Tadeusz Chudoba

Drying Kinetics of Apple Tissue Treated by Pulsed Electric Field

The aim of this work was to study the influence of pulsed electric field (PEF) on the drying kinetics of apple tissue. Therefore, mathematical models that are commonly used in the literature were applied to describe the process. PEF treatment of the samples was carried out at an intensity of E = 5–10 kV/cm and 10–50 pulse numbers. Subsequently, the apples were convectively dried at 70°C and air velocity of 2 m/s. Based on electrical conductivity measurement, the cell disintegration index Z p was computed. Midilli et al.s(Drying Technology, Vol. 20, pp. 1503–1513, 2001) model was evaluated as the most adequate to describe the moisture transfer in PEF-treated and intact samples. PEF pretreatment induced a reduction in drying time of up to 12% when 10 kV/cm and 50 pulses were applied. For instance, after 60 min of drying, the dimensionless moisture ratio for PEF-treated (10 kV/cm, 50 pulses) samples was 0.18 compared to 0.26 for the untreated apples. The effective moisture diffusivity, calculated on the basis of the Ficks second law, was 1.04 × 10−9 m/s for intact samples and from 1.09 × 10−9 to 1.25 × 10−9 m2/s for PEF-treated samples at 10 pulses at 5 kV/cm and 50 pulses at 10 kV/cm, respectively.

Pulsed Electric Field Pretreatment for Osmotic Dehydration of Apple Tissue: Experimental and Mathematical Modeling Studies

The aim of this study was to analyze the influence of pulsed electric field pretreatment (PEF) on the osmotic dehydration of apple tissue. Osmotic dehydration was carried out in sucrose solution at 40°C and 100 rpm in a water-bath shaker. PEF pretreatment was performed using varying field strength of 5 and 10 kV/cm and 10 and 50 pulses. On the basis of electric conductivity measurement, the cell disintegration index was calculated. The course of osmotic dehydration was described by means of water loss, solid gain, weight reduction, and water content changes. Moreover, the course of the process was described by different mathematical models that are commonly used in the literature. PEF application before osmotic dehydration significantly increased water loss after 60 minutes of the process. In turn, no significant differences were found in the case of solid gain. The highest osmotic dehydration efficiency ratio (WL/SG) was noticed for samples treated by PEF at the electric field strength of 5 kV/cm and 10 pulses. The statistical analysis of mathematical modeling of the process showed the equations utilized generally exhibit a good fit to the experimental data.

Highly biocompatible, nanocrystalline hydroxyapatite synthesized in a solvothermal process driven by high energy density microwave radiation.

A microwave, solvothermal synthesis of highly biocompatible hydroxyapatite (HAp) nanopowder was developed. The process was conducted in a microwave radiation field having a high energy density of 5 W/mL and over a time less than 2 minutes. The sample measurements included: powder X-ray diffraction, density, specific surface area, and chemical composition. The morphology and structure were investigated by scanning electron microscopy as well as transmission electron microscopy (TEM). The thermal behavior analysis was conducted using a simultaneous thermal analysis technique coupled with quadruple mass spectrometry. Additionally, Fourier transform infrared spectroscopy tests of heated samples were performed. A degradation test and a biocompatibility study in vitro using human osteoblast cells were also conducted. The developed method enables the synthesis of pure, fully crystalline hexagonal HAp nanopowder with a specific surface area close to 240 m2/g and a Ca/P molar ratio equal to 1.57. TEM measurements showed that this method results in particles with an average grain size below 6 nm. A 28-day degradation test conducted according to the ISO standard indicated a 22% loss of initial weight and a calcium ion concentration at 200 μmol/dm3 in the tris(hydroxymethyl)aminomethane hydrochloride test solution. The cytocompatibility of the obtained material was confirmed in a culture of human bone derived cells, both in an indirect test using the material extract, and in direct contact. A quantitative analysis was based on the 2,3-bis-(2-methoxy-4-nitro-5-sulfophenyl)-2H-tetrazolium-5-carboxanilide. Viability assay as well as on DNA content measurements in the PicoGreen test. Indirect observations were performed at one point in time according to the ISO standard for in vitro cytotoxicity (ie, after 24 hours of cell exposure to the extracts). The direct contact tests were completed at three time points: after 24 hours, on day 7, and on day 14 of a culture in an osteogenic medium. All of the tests revealed good tolerance of cells toward the material; this was also shown by means of live/dead fluorescent staining. Both quantitative results and morphological observations revealed much better cell tolerance toward the obtained HAp compared to commercially available HAp NanoXIM, which was used as a reference material.

Effect of pressure on synthesis of Pr-doped zirconia powders produced by microwave-driven hydrothermal reaction

A high-pressure microwave reactor was used to study the hydrothermal synthesis of zirconia powders doped with 1 mol % Pr. The synthesis was performed in the pressure range from 2 to 8 MPa corresponding to a temperature range from 215°C to 305°C. This technology permits a synthesis of nanopowders in short time not limited by thermal inertia of the vessel. Microwave heating permits to avoid contact of the reactants with heating elements, and is thus particularly well suited for synthesis of doped nanopowders in high purity conditions. A mixture of ZrO2 particles with tetragonal and monoclinic crystalline phases, about 15nm in size, was obtained. The p/T threshold of about 5-6MPa/265-280°C was necessary to obtain good quality of zirconia powder. A new method for quantitative description of grain-size distribution was applied, which is based on analysis of the fine structure of the X-ray diffraction line profiles. It permitted to follow separately the effect of synthesis conditions on the grain-size distribution of the monoclinic and tetragonal phases.

Paramagnetism of cobalt-doped ZnO nanoparticles obtained by microwave solvothermal synthesis.

Summary Zinc oxide nanopowders doped with 1–15 mol % cobalt were produced by the microwave solvothermal synthesis (MSS) technique. The obtained nanoparticles were annealed at 800 °C in nitrogen (99.999%) and in synthetic air. The material nanostructure was investigated by means of the following techniques: X-ray diffraction (XRD), helium pycnometry density, specific surface area (SSA), inductively coupled plasma optical emission spectrometry (ICP-OES), extended X-ray absorption fine structure (EXAFS) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and with magnetometry using superconducting quantum interference device (SQUID). Irrespective of the Co content, nanoparticles in their initial state present a similar morphology. They are composed of loosely agglomerated spherical particles with wurtzite-type crystal structure with crystallites of a mean size of 30 nm. Annealing to temperatures of up to 800 °C induced the growth of crystallites up to a maximum of 2 μm in diameter. For samples annealed in high purity nitrogen, the precipitation of metallic α-Co was detected for a Co content of 5 mol % or more. For samples annealed in synthetic air, no change of phase structure was detected, except for precipitation of Co3O4 for a Co content of 15 mol %. The results of the magentometry investigation indicated that all as-synthesized samples displayed paramagnetic properties with a contribution of anti-ferromagnetic coupling of Co–Co pairs. After annealing in synthetic air, the samples remained paramagnetic and samples annealed under nitrogen flow showed a magnetic response under the influences of a magnetic field, likely related to the precipitation of metallic Co in nanoparticles.

Size-dependent density of zirconia nanoparticles

Summary The correlation between density and specific surface area of ZrO2 nanoparticles (NPs) was studied. The NPs were produced using a hydrothermal process involving microwave heating. The material was annealed at 1100 °C which resulted in an increase in the average grain size of the ZrO2 NPs from 11 to 78 nm and a decrease in the specific surface area from 97 to 15 m2/g. At the same time, the density increased from 5.22 g/m3 to 5.87 g/m3. This effect was interpreted to be the result of the presence of a hydroxide monolayer on the NP surface. A smaller ZrO2 grain size was correlated with a larger contribution of the low density surface layer to the average density. To prove the existence of such a layer, the material was synthesized using 50% heavy water. Fourier transform infrared spectroscopy (FTIR) permitted the identification of the –OD groups created during synthesis. It was found that the –OD groups persisted on the ZrO2 surface even after annealing at 1100 °C. This hydroxide layer is responsible for the decrease in the average density of the NPs as their size decreases. This study of the correlation between particle size and density may be used to assess the quality of the NPs. In most cases, the technological aim is to avoid an amorphous layer and to obtain fully crystalline nanoparticles with the highest density possible. However, due to the effect of the surface layers, there is a maximum density which can be achieved for a given average NP diameter. The effect of the surface layer on the NP density becomes particularly evident for NPs smaller than 50 nm, and thus, the density of nanoparticles is size dependent.

A Novel Reactor for Microwave Hydrothermal Scale-up Nanopowder Synthesis

Abstract The article presents a novel microwave reactor for hydrothermal synthesis of nanopowders. The reactor has a unique design of a process chamber, which, when used in conjunction with a batch control system, allows a highly efficient production of nanopowders. The design of the reactor together with the new principles of operation, structural materials and distribution of electromagnetic field are described. The article also presents a control system for the reactor, which allows for an automatic operation in the stop–flow mode, control of process pressure, continuous monitoring of process parameters and safe operation of the device. The device verification process is shown on the basis of the results of cobalt-doped zinc oxide nanopowder synthesis.

Effect of Water Content in Ethylene Glycol Solvent on the Size of ZnO Nanoparticles Prepared Using Microwave Solvothermal Synthesis

Zinc oxide nanoparticles ZnO NPs were obtained by the microwave solvothermal synthesis MSS method. The precursor of the MSS reaction was a solution of hydrated zinc acetate in ethylene glycol with water addition. It was proved that by controlling the water concentration in the precursor it was possible to control the size of ZnO NPs in a programmed manner. The less the water content in the precursor, the smaller the size of ZnO NPs obtained. The obtained NPs with the average particle size ranging from 25 nm to 50 nm were characterised by homogeneous morphology and a narrow distribution of particle sizes. The following parameters of the obtained ZnO NPs were determined: pycnometric density, specific surface area, phase purity, chemical composition, lattice parameters, average particle size, and particle size distribution. The average size of ZnO NPs was determined using Scherrer’s formula, Nanopowder XRD Processor Demo web application, by converting the results of the specific surface area, and TEM tests using the dark field technique. ZnO morphology and structure were determined using scanning electron microscopy SEM and transmission electron microscopy TEM. The test performed by the X-ray powder diffraction XRD confirmed that crystalline ZnO, pure in terms of phase, had been obtained.

Hydroxyapatite nanopowder synthesis with a programmed resorption rate

A microwave, solvothermal synthesis of hydroxyapatite (HAp) nanopowder with a programmed material resorption rate was developed. The aqueous reaction solution was heated by a microwave radiation field with high energy density. The measurements included powder X-ray diffraction (PXRD) and the density, specific surface area (SSA), and chemical composition as specified by the inductively coupled plasma optical emission spectrometry technique (ICP-OES). The morphology and structure were investigated using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). A degradation test in accordance with norm ISO 10993-4 was conducted. The developed method enables control of the average grain size and chemical composition of the obtained HAp nanoparticles by regulating the microwave radiation time. As a consequence, it allows programming of the material degradation rate and makes possible an adjustment of the material activity in a human body to meet individual resorption rate needs. The authors synthesized a pure, fully crystalline hexagonal hydroxyapatite nanopowder with a specific surface area from 60 to almost 240m2/g, a Ca/P molar ratio in the range of 1.57-1.67, and an average grain size from 6nm to over 30 nm. A 28-day degradation test indicated that the material solubility ranged from 4 to 20 mg/dm3.

Luminescence Properties and Energy Transfer Processes in Nanosized Cerium Doped YAG

Luminescence properties of cerium doped Y3Al5O12 (YAG) nanocrystals in form of nanopowders and nanoceramics have been studied. The comparative analysis of luminescence characteristics for nano- and single-crystals has been done. It was detected that an excitonic mechanism of the energy transfer from the host lattice to cerium ions does not work in nanopowders and nanoceramics. It was also shown that antisite-related and self-trapped exciton-related luminescence bands are suppressed strongly in nanopowders, and it can be excited only under certain circumstances. These bands practically disappeared in the nanoceramic samples. It was suggested that nanoparticles surface, which is an efficient trap for excitons and charge carriers, plays the crucial role in peculiarities of luminescence characteristics in nanocrystals.