The aim of the paper is to explain the mechanism of zinc oxide (ZnO) nanoparticle (NP) size control, which enables the size control of ZnO NPs obtained in microwave solvothermal synthesis (MSS) within the size range between circa 20 and 120 nm through the control of water content in the solution of zinc acetate in ethylene glycol. Heavy water was used in the tests. The mechanism of ZnO NPs size control was explained, discussed and experimentally verified. The discovery and investigation of this mechanism was possible by tracking the fate of water molecules during the whole synthesis process. All the synthesis products were identified. It was indicated that the MSS of ZnO NPs proceeded through the formation and conversion of intermediates such as Zn(OH)(CHCOO) · xHO. Esters and HO were the by-products of the MSS reaction of ZnO NPs. We justified that the esterification reaction is the decisive stage that is a prerequisite of the formation of ZnO NPs. The following parameters of the obtained ZnO NPs and of the intermediate were determined: pycnometric density, specific surface area, phase purity, average particles size, particles size distribution and chemical composition. The ZnO NPs morphology and structure were determined using scanning electron microscopy.
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 (HAp) nanoparticles of tunable diameter were obtained by the precipitation method at room temperature and by microwave hydrothermal synthesis (MHS). The following parameters of the obtained nanostructured HAp were determined: pycnometric density, specific surface area, phase purity, lattice parameters, particle size, particle size distribution, water content, and structure. HAp nanoparticle morphology and structure were determined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). X-ray diffraction measurements confirmed crystalline HAp was synthesized, which was pure in terms of phase. It was shown that by changing the synthesis parameters, the diameter of HAp nanoparticles could be controlled. The average diameter of the HAp nanoparticles was determined by Scherrer’s equation via the Nanopowder XRD Processor Demo web application, which interprets the results of specific surface area and TEM measurements using the dark-field technique. The obtained nanoparticles with average particle diameter ranging from 8–39 nm were characterized by having homogeneous morphology with a needle shape and a narrow particle size distribution. Strong similarities were found when comparing the properties of some types of nanostructured hydroxyapatite with natural occurring apatite found in animal bones and teeth.
Naturally derived prodrugs have a wide range of pharmacological activities, including anticancer, antioxidant, and antiviral effects. However, significant barriers inhibit their use in medicine, e.g. their hydrophobicity. In this comprehensive study, we investigated simple and effective nanoformulations consisting of amine-functionalized and conjugated with folic acid (FA) mesoporous silica nanoparticles (MSNs). Two types of MSNs were studied: KCC- 1, with mean size 324 nm and mean pore diameter 3.4 nm, and MCM - 41, with mean size 197 and pore diameter 2 nm. Both types of MSNs were loaded with three anticancer prodrugs: curcumin, quercetin, and colchicine. The nanoformulations were tested to target in vitro human hepatocellular carcinoma cells (HepG2) and HeLa cancer cells. The amine-functionalized and FA-conjugated curcumin-loaded, especially KCC-1 MSNs penetrated all cells organs and steadily released curcumin. The FA-conjugated MSNs displayed higher cellular uptake, sustained intracellular release, and cytotoxicity effects in comparison to non-conjugated MSNs. The KCC-1 type MSNs carrying curcumin displayed the highest anticancer activity. Apoptosis was induced through specific signaling molecular pathways (caspase-3, H2O2, c-MET, and MCL-1). The nanoformulations displayed also an enhanced antioxidant activity compared to the pure forms of the prodrugs, and the effect depended on the time of release, type of MSN, prodrug, and assay used. FA-conjugated MSNs carrying curcumin and other safe natural prodrugs offer new possibilities for targeted cancer therapy.
Application of the in situ high pressure powder diffraction technique for examination of specific structural properties of nanocrystals based on the experimental data of SiC nanocrystalline powders of 2-30 nm in diameter is presented. Limitations and capabilities of the experimental techniques themselves and methods of diffraction data elaboration applied to nanocrystals with very small dimensions (<30 nm) are discussed. It is shown that a unique value of the lattice parameter cannot be determined for such small crystals using a standard powder diffraction experiment. It is also shown that, due to the complex structure constituting a two-phase, core/surface shell system, no unique compressibility coefficient can satisfactorily describe the behaviour of nanocrystalline powders under pressure. We offer a tentative interpretation of the distribution of macro-and micro-strains in nanoparticles of different grain size.
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