L. Pająk

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.

Structure of Fe-Based Metallic Glass after Crystallization Process

The work presents a crystallization process of Fe-based amorphous alloy by characterization of the influence of annealing temperature on structural changes and magnetic properties of Fe72B20Si4Nb4 metallic glass. The studies were performed on the samples in the form of ribbons and rods. Crystallization behaviour of the studied alloy was examined by X-ray diffraction (XRD) and transmission electron microscopy (TEM) methods. The studies of soft magnetic properties of tested material involved magnetic permeability, saturation induction, coercive field and magnetic after-effects measurements.

Structure analysis of nanocrystalline MgO aerogel prepared by sol-gel method

Wet gel obtained by sol-gel technique was dried in supercritical CO2 to prepare hydrated form of magnesium oxide. Calcination at 723 K under vacuum yielded nanocrystalline MgO aerogel. Structure studies were performed by X-ray diffraction, scanning and transmission electron microcopies. Electron microscopy images reveal rough, unfolded and ramified structure of solid skeleton. Specific surface area SBET was equal to 238 m2/g. X-ray pattern reveals the broadened diffraction lines of periclase, the only crystalline form of magnesium oxide. The gamma crystallite size distribution was determined using FW 5 4 / 5 1 M method proposed by R. Pielaszek. The obtained values of and σ (measure of polydispersity) of particle size parameters are equal to 6.5 nm and 1.8 nm, respectively, whereas the average crystallite size estimated by Williamson-Hall procedure was equal to 6.0 nm. The obtained at Rietveld refinement Rwp, and S fitting parameters equal to 6.62% and 1.77, respectively, seem to be satisfactory due to the nanosize of MgO crystallites and because of the presence of amorphous phase.

Influence of Alloying Additions on Enhancement of Soft Magnetic Properties Effect and Crystallization in FeXSiB (X=Cu, V, Co, Zr, Nb) Amorphous Alloys

The crystallization and optimization of magnetic properties effects in FeXSiB (X=Cu, V, Co, Zr, Nb) amorphous alloys were studied by applying X-ray diffraction methods, high resolution transmission electron microscopy (HRTEM), resistometric and magnetic measurements. The temperatures of the first and the second stage of crystallization, the 1h optimization annealing temperature and the Curie temperature were determined for different amorphous alloys. Activation energies of crystallization process were obtained by applying the Kissinger method. The influence of alloy additions on optimization effect and crystallization processes was carefully examined.

Structural Studies of Metallic Powders Fe-Al-X (X= Fe, Ni, Cu, Cr) Type Obtained by the Self-Decomposition Method and Electro-Magneto-Mechanical Grinding

The Fe-Al-X and Fe-Al-Ni-X (X = Fe,Ni,Cu,Cr) metallic powders obtained by the selfdecomposition method and next intensive grinding in an electro-magneto-mechanical mill were examined by X-ray powder diffraction (XRD). Morphology of powders was determined by scanning electron microscopy (SEM) whereas energy dispersive spectroscopy (EDS) was applied to identify the composition of phases. The FeAlX and FeAlNiX phases both of B2 type structure were found besides small amounts of Al(OH)3 and rest of metallic additions.

Crystallization and Optimization of Soft Magnetic Properties Effect in FeSiB, FeNbSiB, FeCuNbSiB, FeCuZrCoSiB Amorphous Alloys

The aim of the present paper is to find correlations between structural changes and electrical, mechanical and magnetic properties in Fe78Si13B9, Fe76Nb2Si13B9, Fe75Cu1Nb2Si13B9, Fe75Cu1Zr1Co1Si13B9, amorphous and nanocrystalline alloys obtained by melt spinning technique. The influence of annealing on material brittleness, magnetic and electric properties was examined. It was found that the optimization of soft magnetic properties effect is a thermally activated process and its diffusion parameters were determined. It was shown that for the alloys containing Cu, Nb and Zr as alloying additions, the optimization process can be attributed to formation of a nanocrystalline phase. In contrast to this for the FeSiB and FeNbSiB alloys the optimization process should be related to the relaxed amorphous phase.

Study of Fe75Al25 Alloys by the Mössbauer Spectroscopy Positron Annihilation Lifetime Spectroscopy (PALS), XRD and SEM

The structure, point defect and ordering parameter of Fe25Al samples is examined with the Mössbauer spectroscopy Positron Annihilation Lifetime Spectroscopy XRD and SEM. The studies are carried out for samples in as-cast state and after heat treatments: annealing for 24 hours at 900°C (or 1050°C) and either slow cooling with furnace or quenching to oil. Among the research method used, Mössbauer spectroscopy for determination of hyperfine structure parameters was adopted. These parameters, sensitive to changes in spin and charge electron densities in the nearest neighbourhood of a Mössbauer isotope nucleus, caused by specific configurations of atoms, are directly connected with the degree of ordering of a compound. Spectral analysis has been carried out using an authors’ software developed based on a theoretical model relating the shape of a Mössbauer spectrum to the sample microstructure. It has been shown that Mössbauer spectroscopy enables quantitative evaluation of the degree of ordering of phases occurring in samples characterised by large graining, in the case of which it is not possible to determine the long-range order parameter by X-ray diffraction. The PALS method only one type of defects is detected. The positron lifetime in these defects (V) suggests that they are quenched-in Fe-monovacancies (VFe). The vacancy concentration strongly depends on the rate of cooling.

New, Experimental Powder Diffraction Data for Metastable Fe3B Phase Prepared According to ICDD Standards

In the present work X-ray studies were performed on annealed Fe78Nb2B20 amorphous alloy prepared by melt-spinning technique. All the samples were annealed in vacuum for 1 hour at temperatures up to 800°C. For the studied alloy -Fe and Fe2B are the stable, crystalline phases. The -Fe crystallized as the first crystalline phase in the sample annealed at 350°C. On the other hand, metastable Fe3B phase appeared to be stable during annealing in 425-800°C temperature range. The best fitting of the experimental X-ray data to as jet available ICDD files was obtained for Ni3P type structure (39-1315 – S.G.: I (82)). New, experimental powder diffraction data for metastable Fe3B phase prepared according to ICDD standards were elaborated for the sample annealed at 600°C. For this sample the best agreement between the calculated values of lattice constants and positions of experimental diffraction lines was obtained. The X-ray data were collected using X-Pert Philips diffractometer equipped with curved graphite monochromator on diffracted beam. The Treor program was applied for the analysis of X-ray diffraction data.

Magnetic and Electric Properties of FeNbB Melt Spun Ribbons

In the paper Fe82Nb2B16, Fe80Nb2B18 and Fe78Nb2B20 amorphous alloys, obtained by melt spinning, were examined. It was shown that the alloys studied in the as quenched state and in the relaxed amorphous state or in nanocrystalline state (after a suitable annealing) belong to very good soft magnetic materials with relatively high resistivity. The influence of annealing on brittleness as well as magnetic and electric properties measured at room temperature was examined. A correlation between sample microstructure (in the as quenched state and after annealing) and different physical properties is discussed. It was shown that the observed changes of relative magnetic permeability can be explained by changes of magnetoelastic energy, concentration of microvoids frozen during production process, effective anisotropy constant and magnetic polarisation.