Search results for: mechanochemical%20activation

Authors: Arezoo Hakimi, Afshin Farahbakhsh

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Herein, we comparison synthesized Fe3O4 using, hydrothermal method, Mechanochemical processes and solvent thermal method. The Hydrothermal Technique has been the most popular one, gathering interest from scientists and technologists of different disciplines, particularly in the last fifteen years. In the hydrothermal method Fe3O4 microspheres, in which many nearly monodisperse spherical particles with diameters of about 400nm, in the mechanochemical method regular morphology indicates that the particles are well crystallized and in the solvent thermal method Fe3O4 nanoparticles have good properties of uniform size and good dispersion.

Keywords: Fe3O4 nanoparticles, hydrothermal method, mechanochemical processes, solvent thermal method

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Authors: Morteza Mohri Esfahani, Amir S. H. Rozatian, Morteza Mozaffari

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Single phase magnetite nanoparticles and Bi-substituted ones were prepared by mechanochemical processing (MCP). The effects of Bi-substitution on the structural and magnetic properties of the nanoparticles were studied by X-ray Diffraction (XRD) and magnetometry techniques, respectively. The XRD results showed that all samples have spinel phase and by increasing Bi content, the main diffraction peaks were shifted to higher angles, which means the lattice parameter decreases from 0.843 to 0.838 nm and then increases to 0.841 nm. Also, the results revealed that increasing Bi content lead to a decrease in saturation magnetization (Ms) from 74.9 to 48.8 emu/g and an increase in coercivity (Hc) from 96.8 to 137.1 Oe.

Keywords: bi-substituted magnetite nanoparticles, mechanochemical processing, X-ray diffraction, magnetism

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Authors: Behrooz Ghasemi, Bahram Sharijian

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Al2O3/Mo nanocomposite powders were successfully synthesized by mechanical milling through mechanochemical reaction between MoO3 and Al. The structural evolutions of powder particles during mechanical milling were studied by X-ray diffractometry (XRD), energy dispersive X-ray spectroscopy(EDX) and scanning electron microscopy (SEM). Results show that Al2O3-Mo was completely obtained after 5 hr of milling. The crystallite sizes of Al2O3 and Mo after milling for 20 hr were about 45 nm and 23 nm, respectively. With longer milling time, the intensities of Al2O3 and Mo peaks decreased and became broad due to the decrease in crystallite size. Morphological features of powders were influenced by the milling time. The resulting Al2O3- Mo nanocomposite powder exhibited an average particle size of 200 nm after 20 hr of milling. Also nanocomposite powder after 10 hr milling had relatively equiaxed shape with uniformly distributed Mo phase in Al2O3 matrix.

Keywords: Al2O3/Mo, nanocomposites, mechanochemical, mechanical milling

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Authors: Z. Ž. Lazarević, Č. Jovalekić, V. N. Ivanovski, N. Ž. Romčević

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Nickel-zinc ferrite, Ni0.5Zn0.5Fe2O4 was prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2, Zn(OH)2 and Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 5 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase Ni0.5Zn0.5Fe2O4 samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra alows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Keywords: ferrite, X-ray diffraction, infrared spectroscopy, Raman spectroscopy, Mössbauer spectroscopy

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Authors: Z. Ž. Lazarević, D. L. Sekulić, V. N. Ivanovski, N. Ž. Romčević

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NiFe2O4 (nickel ferrite), ZnFe2O4 (zinc ferrite) and Ni0.5Zn0.5Fe2O4 (nickel-zinc ferrite) were prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2/Fe(OH)3, Zn(OH)2/Fe(OH)3 and Ni(OH)2/Zn(OH)2/Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 25 h, 18 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase ferrite samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra allows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Keywords: ferrites, Raman spectroscopy, IR spectroscopy, Mössbauer measurements

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Authors: Sarah Triller, Ferdi Schüth

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The challenges encountered in upscaling the mechanochemical synthesis of high surface area α-alumina are investigated in this study. After lab-scale experiments in shaker mills and planetary ball mills, the optimization of reaction parameters of the conversion in the smallest vessel of a scalable mill, named Simoloyer, was developed. Furthermore, the future perspectives by scaling up the conversion in several steps are described. Since abrasion from the steel equipment can be problematic, the process was transferred to a ceramically lined mill, which solved the contamination problem. The recovered alpha-alumina shows a high specific surface area in all investigated scales.

Keywords: mechanochemistry, scale-up, ball milling, ceramic lining

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Authors: Ismail Seckin Cardakli, Mustafa Engin Kocadagistan, Ersin Arslan

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In this study, mechanochemical behaviour of aluminium - boron oxide - melamine ternary system was investigated by high energy ball milling. According to the reaction Al + B₂O₃ = Al₂O₃ + B, stochiometric amount of aluminium and boron oxide with melamine up to ten percent of total weight was used in the experiments. The powder characterized by X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Scanning Electron Microscopy (SEM) after leaching of product by 1M HCl acid. Results show that mechanically induced self-sustaining reaction (MSR) between aluminium and boron oxide takes place after four hours high energy ball milling. Al₂O₃/h-BN composite powder is obtained as the product of aluminium - boron oxide - melamine ternary system.

Keywords: high energy ball milling, hexagonal boron nitride, mechanically induced self-sustaining reaction, melamine

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Authors: Qian Qiao, Tongjin Xiao, Hongtu He, Jiaxin Yu

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This study is focused on the synergetic effects of water and sulfur dioxide treatments (SO₂ treatments) on the mechanochemical wear of SLS glass. It is found that the wear behavior of SLS glass in humid air is very sensitive to the water and SO₂ treatment environments based on the wear test using a ball-on-flat reciprocation tribometer. When SLS glass is treated with SO₂-without, the presence of water, the wear resistance of SLS glass in humid air becomes significantly higher compared to the pristine glass. However, when SLS glass is treated with SO₂ with the presence of water, the wear resistance of SLS glass decreases remarkably with increasing in the relative humidity (RH) from 0% to 90%. Further analyses indicate that when sodium ions are leached out of SLS glass surface via the water and SO₂ treatments, the mechanochemical properties of SLS glass surface become different depending on the RH. At lower humidity, the nano hardness of the Na⁺-leached surface is higher, and it can contribute to the enhanced wear resistance of SLS glass. In contrast, at higher humidity conditions, the SLS glass surface is more hydrophilic, and substantial wear debris can be found inside the wear track of SLS glass. Those phenomena suggest that adhesive wear and abrasive wear dominate the wear mechanism of SLS glass in humid air, causing the decreased wear resistance of SLS glass with increasing the RH. These results may not only provide a deep understanding of the wear mechanism of SLS glass but also helpful for operation process of functional and engineering glasses.

Keywords: soda lime silicate glass, wear, water, SO₂

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Authors: Areej Almalkawi, Sameer Hamadna, Parviz Soroushian, Nalin Darsana

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The work on indigenous binders in this paper focused on the following indigenous raw materials: red clay, red lava and pumice (as primary aluminosilicate precursors), wood ash and gypsum (as supplementary minerals), and sodium sulfate and lime (as alkali activators). The experimental methods used for evaluation of these indigenous raw materials included laser granulometry, x-ray fluorescence (XRF) spectroscopy, and chemical reactivity. Formulations were devised for transforming these raw materials into alkali aluminosilicate-based hydraulic cements. These formulations were processed into hydraulic cements via simple heating and milling actions to render thermal activation, mechanochemical and size reduction effects. The resulting hydraulic cements were subjected to laser granulometry, heat of hydration and reactivity tests. These cements were also used to prepare mortar mixtures, which were evaluated via performance of compressive strength tests. The measured values of strength were correlated with the reactivity, size distribution and microstructural features of raw materials. Some of the indigenous hydraulic cements produced in this reporting period yielded viable levels of compressive strength. The correlation trends established in this work are being evaluated for development of simple and thorough methods of qualifying indigenous raw materials for use in production of indigenous hydraulic cements.

Keywords: one-part geopolymer cement, aluminosilicate precursors, thermal activation, mechanochemical

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Authors: Mazaher Yarmohamadi-Vasel, Ali Reza Modarresi-Alama, Sahar Shabzendedara

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Purpose/Objectives: The first purpose was synthesize Poly(N-(sulfophenyl)aniline) nanoflowers (PSANFLs) and Poly(N-(sulfophenyl)aniline) nanofibers/titanium dioxide nanoparticles ((PSANFs/TiO2NPs) by a solid-state mechano-chemical reaction and template-free method and use them in hybrid solar cell. Also, our second aim was to increase the solubility and the processability of conjugated nanomaterials in water through polar functionalized materials. poly[N-(4-sulfophenyl)aniline] is easily soluble in water because of the presence of polar groups of sulfonic acid in the polymer chain. Materials/Methods: Iron (III) chloride hexahydrate (FeCl3∙6H2O) were bought from Merck Millipore Company. Titanium oxide nanoparticles (TiO2, <20 nm, anatase) and Sodium diphenylamine-4-sulfonate (99%) were bought from Sigma-Aldrich Company. Titanium dioxide nanoparticles paste (PST-20T) was prepared from Sharifsolar Co. Conductive glasses coated with indium tin oxide (ITO) were bought from Xinyan Technology Co (China). For the first time we used the solid-state mechano-chemical reaction and template-free method to synthesize Poly(N-(sulfophenyl)aniline) nanoflowers. Moreover, for the first time we used the same technique to synthesize nanocomposite of Poly(N-(sulfophenyl)aniline) nanofibers and titanium dioxide nanoparticles (PSANFs/TiO2NPs) also for the first time this nanocomposite was synthesized. Examining the results of electrochemical calculations energy gap obtained by CV curves and UV–vis spectra demonstrate that PSANFs/TiO2NPs nanocomposite is a p-n type material that can be used in photovoltaic cells. Doctor blade method was used to creat films for three kinds of hybrid solar cells in terms of different patterns like ITO│TiO2NPs│Semiconductor sample│Al. In the following, hybrid photovoltaic cells in bilayer and bulk heterojunction structures were fabricated as ITO│TiO2NPs│PSANFLs│Al and ITO│TiO2NPs│PSANFs /TiO2NPs│Al, respectively. Fourier-transform infrared spectra, field emission scanning electron microscopy (FE-SEM), ultraviolet-visible spectra, cyclic voltammetry (CV) and electrical conductivity were the analysis that used to characterize the synthesized samples. Results and Conclusions: FE-SEM images clearly demonstrate that the morphology of the synthesized samples are nanostructured (nanoflowers and nanofibers). Electrochemical calculations of band gap from CV curves demonstrated that the forbidden band gap of the PSANFLs and PSANFs/TiO2NPs nanocomposite are 2.95 and 2.23 eV, respectively. I–V characteristics of hybrid solar cells and their power conversion efficiency (PCE) under 100 mWcm−2 irradiation (AM 1.5 global conditions) were measured that The PCE of the samples were 0.30 and 0.62%, respectively. At the end, all the results of solar cell analysis were discussed. To sum up, PSANFLs and PSANFLs/TiO2NPs were successfully synthesized by an affordable and straightforward mechanochemical reaction in solid-state under the green condition. The solubility and processability of the synthesized compounds have been improved compared to the previous work. We successfully fabricated hybrid photovoltaic cells of synthesized semiconductor nanostructured polymers and TiO2NPs as different architectures. We believe that the synthesized compounds can open inventive pathways for the development of other Poly(N-(sulfophenyl)aniline based hybrid materials (nanocomposites) proper for preparing new generation solar cells.

Keywords: mechanochemical synthesis, PSANFLs, PSANFs/TiO2NPs, solar cell

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Authors: Katerina Zaharieva, Vicente Rives, Martin Tsvetkov, Raquel Trujillano, Boris Kunev, Ivan Mitov, Maria Milanova, Zara Cherkezova-Zheleva

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The nanostructured cobalt ferrite-type materials Sample A - Co0.25Fe2.75O4, Sample B - Co0.5Fe2.5O4, and Sample C - CoFe2O4 were prepared by co-precipitation in our previous investigations. The co-precipitated Sample B and Sample C were mechanochemically activated in order to produce Sample D - Co0.5Fe2.5O4 and Sample E- CoFe2O4. The PXRD, Moessbauer and FTIR spectroscopies, specific surface area determination by the BET method, thermal analysis, element chemical analysis and temperature-programmed reduction were used to investigate the prepared nano-sized samples. The changes of the Malachite green dye concentration during reaction of the photocatalytic decolorization using nanostructured cobalt ferrite-type catalysts with different chemical composition are included. The photocatalytic results show that the increase in the degree of incorporation of cobalt ions in the magnetite host structure for co-precipitated cobalt ferrite-type samples results in an increase of the photocatalytic activity: Sample A (4 х10-3 min-1) < Sample B (5 х10-3 min-1) < Sample C (7 х10-3 min-1). Mechanochemically activated photocatalysts showed a higher activity than the co-precipitated ferrite materials: Sample D (16 х10-3 min-1) > Sample E (14 х10-3 min-1) > Sample C (7 х10-3 min-1) > Sample B (5 х10-3 min-1) > Sample A (4 х10-3 min-1). On decreasing the degree of substitution of iron ions by cobalt ones a higher sorption ability of the dye after the dark period for the co-precipitated cobalt ferrite materials was observed: Sample C (72 %) < Sample B (78 %) < Sample A (80 %). Mechanochemically treated ferrite catalysts and co-precipitated Sample B possess similar sorption capacities, Sample D (78 %) ~ Sample E (78 %) ~ Sample B (78 %). The prepared nano-sized cobalt ferrite-type materials demonstrate good photocatalytic and sorption properties. Mechanochemically activated Sample D - Co0.5Fe2.5O4 (16х10-3 min-1) and Sample E-CoFe2O4 (14х10-3 min-1) possess higher photocatalytic activity than that of the most common used UV-light catalyst Degussa P25 (12х10-3 min-1). The dependence of the photo-catalytic activity and sorption properties on the preparation method and different degree of substitution of iron ions by cobalt ions in synthesized cobalt ferrite samples is established. The mechanochemical activation leads to formation of nano-structured cobalt ferrite-type catalysts (Sample D and Sample E) with higher rate constants than those of the ferrite materials (Sample A, Sample B, and Sample C) prepared by the co-precipitation procedure. The increase in the degree of substitution of iron ions by cobalt ones leads to improved photocatalytic properties and lower sorption capacities of the co-precipitated ferrite samples. The good sorption properties between 72 and 80% of the prepared ferrite-type materials show that they could be used as potential cheap absorbents for purification of polluted waters.

Keywords: nanodimensional cobalt ferrites, photocatalyst, synthesis, mechanochemical activation

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Authors: Katerina Zaharieva, Katya Milenova, Zara Cherkezova-Zheleva, Alexander Eliyas, Boris Kunev, Ivan Mitov

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The synthesized nanosized manganese ferrite-type of samples have been tested as photocatalysts in the reaction of oxidative degradation of model contaminant Reactive Black 5 (RB5) dye in aqueous solutions under UV irradiation. As it is known this azo dye is applied in the textile-coloring industry and it is discharged into the waterways causing pollution. The co-precipitation procedure has been used for the synthesis of manganese ferrite-type of materials: Sample 1 - Mn0.25Fe2.75O4, Sample 2 - Mn0.5Fe2.5O4 and Sample 3 - MnFe2O4 from 0.03M aqueous solutions of MnCl2•4H2O, FeCl2•4H2O and/or FeCl3•6H2O and 0.3M NaOH in appropriate amounts. The mechanochemical activation of co-precipitated ferrite-type of samples has been performed in argon (Samples 1 and 2) or in air atmosphere (Sample 3) for 2 hours at a milling speed of 500 rpm. The mechano-chemical treatment has been carried out in a high energy planetary ball mill type PM 100, Retsch, Germany. The mass ratio between balls and powder was 30:1. As a result mechanochemically activated Sample 4 - Mn0.25Fe2.75O4, Sample 5 - Mn0.5Fe2.5O4 and Sample 6 - MnFe2O4 have been obtained. The synthesized manganese ferrite-type photocatalysts have been characterized by X-ray diffraction method and Moessbauer spectroscopy. The registered X-ray diffraction patterns and Moessbauer spectra of co-precipitated ferrite-type of materials show the presence of manganese ferrite and additional akaganeite phase. The presence of manganese ferrite and small amounts of iron phases is established in the mechanochemically treated samples. The calculated average crystallite size of manganese ferrites varies within the range 7 – 13 nm. This result is confirmed by Moessbauer study. The registered spectra show superparamagnetic behavior of the prepared materials at room temperature. The photocatalytic investigations have been made using polychromatic UV-A light lamp (Sylvania BLB, 18 W) illumination with wavelength maximum at 365 nm. The intensity of light irradiation upon the manganese ferrite-type photocatalysts was 0.66 mW.cm-2. The photocatalytic reaction of oxidative degradation of RB5 dye was carried out in a semi-batch slurry photocatalytic reactor with 0.15 g of ferrite-type powder, 150 ml of 20 ppm dye aqueous solution under magnetic stirring at rate 400 rpm and continuously feeding air flow. The samples achieved adsorption-desorption equilibrium in the dark period for 30 min and then the UV-light was turned on. After regular time intervals aliquot parts from the suspension were taken out and centrifuged to separate the powder from solution. The residual concentrations of dye were established by a UV-Vis absorbance single beam spectrophotometer CamSpec M501 (UK) measuring in the wavelength region from 190 to 800 nm. The photocatalytic measurements determined that the apparent pseudo-first-order rate constants calculated by linear slopes approximating to first order kinetic equation, increase in following order: Sample 3 (1.1х10-3 min-1) < Sample 1 (2.2х10-3 min-1) < Sample 2 (3.3 х10-3 min-1) < Sample 4 (3.8х10-3 min-1) < Sample 6 (11х10-3 min-1) < Sample 5 (15.2х10-3 min-1). The mechanochemically activated manganese ferrite-type of photocatalyst samples show significantly higher degree of oxidative degradation of RB5 dye after 120 minutes of UV light illumination in comparison with co-precipitated ferrite-type samples: Sample 5 (92%) > Sample 6 (91%) > Sample 4 (63%) > Sample 2 (53%) > Sample 1 (42%) > Sample 3 (15%). Summarizing the obtained results we conclude that the mechanochemical activation leads to a significant enhancement of the degree of oxidative degradation of the RB5 dye and photocatalytic activity of tested manganese ferrite-type of catalyst samples under our experimental conditions. The mechanochemically activated Mn0.5Fe2.5O4 ferrite-type of material displays the highest photocatalytic activity (15.2х10-3 min-1) and degree of oxidative degradation of the RB5 dye (92%) compared to the other synthesized samples. Especially a significant improvement in the degree of oxidative degradation of RB5 dye (91%) has been determined for mechanochemically treated MnFe2O4 ferrite-type of sample with the highest extent of substitution of iron ions by manganese ions than in the case of the co-precipitated MnFe2O4 sample (15%). The mechanochemically activated manganese ferrite-type of samples show good photocatalytic properties in the reaction of oxidative degradation of RB5 azo dye in aqueous solutions and it could find potential application for dye removal from wastewaters originating from textile industry.

Keywords: nanostructured manganese ferrite-type materials, photocatalytic activity, Reactive Black 5, water treatment

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Authors: Ahmed Metawea, Rodrigo Soto, Majeida Kharejesh, Gavin Walker, Ahmad B. Albadarin

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In this study, towards a green approach, we have investigated the effect of operating conditions of solvent assessed twin-screw extruder (TSE) for the production of 4, 4-bipyridine (1-dimensional coordinated polymer (1D)) based coordinated polymer using cobalt nitrate as a metal precursor with molar ratio 1:1. Different operating parameters such as solvent percentage, screw speed and feeding rate are considered. The resultant product is characterized using offline characterization methods, namely Powder X-ray diffraction (PXRD), Raman spectroscopy and scanning electron microscope (SEM) in order to investigate the product purity and surface morphology. A lower feeding rate increased the product’s quality as more resident time was provided for the reaction to take place. The most important influencing factor was the amount of liquid added. The addition of water helped in facilitating the reaction inside the TSE by increasing the surface area of the reaction for particles

Keywords: MOFS, multivariate analysis, process optimization, chemometric

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Authors: Srinivasa Reddy Mallampati, Byoung Ho Lee, Yoshiharu Mitoma, Simion Cristian

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In recent years, environmental nanotechnology has risen to the forefront and the new properties and enhanced reactivates offered by nanomaterial may offer a new, low-cost paradigm to solving complex environmental pollution problems. This study assessed the synthesis and application of multi-functioned nano-size metallic calcium (nMC) composite for detoxification of hazardous inorganic (heavy metals (HMs)/organic chlorinated/brominated compound (CBCs) contaminants in automobile shredder residue (ASR). ASR residues ball milled with nMC composite can achieve about 90-100% of HMs immobilization and CBCs decomposition. The results highlight the low quantity of HMs leached from ASR residues after treatment with nMC, which was found to be lower than the standard regulatory limit for hazardous waste landfills. The use of nMC composite in a mechanochemical process to treat hazardous ASR (dry conditions) is a simple and innovative approach to remediate hazardous inorganic/organic cross-contaminates in ASR.

Keywords: nano-sized metallic calcium, automobile shredder residue, organic/inorganic contaminants, immobilization, detoxification

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Authors: Meltem Bolluk, Ismail Duman

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Boron exhibits the properties of high melting temperature (2273K to 2573 K), high hardness (Mohs: 9,5), low density (2,340 g/cm3), high chemical resistance, high strength, and semiconductivity (band gap:1,6-2,1 eV). These superior properties enable to use it in several high-tech areas from electronics to nuclear industry and especially in high temperature metallurgy. Amorphous boron and crystalline boron have different application areas. Amorphous boron powder (directly amorphous and/or α-rhombohedral) is preferred in rocket firing, airbag inflating and in fabrication of superconducting MgB2 wires. The conventional ways to produce elemental boron with a purity of 85 pct to 95 prc are metallothermic reduction, fused salt electrolysis and mechanochemical synthesis; but the only way to produce high-purity boron powders is Chemical Vapour Deposition (Hot Surface CVD). In this study; amorphous boron powders with a minimum purity of 99,9 prc were synthesized in quartz tubes using BCl3-H2 gas mixture by CVD. Process conditions based on temperature and gas flow rate were determined. Thermodynamical interpretation of BCl3-H2 system for different temperatures and molar rates were performed using Fact Sage software. The characterization of powders was examined by using Xray diffraction (XRD), Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM), Stereo Microscope (SM), Helium gas pycnometer analysis. The purities of final products were determined by titration after lime fusion.

Keywords: amorphous boron, CVD, powder production, powder characterization

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Authors: Maninderjeet K. Grewal, Sakshi Bhatnor, Renu Chadha

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The composition of pharmaceutical entities and the molecular interactions can be altered to optimize drug properties such as solubility and bioavailability by the crystal engineering technique. The present work has emphasized on the preparation, characterization, and biopharmaceutical evaluation of co-crystal of BCS Class II anti-osteoarthritis drug, Oxaprozin (OXA) with aspartic acid (ASPA) as co-former. The co-crystals were prepared through the mechanochemical solvent drop grinding method. Characterization of the prepared co-crystal (OXA-ASPA) was done by using analytical tools such as differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FT-IR), powder X-ray diffraction (PXRD). DSC thermogram of OXA-ASPA cocrystal showed a single sharp melting endotherm at 235 ºC, which was between the melting peaks of the drug and the counter molecules suggesting the formation of a new phase which is a co-crystal that was further confirmed by using other analytical techniques. FT-IR analysis of OXA-ASPA cocrystal showed a shift in a hydroxyl, carbonyl, and amine peaks as compared to pure drugs indicating all these functional groups are participating in cocrystal formation. The appearance of new peaks in the PXRD pattern of cocrystals in comparison to individual components showed that a new crystalline entity has been formed. The Crystal structure of cocrystal was determined using material studio software (Biovia) from PXRD. The equilibrium solubility study of OXA-ASPA showed improvement in solubility as compared to pure drug. Therefore, it was envisioned to prepare the co-crystal of oxaprozin with a suitable conformer to modulate its physiochemical properties and consequently, the biopharmaceutical parameters.

Keywords: cocrystals, coformer, oxaprozin, solubility

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Authors: Adishirin Mammadov

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Polymers and polymer composites play vital roles in diverse industries, including food and beverage packaging, transportation innovations, and medical advancements. However, the advancements in polymer technology bring certain risks, particularly concerning water and soil pollution due to the presence of polymers. The creation of new polymers is a critical aspect of this field. While the primary focus is on improving their physical and chemical properties, ensuring their ecological compatibility is equally important. An advanced method for developing innovative polymer types involves integrating fillers with diverse characteristics, offering advantages such as cost reduction and improved quality indicators. In the conducted research, efforts were made to enhance environmental aspects by employing waste fillers. Specifically, low-density polyethylene (LDPE) was used as the polymer, and waste from cocoon factories was chosen as the filler. Following a process of cleaning, drying, and crushing the filler to specific dimensions, it was incorporated into polyethylene through a mechanical-chemical method under laboratory conditions. The varied rheological properties of the resulting polyethylene compositions examined at temperatures ranging from 145 to 165 degrees Celsius. These compositions demonstrated different rheological properties at various temperature intervals. Achieving homogeneity in the obtained compositions is crucial in the polymers mechanochemical process. Beyond rheological properties, swelling rates in different environments and percentages of mass loss at different temperatures learned using the differential thermal analysis method. The research revealed that, to a certain extent, the physico-chemical properties of polyethylene were not significantly affected by the polymer compositions. This suggests that incorporating cocoon waste enables cost reduction in composite production while positively impacting the environment.

Keywords: polyethylene, polymer, composites, filler, reology

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Authors: Karen L. Rincon-Granados, América R. Vázquez-Olmos, Adriana-Patricia Rodríguez-Hernández, Gina Prado-Prone, Margarita Rivera, Roberto Y. Sato-Berrú

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In this work, a hybrid film based on poly-3-hydroxybutyrate (P3HB) and nickel ferrite (NiFe₂O₄) nanoparticles (NPs) was obtained by a simple and reproducible methodology in order to study its antibacterial and cytotoxic properties. The motivation for this research is the current antimicrobial resistance (RAM). This is a threat to human health and development worldwide. RAM is caused by the emergence of bacterial strains resistant to traditional antibiotics that were used as treatment. Due to this, the need to investigate new alternatives for preventing and treating bacterial infections emerges. In this sense, metal oxide NPs have aroused great interest due to their unique physicochemical properties. However, their use is limited by the nanostructured nature, commonly obtained by chemical and physical synthesis methods, as powders or colloidal dispersions. Therefore, the incorporation of nanostructured materials in polymer matrices to obtain hybrid materials that allow disinfecting and preventing the spread of bacteria on various surfaces. Accordingly, this work presents the synthesis and study of the antibacterial properties of the P3HB@NiFe₂O₄ hybrid film as a potential material to inhibit bacterial growth. The NiFe₂O₄ NPs were previously synthesized by a mechanochemical method. The P3HB and P3HB@NiFe₂O₄ films were obtained by the solvent casting method. The films were characterized by X-ray diffraction (XRD), Raman scattering, and scanning electron microscopy (SEM). The XRD pattern showed that the NiFe₂O₄ NPs were incorporated into the P3HB polymer matrix and retained their nanometric sizes. By energy dispersive X-ray spectroscopy (EDS), it was observed that the NPs are homogeneously distributed in the film. The bactericidal effect of the films obtained was evaluated in vitro using the broth surface method against two opportunistic and nosocomial pathogens, Staphylococcus aureus and Pseudomonas aeruginosa. The bacterial growth results showed that the P3HB@NiFe₂O₄ hybrid film was inhibited by 97% and 96% for S. aureus and P. aeruginosa, respectively. Surprisingly, the P3HB film inhibited both bacterial strains by around 90%. The cytotoxicity of the NiFe₂O₄ NPs, P3HB@NiFe₂O₄ hybrid film, and the P3HB film was evaluated using human skin cells, keratinocytes, and fibroblasts, finding that the NPs are biocompatible. The P3HB film and hybrids are cytotoxic, which demonstrated that although P3HB is known and reported as a biocompatible polymer, under our work conditions, P3HB was cytotoxic. Its bactericidal effect could be related to this activity. Its films are bactericidal and cytotoxic to keratinocytes and fibroblasts, the first barrier of human skin. Despite this, the hybrid film of P3HB@NiFe₂O₄ presents synergy with the bactericidal effect between P3HB and NPs, increasing bacterial inhibition. In addition, NPs decrease the cytotoxicity of P3HB to keratinocytes. The methodology used in this work was successful in producing hybrid films with antibacterial activity. However, future challenges are generated to find relationships between NPs and P3HB that allow taking advantage of their bactericidal properties and do not compromise biocompatibility.

Keywords: poly-3-hydroxybutyrate, nanoparticles, hybrid film, antibacterial

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Authors: Laura Kocsor, Laszlo Peter, Laszlo Kovacs, Zsolt Kis

Abstract:

The aim of our research is to prepare rare-earth-doped lithium niobate (LiNbO3) nanocrystals, having only a few dopant ions in the focal point of an exciting laser beam. These samples will be used to achieve individual addressing of the dopant ions by light beams in a confocal microscope setup. One method for the preparation of nanocrystalline materials is to reduce the particle size by mechanical grinding. High-energy ball-milling was used in several works to produce nano lithium niobate. Previously, it was reported that dry high-energy ball-milling of lithium niobate in a shaker mill results in the partial reduction of the material, which leads to a balanced formation of bipolarons and polarons yielding gray color together with oxygen release and Li2O segregation on the open surfaces. In the present work we focus on preparing LiNbO3 nanocrystals by high-energy ball-milling using a Fritsch Pulverisette 7 planetary mill. Every ball-milling process was carried out in zirconia vial with zirconia balls of different sizes (from 3 mm to 0.1 mm), wet grinding with water, and the grinding time being less than an hour. Gradually decreasing the ball size to 0.1 mm, an average particle size of about 10 nm could be obtained determined by dynamic light scattering and verified by scanning electron microscopy. High-energy ball-milling resulted in sample darkening evidenced by optical absorption spectroscopy measurements indicating that the material underwent partial reduction. The unwanted lithium oxide loss decreases the Li/Nb ratio in the crystal, strongly influencing the spectroscopic properties of lithium niobate. Zirconia contamination was found in ground samples proved by energy-dispersive X-ray spectroscopy measurements; however, it cannot be explained based on the hardness properties of the materials involved in the ball-milling process. It can be understood taking into account the presence of lithium hydroxide formed the segregated lithium oxide and water during the ball-milling process, through chemically induced abrasion. The quantity of the segregated Li2O was measured by coulometric titration. During the wet milling process in the planetary mill, it was found that the lithium oxide loss increases linearly in the early phase of the milling process, then a saturation of the Li2O loss can be seen. This change goes along with the disappearance of the relatively large particles until a relatively narrow size distribution is achieved in accord with the dynamic light scattering measurements. With the 3 mm ball size and 1100 rpm rotation rate, the mean particle size achieved is 100 nm, and the total Li2O loss is about 1.2 wt.% of the original LiNbO3. Further investigations have been done to minimize the Li2O segregation during the ball-milling process. Since the Li2O loss was observed to increase with the growing total surface of the particles, the influence of ball-milling parameters on its quantity has also been studied.

Keywords: high-energy ball-milling, lithium niobate, mechanochemical reaction, nanocrystals

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