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1.
Turk J Chem ; 47(2): 436-447, 2023.
Article in English | MEDLINE | ID: mdl-37528933

ABSTRACT

Cu0 NPs supported on tungsten (VI) oxide (WO3) were in situ generated from the reduction of Cu2+ ions during dehydrogenation of dimethylamine borane (DMAB). The Cu0/WO3 NPs displayed tangible catalytic activity in H2 (g) releasing reaction and they were identified by using advanced techniques. Cu0/WO3 NPs were found as active catalyst providing one equiv. H2(g) per mole of DMAB. The results from TEM images display the formation of Cu0 NPs with an average particle size of 4.6 ± 1.0 nm on the surface of WO3. Moreover, Cu0/WO3 NPs with various metal loadings were prepared and tested as catalyst in dehydrogenation reaction to find the optimum metal loading on WO3 support. The highest H2 generation rate was achieved for 4.0% wt. Cu0/WO3 catalyst with TOF value of 39 h-1 in the reaction conditions. Additionally, effect of various catalyst concentration and temperature is discussed on the reaction kinetics for reaction catalyzed by Cu0/WO3 NPs.

2.
J Mech Behav Biomed Mater ; 135: 105454, 2022 11.
Article in English | MEDLINE | ID: mdl-36115175

ABSTRACT

This multidisciplinary study examined sensitively the change in the dynamics of main mechanical performance, stability of crystal structure, crystallinity quality, strength, corrosion resistance, biocompatibility, resistance to structural degradation/separations and mechanical durability features of hydroxyapatite (HAp) biomedical materials based on the fluorine addition and degradation process to guide future medical and dental treatment studies. In the study, the fluorine ions were used to be the dental coating, filling and supporting material for biologically or synthetically produced bone minerals. The general characteristic properties were investigated by means of standard spectroscopic, structural and mechanical analysis methods including RAMAN, SEM-EDS, TEM, Vickers micro-indentation hardness and density measurements. A time dependent release test was performed to evaluate possible fluorine ion release after the degradation process. It was found that the fundamental characteristic properties of HAp biomedical materials are noted to improve with the increase in the fluoride level up to 2% due much more stabilization of HAp crystal system. The combination of RAMAN spectra and powder XRD analyzes indicates that 2% addition level affects positively the formation velocity of characteristic HAP phase. Besides, fluorine doped HAp materials all exhibited the main characteristic peaks after degradation process. This is attributed to the fact that the fluorine ions enabled the hydroxyapatite to enhance the structural quality and stability towards the corrosion environment. However, in case of excess dopant level of 3% the degradation rates were obtained to increase due to higher contribution rate and especially electrostatic interactions. As for the surface morphology examinations, 2% fluorine added HAp with the highest density of 3.0879 g/cm3 was determined to present the superior crystallinity quality (smallest grain size, best smooth surface, honeycomb pattern, regular shaped particles and densest particle distributions through the specimen surface). Conversely, the excess fluorine triggered to increase seriously degree of micro/macro porosity in the surface morphology and microscopic structural problems in the crystal system. Thus, the HAp doped with 3% was the most affected material from the degradation process. Additionally, the fluorine ion values read after the release process were quite far from the value that could cause toxic effects. Lastly, the optimum fluorine addition provides the positive effects on the highest durability, stiffness and mechanical fracture strength properties as a consequence of differentiation in the surface residual compressive stress regions (lattice strain fields), amplification sites and active operable slip systems in the matrix. Hence, the crack propagations prefer to proceed in the transcrystalline regions rather than the intergranular parts. Similarly, it was found that Vickers micro-indentation hardness tests showed that the microhardness parameters increased after the degradation process. All in all, the fluorine addition level of 2% was noted to be good choice to improve the fundamental characteristic properties of hydroxyapatite biomedical materials for heavy-duty musculoskeletal, orthopedic implant, biological and therapeutic applications in medicine and dentistry application fields.


Subject(s)
Durapatite , Fluorine , Biocompatible Materials/chemistry , Durapatite/chemistry , Fluorides , Powders
3.
Turk J Chem ; 46(2): 394-403, 2022.
Article in English | MEDLINE | ID: mdl-38143470

ABSTRACT

The study reports preparation, characterization, and catalytic activity of Pd0/WO3 nanoparticles in H2 evolution from dimethylamine borane (DMAB). The active catalyst called Pd0/WO3 NPs were obtained from the in situ reduction of Pd2+/WO3 precatalyst and tested in H2 releasing from DMAB. Pd0/WO3 NPs were found as remarkable catalysts providing a turnover frequency value of 948.0 h-1 in H2 releasing from DMAB at 60.0 ± 0.5 °C. The results of some advanced analytical techniques reveal that Pd0 NPs show uniform dispersion on the surface of tungsten(VI) oxide (WO3) with 5.85 ± 0.57 nm of particle size. The reducible nature of tungsten(VI) oxide improves the catalytic efficiency of Pd0/WO3 NPs in H2 generation from DMAB. Pd0/WO3 NPs were found as active catalysts even after the 6th run of dehydrogenation reaction. The report also covers the kinetic performance of the catalyst.

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