Synthesis of CoFe2O4 nanoparticles embedded in a silica matrix by the citrate precursor technique

A metals–citrate–silica gel was prepared from metallic salts, citric acid and tetraethylorthosilicate by sol–gel method (citrate precursor technique) and it was further used to prepare magnetic nanocomposites. The gel was dried at 100 °C and then calcined at temperatures between 600 and 1000 °C to obtain powder samples. The nanocomposites were characterized by XRD, IR, VSM and TEM techniques. The diffraction patterns show the formation of a single magnetic phase identified as CoFe₂O₄. Magnetic nanoparticles with average size less than 50 nm were obtained which are well dispersed in the silica matrix. The combination of different metals concentrations and calcining temperatures allowed obtaining samples with magnetization ranging from 3.6 to 25.3 emu/g.     

Ionic conductivity of covalently interconnected polyphosphazene–silicate hybrid networks

Silicate sol–gel precursors of poly[bis(methoxyethoxyethoxy)phosphazene] and their corresponding hybrid networks were synthesized by hydrolysis and condensation reactions. Conversion of the precursor polymers to covalently interconnected hybrid networks with controlled morphologies and physical properties was achieved. Thermal analyses showed no melting transitions for the networks and low glass transition temperatures that ranged from approximately − 38 to − 67 °C. Solid solutions with lithium bis(trifluoromethanesulfonyl)amide in the network showed a maximum ionic conductivity value of 7.69 × 10^− 5 S/cm, making these materials interesting candidates for dimensionally stable solid polymer electrolytes.     

Investigation of ionic conduction and mechanical properties of PMMA–PVdF blend-based polymer electrolytes

Polymeric gel electrolytes, based on a blend of poly(methylmethacrylate)/poly(vinylidene fluoride) (PMMA/PVdF), ethylene carbonate/propylene carbonate (EC/PC) as plasticizer and lithium perchlorate as electrolyte, have been studied as a function of the different polymeric ratios to obtain the best compromise between ionic conduction and mechanical properties of the systems involved. Ionic conductivity and the lithium self-diffusion coefficient were measured by the PFG–NMR method, which revealed a maximum of lithium mobility for the composition PMMA 60%–PVdF 40%. The Raman spectroscopic study revealed a change of the interaction between that of the lithium cations and the plasticizer molecules for different PMMA / PVdF ratios. Oscillatory rheological tests have shown better mechanical properties for the intermediate compositions of the blend.     

Theoretical investigation into the low-temperature oxidation of ethylbenzene

The classical topic on the oxidation of alkylbenzene has been revisited via performing accurate theoretical calculations to address the salient features for the initial oxidation of ethylbenzene. Potential energy surfaces are mapped out for all possible reactions in the systems of (1-phenylethyl + O₂ and 2-phenylethyl + O₂). Reaction rate constants at the high-pressure limit are calculated for all possible reactions in these two systems. Direct H abstraction from 1-phenylethyl radical by oxygen molecule appears to be an important route for the formation of styrene from the oxidation of ethylbenzene. Concerted elimination of HO₂ is predicted to contribute significantly the production of styrene from system of 2-phenylethyl + O₂; especially at the atmospheric pressure and intermediate temperatures. Formation of the other major experimental product, benzaldehyde, is attributed to the unimolecular decomposition of C₆H₅CH₂(O)CH₃ rather than to unimolecular isomerisation of the two initial peroxy adducts. Kinetic and mechanistic data presented herein are instrumental for better understanding of the oxidative decomposition of ethylbenzene, i.e., major constituents of commonly formulated fuel surrogates.     

Rare-earth doped (Lu0.85Y0.15)2SiO5 nanocrystalline powders obtained by polymer assisted sol–gel synthesis

In the present work we explored the possibility of obtaining nanocrystalline (Lu_0.85Y_0.15)₂SiO₅ (LYSO) powders using polymer assisted sol–gel method. The synthesis started from TEOS as alkoxide precursor while polyethylene glycol with average molecular weight of 4000 was used as fuel. The resulting powders were obtained by firing gels in two ways: in conventional furnace and in microwave oven, with further annealing. This modified sol–gel synthetic route enabled production of pure phase LYSO powders at much lower temperatures (1050 °C) compared to classical, -solid-state methods (1400 °C). Crystallization kinetics are examined using differential thermal analysis, and rather low values of crystallization activation energies (around 12 kJ/mol) were found, revealing good potential of this method for low-temperature production of LYSO powder.     

Infrared absorption cross sections for methanol

Infrared absorption cross sections for methanol, CH₃OH, have been determined near 3.4 and 10 μm from spectra recorded using a high-resolution FTIR spectrometer (Bruker IFS 125HR) and a multipass cell with a maximum optical path length of 19.3 m. Methanol/dry synthetic air mixtures were prepared and spectra were recorded at 0.015 cm^?1 resolution (calculated as 0.9/MOPD) at a number of temperatures and pressures (50–760 Torr and 204–296 K) appropriate for atmospheric conditions. Intensities were calibrated using composite methanol spectra taken from the Pacific Northwest National Laboratory (PNNL) IR database. The new measurements in the 10 μm region indicate problems with the existing methanol spectroscopic line parameters in the HITRAN database, which will impact the accuracy of satellite retrievals.     

Three-dimensional black-blood T2 mapping with compressed sensing and data-driven parallel imaging in the carotid artery

PurposeTo develop a 3D black-blood T₂ mapping sequence with a combination of compressed sensing (CS) and parallel imaging (PI) for carotid wall imaging.Materials and methodsA 3D black-blood fast-spin-echo (FSE) sequence for T₂ mapping with CS and PI was developed and validated. Phantom experiments were performed to assess T₂ accuracy using a Eurospin Test Object, with different combination of CS and PI acceleration factors. A 2D multi-echo FSE sequence was used as a reference to evaluate the accuracy. The concordance correlation coefficient and Bland-Altman statistics were calculated. Twelve volunteers were scanned twice to determine the repeatability of the sequence and the intraclass correlation coefficient (ICC) was reported. Wall-lumen sharpness was calculated for different CS and PI combinations. Six patients with carotid stenosis > 50% were scanned with optimised sequence. The T₂ maps were compared with multi-contrast images.ResultsPhantom scans showed good correlation in T₂ measurement between current and reference sequence (r = 0.991). No significant difference was found between different combination of CS and PI accelerations (p = 0.999). Volunteer scans showed good repeatability of T₂ measurement (ICC: 0.93, 95% CI 0.84–0.97). The mean T₂ of the healthy wall was 48.0 ± 9.5 ms. Overall plaque T₂ values from patients were 54.9 ± 12.2 ms. Recent intraplaque haemorrhage and fibrous tissue have higher T₂ values than the mean plaque T₂ values (88.1 ± 6.8 ms and 62.7 ± 9.3 ms, respectively).ConclusionThis study demonstrates the feasibility of combining CS and PI for accelerating 3D T₂ mapping in the carotid artery, with accurate T₂ measurements and good repeatability.     

Growth-induced perpendicular magnetic anisotropy and clustering in NixPt1−x alloys

Polycrystalline and epitaxial (1 0 0), (1 1 0), and (1 1 1)-oriented Ni₃Pt, NiPt, and NiPt₃ films were deposited over a range of growth temperatures from 80°C to 700°C. Films grown at moderate temperatures (200–400°C) exhibit growth-induced properties similar to Co–Pt alloys: enhanced and broadened Curie temperature, perpendicular magnetic anisotropy and large coercivity. As in Co–Pt, the magnetic properties suggest a clustering of Ni into platelets on the growth surface, as the films are being grown. Unlike Co–Pt, however, NiPt films exhibit a strong orientational dependence of anisotropy and enhanced Curie temperature, possibly resulting from different types of surface reconstructions which affect the growth surface.     

Preparation of proton conductive composites with CsHSO4/CsH2PO4 and phosphosilicate gel

New composite materials were prepared using cesium hydrogen sulfate (CsHSO₄) or cesium dihydrogen phosphate (CsH₂PO₄) and phosphosilicate gel (P₂O₅–SiO₂ gel). In X-ray diffraction patterns of these composites, diffraction peaks due to Cs₂H₅(SO₄)₂(PO₄) and CsH₅(PO₄)₂ were observed for CsHSO₄–(P₂O₅–SiO₂ gel) composites and CsH₂PO₄–(P₂O₅–SiO₂ gel) composites, respectively. These composites showed high conductivities in the order of 10^− 3 S cm^− 1 at 150 °C due to melting of Cs₂H₅(SO₄)₂(PO₄) or CsH₅(PO₄)₂ in the composites. In the cooling process, the CsHSO₄–(P₂O₅–SiO₂ gel) composites kept relatively high conductivity to 110 °C where solidification of Cs₂H₅(SO₄)₂(PO₄) occurs, whereas CsH₂PO₄–(P₂O₅–SiO₂ gel) composites showed relatively high conductivity continuously to ambient temperature.     

Effect of nanosize titanium oxide on electrochemical characteristics of activated carbon electrodes

Energy-storage composite electrodes were prepared by mixing activated carbons (ACs) modified with nanosize titanium oxide (TiO₂) through ultrasonic vibration in ethanol solution for 30 min. We examined the cyclic voltammetry of the composite electrodes in an aqueous electrolyte, 1 M H₂SO₄. It was found that the specific capacitance of the composite electrodes measured in a range of 0–0.8 V was increased from 100 to 155 F/g compared electrodes comprised of ACs only. This was attributed to a reduction of polarization of the ACs modified by nanosized TiO₂.     

Rapid ultrasound-assisted magnetic microextraction of gallic acid from urine,plasma and water samples by HKUST-1-MOF-Fe3O4-GA-MIP-NPs: UV–vis detection and optimization study

Magnetite (Fe₃O₄ nanoparticles (NPs)) HKUST-1 metal organic framework (MOF) composite as a support was used for surface imprinting of gallic acid imprinted polymer (HKUST-1-MOF-Fe₃O₄-GA-MIP) using vinyltrimethoxysilane (VTMOS) as the cross-linker. Subsequently, HKUST-1-MOF-Fe₃O₄-NPs-GA-MIP characterized by FT-IR, XRD and FE-SEM analysis and applied for fast and selective and sensitive ultrasound assisted dispersive magnetic solid phase microextraction of gallic acid (GA) by UV–Vis (UA-DMSPME-UV-Vis) detection method. Plackett–Burman design (PBD) and central composite design (CCD) according to desirability function (DF) indicate the significant variables among the extraction factors vortex (mixing) time (min), sonication time (min), temperature (°C), eluent volume (L), pH and HKUST-1-MOF-Fe₃O₄-NPs-GA-MIP mass (mg) and their contribution on the response. Optimum conditions and values correspond to pH, HKUST-1-MOF-Fe₃O₄-NPs-GA-MIP mass, sonication time and the eluent volume were set as follow 3.0, 1.6 mg, 4.0 min and 180 μL, respectively. The average recovery (ER%) of GA was 98.13% with desirability of 0.997, while the present method has best operational performance like wide linear range 8–6000 ng mL⁻¹ with a Limit of detection (LOD) of 1.377 ng mL⁻¹, limit of quantification (LOQ) 4.591 ng mL⁻¹ and precision (<3.50% RSD). The recovery of GA in urine, human plasma and water samples within the range of 92.3–100.6% that strongly support high applicability of present method for real samples analysis, which candidate this method as promise for further application.     

Spray pyrolyzed NiO–C nanocomposite as an anode material for the lithium-ion battery with enhanced capacity retention

NiO–C nanocomposite was prepared by a spray pyrolysis method using a mixture of Ni(NO₃)₂ and citric acid solution at 600 °C. The microstructure and morphology of the NiO–C composite were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS) mapping, and thermogravimetric analysis (TGA). The results showed that the NiO nanoparticles were surrounded by amorphous carbon. Electrochemical tests demonstrated that the NiO–C nanocomposites exhibited better capacity retention (382 mAh g^− 1 for 50 cycles) than that of pure NiO (141 mAh g^− 1 for 50 cycles), which was also prepared by spray pyrolysis using only Ni(NO₃)₂ as precursor. The enhanced capacity retention can be mainly attributed to the NiO–C composite structure, composed of NiO nanoparticles surrounded by carbon, which can accommodate the volume changes during charge–discharge and improve the electrical conductivity between the NiO nanoparticles.     

Ionic and electronic conductivities,stability and thermal expansion of La10 − x(Si,Al)6O26 ± δ solid electrolytes

Apatite-type La_10 − xSi_6 − yAl_yO_{27 − 3x/2 − y/2} (x = 0–0.33; y = 0.5–1.5) exhibit predominant oxygen ionic conductivity in a wide range of oxygen partial pressures. The conductivity of silicates containing 26.50–26.75 oxygen atoms per formula unit is comparable to that of gadolinia-doped ceria at 770–870 K. The average thermal expansion coefficients are (8.7–10.8) × 10^− 6 K^− 1 at 373–1273 K. At temperatures above 1100 K, silicon oxide volatilization from the surface layers of apatite ceramics and a moderate degradation of the ionic transport with time are observed under reducing conditions, thus limiting the operation temperature of Si-containing solid electrolytes.     

Ultrasound assisted combined molecularly imprinted polymer for selective extraction of nicotinamide in human urine and milk samples: Spectrophotometric determination and optimization study

Ultrasound-assisted dispersive solid phase microextraction followed by UV–vis spectrophotometer (UA-DSPME-UV–vis) was designed for extraction and preconcentration of nicotinamide (vitamin B₃) by HKUST-1 metal organic framework (MOF) based molecularly imprinted polymer (MIP). This new material was characterized by FTIR and FE-SEM techniques. The preliminary Plackett–Burman design was used for screening and subsequently the central composite design justifies significant terms and possible construction of mathematical equation which give the individual and cooperative contribution of variables like HKUST-1-MOF-NA-MIP mass, sonication time, temperature, eluent volume, pH and vortex time. Accordingly the optimum condition was set as: 2.0 mg HKUST-1-MOF-NA-MIP, 200 μL eluent and 5.0 min sonication time in center points other variables were determined as the best conditions to reach the maximum recovery of the analyte. The UA-DSPME-UV–vis method performances like excellent linearity (LR), limits of detection (LOD), limits of quantification of 10–5000 μg L⁻¹ with R² of 0.99, LOD (1.96 ng mL⁻¹), LOQ (6.53 μg L⁻¹), respectively show successful and accurate applicability of the present method for monitoring analytes with within- and between-day precision of 0.96–3.38%. The average absolute recoveries of the nicotinamide extracted from the urine, milk and water samples were 95.85–101.27%.     

Dielectric and piezoelectric properties of PZT–silica fume cement composites

PZT–silica fume cement (PZT–SFC) composites were produced using PZT (at 50% and 60% by volume) and silica fume cement (cement containing silica fume of 5% and 10% by weight). PZT–Portland cement with no silica fume was also produced to allow comparison of the results. Dielectric constants of PZT–SFC composites are found to be higher than that of PZT–PC composite where ε_r value was found to increase with increasing SF content (ε_r values of composite with SF at 0%, 5% and 10% are 117, 125 and 178, respectively). PZT–SFC composites were successfully poled and d₃₃ results of PZT–SFC composites (d₃₃ = 18 pC/N) were found to be marginally higher than that of PZT–PC composite (d₃₃ = 17 pC/N). SEM micrograph also shows a dense matrix of SFC hydration product surrounding the PZT particles. From the results, these PZT–SFC composites are therefore promising materials for use in structural applications and should be ideal for high strength structures where SFC is used in the host structure.     

Low-cost micro-lens arrays fabricated by photosensitive sol–gel and multi-beam laser interference

In this paper, we introduce a low-cost approach for fabricating micro-lens arrays that is based on photosensitive sol–gel and multi-beam laser interference. UV photosensitive ZrO₂ gel films are prepared with Zr(O(CH₂)₃CH₃)₄ and BzAcH as the precursor and chemical modifier, respectively. With UV laser irradiation via different dose, nonlinear photodecomposition occurs in this film. Large scale 2D micro lens arrays with the sizes of 830 nm × 830 nm and 280 nm × 280 nm are fabricated by four-beam laser interference. The surface profile modeling shows that the micro lens is plano convex lens, and the effective focal lengths are 812.0 nm and 317.6 nm, respectively.     

Sonoluminescence quenching and cavitation bubble temperature measurements in an ionic liquid

A comparison between the temperatures within imploding acoustic cavitation bubbles and the extent of sonoluminescence (SL) quenching by C₁–C₅ aliphatic alcohols in 1-ethyl-3-methylimidazolium ethylsulfate ([EMIM][EtSO₄], a well known imidazolium based room temperature ionic liquid (RTIL)), has been made at an ultrasound frequency of 213 kHz. The temperatures obtained ranged from 3500 ± 200 K, in neat [EMIM][EtSO₄], to about 3200 ± 200 K in RTIL-alcohol containing solutions. It was also found that the SL intensity decreased with increasing concentration (up to 1 M) of the alcohols to a greater extent compared with the relative changes to the bubble temperatures. Both the extent of the reduction in the bubble temperatures and the SL quenching were much smaller than those obtained in comparable aqueous solutions containing aliphatic alcohols. Possible reasons for the differences in the observed trends between water/alcohol and [EMIM][EtSO₄]/alcohol systems under sonication at 213 kHz are discussed.     

Electronic properties of the polycrystalline tin dioxide interface with conjugated organic layers

The results on the electronic structure of the unoccupied electronic states of the polycrystalline SnO₂ in the energy range from 5 eV to 25 eV above the Fermi level are presented. The modification of the electronic structure and of the surface potential upon deposition of the ultrathin films of copper phthalocyanine (CuPc) and of perylene tetracarboxylic acid dianhydride (PTCDA) film onto the SnO₂ surface were studied using the very low energy electron diffraction (VLEED) method and the total current spectroscopy (TCS) measurement scheme. A substantial attenuation of the TCS signal coming from the SnO₂ surface was observed upon formation of a 1.5–2 nm thick organic deposit layer while no new spectral features from the deposit were distinguishable. It was observed that the electronic structure typical for the organic films was formed within the organic deposit thickness range from 2 nm to 7 nm. The interfacial charge transfer was characterized by the formation of the polarization layer up to 5 nm thick in the organic films. The PTCDA deposition on SnO₂ was accompanied by the negative charge transfer onto the organic layer and to the 0.65 eV increase the surface work function. At the CuPc/SnO₂ interface, the negative charge was transferred to the SnO₂ surface and the overall surface work function decreased by 0.15 eV.     

Er–Pr doped tellurite glass nanocomposites for white light emitting diodes

In this paper, optical glass nanocomposites (nanoparticles sizes up to 100 nm) with composition TeO₂–WO₃–PbO–xEr₂O₃–yPr₆O₁₁ (x = 0.30 mol%, y = 0.70 mol%) embedded into polymer matrices was reported. The two types of polymers chosen for present study were: photopolymer oligoetheracryalte (OEA) and polymethylmethacrylate (PMMA), respectively. The incorporation of the titled nanoparticles into the polymer matrices is analyzed optically. The fluorescence spectra of the nanocomposites were compared with the fluorescence spectra of bulk glasses. Based on the comparison of Er^3 + and Pr^3 + ions' energy level schemes, possible energy transfer processes were identified. The prepared glasses are promising candidates for the white light emitting diodes applications.     

Mesopore size dependence of the ionic diffusivity in alumina based composite lithium ionic conductors

Ordered-mesoporous Al₂O₃ was synthesized by a sol–gel method using neutral copolymer surfactants as structure-directing agents. The pore size was controlled over the 3–15 nm range by the use of various surfactants. Composites composed of the synthesized mesoporous Al₂O₃ and a lithium ion conductor (LiI) were prepared. The maximum dc electrical conductivity, 2.6 × 10^− 4 S cm^− 1 at 298 K, was observed for 50 LiI·50 Al₂O₃ composite with 4.2 nm average mesopore size, which was considerably higher than the previously reported LiI-alumina composites. A systematic dependence of conductivity upon pore size was observed, in which conductivity increased with decreasing pore size, except for samples with a pore size of 2.8 nm. The lithium ion diffusion coefficient determined by the ⁷Li pulsed field gradient nuclear magnetic resonance (PFG-NMR) showed excellent agreement with the measured conductivity calculated by the Nernst-Einstein equation. On the other hand, lithium migration activation energies obtained by quasielastic neutron scattering (QENS) and ⁷Li NMR spin-lattice relaxation time (T₁) were considerably smaller than those obtained from electrical conductivity and PFG-NMR. This could be explained by the ion migration mechanism in heterogeneous composites and a possible enhancement of conductivity in mesoscopically confined spaces.