Rise In Calcination Temperature Research Articles

Hydrodeoxygenation of C15 furanic precursor over mesoporous NiMo-ZrO2 composite catalysts for the production of sustainable aviation fuel

Sustainable aviation fuel (SAF) is essential for achieving carbon neutrality in the transportation sector. This study elucidates the production of SAF range C9-C15 branched alkanes by hydrodeoxygenation (HDO) of C15 furanic precursor derived from 2-methylfuran and furfural via hydroxyalkylation-alkylation reaction. HDO reaction was performed using high surface area mesoporous NiMo-ZrO2 composite catalysts that exhibited high selectivity to central SAF alkanes (C13-C14). Deoxygenation follows a complex reaction network involving furanic double bond saturation and furan-ring opening reactions in series, followed by the cascade of HDO, dehydroformylation, and C-C bond cleavage. The present investigation enlightens the impact of calcination temperatures and metal (Mo and Ni) contents on structural stability, physicochemical properties, and catalytic performance of NiMo-ZrO2. Both Ni and Mo stabilized the tetragonal ZrO2 phases with improved surface area. The catalytic activity proliferated with rising calcination temperature till 873 K due to the enrichment of Mo-O-Zr acidic species and deteriorated beyond this temperature owing to the generation of crystalline MoO3/Zr(MoO4)2 species. NiMo alloy formation was enhanced, and concurrently, acidity was reduced with increasing Mo content. 30 wt% MoO3-containing catalyst showed the best catalytic activity due to the proper balance between acidity and NiMo alloy. Oxygenate conversion was boosted by increasing NiO addition up to 15 wt% due to the enhanced Ni and NiMo alloy formation and decreased at 20 wt% owing to the evolution of catalytically inactive bulk metal oxide species. Catalytic cracking was prominent at elevated reaction temperatures, with significant amounts of C13 alkane.

Highly efficient electrocatalytic water oxidation based on non-precious metal oxides/sulfides derived from a FeCoNi-metal organic framework

One of the main challenges for oxygen evolution reaction (OER) is to develop electrocatalysts with high performance, suitable stability, and low cost. First-row transition metal compounds have received attention due to their high electrocatalytic activity and diverse electronic structure. Meanwhile, metal-organic frameworks (MOFs) have emerged as promising alternative for OER due to their porous structure and unsaturated metal sites. In this study, FeCoNi-MOF based on MIL-88B was synthesized by a hydrothermal method. Then, the performance of the catalyst was investigated and improved by calcination and sulfidation at three temperatures of 250 ℃, 350 ℃, and 450 ℃. The phase development and crystal structure parameters of the synthesized samples were confirmed through X-ray diffraction. Additionally, the intensity of the peaks increased with the rise in calcination temperature. Field emission scanning electron microscopy revealed well-defined and uniformly distributed nanorods and nanospheres particles of calcinated and sulfides samples. The weight percentage (wt%) of the elements in the samples were verified to align with their stoichiometric ratios. The synthesized catalysts were loaded onto a nickel foam by a one-step method, and their electrocatalytic properties were examined in the OER process in 1.0 M KOH alkaline solution. The (FeCoNi)-O250 ℃ electrocatalyst, maintaining its nanorod morphology, exhibited an overpotential of 313 mV at a current density of 10 mA.cm-² and a small, stable Tafel slope of 31.5 mV.dec−1 and good charge transfer of 0.73 mF. Cm−2. However, the (FeCoNi)-S250 ℃ electrocatalyst showed better performance in the OER process with an overpotential of 298 mV at a current density of 10 mA.cm-² and a small and stable Tafel slope of 29 mV.dec−1 and good charge transfer of 0.82 mF. Cm−2. In other words, a higher Cdl increased reaction rates or lower overpotentials required for the reaction to occur. Furthermore, the activity of this catalyst remained constant at a fixed current density of 10 mA.cm-² for 18 hours. Based on the electron microscopy observations, and electrochemical evaluations, this superior performance can be attributed to the morphological change from nanorods to porous nanospheres due to sulfidation, resulting in increased electrochemically active sites and decreased charge transfer resistance.

The Effect of Calcination Temperature on the Characteristics of CeO2 Synthesized Using the Precipitation Method

Cerium oxide (CeO2) was synthesized using the precipitation method at various calcination temperatures ranging from 500 to 700°C. Cerium(III) nitrate hexahydrate (Ce(NO)3.6H2O) was used as the precursor for cerium, while Cetyltrimethylammonium bromide (CTAB) acted as the morphology-directing agent. Characterization results indicated that pure CeO2 was obtained at all calcination temperature variations. Calcination temperature influences crystallinity, crystal size, and CeO2 crystal parameters. The crystallinity and crystal size of CeO2 increased with the rising calcination temperature, reaching values of 81.1–84.5% and 15.58–23.12 nm, respectively, along with larger crystal parameters as the temperature increased (a = 5.406–5.410 Å). Surface morphology showed irregular shapes of CeO2 particles, with decreasing sizes as the calcination temperature increased, ranging from 0.2-5.6 μm at 600°C to 0.12-2.9 μm at 700°C. The Ce/O ratio on the surface increased with the rising calcination temperature, reaching a range of 0.48–0.57. CeO2 obtained from calcination at 600°C exhibited the highest fluorescence emission intensity (λ= 496 nm), indicating the least oxygen vacancies presence. Therefore, for antioxidant and catalyst applications, it is preferable to calcinate CeO2 at 700°C.

Synthesis of Cu0.5Zn0.5-xNixFe2O4 nanoparticles as heating agents for possible cancer treatment

Magnetic mixed ferrites with high heating efficacy have attracted lots of attention as a complementary method for cancer treatment via magnetic hyperthermia therapy. In the present study, magnetic Cu0.5Zn0.5-xNixFe2O4 nanoparticles were synthesized via a sol–gel combustion method. The effects of nickel substitution (x = 0.1, 0.2, 0.3, 0.4 and 0.5) on the magnetic and structural properties of the produced nanoparticles were investigated. The produced magnetic nanopowders were studied via X-ray diffraction (XRD), scanning electron microscopy (SEM), simultaneous thermal analysis (STA), Fourier-transform infrared spectroscopy (FTIR), Transmission electron microscopy (TEM), and vibrating-sample magnetometry (VSM) techniques. The results showed that the saturation magnetization and coercivity of ZnCuFe2O4 nanoparticles were strongly affected by nickel substitution in the structure so that saturation magnetization decreased from 55.4 emu/g to 36.0 emu/g, whereas coercivity increased from 87.9 Oe to 156.4 Oe. In addition, saturation magnetization for the Cu0.5Zn0.4Ni0.1Fe2O4 sample increases from 55 to 58.1 emu/g with a rise in calcination temperature from 400 to 700 °C, respectively. The heating efficiency of the samples was investigated under different magnetic fields for magnetic hyperthermia therapy. The Cu0.5Zn0.4Ni0.1Fe2O4 sample exhibits a temperature increase from 37 °C to 49.5 °C during 10 min in the exposure of a magnetic field of 400 Oe and frequency of 200 kHz. The specific absorption rate value calculated for the Cu0.5Zn0.5-xNixFe2O4 nanoparticles was 53.1 W/g. With the increase in the viscosity of the environment, the heating efficiency of nanoparticles is reduced. Despite this decrease, the magnetic characteristics of nanoparticles remained strong enough to envision their usage as heating agents in magnetic hyperthermia.

Calcination temperature dependence of tri-magnetic nanoferrite Ni0.33Cu0.33Zn0.33Fe2O4: Structural, morphological, and magnetic properties

The calcination temperature plays a pivotal role in determining the physical and magnetic properties of ferrite nanoparticles, influencing their performance and applicability in various applications. In this study, Ni0.33Cu0.33Zn0.33Fe2O4 nano ferrites were produced using the coprecipitation method and subsequently calcined at different temperatures, specifically 500 °C, 550 °C, 600 °C, 650 °C, and 700 °C. The X-ray diffraction analysis confirmed the presence of cubic spinel ferrite phase (Fd-3m) and revealed an increase in crystallite size from 12.84 to 20.19 nm as the calcination temperature increased from 500 °C to 700 °C. X-ray photoelectron spectroscopy analysis provided insights into chemical oxidation states. Scanning electron microscopy and transmission electron microscopy images revealed that at higher calcination temperatures, nanoparticles tend to aggregate. This aggregation is associated with an observable rise in particle size, increasing from 18.16 to 29.11 nm for nanoparticles calcined at 500 °C and 700 °C, respectively. Energy-dispersive X-ray confirmed pure elemental compositions. Fourier transform infrared spectroscopy identified red and blue shifts in wavenumbers corresponding to tetrahedral and octahedral group complexes, respectively. Nanoparticles calcined at 700 °C exhibited the highest saturation magnetization (62.642 emu/g) and coercivity (75.27 G), as revealed from the vibrating sample magnetometry analysis. Upon increasing the calcination temperature from 500 °C to 700 °C, the ferromagnetic contribution was improved from 24.26% to 98.64% along with a reduction in superparamagnetic contribution from 75.74% to 1.34%, respectively. The electron paramagnetic resonance (EPR) study showed an increase in the values of g and ΔHpp with the rise in calcination temperature. This observation suggests an enhancement in dipole–dipole interactions. Furthermore, a linear relationship was discovered between the g factor and crystallite size, inducting the formation of single domain. Finally, altering the calcination temperature adjusted the physical and magnetic properties of Ni0.33Cu0.33Zn0.33Fe2O4 nanoparticles. This adjustment indicates their potential for versatile applications, particularly in hyperthermia treatment and as T2 contrast agents in magnetic resonance imaging.

High stable NiCoAl catalyst prepared by combustion method for the hydrodeoxygenation of lignin-derived phenolic compounds: Effect of calcination temperature

The hydrodeoxygenation of lignin-derived phenolic compounds holds great promise for biomass-derived liquid fuel production. However, achieving a consistently high cyclohexane yield poses a formidable challenge. In this study, NiCoAl catalysts were successfully synthesized using the solution combustion method for the hydrodeoxygenation of lignin-oil. The impact of calcination temperature on the preparation of NiCoAl catalysts was investigated. The results indicate that the selectivity of cyclohexane exhibits an initial increase followed by a decrease as the calcination temperature rises. Notably, the NiCoAl-600 catalyst reached 99.99% guaiacol conversion, with the highest selectivity of cyclohexane (97.96%) achieved. Characterization results demonstrate that the transition of the spinel structure from normal to inverse with rising calcination temperature. Moreover, the catalyst particle size initially decreases and then increases, while the oxygen vacancy concentration in the catalyst increases. It was found that these properties contribute to a better hydrodeoxygenation performances of guaiacol and other phenolic compounds over non-noble NiCoAl catalyst. Possible reaction pathway and mechanism are proposed and discussed. Additionally, the spinel-structured NiCoAl-600 catalyst has good thermal stability, ensuring potential application in the upgrading of lignin-oil.

Effect of synthesis temperature on crystal structure, optical and magnetic properties of SmCuO3-δ ceramic phosphor

Effect of synthesis temperature on crystal structure, optical and magnetic properties of SmCuO3-δ ceramic phosphor is investigated in this work. The SmCuO3-δ ceramic has been synthesized using a sol-gel method. Rietveld analysis reveals that SmCuO3-δ ceramic crystallizes into coexisting tetragonal (I4/mmm) and monoclinic (C2/c) crystal structures. The phase fraction of the tetragonal and monoclinic phases strongly depends on the synthesis temperature. The crystallite size and particle size increase with increasing calcination temperature. The X-ray photoelectron spectroscopic spectra reveal the presence of (Cu2+, Cu3+) and (Sm2+, Sm3+) ions alongwith the oxygen vacancy centres in the phosphor. The SmCuO3-δ ceramic shows multiple magnetic phase transitions. The FTIR spectra show the presence of vibrational bands due to Cu-O and Sm-O groups. The optical band gap of the SmCuO3-δ phosphor decreases with an increase in calcination temperature and crystallite size. The photoluminescence excitation spectra show the peaks at 363, 402, 505 and 542 nm at the fixed emission wavelength of 609 nm, whereas the photoluminescence emission spectra contain peaks at 465, 515 and 609 nm at the fixed excitation wavelength of 402 nm. The photoluminescence emission intensity of the sample increases with the rising calcination temperature upto 900 °C and finally, it quenches at 1000 °C. Therefore, the SmCuO3-δ ceramic phosphor may be useful for solid state lighting, LEDs and magnetic devices.

Improvement of the structural, dielectric, ferroelectric, and piezoelectric of PbZr0.52Ti0.48O3 nanopowder features for ultrasonic applications

Smart ferroelectric lead zirconate titanate (PbZr0.52Ti0.48O3) was synthesized in the morphotropic phase boundary by a sol-gel auto-combustion strategy. The as-prepared powder was calcined at three different temperatures, 700, 800, and 900 °C for 3 h, each. The tetragonality of the final product increases with the rise of calcination temperature. Thermal gravimetric analysis and differential thermal gravimetric analysis depicted that complete crystallization of PZT was observed at 400 °C. Structural, vibrational, and microstructure studies were investigated using X-ray diffraction (XRD), Fourier transform infrared spectroscopy, scanning electron microscopy, and energy-dispersive X-ray spectroscopy investigated for grains and elemental analyses and high-resolution transmission electron microscopy (HR-TEM). Results of XRD and HR-TEM were compatible, showing the formation of nanocrystalline powder with coexisting tetragonal and rhombohedral phases. Rietveld refinement of XRD data was carried out using material analysis using diffraction software in order to obtain the lattice constants. For mechanical and electrical measurements, disks were pressed at 10 MPa. The samples were burned out at 500 °C for 1 h and then 1100 °C for 2 h to obtain more dense disks. The surfaces of the disks were coated with silver paste, followed by burning out for almost an hour. Dielectric and piezoelectric characteristics for the fabricated PZT samples were determined in detail. From these analytical techniques and collected data, one can deduce that the sample annealed at 900 °C can be used as an ultrasonic transducer in various metrological applications.

Investigating the impact of calcination temperature on the structural and optical properties of chromium-substituted Mg–Co ferrite nanoparticles

The primary objective of this study is to comprehensively examine how the calcination temperature affects the structural, infrared, and optical properties of Mg0.6Co0.4FeCrO4 compounds. These compounds were synthesized using the sol-gel method and subjected to calcination at two distinct temperatures, namely 900 °C and 1100 °C. The X-ray diffraction measurements confirmed that the compounds adopt a cubic crystal structure with a space group of Fd3¯m. Furthermore, the FTIR analysis of these compounds revealed the presence of an absorption band corresponding to the stretching vibration of the oxygen atom and metal ions within the tetrahedral site. As the calcination temperature increased, various properties showed notable changes. The crystallite size, determined using the Debye-Scherrer equation from the strongest diffraction peak, increased from 48 nm at 900 °C to 56 nm at 1100 °C for the compounds. Additionally, the direct optical band gap energy (Eg) decreased from 1.346 eV to 1.322 eV with the rise in calcination temperature from 900 °C to 1100 °C. Furthermore, the Urbach energy values decreased from 0.491 eV to 0.310 eV as the calcination temperature increased from 900 °C to 1100 °C. The compounds exhibited direct optical transitions as per the absorption coefficient (α) and Tauc's model. The study delved into the impact of calcination temperature on various optical properties. Specifically, the penetration depth, extinction coefficient, and refractive index were thoroughly investigated and their findings interpreted. In addition, the dispersion parameters were examined using the Wemple and DiDomenico single oscillator model and it was discovered that these parameters were significantly influenced by the calcination temperature. Moreover, as the calcination temperature increased, the optical dispersion moments (M−1 and M−3) exhibited a decrease. Finally, the study also explored and interpreted the influence of calcination temperature on the real and imaginary parts of the dielectric permittivity and conductivity of the compounds. These analyses provide valuable insights into how calcination temperature affects the optical characteristics of the studied compounds.

In-situ catalytic upgrading of Hami coal pyrolysis volatiles over acid-modified kaolin

Low-cost kaolin was modified by calcination at different temperatures, followed by HCl leaching, and used as catalyst for in-situ upgrading of Hami coal pyrolysis volatiles in a fixed-bed reactor. The catalyst characteristics, pyrolysis product distributions and tar properties were investigated by multiple methods to understand the relationship between catalyst properties and tar quality. The results indicated that calcination of kaolin promoted the formation of amorphous metakaolin, then the HCl leaching removed most metakaolin framework Al, leading to the production of abundant micro-/mesopores and acid sites. As the rising calcination temperature, the specific surface area and pore volume of acid-modified kaolin (AMK) showed a trend of increasing and then decreasing, and the Brønsted acid sites (BAS) displayed an increasing trend. Compared to non-catalytic pyrolysis, the high specific surface area and certain acid sites of AMKs enhanced the light tar fraction from 37.81 wt% to 43.00–48.45 wt%, and the relative content of aromatics in tar increased from 9.76% to 16.65–22.11%, with monocyclic aromatics, naphthalenes and polycyclic aromatics increasing to 3.5–4.2, 1.2–1.8 and 2.1–3.3 times higher, respectively. AMKs also reduced the content of element O in tar by 17.92–31.54% by promoting the deoxygenation reaction. The tar upgrading performance was determined by the BAS amount and the pore structure of AMKs together. Among all AMKs, AMK800 (calcined at 800 °C and treated by HCl) exhibited the optimum performance for heavy tar conversion, aromatics generation and oxygen removal due to its highest specific surface area and the maximum BAS except AMK900. The acid-modified kaolin has the potential to be an inexpensive and efficient catalyst for future practical applications of upgrading coal pyrolysis tar.

Acidity and Stability of Brønsted Acid Sites in Green Clinoptilolite Catalysts and Catalytic Performance in the Etherification of Glycerol

Natural zeolite clinoptilolite CLIN with a framework ratio of Si/Al ≥ 4 containing mainly potassium and calcium ions in its internal channel system was used as a starting material. The acidic HCLIN catalysts were prepared under soft conditions avoiding the use of environmental less-benign mineral acids. The starting material was ion exchanged using a 0.2 M aqueous ammonium nitrate solution at a temperature 80 °C for 2 h. The obtained NH4CLIN was converted into the acid HCLIN catalyst by calcination at 300–600 °C. The obtained samples were characterized by XRD, FTIR, SEM/TEM, AAS, and EDX element mapping. The state of aluminium and silicon was studied by 27Al- and 29SiMAS NMR spectroscopy. The textural properties of the catalysts were investigated by nitrogen adsorption and desorption measurements. The Brønsted acidity of the HCLIN catalysts was studied by temperature-programmed decomposition of the exchanged ammonium ions releasing ammonia as well as 1H MAS NMR, {1H–27Al} Trapdor, and {1H–27Al} Redor experiments. The strongly agglomerated samples were crystalline and thermally stable up to >500 °C. Although a part of the clinoptilolite framework is maintained up to 600 °C, a loss of crystallinity is already observed starting from 450 °C. The specific surface areas of the starting CLIN and ammonium exchanged NH4CLIN are low with ca. 26 m2/g. The pores are nearly blocked by the exchangeable cations located in the zeolite pores. The thermal decomposition of the ammonium ions by calcination at 400 °C causes an opening of the pore entrances and a markable increase in the specific micropore area and micropore volume to ca. 163 m2/g and 0.07 cm3/g, respectively. It decreases with further rising calcination temperature indicating some structural loss. The catalysts show a broad distribution of Brønsted acid sites (BS) ranging from weak to strong sites as indicated the thermal decomposition of exchanged ammonium ions (TPDA). The ammonium ion decomposition leaving BS, i.e., H+ located at Al–O–Si framework bridges, starts at ≥250 °C. A part of the Brønsted sites is lost after calcination specifically at 500 °C. It is related to the formation of penta-coordinated aluminium at the expense of tetrahedral framework aluminium. The Brønsted sites are partially recreated after repeated ammonium ion exchange. The catalytic performance of the acidic HCLIN catalysts was tested in the etherification of glycerol as a green renewable resource with different C1-C4 alcohols. The catalysts are highly active in the etherification of glycerol, especially with alcohols containing the branched, tertiary alkyl groups. Highest activity is observed with the soft activated catalyst HCLIN300 (300 °C, temperature holding time: 1 min). A total of 78% conversion of glycerol to mono and di ether were achieved with tert-butanol at 140 °C after 4 h of reaction. The mono- and di-ether selectivity were 75% and 25%, respectively. The catalyst can be reused.

Influence of Thermal Activation and Silica Modulus on the Properties of Clayey-Lateritic Based Geopolymer Binders Cured at Room Temperature

In this study, a laterite soil which is a locally available material in many parts of the world was used as the aluminosilicate precursor. The main objective of this study is to investigate the effect of calcination temperature on physicochemical properties of the resulting geopolymers synthesized from calcined laterite soils. In order to produce the geopolymer binders, the laterite soil was activated thermally through calcination (from 550 to 750 °C) and the resulting calcined laterite was activated with an alkali activator composed of 8 and 10 M of sodium hydroxide (NaOH) and sodium silicate (Na2SiO3) in mass of 0.5. Then, the calcined laterite soils and synthesized geopolymer products were analyzed using X-ray diffraction (XRD), Brunner-Emmet-Teller (BET), Fourier Transform Infra-Red (FTIR), X-Ray Fluorescence (XRF), thermogravimetry (TG), scanning electron microscopy (SEM/EDX), and differential scanning calorimetry (DSC). The results from this study indicate that increasing the calcination temperature from 550 to 750 °C resulted in the transformation of phases and an increase in the reactivity of the laterites, resulting in material with improved properties. The use of laterite calcined at 750 °C and activated with 8 M NaOH solution resulted to an increase in the 28 days compressive strength by 35.3 MPa when compared to laterite calcined at 550 °C. Increasing the concentration of the NaOH solution was also found to yield higher material performance. Microstructural investigations showed a heterogeneous compact and dense structure resulting from high polycondensation much pronounced with the rise of calcination temperature from 550 to 750 °C.

Tuning structural and optical properties of copper oxide nanomaterials by thermal heating and its effect on photocatalytic degradation of Congo Red dye

In this study, Copper oxide (CuO) nanoparticles (NPs) were prepared using the chemical co-precipitation method and treated at different calcination temperatures. The synthesized CuO NPs have been calcinated at 300 °C, 500 °C, and 700 °C. The X-ray Diffraction (XRD) results exhibited a decrease in the width of the principle diffraction peak with the temperature rise. Crystallite size was determined by Scherrer’s formula, whereas, Williamson-Hall method presented drastic variation in size indicating the creation of lattice strain with the rise in calcination temperature. Scanning Electron Microscopy (SEM) images showed an increase in grain size and vary from 170 nm – 430 nm. X-ray Energy Dispersive Spectroscopy (EDS) results indicate the formation of CuO NPs and relative Cu contents increased (52.9 to 72.5 Atomic percentage) with temperature. Optical properties are also affected by the calcination temperature and a reduction in bandgap is observed with the increase in temperature. Fourier Transform Infra-red spectroscopy (FTIR) spectra of different samples showed identical bonding behavior and no apparent change in bonding was observed. Photo-degradation of Congo Red dye was performed with CuO NPs treated at different temperatures and NPs treated at 500 °C, have shown maximum degradation efficiency in 75 min under visible light.

The toxicity of SiO2 NPs on cell proliferation and cellular uptake of human lung fibroblastic cell line during the variation of calcination temperature and its modeling by artificial neural network.

The online version contains supplementary material available at 10.1007/s40201-021-00663-4.

Effects of Calcination Temperature on the Phase Composition, Photocatalytic Degradation, and Virucidal Activities of TiO2 Nanoparticles.

The application of TiO2 nanoparticles in the photocatalytic treatment of chemically or biologically contaminated water is an attractive, albeit unoptimized, method for environmental remediation. Here, TiO2 nanoparticles with mixed brookite/rutile phases were synthesized and calcined at 300–1100 °C to investigate trends in photocatalytic performance. The crystallinity, crystallite size, and particle size of the calcined materials increased with calcination temperature, while the specific surface area declined significantly. The TiO2 phase composition varied: at 300 °C, mixed brookite/rutile phases were observed, whereas a brookite-to-anatase phase transformation occurred above 500 °C, reaching complete conversion at 700 °C. Above 700 °C, the anatase-to-rutile phase transformation began, with pure rutile attained at 1100 °C. The optical band gaps of the calcined TiO2 nanoparticles decreased with rising calcination temperature. The mixed anatase/rutile phase TiO2 nanoparticles calcined at 700 °C performed best in the photocatalytic degradation of methylene blue owing to the synergistic effect of the crystallinity and phase structure. The photocatalytic virus inactivation test demonstrated excellent performance against the MS2 bacteriophage, murine norovirus, and influenza virus. Therefore, the mixed anatase/rutile phase TiO2 nanoparticles calcined at 700 °C may be considered as potential candidates for environmental applications, such as water purification and virus inactivation.

Performance of carbon-modified Pd/SBA-15 catalyst for 2-ethylanthraquinone hydrogenation

Abstract Silica SBA-15 without removal of template P123 was calcined in an inert atmosphere and the carbon-modified SBA-15 thus obtained was used as the support of Pd catalyst for the hydrogenation of 2-ethylanthraquinone (EAQ). The effects of extraction times of P123 in SBA-15 with water prior to inert calcination and calcination temperature on the structure and catalytic performance of Pd catalyst were studied. The results of elemental analysis, X-ray diffraction, X-ray photoelectron spectroscopy, inductively coupled plasma, Fourier transform infrared spectroscopy, Raman spectra, water contact angle measurement, N2 adsorption-desorption, transmission electron microscopy and energy dispersive X-ray mapping showed that carbon content of catalysts varied in the range of 3.4 % and 1.1 % with increasing extraction times from 0 to 6 due to the decrease in the residual amount of P123 in uncalcined SBA-15. With rising calcination temperature, the occurrence state of carbon in catalysts was converted from amorphism into graphite. The Pd catalyst supported on SBA-15 extracted for 3 times and calcined at 650 °C had 2.0 % carbon, and exhibited the highest activity (0.37 molH2·gPd−1·min−1) and selectivity (98.9 %). This is due to the presence of appropriate amount of carbon, which provided a relatively high hydrophobicity without significantly reducing the specific surface area and pore size of SBA-15 support. The high hydrophobicity benefits the adsorption of EAQ from the working solution to the surface of catalyst.

Mechanochemical synthesis of ZnO.Al2O3 powders with various Zn/Al molar ratios and their applications in reverse water-gas shift reaction.

ZnO.Al2O3 powders with various Zn/Al molar ratios were prepared via a solid-state reaction using a mechanochemical synthesis method, and the selected powder with a ZnO/Al2O3 molar ratio of 1 was used as support for the preparation of 15% Ni/ZnO.Al2O3 catalyst. The activity of the prepared catalyst was studied in the reverse water-gas shift (RWGS) reaction. The synthesized samples were characterized by XRD, BET, TGA/DTA, TPR, FTIR, and SEM techniques. The results indicated that the prepared powders possessed mesoporous structure with pores having small diameters with crystallite sizes in the nanometer range (6.35-12.08nm). The results showed that the increment in Zn/Al molar ratio reduced the BET area and the pure Al2O3 powder possessed the highest BET area (235.4m2g-1). The results also indicated that the rise of calcination temperature remarkably decreased the BET area. The prepared nickel-based catalyst also exhibited a high activity in RWGS reaction.

Influence of calcination temperature on the evolution of Fe species over Fe-SSZ-13 catalyst for the NH3-SCR of NO

To shed light on the relationships among catalyst calcination temperature, physicochemical properties and catalytic properties of Fe-SSZ-13, a series of catalysts prepared by aqueous post-synthetic exchange and calcined at different temperatures are characterized and evaluated in NH3-SCR reaction. The characterizations and kinetic analysis indicate that the calcination temperature has a great effect on the acidity, Fe species distribution and catalytic properties of the Fe-SSZ-13 catalyst. The rise of calcination temperature decreases the low-temperature activity (< 425℃) and conversely improves the high-temperature activity of Fe-SSZ-13. It could be attributed to the following reasons: under low calcination temperatures, more isolated Fe3+ ions are maintained which can behave as Lewis acid sites and active sites in low reaction temperatures. Simultaneously, stronger surface acidity helps to alleviate NH3 inhibition effect at low temperatures, resulting in good low-temperature activity. On the other hand, the high calcination temperature brings about slight aggregation of isolated Fe3+ to form dimeric/oligomeric Fe clusters, leading more superior high-temperature activity. On the whole, the major active Fe species as well as the contribution of acid sites for low/high temperature activity are different. It could be concluded that the isolated Fe3+ ions and oligomeric Fe clusters are the active sites for low/high SCR reaction temperature, respectively. And zeolite acidity plays a more important role in low-temperature SCR reaction catalyzed by Fe-SSZ-13.

Morphological, structural and optical behaviour of PVA capped binary (NiO)0.5 (Cr2O3)0.5 nanoparticles produced via single step based thermal technique

In this research study, a thermal treatment approach based on a novel single-step has been utilised to addresses the synthesis of binary NiO0.5Cr2O30.5 nanoparticles. Characteristics of these binary metal oxide nanoparticles were examined by employing appropriate characterization tools. Sample patterns of X-ray diffractions were used, calcined with temperature (Temp), set to 500 °C revealed the existence of face-centred cubic (fcc) and hexagonal crystalline structures (hcs). It was noted that with a rising calcination temperature, the nanoparticle dispersal was enhanced further. On the other hand, TEM micrographs have been used to calculate the size of the mean particle. It was found that there was a rising tendency with the increased calcination temperature and this the growth of the mean particle. Increased particle size inherited a rise of nanoparticles' photoluminescence intensity, as suggested by recorded spectra, and various energy band gaps. This result would have been reduced as an effect once calcination temperature was increased. Resulting NiO0.5Cr2O30.5 nanoparticles could be used in the realm of semiconductors and energy applications.

Crystal Structure, Lattice Strain, Morphology, and Electrical Properties of SnO2 Nanoparticles Induced by Low Calcination Temperature

The electrical properties of tin dioxide (SnO2) nanoparticles induced by low calcination temperature were systematically investigated for gas sensing applications. The precipitation method was used to prepare SnO2 powders, while the sol‐gel method was adopted to prepare SnO2 thin films at different calcination temperatures. The characterization was done by X‐ray diffraction, scanning electron microscopy (SEM), and atomic force microscopy (AFM). The samples were perfectly matched with the rutile tetragonal structure. The average crystallite sizes of SnO2 powders were 45 ± 2, 50 ± 2, 62 ± 2, and 65 ± 2 nm at calcination temperatures of 300, 350, 400, and 450°C, respectively. SEM images and AFM topographies showed an increase in particle size and roughness with the rise in calcination temperature. The dielectric constant decreased with the increase in the frequency of the applied signals but increased on increasing calcination temperature. By using the UV‐Vis spectrum, the direct energy bandgaps of SnO2 thin films were found as 4.85, 4.80, 4.75, and 4.10 eV for 300, 350, 400, and 450°C, respectively. Low calcination temperature as 300°C allows smaller crystallite sizes and lower dielectric constants but increases the surface roughness of SnO2, while lattice strain remains independent. Thus, low calcination temperatures of SnO2 are promising for electronic devices like gas sensors.