High-energy-low-temperature technologies for the synthesis of nanoparticles: Microwaves and high pressure

Microwave Solvothermal Synthesis (MSS) is a chemical technology, where apart from possible effects of microwaves on the chemical reaction paths, microwave heating allows the precise planning of a time-temperature schedule, as well as to achieve high super-saturation of the reagents uniformly in the reactor vessel. Thus, MSS is suitable for production of nanoparticles with small grain size distribution and a high degree of crystallinity. A further advantage of the technology is a much lower synthesis temperature than for gas phase, plasma or sol-gel technologies. New reactors have been developed to exploit these advantages of the MSS technology of nanoparticles synthesis and to scale up the production rate. Reactor design and realization has been shown to be decisive and critical for the control of the MSS technology. Examples of oxidic and phosphatic nanoparticles synthesis have been reported

Microstructure/phase evolution in mechanical alloying/milling of stainless steel and aluminum powder blends

The present study aims to examine the phase evolution in blends comprising different proportions of stainless steel (316SS) and Al (0, 25, 65, and 85 wt pct) powders during high-energy ball milling through X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and high-resolution transmission electron microscopy (HRTEM). An attempt has also been made to study the hardness value of the bulk samples obtained by hot pressing the ball-milled powder blend at suitable temperature and pressure. The results on changes in the constituent phases and hardness value of the bulk samples obtained after consolidation of ball-milled alloy using the high-pressure technique have been reported

Dispersing hydrophilic nanoparticles in hydrophobic polymers: HDPE/ZnO nanocomposites by a novel template-based approach

The efficiency of a novel template-based approach for the dispersion of hydrophilic nanoparticles within hydrophobic polymer matrices is investigated. The procedure envisages the permeation of a well dispersed nanoparticle suspension inside a micro-porous matrix, obtained through selective extraction of a sacrificial phase from a finely interpenetrated co-continuous polymer blend. Specifically, a blend of high density polyethylene (HDPE) and polyethylene oxide (PEO) at 50/50 wt% is prepared by melt mixing. The addition of small amounts of organo-clay promotes the necessary refinement of the blend morphology. Once removed the PEO, the micro-porous HDPE matrix is dipped in a colloidal suspension of zinc oxide nanoparticles which exhibits low interfacial tension with HDPE. A system prepared by traditional melt mixing is used as reference. Melt- and solid-state viscoelastic measurements reveal a good quality of the filler dispersion despite the uneven distribution on micro-scale. The latter can be capitalized to minimize the filler content to attain a certain improvement of the material properties or to design nano-structured polymer composites. © BME-PT

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 8MPa 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 heatingpermits to avoid contact of the reactants with heating elements, and is thus particularly well suited for synthesis of dopednanopowders in high purity conditions. A mixture of ZrO2 particles with tetragonal and monoclinic crystalline phases, about15nm in size, was obtained. The p/T threshold of about 5-6MPa/265–280◦C was necessary to obtain good quality of zirconiapowder. A new method for quantitative description of grain-size distribution was applied, which is based on analysis of the finestructure 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

Improving osteoblasts cells proliferation via femtosecond laser surface modification of 3D-printed poly-ε-caprolactone scaffolds for bone tissue engineering applications

Synthetic polymer biomaterials incorporating cells are a promising technique for treatment of orthopedic injuries. To enhance the integration of biomaterials into the human body, additional functionalization of the scaffold surface should be carried out that would assist one in mimicking the natural cellular environment. In this study, we examined poly-epsilon-caprolactone (PCL) fiber matrices in view of optimizing the porous properties of the constructs. Altering the porosity of a PCL scaffold is expected to improve the material's biocompatibility, thus influencing its osteoconductivity and osteointegration. We produced 3D poly-epsilon-caprolactone (PCL) matrices by a fused deposition modeling method for bone and cartilage tissue engineering and performed femtosecond (fs) laser modification experiments to improve the surface properties of the PCL construct. Femtosecond laser processing is one of the useful tools for creating a vast diversity of surface patterns with reproducibility and precision. The processed surface of the PCL matrix was examined to follow the effect of the laser parameters, namely the laser pulse energy and repetition rate and the number (N) of applied pulses. The modified zones were characterized by scanning electron microscopy (SEM), confocal microscopy, X-ray computed tomography and contact angle measurements. The results obtained demonstrated changes in the morphology of the processed surface. A decrease in the water contact angle was also seen after fs laser processing of fiber meshes. Our work demonstrated that a precise control of material surface properties could be achieved by applying a different number of laser pulses at various laser fluence values. We concluded that the structural features of the matrix remain unaffected and can be successfully modified through laser postmodification. The cells tests indicated that the micro-modifications created induced MG63 and MC3T3 osteoblast cellular orientation. The analysis of the MG63 and MC3T3 osteoblast attachment suggested regulation of cells volume migration

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 215C∘ to 305C∘. 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 15 nm in size, was obtained. The p/T threshold of about 5-6 MPa/265–280C∘ 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

Electrical properties of ZrO₂ in nano- and polycrystalline states at high pressure

We present the results of the research work devoted to the problem: how the crystallites influence the electrical properties of stabilized zirconia at pressures of 22−50 GPa and in the temperature range of 77−450 K. The measurements were conducted in the highpressure chamber under direct current on nanocrystalline powders of ZrO₂ stabilized by Pr (0.5%) and on compact powder samples of «partially stabilized» ZrO₂ including 5% Y₃P₃. The nanocrystallite size equals 10, 12 and 56 nm. The change of electronic properties of stabilized zirconia at 31.5–37.5 GPa, 40–44 GPa and 45.5–48.5 GPa in nano- and polycrystalline states has been discovered. It gives us a possibility to verify the phase diagram of ZrO₂ at those intervals of pressure. Besides, it has been revealed that stabilization as nanocrystallinity leads to appearance of additional mechanisms of conductivity in ZrO₂

White-etching matter in bearing steel. Part II: Distinguishing cause and effect in bearing steel failure

The premature failure of large bearings of the type used in wind turbines, possibly through a mechanism called “white-structure flaking”, has triggered many studies of microstructural damage associated with “white-etching areas” created during rolling contact fatigue, although whether they are symptoms or causes of failure is less clear. Therefore, some special experiments have been conducted to prove that white-etching areas are the consequence, and not the cause, of damage. By artificially introducing a fine dispersion of microcracks in the steel through heat treatment and then subjecting the sample to rolling contact fatigue, manifestations of hard white-etching matter have been created to a much greater extent than samples similarly tested without initial cracks. A wide variety of characterization tools has been used to corroborate that the white areas thus created have the same properties as reported observations on real bearings. Evidence suggests that the formation mechanism of the white-etching regions involves the rubbing and beating of the free surfaces of cracks, debonded inclusions, and voids under repeated rolling contact. It follows that the focus in avoiding early failure should be in enhancing the toughness of the bearing steel in order to avoid the initial microscopic feature event.Funding by CONACyT, the Cambridge Overseas Trust, and the Roberto Rocca Education Programme is highly appreciated and acknowledged.This is the accepted manuscript version. The final published version is available from Springer at http://link.springer.com/article/10.1007%2Fs11661-014-2431-x