Effect of processing conditions on sonochemical synthesis of nanosized copper aluminate powders

Nanosized copper aluminate (CuAl₂O₄) spinel particles have been prepared by a precursor approach with the aid of ultrasound radiation. Mono-phasic copper aluminate with a crystallite diameter of 17 nm along the (3 1 1) plane was formed when the products were synthesized using Cu(NO₃)₂·6H₂O and Al(NO₃)₃·9H₂O as starting materials, with urea as a precipitation agent at a concentration of 9 M. The reaction was carried out under ultrasound irradiation at 80 °C for 4 h and a calcination temperature of 900 °C for 6 h. The synthesized copper aluminate particles and the effect of different processing conditions such as the copper source, precipitation agents, sonochemical reaction time, calcination temperature and time were analyzed and characterized by the techniques of powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM) and Fourier transformation infrared spectroscopy (FT–IR).     

A new method of synthesis on high-quality AgGaS2 polycrystalline

High-pure, single-phase, free of voids and high mass density AgGaS₂ polycrystalline was synthesized by a new method, i.e. two-temperature zone vapor-transporting together with the mechanical and melt temperature oscillation method (TVMMTOM), directly from high-purity (6 N) elements silver, gallium and sulfur with excess sulfur. The mechanism and advantages of the new method for synthesizing high-quality AgGaS₂ were discussed. It is found that the polycrystalline material synthesized by the new method is superior to that synthesized by the conventional method, what is more the new method can avoid the explosion of the synthetic quartz ampoule. Adopting the modified Bridgman method an integral and crack-free AgGaS₂ single crystal with diameter of 14 mm and length of 63 mm has been obtained. It was found that there was a (1 0 1) cleavage face and the four order X-ray spectrum of the {1 0 1} faces was observed. By the method of DSC analysis the melting and freezing points of the AgGaS₂ single crystal were about 995 and 955 °C. The transmission spectra of the AgGaS₂ sample of 10 × 8 × 2 mm³ were obtained by means of UV and IR spectrophotometer. The limiting wavelength was 470 nm and the band gap was 2.64 eV. It can be found in the infrared spectrum that the infrared transmission was above 55% from 4000 to 800 cm⁻¹, and the infrared transmittance of the crystal is up to 63% at 10.6 μm, which is higher than that of the crystal grown using polycrystalline materials synthesized by the conventional method. The value of α in 10.6 μm was 0.267 cm⁻¹. Above mentioned results showed that the crystal was of good quality and TVMMTOM is preferable for synthesizing high-quality AgGaS₂ polycrystalline materials.     

Template-free sonochemical synthesis of hierarchically porous NiO microsphere

A novel template-free sonochemical synthesis technique was used to prepare NiO microspheres combined with calcination of NiO_2.45C_0.74N_0.25H_2.90 precursor at 500 °C. The NiO microspheres samples were systematically investigated by the thermograviometric/differential scanning calorimetry (TG/DSC), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), fourier-transformed infrared spectroscopy (FT-IR), Brunnauer–Emmett–Teller (BET) nitrogen adsorption–desorption isotherms, laser particle size analyzer, and ultraviolet–visible spectroscopy (UV–Vis). The morphology of the precursor was retained even after the calcination process, and exhibited hierarchically porous sphericity. The morphology changed over the ultrasonic radiation time, and the shortest reaction time was 70 min, which was much less than 4 h for the mechanical stirring process. The mechanical stirring was difficult to form the complete hierarchically porous microsphere structure. The BET specific surface area and the median diameter of the hierarchically porous NiO microspheres were 103.20 m²/g and 3.436 μm, respectively. The synthesized NiO microspheres were mesoporous materials with a high fraction of macropores. The pores were resulted from the intergranular accumulation. The ultraviolet absorption spectrum showed a broad emission at the center of 475 nm, and the band gap energy was estimated to be 3.63 eV.     

Low temperature synthesis of layered LiNiO2 cathode material in air atmosphere by ion exchange reaction

The layered LiNiO₂ cathode material for lithium ion battery was synthesized by ion-exchange reaction at low temperature in air atmosphere. The influence of synthesis conditions on the electrochemical performance of the resulting LiNiO₂ was investigated. The LiNiO₂ samples were characterized by X-ray powder diffraction (XRD), scanning electron microscope (SEM) and infrared (IR) analysis. The results indicate that low temperature fabricated LiNiO₂ powders keep a single layered hexagonal structure and homogenous spheric shape like the raw material NiOOH. Charge and discharge tests show that the resultant LiNiO₂ exhibits good electrochemical properties. The first charge and discharge capacities of the sample are 183.4 mA h g^− 1 and 169.5 mA h g^− 1 at 0.5 mA cm^− 2, respectively. Galvanic charge/discharge and cyclic voltammetry tests reflect that LiNiO₂ electrode exhibits good cycle reversibility.     

Effects of high power ultrasonic vibration on temperature distribution of workpiece in dry creep feed up grinding

Temperature history and distribution of steel workpiece (X20Cr13) was measured by a high tech infrared camera under ultrasonic assisted dry creep feed up grinding. For this purpose, a special experimental setup was designed and fabricated to vibrate only workpiece along two directions by a high power ultrasonic transducer. In this study, ultrasonic effects with respect to grinding parameters including depth of cut (a_e), feed speed (v_w), and cutting speed (v_s) has been investigated. The results indicate that the ultrasonic vibration has considerable effect on reduction of temperature, depth of thermal damage of workpiece and width of temperature contours. Maximum temperature reduction of 25.91% was reported at condition of v_s = 15 m/s, v_w = 500 mm/min, a_e = 0.4 mm in the presence of ultrasonic vibration.     

Preparation of monodisperse magnetite nanoparticles under mild conditions

In this paper, we reported a method to prepare monodisperse magnetite nanoparticles at mild temperature using cheap and non-toxic precursors. It overcomes the shortages of chemical co-precipitation method and thermal decomposition method and combines the advantages of facile, cheap, large-scale, monodisperse, nanosize, and low synthesis temperature and low toxic. In this method, FeCl₃ · 6H₂O, FeCl₂ · 4H₂O and sodium oleate were mixed in toluene/ethanol/water mixture solvent and refluxed at 74 °C to prepare magnetite nanoparticles directly. The nanoparticles were characterized by transmission electron microscopy, dynamic light scattering, X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectrometer and thermogravimetric analysis. The magnetic properties of nanoparticles were measured by superconducting quantum interference device. The results showed that the nanoparticles are well-monodisperse with about 4–5 nm of average diameter. The nanoparticles were proved to be superparamagnetic with saturated magnetization 23.6 emu/g and blocking temperature 24.4 K. A possible formation mechanism of monodisperse magnetite nanoparticles was presented at the same time.     

Sonochemical synthesis of cobalt aluminate nanoparticles under various preparation parameters

Cobalt aluminate (CoAl₂O₄) nanoparticles were synthesized using a precursor method with the aid of ultrasound irradiation under various preparation parameters. The effects of the preparation parameters, such as the sonochemical reaction time and temperature, precipitation agents, calcination temperature and time on the formation of CoAl₂O₄ were investigated. The precursor on heating yields nanosized CoAl₂O₄ particles and both these nanoparticles and the precursor were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and atomic force microscopy (AFM). The use of ultrasound irradiation during the homogeneous precipitation of the precursor reduces the duration of the precipitation reaction. The mechanism of the formation of cobalt aluminate was investigated by means of Fourier transformation infrared spectroscopy (FT-IR) and EDX (energy dispersive X-ray). The thermal decomposition process and kinetics of the precursor of nanosized CoAl₂O₄ were investigated by means of differential scanning calorimetry (DSC) and thermogravimetry (TG). The apparent activation energy (E) and the pre-exponential constant (A) were 304.26 kJ/mol and 6.441 × 10¹⁴ s^?1, respectively. Specific surface area was investigated by means of Brunauer Emmett Teller (BET) surface area measurements.     

Ultrasonic assisted synthesis of Bikitaite zeolite: A potential material for hydrogen storage application

Li containing Bikitaite zeolite has been synthesized by an ultrasound-assisted method and used as a potential material for hydrogen storage application. The Sonication energy was varied from 150 W to 250 W and irradiation time from 3 h to 6 h. The Bikitaite nanoparticles were characterized by X-ray diffraction (XRD), infrared (IR) spectral analysis, and field-emission scanning electron microscopy (FESEM) thermo-gravimetrical analysis and differential thermal analysis (TGA, DTA). XRD and IR results showed that phase pure, nano crystalline Bikitaite zeolites were started forming after 3 h irradiation and 72 h of aging with a sonication energy of 150 W and nano crystalline Bikitaite zeolite with prominent peaks were obtained after 6 h irradiation of 250 W sonic energy. The Brunauer–Emmett–Teller (BET) surface area of the powder by N₂ adsorption–desorption measurements was found to be 209 m²/g. The TEM micrograph and elemental analysis showed that desired atomic ratio of the zeolite was obtained after 6 h irradiation. For comparison, sonochemical method, followed by the hydrothermal method, with same initial sol composition was studied. The effect of ultrasonic energy and irradiation time showed that with increasing sonication energy, and sonication time phase formation was almost completed. The FESEM images revealed that 50 nm zeolite crystals were formed at room temperature. However, agglomerated particles having woollen ball like structure was obtained by sonochemical method followed by hydrothermal treatment at 100 °C for 24 h. The hydrogen adsorption capacity of Bikitaite zeolite with different Li content, has been investigated. Experimental results indicated that the hydrogen adsorption capacities were dominantly related to their surface areas as well as total pore volume of the zeolite. The hydrogen adsorption capacity of 143.2 c.c/g was obtained at 77 K and ambient pressure of (0.11 MPa) for the Bikitaite zeolite with 100% Li, which was higher than the reported values for other zeolites. To the best of our knowledge, there is no report on the synthesis of a Bikitaite zeolite by sonochemical method for H₂ storage.     

Thermal imaging during infrared final cooking of semi-processed cylindrical meat product

The temperature measurements during the infrared cooking of the semi-cooked cylindrical minced beef product (koefte) were taken by both contact (thermocouples) and non-contact (thermal imaging) techniques. The meat product was semi-cooked till its core temperature reached up to 75 °C by ohmic heating applied at 15.26 V/cm voltage gradient. Then, infrared cooking was applied as a final cooking method at different combinations of heat fluxes (3.7, 5.7 and 8.5 kW/m²), applied distances (10.5, 13.5 and 16.5 cm) and applied durations (4, 8 and 12 min). The average surface temperature increased as the heat flux and the applied duration increased but the applied distance decreased. The temperature distribution of the surface during infrared cooking was determined successfully by non-contact measurements. The temperature homogeneity varied between 0.77 and 0.86. The process condition of 8.5 kW/m² for 8 min resulted in core temperature greater than 75 °C, which was essential for safe production of ready-to-eat (RTE) meat products. Thermal imaging was much more convenient method for minimizing the point measurement mistakes and determining temperature distribution images more clear and visual.     

Simple one-step ultrasonic synthesis of anatase titania/polypyrrole nanocomposites

In this work, hybrid nanocomposites based on anatase titania:polypyrrole (TiO₂:PPy) were directly obtained from a simple, one-step, ultrasonic (UT)-assisted synthesis. The properties of these crystalline nanocomposites were compared with those of others fabricated using cold (Cold)-assisted synthesis without any UT assistance, which required a hydrothermal treatment (HT) to yield crystalline anatase titania in the nanocomposite (TiO₂:PPy) at low temperature (130 °C) and in a short time (3 h). The SEM results demonstrated that the UT-assisted synthesis is a feasible method to obtain anatase TiO₂:PPy nanocomposites with controlled morphology using low energy. The Fourier transform infrared (FT-IR) bands of the crystalline nanocomposites exhibited a shift with respect to neat components, which was attributed to the strong interaction between the secondary amine groups (N–H) of PPy and the oxygen from TiO₂. The acceptable absorption in the visible region (λ_max = 670 nm) indicates that these nanocomposites are good candidates for harvesting energy in solar cells. Devices based on these nanocomposites were built to evaluate their electrical properties. An increase in the photocurrent was observed for the devices prepared with the nanocomposites from the UT-assisted synthesis.     

Hexamethylenetetramine assisted hydrothermal synthesis of BiPO4 and its electrochemical properties for supercapacitors

The well defined microstructures of BiPO₄ were successfully synthesized by the facile hexamethylenetetramine (HMT) assisted hydrothermal method. The low temperature monoclinic BiPO₄ structure with space group P2₁/n, were obtained from X-ray diffraction (XRD) for the pristine and HMT-assisted BiPO₄ with 1, 3, 5 and 10 mmole concentration. A transformation from low temperature monazite-type phase to the high temperature SbPO₄-type phase of BiPO₄ was observed at the 10 mmole concentration. There was a variation in the morphology from polyhedron to octahedra-like and finally into cube shape upon an increase in concentration of HMT. The role of reaction time in the morphology of BiPO₄ particles was investigated. The selected area electron diffraction (SAED) pattern elucidated the ordered dot pattern and the calculated d-spacing revealed the formation of BiPO₄. An increased specific capacitance of HMT assisted materials (202 F/g) compared with pristine BiPO₄ (89 F/g) at 5 mA/cm² was observed upon morphological variation due to HMT addition.     

Temperature measurements inside an Er3+–Yb3+ co-doped fluoride crystal heated by a NIR laser diode and probed by red-to-green upconversion

The temperature of a transparent Cd_0.7Sr_0.3F₂: Er³⁺(4%)–Yb³⁺(6%) crystalline plate 0.3 mm thick heated by a near-infrared (974 nm) laser diode and probed by a red (652 nm) laser was accurately evaluated as a function of the infrared power absorbed by the Yb³⁺ ions.The green emission generated by the Er³⁺ ions directly excited by the red laser consists of three major lines (coming from three individual Stark levels in thermal equilibrium) whose intensities were measured according to the absorbed infrared power and the distance between the heated and probed volumes, to evaluate the heating induced by the excitation of Yb³⁺ and Er³⁺ ions at 974 nm by applying the Boltzmann's equation linking the populations of emitting levels to the temperature. In the case where the Yb³⁺ ions excited by the laser diode are situated at a distance of about 0.5 mm from the edge of the crystal and for an absorbed infrared power of 100 mw, the crystal's edge temperature is reaching 80 °C after 20 s of continuous excitation at 974 nm.     

Quick response PZT/P(VDF-TrFE) composite film pyroelectric infrared sensor with patterned polyimide thermal isolation layer

The fabrication method and the pyroelectric response of a single element infrared sensor based lead zirconate titanate (PZT) particles and polyvinylidene fluoride P(VDF-TrFE) copolymer composite thick film is reported in this paper. A special thermal insulation structure, including polyimide (PI) thermal insulation layer and thermal insulation tanks, was used in this device. The thermal insulation tanks were fabricated by laser micro-etching technique. Voltage responsivity (R_V), noise voltage (V_noise), noise equivalent power (NEP), and detectivity (D^*) of the PZT/P(VDF-TrFE) based infrared sensor are 1.2 × 10³ V/W, 1.25 × 10⁻⁶ V Hz^1/2, 1.1 × 10⁻⁹ W and 1.9 × 10⁸ cm Hz^1/2 W⁻¹ at 137.3 Hz modulation frequency, respectively. The thermal time constant of the infrared sensor τ_T was about 15 ms. The results demonstrate that the composite infrared sensor show a high detectivity at high chopper frequency, which is an essential advantage in infrared detectors and some other devices.     

Effect of CuI on the formation and properties of Te-based far infrared transmitting chalcogenide glasses

A series of Ge–Te–CuI far infrared transmitting chalcohalide glasses were prepared by traditional melt-quenching method and the glass-forming region was determined. Properties measurements include density, DTA, XRD, SEM, Vis–NIR and infrared (IR) transmission spectra. The results show that with the addition of CuI, the glass-forming ability is improved and nearly 30 mol% CuI can be dissolved into the Ge₂₀Te_80?x(CuI)_x glass system. The density and glass transition temperature of Ge–Te–CuI chalcohalide glasses are within the range 5.459–5.960 g cm^?3 and 150–184 °C, respectively. These glasses all have wide optical transmission window from 1.8 to 25 μm and offer an alternative solution for far infrared transmitting materials.     

Improved synthesis of sucrose fatty acid monoesters under ultrasonic irradiation

Sucrose fatty acid esters were synthesized by the transesterification of sucrose with aliphatic esters under ultrasound irradiation in good yield (?73%). The optimum reaction conditions for the transesterification reaction include a molar ratio of sucrose to fatty acid ethyl ester of 2:1 and the use of a 13% mol anhydrous K₂CO₃ catalyst. The optimum reaction temperature was set at 70 °C, the optimum reaction time was 2 h, and the optimum reaction pressure was 11 kPa. The reaction had excellent monoester selectivity. The proportion of monoester (6-monoester + 6′-monoester) in the purified products was up to 92–95% via flash column chromatography over silica gel, the ratios of 6-monoester/6′-monoester are 2.1–2.7, and the sucrose monoesters were identified by HPLC–MS, NMR and IR.     

Boron-doped nanocrystalline silicon germanium thin films for uncooled infrared bolometer applications

In this paper, boron-doped nanocrystalline Si_0.78Ge_0.22:H thin film is assessed for use as resistive sensing layer in uncooled infrared bolometer applications. The silicon germanium thin films were deposited by PECVD (plasma enhanced chemical vapor deposition) through decomposition of silane, germane and diborane diluted with argon at substrate temperature of 230 °C. Under optimum deposition parameters, the sensing films with modulate electrical resistivity (<10⁴ Ω cm) and high temperature coefficient of resistance (TCR) (>−3%/K) were obtained at room temperature. 1/f noise character in the form of the normalized Hooge parameter was measured in the frequency range of 1–64 Hz, resulting in a lower 1/f noise compared to other materials currently used for device application.     

On the stability of the CO adsorption-induced and self-organized CuPt surface alloy

The stability of the recently discovered CO-induced and self-organized CuPt surface alloy was explored at near ambient pressures of O₂ (200 mbar) at room temperature, in a CO + H₂ mix (P_tot = 220 mbar, 4% CO) from room temperature to 573 K, as well as in a CO + H₂O mix (P_tot = 17 mbar, 50% CO) from room temperature to 673 K. No indications of substantial changes in surface structure were observed under the latter conditions compared to CO alone whereas the O₂ oxidation resulted in CO removal and the build-up of an ultrathin CuO_x-film. However, the oxidized CO/CuPt surface alloy could be regenerated by reducing the CuO_x in 100 mbar CO for 10 min at room temperature. The results show, amongst others, the stability of the CuPt surface alloy in various environments containing CO and how a novel coinage/Pt-group bimetallic surface alloy catalyst induced by CO adsorption can be reactivated before use in applications such as electrochemistry at ambient temperatures.     

Ultrasound with low intensity assisted the synthesis of nanocrystalline TiO2 without calcination

A novel method has been developed for the preparation of nano-sized TiO₂ with anatase phase. Nanoparticles with diameter about 6 nm were prepared at a relatively low temperature (75 °C) and short time. The synthesis was carried out by the hydrolysis of titanium tetra-isopropoxide (TTIP) in the presence of water, ethanol, and dispersant under ultrasonic irradiation (500 kHz) at low intensity. The results show that variables such as water/ethanol ratio, irradiation time, and temperature have a great influence on the particle size and crystalline phases of TiO₂ nanoparticles. Characterization of the product was carried out by different techniques such as powder X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM) and UV–vis spectroscopy.     

Fast and wide-band response infrared detector using porous PZT pyroelectric thick film

Porous lead zirconate titanate (PbZr_0.3Ti_0.7O₃, PZT30/70) thick films and detectors for pyroelectric applications have been fabricated on alumina substrates by screen-printing technology. Low temperature sintering of PZT thick films have been achieved at 850 °C by using Li₂CO₃ and Bi₂O₃ sintering aids. The microstructure of PZT thick film has been investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The dielectric properties were measured using HP 4284 at 1 kHz under 25 °C. The permittivity and loss tangent of the thick films were 94 and 0.017, respectively. Curie temperature of PZT thick film was 425 °C as revealed by dielectric constant temperature measurement. The pyroelectric coefficient was determined to be 0.9 × 10⁻⁸ Ccm⁻² K⁻¹ by dynamic current measurement. Infrared detector sensitive element of dual capacitance was fabricated by laser directly write technology. Detectivity of the detectors were measured using mechanically chopped blackbody radiation. Detectivity ranging from 1.23 × 10⁸ to 1.75 × 10⁸ (cm Hz^1/2 W⁻¹) was derived at frequency range from 175.5 Hz to 1367 Hz, and D^*’s −3 dB cut-off frequency bandwidth was 1.2 kHz. The results indicate that the infrared detectors based on porous thick films have great potential applications in fast and wide-band frequency response conditions.     

Near-infrared photoluminescence and thermally stimulated current in Cu3Ga5Se9 layered crystals: A comparative study

Near-infrared photoluminescence (PL) and thermally stimulated current (TSC) spectra of Cu₃Ga₅Se₉ layered crystals grown by Bridgman method have been studied in the photon energy region of 1.35–1.46 eV and the temperature range of 15–115 K (PL) and 10–170 K (TSC). An infrared PL band centered at 1.42 eV was revealed at T = 15 K. Radiative transitions from shallow donor level placed at 20 meV to moderately deep acceptor level at 310 meV were suggested to be the reason of the observed PL band. TSC curve of Cu₃Ga₅Se₉ crystal exhibited one broad peak at nearly 88 K. The thermal activation energy of traps was found to be 22 meV. An energy level diagram demonstrating the transitions in the crystal band gap was plotted taking account of results of PL and TSC experiments conducted below room temperature.