained by thermal evaporation in a UHV system, on the silicon substrate. The experimental XR curves contained critical angle and classical Kiessig’s fringes. For these materials the density (), the thickness () and interface roughness () information for every layer separately were calculated. The experimental reflectometry curves were analyzed using the WinGixa programme X’Pert software. The values of layer density show that they are reached in neighbor density and it is connected with the creation of the Cu-Au or Ag-Cu interlayer reached into Cu, Au or Ag, respectively. The analysis of roughness show that there are comparable to roughness of substrate only for 2-3 first layers. Further the roughness of Cu, Au, Ag layers are increasing. The comparison of results show that increasing of Ag an Au roughness is bigger than Cu.