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A new photocatalyst for CO2 reduction has been presented. The photocatalyst was prepared from a combination of a commercial P25 with a mesopore structure and carbon spheres with a microporous structure with high CO2 adsorption capacity. Then, the obtained hybrid TiO2-carbon sphere photocatalysts were deposited on a glass fiber fabric. The combined TiO2-carbon spheres/silica cloth photocatalysts showed higher efficiency in the two-electron CO2 reduction towards CO than in the eight-electron reaction to methane. The 0.5 g graphitic carbon spheres combined with 1 g of TiO2 P25 resulted in almost 100% selectivity to CO. From a practical point of view, this is promising as it economically eliminates the need to separate CO from the gas mixture after the reaction, which also contains CH4 and H2.

Three nanocrystalline samples of ZnO doped with MnO (with 20, 30, and 40 wt% of MnO in initial mixture) were synthesized by the wet chemical method. Previous X-ray diffraction study has found that they contained only hexagonal ZnO and cubic ZnMnO3 nanocrystals. DC magnetization study revealed a paramagnetic (PM) state above 50 K, the presence of mixed valence of Mn ions (Mn3+ and Mn4+) and an important role played by magnetic clusters influencing the behavior of the effective magnetic moment and effective interaction type. Low temperature results indicated a chain of magnetic transformation from PM to ferrimagnetic, to superparamagnetic and to blocked states. Electron spin resonance (ESR) provided additional information about magnetic relaxation of the spin clusters and possible location of separate Mn2+ and Mn4+ ions. Large magnetic inhomogeneity of our samples was evidenced, and it is the result of magnetic ions clustering, various valences of Mn ions, distribution of nanoparticle sizes, and competition of magnetic interactions.

This work aimed to obtain hybrid composites based on photoactive metal oxide and carbon having adsorption properties. The materials, composed of titanium dioxide or zinc oxide and spherical carbon, were obtained from resorcinol-formaldehyde resin, treated in a solvothermal reactor heated with microwaves and then subjected to carbonization, were received. The functional groups of pure carbon spheres (unsaturated stretching C=C, stretching C-OH and C-H bending vibrations), CS/ZnO and CS/TiO

A new approach to hydrogen production from water is described. This simple method is based on carbon dioxide-mediated water decomposition under UV radiation. The water contained dissolved sodium hydroxide, and the solution was saturated with gaseous carbon dioxide. During saturation, the pH decreased from about 11.5 to 7-8. The formed bicarbonate and carbonate ions acted as scavengers for hydroxyl radicals, preventing the recombination of hydroxyl and hydrogen radicals and prioritizing hydrogen gas formation. In the presented method, not yet reported in the literature, hydrogen production is combined with carbon dioxide. For the best system with alkaline water (0.2 m NaOH) saturated with CO

Zinc chloride and potassium oxalate are often applied as activating agents for carbon materials. In this work, we present the preparation of ZnO/carbon spheres composites using resorcinol-formaldehyde resin as a carbon source in a solvothermal reactor heated with microwaves. Zinc chloride as a zinc oxide source and potassium oxalate as an activating agent were applied. The effect of their addition and preparation conditions on the adsorption properties towards carbon dioxide at 0 °C and 25 °C were investigated. Additionally, for all tested sorbents, the CO

This study determines the effect of spent garnet as a replacement for natural sand in 3D-printed mortar at early ages. Five mixes with different spent garnet amounts were prepared (0%, 25%, 50%, 75% and 100% by volume). The ratio of binder to aggregate remained unchanged. In all mixes the water/binder ratio was assumed as a constant value of 0.375. Tests were performed to confirm the printability of the mix (a path quality test using a gantry robot with an extruder). Determinations of key buildability properties of the mix (green strength and Young’s Modulus) during uniaxial compressive strength at 15 min, 30 min and 45 min after adding water were conducted. A hydraulic press and the GOM ARAMIS precision image analysis system were used to conduct the study. The results showed that an increase in spent garnet content caused a decrease in green strength and Young’s Modulus (up to 69.91% and 80.37%, respectively). It was found that to maintain proper buildability, the recommended maximum replacement rate of natural sand with garnet is 50%. This research contributes new knowledge in terms of using recycled waste in the 3D printing technology of cementitious materials.

This paper examines the synthesis of the ZnO/carbon spheres composites using resorcinol—formaldehyde resin as a carbon source and zinc nitrate as a zinc oxide source in a solvothermal reactor heated with microwaves. The influence of activation with potassium oxalate and modification with zinc nitrate on the physicochemical properties of the obtained materials and CO2 adsorption capacity was investigated. It was found that in the case of nonactivated material as well as activated materials, the presence of zinc oxide in the carbon matrix had no effect or slightly increased the values of CO2 adsorption capacity. Only for the material where the weight ratio of carbon:zinc was 2:1, the decrease of CO2 adsorption capacity was reported. Additionally, CO2 adsorption experiments on nonactivated carbon spheres and those activated with potassium oxalate with different amounts of zinc nitrate were carried out at 40 °C using thermobalance. The highest CO2 adsorption capacity at temperature 40 °C (2.08 mmol/g adsorbent) was achieved for the material after activation with potassium oxalate with the highest zinc nitrate content as ZnO precursor. Moreover, repeated adsorption/desorption cycle experiments revealed that the as-prepared carbon spheres were very good CO2 adsorbents, exhibiting excellent cyclic stability with a performance decay of less than 10% over up to 25 adsorption-desorption cycles.

A simple method of hydrogen production through the decomposition of water subjected to UV radiation is presented. Water contained dissolved sodium hydroxide and the solution was saturated with carbon dioxide gas. During saturation, the pH value dropped from about 11.5 to 7-8. The produced bicarbonate and carbonate ions acted as scavengers for hydroxyl radicals, preventing recombination of hydroxyl and hydrogen radicals, and giving priority to the formation of hydrogen gas.In the presented method, the production of hydrogen is combined with the utilization of carbon dioxide.

In this work, low-pressure synthesis of carbon spheres from resorcinol and formaldehyde using an autoclave is presented. The influence of reaction time and process temperature as well as the effect of potassium oxalate, an activator, on the morphology and CO2 adsorption properties was studied. The properties of materials produced at pressureless (atmospheric) conditions were compared with those synthesized under higher pressures. The results of this work show that enhanced pressure treatment is not necessary to produce high-quality carbon spheres, and the morphology and porosity of the spheres produced without an activation step at pressureless conditions are not significantly different from those obtained at higher pressures. In addition, CO2 uptake was not affected by elevated pressure synthesis. It was also demonstrated that addition of the activator (potassium oxalate) had much more effect on key properties than the applied pressure treatment. The use of potassium oxalate as an activator caused non-uniform size distribution of spherical particles. Simultaneously higher values of surface area and total pore volumes were reached. A pressure treatment of the carbon materials in the autoclave significantly enhanced the CO2 uptake at 25 &deg, C, but had no effect on it at 0 &deg, C.

ZnO nanoparticles doped with transition metal ions are intensively studied nanomaterials, due to their charges and the spins of electrons that provides new magnetic, optical and transport properties. They find a vast range of applications, ranging from optoelectronics to spintronics. In this context especially important is the room temperature ferromagnetism observed for ZnO doped nanomaterials, although this phenomenon is still a controversial and open topic in material science, mostly due to low reproducibility of results from samples prepared by different techniques. In the first part of this article a short review of papers using magnetometric methods to determine the magnetic characteristics of Co-doped ZnO nanomaterials is presented. Different models introduced to explain room temperature ferromagnetism (carrier mediated ferromagnetism, Co2+-oxygen vacancy pairs, blocked superparamagnetic clusters, Co2+-Zn interstitial pairs, heterogeneous distribution of magnetic ions) are examined and discussed. In the second part, magnetisation study of a new series of nCoO/(1-n)ZnO nanocomposites synthesized by hydrothermal method under higher than previously applied pressure will be described. The obtained experimental results will be analysed and information on magnetic systems responsible for the observed characteristics and the involved magnetic interactions will be deduced.

Carbon spheres were prepared by carbonisation of phenolic resin spheres obtained using a modified Stober method in a microwave assisted solvothermal reactor. Preparation process involved water–ethanol, ammonia water, resorcinol, potassium oxalate and formaldehyde. The mixture was stirred for 24 h at room temperature and then subjected to a pressure treatment, in which the solution was treated in a microwave assisted solvothermal reactor for 15 min at a pressure of 1–3 MPa. The proposed synthesis resulted in a material containing microporous carbon spheres having high surface area (from 1178 to 1648 m2/g), with diameters from 200 to 350 nm, total pore volume from 0.49 to 0.78 cm3/g, and high CO2 adsorption capacity from 3.86 to 5.03 mmol/g measured at 0.1 MPa and 25 °C. Taking into account the properties of the obtained material, it can be applied as a sorbent for CO2 capture.

Zinc oxide (ZnO) nanocrystals containing Fe2O3 have been synthesized by the calcination method. Ferromagnetic resonance (FMR) and dc magnetization measurements of 0.40(Fe2O3)/0.60(ZnO) nanocomposite have been carried out in the 4–300 K range to study the magnetic properties of agglomerated magnetic zinc ferrite ZnFe2O4 (ZFO) nanoparticles with an average crystallite size of 12 nm. Temperature dependence of the resonance field, linewidth, and the integrated intensity calculated from FMR spectra have been determined to obtain the value of the uniaxial anisotropy field and to establish the ranges of different relaxation types. Magnetization measurements in ZFC and FC modes as well as the study of hysteresis loops allowed calculating different magnetic characteristics—blocking/freezing temperature, magnetic moment, anisotropy constant, and anisotropy field. The observed magnetic properties of 0.40(Fe2O3)/0.60(ZnO) nanocomposite were explained based on the core-shell model of ZFO nanoparticles. From comparison of FMR and dc magnetization measurements, the temperature ranges of magnetic phases existing in ZFO nanoparticles in 0.40Fe2O3/0.60ZnO nanocomposite are proposed.

Nanocrystalline samples of ZnO(Mn) were characterized by X-ray diffraction to determine composition of the samples (ZnO, Mn3O4, ZnMn2O4 and ZnMnO3) and the mean crystalline size (between 9 and 13 nm for ZnMnO3 phases, from 24 to 47 nm for Mn3O4 phases and above 100 nm for ZnO and ZnMn2O4 phases). In this paper we report the experimental spectra of Raman scattering (from 200 to 1600 cm−1) with surface optical phonons (SOP) in range of 520–575 cm−1. The phonon of registered phases exhibits effects connected to phase concentration, while the SOP phonon mode exhibits significant confinement effect.

The aim of the present work is to study the magnetic properties of nanocrystals of ZnO(Co) prepared by two methods of synthesis. We used the microwave assisted hydrothermal synthesis and traditional wet chemistry method followed by calcination. The detailed structural characterization was performed by means of X-ray diffraction and micro-Raman spectroscopy measurements. The magnetic properties were studied by means of AC susceptibility χ. All samples demonstrated Curie–Weiss behavior at higher temperatures. For calcination process, the negative values of the Curie–Weiss θ temperature were observed indicating the predominance of antiferromagnetic interactions. For samples prepared by hydrothermal synthesis, we observed the breakdown of predominance of antiferromagnetic interactions.

On Raman scattering spectra of nanocrystaline samples ZnO(Co) prepared by use of the microwave assisted hydrothermal synthesis, surface optical phonons (SOP) where observed in the range of 519 - 572 cm-1. The mean crystalline size (33 - 300 nm) as well as the phase composition of obtained samples (ZnO, ZnCo2O4) where determinate with X - ray diffraction measurements. These measurements aloud us to study the change of SOP modes position with crystalline size and how change in concentration of doping element CoO influence the change of SOP modes intensity.

Currently, wide-gap ZnO nanoparticles bear important potential application in electro-optical devices, transparent ultraviolet protection films, and spintronic devices. We have studied the magnetic properties of nanocrystals of ZnO(Fe, Co, Mn) prepared by two methods of synthesis. We have used the microwave assisted hydrothermal synthesis and traditional wet chemistry method followed by calcination. The detailed structural characterization was performed by means of X-ray diffraction and micro-Raman spectroscopy measurements. The morphology of the samples was studied by means of SEM and TEM microscopy. The results of systematic measurements of AC magnetic susceptibility as a function of temperature and frequency as well as SQUID magnetization are presented. The SQUID magnetization measurements revealed a clear bifurcation of the FC and ZFC plots. Such behavior suggested superparamagnetic behavior above the blocking temperature. The dynamic magnetic measurements were performed at small AC magnetic field with amplitude not exceeding 5 Oe and different frequency values (from 7 Hz to 9970 Hz). For ZnO(Fe) and ZnO(Mn), the AC susceptibility maxima has been found for in-phase susceptibility Re(χ) and for out of phase susceptibility Im(χ). We analyzed the observed frequency dependence of the peak temperature in the AC susceptibility curve using the empirical parameter Φ that is a quantitative measure of the frequency shift and is given by the relative shift of the peak temperature per decade shift in frequency, as well as Vogel- Fulcher law. We observed two different types of magnetic behavior, spin-glasslike behavior or superparamagnetic behavior, depending on the synthesis process. For ZnO(Co) nanocrystalline samples high temperature Curie-Weiss behavior in AC magnetic susceptibility was observed. We observed that the determined negative values of the Curie- Weiss temperature θ depend strongly on the nominal content of cobalt oxide. It was shown that for calcination method the values of θ increase with the increase of magnetic ion content indicating enhancement of predominance of antiferromagnetic interactions. For hydrothermal method the opposite effect was observed indicating the breakdown of predominance of aniferromagnetic coupling with the increase of nominal magnetic ion content. This paper gives an in-depth discussion of the structural and magnetic properties of ZnO nanocrystals in addition to the technological issues such as different methods of wet chemical synthesis.

Surface optical phonons (SOP) were observed in the range of 496–572 cm−1 on Raman scattering spectra of nanocrystalline samples of ZnO(Co) prepared by use of the microwave assisted hydrothermal synthesis and traditional wet chemistry method followed by calcinations. The phase composition of the samples (ZnO, Co3O4, ZnCo2O4) and the mean crystalline size (14–300 nm) were determined using X-ray diffraction measurements. The SOP phonon mode exhibit significant size confinement effect, while the phonons of registered phases exhibit effects connected to phase concentration.

Fine particles n(MnO)/(1 − n)ZnO (n = 0.05 to 0.95) were prepared by wet chemistry method. According to X-ray diffraction analysis the obtained samples with n = 0.95, 0.90, 0.80, 0.70, 0.60 contained Mn3O4 and ZnMn2O4 phases, while samples with n = 0.05, 0.10, 0.20, 0.30, 0.40 and 0.50 contained ZnMnO3 and ZnO phases. The mean crystalline size of ZnMnO3 varied from 8 to 13 nm. The magnetic resonance investigations have been carried out at room temperature. Slightly asymmetric, broad and intense magnetic resonance line is recorded for all samples. The magnetic resonance spectra parameters showed marked differences depending on the composition index n. This could be explained by the variation of the magnetic susceptibility and a much slower evolution of spin relaxation, associated with the interaction of crystal field and superexchange interactions. Taking into account the values of magnetic resonance parameters, the investigated samples could be divided into two groups: these with the composition index n 0.50. A detailed discussion of the magnetic properties of different phases in the n(MnO)/(1−n)ZnO system is presented.

The aim of the present work is to study the magnetic properties of ZnO(Fe) nanocrystalline samples prepared by two methods of synthesis. We have used the microwave assisted hydrothermal synthesis and traditional wet chemistry method followed by calcination. The detailed structural characterization was performed by means of X-ray diffraction and micro-Raman spectroscopy measurements. The dynamic magnetic properties were studied by means of AC susceptibility χ . The measurements were performed at small AC magnetic field with amplitude not exceeding 5 Oe and different frequency values (from 7 Hz to 9970 Hz). The AC susceptibility maxima have been found for in-phase susceptibility Re ( χ ) and for out of phase susceptibility Im ( χ ). We analyzed the observed frequency dependence of the peak temperature in the AC susceptibility curve using the empirical parameter Φ that is a quantitative measure of the frequency shift and is given by the relative shift of the peak temperature per decade shift in frequency, as well as Vogel–Fulcher law.

Nanocrystaline samples of ZnO(Fe) were synthesized by wet chemical method. Samples were characterized by X-ray diffraction to determine composition of the samples (ZnO, Fe 2 O 3 , ZnFe 2 O 4 ) and the mean crystalline size (8–52 nm). In this paper we report the experimental spectra of Raman scattering. Main characteristics of experimental Raman spectrum in 200–1600 cm −1 spectral region are: sharp peak at 436 cm −1 and broad two-phonon structure at ∼1150 cm −1 , typical for ZnO; broad structure below 700 cm −1 that has different position and shape in case of ZnFe 2 O 4 or Fe 2 O 3 nanoparticles. Low-frequency Raman modes were measured and assigned according to confined acoustic vibrations of spherical nanoparticles. Frequencies of these vibrational modes were analyzed in elastic continuum approximation, which considers nanoparticle as homogeneous elastic sphere.

Nanocrystalline samples of ZnO(Fe) were synthesized by wet chemical method. Samples were characterized by X-ray diffraction to determine composition of the samples (ZnO, Fe2O3, ZnFe2O4) and the mean crystalline size (8–52 nm). In this paper we report the experimental spectra of the Raman scattering (from 200 to 1600 cm−1). Main characteristics of experimental Raman spectrum in 200 to 1600 cm−1 spectral region are: sharp peak at 436 cm−1 and broad two-phonon structure at ≈ 1150 cm−1, typical of ZnO; broad structure below 700 cm−1 that has different position and shape in case of ZnFe2O4 or Fe2O3 nanoparticles. PACS numbers: 63.20.−e, 78.30.Fs, 78.67.−n

Nanocrystalline samples of ZnO doped with Fe2O3 were synthetized by wet chemical method. The series of ZnO nanosized samples in the wide range of Fe2O3 concentration (from 5 wt.% to 95 wt.%) was prepared by precipitation from nitrate solutions using ammonia. The phase composition of the samples was determined using X-ray diffraction measurements. The phases of hexagonal ZnO, and/or rhombohedric Fe2O3, and/or ZnFe2O4 were identified. The mean crystalline size of nanocrystals, determined with the use of Scherrer’s formula, varied from 8 to 52 nm. The preliminary micro-Raman spectroscopy measurements were performed. The observed features are typical of Fe doped ZnO nanoparticles. The magnetic measurements revealed the presence of different types of magnetic behavior. For samples with high Fe2O3 contents (above 70 wt.%) the ferromagnetic ordering was observed at room temperature. For samples with lower Fe2O3 contents we observed the phenomenon of superparamagnetism above the blocking temperature.

Utilization of spent iron catalyst for ammonia synthesis Several methods of the utilization of spent iron catalyst for ammonia synthesis have been presented. The formation of iron nitrides of different stoichiometry by direct nitriding in ammonia in the range of temperatures between 350°C and 450°C has been shown. The preparation methods of carbon nanotubes and nanofibers where iron catalyst catalyse the decomposition of hydrocarbons have been described. The formation of magnetite embedded in a carbon material by direct oxidation of carburized iron catalyst has been also presented.

FourseriesofZnOnanopowdersobtainedbyamicrowavehydrothermalmethodareexamined. Twodifferentsolvents (ethanol and distilled water) and different values of pressure during heating in the reactor were used.The obtained nanopowders show a bright emission covering visible light spectral region, including the bandedge emission. Results of scanning electron microscopy, X-ray diffraction, photo- and cathodoluminescenceinvestigationsandalsoCIE1961chromaticitydiagramarepresented.PACS:78.67.

R. Kostic, N. Romcevica,∗, M. Romcevic, B. Hadžic, R. Rudolf, I. Kuryliszyn-Kudelska, W. Dobrowolski, U. Narkiewicz and D. Sibera Institute of Physics, Pregrevica 118, 11080 Belgrade, Serbia Faculty of Mechanical Engineering, University of Maribor, Smetanova 17, 2000 Maribor, Slovenia Zlatarna Celje d.d., Kresnikova 19, 3000 Celje, Slovenia Institute of Physics, Polish Academy of Sciences, al. Lotnikow 32/46, 02-668 Warszawa, Poland Szczecin University of Technology, Institute of Chemical and Environment Engineering

Magnetic properties of nanosize ZnO powders doped with MnO magnetic dopand have been studied. Sample designated as 0.10MnO/0.90ZnO was characterized by XRD that revealed the presence of ZnO and ZnMnO3 phases. An average size of magnetic ZnMnO3 nanocrystallites was 9 nm. Magnetic resonance study has been carried out in the 4-290 K temperature range. The spectrum at each temperature was analyzed in terms of three components. The temperature dependences of resonance field, linewidth and integrated intensity of these components have been determined. Magnetic centers responsible for producing the observed spectra have been proposed.

Microwave radiation was used in the acquisition of aluminium ammonium calcium phosphates. The substrates such as CaCO3, H3PO4, aqueous ammonia were reagent grade, whereas Al(OH)3 was prepared afresh. The influence of process parameters (pH 6 ± 2, molar ratios of Al3+: Ca2+: PO43− in the substrates, respectively 0.31: 0.62: 1; 0.5: 0.5: 1; 0.72: 0.36: 1) on the phase composition and the product properties was determined. Statistical software STATISTICA 10 was used for planning and evaluation of the experiments. The process parameters making it possible to acquire the material with the anticipated physicochemical properties were determined based on statistical evaluation of the planned research by the plan fractional factorial design at three levels 3(k−p). The phase composition of the samples was studied using XRD analysis. The specific surface area was calculated using the BET method and the particle size was determined by LSM. Materials with a molar ratio of Al3+: Ca2+ and Al3+: NH4+ in the range of 0.07–0.76 and 0.75–3.4, respectively, with an absorption oil number of 36–56 g per 100 g, S BET within 8.2–73 m2 g−1, and particle size in the range of 156–252 nm were obtained.

A magnetic ZnFe2O4 (MNZnFe) was synthesized by microwave assisted hydrothermal method and was used as an adsorbent for the removal of acid dye Acid Red 88 (AR88) from aqueous solution. The effects of various parameters such as initial AR88 concentration (10-56 mg L(-1)), pH solution (3.2-10.7), and temperature (20-60°C) were investigated. Prepared magnetic ZnFe2O4 was characterized by XRD, SEM, HRTEM, ICP-AES, BET, FTIR, and measurements of the magnetic susceptibility. The experimental data were analyzed by the Langmuir and Freundlich models of adsorption. Equilibrium data fitted well with the Langmuir model. Pseudo-first-order and pseudo-second-order kinetic models and intraparticle diffusion model were used to examine the adsorption kinetic data. The adsorption kinetics was found to follow the pseudo-second-order kinetic model. Thermodynamics parameters, ΔG°, ΔH° and ΔS°, indicate that the adsorption of AR88 onto MNZnFe was spontaneous and exothermic in nature.

Fine particles of ZnFe2O4 were synthesized by a wet chemical method in the (80 wt.% Fe2O3 + 20 wt.% ZnO) system. The morphological and structural properties of the mixed system were investigated by scanning electron microscopy, X-ray diffraction, inductively coupled plasma atomic emission, and X-ray photoelectron spectroscopy. The major phase was determined to be the ZnFe2O4 spinel with particle size of 11 nm. The magnetic properties of the material were investigated by ferromagnetic resonance (FMR) in the temperature range from liquid helium to room temperature. A very intense, asymmetric FMR signal from ZnFe2O4 nanoparticles was recorded, which has been analyzed in terms of two Callen-lineshape lines. Temperature dependence of the FMR parameters was obtained from fitting the experimental lines with two component lines. Analysis of the FMR spectra in terms of two separate components indicates the presence of strongly anisotropic magnetic interactions.

We have studied the magnetic properties of ZnO nanocrystals doped with MnO and CoO in the wide range of magnetic dopant (from 5 to 95 wt. %), synthetized by wet chemical method. The samples were characterized by means of XRD and micro-Raman spectroscopy. The results of systematic measurements of magnetic susceptibility as a function of temperature and frequency as well as SQUID magnetization are presented. We observed different types of magnetic behavior. ZnO nanocrystals doped with CoO demonstrate Curie-Weiss behavior at higher temperatures. For samples doped with MnO, we observed the superparamagnetism above the blocking temperature.