Papers by Author: Eugeniusz Łągiewka

Abstract: The Ni+W+Mo+Si composite coatings were prepared by electrodeposition under the galvanostatic conditions (j_dep = -100 mA cm^-2) from the nickel bath containing powders of tungsten, molybdenum and silicon. Thermal treatment of the obtained coatings was conducted in argon atmosphere. Chemical composition of the coatings was determined by energy dispersive spectrocopy (EDS). Phase composition investigations were conducted by X-ray diffraction (XRD) method. Studies of electrochemical corrosion resistance were carried out in 5 M KOH solution. On the basis of these investigations it was found that Ni+W+Mo+Si thermally treated coating is more corrosion resistant than Ni+W+Mo+Si as-deposited coating.

Abstract: The Ni-P, Ni-Co-P and Ni-P+Co coatings were obtained in galvanostatic conditions at the current density of j_dep= -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.

Abstract: The Ni+Mo composite coatings were prepared by electrodeposition under the galvanostatic conditions (j_dep = -300 mA cm^-2) from the nickel bath containing molybdenum powders of different granulation (3-7 μm, <150 μm, <100 nm). Thermal treatment of the obtained coatings was conducted in the argon atmosphere. The surface morphology of the coatings was studied using a scanning electron microscopy (SEM). Chemical composition of the electrodeposits was determined by X-ray fluorescence spectroscopy (XRF). Phase composition investigations were conducted by X-ray diffraction (XRD) method. Investigations of hydrogen evolution reaction (HER) and electrochemical corrosion resistance were carried out in 5 M KOH solution. It was found that for the Ni+Mo thermally treated coatings the decrease in activity towards the HER was observed. Simultaneously these coatings are more corrosion resistant than Ni+Mo as-deposited coatings. The reasons for the electrochemical properties of these coatings have been discussed.

Abstract: Electrodeposited Ni-P, Ni-W-P, Ni-P+W and Ni-P+NiO+W coatings were obtained in the galvanostatic conditions at the current density j_dep = -200 mA cm^-2. A stereoscopic microscope was used for surface characterization of the coatings. The phase composition of the coatings was determined using X-ray diffraction (XRD) method. The chemical composition of the deposits was determined using atomic absorption spectroscopy (AAS). It was found out that the introduction of the tungsten powder in one case, and the nickel oxide and tungsten powder in the other into the electrolytic Ni-P matrix results in obtaining the coatings with a very rough surface. The coatings obtained in this way may be useful while applying them as electrode materials in electrochemistry.

Abstract: The Ni+W+Si and Ni+W+Mo+Si composite coatings were obtained by electrodeposition of crystalline nickel from an electrolyte containing suspension of suitable metallic and non-metallic components (W, Mo and Si). These coatings were obtained under galvanostatic conditions, at the current density of j_dep = -0.100 A cm^-2 and at the temperature of 338 K. For comparison the Ni coating were also obtained and investigated in the same manner. Obtained coatings were modified in the air atmosphere by thermal treatment at the temperature of 973 K for 1 h. Thus obtained coatings may be useful in application as electrode material for the oxygen evolution reaction.

Abstract: The Ni+Al+Ti composite coatings were prepared by the electrodeposition under the galvanostatic conditions at the deposition current denisty of j_dep = -225 mA cm^-2. Phase composition investigations were conducted by X-ray diffraction (XRD) method. The surface morphology, cross-section and chemical composition of the coatings were examined using a scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS), respectively. Thermal treatment of the obtained composite coatings was conducted in argon atmosphere at the temperature of 800^oC for 12 h. It was found that the as-deposited Ni+28at.%Al+25at.%Ti composite coating is a three-phase material (Ni, Al and Ti phases). The thermal treatment caused the chemical reaction in solid state of the heated coating, and a new multi-phase material was formed containing Ni and Al metallic phases as well as NiAl, Ni₂Al₃, Ni₃Al, NiTi, NiTi₂ and Ni₃Ti intermetallic phases. Thus obtained composite coatings may be useful in the applications as materials in the electrochemical processes.

Abstract: The Ni-P and Ni-Co-P coatings were electrodeposited at the deposition current density of j_dep = -20 mA cm^-2. Thermal treatment of these coatings was conducted in air at 400^oC for 1 h. Scanning electron microscopy (SEM) was used for surface morphology characterization of the coatings. Phase composition was investigated by X-ray diffraction (XRD) method. Atomic absorption spectrometry (AAS) was applied to specify chemical composition of obtained coatings. It was found that introduction of Co into amorphous Ni matrix caused the surface development of the obtained deposit. The Ni-P coating revealed an amorphous structure. The Ni-Co-P coating was formed of the amorphous matrix and the amorphous alloy ingredient. Thermal treatment of the coatings allowed to obtain new multi-phase materials with slightly developed surface.

Abstract: 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.

Abstract: The Zinc composite coatings containing Ni powder were obtained by the electrodeposition and electroless methods. Electrodeposited Zn+Ni coatings were plated with the current density jk = 150 mA/cm2 from the zinc chloride bath containing the suspension of nickel powder. Electroless (Zn-Ni)+Ni coatings were obtained by chemical reduction of Ni2+ and Zn2+ ions from the sulphate bath containing sodium hypophosphite as a reducing agent and mechanically dispersed Ni powder suspension. The thickness of (Zn-Ni)+Ni layer was ~8 m. In order to enhance the Zn content the obtained coatings were covered with the electrolytic Zn layers of different thickness (5 m, 8 m and 14 m) – (Zn-Ni)+Ni/Zn. The thermal treatment of the obtained composites was carried out at a temperature of 320oC, during 2h in argon atmosphere. The electrodeposited coatings show the presence of Zn, Ni(Zn) and ZnO phases. The electroless coatings show the presence of Zn, Ni(Zn) and ZnO phases. The additional electrodeposition of Zn leads to the creation of dilayer coatings (Zn-Ni)+Ni/Zn. The annealing of such obtained coatings leads to the creation of Ni2Zn11 intermetalic phase. The average Ni(Zn) and Ni crystallite size before annealing is in a range of 200 Å and after annealing the size is increasing to values of 600-800 Å.

Abstract: 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.