Effect of calcination temperature on structural,morphological and electrochemical properties of Sn doped Co3O4 nanorods

Tremendous attention has been devoted for the development of highly efficient and stable electrode materials for supercapacitor applications. In this study, Sn-doped Co₃O₄ nanorods were prepared via solvothermal process using PVP and oxalic acid as surfactants. The phase, morphology and composition of Sn-doped Co₃O₄ nanorods were examined by XRD and SEM/EDX techniques. The electrochemical properties were studied via cyclic voltammetry (CV), galvanostatic charging-discharging (GCD), electrochemical impedance spectroscopy (EIS) measurements. The CV results show that electrode based on 5 at. % Sn-doped Co₃O₄ (5Sn-doped Co₃O₄) nanorods delivered the highest specific capacitance (842.44 F/g) at 5 mV/s than that of the electrode based on pure Co₃O₄ (729.39 F/g). In order to further tune the performance of this electrode, the structure, morphology and electrochemical behavior of 5Sn-doped Co₃O₄ sample were optimized via variety of calcination temperatures ranging from 250 to 400 °C. Notably, the 5Sn-doped Co₃O₄ sample calcined at 350 °C exhibited higher electrochemical performance (specific capacitance ~913.10 F/g) than other samples calcined at low or high calcination temperatures. The CV curves of 5Sn-doped Co₃O₄/T-350 °C at scan rates of 5–35 mV/s also showed pseudocapacitor behavior and good electrochemical reversibility. Moreover, the prepared novel electrode material has also displayed good rate capability (71.77%) at current density of 1–10 A/g and long-term stability of 92.23% after 3000 cycles. These excellent electrochemical characteristics of 5Sn–Co₃O₄/T-350 °C nanorods verified that it will be highly suitable electrode material for supercapacitor applications.     

Preparation of Co3O4/ZrO2(Y2O3) Catalyst and its Enhanced Catalytic Oxidation of CO

Yttria-stabilized zirconia powders were prepared by the sol–gel method coupled with supercritical CO₂ fluid-drying technology, using ZrOCl₂·8H₂O as the precursor, urea as the precipitant, and yttria as the stabilizer. The particles were characterized by X-ray diffraction, TEM and BET. The Co₃O₄/ZrO₂(Y₂O₃) catalysts were prepared by the impregnation method. The content of cobalt was varied from 5 to 12 wt%. The prepared catalysts were calcined at 200–500 °C and the pretreating temperature was varied from 200–400 °C. The performance of CO catalytic oxidation was tested and the catalyst with 8% Co loading, calcined at 200 °C, and with a pretreating temperature of 300 °C, showed the highest catalytic activity. The temperature for 95% CO conversion was as low as 113 °C; and, the catalyst showed both good cycling stability and excellent long-term stability.     

Magnesium Ferrite (MgFe2O4) Nanostructures Fabricated by Electrospinning

Magnesium ferrite (MgFe₂O₄) nanostructures were successfully fabricated by electrospinning method. X-ray diffraction, FT-IR, scanning electron microscopy, and transmission electron microscopy revealed that calcination of the as-spun MgFe₂O₄/poly(vinyl pyrrolidone) (PVP) composite nanofibers at 500–800 °C in air for 2 h resulted in well-developed spinel MgFe₂O₄ nanostuctures. The crystal structure and morphology of the nanofibers were influenced by the calcination temperature. Crystallite size of the nanoparticles contained in nanofibers increased from 15 ± 4 to 24 ± 3 nm when calcination temperature was increased from 500 to 800 °C. Room temperature magnetization results showed a ferromagnetic behavior of the calcined MgFe₂O₄/PVP composite nanofibers, having their specific saturation magnetization (M _s) values of 17.0, 20.7, 25.7, and 31.1 emu/g at 10 Oe for the samples calcined at 500, 600, 700, and 800 °C, respectively. It is found that the increase in the tendency of M _s is consistent with the enhancement of crystallinity, and the values of M _s for the MgFe₂O₄ samples were observed to increase with increasing crystallite size.     

Electrospun Fe2O3 nanotubes and Fe3O4 nanofibers by citric acid sol‐gel method

Citric acid‐based sol‐gel method has been used to synthesize metal oxides widely. Iron‐based one‐dimensional nanostructured materials, including Fe₂O₃ nanotubes and Fe₃O₄ nanofibers, have been successfully prepared by directly annealing electrospun citric acid‐based precursor fibers under different atmospheres in this study. Thermo‐gravimetric and differential thermal analyses were carried out from room temperature to 800°C under air and argon atmosphere, respectively. The results reveal the formation mechanisms for Fe₂O₃ nanotube and Fe₃O₄ nanofiber. Fe₂O₃ tubular structures with average inner diameter about 500 nm and wall thickness about 20 nm were obtained. Fe₃O₄ nanoparticles were self‐assembled along the one dimensional orientation to form Fe₃O₄ nanofibers with average diameter around 500 nm. The reflection losses as a function of frequency for the samples with 23 and 33 wt% Fe₃O₄ nanofibers in paraffin were examined. The frequency dependence of reflection losses under various matching thicknesses (2, 3, 4, 6 and 8 mm) was simulated. The as‐fabricated Fe₃O₄ nanofibers can be believed to be promising candidates as highly effective microwave absorbers.     

Novel Glass‐Ceramic Composition as Sealant for SOFCs

This work deals with the design, the characterization, and testing of a novel glass‐ceramic to be used as sealant for planar solid oxide fuel cells and its compatibility with Mn_1.5Co_1.5O₄‐coated Crofer22APU. Thermal, sintering, and crystallization behavior and thermo mechanical properties of the sealant are reviewed and discussed, indicating therefore that these compositions can be deposited at 850°C and provide an excellent compatibility with both the Mn_1.5Co_1.5O₄‐coated Crofer22APU and the anode‐supported electrolyte. In particular, Mn_1.5Co_1.5O₄‐coated Crofer22APU/sealant/anode‐supported‐electrolyte joined samples have been submitted to thermal tests (in air atmosphere) from RT to 800°C (SOFC operating temperature) up to 500 h. No interactions, cracks formation, or failure were observed at the Mn_1.5Co_1.5O₄‐coated Crofer22APU/sealant interface and between the glass‐ceramic and the anode‐supported‐electrolyte after 500 h of thermal tests in air atmosphere.     

Factors influencing the PVA polymer-assisted freeze-drying synthesis of Al2O3 nanofibers

Three-dimensional (3D) nanofibrous structured Al₂O₃ was successfully synthesized using the poly (vinyl alcohol) (PVA) polymer-assisted freeze-drying method, and a series of factors that influence fiber performance were investigated in depth. PVA nanofibers were also investigated for the first time. The surface morphology, structure, and other properties of PVA nanofibers, precursor Al₂O₃/PVA nanofibers, and calcined Al₂O₃ nanofibers were characterized by scanning electron microscopy, X-ray diffraction, and nitrogen adsorption measurements. The results showed that Al₂O₃ nanofibers with good performances could be obtained at the optimum conditions where the precursor solution was prepared by boehmite nanoparticles (0.01 wt%) and PVA (0.1 wt%, DP = 500) with a mass ratio of 7: 3, followed by the use of the rapid freezing method at −196 °C under liquid nitrogen in the pre-frozen process; subsequently, calcination was performed at 500 °C for 5 h to form Al₂O₃ nanofibers. The increasing calcination temperature (500 °C–1300 °C) enabled the transformation of the Al₂O₃ crystalline phase from γ-Al₂O₃ to α-Al₂O₃. It also improved the specific surface area from 44.5 m² g⁻¹ for the precursor Al₂O₃/PVA nanofibers to 263.4 m² g⁻¹ for the Al₂O₃ nanofibers calcinated at 500 °C. However, an excessive calcination temperature at 1300 °C was detrimental to the specific surface area, presumably due to sintering or blocking by metal particles. This work provides optimum conditions that make Al₂O₃ nanofibers valuable for further development, and it has the potential for industrial applications.     

Facile synthesis of In2O3 nanoparticles with high response to formaldehyde at low temperature

In₂O₃ nanoparticles with uniform particle size (10-25 nm) were obtained using the facile precipitation strategy at room temperature with following calcined treatment. The gas-sensing performance of In₂O₃ nanoparticles with different calcined temperatures was investigated. The results demonstrated that the In₂O₃ nanoparticles calcined at 500°C exhibited highest sensing response (R_a/R_g = 68.1) to 10 ppm HCHO at 100°C with good selectivity, stability, reproducibility, and ultra-low limit of detection (1 ppm). The results of XPS, UV, and other characterizations indicated that In₂O₃-500 possessed the most absorbed oxygen species, the highest carrier mobility, and lowest band gap energies. Our work offers new insights into the development of sensing materials to the detection of volatile organic compounds (VOCs).     

Effects of calcination temperature on structure and magnetic properties of pure FeCo2O4 powders

A series of FeCo₂O₄ powders was initially synthesized using a hydrothermal method and subsequently calcined at various temperatures to produce the final product. Pure phase FeCo₂O₄ powders can only be formed in the temperature range of 950–1050 °C. In this work, we study the cation occupation, cation valence, bond length and bond angle changes of the pure phase FeCo₂O₄ powders formed in such a narrow temperature range. Octahedral lattice distortion in the pure phase FeCo₂O₄ samples has been observed. More tetrahedral Fe³⁺ and octahedral Co²⁺ are excited and exchanged their sites as the calcination temperature increases from 950 °C to 1000 °C, and part of Co³⁺ ions are reduced to Co²⁺ in the sample calcined at 1050 °C. The structure of the sample calcined at 1000 °C is close to that of the ideal FeCo₂O₄ spinel. Magnetic measurements show that ferrimagnetism and anti-ferromagnetism coexist in the pure phase FeCo₂O₄ samples. Interaction changes between ferrimagnetism and antiferromagnetism caused by the structural changes of the samples have been studied. Due to the pinning of the local anti-ferromagnetism to ferrimagnetism in the sample, the sample shows a Barkhausen jump below 150 K. As the measurement temperature increases further, the system enters into a reentrant spin glass state.     

Solution combustion of spinel CuMn2O4 ceramic pigments for thickness sensitive spectrally selective (TSSS) paint coatings

A series of spinel-type CuMn₂O₄ ceramic pigments were prepared by a facile and low-cost sol-gel solution combustion method and used as cost-effective materials to fabricate thickness sensitive spectrally selective (TSSS) paint coatings by a convenient spray-coating technique. The chemical component, crystalline morphology, and optical property of the copper manganese oxide ceramic pigment could be accurately controlled by altering the annealing temperature. X-ray diffraction (XRD) analysis confirmed that the ceramic pigments annealed at 500 °C for 1 h coincided well with the XRD patterns of crystalline CuMn₂O₄ in the JCPDS database, and there were segregated phases of CuO and Mn₂O₃. Furthermore, the pure spinel CuMn₂O₄ phase could be achieved at 900 °C for 1 h. The copper manganese oxide ceramic pigments could serve as an effective pigment for fabricating the TSSS paint coating, and the TSSS paint coatings based on ceramic pigments calcined at 900 °C showed solar absorptance of 0.895–0.905 and thermal emittance of 0.186–0.310. In addition, the accelerated thermal stability test revealed that the TSSS paint coating exhibited good thermal stability when it was exposed to air at a temperature of 300 °C for 300 h. Hence, the fabricated TSSS paint coating could be used as a solar absorber coating in the low-to-mid temperature domain.     

Preparation of nanostructured porous carbon composite fibers from ferrum alginate fibers

Nano‐microstructured porous carbon composite fibers (Fe₂O₃@C/FeO@C/Fe@C) were synthesized by the thermal decomposition of ferrum alginate fibers. The ferrum alginate fiber precursors were prepared by wet spinning, and calcined at 300–1000°C in high purity nitrogen. The resulting composite fibers consist of carbon coated Fe₂O₃/FeO/Fe nanoparticles and porous carbon fibers. All the prepared nanostructures were investigated using thermal gravimetry, X‐ray diffraction (XRD), Fourier transform infrared spectroscopy, transmission electron microscope (TEM), and nitrogen adsorption–desorption isotherm. The results show that there are five stages in the decomposition process of the ferrum alginate fibers. Transitions between the five stages are affected by the decomposition temperature. XRD results show that maghemite (Fe₂O₃), wüstite (FeO), martensite (Fe) nanoparticles were formed at 300–500°C, 600–700°C, 800–1000°C, respectively. Scanning electron microscopy and TEM results indicate that the composite fibers consist of nanoparticles and porous carbon. The diameter of the nanosized particles increased from 100 to 500 nm with increasing reaction temperature. The nitrogen adsorption–desorption results also show that the composite fibers have a micro‐ and mesoporous structure. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Synthesis and Properties of Boron Doped NaxCo2O4 Nanocrystalline Ceramics

Sodium cobalt oxide (NaCo₂O₄) nanofibers with diameters ranging between 20 and 200?nm were prepared by electrospinning a precursor mixture of PVA/(Na–Co) acetate. This was the first time any such attempt was made. Afterwards, the electrospun nanofibers were subjected to calcination treatment. The characteristics of the fibers were investigated using a Fourier transform infrared spectroscopy, a X-ray diffractometer, and a scanning electron microscopy. The boron doped and undoped NaCo₂O₄ nanofibers calcined at 850?°C were polycrystalline of the γ Na_xCo₂O₄ phase having diameters ranging between 20 and 60?nm with grain sizes of 5–10?nm, and the nanofibers calcined at 800?°C were single crystals having linked particles or crystallites with particle sizes ranging between 60 and 200?nm. The results indicated a significant effect of calcination temperature on the crystalline phase and morphology of the nanofibers. It could be seen in the SEM micrograph of the fibers that when boron was added, this resulted in the formation of cross-linked bright-surfaced fibers. The average fiber diameter for boron doped and undoped fiber mats were 204 and 123?nm, respectively. The grain diameters of boron doped and undoped nanocrystalline sintered powders were measured as 140 and 118?nm, respectively.     

Preparation of Li6Zr2O7 Nanofibers with High Li‐Ion Conductivity by Electrospinning

Li₆Zr₂O₇ nanofibers were synthesized by a simple electrospinning technique. The thermal decomposition behavior, crystal structure, micromorphology, and electrical conductivity of the as‐prepared Li₆Zr₂O₇ nanofibers were characterized. The results show that Li₆Zr₂O₇ nanofibers were of pure phase after calcined at 750°C for 1 h. In addition, the as‐prepared Li₆Zr₂O₇ nanofibers reveal high conductivity in the measured temperature region, which can be attributed to the huge surface and nanosize effect of the nanofiber electrolyte. Moreover, we provide a general method to improve the conductivity of Li‐ion solid electrolyte.     

A novel foam combustion approach for the synthesis of nano-crystalline cobalt oxide powder

This article focuses on the nano-crystalline tricobalt tetraoxide (Co₃O₄) synthesis using the combustion method. The fabrication process involves the combustion a mixture of cobalt nitrate as oxidized and expanded polystyrene (EPS) as a novel fuel. The effects of fuel/oxidizer ratio on the phases formed, Co₃O₄ as a major phase and CoO as an impurity, and the Co₃O₄ crystallite size have been addressed. Based on the thermal analyses data (TGA and DTA), which follow the phase changes during the heat treatment of the parent fuel/oxidizer precursor, the different parent precursors have been calcined at 500?°C. Characterization of the formed solids has been performed using various tools (XRD, FT-IR, SEM, TEM, and XPS). It was concluded that the EPS content, in the combustion precursor mixtures, is a key parameter that controls the phase features of the prepared nanomaterials. CoO impurity was detected for the solids with EPS?>?4?wt%. The crystallite size, morphology, and the surface elemental concentration are influenced by changing the EPS content. The activity of the different powders towards hydrogen peroxide decomposition has been evaluated at the 35–50?°C temperature range.     

Low-temperature sintering and high frequency properties of Cu-modified Co2Z hexaferrite

The low temperature sintering behaviors and high frequency properties of Cu-modified Co₂Z hexaferrites have been investigated. Normally, Cu-modified Co₂Z hexaferrite is difficult to be sintered at temperature lower than 1150 °C. By adding a small amount of sintering aid Bi₂O₃, Cu-modified Co₂Z ceramics with high density (more than 95% theoretical density) have been prepared successfully after sintering below 900 °C. The microstructures and properties are significantly influenced by the sintering temperature, the amount of Bi₂O₃ addition, as well as Cu content. The modified hexaferrite ceramics sintered at 900 °C, exhibited excellent high frequency properties, such as high initial permeability up to 6.6, high quality factor more than 30, high resistivity over 10⁹ Ω cm and good thermal stability. The experimental results show that these materials have a great potential as soft magnetic media for high frequency MLCIs applications.     

Changes in the chemical composition of V2O5-loaded CVC-TiO2 materials with calcination temperatures for NH3-SCR of NOx

In this study, the aim was to evaluate the effect of calcinations temperature on the catalytic activity and chemical composition of V₂O₅/TiO₂. We prepared V₂O₅-loaded CVC-TiO₂ catalysts by a combination of chemical vapor condensation (CVC) and impregnation method at different calcination temperatures. These catalysts were analyzed for their ability to catalyze NH₃-based selective catalytic reduction of NO_x. Compared with V₂O₅ loaded P25-TiO₂ (commercial). V₂O₅/CVC-TiO₂ catalysts calcined above 200 °C exhibited better performance towards NO_x conversion than that by a commercial catalyst prepared using P25-TiO₂ (calcined at 500 °C). In addition, the NO_x conversion rate obtained with the sample calcined at 500 °C gave the best result (90 %) at a reaction temperature of 200 °C. From the XPS results, we observed that the V^4+/5+ ratio was well balanced when the V₂O₅ loaded CVC-TiO₂ sample was calcined at 500 ºC.     

Preparation and electrochemical characterization of LiNi<Subscript>0.8</Subscript>Co<Subscript>0.2</Subscript>O<Subscript>2</Subscript> cathode material by a modified sol–gel method

LiNi_0.8Co_0.2O₂ cathode powders for lithium-ion batteries were prepared by a modified sol–gel method with citric acid as chelating agent and a small amount of hydroxypropyl cellulose as dispersant agent. The structure and morphology of LiNi_0.8Co_0.2O₂ powders calcined at various temperatures for 4 h in air were characterized by means of powder X-ray diffraction analyzer, scanning electron microscope, thermogravimetric analyzer and differential thermal analyzer, and Brunauer–Emmett–Teller specific surface area analyzer. The results show that LiNi_0.8Co_0.2O₂ powders calcined at 800 °C exhibit the best layered structure ordering and appear to have monodispersed particulates surface. In addition, the electrochemical properties of LiNi_0.8Co_0.2O₂ powders as cathode material were investigated by the charge–discharge and cyclic voltammetry studies in a three-electrode test cell. The initial charge–discharge studies indicate that LiNi_0.8Co_0.2O₂ cathode material obtained from the powders calcined at 800 °C shows the largest charge capacity of 231 mAh g⁻¹ and the largest discharge capacity of 191 mAh g⁻¹. And, the cyclic voltammetry studies indicate that Li⁺ insertion and extraction in LiNi_0.8Co_0.2O₂ powders is reversible except for the first cycle.     

High performance multi-layer varistor (MLV) from doped ZnO nanopowders by water based tape casting: Rheology,sintering, microstructure and properties

In this work, we report the fabrication of a high performance multi-layer varistor (MLV) via water based tape casting method using novel compositions of nanomaterials. Bi₂O₃, CaO and Co₃O₄ doped ZnO nanopowders were prepared by solution combustion synthesis (SCS) route, calcined at different temperatures (550, 650, 750 and 850?°C) and characterized by TEM, XRD, SEM and AFM. The nanopowder (crystallite size ~30?nm) calcined at 650?°C for 1?h was used as the starting material for MLV fabrication. Compositions of the slurry containing doped ZnO nanopowders, binder and plasticizer in water solvent were optimized for the fabrication of thick film. The rheological properties of the slurries having different solid loadings were analysed and thick films of various thicknesses (50–500?µm) were prepared by varying the feeding rate of tape casting. The film roughness of 38.3?nm for the thick film made from 40?wt% solid slurry was found to be superior compared to other samples due to the presence of reduced crack and shrinkage. MLV fired at 950?°C for 1.5?h exhibited a coefficient of nonlinearity of 18 and breakdown voltage of 291.5?V that yields superior properties compared to commercial MLVs.     

Carbon nanotube/graphene oxide‐added CaO‐B2O3‐SiO2 glass/Al2O3 composite as substrate for chip‐type supercapacitor

A CaO‐B₂O₃‐SiO₂ (CBS) glass/40 wt% Al₂O₃ composite sintered at 900°C exhibited a dense microstructure with a low porosity of 0.21%. This composite contained Al₂O₃ and anorthite phases, but pure glass sintered at 900°C has small quantities of wollastonite and diopside phases. This composite was measured to have a high bending strength of 323 MPa and thermal conductivity of 3.75 W/(mK). The thermal conductivity increased when the composite was annealed at 850°C after sintering at 900°C, because of the increase in the amount of the anorthite phase. 0.25 wt% graphene oxide and 0.75 wt% multi‐wall carbon nanotubes were added to the CBS/40 wt% Al₂O₃ composite to further enhance the thermal conductivity and bending strength. The specimen sintered at 900°C and subsequently annealed at 850°C exhibited a large bending strength of 420 MPa and thermal conductivity of 5.51 W/(mK), indicating that it would be a highly effective substrate for a chip‐type supercapacitor.     

Preparation and catalytic activity in ethanol combustion reaction of cobalt–iron spinel catalysts

Iron–cobalt spinel catalysts were prepared via the coprecipitation method. The effect of different parameters on textural, structural and catalytic properties, in ethanol combustion, was investigated. The CoFe₂O₄ phase was obtained at calcination temperatures as low as 500 °C and the usage of ammonia as precipitating agent, results in the formation of Fe₂O₃ in addition to the spinel phase. The catalyst prepared using nitrate salts, NaOH as precipitation agent and calcined at 600 °C had the best catalytic performance achieving ethanol complete oxidation at 271 °C.     

Effect of calcination temperature on use of high-boron-content waste for low-temperature wall tile production

The effects of the calcination temperature on raw-colemanite-waste properties and calcined waste content on wall tile production were investigated. Waste containing 11.24% B₂O₃ calcined between 500 and 800°C was added to wall tile granules in various ratios (0–100 wt.%) to produce a low-temperature-sintered wall tile by adding the maximum content of boron waste, as determined through optimal calcination. The low-temperature (850–1000°C) sinterability of the samples and the effect of the calcined colemanite-waste content on the wall tile properties were investigated. The samples were characterised using X-ray fluorescence, X-ray powder diffraction, differential thermal analysis, thermogravimetric analysis, Fourier-transform infrared spectroscopy, scanning electron microscopy, and colourimetry. The waste calcined at 800°C exhibited a substantially different phase distribution, bond structure, morphology, and colour. The wall tile produced using 40 wt.% colemanite waste calcined at 800°C and subsequently sintered at 950°C exhibited the optimal properties. The linear firing shrinkage, water absorption, and flexural strength of the optimised wall tile were 0.88%, 16.04%, and 36.07 MPa, respectively. The optimised wall tile exhibited major albite, quartz, and diopside phases and 64% higher strength. The sample calcined at 800°C showed that high colemanite-waste content could be incorporated into ceramic bodies.