Annealing effects for calcination of tin oxide powder prepared via homogeneous precipitation

Tin oxide powders were prepared from a homogeneous precipitation using the aqueous solution of SnCl₄ with urea as a precipitator at 90 °C and followed by a calcination process. The calcination was performed using two different methods; conventional furnace annealing (CFA) and rapid thermal annealing (RTA). The crystallization of the tin oxide finished at 600 °C regardless of the calcination method used. The crystallite size increased with as the calcination temperature increased due to the crystal growth and agglomeration. The tin oxide calcined using RTA has a relative smaller crystallite size than CFA at the same temperature. The tin oxide powders calcined with RTA showed higher specific surface areas than those that used CFA over a wide range of temperatures.     

Synthesis and characterization of nanometric gadolinia powders by room temperature solid-state displacement reaction and low temperature calcination

Nanometric-sized gadolinia (Gd₂O₃) powders were obtained by applying solid-state displacement reaction at room temperature and low temperature calcination. The XRD analysis revealed that the room temperature product was gadolinium hydroxide, Gd(OH)₃. In order to induce crystallization of Gd₂O₃, the subsequent calcination at 600 ∼ 1200 °C of the room temperature reaction products was studied. Calculation of average crystallite size (D) as well as separation of the effect of crystallite size and strain of nanocrystals was performed on the basic of Williamson-Hall plots. The morphologies of powders calcined at different temperatures were followed by scanning electron microscopy. The pure cubic Gd₂O₃ phase was made at 600 °C which converted to monoclinic Gd₂O₃ phase between 1400° and 1600 °C. High-density (96% of theoretical density) ceramic pellet free of any additives was obtained after pressureless sintering at 1600 °C for 4 h in air, using calcined powder at 600 °C.     

Phase transformation and nanocrystallite growth behavior of 2 mol% yttria-partially stabilized zirconia (2Y-PSZ) powders

Two mol% yttria-partially stabilized zirconia (2Y-PSZ) precursor powders were obtained through a co-precipitation process using ZrOCl₂.8H₂O and Y(NO₃)₃.6H₂O as starting materials. Phase transformation and crystallite growth behavior have been investigated using X-ray diffraction (XRD), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). XRD results show that the crystal structure to be composed of coexisting tetragonal ZrO₂ (t-ZrO₂) and monoclinic ZrO₂ (m-ZrO₂) when the 2Y-PSZ freeze dried precursor powders was calcined at 773–1273 K for 2 h. The fraction of m-ZrO₂ content is lower than 3.0 % when the calcination temperature is lower than 1073 K, whereas m-ZrO₂ content rapidly increases to 8.7 % with the increase of calcination temperature to 1273 K. The crystallite size of t-ZrO₂ increases from 12.3 to 30.2 nm when calcination temperature increased from 773 to 1273 K. In addition, the activation energy of t-ZrO₂ and m-ZrO₂ crytallite growth in 2Y-PSZ freeze dried precursor powders are 29.2 and 21.8 kJ/mol, respectively.     

Densification of zirconia doped yttria transparent ceramics using co-precipitated powders

Ho:Y₂O₃ ceramics were prepared using co-precipitated powders, with ammonium sulfate as dispersant. Y³⁺ was co-precipitated together with Ho³⁺ and Zr⁴⁺ to produce precursors, which were calcined at 1100–1400 °C to produce yttria-based powders. At calcination temperatures of ≤1300 °C, agglomeration of powders was not observed. When the temperature was increased to 1400 °C, severe agglomeration was detected. Densification was closely related to the calcination temperature: a lower calcination temperature resulted in a faster densification of ceramics to the relative density of 99.7%. The ultimate densification to ~100% was also closely related to powders' impurity level and agglomeration. Grain growth was mainly determined by sintering temperature, but not by the initial crystallite size of powders. The optimal calcination temperature was 1300 °C, at which the obtained Ho:Y₂O₃ powder was free from agglomeration. Using this powder, the resultant Ho:Y₂O₃ ceramics showed pore-free microstructure and good optical transparency.     

Synthesis and characterization of NiO and Ni nanoparticles using nanocrystalline cellulose (NCC) as a template

In this study, nanosized nickel oxide (NiO) and nickel (Ni) powders were synthesised via glycine-nitrate (GN) combustion process, assisted by nanocrystalline cellulose (NCC) as a template. Despite the unique morphology of NCC, it has yet to be applied as a sacrificial bio-template for GN combustion process. In addition, NiO and Ni nanoparticles were obtained at relatively low temperatures in this study, whereby the calcination temperatures were varied from 400 °C to 600 °C, with calcination durations of 2, 4, and 6 h. The morphological analysis of the resulting products were conducted using FESEM, which showed uniformly dispersed NiO and Ni particles with average crystallite size of 25 nm and 27 nm, respectively. These results were confirmed using X-ray diffraction (XRD) technique. The Raman and Fourier transform infrared (FTIR) spectra revealed that the molecular fingerprints of the samples were in agreement with each other. Further analyses revealed that samples calcined at 600 °C for 4 h showed the lowest particle size for pure NiO, whereas the lowest particle size for pure Ni was obtained at 400 °C for 4 h. The TGA results were also consistent with the XRD analysis, whereby pure Ni was initially formed and upon heating, had gradually converted into NiO.     

Effect of calcination temperature on morphology of mesoporous YSZ

A nano-structured mesoporous yttria-stabilized zirconia (YSZ) powders were prepared for the first time using cetyltrimethylammonium bromide (CTAB) as the surfactant and urea as the hydrolyzing agent and using ZrO(NO₃)·6H₂O and Y(NO₃)₃·6H₂O as inorganic precursors. The Brunauer–Emmett–Teller (BET) surface area, Barrett–Joyner–Halender (BJH) pore size distribution and crystallite/particle size of mesoporous YSZ varied with calcine temperatures were studied. Characterizations revealed that the mesoporous YSZ powder calcined at 600 °C was weakly agglomerated and had a high surface area of 137 m²/g with an average grain size of ∼5.8 nm. It was demonstrated that the mesoporous structure remained up to 900 °C. The low-densified YSZ sample with porosity as high as 33% was prepared from mesoporous YSZ powder sintered at 1500 °C for 6 h.     

Ionic–gelation synthesis of gadolinium doped ceria (Ce0.8Gd0.2O1.90) nanocomposite powder using sodium-alginate

Nanocomposite powders of gadolinium-doped ceria (GDC, Ce_0.8Gd_0.2O_1.9) were synthesized via thermal treatment of the gel formed by contacting ionic solutions of sodium alginate as the jelling template and metal (gadolinium/cerium) nitrates as the starting material. The influence of calcination temperature and sodium alginate loading fraction on the properties of the synthesized GDC nanocomposite powders was investigated. Characterization was performed by energy dispersive X-ray spectroscopy, powder X-ray diffraction, thermogravimetric analysis, Field Emission Scanning Electron Microscopy, Fourier transformed infrared spectroscopy and nitrogen adsorption/desorption analysis. It was observed that the particle size and the surface area of the produced GDC nanocomposite powders are dominantly controlled by the calcination temperature, while the effect of sodium alginate loading fraction is limited by the range of the calcination temperature. In this study, the smallest mesoporous GDC nanocomposite powder with cubic fluorite structure (8 nm crystallite size and 3.05±0.005 m²/g surface area) was synthesized using 2 wt% of sodium alginate at a calcination temperature of 550 °C (for 4 h). The results of this study could help to perceive the influence of the basic processing variables on the particle size and the other physiochemical properties of GDC nanocomposite powders produced by the ionic-gelation method.     

Hydrothermal synthesis,magnetic properties and characterization of CoFe2O4 nanocrystals

Magnetic cobalt ferrite (CoFe₂O₄) nanocrystals were synthesized via the hydrothermal method and the crystallite size was measured using Sherrer's equation. Instrumental broadening was a significant parameter for determining crystallite size. The effect of annealing time and calcination on crystallite size and magnetic properties was discussed. It was found that the coercivity was highly dependent on the crystallite size. As the crystallite size increased from 61 to 68.2 nm, room temperature coercivity increased from 1488 Oe to 1700 Oe, while high coercivity (5.2 kOe) was achieved at lower temperature (80 K). It was found that the presence of hematite could affect the crystallite size after calcination.     

Structural,textural, surface chemistry and sensing properties of mesoporous Pr,Zn modified SnO2–TiO2 powder composites

Mesoporous Zn and Pr modified SnO₂-TiO₂ mixed powders (Sn:Ti:Zn:Pr contents 60:20:15:5) have been prepared by a modified sol–gel method involving Tripropylamine (TPA) as chelating agent, TritonX100 as template and Polyvinylpyrrolidone as dispersant and stabilizer, respectively. The obtained gels have been dried at different temperatures and calcined in air at 600 and 800 °C, respectively. Phase identification of the synthesized samples and their evolution with the calcination temperature has been performed by X-ray diffraction. N₂ adsorption/desorption isotherms were found to be characteristic for mesoporous materials, showing relatively low values for the specific surface area (15–32 m² g⁻¹) and nanometric sized pores. In case of the sample calcined at 800 °C, a bimodal pore size distribution can be observed, with maxima at 20 and 60 nm. SEM results demonstrate a porous nanocrystalline morphology stable up to 800 °C. The surface chemistry investigated by XPS reveals the presence of the elements on the surface as well as the oxidation states for the detected elements. At 800 °C a diffusion process of Sn from surface to the subsurface/bulk region accompanied by a segregation of Ti and Zn to the surface is noticed, while Pr content is unchanged. The sensing properties of the prepared powders for CO detection have been tested in the range of 250–2000 ppm and working temperatures of 227–477 °C.     

A novel CO and C3H8 sensor made of CuSb2O6 nanoparticles

Trirutile-type CuSb₂O₆ nanoparticles were synthesized by a simple and economical route, starting from copper nitrate, antimony chloride, ethylenediamine, and ethyl alcohol as solvent. The latter was evaporated by microwave radiation at 140 W. The precursor material was calcined at 200, 300, 400, 500, and 600 °C, and analyzed by powder XRD. The oxide phase was obtained at the last calcination step (600 °C), whose powders were analyzed by field-emission scanning electron (FE-SEM) and transmission electron (TEM) microscopies. Microrods, hexagonal microplates, and nanoparticles with an average size of ~ 51.2 nm were observed. A forbidden bandwidth of 3.41 eV was detected for the direct transition with UV–vis. Tests were carried out on pellets made of the powders in carbon monoxide (CO) and propane (C₃H₈) atmospheres at different concentrations and operating temperatures, obtaining high response at 300 ppm of CO and 500 ppm of C₃H₈, both at 300 °C.     

Sol–gel synthesis of La0.6Sr0.4CoO3−x and Sm0.5Sr0.5CoO3−x cathode nanopowders for solid oxide fuel cells

Nano-powders of La_0.6Sr_0.4CoO_3?x (LSC) and Sm_0.5Sr_0.5CoO_3?x (SSC) compositions, which are being investigated as cathode materials for intermediate temperature solid oxide fuel cells (IT-SOFCs) with La(Sr)Ga(Mg)O_3?x (LSGM) as the electrolyte, were synthesized by low-temperature sol–gel method using metal nitrates and citric acid. Thermal decomposition of the citrate gels was followed by simultaneous DSC/TGA methods. Development of phases in the gels, on heat treatments at various temperatures, was monitored by X-ray diffraction. Sol–gel powders calcined at 550–1000 °C consisted of a number of phases. Single perovskite phase La_0.6Sr_0.4CoO_3?x or Sm_0.5Sr_0.5CoO_3?x powders were obtained at 1200 °C and 1300 °C, respectively. Morphological analysis of the powders calcined at various temperatures was done by scanning electron microscopy. The average crystallite size of the powders was ～15 nm after 700 °C calcinations and slowly increased to 70–100 nm after heat treatments at 1300–1400 °C.     

Chromium substituted copper ferrites via gluconate precursor route

CuFe_2−xCr_xO₄ spinel (0≤x≤2) powders were synthesized by a soft chemistry method—the gluconate multimetallic complex precursor route. The complex precursors were characterized by elemental chemical analysis, infrared (IR) and ultraviolet–visible (UV–vis) spectroscopy, thermal analysis and Mössbauer spectroscopy. The oxide powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), IR, Raman and Mössbauer spectroscopy. It was shown that the structure, morphology and magnetic properties of the obtained spinel powders depend on the concentration of Cr³⁺ ion. The XRD of the chromium substituted copper ferrite powders calcined at 700 °C/1 h indicated the formation of a cubic spinel type structure for x=0.5, 1.0 and a tetragonal structure for x=0, 0.2, 2. The crystallite size ranged from 19 nm to 39 nm. The Mössbauer spectroscopy revealed the site occupancy of iron ions, relative abundance and internal hyperfine magnetic fields in both tetrahedral and cubic CuFe_2−xCr_xO₄ spinels.     

Thermal kinetics and phase stability of 8 mol% samaria doped zirconia nanopowders prepared via reverse coprecipitation

Nanocrystalline samaria (8 mol%) doped zirconium oxide (8SmSZ) was synthesized using reverse co-precipitation technique, the calcination temperature ranging from 873 K to 1273 K for 2 h. XRD structural analysis results confirm the tetragonal(t) nature of the synthesized 8SmSZ nanocrystalline powder. The calculated crystallite size of tetragonal zirconia calcined at 873 K is around 9.0±0.5 nm and with increase in calcination temperature the size increases to 16.0±0.8 nm (1273 K). Thermogravimetric-Differential thermal analysis (TG-DTA) was carried out to study the crystallisation kinetics and growth behaviour of the 8SmSZ. The activation energy for the crystallisation of tetragonal ZrO₂ formation in the 8SmSZ powder was found to be 308.1 kJ/mol by a non-isothermal DTA method. The growth morphology parameter was found to be n=2 indicating two-dimensional growth. The phase stability of the samples after annealing at 1573 K for 100 h was investigated by Raman spectroscopy and it was found that samaria doped zirconia exhibits better phase stability. These preliminary results confirmed the higher phase stability at elevated temperature thereby confirming its suitability in thermal barrier coating (TBC) applications.     

Chemically induced order disorder transition in magnesium aluminium spinel

Magnesium aluminate spinel (MgAl₂O₄) spinel powder was synthesized by nitrate citrate auto-ignition route taking different ratios of nitrate and citrate solution. The ‘as prepared’ black ash was calcined at different temperatures in the range 650–1250 °C for 9 h. Phase evolution of calcined powder samples as studied by X-ray diffraction indicates the presence of disorder at lower calcination temperatures, which transforms to an ordered structure at higher calcination temperatures. Finally, Raman spectroscopy confirms the order–disorder phase transition in spinel sample.     

Synthesis of zinc oxide nanocrystalline powders for cosmetic applications

The synthesis of zinc oxide (ZnO) nanocrystalline powders for cosmetic applications by a coprecipitation process has been investigated. When the Zn(OH)₂ precipitates are calcined at 373 K for 10 min, the crystalline phases comprise the major phase of Zn(OH)₂ and the minor phase of ZnO. XRD pattern shows that only ZnO is present and no other phase is detected when the Zn(OH)₂ precipitates calcined at 413 K for 10 min. The nanocrystallite size of ZnO increases slightly from 32.3 to 44.3 nm when the calcination temperature increases from 413 to 873 K. The activation energy of ZnO nanocrystallite growth is 2.02 kJ/mol, which reveals that the nanocrystalline ZnO is easily grown at low temperature. The UV transmission of ZnO nanocrystallites in the wavelength range from 290 to 375 nm is about 35%, indicating that the ZnO nanocrystallites have an excellent UV-absorbing capability.     

TiO2 nanopowders via radio-frequency thermal plasma oxidation of organic liquid precursors: Synthesis and characterization

TiO₂ nanopowders have been synthesized via Ar/O₂ thermal plasma oxidation of titanium butoxide (TBO) solutions stabilized with diethanolamine (DEA). Experiments were conducted by varying the O₂ input in the plasma sheath (10–90 L/min) and the DEA/TBO molar ratio (R), while keeping the plasma generation power at 25 kW and the reactor pressure at 500 Torr. The resultant powders are mixtures of the anatase and rutile polymorphs in the studied range, whose anatase content and crystallite size exhibit weak dependence on the O₂ input at a fixed R. Increasing R decreases the anatase content, signifying the role of CO gas, generated via oxidation of the organic precursor, on the phase structure. FE-SEM and TEM analysis show that the resultant powders contain majority of nanoparticles (<50 nm) and some large spheres (>100 nm), whose size and/or number tends to decrease at a higher O₂ input, leading to gradually increased specific surface area. Raman spectroscopy reveals no significant differences in the crystallite size and oxygen-vacancy concentration of the nanocrystals by varying the O₂ input.     

The influence of reactive milling on the structure and magnetic properties of nanocrystalline MnFe2O4

Nanocrystalline manganese ferrites (MnFe₂O₄) have been synthesized by direct milling of metallic manganese (Mn) and iron (Fe) powders in distilled water (H₂O). In order to overcome the limitation of wet milling, dry milling procedure has also been utilized to reduce crystallite size. The effects of milling time on the formation and crystallite size of wet milled MnFe₂O₄ nanoparticles have been investigated. It has been observed that single phase 18.4 nm nanocrystalline MnFe₂O₄ is obtained after 24 h milling at 400 rpm. Further milling caused deformation of the structure as well as increased crystallite size. With the aim of reducing the crystallite size of 18.4 nm, MnFe₂O₄ sample dry milling has been implemented for 2 and 4 h at 300 rpm. As a result, the crystallite size has been reduced to 12.4 and 8.7 nm, respectively. Effects of the crystalline sizes on magnetic properties were also investigated. Magnetization results clearly demonstrated that crystallite size has much more effect on the magnetic properties than average particle size.     

Microstructure and mechanical properties of ceramics obtained from chemically co-precipitated Al2O3-GdAlO3 nano-powders with eutectic composition

An efficient and flexible chemical co-precipitation method has been used to synthesize nanoscale Al₂O₃-GdAlO₃ powders with eutectic composition. The as-synthesized powders exhibit a highly dispersive and homogeneous distribution with an average particle size of 50 nm. The phase transition in the resulting powders strongly depends upon the calcination temperature. GdAlO₃ undergoes complete crystallization after calcination at 1050 °C, however, the diffraction peaks of α-Al₂O₃ are found at a relatively high calcination temperature of at least 1300 °C. The fully-densified Al₂O₃-GdAlO₃ ceramic with eutectic composition obtained by hot pressing the nanoscale powders at 1500 °C exhibits a room temperature flexural strength of 556 MPa, a Vickers hardness of 17.3 GPa and a fracture toughness of 7.5 MPa m^1/2. The high temperature flexural strength of the as-sintered Al₂O₃-GdAlO₃ ceramic is measured to be 515 MPa after bending tests at 1000 °C.     

Effect of calcination temperature on the fabrication of transparent lutetium titanate by spark plasma sintering

Transparent lutetium titanate (Lu₂Ti₂O₇) bodies were fabricated by spark plasma sintering using Lu₂O₃ and TiO₂ powders calcined from 700 °C to 1200 °C. No solid-state reaction was identified after calcination at 700 °C, whereas single-phase Lu₂Ti₂O₇ powder was prepared at 1100 and 1200 °C. The calcination at 700 °C promoted densification at the early stages of sintering, whereas residual pores at grain boundaries resulted in Lu₂Ti₂O₇ bodies with low transparency. Low-density and opaque Lu₂Ti₂O₇ bodies formed owing to the coarsening of the powder calcined at 1200 °C. The Lu₂Ti₂O₇ body sintered using the powder calcined at the moderate temperature of 1100 °C had a density of 99.5% with the highest transmittances of 41% and 74% at wavelengths of 550 nm and 2000 nm, respectively.     

Characterization of Ce(1−x)ZrxO2 yellow nanopigments synthesized by a green sol-gel method

In this paper, we report on the synthesis of Ce_(1−x)Zr_xO₂ yellow nanopigments (NPs) by a simple green sol-gel method, using gelatin as the stabilization and polymerization agent. Thermogravimetric analysis (TGA) was employed to obtain the optimum gel calcination temperature. The synthesized Ce_(1−x)Zr_xO₂ powders were characterized by X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM), UV–vis spectroscopy and CIE-L^*a^*b^* measurement. The XRD patterns of the samples calcined at 600 °C revealed the formation of the desired crystal structures without any secondary phases, confirmed by Raman analysis. The TEM images indicated that the pigments' particle shapes are almost spherical with average particle size of about 8 nm. It was found that by increasing Zr⁺⁴ concentrations the absorption edge of the produced NPs have a red-shift. The produced NPs had brilliant yellow colour, derived from CIE-L^*a^*b^* coordinates.