Mechanochemical Synthesis of Nanocrystalline CeO2: The Effect of Annealing Temperatures on the Particle Size

2006 ◽  
Vol 517 ◽  
pp. 252-256 ◽  
Author(s):  
Abdul Hadi ◽  
Iskandar Idris Yaacob ◽  
Lee Seok Ling

Cerium dioxide (CeO2) nanoparticles were synthesized by a novel mechanochemical process. The precursors of Ce2(CO3)3.xH2O and NaOH were mixed at a weight ratio of 4 to 1. The mixtures were milled using a planetary ball mill with ball to powder ratio of 10:1. The products were then characterized using a battery of characterization methods, including X-ray diffraction (XRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and gas adsorption-desorption measurement. The as-prepared particles were largely amorphous with an average specific surface area of about 119.94 m2/g. Nanocrystalline CeO2 with crystallite size of 4.5 nm was obtained when the sample was annealed in air at 350 oC. The heat treatment results showed that the crystallinity of nanocrystalline CeO2 increased with increasing annealing temperature.

2012 ◽  
Vol 1520 ◽  
Author(s):  
Monica Sorescu ◽  
Tianhong Xu ◽  
Steven Herchko

ABSTRACTDifferential scanning calorimetry, X-ray diffraction, and room temperature Mössbauer spectrum measurements of Fe73.5Cu1Nb3Si13.5B9 (Finemet) alloy have been carried out in order to study its structural and magnetic properties as a function of annealing temperature. The Mössbauer spectra of annealed Finemet alloy could be fitted with 4 or 5 sextets and one doublet at higher annealing temperatures, revealing the appearance of different crystalline phases corresponding to the different Fe sites above the crystallization temperature. The appearance of the nanocrystalline phases at different annealing temperatures was further confirmed by the recoilless fraction measurements. These made use of our recently-developed dual absorber method, which made it possible to determine precisely the recoilless fractions of the amorphous, nanocrystalline and grain boundary phases separately.


Energies ◽  
2019 ◽  
Vol 12 (16) ◽  
pp. 3148 ◽  
Author(s):  
Ziad Abu El-Rub ◽  
Joanna Kujawa ◽  
Esra’a Albarahmieh ◽  
Nafisah Al-Rifai ◽  
Fathieh Qaimari ◽  
...  

Oil shale is an important possible solution to the problem of energy in Jordan. To explore the technical and the economic feasibility of oil shale deposits, numerous samples are analyzed using the standard Fischer Assay (FA) method. However, it would be useful to develop faster, cheaper, and reliable methods for determining the oil content of oil shale. Therefore, the aim of this work was to propose and investigate rapid analytical techniques for the screening of oil shale deposits and to correlate them with the FA method. The Omari deposit located east of Jordan was selected as a case study for analysis using thermogravimetric analysis (TGA) coupled with Fourier-transform infrared (FTIR), differential scanning calorimetry (DSC), elemental analysis, X-ray fluorescence (XRF), X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray (EDX) analysis. Results obtained from the TGA method were linearly correlated with FA with high regression factor (R2 = 0.99); a quadratic correlation (R2 = 0.98) was maintained between the FA and the elemental hydrogen mass content, and a quadratic correlation (R2 = 0.97) was found between the FA and the aliphatic hydrocarbons (FTIR peak at 2927 cm−1) produced in the pyrolysis zone. Although other techniques were less correlated, further investigation might lead to better results. Subsequently, these correlated techniques can be a practical alternative to the conventional FA method when, in particular, specific correlation is made for each deposit.


2006 ◽  
Vol 517 ◽  
pp. 105-110 ◽  
Author(s):  
Abdul Hadi ◽  
Iskandar Idris Yaacob ◽  
Cheah Seok Gaik

Nanocrystalline cerium dioxide (CeO2) has been successfully synthesized by mechanochemical technique at 12, 24, 36, 48 and 60 hours milling times. The starting materials, hydrated cerium carbonate and sodium hydroxide, were mixed in a weight ratio of 4:1 and were milled in a planetary ball mill with ball to powder ratio of 10:1. The high energy impact forces provided by the milling media caused collision of starting materials and allowed the chemical reaction to occur thus produced nanocrystalline cerium dioxide. The products were characterized using a battery of characterization methods, including thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), and gas adsorption-desorption measurement. The nanocrystalline CeO2 with 6.7 nm of crystallite size and specific surface area of 66.66 m2/g was obtained when the sample was milled for 60 hrs and they annealed in air at 350 oC. The result showed that the crystallinity of nanocrystalline CeO2 decreased with increasing milling time.


2015 ◽  
Vol 2015 ◽  
pp. 1-10 ◽  
Author(s):  
L. Guerbous ◽  
A. Boukerika

Cerium trivalent (Ce3+) doped YAG nano-sized phosphors have been successfully synthesized by sol-gel method using different annealing temperatures. The samples have been characterized by X-ray diffraction (XRD), thermogravimetry (TG), differential scanning calorimetry (DSC) analysis, Fourier transform infrared (FTIR) spectroscopy, and steady photoluminescence (PL) spectroscopy. X-ray diffraction analysis indicates that the pure cubic phase YAG was formed and strongly depends on the cerium content and the annealing temperature. It was found that the grain size ranges from 30 to 58 nm depending on the calcination temperature. The YAG: Ce nanophosphors showed intense, green-yellow emission, corresponding to Ce3+5d1→2F5/2,2F7/2transitions and its photoluminescence excitation spectrum contains the two Ce3+4f1→5d1, 5d2bands. The crystal filed splitting energy levels positions 5d1and 5d2and the emission transitions blue shift with annealing temperatures have been discussed. It was found that the Ce3+4f1ground state position relative to valence band maximum of YAG host nanomaterial decreases with increasing the temperature.


2008 ◽  
Vol 23 (11) ◽  
pp. 2880-2885 ◽  
Author(s):  
Herbert Willmann ◽  
Paul H. Mayrhofer ◽  
Lars Hultman ◽  
Christian Mitterer

Microstructure and hardness evolution of arc-evaporated single-phase cubic Al0.56Cr0.44N and Al0.68Cr0.32N coatings have been investigated after thermal treatment in Ar atmosphere. Based on a combination of differential scanning calorimetry and x-ray diffraction studies, we can conclude that Al0.56Cr0.44N undergoes only small structural changes without any decomposition for annealing temperatures Ta ⩽ 900 °C. Consequently, the hardness decreases only marginally from the as-deposited value of 30.0 ± 1.1 GPa to 29.4 ± 0.9 GPa with Ta increasing to 900 °C, respectively. The film with higher Al content (Al0.68Cr0.32N) exhibits formation of hexagonal (h) AlN at Ta ⩾ 700 °C, which occurs preferably at grain boundaries as identified by analytical transmission electron microscopy. Hence, the hardness increases from the as-deposited value of 30.1 ± 1.3 GPa to 31.6 ± 1.4 GPa with Ta = 725 °C. At higher temperatures, where the size and volume fraction of the h-AlN phase increases, the hardness decreases to 27.5 ± 1.0 GPa with Ta = 900 °C.


2013 ◽  
Vol 27 (27) ◽  
pp. 1350153 ◽  
Author(s):  
ALI BAHARI ◽  
REZA GHOLIPUR ◽  
MARYAM DERAKHSHI

Styrene-doped ZrLaO y nanostructures were obtained by sol–gel method low-temperature synthesis. The nanostructures were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), atomic force microscope (AFM) and transmission electron microscopy (TEM) techniques. The observation using SEM and TEM revealed that the ring-shaped nanostructures were very uniform. Further characterization using XRD disclosed that the cohesion of the samples was controllable with annealing temperatures in the range of 800–1500°C. Cohesion property was investigated for the samples. The cohesion increased when increasing the annealing temperature. This was linked to the reinforcement of the oxygen bound on the ZrLaO y nanostructures The shape of nanostructures showed a transformation from a ring-shaped growth mode to a hole-surfaced growth mode with increasing annealing temperature. The styrene-doped ZrLaO y nanostructures with controllable crystallinity will have great potential for various applications in fuel, cells, batteries, electronics devices and chemical sensors.


2003 ◽  
Vol 801 ◽  
Author(s):  
A. Bassetti ◽  
E. Bonetti ◽  
A. L. Fiorini ◽  
J. Grbovic ◽  
A. Montone ◽  
...  

ABSTRACTMagnesium carbon nanocomposites for hydrogen storage have been synthesized by ball milling with different amount of benzene, acting as a lubricant. Their microstructure has been studied by X-ray diffraction and scanning electron microscopy, while the hydrogen desorption temperature has been tested by differential scanning calorimetry. Experimental results show that the microstructure after milling, the hydrogenation capabilities of the material and the reactivity with the air are related to the amount of additives. In particular the carbon to benzene ratio seems to play a major role. In fact, with an optimum value of carbon to benzene weight ratio of 1/6, the amount of carbon being 15 wt% of the milled mixture, a decomposition heat equal to 57% of pure MgH2 was measured, even after air manipulation of the sample.


Chemosensors ◽  
2020 ◽  
Vol 8 (3) ◽  
pp. 79
Author(s):  
Tatiana N. Myasoedova ◽  
Nina K. Plugotarenko ◽  
Tatiana A. Moiseeva

The citrate sol–gel method was utilized for the fabrication of copper-containing films sensitive to NO2 gas. Effect of annealing temperature on the film phase composition, morphology, and sensor response was studied. X-ray diffraction reveals the formation of Cu2Cl(OH)3 phase at 250 °C and the CuO phase at 350 and 500 °C. It was found out that the films annealed at 250 °C and 350 °C showed the best sensor characteristics. The influence of thermal degradation on the probability of percolation effect in films and its connection to a decrease of gas sensitivity was studied. The kinetics of the NO2 gas adsorption on the film’s surface was described following the Elovich model. Activation energy estimated from the ln(S) vs. 1/T plots was 252 and 30 kJ/mol for the films annealed at 250 and 350 °C, respectively.


2000 ◽  
Vol 644 ◽  
Author(s):  
Jörg F. Löffler ◽  
X.-P. Tang ◽  
Yue Wu ◽  
William L. Johnsona

AbstractWe present crystallization studies on Zr41.2Ti13.8Cu12.5Ni10Be22.5 (Vit1) and on other alloys, where the (Zr,Ti) and (Cu,Be) contents, along the line in composition space connecting Vit1 and Zr46.8Ti8.2Cu7.5Ni10Be27.5 (Vit4), were varied. Results from x-ray diffraction (XRD), small-angle neutron scattering (SANS) and differential scanning calorimetry (DSC) are combined to describe the crystallization behavior of these alloys at deep undercooling. SANS gives evidence for decomposition and the formation of nanometer sized crystals below a critical temperature Tc, which varies drastically as a function of composition. When Tc intersects with the glass transition temperature Tg, changes in the crystallization behavior are observed by DSC and XRD. At annealing temperatures near Tg, XRD resolves quasicrystalline phases for all alloy compositions from Vit1 to Vit4. From 9Be nuclear magnetic resonance (NMR) experiments performed on Vit1 upon annealing, we obtain information about the electronic structure and volume fraction of Be containing crystalline and quasicrystalline phases.


2012 ◽  
Vol 557-559 ◽  
pp. 1281-1287 ◽  
Author(s):  
Zhao Wei Feng ◽  
Xu Jun Mi ◽  
Jiang Bo Wang ◽  
Zhi Shan Yuan ◽  
Jin Zhou

Transformation behaviors and texture of Ni47Ti44Nb9 cold-rolled plates were studied by differential scanning calorimetry and X-ray diffraction test. R phase transformation does not occur in Ni47Ti44Nb9cold-rolled plate annealed at 350°C-750°C followed by quenching into the water. Martensite transformation temperature first increases and then decreases with increment of annealing temperature, and the maximum achieves at 700°C. The heat of reverse martensite transformation increases, while hardness decreases as annealing temperature increases. The major texture of cold-rolled plate is {332} and spread from {332} to {110}. When the annealing temperature is above 600°C, the major textures are {332} and {111} recrystallization texture in secondary cold-rolled plate.


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