Microstructural and Mössbauer properties of low temperature synthesized Ni-Cd-Al ferrite nanoparticles

We report the influence of Al³⁺ doping on the microstructural and Mössbauer properties of ferrite nanoparticles of basic composition Ni_0.2Cd_0.3Fe_{2.5 - x}Al_xO₄ (0.0 ≤ x ≤ 0.5) prepared through simple sol-gel method. X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray, transmission electron microscopy (TEM), Fourier transformation infrared (FTIR), and Mössbauer spectroscopy techniques were used to investigate the structural, chemical, and Mössbauer properties of the grown nanoparticles. XRD results confirm that all the samples are single-phase cubic spinel in structure excluding the presence of any secondary phase corresponding to any structure. SEM micrographs show the synthesized nanoparticles are agglomerated but spherical in shape. The average crystallite size of the grown nanoparticles was calculated through Scherrer formula and confirmed by TEM and was found between 2 and 8 nm (± 1). FTIR results show the presence of two vibrational bands corresponding to tetrahedral and octahedral sites. Mössbauer spectroscopy shows that all the samples exhibit superparamagnetism, and the quadrupole interaction increases with the substitution of Al³⁺ ions.     

Natural fuel assisted synthesis of Mg–Cu ferrite nanoparticles: Evaluation of structural,dielectric, magnetic and humidity sensing properties

The effects of lemon juice and annealing treatment on phase composition, vibrational modes, microstructural and dielectric behavior of Mg doped copper ferrite nanoparticles have been synthesized and analyzed in detail in this present work. The various characterization techniques are used to examine the phase, microstructural, vibrational and dielectric nature of the samples at different annealing temperatures (600 °C and 900 °C). The phase and microstructure of Mg substituted CuFe₂O₄ nanoparticles have been analyzed by XRD, SEM and TEM. The secondary phase peaks free XRD spectra revealed that the as burst and the annealed Mg–CuFe₂O₄ nanoparticles have single phase cubic spinel structure. The average crystallite size of the as burnt, annealed 600 °C and annealed 900 °C of as prepared nanoparticles are calculated as 8.9 nm, 12.8 nm and 31.6 nm respectively. Another verification of the spherical shaped particle's size was confirmed by TEM analysis and it found as average size of 28.7 nm, this result is well matched with XRD analysis. The effect of size with impact of annealing treatment on magnetic and dielectric properties also analyzed. The size-dependent Mg–CuFe₂O₄ nanostructures exhibit promising sensing properties which ensure them as a potential candidate for humidity sensor applications. The as-burnt and annealed samples both show a humidity response over the humid range of 10–95 %RH. The sample annealed at 900 °C has the highest average sensor response (6.02 MΩ/%RH) among the as-burnt sample (6.38 MΩ/%RH) and annealed sample at 600 °C (7.11 MΩ/%RH).     

Double-perovskite magnetic La2NiMnO6 nanoparticles for adsorption of bovine serum albumin applications

Double-perovskite La₂NiMnO₆ (LNMO) nanoparticles were synthesized by co-precipitation process, and the adsorption of bovine serum albumin (BSA) protein on these nanoparticles was carried out. The powder samples were annealed at 750, 850, 950, and 1,050°C, respectively. X-ray diffraction (XRD) results reveal that there are double perovskites and exhibit mixed orientations, without any impurity phases. Transmission electron microscopy results as well as the XRD estimate results show that the crystalline size is about 34 to 40 nm. The adsorption of BSA on the magnetic nanoparticles was analyzed using a UV spectrophotometer at room temperature. The results show that the as-prepared LNMO nanoparticles display a good adsorbing ability for BSA, and the nanoparticle sintered at 850°C has the highest value of 219.6 mg/g, which is much higher than others.     

Growth of Mg2GeO4 nano-crystals on Si substrate and modulation of Seebeck coefficient by post growth annealing technique

We have reported the successful growth of Mg₂GeO₄ nano-crystals by simple thermal evaporation technique. The Mg and Ge metal powders were evaporated on the Si substrate and kept the oxygen flow rate of 100 sccm. The modulation of structural, morphological, thermoelectric and electrical properties was performed by controlling the thermal energy of carriers using different annealing temperatures. XRD data showed a peak at 61.8⁰ which was related to (212) plane of Mg₂GeO₄. XRD data further suggested that sample annealed at 700 °C has stable crystal structure while sample annealed at 800 °C posses degraded structure because the presence of highest density of donors defects. This defect concentration causes an increase in the conductivity of annealed samples as evident by the Hall data. This argument was also supported by Raman spectroscopy which showed that sample annealed at 700 °C has strongest Mg₂GeO₄ Raman peak. SEM images also verified the smooth surface of the sample annealed at 700 °C. The temperature dependent (25–100 °C) Seebeck effect measurements were performed to calculate the Seebeck coefficient of Mg₂GeO₄ nano-crystals at different measurement temperatures. The highest value of room temperature Seebeck coefficient (397 μV/⁰C) for the sample annealed at 800 °C is due the high density of carrier concentration.     

Effects of annealing temperature on some structural and optical properties of ZnO nanoparticles prepared by a modified sol-gel combustion method

Plate-shaped zinc oxide nanoparticles (ZnO-NPs) were successfully synthesized by a modified sol-gel combustion method. Zinc acetate, pure water and isopropanol were used as the starting materials. Acetic acid, diethanolamine and nitric acid were used as the polymerization agent, complexing agent and fuel, respectively. The precursors were formed by mixing aqueous solutions of zinc acetate, acetic acid and diethanolamine. Nitric acid was used to dry the produced gel. The resulting xerogel was annealed at 600 °C, 650 °C and 750 °C for 1 h. The synthesized ZnO-NPs were characterized by X-ray diffraction analysis (XRD), thermogravimetric analysis (TGA) and high-magnification transmission electron microscopy (TEM). The XRD results revealed that the samples produced were crystalline with a hexagonal wurtzite phase. The TEM results showed single-crystal ZnO-NPs with nearly hexagonal plate shapes. The optical properties of the ZnO-NPs were studied by UV-visible and Fourier-transform infrared spectroscopy (FTIR). The UV-vis absorption spectra of the ZnO-NPs indicated absorption peaks in the UV region, which were attributed to the band gap of the ZnO-NPs. The results of the FTIR and UV-vis studies showed that the optical properties of the ZnO-NPs depended on the annealing temperature.     

Optimization of different wet chemical routes and phase evolution studies of MnFe2O4 nanoparticles

Facile and low cost micro-emulsion method for the synthesis of single phase manganese ferrite (MnFe₂O₄) nanoparticles was explored. In an attempt to synthesize monodisperse and single phase manganese ferrite (MnFe₂O₄) nanoparticles, micro-emulsion method using different oil phases such as dodecanol, toluene and low cost paraffin was adapted. Simple co-precipitation method was also followed for comparison purpose. In this facile approach, the strategy to control the particle size at nano-level has been explained in detail. Formation mechanism of single phase manganese ferrite and appearance of different phases (such as goethite, manganite, hematite, hausmanite, maghemite, magnetite, etc) by these synthesis methods have been investigated and discussed. The samples were annealed at various temperatures to probe the thermal stability. Effect of annealing under air and under vacuum was studied. Thermal gravimetric analysis (TGA) was used to study the phase transitions along with the investigation of appropriate annealing temperature for spinel ferrite formation. X-ray Diffraction (XRD) analysis was used to study the crystal structure and phase identification. Microstructural properties were studied using scanning electron microscopy (SEM). Fourier transform infrared spectroscopy (FTIR) was used to study the bond stretching (Metal-Oxygen) and cubic spinel structure of MnFe₂O₄.     

Impact of Annealing Temperature on the Morphological,Optical and Photoelectrochemical Properties of Cauliflower-like CdSe0.6Te0.4 Photoelectrodes; Enhanced Solar Cell Performance

We are reporting on the impact of air annealing temperatures on the physicochemical properties of electrochemically synthesized cadmium selenium telluride (CdSe_0.6Te_0.4) samples for their application in a photoelectrochemical (PEC) solar cell. The CdSe_0.6Te_0.4 samples were characterized with several sophisticated techniques to understand their characteristic properties. The XRD results presented the pure phase formation of the ternary CdSe_0.6Te_0.4 nanocompound with a hexagonal crystal structure, indicating that the annealing temperature influences the XRD peak intensity. The XPS study confirmed the existence of Cd, Se, and Te elements, indicating the formation of ternary CdSe_0.6Te_0.4 compounds. The FE-SEM results showed that the morphological engineering of the CdSe_0.6Te_0.4 samples can be achieved simply by changing the annealing temperatures from 300 to 400 °C with intervals of 50 °C. The efficiencies (ƞ) of the CdSe_0.6Te_0.4 photoelectrodes were found to be 2.0% for the non-annealed and 3.1, 3.6, and 2.5% for the annealed at 300, 350, and 400 °C, respectively. Most interestingly, the PEC cell analysis indicated that the annealing temperatures played an important role in boosting the performance of the photoelectrochemical properties of the solar cells.     

Synthesis, magnetic and optical properties of core/shell Co1-xZnxFe2O4/SiO2 nanoparticles

The optical properties of multi-functionalized cobalt ferrite (CoFe₂O₄), cobalt zinc ferrite (Co_0.5Zn_0.5Fe₂O₄), and zinc ferrite (ZnFe₂O₄) nanoparticles have been enhanced by coating them with silica shell using a modified Stöber method. The ferrites nanoparticles were prepared by a modified citrate gel technique. These core/shell ferrites nanoparticles have been fired at temperatures: 400°C, 600°C and 800°C, respectively, for 2 h. The composition, phase, and morphology of the prepared core/shell ferrites nanoparticles were determined by X-ray diffraction and transmission electron microscopy, respectively. The diffuse reflectance and magnetic properties of the core/shell ferrites nanoparticles at room temperature were investigated using UV/VIS double-beam spectrophotometer and vibrating sample magnetometer, respectively. It was found that, by increasing the firing temperature from 400°C to 800°C, the average crystallite size of the core/shell ferrites nanoparticles increases. The cobalt ferrite nanoparticles fired at temperature 800°C; show the highest saturation magnetization while the zinc ferrite nanoparticles coated with silica shell shows the highest diffuse reflectance. On the other hand, core/shell zinc ferrite/silica nanoparticles fired at 400°C show a ferromagnetic behavior and high diffuse reflectance when compared with all the uncoated or coated ferrites nanoparticles. These characteristics of core/shell zinc ferrite/silica nanostructures make them promising candidates for magneto-optical nanodevice applications.     

Synthesis and characterizations of Ni-NiO nanoparticles on PDDA-modified graphene for oxygen reduction reaction

We are presenting our recent research results about the Ni-NiO nanoparticles on poly-(diallyldimethylammonium chloride)-modified graphene sheet (Ni-NiO/PDDA-G) nanocomposites prepared by the hydrothermal method at 90°C for 24 h. The Ni-NiO nanoparticles on PDDA-modified graphene sheets are measured by transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), and selected area electron diffraction (SAED) pattern for exploring the structural evidence to apply in the electrochemical catalysts. The size of Ni-NiO nanoparticles is around 5 nm based on TEM observations. The X-ray diffraction (XRD) results show the Ni in the (012), (110), (110), (200), and (220) crystalline orientations, respectively. Moreover, the crystalline peaks of NiO are found in (111) and (220). The thermal gravimetric analysis (TGA) result represents the loading content of the Ni metal which is about 34.82 wt%. The electron spectroscopy for chemical analysis/X-ray photoelectron spectroscopy (ESCA/XPS) reveals the Ni⁰ to Ni^II ratio in metal phase. The electrochemical studies with Ni-NiO/PDDA-G in 0.5 M aqueous H₂SO₄ were studied for oxygen reduction reaction (ORR).     

Time-resolved photoluminescence studies of annealed 1.3-μm GaInNAsSb quantum wells

Time-resolved photoluminescence (PL) was applied to study the dynamics of carrier recombination in GaInNAsSb quantum wells (QWs) emitting near 1.3 μm and annealed at various temperatures. It was observed that the annealing temperature has a strong influence on the PL decay time, and hence, it influences the optical quality of GaInNAsSb QWs. At low temperatures, the PL decay time exhibits energy dependence (i.e., the decay times change for different energies of emitted photons), which can be explained by the presence of localized states. This energy dependence of PL decay times was fitted by a phenomenological formula, and the average value of E₀, which describes the energy distribution of localized states, was extracted from this fit and found to be smallest (E₀ = 6 meV) for the QW annealed at 700°C. In addition, the value of PL decay time at the peak energy was compared for all samples. The longest PL decay time (600 ps) was observed for the sample annealed at 700°C. It means that based on the PL dynamics, the optimal annealing temperature for this QW is approximately 700°C.     

Molecular-solution printing of Cu2ZnSnS4 (CZTS) thin film

In this work, a novel molecular-solution printing approach combined with a rapid thermal annealing process for the facile fabrication of Cu₂ZnSnS₄ (CZTS) thin film is reported. The intrinsic relationship between annealing parameters (temperature and time) and the properties of the fabricated samples was investigated systematically. Furthermore, the mechanism behind this CZTS formation approach was studied in detail. The results show that the best properties were obtained for the sample annealed at 600 °C for 45 min, which displayed a pure kesterite CZTS phase, acceptable morphology consisting of 1.0–1.5 μm size nanoparticles, a satisfactory Cu-poor and Zn-rich composition, and an ideal bandgap of ~1.42 eV. Thus, the prepared sample is a promising candidate for the fabrication of high-performance photovoltaic devices.     

Influence of multi-step annealing on nanostructure and surface morphology of Y2O3:SiO2 powder

Y₂O₃:SiO₂ powder was synthesized by a sol–gel method, using hydrous yttrium nitrate and hydrous silicon oxide as precursors and HCl as a catalyst. The dried samples were submitted to multi-step annealing schedule in air without applying pressure. A simple four-step annealing schedule with a final stage of about 900 °C for 6.0 h was followed. The samples of Y₂O₃:SiO₂ nanocomposites were obtained with well defined size and shape. Structural changes of the nanocomposites were investigated by XRD, FTIR and TEM. Multi-step annealing scheme with different ramp rates and incubation times allows recovery-relaxation processes within the boundaries and leading to a concomitant linear increase of crystallite size and densification. Almost fully dense quasi-spherical cubic-yttria nanopowder has been demonstrated with an average grain size distribution of 10–40 nm; can be uniformly dispersed in silica matrix.     

Effect of annealing temperature on wettability of TiO2 nanotube array films

Highly ordered TiO₂ nanotube array (TN) films were prepared by anodization of titanium foil in a mixed electrolyte solution of glycerin and NH₄F and then annealed at 200°C, 400°C, 600°C, and 800°C, respectively. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), water contact angle (WCA), and photoluminescence (PL). It was found that low temperature (below 600°C) has no significant influence on surface morphology, but the diameter of the nanotube increases from 40 to 50 nm with increasing temperature. At 800°C, the nanotube arrays are completely destroyed and only dense rutile film is observed. Samples unannealed and annealed at 200°C are amorphous. At 400°C, anatase phase appears. At 600°C, rutile phase appears. At 800°C, anatase phase changes into rutile phase completely. The wettability of the TN films shows that the WCAs for all samples freshly annealed at different temperatures are about 0°. After the annealed samples have been stored in air for 1 month, the WCAs increase to 130°, 133°, 135°, 141°, and 77°, respectively. Upon ultraviolet (UV) irradiation, they exhibit a significant transition from hydrophobicity to hydrophilicity. Especially, samples unannealed and annealed at 400°C show high photoinduced hydrophilicity.     

Nanotwinning and structural phase transition in CdS quantum dots

Nanotwin structures are observed in high-resolution transmission electron microscopy studies of cubic phase CdS quantum dots in powder form by chemical co-precipitation method. The deposition of thin films of nanocrystalline CdS is carried out on silicon, glass, and TEM grids keeping the substrates at room temperature (RT) and 200°C by pulsed laser ablation. These films are then subjected to thermal annealing at different temperatures. Glancing angle X-ray diffraction results confirm structural phase transitions after thermal annealing of films deposited at RT and 200°C. The variation of average particle size and ratio of intensities in Raman peaks I_2LO/I_1LO with annealing temperature are studied. It is found that electron-phonon interaction is a function of temperature and particle size and is independent of the structure. Besides Raman modes LO, 2LO and 3LO of CdS at approximately 302, 603, and 903 cm⁻¹ respectively, two extra Raman modes at approximately 390 and 690 cm⁻¹ are studied for the first time. The green and orange emissions observed in photoluminescence are correlated with phase transition.     

Passivation mechanism of thermal atomic layer-deposited Al2O3 films on silicon at different annealing temperatures

Thermal atomic layer-deposited (ALD) aluminum oxide (Al₂O₃) acquires high negative fixed charge density (Q_f) and sufficiently low interface trap density after annealing, which enables excellent surface passivation for crystalline silicon. Q_f can be controlled by varying the annealing temperatures. In this study, the effect of the annealing temperature of thermal ALD Al₂O₃ films on p-type Czochralski silicon wafers was investigated. Corona charging measurements revealed that the Q_f obtained at 300°C did not significantly affect passivation. The interface-trapping density markedly increased at high annealing temperature (>600°C) and degraded the surface passivation even at a high Q_f. Negatively charged or neutral vacancies were found in the samples annealed at 300°C, 500°C, and 750°C using positron annihilation techniques. The Al defect density in the bulk film and the vacancy density near the SiO_x/Si interface region decreased with increased temperature. Measurement results of Q_f proved that the Al vacancy of the bulk film may not be related to Q_f. The defect density in the SiO_x region affected the chemical passivation, but other factors may dominantly influence chemical passivation at 750°C.     

The effect of thermal annealing on Fe/TiO2 coatings deposited with the help of RF PECVD method. Part I. Chemical and phase composition

Results of the studies on chemical structure and phase composition of both non-annealed and thermally annealed iron doped TiO₂ coatings are presented. The coatings were synthesized with the help of radio frequency plasma enhanced chemical vapor deposition (RF PECVD) and characterized by iron content in the range of 0–4.76 at%. In these studies, an analysis of both elemental composition and chemical bonding was performed with the help of X-ray photoelectron spectroscopy (XPS). X-ray diffraction (XRD) was applied to determine phase composition and Fourier transform infrared spectroscopy (FTIR) was used as a supplementary source of information. The obtained elemental composition data show that, apart from titanium, oxygen and iron, traces of chlorine as well as substantial amounts of carbon are present in the coatings. While chlorine has originated from plasma decomposition of TiCl_4, used as a source of titanium, a presence of carbon is associated with a surface contamination resulting from photocatalytic reactions of TiO₂ with the adsorbed carbon dioxide. The results of XPS and FTIR indicate that thermal annealing not only modifies phase composition of these materials, but also affects chemical bonding. Finally, XRD analysis shows that iron content has an effect on the size of coherent diffraction domains present in the films.     

The Properties of Sintered Calcium Phosphate with [Ca]/[P] = 1.50

In order to obtain the properties of the sintered as-dried calcium phosphate with [Ca]/[P] = 1.50, the characteristics of sintered pellets have been investigated using X-ray diffraction (XRD), inductively coupled plasma-mass spectrometry (ICP-MS), Fourier-transform infrared (FT-IR) spectra, Vickers hardness indentation and scanning electron microscopy (SEM). When the pellet samples were sintered between 700 °C and 1200 °C for 4 h, the hydroxyapatite (Ca₁₀(PO₄)₆(OH)₂, HA) still maintained the major phase, accompanied with the rhenanite (NaCaPO₄) as the secondary phase and β-tricalcium phosphate (β-Ca₃(PO₄)₂, β-TCP) as the minor phases. In addition, the HA partially transformed to α-tricalcium phosphate (α-Ca₃(PO₄)₂, α-TCP) and tetracalcium phosphate (Ca₄(PO4)₂O, TTCP), when the pellet samples were sintered at 1300 °C and 1400 °C, respectively, for 4 h. The maximum density and Vickers Hardness (HV) of sintered pellet samples were 2.85 g/cm³ (90.18% theoretical density (T.D.)) and 407, which appeared at 1200 °C and 900 °C, respectively.     

Elucidation of morphological and optoelectronic properties of highly crystalline chalcopyrite (CuInSe2) nanoparticles synthesized via hot injection route

CuInSe₂ (CIS) nanoparticles have been prepared by the hot-injection method with sizes ～25 nm, and the thermal annealing influence on the size, morphology and optoelectronic properties of crystalline CuInSe₂ nanoparticles has been elucidated. Microstructural analysis of synthesized nanoparticles was performed by various characterization methods including high-resolution transmission electron microscopy (HR-TEM), Scanning TEM (STEM), Xray diffraction, X-ray photoelectron spectroscopy (XPS) and photoluminescence (PL) spectroscopy. The fast Fourier transform (FFT) pattern of HR-TEM image of annealed CuInSe2 nanoparticles illustrates that the particles have quasisingle crystal tetragonal structure, as also confirmed by the XRD pattern. The HR-TEM image clearly shows the fringe widths are in order without any defect with 0.32 nm. Microstructural analysis results clearly indicate that the synthesized and air-annealed nanoparticles are in highly crystalline state with near stoichiometric atomic composition.     

Annealing impact on the structural and optical properties of electrospun SnO2 nanofibers for TCOs

Tin oxide (SnO₂) nanofibers were fabricated by electrospinning technique and subsequent annealed at different temperatures. The structure, morphology and optical properties of the annealed samples were characterized by X-ray diffraction (XRD), Raman, scanning electron microscopy/energy dispersive spectroscopy (SEM/EDS), transmission electron microscopy (TEM), Fourier transformed infrared (FTIR),and optical absorption techniques. The phase of SnO₂ of all samples is rutile (tetragonal), and at higher annealing temperatures, good crystallinity and lower absorption were obtained. Annealing of the samples at 600 °C caused the lower absorption and higher optical band gap, and the decrease of the absorption was probably because the fiber structure changed from solid to hollow structure. From PL spectra, it was observed that the SnO₂ hollow nanofibers annealed at 600 °C revealed green emission at 530 nm.     

LaFeO3 ceramics as selective oxygen sensors at mild temperature

In this study, an investigation about the oxygen sensing properties of lanthanum orthoferrite (LaFeO₃) ceramics is reported. LaFeO₃ nanoparticles were synthesized by using tartaric sol-gel route and annealed in air at different temperatures (500, 700 and 900 °C). The samples have been characterized by using thermal analysis (TA), BET surface area and porosity, Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, X-ray diffraction (XRD), and scanning electron microscopy (SEM). Results of sensing tests indicate that LaFeO₃ nanoparticles exhibit good response to oxygen at mild temperatures (300–450 °C). The effect of annealing temperature on gas sensing performance was investigated, demonstrating that LaFeO₃ ceramics obtained after annealing at 500 °C display better characteristics with respect to others. The oxygen sensor developed shows also high stability in humid environment and excellent selectivity to oxygen over other interfering gases such as CO, NO₂, CO₂, H₂ and ethanol.