Impact of high temperatures on aluminoceladonite studied by Mössbauer, Raman, X-ray diffraction and X-ray photoelectron spectroscopy

Mössbauer, Raman, X-ray diffraction and X-ray photoelectron spectroscopies were used to examine the effects of temperature on the structure of two aluminoceladonite samples. The process of oxidation of Fe2+ to Fe3+ ions started at about 350 °C for the sample richer in Al and at 300 °C for the sample somewhat lower Al-content. Mössbauer results show that this process may be associated with dehydroxylation or even initiate it. The first stage of dehydroxylation takes place at a temperature > 350 °C when the adjacent OH groups are replaced with a single residual oxygen atom. Up to ~500 °C, Fe ions do not migrate from cis-octahedra to trans-octahedra sites, but the coordination number of polyhedra changes from six to five. This temperature can be treated as the second stage of dehydroxylation. The temperature dependence on the integral intensity ratio between bands centered at ~590 and 705 cm−1 (I590/I705) clearly reflects the temperature at which six-coordinated polyhedra are transformed into five-coordinated polyhedra. X-ray photoelectron spectra obtained in the region of the Si2p, Al2p, Fe2p, K2p and O1s core levels, highlighted a route to identify the position of Si, Al, K and Fe cations in a structure of layered silicates with temperature. All the measurements show that the sample with a higher aluminum content and a lower iron content in octahedral sites starts to undergo a structural reorganization at a relatively higher temperature than the less aluminum-rich sample does. This suggests that iron may perform an important role in the initiation of the dehydroxylation of aluminoceladonites

Formation of Fe and Ni substituted LiMn2-XMXO4 nanopowders and their crystal and electronic structure and magnetic properties

The Pechini sol-gel method was applied to obtain LiMn2-xTxO4 (T = Ni, Fe; x = 0.1 to 0.5) nanopowders. Crystal and electronic structures, chemical composition and magnetic properties of the materials were characterized by X-ray diffraction, XPS, SEM/EDX microscopy, prompt gamma-ray activation analysis (PGAA), Mössbauer spectroscopy and magnetic susceptibility, respectively. XRD measurements showed that the LiMn2-xNixO4 were single phase for x = 0.1 and 0.2. Three samples with higher Ni content contained some addition of a second phase. Analysis of the oxidation state of the dopants by XPS revealed ionic Ni2+ and Fe3+. Mössbauer spectroscopy also confirmed 3+ oxidation state of iron and its location in octahedral sites, which excluded the inverse spinel configuration. XPS examinations showed that Mn3+ ions dominated in the iron substituted series whereas the Mn4+ was dominant in the nickel serie

Biocompatibility of Titania Nanotube Coatings Enriched with Silver Nanograins by Chemical Vapor Deposition

Bioactivity investigations of titania nanotube (TNT) coatings enriched with silver nanograins (TNT/Ag) have been carried out. TNT/Ag nanocomposite materials were produced by combining the electrochemical anodization and chemical vapor deposition methods. Fabricated coatings were characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy. The release effect of silver ions fromTNT/Ag composites immersed in bodily fluids, has been studied using inductively coupled plasmamass spectrometry (ICP-MS). Themetabolic activity assay (MTT) was applied to determine the L929 murine fibroblasts adhesion and proliferation on the surface of TNT/Ag coatings. Moreover, the results of immunoassays (using peripheral blood mononuclear cells—PBMCs isolated from rats) allowed the estimation of the immunological activity of TNT/Ag surface materials. Antibacterial activity of TNT/Ag coatings with different morphological and structural features was estimated against two Staphylococcus aureus strains (ATCC 29213 and H9). The TNT/Ag nanocomposite layers produced revealed a good biocompatibility promoting the fibroblast adhesion and proliferation. A desirable anti-biofilm activity against the S. aureus reference strain was mainly noticed for these TiO2 nanotube coatings, which contain dispersed Ag nanograins deposited on their surface

A deeper insight into (Lu,Y)AG : Pr scintillator crystals

Interior of Czochralski-grown (Lu,Y)AG:Pr crystals has been examined by means of several techniques, such as X-Ray Photoelectron Spectroscopy, X-Ray Diffraction, Time-of-Flight Secondary Ion Mass Spectrometry, and magnetic susceptibility measurements. Additionally, their luminescence has been monitored at various combinations of a double-beam (X-ray/IR) excitation

Revisiting properties of CaCoSinO2n+2. Crystal and electronic structure

In a public space there are several reports of materials with general stoichiometry CaCoSinO2n+2. Pyroxene CaCoSi2O6 is probably the best-known representative for n = 2 but not much is known about materials with n = 3 and n = 4. In this study, attempts were carried out to synthesize those phantom materials and it was found that they do not exist as a single phase. A quantitative XRD analysis revealed that their chemical composition is correct but the formula should be written as CaCoSi2O6 + (n-2)SiO2. Similar qualitative conclusions were drawn from investigation of magnetic (DC magnetometry) and electronic properties using X-ray Photoelectron Spectroscopy (XPS) and Si K edge X-ray Absorption Spectroscopy (XAS). Additionally, the DFT ab initio calculations were carried out to obtain electronic signature from band structure of CaCoSi2O6. The apparent influence of the excess of SiO2 on magnetic properties of this “series” can be understood in terms of presence and suppression of secondary phases like Ca2CoSi2O7, which form when the starting materials are not homogenized properly. Addition of surplus SiO2 suppresses their formation leaving clear signature from CaCoSi2O6, which also can be synthesized from stoichiometric mixture using proper techniques

Synthesis and applications of [60]fullerene nanoconjugate with 5- aminolevulinic acid and its glycoconjugate as drug delivery vehicles

The 5-aminolevulinic acid (5-ALA) prodrug is widely used in clinical applications, primarily for skin cancer treatments and to visualize brain tumors in neurosurgery. Unfortunately, its applications are limited by unfavorable pharmacological properties, especially low lipophilicity; therefore, efficient nanovehicles are needed. For this purpose, we synthesized and characterized two novel water-soluble fullerene nanomaterials containing 5-ALA and D-glucuronic acid components. Their physicochemical properties were investigated using NMR, XPS, ESI mass spectrometry, as well as TEM and SEM techniques. In addition, HPLC and fluorescence measurements were performed to evaluate the biological activity of the fullerene nanomaterials in 5-ALA delivery and photodynamic therapy (PDT); additional detection of selected mRNA targets was carried out using the qRT-PCR methodology. The cellular response to the [60]fullerene conjugates resulted in increased levels of ABCG2 and PEPT-1 genes, as determined by qRT-PCR analysis. Therefore, we designed a combination PDT approach based on two fullerene materials, C60-ALA and C60-ALA-GA, along with the ABCG2 inhibitor Ko143

A multi-analytical approach for the analysis of cation distribution in a aluminoceladonite structure

In this paper cation arrangement in two samples of aluminoceladonite, emerald green and dark-green were studied by Mössbauer, Raman and X-ray photoelectron spectroscopies. The X-ray photoelectron spectroscopy (XPS) spectra obtained in the region of the Si2p, Al2p, Fe2p, K2p, and O1s core levels provided information, for the first time highlighting a route to identify the position of Si, Al, K, and Fe cations in a structure of layered silicates. The XPS analysis showed the presence of Al in tetrahedral and octahedral coordination while the K2p line indicated the possibility of K+ substitution by other cations in interlayer sites. Mössbauer spectroscopy provided information about crystal chemistry with respect to the local electronic and geometric environment around the Fe atom and to distortions of the polyhedra. It turned out that iron was located mostly in the cis-octahedra position wherein about 75% of iron appeared in the form of Fe3+. The most preferred cation combinations around Fe corresponded to 3Fe3+ ions and MgFe2+Fe3+/2MgFe3+. Raman spectroscopy illustrated aluminium substitution in silicon and iron positions wherein the concentration of the aluminium determined the degree of structural distortion within the layered system. These isomorphic substitutions implied a typical band arrangement in the hydroxyl region, which has not been observed in celadonites so far