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This study characterizes oak (sessile and pedunculate oak) and alternative wood (black locust, Myrobalan plum, wild cherry, and mulberry) species as important sources of volatile compounds of aged spirits. Nowadays, their fragments are used to hasten the brandies’ aging process. The ATR-FTIR spectra of analyzed wood samples are similar, only the mulberry FTIR spectrum contains unique peaks primarily due to its highest lignin content (40.93%). Using the untargeted GC-MS approach, a total of forty-one volatile compounds were identified in the wood extracts in a model spirit solution. The volatile profiles of alternative wood extracts in a model spirit solution were significantly different, both quantitatively and qualitatively, compared to those of oak. Coniferyl (23.14 μg/g—26.6 μg/g) and sinapyl (23.56 μg/g—25.82 μg/g) alcohols were the most abundant volatile compounds in investigated oak extracts. Resorcinol and coniferyl alcohol were the most abundant volatile compounds in black locust, sakuranin in wild cherry, while resorcinol and β-resorcinaldehyde in mulberry wood. To the best of our knowledge, sakuranin has not been detected in wild cherry wood until now. Besides wood chemical characteristics, the technology used during the aging process strongly influences on volatile profiles of aged brandies, thus, these compounds are potential chemical markers for discrimination between wood species as well as aging technologies.

Introduction/Objective. Artificial enamel caries lesions are commonly created to simulate in vivo caries development and to examine the effect of non-invasive and microinvasive approaches in treatment of initial caries lesions. The objective of the present study was to compare three different demineralizing solutions and exposing times in terms of the formation of artificial white spot lesions and to evaluate their demineralization effect through scanning electron microscopy observations. Methods. Twenty intact human premolars, extracted for orthodontic reasons, were thoroughly cleaned, stored in 0.1% thymol solution at room temperature and cut at the cementoenamel junction before demineralizing process. The specimens were randomly divided into three experimental groups, according to the used demineralization agent and the time of exposure: Group I (acetic acid; pH = 4.4; 96 hours); Group II (lactic acid; pH = 4.5; 120 hours); Group III (Lactic acid; pH = 4.3; 504 hours) and one control group (saline). After demineralisation, macroscopic appearance was checked and all specimens were observed under scanning electron microscope to evaluate the enamel characteristics and caries lesion depths. Results. In Group I and II enamel subsurface porosity with dissolution of enamel crystals is detected and the mean depths of white spot lesions were 48.55 μm (SD = 1.11) and 43.23 μm (SD = 6.74), respectively. In Group III structural integrity of enamel surface was not preserved. Conclusion. Demineralizing solutions used in experimental groups I and II resulted in artificial initial caries lesions with satisfactory characteristics and similar appearance on scanning electron microscopy. The outcome of demineralizing process which lasted 504 hours were cavitated enamel lesions.

To investigate the effect of synthesis procedure and sintering temperature on the functional properties of perovskite/spinel ceramics, BaTiO3/CoFe2O4 composites were prepared by thermal decomposition, coprecipitation, and microemulsion method, and sintered at 1150°C and 1300°C. The phase composition and morphology of as-prepared powders as well as sintered ceramics were thoroughly examined by X-ray powder diffraction (XRPD) and scanning electron microscopy (SEM) coupled with electron dispersive spectroscopy (EDS). The dielectric and ferroelectric measurements were performed in detail. Generally, the samples sintered at 1300°C had better performances than those sintered at 1150°C. The composite synthesized by thermal decomposition and sintered at 1300°C stands out among other prepared BaTiO3/CoFe2O4 ceramics, owing to high stability in the wide frequency range and low leakage currents. The obtained results indicate that such composite might be successfully applied as a functional multiferroic.

Phyllosilicate mineral pyrophyllite is predominantly used in the ceramic industry because it exhibits high refractoriness. Due to its thermal transformation into mullite, pyrophyllite is stable at elevated temperatures, making it a suitable mineral additive for refractory non-shaped materials and various ceramic shaped products. In this study, pyrophyllite is employed as 50 % clay replacement in the ceramics and up to 30 % cement replacement in mortars. Physico-mechanical properties were investigated. The firing shrinkage in the ceramics treated at 1200 °C was reduced by pyrophyllite addition. Pyrophyllite acted as additional pozzolana during cement hydration. Within the microstructure, it formed micro-reinforcement in the shape of crystalline folia, which improves the mechanical properties of ordinary Portland cement, high aluminate cement, and blended cement mortars. The investigation proved the efficiency and suitability of pyrophyllite employed as a substitution for clay in ceramics and a cement replacement in mortars.

BZT ceramics was prepared by using fine powder mixture of BaCO3, TiO2 and ZrO2 in the respective molar ratio to form Ba(Zr0.10Ti0.90)O3 via solid state reaction at elevated temperature. The prepared BZT was milled in the planetary ball mill from 0-120 min to achieve different powder grades from micron to nano-sized particles. After the powder characterization by XRD and SEM the samples were pressed in disc shape and sintered at different temperatures from 1100-1350°C in the air. The sintered samples were characterized by SEM and their density and average grain size was determined and presented vs. sintering temperature and powder grades (milling time). After that the silver epoxy electrodes were deposited on sintered disc samples. The disc samples capacity and resistivity were measured at low frequency region from 1 Hz to 200 kHz using low frequency impedance analyzer. The sintering temperatures and powder grades were used as parameters. Finally the specific resistance ρ, dielectric constant (ε' + jε") and tgδ where determined from the impedance measurements. The behavior of electronic properties where analyzed e.g. the relaxation effect of the space charge (inter-granular electric charges) vs. sintering temperature and ceramic grades. The results obtained were compared with best literature data for the losses in BZT ceramics at low frequencies.

Powder mixture consisted of ZnO, Mn2O3 (MnCO3) and Fe2O3 blended powders, was found laminating during compaction. Polyvinyl alcohol (PVA) and a combination of PVA with polyethylene glycol (PEG) added as a plasticizer, were introduced as polymer binders to improve the compaction of oxide mixtures. It has been done by forming a suspension of oxide mixture and varying the polymer solution concentration and composition. By evaporating the solvent, new materials were obtained, which consist of oxide particles bound via polymer. In such a manner obtained hybrid materials were characterized with attenuated total reflection Fourier transformed infrared (ATR-FTIR) spectroscopy, differential thermal analysis (DTA) and transmission electron microscopy (TEM). The oxide polymer material was compacted at 200 MPa and the expansion of this compact during heating was monitored in temperature range up to 550ºC with dilatometer. It was found that PVA forms graft polymer with PEG and specific interaction with oxide particles surface was revealed.

Magnesium aluminate has the spinel structure along with good mechanical, chemical, and thermal properties. Magnesium aluminate has a wide range of applications including refractory ceramics, optically transparent ceramic windows, and armors. Its low dielectric permeability and low loss tangent enable its applications for integrated electronic devices, as well. In this paper, MgO and Al2O3 powders were mixed in a one-to-one molar ratio and calcined at temperatures ranging from 1500 to 1800oC to produce phase pure spinel. Thereafter, pellets were crushed and treated in a planetary ball mill for 60 min to obtain a fine powder. All powders were examined for phase composition, crystal structure, and morphology. The obtained results showed that by increasing the temperature, samples with higher density were synthesized. Milling for 1 h led to formation of larger particles, but finer powders after milling. XRPD and Raman spectroscopy showed disorder in the crystal structure after milling.

In this study, microstructure evolution and dielectric properties of SrTiO3 ceramic have been investigated, whereby mechanical activation of SrTiO3 powders was used to modify the functional properties of ceramic materials. Microstructural SEM analysis of SrTiO3 ceramics showed that the increase in mechanical activation time results in less porous samples. Raman spectroscopy indicated changes in the broadening and asymmetry of the TO2 mode with a change in the time of mechanical activation. TO2 mode showed a Fano asymmetry due to its interaction with polarization fluctuations in polar micro-regions, which are a consequence of the presence of oxygen vacancies caused by activation. The maximum value of dielectric permittivity was observed in the sample activated for 10 min. Also, the sample activated for 10 min exhibits relatively low values of loss tangent, compared to the other mechanically activated samples, providing the best overall dielectric performance compared to other samples.

The impact of the type and amounts of nanofiller on the features of the glycidyl methacrylate-co-ethylene glycol dimethacrylate (GMA-co-EGDMA)/organomodified montmorillonite (OMt) nanocomposites that were prepared by in situ radical suspension polymerization, was examined. Cloisite 30B and Cloisite 25A were used in this study as nanofillers, in amounts of 2 and 10 wt.%. The structure, morphology, thermal stability and porosity of the initial GMA-co-EGDMA copolymer and their nanocomposites were examined by ATR-FTIR analysis, wide angle X-ray diffraction (XRD), scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDS), transmission electron microscopy (TEM), thermogravimetric analysis (TG) and mercury porosimetry. It has been established that both clay nanofillers were successfully incorporated into the structure of the initial copolymer, simultaneously on their surface and also on cross-sectional area. Prepared samples with 2 wt.% have predominantly exfoliated, while samples with 10 wt.% have some tactoids-aggregates structure of the OMt layers. Thermogravimetric analysis revealed that after ~ 30 % of degradation, all nanocomposites become more thermal stable than the initial copolymer. The obtained results indicate that porosity parameters can be easily modified with the addition of clay nanofillers and thus prepared nanocomposites adjusted to specific purposes.

Pure Ti films deposited by radio-frequency magnetron sputtering on FTO glass were anodized to fabricate TiO2 nanotubes (NTs) arrays. The TiO2 NTs/FTO samples were sintered at 450, 550 and 630°C, in ambient air. The thermal treatment did not influence the crystal phase composition, preserving in all cases the anatase single phase. As expected, the crystalline anatase quality improved with the annealing temperature. Nevertheless, slight differences in nanotubular morphology, such as the appearance of grains inside the walls, were observed in the case of the sample sintered at 630°C. Chemical analysis by X-ray Photoelectron Spectroscopy of annealed samples revealed the presence of Sn inside TiO2 NTs, due to diffusion of Sn from the substrate to TiO2. For the substrate was used FTO glass whose top layer consists of SnO2 doped with F. Rutherford Backscattering Spectrometry and Time-of-Flight Elastic Recoil Detection Analysis were carried out to study the elemental depth profile of the films. It was found that the temperature of sintering controls the Sn diffusion inside TiO2 film. Sn atoms diffuse towards the TiO2 NTs surface for the samples annealed at 450 and 550°C. The diffusion is however hindered in the case of the heat treatment at 630°C. Besides, the Ti diffusion into the SnO2 underlayer was observed, together with the formation of TiO2/SnO2 interfaces. One then expected but not a great difference in absorption between samples, since all contained anatase phase, as confirmed by Diffuse Reflectance Spectroscopy. A higher amount of Sn was however detected for the sample annealed at 550°C, which accounts for a slight red absorption shift. The importance of controlling the annealing parameters of the anodized TiO2/FTO structures was highlighted through the formation of TiO2-SnO2 interfaces and the Sn insertion from FTO, which can play an essential role in increasing the photoperformances of TiO2 NTs/FTO based structures of photovoltaic cells.

The effect of zircon (ZrSiO4) on the physico-chemical and mechanical properties of geopolymer/zircon composites was examined in this study. Four geopolymer/zircon composites containing 10, 20, 30 and 40 wt.% zircon were prepared from metakaolin with alkali activators. Characterization of the obtained geopolymers was performed by X-ray diffraction (XRD), Scanning electron microscope (SEM-EDS), Fourier transform infrared spectroscopy (FTIR) and Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF). XRD results did not confirmed the formation of interconnected phases between added zircon, starting aluminum silicates and alkali activators. Compressive strength of prepared geopolymer was examined. The maximum obtained compressive strength of 70.15 MPa was measured in sample containing the smallest fraction of zircon, i.e., 10 wt.%. Addition of larger amount of zircon (20 wt.%) hinders the progress of geopolymerization reaction and consequently decreases compressive strength.

In this study, the structure, morphology and composition of the synthesized magnetite/3D-printed wollastonite (3D_W/M) composite were characterized, and its adsorption performance with respect to As(V) and Cr(VI) were studied. Magnetite (MG) modified 3D printed wollastonite was obtained by two step procedure: modification of 3D_W with 3-aminoproylsilane (APTES) followed by controlled magnetite (MG) deposition to obtain 3D_W/M adsorbent. The structure/properties of 3D_W/M were confirmed by applying FTIR, XRD, TGD/DTA, and SEM analysis. The adsorption properties of hybrid adsorbents were carried out for As(V) and Cr(VI) removal - one relative to the initial pH value, the adsorbent mass, the temperature, and the adsorption time. Time-dependent adsorption study was best described by pseudo-second order equation, while Weber Morris analysis showed that intraparticle diffusion controled diffusional transport. Similar activation energy, 17.44 and 14.49 kJ•mol-1 for adsorption As(V) and Cr(VI) on 3D_W/M, respectively, indicated main contribution of physical adsorption. Determination of adsorption parameters was performed by applying different adsorption isotherm models, and the best fit was obtained using Freundlich model. The adsorption capacity of 24.16 and 29.6 mg g-1 for As(V) and Cr(VI) at 2ºC, Co = 5.5 and 5.3 mg L-1, respectively, were obtained. Thermodynamic study indicated favourable process at a higher temperature. Preliminary fixed-bed column study and results fitting with Bohart-Adams, Yoon-Nelson, Thomas, and Modified dose-response model showed good agreement with results from the batch study.

As a secondary industrial product, peach waste (PW) presents an ecological problem, but is potentially a rich source of natural antioxidants. A potential and novel way to improve the phytochemical stability of waste rich in phytochemicals is encapsulation in yeast cells that possess good structural characteristics. In the present study, PW extract was encapsulated in non-plasmolyzed, plasmolyzed and living Saccharomyces cerevisiae cells using the freeze-drying method. HPLC analysis revealed that β-carotene is the most abundant carotenoid, while epicatechin and catechin are the most abundant phenolics in PW. The highest encapsulation efficiency of carotenoids (86.59 %), as well as phenolics (66.98 %), was obtained with freeze-dried non-plasmolyzed yeast cells used as carriers. Although plasmolysis can cause some changes in the structure and properties of yeast cells, it did not enhance the encapsulation efficiency of present phytochemicals. Successful encapsulation of PW extract in yeast cells was confirmed by FTIR spectroscopy and SEM imaging. The obtained results present the encapsulation of sensitive compounds in yeast cells by freeze-drying as an excellent method for preserving valuable compounds and their potential use in the food and pharmaceutical industries.

Development in many areas of engineering and technology are closely linked to the development of new or improvement of existing materials. Having in mind wide use of bacterial nanocellulose (BNC) in various areas of everyday life, from biomedicine, ecology to electronics, BNC-based composites are becoming widely used and attracting the attention of the scientific community. It is especially important to examine in detail the synthesis parameters that affect the changes in the crystal structure and morphology of the obtained composites, having in mind that these changes have a crucial influence on their final functional properties. In this paper, a composite material based on bacterial nanocellulose BNC (as the matrix) and ferromagnetic Fe3O4 was studied. BNC was obtained by the activity of acetic fermentation bacteria after 7 days of growth in a suitable medium. The research is aimed to optimization of the Fe3O4 precipitation conditions. It's especially considering the time interval of BNC films spend in the iron salt solution. The influence of the performed synthesis conditions was considered by the SEMEDS, FTIR and XRD methods.

Magnetite (MG) modified cellulose membrane (Cell-MG), obtained by reaction of 3-aminosilane and subsequently with diethylenetriaminepentaacetic acid dianhydride functionalized waste Cell fibers (Cell-NH2 and Cell-DTPA, respectively), and amino-modified diatomite was used for Azoxystrobin and Iprodione removal from water. Cell-MG membrane was structurally and morphologically characterized using FT-IR and FE-SEM techniques. The influences of operational parameters, i.e. pH, contact time, temperature, and the mass of adsorbent on adsorption and kinetics were studied in a batch system. The calculated capacities of 35.32 and 30.16 mg g-1 for Azoxystrobin and Iprodione, respectively, were obtained from non-linear Langmuir model fitting. Weber-Morris model fitting indicates the main contribution of intra-particle diffusion to overall mass transport resistance. Thermodynamic data indicate spontaneous and endothermic adsorption. The reusability of adsorbent and results from wastewater purification showed that Cell-MG could be used as general-purpose adsorbent. The adsorbent/adsorbate surface interaction was considered from the results obtained using density functional theory (DFT) and calculation of molecular electrostatic potential (MEP). Thus, a better understanding of the relation between the adsorption performances and contribution of non-specific and specific interactions to adsorption performances and design of novel adsorbent with improved properties was deduced

A novel magnetic polymer/bentonite composite was prepared by suspension copolymerization of glycidyl methacrylate and ethylene glycol dimethacrylate in the presence of magnetic bentonite (MB-PGME) and functionalized with ethylene diamine and hexamethylene diamine (MB-PGME-ED and MB-PGME-HD). The obtained samples were characterized in terms of structure as well as thermal, magnetic and morphological properties. The sorption of rhenium (Re) and tungsten (W) from aqueous solution onto MB-PGME-ED and MB-PGME-HD was investigated considering their contact time and different initial ion concentration, giving possibility for usage of these composites as commercial sorbents. The sorption system follows the pseudo-second order and intraparticle diffusion kinetic models. The results indicated a better fit with the Freundlich isotherm model.

This work is the first report of a very simple and fast one-pot synthesis of nickel oxide (NiO) and hematite (α-Fe2O3) nanoparticles by thermal decomposition of transition metal aqua complexes with camphor sulfonate anions. Obtained nanopowders were characterized by X-ray powder diffraction, Fourier transform IR analysis, scanning electron microscopy, and Energy-dispersive X-ray spectroscopy. X-ray powder diffraction confirmed the formation of high purity NiO and α-Fe2O3 crystal phases. In the case of α-Fe2O3, about five times larger average crystallite size was obtained. Fourier transform IR spectra of synthesized materials showed characteristic peaks for NiO and α-Fe2O3 nanostructures. To visualize the morphology and the chemical composition of the final products Scanning electron microscopy and Energy-dispersive X-ray spectroscopy were performed. The thermogravimetric analysis was done for a better understanding of the general thermal behavior of precursor compounds. This easy-to-perform and fast preparation method opens a broad range of obtained materials’ usage, particularly due to its economic viability

The aim of the study was to investigate the influence of low heating temperatures with two different retention times to optimize the process for obtaining nanosized hydroxyapatite material that can possibly be used in the fields of biology and pharmacy. Nanosized hydroxyapatite was successfully obtained by wet chemical precipitation. The annealing of the material performed at 300 oC with two different retention times i.e. 3 and 6 hours in air atmosphere. Low annealing temperature with extended retention time was selected in terms to reduce energy consumption. FTIR spectroscopy was used to confirm characteristic vibrational bands of hydroxyapatite samples, and presence of carbonate bands of hydroxyapatite annealed for 3h and 6h. X-Ray powder diffraction analysis were used to examine phase composition, determine the size of unit cells and crystallite sizes, and SEM-EDS methods were used to obtain particle size and arrangement also grain growth morphology and confirmed the presence of calcium, phosphorous oxygen and carbonate peaks. The results show that different retention time has influence on particle growth as well as unit cell parameters and crystallite sizes changes of hydroxyapatite material

The influence of mechanical activation on the formation, sintering kinetics and morphology was investigated in sintered barium strontium titanate (BST) ceramics with different Ba-to-Sr ratios. Initial powders were mechanically activated for 20 and 120 min, leading to mechano-chemical reaction and formation of BaxSr1-xTiO3 phases. Agglomeration was found to represent an important factor in the process of formation of BaxSr1-xTiO3 phases around 800°C and during sintering. It reduces the effectiveness of mechanical activation on formation of BaxSr1-xTiO3 phases beyond the short period (20 min), while in the process of sintering, prolonged mechanical activation (120 min) leads to a significant reduction in sintering temperature and the corresponding value of activation energy. In addition, all three systems show a phase transformation around 1100°C, attributed to the hexagonal-to-cubic phase transition. Morphology of the final sintered ceramics can be correlated primarily with the state of the pre-sintered powder, where mechanically activated powders with smaller particle size produced more compact and less porous final product.

Single phase MgAl2O4 was made from a one-to-one molar ratio of MgO and Al2O3 powders mixed using ball-milling. Mixtures of MgO and Al2O3 were subsequently treated in planetary ball mill for 30, 60, 90 and 120 minutes in air. The aim of this study was to examine phase composition, microstructure, and densification behavior of sintered specimens. After sintering in dilatometer at 1500°C, the powder was converted to single phase MgAl2O4. The results show that mechanical activation improved the densification behavior of MgAl2O4 sintered specimens, and it reduced the onset temperature for sintering by approx. 100°C. Based on dilatometer data, powders were subsequently densified at 1450°C by hot pressing. Almost аll specimens exhibited full density, while sample activated for 30 minutes showed the fastest densification rate. [Project of the Serbian Ministry of Education, Science and Technological Development, Grant no. OI 172057, and Grant no. III 45007]

The purpose of this investigation is to investigate the hydrophobicity of geopolymers, new alumino-silicate materials and the influence of Si/Al ratio on their surface properties. Contact angle measurement (CAM) as reliable indicator of hydrophobicity was determined for synthesized geopolymers using water and ethylene-glycol as reference liquids. Geopolymers were synthesized from various precursors: kaolin, bentonite and diatomite. Characterization of phase structure and microstructure was performed by XRD, FTIR, SEM/EDX methods. Contact angle measurements confirmed that the geopolymers synthesized from metakaolin are the most porous, which can be explained by the smallest Si/Al ratio. The maximum value of contact angle and free surface energy (110.2 mJ/m2) has been achieved for geopolymer synthesized by diatoms (GPMD). SEM micrograph of GPMD shows a homogeneous surface with some longitudinal cavities in the gel and is significantly different from the micrographs of other two geopolymer samples, GPMB and GPMK. [Project of the Serbian Ministry of Education, Science and Technological Development, Grant no. III 45012 and Grant no. III 45005]

Corundum (α-alumina) is a suiTab. material for usage in various industry fields owing to its chemical stability, electrical and mechanical features. It is known that properties of ceramics could be modified by addition of different oxides, as well as by changing the consolidation parameters. In this respect, alumina was doped with 1 wt.% of Cr2O3, Mn2O3 and NiO, followed by 1 hour of mechanical activation in a high-energy planetary ball mill. A sensitive dilatometer was used for sintering of powder mixtures up to 1400 oC and recording the obtained dilatation. The final density varied between cca. 1.9 and 3.3 g/cm3. Microstructural changes were detected by SEM measurements. Changes in electrical permittivity and loss tangent were associated with the preparation conditions (types of additives, duration of mechanical activation). For a given mixture, the sintering increases the relative permittivity and decreases losses, exhibiting the optimal values of 8.32 and 0.027, respectively, for the sample activated 60 minutes and sintered, with the addition of MnO2. Mechanical measurements indicate significant differences in strength with the addition of different transition metal oxides. Samples with Mn and Ni, activated and sintered, with strength of 121 and 86 MPa, respectively, have a significantly higher tensile strength than the other tested samples, due to their more compact microstructures. [Project of the Serbian Ministry of Education, Science and Technological Development, Grant no. OI 172057, Grant no. III 45007 and Grant no. III 45019]

One-dimensional (1D) TiO2 nanotubes perpendicular to the substrate were obtained by electrochemical oxidation of titanium foil in an acid electrolyte. In order to alter the crystallinity and the morphology of films the as-anodized amorphous TiO2 nanotube films were sintered at elevated temperatures. The evolution of the morphology was visualized via scanning electron microscopy (SEM), while the crystalline structure was investigated by X-ray diffraction (XRD) and Raman spectroscopy. The chemical composition was studied by X-ray photoelectron spectroscopy (XPS). The effects of crystallinity and morphology of TiO2 nanotube (NTs) films on photocatalytic degradation of methyl orange (MO) in an aqueous solution under UV light irradiation were also investigated. The TiO2 nanotubes sintered at 650°C for 30 min had the highest degree of crystallinity and exhibited the best photocatalytic activity among the studied TiO2 nanotube films. [Project of the Serbian Ministry of Education, Science and Technological Development, Grant no. OI 172057 and Grant no. III 45019]

In this study the characterization of FeCo-2V alloys toroidal samples produced by PIM/MIM technology was presented. The feedstock for metal injection molding (MIM) was prepared by mixing starting FeCoV powder with a low viscosity binder. Green samples were subjected to solvent debinding and subsequent thermal debinding followed by sintering. Sintering was performed during 3.5 hours from 1370°C to 1460°C in hydrogen atmosphere in order to attain the appropriate mechanical and magnetic properties. Microstructure, hardness HV10 and magnetic hysteresis B(H) were investigated as a function of sintering temperature. Optimum combination of functional properties was observed after sintering at temperature of 1370°C. In addition, magnetic properties were analyzed as frequency dependent and successfully simulated in operating frequency range from 5 Hz to 60 Hz. [Project of the Serbian Ministry of Education, Science and Technological Development, Grant no. OI 172057]

Due to pozzolanic characteristics, fly ash is commonly used as a cement replacement in construction composites. Addition of natural clays with sorption ability (i.e. zeolite and bentonite) in to the fly ash based construction materials is of both scientific and industrial interest. Namely, due to the application of sorptive clay minerals, it is possible to immobilize toxic heavy metals from the composite structure. The thermal compatibility of fly ash and zeolite, as well as fly ash and bentonite, within the composite was observed during sintering procedure. The starting components were used in 1:1 ratio and they were applied without additional mechanical treatment. The used compaction pressure for the tablets was 2 t•cm-2. The sintering process was conducted at 1000ºC and 1200ºC for two hours in the air atmosphere. The mineralogical phase composition of the non-treated and sintered samples was analyzed using X-ray diffraction method. Scanning electron microscopy was applied in the analysis of the microstructure of starting and sintered samples. The thermal behavior was observed via DTA method. The influence of temperature on the properties of fly ash-zeolite and fly ash-bentonite composites was investigated. [Project of the Serbian Ministry of Education, Science and Technological Development, Grant no. III 45008 and OI 172057]

In the present study, the influence of different encapsulation techniques (lyophilization and spray drying) on gelatin, as a carrier system for delivery of polyphenols compounds, on wild thyme extracts and on encapsulated extracts was investigated. FTIR analyses has shown the presence of carbohydrates, polysaccharides, polyphenols, flavonoids, monoterpenes and carboxylates in the dried extracts, while FTIR spectrum of the encapsulated extracts has shown almost exclusively gelatin-based stripes, indicating the efficient encapsulation of the active ingredients of the extracts and therefore their protection. Scanning electron microscopy has shown that the lyophilization process produced irregularly shaped particles, while spray drying formed spherical and pseudo-spherical particles with rough surface. Using the method of diffraction of laser light, it has been found that spray dried encapsulate possessed significantly lower particle size and significantly better uniformity in comparison to the lyophilized sample. According to the results obtained in differential scanning calorimetry, endothermic peak of lyophilized gelatin encapsulate appeared at higher temperature, thus it can be concluded that lyophilized sample was more thermostable than spray dried parallel. Additionally, the values of enthalpy of gelatin encapsulates were significantly higher compared to pure extracts, which confirmed the presence of stabilizing interactions between the encapsulated components and a carrier.

Post-sintering of magnesium titanate ceramics by hot isostatic pressing (HIP) in an oxygen-free atmosphere significantly alters various electrical properties of the product. In particular, the sintered material becomes a semiconductor. The aims of this paper are: to extend our investigations of the electrical properties of this material by expanding the frequency range of measurements, to design interpolation formulas for the frequency dependence of the complex relative permittivity, and to propose HIP-sintered magnesium titanate as a material for thermistors that have a negative-temperature-coefficient resistance (NTCR), as well as for varistors. [Project of the Serbian Ministry of Education, Science and Technological Development, Grant no. TR 32005 and Grant no. ON 172057]

In this paper, synthesis of porous wollastonite-based ceramics was reported. Ceramic precursor, methylhydrocyclosiloxane, together with micro-sized CaCO3, was used as starting material. After 20 min of ultrasound treatment, and calcination at 250 oC for 30 min, yeast as a pore-forming agent was added to the as-obtained powders. Sintering regime was set up based on the results obtained by differential thermal analysis. Prepared mixture was pressed into pallets and sintered at 900 oC for 1 h. After the sintering regime, porous wollastonite-based ceramics was obtained. The phase composition of the sintered samples as well as microstructures was analyzed by X-ray diffraction method and SEM. In a batch test, the influence of pH, contact time and initial ion concentration on adsorption efficiency of As+5, Cr+6, and phosphate ions on synthesized wollastonite-based ceramics were studied. Time-dependent adsorption was best described by pseudo-second-order kinetic model and Weber-Morris model that predicted intra-particle diffusion as a rate-controlling step of overall process. High adsorption capacities 39.97, 21.87, and 15.29 mgg-1 were obtained for As+5, Cr+6, and phosphate ions, respectively.

Commercial Mn-Zn powder (Mn0.63Zn0.37Fe2O4, 93 wt. % and Fe2O3 7 wt. %) was milled 0.5, 1, 2 and 4 hours in a planetary ball mill. The goal was to observe intensive milling influences on oxidation and reduction processes that will happen during subsequent heating. Powders were characterized with XRD, SEM and particle seizer. Subsequent heating was monitored on TGA/DTA in an air atmosphere. After compaction of the milled powders, sintering was also performed in a dilatometric device. Sintered specimens were characterized micro structurally with SEM on a fresh breakage. Obtained differential TGA diagrams suggest intensive changes during prolonged milling of the oxidation kinetics on heating. Ferrite powders changed with milling as well as with second run heating were characterized to enable determination of the potentially best ratio of milling and heating to be applied to obtain the desired microstructure. [Project of the Serbian Ministry of Education, Science and Technological Development, Grant no. OI172057 and Grant no. III45014]

Cordierite 2MgO+2Al2O3+5SiO2 is frequently used ceramic material, that is commonly used as a carrier of electrical components due to its low dielectric constant (~ 5), and low temperature thermal expansion coefficient (20·10-7 oC-1). In order to accelerate the process of sintering, 5.00 mass% TeO2 was added to the starting mixtures. System was tested in two parallel mixtures, one with no additives, and the other one with TeO2. The mechanical activation of the both mixtures was performed in a highenergy ball mill in time intervals from 0 to 40 min with ball to powder mass ratio 1:40. The particle size analysis (PSA) was employed in order to determine the changes in the particle size of the mechanically treated powders. The phase composition of the starting powders as well as microstructures was analyzed by the means of X-ray diffraction method and SEM.

Cordierite-based ceramic materials are attracting much interest for their various applications in industry, for manufacturing multilayer circuit boards, catalytic converters, filters, thermal insulation, kiln furniture, components of portable electronic devices, etc. In order to reduce production costs and modify cordierite-based materials, mechanical activation can be used. In this study, microstructural and electrical properties of mechanically activated MgO-Al2O3-SiO2 system have been analyzed. The mixtures of MgO-Al2O3-SiO2 powders were mechanically activated in a planetary ball mill for the time periods from 0 to 160 min. Morphological investigations have been performed on the obtained powders. The effects of activation and two-step sintering process on microstructure were investigated by scanning electron microscopy (SEM). Electrical measurements showed variations of the dielectric constant (εr) and loss tangent (tan δ) as a function of time of mechanical treatment.

This paper presents a study of the profile distribution of available micronutrients Fe, Mn, Cu and Zn and radionuclide 137Cs in cultivated soil at the experimental field "Radmilovac" (property of Agricultural Faculty, Belgrade University) in the vicinity of Vinĉa Institute of Nuclear Sciences. The soil belongs to the anthrosol class of anthropogenic soils according to FAO (2006). At first, the deep plowing was performed while preparing soil for planting peach trees followed by cultivation of soil for 12 years. All agricultural treatments at the experimental field ceased for three years. After that period, soil sampling was carried out. Contents of DTPA-extracted Fe, Mn, Cu and Zn were in the range of (mg kg-1): 5.8-41.6; 9.2-34.2; 1-7.6 and 0.2-1.3, respectively. Detected activity concentration (Bq kg-1) for 137Cs ranged from 1.8 to 35. It was noticed that distribution patterns of 137Cs radionuclide and available Cu and Zn along soil depth were very similar and they were analyzed by simple linear regression; mutual affinity for the soil organic matter might affect their distribution in soil. Contents of available Fe and Mn exhibited different, more constant distribution within a soil horizon.

The aim of this study was to investigate the Cs+ ions sorption on natural minerals clinoptilolite. The analysis of clinoptilolite and clinoptilolite with adsorbed Cs+ ion was con- ducted by X-ray diffraction, scanning electron microscopy, X-ray fluorescence, and gamma spectrometry. The specific activity of naturally occurring radionuclides in clinoptilolite was determined by gamma spectrometry by using the HPGe semiconductor detector. Obtained activity concentrations ranged from 49 Bq/kg to 810 Bq/kg for 40K, 5.7 Bq/kg to 10 Bq/kg for 238U, 5.8 Bq/kg to 70 Bq/kg for 232Th(228Ac), and the presence of artificial radionuclides was not detected (137Cs < 0.02 Bq/kg). The study of the thermal decomposition of raw clinoptilolite and Cs adsorbed clinoptilolite by differential thermal analysis is presented in this paper. The activation energy of the reaction phase transformation of raw clinoptilolite is 156.7 kJ/mol, while Cs adsorbed clinoptilolite is 121.7 kJ/mol. The lower value of activation energy reaction of the phase transformation Cs adsorbed clinoptilolite indicates that Cs which is adsorbed destabilizes the crystal structure of clinoptilolite and thus facilitates the transition to the amorphous state. [Projekat Ministarstva nauke Republike Srbije, br. 45012]

The aim of this paper was mechanochemical preparation of magnesium titanates. Powder mixtures of starting oxides MgO and TiO2 were mechanically activated in a planetary ball mill for the time interval from 0 to 160 minutes. Structural, stereological, thermal characterizations were performed on produced powders. The effects of activation on morphology were investigated by scanning electron microscopy and particle size analyses, while the changes in the phase composition were determined by X-ray diffraction. It is determined that the first traces of MgTiO3 became detectable after 40 minutes of milling, while after 160 minutes the pure magnesium titanates were noticed. The differential thermal analyses and thermo gravimetric analysis, in temperatures range from 25 oC to 1100 oC, has been performed in order to investigate thermal behavior of the mixtures.

Introduction. Therapy with fixed orthodontic appliances starts with bracket bonding and ends with debonding of brackets, leaving enamel surface varied. Objective. The aim of this pilot study was to examine enamel surface before and after debonding of orthodontic brackets by the use of scanning electron microscopy (SEM). Methods. Epoxy replicas of four patients’ premolars indicated for therapy with fixed orthodontic appliances were made and brackets were bonded to their teeth with a different adhesives (Enlight, No-mix, Fuji Ortho LC and Heliosit Orthodontic) (n=4). Two months later, brackets on premolars were debonded and amounts of adhesive left on the tooth surfaces and the bracket bases were evaluated with the adhesive remnant index (ARI). After resin removal, epoxy replicas were made and the surface of premolars was evaluated with the enamel surface index (ESI). All replicas of premolars (n=32) were prepared for SEM examination and compared under different magnifications. Tooth damage was estimated based on correlation between ARItooth and ESI. Results. Pearson’s χ2 test showed no significant differences between ARItooth and ARIbracket of four materials used. Nonparametric correlations showed significant differences between ARItooth and ARIbracket, ESI and ARItooth, and between ESI and ARIbracket. Increasing of ARItooth is followed with the descent of ARIbracket and the ascent of ESI. Multivariate regression analysis showed a significant correlation between ESI and ARItooth. Conclusion. Most bond failures took place at enamel-adhesive interface. ARItooth was a predictor to enamel surface damage. The type of material did not affect enamel surface damage.

Distribution of natural gamma-emitting radionuclides 238U and 40K were determined in the soil profiles from the peach-trees field on experimental farm Radmilovac, southeast Belgrade. Internal soil morphology has been changed in 1992. when soil rigosol type with deep Ap-horizon (0-80 cm) has been formed by special treatment of parent soil, chernozem type. Gamma-spectrometry method is applied in measurement of radionuclide activities in soil samples by using hyperpure coaxial gamma-ray detector, Canberra type. Investigation results has been shown that the natural activity contents obtained in the experiment are within the range of normal background activity according to UNSCEAR (2000) and that radionuclide activity decreased in the plant root zone. .

In this paper the changes that occurred in differently activated ZnO-SnO2 and sintered samples were investigated using photoacoustic spectroscopy. ZnO and SnO2 powders, mixed in the molar ratio 2:1, were mechanically activated in a planetary ball mill for 10-160 min. The mixtures were pres­sed and isothermally sintered at 1300°C for two hours. X-ray diffraction analysis of the obtained sintered samples was performed in order to investigate changes of the phase composition and confirmed only the presence of a pure zinc stannate (Zn2SnO4) phase in all the sintered samples as a result of the solid state reaction and reaction sintering between the starting ZnO and SnO2 powders. The microstructure of the sintered sam­ples was examined by scanning electron microscopy and showed that mechanical activation leads to the formation of a structure with reduced particle size which accelerates spinel formation. Grain growth of the spinel phase slows down the densification process and together with the agglomerates formed during mechanical activation causes the appearance of a porous microstructure. The photoacoustic (PA) phase and amplitude spectra of the sintered samples were recorded as a function of the chopped frequency of the laser beam used (red laser with a power of 25 mW, λ=632 nm) in a thermal-transmission detection configuration. PA experimental data were analyzed using the Rosenzweig-Gersho thermal-piston model, which enabled determination of the thermal diffusivity, Z)T (m2s-1), diffusion coefficient of the minority free carriers D (m2s-1) and the optical absorption coefficient (m-1). The detected differences of the measured thermal-electrical properties of the obtained Zn2SnO4 ceramics indicate changes in the material induced by the different preparation procedure of the starting powders before the sintering process.

The SnCl4 catalyzed glycosylation reaction of peracetylated β-D-derivatives with terminally unsaturated C3–C11 alkenols was used for the synthesis of some C3–C11 alkenyl β-D-galactopyranosides, as precursors for unsaturated neutral bolaforms.