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Superparamagnetic iron oxide nanoparticles are well known for biomedical applications. The particle size, morphology, surface area, and functionalization are the key parameters that affect their bioactivity properties. Inline to this, the superparamagnetic Fe3O4 nanoparticles were prepared via chemical coprecipitation method with an average particle size of 6 ± 3 nm. The particles were surface-functionalized with chitosan and in-house prepared reduced graphene oxide (rGO) to obtain chitosan-coated Fe3O4 nanoparticles (C-Fe3O4) and rGO-Fe3O4 nanocomposites (G-Fe3O4), respectively. Upon functionalization, the physicochemical properties of the materials were characterized thoroughly using X-ray diffraction, transmission electron microscopy, vibrating sample magnetometer, Raman Spectroscopy, and thermal gravimetric analysis. Furthermore, they have subjected to cytotoxicity assay, agar two-fold broth dilution test, and disc diffusion assay experiments for the determination of cytotoxicity and antibacterial activities. The effect of surface functionalization on their bioactivity was investigated thoroughly. The surface functionalization with chitosan and rGO has enhanced the bioactivity of the Fe3O4 nanoparticles.
The crystal structure of atropine sulfate monohydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Atropine sulfate monohydrate crystallizes in space group P21/n (#14) with a = 19.2948(5), b = 6.9749(2), c = 26.9036(5) Å, β = 94.215(2)°, V = 3610.86(9) Å3, and Z = 4. Each of the two independent protonated nitrogen atoms participates in a strong hydrogen bond to the sulfate anion. Each of the two independent hydroxyl groups acts as a donor in a hydrogen bond to the sulfate anion, but only one of the water molecule hydrogen atoms acts as a hydrogen bond donor to the sulfate anion. The hydrogen bonds are all discrete but link the cations, anion, and water molecule along [101]. Although atropine and hyoscyamine (atropine is racemic hyoscyamine) crystal structures share some features, such as hydrogen bonding and phenyl–phenyl packing, the powder patterns show that the structures are very different. The powder pattern for atropine sulfate monohydrate has been submitted to ICDD for inclusion in the Powder Diffraction File™.
We report the dielectric properties of ACu3Ti4O12 (A = Eu2/3, Tb2/3, and Na1/2Eu1/2) (ACTO) in the frequency range of 40 Hz–2.5 MHz and in the temperature range of 293–473 K. The experimental results show that substituting for Ca improves the loss tangent of CaCu3Ti4O12 (CCTO). Although the dielectric constants largely decrease, they remain at a high level of 103. To identify the observed dielectric performances of ACTO, scanning electron microscopy and complex impedance measurements were conducted. The conducting mechanism for the grain of ACTO was found to be ion jumping rather than electron hopping (for the grain of CCTO). The results show that the decreased dielectric constant may be related to the decreased grain size, the different carrier in the grain, the different grain boundary properties, or a combination of these factors. All these factors are associated with the deficiency of oxygen vacancies in the samples of ACTO. The decreased loss tangent may be due to the increase in the grain boundary resistance.
Thermal stable chloride melts were used as the reaction medium for modifying the chemical composition of complex oxides ensuring a marked improvement of their working properties. This paper discusses the original results of the direct effect of molten KCl–CoCl2 mixtures on the fine Ni4Nb2O9 powders under argon- and oxygen-containing gaseous atmospheres at 500 °C. The initial Ni4Nb2O9 powder and the reaction products were studied in detail using the differential scanning calorimetry, thermogravimetry, x-ray diffractometry, Raman and IR spectroscopies, scanning electron microscopy, energy-dispersive x-ray spectroscopy, chemical analysis, and conductometry which demonstrated clearly the formation of the thermal stable single-phase Ni–Co niobates.
This mini review summarizes recent advances in experimental thermodynamics of metal–organic frameworks (MOFs). Taking advantage of the development in mechanochemistry, near-room temperature solution calorimetry, and low-temperature heat capacity measurements, the energetic landscape, entropy trends, and Gibbs free energy evolutions of MOFs with true polymorphism [Zn(MeIm)2, Zn(EtIm)2, and Zn(CF3Im)2] as framework topology varies were thoroughly explored by integrated calorimetric and computational methodologies. In addition, the formation enthalpies of MOFs with ultrahigh porosity (MOF-177 and UMCM-1) and the simplest structure (metal formates) have been determined. The studies summarized below highlight the complex interplays among interrelated compositional, chemical, and topological (structural) factors in the determination of the thermodynamic parameters of MOFs.
A novel tetragonal B2CO structure (tP16-B2CO), formed by strong covalent sp2–sp3 B–C and B–O bonds, was predicted with aid of an unbiased structure searching method. With the energy lower than those of previously proposed candidates, except oI16-B2CO, tP16-B2CO was identified as the thermodynamic metastable phase for B2CO compound. The elastic matrix and phonon dispersion spectra declare that tP16-B2CO is mechanically and dynamically stable. The electronic band structure calculation at ambient pressure and a series of high pressure has manifested the indirect semiconducting and band gap increases first and then decreases with pressure increases. The calculation of mechanical properties such as hardness and stress–strain relations of tP16 structure revealed its common hard nature with high hardness of 23.19 GPa and anisotropy with the max stress along [001] is far higher than that along [100].
Anatase phase NOx/S6+–TiO2 (x= 0, 1) film with high solar-driven activity has been successfully prepared via electro-assisted oxidation processes. The morphological and structural properties of the film were characterized by scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, and X-ray diffraction, while the optical property was detected by UV-vis-NIR absorption spectroscopy. The results showed that the NOx/S6+–TiO2 film was composed of “flower-like” microvoids structure and displayed broad and strong optical absorption at around 544 and 1500 nm. Transient photocurrent response, photoluminescence spectroscopy, and electrochemical impedance spectroscopy indicated that the generation and separation of photogenerated charges were significantly enhanced under simulated solar irradiation. The NOx/S6+–TiO2 film exhibited excellent photoelectrocatalytic activity for the degradation of methyl orange (MO), and the decoloration rate and TOC removal respectively reached 98.97 and 59.44% at 20 min under solar irradiation. The film still had good stability after reusing ten times. Furthermore, a possible mechanism of photoelectrocatalysis was suggested in MO degradation by using NOx/S6+–TiO2 film.
The extending market of concentrated solar power plants requires high-temperature materials for solar surface receivers that would ideally heat an air coolant beyond 1300 K. This work presents investigation on high-temperature alloys with ceramic coatings (AlN or SiC/AlN stacking) to combine the properties of the substrate (creep resistance, machinability) and coating (slow oxidation kinetics, high solar absorptivity). The first results showed that high-temperature oxidation resistance and optical properties of metallic alloys were improved by the different coatings. However, the fast thermal shocks led to high stress levels not compatible due to the differences in thermal expansion coefficients.
The microstructure contribution to the very low fracture toughness of freestanding metallic thin films was investigated by bulge fracture tests on 200-nm-thick {100} single-crystalline and polycrystalline silver films. The single-crystalline films exhibited a significantly lower fracture toughness value (KIC= 0.88 MPa m1/2) than their polycrystalline counterparts (KIC= 1.45 MPa m1/2), which was rationalized by the observation of an unusual crack initiation behavior—characterized by twinning in front of the notch tip—during in situ testing in the atomic force microscope. Twinning was also observed as a dominant deformation mechanism in atomistic simulations. This twinning tendency is explained by comparing the resolved shear stresses acting on the leading partial dislocation and the full dislocation, which allows to develop a size- and orientation-dependent twinning criterion. The fracture toughness of polycrystalline samples was found to be higher because of the energy dissipation associated with full dislocation plasticity and because of crack meandering along grain boundaries.
In the scope of this work, a micromechanical model based on the crystal plasticity finite element method is proposed and applied to describe the nucleation and growth of microstructurally short fatigue cracks in polycrystalline materials under cyclic loads. The microstructure is generated in the form of a representative volume element of a polycrystalline material with equiaxed grains having columnar structure along thickness and random crystallographic texture. With this model, we investigate the influence of loading amplitude on the crack growth behavior. It is shown that for smaller strain amplitudes, a single crack nucleates and propagates, while for larger strain amplitudes several independent crack nucleation sites form, from which microcracks start propagating. It is also observed that the global plastic strain amplitude decreases from the initial to the final cycle, during total strain-controlled loading. However, this can even increase the crack growth rate because the crack advance is governed by the local plastic slip which accumulates at the crack tip over the number of cycles. With this work, it is shown that micromechanical modeling can strongly improve our understanding of the mechanisms of short-crack nucleation and growth under fatigue loading.
A crucial target in the printed electronics technologies is to realize all-printed thin-film transistors (TFTs), as being applicable to the industry. Here, the authors report printed polymer TFTs through the integration of the SuPR-NaP technique, a promising way for manufacturing ultrafine printed silver electrodes, with printed polymer semiconductor layers. The authors used a class of donor–acceptor-type copolymer, PDVT-10, and found that the devices exhibit excellent TFT characteristics. The devices allow the transfer length method measurements with high accuracy, where the estimated contact resistance is considerably small (4.7 kΩ cm) among the bottom-contact TFTs using printed silver electrodes, with also showing short-channel effects.
Herein, the authors report our pioneering demonstration of the anisotropic thermal properties of black phosphorus (BP) nanoflakes. The nanoflakes were produced using a scotch tape-based mechanical exfoliation technique. Their thickness was characterized using Atomic Force Microscopy The anisotropic direction of the nanoflakes was determined by the Raman Spectroscopy equipped with a polarized laser. Then, a temperature-dependent Raman spectroscopy method was utilized to study the thermal transport properties of the BP nanoflakes. The results indicated that the thermal conductivities of zigzag BP and armchair nanoflakes are 30.6 and 12.6 W/m·K, respectively. This fundamental thermal study gives insight into the future fabrication of nanoscale electronic devices with thermal properties that can be well controlled.
Hot extrusion experiments were conducted on Al–5.50Zn–2.35Mg–1.36Cu (wt%) alloy under various temperatures and extrusion speeds. Results indicated that dynamic recovery occurred at low temperature and then dynamic recrystallization was triggered at higher temperature or speed. High billet temperature reduced the grain size and increased the volume fraction of Al23CuFe4 and AlMgZn. When the extrusion speed was enhanced to 0.5 mm/s, the peak of MgZn2 phase diminished in the results of X-ray diffraction. The strong brass and S components appeared in all the extruded specimens. Texture intensity gradually decreased with increasing temperature and the fraction of texture components was also significantly affected by the extrusion parameters. The extruded alloy exhibited the highest ultimate tensile strength of 350.2 MPa at 480 °C and 0.5 mm/s and the best elongation of 16.78% at 520 °C and 0.1 mm/s. Moreover, the extrusion speed had more significant effects on the tensile properties than that of the temperature.
Polymer redox-active materials (redoxmers) have numerous applications in the emerging electrochemical energy storage systems due to their structural versatility, fast-cycling ability, high theoretical capacity as electrode materials, sustainability, and recyclability. This review examines recent developments in improving the cycling performance of such materials and provides a vista on the future research directions.
Carbonate glasses can be formed routinely in the system K2CO3–MgCO3. The enthalpy of formation for one such 0.55K2CO3–0.45MgCO3 glass was determined at 298 K to be 115.00 ± 1.21 kJ/mol by drop solution calorimetry in molten sodium molybdate (3Na2O·MoO3) at 975 K. The corresponding heat of formation from oxides at 298 K was −261.12 ± 3.02 kJ/mol. This ternary glass is shown to be slightly metastable with respect to binary crystalline components (K2CO3 and MgCO3) and may be further stabilized by entropy terms arising from cation disorder and carbonate group distortions. This high degree of disorder is confirmed by 13C MAS NMR measurement of the average chemical shift tensor values, which show asymmetry of the carbonate anion to be significantly larger than previously reported values. Molecular dynamics simulations show that the structure of this carbonate glass reflects the strong interaction between the oxygen atoms in distorted carbonate anions and potassium cations.
The effect of off-stoichiometry on the microstructures and tensile properties of Ni3Al–Ni3V pseudo-binary alloys was investigated by a scanning electron microscope, a transmission electron microscope, Vickers hardness test, and high-temperature tensile test. As the alloy deviates from a just-stoichiometric composition toward Ni-rich one, the microstructures constituted by two ordered phases, Ni3Al and Ni3V changed to those constituted by two ordered phases, Ni3Al and Ni3V, and one disordered phase, Ni solid solution. Also, the deviation from the stoichiometric composition resulted in a decrease in flow strength as well as Vickers hardness and conversely increase in tensile elongation. Higher tensile elongation in the off-stoichiometric alloys was induced by the transition from intergranular fracturing to transgranular fracturing. The trade-off relation in the yield strength (or hardness) versus tensile elongation curve, which was drawn plotting the data obtained from the alloys with different off-stoichiometric compositions, was most excellent at 600 °C but rapidly became worse at high temperatures beyond 600 °C. It was demonstrated that the deviation to the off-stoichiometric composition in the two-phase Ni3Al–Ni3V pseudo-binary alloy system was a useful alloying parameter to improve the balance of the flow strength and tensile ductility.