Effect of drying environment on grain size of titanium dioxide nano-powder synthesized via sol-gel method

NASA Astrophysics Data System (ADS)

Zandi, Pegah; Hosseini, Elham; Rashchi, Fereshteh

2018-01-01

Titanium dioxide Nano powder has been synthesized from titanium isopropoxide (TTIP) in chloride media by sol-gel method. In this research, the effect of the drying environment, from air to oven drying at 100 °C, calcination time and temperature on nano TiO2 grain size was investigated. The synthesized powder was analyzed by x-ray diffraction and scanning electron microscope. Based on the results, the powder has been crystallized in anatase and rutile phases, due to different calcination temperatures. At temperatures above 600 °C, the Titanium dioxide nano powder has been crystallized as rutile. The crystalline structure of titanium dioxide nano powder changed because of the different calcination temperatures and time applied. The average particle size of the powder dried in air was larger than the powder dried in oven. The minimum particle size of the powder dried in air was 50 nm and in the oven was 9 nm, observed and calculated Williamson-Hall equation. All in all, with overall increasing of calcination time and temperature the grain size increased. Moreover, in the case of temperature, after a certain temperature, the grain size became constant and didn't change significantly.

The effect of heat treatment on the performance of the Ni/(Zr-Sm oxide) catalysts for carbon dioxide methanation

NASA Astrophysics Data System (ADS)

Takano, Hiroyuki; Izumiya, Koichi; Kumagai, Naokazu; Hashimoto, Koji

2011-07-01

The active catalysts for methane formation from the gas mixture of CO 2 + 4H 2 with almost 100% methane selectivity were prepared by reduction of the oxide mixture of NiO and ZrO 2 prepared by calcination of aqueous ZrO 2 sol with Sm(NO 3) 3 and Ni(NO 3) 2. The 50 at%Ni-50 at%(Zr-Sm oxide) catalyst consisting of 50 at%Ni-50 at%(Zr + Sm) with Zr/Sm = 5 calcined at 650 or 800 °C showed the highest activity for methanation. The active catalysts were Ni supported on tetragonal ZrO 2, and the activity for methanation increased by an increase in inclusion of Sm 3+ ions substituting Zr 4+ ions in the tetragonal ZrO 2 lattice as a result of an increase in calcination temperature. However, the increase in calcination temperature decreased BET surface area, metal dispersion and hydrogen uptake due to grain growth. Thus, the optimum calcination temperature existed.

Al3+ environments in nanostructured ZnAl2O4 and their effects on the luminescence properties.

PubMed

da Silva, Alison A; Gonçalves, Agnaldo S; Davolos, Marian R; Santagneli, Silvia H

2008-11-01

Single-phase zinc aluminate (ZnAl2O4) with the spinel structure was successfully obtained by the Pechini method at different calcining temperatures for 4 hours. The nanoparticles are highly crystalline with no impurities related to ZnO or Al2O3 residues. The microstructural environment of aluminium ions changes with heat treatment temperature, as observed by Fourier transform infrared spectroscopy. The spinel structure might present two different AlO6 sites as evidenced by 27Al solid-state magic-angle-spinning nuclear magnetic resonance spectra. Some AlO4 sites were also detected for samples calcined at a temperature lower than 900 degrees C. The photoluminescence spectra show that the emission can be tuned depending on the calcining temperature. This effect was discussed on the basis of symmetry and oxygen vacancies.

The effect of calcination temperature on the microstructure and photocatalytic activity of TiO2-based composite nanotubes prepared by an in situ template dissolution method

NASA Astrophysics Data System (ADS)

Fan, Jiajie; Zhao, Li; Yu, Jiaguo; Liu, Gang

2012-09-01

TiO2-based composite nanotubes, based on an in situ template dissolution method, were one-step fabricated in a mixed aqueous solution of ammonium hexafluorotitanate and boric acid using ZnO nanorods as templates, and then the samples were calcined at different temperatures. The photocatalytic activity of the samples was evaluated by photocatalytic decoloration of Methyl Orange (MO) aqueous solution at ambient temperature under UV light. The results showed that the prepared sample possessed nanoscale tubular morphology with a wall thickness of ca. 30-50 nm, inner diameters of ca. 50-150 nm and lengths of ca. 400-2000 nm. The calcined samples exhibited excellent stabilization of the anatase phase in a wide temperature range of 300-800 °C. The un-calcined and calcined samples possessed hierarchically macro-mesoporous structures. The sample calcined at 600 °C exhibited the highest photocatalytic activity, corresponding to the maximal formation rate of \\z.rad OH on the photocatalyst. This is attributed to the improvement of anatase TiO2 crystallization, the formation of multi-phase structures including anatase, cubic Zn2TiO4, hexagonal ZnTiO3 and cubic ZnTiO3, and the presence of hierarchically macro-mesoporous structures.

Effect of calcination temperature on microstructure and magnetic properties of Ni{sub 0.5}Zn{sub 0.25}Cu{sub 0.25} Fe{sub 2}O{sub 4} nanoparticles synthesized by sol-gel method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pransisco, Prengki, E-mail: prengkipransisco@gmail.com, E-mail: afza@petronas.com.my; Shafie, Afza, E-mail: prengkipransisco@gmail.com, E-mail: afza@petronas.com.my; Guan, Beh Hoe, E-mail: beh.hoeguan@petronas.com.my

2014-10-24

This paper examines the effect of calcination process on the structural and magnetic properties material nanostructure composite of Ni{sub 0Ð}œ‡{sub 5}Zn{sub 0Ð}œ‡{sub 25}Cu{sub 0.25} Fe{sub 2}O{sub 4} ferrites. The samples were successfully prepared by sol-gel method at different calcination temperature, which are 600°C, 700°C, 800°C and 900°C. Morphological investigation, average crystallite size and microstructure of the material were examined by using X-ray diffraction (XRD) and confirmed by high resolution transmission electron microscope (HRTEM) and field emission scanning electron microscope (FESEM). The effects of calcination temperature on the magnetic properties were calculated by using vibrating sample magnetometer (VSM). The XRD resultmore » shows single-phase cubic spinel structure with interval average size 5.9-38 nm, and grain size microstructure of the material was increasing with temperature increases. The highest magnetization saturation was reached at a temperature 800°C with value 53.89 emu/g, and the value coercive force (Hc) was inversely with the grain size.« less

Effect of calcination temperature on the microstructure and electronic properties of TiO2-ZnO nanocomposites and implications on photocatalytic activity

NASA Astrophysics Data System (ADS)

Menon, N. Gayathri; Tatiparti, Sankara Sarma V.; Mukherji, Suparna

2018-04-01

TiO2-ZnO nanocomposites with a constant Ti:Zn molar ratio of 1:0.1 were prepared via sol-gel process followed by calcination at 300, 400, 500, 600, and 700 °C. The structural and compositional characterizations of these nanocomposites were performed through XRD, FTIR, SEM, and EDAX. Bandgap was measured using DRS. Photocatalytic performance of the nanocomposites was evaluated by decolorization of methyl orange dye under UV and visible irradiation with and without aeration. The results showed that increase in calcination temperature resulted in nanocomposites with well-defined morphology. Although the particle size increased with increase in calcination temperature, the crystallinity of the particles also increased, resulting in enhanced photocatalytic activity. A temperature-dependent anatase-to-rutile phase transformation was observed in TiO2-ZnO nanocomposite beyond 600 °C. The calcination temperature influenced both dye adsorption on the nanocomposites and also dye decolorization by photocatalysis. Even when present at low molar concentration, ZnO in the nanocomposite caused sufficient decrease in bandgap (2.6 eV) at temperatures as low as 400 °C, such that visible irradiation could cause dye decolorization. However, the best decolorization performance was observed in the presence of the nanocomposite calcined at 600 °C. Aerated systems showed better performance in all cases. Desorption of the dye remaining adsorbed on the nanocomposite at the end of the photocatalytic reaction, confirmed that adsorption accounted for only 6.6 and 3% of dye removal in the nanocomposites calcined at 600 °C with UV and visible irradiation, respectively. However, in other systems, ignoring adsorption may cause significant overestimation in photocatalytic loss of dye from the system.

Effect of ph Value and Calcination Temperature on Structure and Magnetic Properties of Strontium Hexaferrite Thin Film

NASA Astrophysics Data System (ADS)

Shanaghi, A.

2012-02-01

Strontium hexaferrite was widely used in the fabrication of commercial permanent magnets and certain microwave devices. In this study, the strontium hexaferrite nanoparticle coatings were prepared by sol-gel method and using spin coating process on silicon substrate, then the effect of pH value, such as 5, 7 and 9, and calcination temperatures, such as 600°C, 800°C, and 1000°C, on structural and magnetic properties of strontium hexaferrite thin films were investigated by XRD, SEM and VSM measurements. The maximum saturation magnetization value of 57.43 emu/g and coercivity value of 3908 Oe were achieved for the thin film with crystallite size approximately 41 nm, prepared at pH value of 7 and calcinations temperature of 800°C.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bundy, R.D.; Alderfer, R.B.

Bench-scale tests of the direct calcination process for Portsmouth were conducted using batch pot calcination of simulated and actual raffinate wastes. These studies included investigation of the evaporation step needed to concentrate the raffinate before calcination. Tests were conducted at calcination temperatures of 600, 700, 1000, and 1200/sup 0/F with two levels of evaporative concentration before calcination at 1000/sup 0/F. Evaporation only tests were also made. Performance of the bench-scale system was excellent. A calcination temperature of 715/sup 0/F indicated that 80 to 100% of the Tc was retained in the calcined solids, while all of the nitrates were decomposedmore » to oxides. With calcination temperatures of greater than or equal to 1000/sup 0/F, part of the Tc escaped from the calcination pot to the scrubber. Below 700/sup 0/F, not all of the nitrates were decomposed to oxides. Most of the U remained in the calcined solids for calcination temperatures of less than or equal to 1000/sup 0/F. The mass of solids remaining after calcination was 4 to 5% of the original raffinate for calcination temperatures from 700 to 1000/sup 0/F. Flow rate through the off-gas treatment system was variable. The water scrubber had a good removal efficiency for nitrate and most metals, but not for uranium. The trapping efficiency of the limestone trap for nitrate was low. Flowsheet studies indicate that enough U would pass through the scrubber and chemical traps to cause an unacceptably high release of radioactivity if the assay of the uranium exceeded 33%. A small HEPA filter after the limestone chemical traps is recommended to reduce U emissions. A flowsheet was developed for a full-scale process for the direct calcination of raffinate waste.« less

Catalytic property of fiber media supported palladium containing alloy nanoparticles and electrospun ceramic fibers biodurability study

NASA Astrophysics Data System (ADS)

Shin, Hyeon Ung

The nanoscale of the supporting fibers may provide enhancements such as restricting the migration of metal catalyst particles. In this work, palladium nanoparticle doped alumina fibers were electrospun into template submicron fibers. These fibers were calcined at temperatures between 650°C and 1150°C to vary the crystal structures of the calcined fibers with the Pd particle size. Higher calcination temperatures led to higher reaction temperatures from 250 to about 450°C for total conversion, indicating the effective reactivity of the fiber-supported catalysts decreased with increase in calcination temperature. Pd-Au alloy nanoparticle doped titania fibers were also fabricated using an electrospinning method and assembled into a fibrous porous medium structure by a vacuum molding process. In reactor tests, the fiber media with Pd-Au alloy nanoparticle catalyst had greater reactivity in conversion of NO and CO gases than that of fiber media with Pd monometallic catalyst alone, attributed to a lower activation energy of the Pd-Au catalyst particles. In carbon monoxide oxidation reaction tests, the results showed that the performance was optimal for a catalyst of composition Pd2Au1 molar ratio that was active at 125°C, which had higher dispersion of active components and better catalytic performance compared to monometallic particle Au/TiO 2 and Pd/TiO2 fiber media. Moreover, the improved reaction activity of Pd2Au1/TiO2 fiber medium was attributed to a decreased in the activation energy. Further experiments were conducted using the electrospun ceramic fibers biodurability study. The properties of nano-sized fiber structures have attracted the attention of recent research on ceramic nanostructures as nonwoven media for applications in hazardous chemical and high temperature environments. However, health and safety concerns of micro and nano scale ceramic materials have not been fully investigated. Little is known about the physicochemical effects of the properties of small alumina fibers, including fiber sizes, surface morphologies, crystalline, phases, and surface areas with respect to submicron sized alumina fibers formed by calcination of electrospun polymeric fibers. Therefore, in this work, sub-micron sized alumina fibers were fabricated by electrospinning and calcination of a polymer template fiber. In the calcination step, different controlled temperature heating cycles were conducted to obtain fibers of different crystalline structures. Their biodurabilities were evaluated in two types of artificial lung fluids (i.e., mimicking the airway and alveolar macrophages). Though the variation in the soak temperature, their dissolution half times were not significantly affected. The solubility half-times of the alumina fibers were shortest for fibers calcined at the fastest temperature ramp rate (though soak temperature did not have an effect).

Bismuth doping effect on crystal structure and photodegradation activity of Bi-TiO2 nanoparticles

NASA Astrophysics Data System (ADS)

Wu, Ming-Chung; Chang, Yin-Hsuan; Lin, Ting-Han

2017-04-01

The bismuth precursor is adopted as dopant to synthesize bismuth doped titanium dioxide nanoparticles (Bi-TiO2 NPs) with sol-gel method following by the thermal annealing treatment. We systematically developed a series of Bi-TiO2 NPs at several calcination temperatures and discovered the corresponding crystal structure by varying the bismuth doping concentration. At a certain 650 °C calcination temperature, the crystal structure of bismuth titanate (Bi2Ti2O7) is formed when the bismuth doping concentration is as high as 10.0 mol %. The photocatalytic activity of Bi-TiO2 NPs is increased by varying the doping concentration at the particular calcination temperature. By the definition X-ray diffraction (XRD) structural identification, a phase diagram of Bi-TiO2 NPs in doping concentration versus calcination temperature is provided. It can be useful for further study in the crystal structure engineering and the development of photocatalyst.

The effect of calcination temperature on the performance of Co3O4-Bi2O3 as a heterogeneous catalyst of peroxymonosulfate

NASA Astrophysics Data System (ADS)

Zhang, Guangshan; Hu, Limin; Wang, Peng; Yuan, Yixing

2017-11-01

In this work, a time-saving microwave-assisted method for synthesis of Co3O4-Bi2O3 was reported. The synthesized Co3O4-Bi2O3 samples were characterized with different techniques to probe their crystalline structures and morphologies. The catalytic performances of synthesized Co3O4-Bi2O3 as peroxymonosulfate activator were evaluated by the degradation of bisphenol A. The effect of calcination temperature on Co3O4-Bi2O3 products was explored and the result showed that the sample calcined at 400 °C possessing superior catalytic activity.

Compositional inhomogeneityand segregation in (K 0.5Na 0.5)NbO 3 ceramics

DOE PAGES

Chen, Kepi; Tang, Jing; Chen, Yan

2016-03-11

The effects of the calcination temperature of (K 0.5Na 0.5)NbO 3 (KNN) powder on the sintering and piezoelectric properties of KNN ceramics have been investigated in this report. KNN powders are synthesized via the solid-state approach. Scanning electron microscopy and X-ray diffraction characterizations indicate that the incomplete reaction at 700 °C and 750 °C calcination results in the compositional inhomogeneity of the K-rich and Na-rich phases while the orthorhombic single phase is obtained after calcination at 900 °C. During the sintering, the presence of the liquid K-rich phase due to the lower melting point has a significant impact on themore » densification, the abnormal grain growth and the deteriorated piezoelectric properties. From the standpoint of piezoelectric properties, the optimal calcination temperature obtained for KNN ceramics calcined at this temperature is determined to be 800 °C, with piezoelectric constant d 33=128.3 pC/N, planar electromechanical coupling coefficient k p=32.2%, mechanical quality factor Q m=88, and dielectric loss tan δ=2.1%.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Kepi; Tang, Jing; Chen, Yan

The effects of the calcination temperature of (K 0.5Na 0.5)NbO 3 (KNN) powder on the sintering and piezoelectric properties of KNN ceramics have been investigated in this report. KNN powders are synthesized via the solid-state approach. Scanning electron microscopy and X-ray diffraction characterizations indicate that the incomplete reaction at 700 °C and 750 °C calcination results in the compositional inhomogeneity of the K-rich and Na-rich phases while the orthorhombic single phase is obtained after calcination at 900 °C. During the sintering, the presence of the liquid K-rich phase due to the lower melting point has a significant impact on themore » densification, the abnormal grain growth and the deteriorated piezoelectric properties. From the standpoint of piezoelectric properties, the optimal calcination temperature obtained for KNN ceramics calcined at this temperature is determined to be 800 °C, with piezoelectric constant d 33=128.3 pC/N, planar electromechanical coupling coefficient k p=32.2%, mechanical quality factor Q m=88, and dielectric loss tan δ=2.1%.« less

Calcination temperature effect on the microstructure and dielectric properties of M-type strontium hexagonal ferrites

NASA Astrophysics Data System (ADS)

Mohammed, J.; Sharma, Jyoti; Kumar, Sachin; Trudel, T. T. Carol; Srivastava, A. K.

2017-07-01

M-type hexagonal ferrites have found wide application in electronics industry due to the possibility of tuning properties such as dielectric properties. An improved dielectric property is useful in high frequency application. In this paper, we studied the effect of calcination temperature on structural and dielectric properties of Al-Mn substituted M-type strontium hexagonal ferrites with chemical composition Sr1-xAlxFe12-yMnyO19 (x=0.3 and y=0.6) synthesized by sol-gel auto-combustion method. The prepared sample was sintered at four different temperatures (T=750°C, 850°C, 950°C and 1050°C) for 5 hours. Characterisations of the synthesized samples were carried out using X-ray diffraction (XRD), impedance analyser, field emission electron microscope (FE-SEM) and energy dispersive X-ray (EDX) spectroscopy. The dielectric properties were explained on the basis of Koop's phenomenological theory and Maxwell Wagner theory. The sample calcinated at 750°C shows the highest value of dielectric constant and AC conductivity whereas that calcinated at 1050°C exhibit the lowest dielectric losses.

Effect of composition and calcination temperature of ceria-zirconia-alumina mixed oxides on catalytic performances of ethanol conversion

NASA Astrophysics Data System (ADS)

Chuklina, S. G.; Maslenkova, S. A.; Pylinina, A. I.; Podzorova, L. I.; Ilyicheva, A. A.

2017-02-01

In the present study, we investigated the effect of preparation method, phase composition and calcination temperature of the (Ce-TZP) - Al2O3 mixed oxides on their structural features and catalytic performance in ethanol conversion. Ceria-zirconia-alumina mixed oxides with different (Ce+Zr)/Al atomic ratios were prepared via sol-gel method. Catalytic activity and selectivity were investigated for ethanol conversion to acetaldehyde, ethylene and diethyl ether.

Investigation of the processing conditions for the synthesis of rod-shaped LiCoO2

NASA Astrophysics Data System (ADS)

Kim, Taejoong; Kim, Yongseon

2018-07-01

We investigate the processing conditions for the synthesis of rod-shaped LiCoO2 (LCO) by a solid-state calcination of a precursor material which was prepared by a hydrothermal method. The rod-like morphology appeared to be easily broken due to the growth of primary crystals recrystallized during the calcination process. Therefore, it is crucial to maintain the temperature under a certain limit. However, the temperature must be high enough to obtain proper crystallinity of the LCO, ideally above 800 °C. Thus, we determined the optimal calcination temperature condition from the common range of temperatures that satisfies both these limiting conditions. The precursor with average diameter of 1 µm sustained the rod shape at calcination temperatures of up to 900 °C; therefore, the optimum calcination temperature could be determined between 800 and 900 °C. Whereas, a proper calcination temperature could not be found for the precursor with 500 nm of diameter because the rod shape did not maintain even at 700 °C. Thus, the maximum temperature at which the rod shape is retained decreases with smaller diameter of the precursor rods, indicating adjusting the diameter above a limiting value is necessary to prepare LCO rod by conventional solid state calcination.

Synthesis of zirconium dioxide by ultrasound assisted precipitation: effect of calcination temperature.

PubMed

Prasad, Krishnamurthy; Pinjari, D V; Pandit, A B; Mhaske, S T

2011-09-01

Nanostructured zirconium dioxide was synthesized from zirconyl nitrate using both conventional and ultrasound assisted precipitation in alkaline medium. The synthesized samples were calcinated at temperatures ranging from 400°C to 900°C in steps of 100°C. The ZrO(2) specimens were characterized using X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The thermal characteristics of the samples were studied via Differential Scanning Calorimetry-Thermo-Gravimetry Analysis (DSC-TGA). The influence of the calcination temperature on the phase transformation process from monoclinic to tetragonal to cubic zirconia and its consequent effect on the crystallite size and % crystallinity of the synthesized ZrO(2) was studied and interpreted. It was observed that the ultrasound assisted technique helped to hasten to the phase transformation and also at some point resulted in phase stabilization of the synthesized zirconia. Copyright © 2011 Elsevier B.V. All rights reserved.

Recovery of SO2 and MgO from By-Products of MgO Wet Flue Gas Desulfurization.

PubMed

Yan, Liyun; Lu, Xiaofeng; Wang, Quanhai; Guo, Qiang

2014-11-01

An industrial demonstration unit using natural gas as a heat source was built to calcine the by-products of MgO wet flue gas desulfurization from power plants; influencing factors on the SO 2 content in calciner gas were comprehensively analyzed; and an advantageous recycling condition of MgO and SO 2 from by-products was summarized. Results showed that the SO 2 content in the calciner gas was increased by more than 10 times under a lower excess air coefficient, a higher feed rate, a lower crystal water in by-products, and a higher feed port position. For the tests conducted under the excess air coefficient above and below one, the effect of the furnace temperature on the SO 2 content in the calciner gas was reversed. Results of activity analysis indicate that particles of MgO generated under the calcination temperature of 900-1,000°C had a high activity. In contrast, due to the slight sintering, MgO generated under the calcination temperature of 1,100°C had a low activity. To recycle SO 2 as well as MgO, a temperature range of 900-927°C for TE103 is proposed. These studies will prompt the desulfurization market diversification, reduce the sulfur's dependence on imports for making sulfuric acid, be meaningful to balance the usage of the natural resource in China, and be regarded as a reference for the development of this technology for other similar developing countries.

Cyclic carbonation calcination studies of limestone and dolomite for CO{sub 2} separation from combustion flue gases - article no. 011801

DOE Office of Scientific and Technical Information (OSTI.GOV)

Senthoorselvan, S.; Gleis, S.; Hartmut, S.

2009-01-15

Naturally occurring limestone and dolomite samples, originating from different geographical locations, were tested as potential sorbents for carbonation/calcination based CO{sub 2} capture from combustion flue gases. Samples have been studied in a thermogravimetric analyzer under simulated flue gas conditions at three calcination temperatures, viz., 750{sup o}C, 875{sup o}C, and 930{sup o}C for four carbonation calcination reaction (CCR) cycles. The dolomite sample exhibited the highest rate of carbonation than the tested limestones. At the third cycle, its CO{sub 2} capture capacity per kilogram of the sample was nearly equal to that of Gotland, the highest reacting limestone tested. At the fourthmore » cycle it surpassed Gotland, despite the fact that the CaCO{sub 3} content of the Sibbo dolomite was only 2/3 of that of the Gotland. Decay coefficients were calculated by a curve fitting exercise and its value is lowest for the Sibbo dolomite. That means, most probably its capture capacity per kilogram of the sample would remain higher well beyond the fourth cycle. There was a strong correlation between the calcination temperature, the specific surface area of the calcined samples, and the degree of carbonation. It was observed that the higher the calcination temperature, the lower the sorbent reactivity. For a given limestone/dolomite sample, sorbents CO{sub 2} capture capacity depended on the number of CCR cycles and the calcination temperature. According to the equilibrium thermodynamics, the CO{sub 2} partial pressure in the calciner should be lowered to lower the calcination temperature. This can be achieved by additional steam supply into the calciner. Steam could then be condensed in an external condenser to single out the CO{sub 2} stream from the exit gas mixture of the calciner. A calciner design based on this concept is illustrated.« less

Molybdenum carbide supported nickel-molybdenum alloys for synthesis gas production via partial oxidation of surrogate biodiesel

NASA Astrophysics Data System (ADS)

Shah, Shreya; Marin-Flores, Oscar G.; Norton, M. Grant; Ha, Su

2015-10-01

In this study, NiMo alloys supported on Mo2C are synthesized by wet impregnation for partial oxidation of methyl oleate, a surrogate biodiesel, to produce syngas. When compared to single phase Mo2C, the H2 yield increases from 70% up to >95% at the carbon conversion of ∼100% for NiMo alloy nanoparticles that are dispersed over the Mo2C surface. Supported NiMo alloy samples are prepared at two different calcination temperatures in order to determine its effect on particle dispersion, crystalline phase and catalytic properties. The reforming test data indicate that catalyst prepared at lower calcination temperature shows better nanoparticle dispersion over the Mo2C surface, which leads to higher initial performance when compared to catalysts synthesized at higher calcination temperature. Activity tests using the supported NiMo alloy on Mo2C that are calcined at the lower temperature of 400 °C shows 100% carbon conversion with 90% H2 yield without deactivation due to coking over 24 h time-on-stream.

Effects on structural, optical, and magnetic properties of pure and Sr-substituted MgFe2O4 nanoparticles at different calcination temperatures

NASA Astrophysics Data System (ADS)

Loganathan, A.; Kumar, K.

2016-06-01

In the present work, pure and Sr2+ ions substituted Mg ferrite nanoparticles (NPs) had been prepared by co-precipitation method and their structural, optical, and magnetic properties at different calcination temperatures were studied. On this purpose, thermo gravimetric and differential thermal analysis (TG-DTA), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy, UV-Visible diffused reflectance spectroscopy, impedance spectroscopy, and vibrating sample magnetometer were carried out. The exo- and endothermic processes of synthesized precursors were investigated by TG-DTA measurements. The structural properties of the obtained products were examined by XRD analysis and show that the synthesized NPs are in the cubic spinel structure. The existence of two bands around 578-583 and 430-436 cm-1 in FT-IR spectrum also confirmed the formation of spinel-structured ferrite NPs. The lattice constants and particle size are estimated using XRD data and found to be strongly dependent on calcination temperatures. The optical, electrical, and magnetic properties of ferrite compositions also investigated and found to be strongly dependant on calcination temperatures.

The effect of calcination on multi-walled carbon nanotubes produced by dc-arc discharge.

PubMed

Pillai, Sreejarani K; Augustyn, Willem G; Rossouw, Margaretha H; McCrindle, Robert I

2008-07-01

Multi-walled carbon nanotubes were synthesized by dc-arc discharge in helium atmosphere and the effect of calcination at different temperatures ranging from 300-600 degrees C was studied in detail. The degree of degradation to the structural integrity of the multi-walled carbon nanotubes during the thermal process was studied by Raman spectroscopy, Scanning electron microscopy and High resolution transmission electron microscopy. The thermal behaviour of the as prepared and calcined samples was investigated by thermogravimetric analysis. Calcination in air at 400 degrees C for 2 hours was found to be an efficient and simple method to eliminate carbonaceous impurities from the nanotube bundles with minimal damage to the tube walls and length. The impurities were oxidized at a faster rate when compared to the nanotubes and gave good yield of about 50%. The nanotubes were observed to be damaged at temperature higher than 450 degrees C. The results show that this method is less destructive when compared liquid phase oxidation with 5 M HNO3.

Calcination Conditions on the Properties of Porous TiO2 Film

NASA Astrophysics Data System (ADS)

Zhang, Wenjie; Pei, Xiaobei; Bai, Jiawei; He, Hongbo

2014-03-01

Porous TiO2 films were deposited on SiO2 precoated glass-slides by sol-gel method using PEG1000 as template. The strongest XRD diffraction peak at 2θ = 25.3° is attributed to [101] plane of anatase TiO2 in the film. The increases of calcination temperature and time lead to stronger diffraction peak intensity. High transmittance and blue shift of light absorption edge are the properties of the film prepared at high calcination temperature. The average pore size of the films increases with the increasing calcination temperature as the result of TiO2 crystalline particles growing up and aggregation, accompanied with higher specific surface area. Photocatalytic activity of porous TiO2 films increases with the increasing calcination temperature. The light absorption edge of the films slightly moves to longer wavelength region along with the increasing calcination time. The mesoporous film calcinated at 500 °C for 2 h has the highest transmittance, the maximum surface area, and the maximum total pore volume. Consequently, the optimum degradation activity is achieved on the porous TiO2 film calcinated at 500 °C for 2 h.

[Spectrum studies on titania photocatalysts].

PubMed

Su, W; Fu, X; Wei, K; Zhang, H; Lin, H; Wang, X; Li, D

2001-02-01

The nano-sized TiO2 photocatalysts were prepared by sol-gel method and characterized by FTIR spectroscopy, FT-Raman spectroscopy and diffuse reflectance spectroscopy(DRS). Photocatalytic degradation of oleic acid over the TiO2 catalysts was investigated. The result showed that calcination temperature has strong effect on crystal structure, energy band structure, optical adsorption and photocatalytic activity of the TiO2 catalysts. It was found that the TiO2 photocatalyst calcined at 400 degrees C has the best apparent optical adsorption, the biggest band edge position and the highest photoactivity. The effect of calcination temperature on photocatalytic activity of TiO2 catalysts has been ascribed to the changes in structure and optical property of catalyst such as crystal size, content of rutile, residual NO3-, and band-edge position of light adsorption.

The effect of cyclic heat treatment on the physicochemical properties of bio hydroxyapatite from bovine bone.

PubMed

Londoño-Restrepo, S M; Jeronimo-Cruz, R; Rubio-Rosas, E; Rodriguez-García, M E

2018-05-02

This paper focus on physicochemical changes in bio-hydroxyapatite (BIO-HAp) from bovine femur obtained by calcination at high temperatures: 520-620 (each 20 °C) at 7.4 °C/min and from 700 to 1100 °C (each 100 °C) at three heating rates: 7.4, 9.9, and 11.1 °C/min. BIO-HAp samples were obtained using a multi-step process: cleaning, milling, hydrothermal process, calcination in an air atmosphere, and cooling in furnace air. Inductively Couple Plasma (ICP) showed that the presence of Mg, K, S, Ba, Zn, and Na, is not affected by the annealing temperature and heating rate. While Scanning Electron Microscopy (SEM) images showed the continuous growth of the HAp crystals during the calcination process due to the coalescence phenomenon, and the Full Width at the Half Maximum for the X-ray patterns for temperatures up to 700 is affected by the annealing temperature and the heating rate. Through X-ray diffraction, thermal, and calorimetric analysis (TGA-DSC), a partial dehydroxylation of hydroxyapatite was found in samples calcined up to 900 °C for the three heating rates. Also, Ca/P molar ratio decreased for samples calcined up to 900 °C as a result of the dehydroxylation process. NaCaPO 4 , CaCO 3 , Ca 3 (PO 4 ) 2 , MgO, and Ca(H 2 PO 4 ) 2 are some phases identified by X-ray diffraction; some of them are part of the bone and others were formed during the calcination process as a function of annealing temperature and heating rate, as it is the case for MgO.

Co-production of hydrogen and carbon nanotubes on nickel foam via methane catalytic decomposition

NASA Astrophysics Data System (ADS)

Ping, Dan; Wang, Chaoxian; Dong, Xinfa; Dong, Yingchao

2016-04-01

The co-production of COx-free hydrogen and carbon nanotubes (CNTs) was achieved on 3-dimensional (3D) macroporous nickel foam (NF) via methane catalytic decomposition (MCD) over nano-Ni catalysts using chemical vapor deposition (CVD) technique. By a simple coating of a NiO-Al2O3 binary mixture sol followed by a drying-calcination-reduction treatment, NF supported composite catalysts (denoted as NiyAlOx/NF) with Al2O3 transition-layer incorporated with well-dispersed nano-Ni catalysts were successfully prepared. The effects of Ni loading, calcination temperature and reaction temperature on the performance for simultaneous production of COx-free hydrogen and CNTs were investigated in detail. Catalysts before and after MCD were characterized by XRD, TPR, SEM, TEM, TG and Raman spectroscopy technology. Results show that increasing Ni loading, lowering calcination temperature and optimizing MCD reaction temperature resulted in high production efficiency of COx-free H2 and carbon, but broader diameter distribution of CNTs. Through detailed parameter optimization, the catalyst with a Ni/Al molar ratio of 0.1, calcination temperature of 550 °C and MCD temperature of 650 °C was favorable to simultaneously produce COx-free hydrogen with a growth rate as high as 10.3% and CNTs with uniform size on NF.

Effects of Coke Calcination Level on Pore Structure in Carbon Anodes

NASA Astrophysics Data System (ADS)

Fang, Ning; Xue, Jilai; Lang, Guanghui; Bao, Chongai; Gao, Shoulei

2016-02-01

Effects of coke calcination levels on pore structure of carbon anodes have been investigated. Bench anodes were prepared by 3 types of cokes with 4 calcination temperatures (800°C, 900°C, 1000°C and 1100°C). The cokes and anodes were characterized using hydrostatic method, air permeability determination, mercury porosimetry, image analysis and confocal microscopy (CSLM). The cokes with different calcination levels are almost the same in LC values (19-20 Å) and real density (1.967-1.985 g/cm3), while the anode containing coke calcined at 900°C has the lowest open porosity and air permeability. Pore size distribution (represented by Anode H sample) can be roughly divided into two ranges: small and medium pores in diameter of 10-400 μm and large pores of 400-580 μm. For the anode containing coke calcined at 800°C, a number of long, narrow pores in the pore size range of 400-580 μm are presented among cokes particles. Formation of these elongated pores may be attributed to coke shrinkages during the anode baking process, which may develop cracking in the anode under cell operations. More small or medium rounded pores with pore size range of 10-400 μm emerge in the anodes with coke calcination temperatures of 900°C, 1000°C and 1100°C, which may be generated due to release of volatiles from the carbon anode during baking. For the anode containing coke calcined at 1100°C, it is found that many rounded pores often closely surround large coke particles, which have potential to form elongated, narrow pores.

Recovery of SO2 and MgO from By-Products of MgO Wet Flue Gas Desulfurization

PubMed Central

Yan, Liyun; Lu, Xiaofeng; Wang, Quanhai; Guo, Qiang

2014-01-01

Abstract An industrial demonstration unit using natural gas as a heat source was built to calcine the by-products of MgO wet flue gas desulfurization from power plants; influencing factors on the SO2 content in calciner gas were comprehensively analyzed; and an advantageous recycling condition of MgO and SO2 from by-products was summarized. Results showed that the SO2 content in the calciner gas was increased by more than 10 times under a lower excess air coefficient, a higher feed rate, a lower crystal water in by-products, and a higher feed port position. For the tests conducted under the excess air coefficient above and below one, the effect of the furnace temperature on the SO2 content in the calciner gas was reversed. Results of activity analysis indicate that particles of MgO generated under the calcination temperature of 900–1,000°C had a high activity. In contrast, due to the slight sintering, MgO generated under the calcination temperature of 1,100°C had a low activity. To recycle SO2 as well as MgO, a temperature range of 900–927°C for TE103 is proposed. These studies will prompt the desulfurization market diversification, reduce the sulfur's dependence on imports for making sulfuric acid, be meaningful to balance the usage of the natural resource in China, and be regarded as a reference for the development of this technology for other similar developing countries. PMID:25371652

Effect of calcination temperature on the lithiation capacities of carbon-coated titania nanotubes synthesized by anodization

NASA Astrophysics Data System (ADS)

Seo, Min-Su; Lee, Hyukjae

2012-06-01

Carbon-coated titania nanotubes are synthesized via anodization in perchlorate containing electrolyte and subsequent hydrothermal reaction with glucose. Carbon coating improves the lithiation capacity of the titania nanotubes only when calcined at temperatures above 600°C, and the maximum capacity is ˜162 mAhg-1 at the 50th cycle from the titania nanotubes calcined at 700°C. The improved capacity of carbon-coated titania nanotubes is caused by the enhanced conductivity from the carbon. This is different from the role of the carbon coating in the hydrothermally prepared carbon-coated titania nanotubes, in which the coated carbon limits severe agglomeration.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhou, Yi, E-mail: zhouyihn@163.com; Huang, Yan; Li, Dang

Graphical abstract: SEM images of the samples synthesized at different hydrothermal temperatures for 8 h: (a) 75; (b) 100; (c) 120; and (d) 140°C, followed by calcination at 450 °C for 2 h. Highlights: ► Effects of calcination temperature on the phase transformation were studied. ► Effects of hydrothermal temperature and time on the morphology growth were studied. ► A two-stage reaction mechanism for the formation was presented. ► The photocatalytic activity was evaluated under sunlight irradiation. ► Effects of calcination temperature on the photocatalytic activity were studied. - Abstract: Novel three-dimensional sea-urchin-like hierarchical TiO{sub 2} superstructures were synthesized onmore » a Ti plate in a mixture of H{sub 2}O{sub 2} and NaOH aqueous solution by a facile one-pot hydrothermal method at a low temperature, followed by protonation and calcination. The results of series of electron microscopy characterizations suggested that the hierarchical TiO{sub 2} superstructures consisted of numerous one-dimensional nanostructures. The microspheres were approximately 2–4 μm in diameter, and the one-dimensional TiO{sub 2} nanostructures were up to 600–700 nm long. A two-stage reaction mechanism, i.e., initial growth and then assembly, was proposed for the formation of these architectures. The three-dimensional sea-urchin-like hierarchical TiO{sub 2} microstructures showed excellent photocatalytic activity for the degradation of Rhodamine B aqueous solution under sunlight irradiation, which was attributed to the special three-dimensional hierarchical superstructure, and increased number of surface active sites. This novel superstructure has promising use in practical aqueous purification.« less

To study the effect of dopant NiO concentration and duration of calcinations on structural and optical properties of MgO-NiO nanocomposites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Rajesh, E-mail: rkkaushik06@gmail.com; Deptt. of Physics,Vaish College of Engineering, Rohtak-124001, Haryana; Praveen,

2016-05-06

In present work Magnesium oxide (MgO) samples were doped with different concentration of Transition metal Nickel Oxide(NiO) by using Chemical co-precipitation method. The doping levels were varied from NiO (5%, 10%, 15%) and all the samples were calcined at 600°C for 4hrs and 8hrs respectively. Structural analysis of these calcined materials is carried out by X-ray diffraction (XRD) techniques which reveals that average crystalline sizes are in nano region i.e. 21.77nm-31.13 nm and tabulated in table 1. The powder of calcined samples were also characterized by using various other techniques i.e. Scanning Electron Microscopy (SEM), Fourier Transformation Infrared Spectroscopy (FTIR), UV-Visiblemore » spectroscopy, Transmission Electron Microscopy (TEM) etc. The effects of dopant concentration, calcined temperature, calcinations duration on samples were studied and also investigate the effect of varying dopant concentration on morphology and optical properties of calcined nanomaterials. From results it was observed that the crystallite size of nanocomposites increases with increases dopant concentration or increases calcinations duration. The optical band gap decreases with increases sintering time and increase with increases dopant concentrations. TEM results coincide with XRD results and show that particles are polycrystalline in nature. FTIR spectra show that for all samples particles are pure in composition and transmission rate increases with calcinations duration.« less

Comparative study of phase transition and textural changes upon calcination of two commercial titania samples: A pure anatase and a mixed anatase-rutile

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kordouli, Eleana; Dracopoulos, Vassileios; Vaimakis, Tiverios

2015-12-15

The effect of calcination temperature and time on structural and textural changes of two commercial TiO{sub 2} samples (pure anatase and a mixture of anatase and rutile) has been investigated using N{sub 2} physisorption, ex-situ and in-situ X-ray powder diffraction, differential scanning calorimetry and UV–vis diffuse reflectance spectroscopy. The increase of the calcination temperature (up to 700 °C) and time (up to 8 h) causes only textural changes in the pure anatase, whereas a transformation of the anatase to rutile takes place, in addition, in the mixed titania (containing anatase and rutile). The textural changes observed in pure anatase samplemore » were attributed to solid state diffusion leading to an increase in the size of anatase nanocrystals, through sintering. Thus, the mean pore diameter shifts to higher values and the pore volume and specific surface area decrease. The successful application of the Johnson–Mehl–Avrami–Kolmogorov model in the kinetic data concerning the pure anatase indicates a mass transfer control of sintering process. Similar textural changes were also observed upon calcination of the sample containing anatase and rutile. In this case not only sintering but the anatase to rutile transformation contributes also to the textural changes. Kinetic analysis showed that the rutile nanocrystals in the mixed titania served as seed for by-passing the high energy barrier nucleation step allowing/facilitating thus the anatase to rutile transformation. A fine control of the anatase to rutile ratio and thus of energy-gap and the population of hetero-junctions may be obtained by adjusting the calcination temperature and time. - Graphical Abstract: Dependence of anatase content of P25 on the calcination temperature (600 °C (■), 650 °C (●), 700 °C (▲)) and time. - Highlights: • Increase of calcination temperature up to 800 °C and time up to 8 h causes only textural changes in pure anatase • Progressive transformation of anatase to rutile with time takes place in the mixed titania above 600 °C • A high activation energy barrier inhibits the solid state transformation in pure anatase • Rutile nanocrystals in mixed titania serve as seeding for favouring transformation • Calcination temperature and time allow a fine control of E{sub g} and heterojunctions population in mixed titania.« less

Effect of calcination temperature of a copper ferrite synthesized by a sol-gel method on its structural characteristics and performance as Fenton catalyst to remove gallic acid from water.

PubMed

López-Ramón, María V; Álvarez, Miguel A; Moreno-Castilla, Carlos; Fontecha-Cámara, María A; Yebra-Rodríguez, África; Bailón-García, Esther

2018-02-01

A copper ferrite synthesized by a sol-gel combustion method was calcined at different temperatures up to 800°C, determining changes in its structural characteristics and magnetic measurements and studying its catalytic performance in gallic acid removal by Fenton reaction. The main objective was to study the effect of the calcination temperature of copper ferrite on its crystalline phase formation and transformation, activity and metal ion leaching. The cubic-to-tetragonal transformation of the spinel occurred via its reaction with the CuO phase, displacing Fe 3+ ions in B (octahedral) sites out of the spinel structure by the following reaction: 2Fe 3+ B +3CuO→Fe 2 O 3 +3Cu 2+ B . The catalysts showed superparamagnetic or substantial superparamagnetic behaviour. At higher calcination temperatures, catalyst activity was lower, and Cu ion leaching was markedly decreased. There was no Fe ion leaching with any catalyst. The as-prepared catalyst showed better catalytic performance than a commercial copper ferrite. Leached Cu ions acted as homogeneous catalysts, and their contribution to the overall removal mechanism was examined. Cu 2 O present in the as-prepared catalysts made only a small contribution to their activity. Finally, the reutilization of various catalysts was studied by performing different catalytic cycles. Copyright © 2017 Elsevier Inc. All rights reserved.

Effect of phase transformation on optical and dielectric properties of zirconium oxide nanoparticles

NASA Astrophysics Data System (ADS)

Chintaparty, Rajababu; Palagiri, Bhavani; Reddy Nagireddy, Ramamanohar; subbha Reddy Imma Reddy, Venkata

2015-09-01

Zirconium oxide nanoparticle (ZrO2) is synthesized by the hydrothermal method at different calcination temperatures. The structural analysis is carried out by X-ray diffraction and Raman spectra. The sample prepared at 400 °C and 1100 °C showed the cubic and monoclinic phase, respectively, and the sample calcined at 600 °C and 800 °C showed the mixed phase with co-existence of cubic and monoclinic phases. Furthermore, the morphology and particle size of these samples were investigated by scanning electron microscope (SEM) and transmission electron microscope (TEM) analysis. The band gap estimated from UV-Vis spectra of ZrO2 (zirconia) nanocrystalline materials calcined at different temperatures from 400 °C to 1100 °C was in the range of 2.6-4.2 eV. The frequency dependence of dielectric constant and dielectric loss was investigated at room temperature. The low frequency region of dielectric constant is attributed to space charge effects.

Choice of precipitant and calcination temperature of precursor for synthesis of NiCo2O4 for control of CO-CH4 emissions from CNG vehicles.

PubMed

Trivedi, Suverna; Prasad, Ram

2018-03-01

Compressed natural gas (CNG) is most appropriate an alternative of conventional fuel for automobiles. However, emissions of carbon-monoxide and methane from such vehicles adversely affect human health and environment. Consequently, to abate emissions from CNG vehicles, development of highly efficient and inexpensive catalysts is necessary. Thus, the present work attempts to scan the effects of precipitants (Na 2 CO 3 , KOH and urea) for nickel cobaltite (NiCo 2 O 4 ) catalysts prepared by co-precipitation from nitrate solutions and calcined in a lean CO-air mixture at 400°C. The catalysts were used for oxidation of a mixture of CO and CH 4 (1:1). The catalysts were characterized by X-ray diffractometer, Brunauer-Emmett-Teller surface-area, X-ray photoelectron spectroscopy; temperature programmed reduction and Scanning electron microscopy coupled with Energy-Dispersive X-Ray Spectroscopy. The Na 2 CO 3 was adjudged as the best precipitant for production of catalyst, which completely oxidized CO-CH 4 mixture at the lowest temperature (T 100 =350°C). Whereas, for catalyst prepared using urea, T 100 =362°C. On the other hand the conversion of CO-CH 4 mixture over the catalyst synthesized by KOH limited to 97% even beyond 400°C. Further, the effect of higher calcination temperatures of 500 and 600°C was examined for the best catalyst. The total oxidation of the mixture was attained at higher temperatures of 375 and 410°C over catalysts calcined at 500 and 600°C respectively. Thus, the best precipitant established was Na 2 CO 3 and the optimum calcination temperature of 400°C was found to synthesize the NiCo 2 O 4 catalyst for the best performance in CO-CH 4 oxidation. Copyright © 2017. Published by Elsevier B.V.

Effect of catalyst calcination temperature in the visible light photocatalytic oxidation of gaseous formaldehyde by multi-element doped titanium dioxide.

PubMed

de Luna, Mark Daniel G; Laciste, Maricris T; Tolosa, Nolan C; Lu, Ming-Chun

2018-03-20

The present study investigates the influence of calcination temperature on the properties and photoactivity of multi-element doped TiO 2 . The photocatalysts were prepared by incorporating silver (Ag), fluorine (F), nitrogen (N), and tungsten (W) into the TiO 2 structure via the sol-gel method. Spectroscopic techniques were used to elucidate the correlation between the structural and optical properties of the doped photocatalyst and its photoactivity. XRD results showed that the mean crystallite size increased for undoped photocatalysts and decreased for the doped photocatalysts when calcination was done at higher temperatures. UV-Vis spectra showed that the absorption cut-off wavelength shifted towards the visible light region for the as-synthesized photocatalysts and band gap narrowing was attributed to multi-element doping and calcination. FTIR spectra results showed the shifting of OH-bending absorption bands towards increasing wave numbers. The activity of the photocatalysts was evaluated in terms of gaseous formaldehyde removal under visible light irradiation. The highest photocatalytic removal of gaseous formaldehyde was found at 88%. The study confirms the effectiveness of multi-element doped TiO 2 to remove gaseous formaldehyde in air by visible light photocatalysis and the results have a lot of potential to extend the application to other organic air contaminants.

Effect of TiO2 calcination temperature on the photocatalytic oxidation of gaseous NH3.

PubMed

Wu, Hongmin; Ma, Jinzhu; Zhang, Changbin; He, Hong

2014-03-01

Carbon-modified titanium dioxide (TiO2) was prepared by a sol-gel method using tetrabutyl titanate as precursor, with calcination at various temperatures, and tested for the photocatalytic oxidation (PCO) of gaseous NH3 under visible and UV light. The test results showed that no samples had visible light activity, while the TiO2 calcined at 400°C had the best UV light activity among the series of catalysts, and was even much better than the commercial catalyst P25. The catalysts were then characterized by X-ray diffractometry, Brunauer-Emmett-Teller adsorption analysis, Raman spectroscopy, thermogravimetry/differential scanning calorimetry coupled with mass spectrometry, ultraviolet-visible diffuse reflectance spectra, photoluminescence spectroscopy and in situ diffuse reflectance infrared Fourier transform spectroscopy. It was shown that the carbon species residuals on the catalyst surfaces induced the visible light adsorption of the samples calcined in the low temperature range (< 300°C). However, the surface acid sites played a determining role in the PCO of NH3 under visible and UV light over the series of catalysts. Although the samples calcined at low temperatures had very high SSA, good crystallinity, strong visible light absorption and also low PL emission intensity, they showed very low PCO activity due to their very low number of acid sites for NH3 adsorption and activation. The TiO2 sample calcined at 400°C contained the highest number of acid sites among the series of catalysts, therefore showing the highest performance for the PCO of NH3 under UV light. Copyright © 2014 The Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences. Published by Elsevier B.V. All rights reserved.

Effect of calcination temperature on formaldehyde oxidation performance of Pt/TiO2 nanofiber composite at room temperature

NASA Astrophysics Data System (ADS)

Xu, Feiyan; Le, Yao; Cheng, Bei; Jiang, Chuanjia

2017-12-01

Catalytic oxidation at room temperature over well-designed catalysts is an environmentally friendly method for the abatement of indoor formaldehyde (HCHO) pollution. Herein, nanocomposites of platinum (Pt) and titanium dioxide (TiO2) nanofibers with various phase compositions were prepared by calcining the electrospun TiO2 precursors at different temperatures and subsequently depositing Pt nanoparticles (NPs) on the TiO2 through a NaBH4-reduction process. The phase compositions and structures of Pt/TiO2 can be easily controlled by varying the calcination temperature. The Pt/TiO2 nanocomposites showed a phase-dependent activity towards the catalytic HCHO oxidation. Pt/TiO2 containing pure rutile phase showed enhanced activity with a turnover frequency (TOF) of 16.6 min-1 (for a calcination temperature of 800 °C) as compared to those containing the anatase phase or mixed phases. Density functional theory calculation shows that TiO2 nanofibers with pure rutile phase have stronger adsorption ability to Pt atoms than anatase phase, which favors the reduction of Pt over rutile phase TiO2, leading to higher contents of metallic Pt in the nanocomposite. In addition, the Pt/TiO2 with rutile phase possesses more abundant oxygen vacancies, which is conducive to the activation of adsorbed oxygen. Consequently, the Pt/rutile-TiO2 nanocomposite exhibited better catalytic activity towards HCHO oxidation at room temperature.

Effect of metal ratio and calcination temperature of chromium based mixed oxides catalyst on FAME density from palm fatty acid distillate

NASA Astrophysics Data System (ADS)

Wan, Z.; Fatimah, S.; Shahar, S.; Noor, A. C.

2017-09-01

Mixed oxides chromium based catalysts were synthesized via sol-gel method for the esterification of palm fatty acid distillate (PFAD) to produce fatty acid methyl ester (FAME). The reactions were conducted in a batch reactor at reaction temperature of 160 °C for 4 h and methanol to PFAD molar ratio of 3:1. The effects of catalyst preparation conditions which are the mixed metal ratio and calcination temperature were studied. The various metal ratio of Cr:Mn (1:0, 0:1, 1:1, 1:2 and 2:1) and Cr:Ti (0:1, 1:1, 1:2 and 2:1) resulted in FAME density ranges from 1.041 g/cm3 to 0.853 g/cm3 and 1.107 g/cm3 to 0.836 g/cm3, respectively. The best condition catalyst was found to be Cr:Ti metal ratio of 1:2 and Cr:Mn metal ratio of 1:1. The calcination temperature of the mixed oxides between 300 °C to 700°C shows effect on the FAME density obtained in the reaction. The calcination at 500°C gave the lowest FAME density of 0.836 g/cm3 and 0.853 g/cm3 for Cr:Ti and Cr:Mn mixed oxides, respectively. The density of FAME is within the value range of the biodiesel fuel property. Thus, mixed oxides of Cr-Ti and Cr-Mn have good potentials as heterogeneous catalyst for FAME synthesis from high acid value oils such as PFAD.

Effects of calcination temperature for rate capability of triple-shelled ZnFe2O4 hollow microspheres for lithium ion battery anodes

NASA Astrophysics Data System (ADS)

Hwang, Hojin; Shin, Haeun; Lee, Wan-Jin

2017-04-01

Triple-shelled ZnFe2O4 hollow microspheres (ZFO) as anode materials for lithium ion battery are prepared through a one-pot hydrothermal reaction using the composite solution consisting of sucrose in water and metal ions in ethylene glycol (EG), followed by different calcination processes. The architectures of ZFO micro spheres are differently synthesized through a mutual cooperation of inward and outward ripening with three different calcination temperatures. Thin triple-shelled ZnFe2O4 hollow microspheres calcined at 450 °C (ZFO-450) delivers a high reversible capacity of 932 mA h g-1 at a current density of 2 A g-1 even at the 200th cycle without obvious decay. Furthermore, ZFO-450 delivers 1235, 1005, 865, 834, and 845 mA h g-1 at high current densities of 0.5, 2, 5, 10, and 20 A g-1 after 100 cycles. Thin triple-shelled hollow microsphere prepared at an optimum calcination temperature provides exceptional rate capability and outstanding rate retention due to (i) the formation of nanoparticles leading to thin shell with morphological integrity, (ii) the facile mass transfer by thin shell with mesoporous structure, and (iii) the void space with macroporous structure alleviating volume change occurring during cycling.

Effects of calcination temperature for rate capability of triple-shelled ZnFe2O4 hollow microspheres for lithium ion battery anodes

PubMed Central

Hwang, Hojin; Shin, Haeun; Lee, Wan-Jin

2017-01-01

Triple-shelled ZnFe2O4 hollow microspheres (ZFO) as anode materials for lithium ion battery are prepared through a one-pot hydrothermal reaction using the composite solution consisting of sucrose in water and metal ions in ethylene glycol (EG), followed by different calcination processes. The architectures of ZFO micro spheres are differently synthesized through a mutual cooperation of inward and outward ripening with three different calcination temperatures. Thin triple-shelled ZnFe2O4 hollow microspheres calcined at 450 °C (ZFO-450) delivers a high reversible capacity of 932 mA h g−1 at a current density of 2 A g−1 even at the 200th cycle without obvious decay. Furthermore, ZFO-450 delivers 1235, 1005, 865, 834, and 845 mA h g−1 at high current densities of 0.5, 2, 5, 10, and 20 A g−1 after 100 cycles. Thin triple-shelled hollow microsphere prepared at an optimum calcination temperature provides exceptional rate capability and outstanding rate retention due to (i) the formation of nanoparticles leading to thin shell with morphological integrity, (ii) the facile mass transfer by thin shell with mesoporous structure, and (iii) the void space with macroporous structure alleviating volume change occurring during cycling. PMID:28418001

Porous α-Fe2O3 nanostructures and their lithium storage properties as full cell configuration against LiFePO4

NASA Astrophysics Data System (ADS)

Veluri, P. S.; Shaligram, A.; Mitra, S.

2015-10-01

A two step approach for synthesis of porous α-Fe2O3 nanostructures has been realized via polyol method by complexing iron oxalate with ethylene glycol. Crystalline Fe2O3 samples with different porosities are obtained by calcination of Fe-Ethylene glycol complex at various temperatures. The as-prepared porous Fe2O3 structures exhibit promising lithium storage performance at high current rates. It is observed that the calcination temperature and the resultant porosity have a significant effect on capacity and cycling stability. Samples calcined at high temperature (600 °C) demonstrates stable cycle life with capacity retention of 1077 mAh g-1 at 500 mA g-1 current rate after 50 charge-discharge cycles. Samples calcined at temperatures of 500 and 600 °C display stable cycle life and high rate capability with reversible capacity of 930 mAh g-1 and 688 mAh g-1 at 5 A g-1, respectively. Impregnation of electrodes with electrolyte before cell fabrication shows enhanced electrochemical performance. The viability of Fe2O3 porous nanostructures as prospective anode material examined against commercial LiFePO4 cathode shows promising electrochemical performance.

Understanding the effect of surface/bulk defects on the photocatalytic activity of TiO2: anatase versus rutile.

PubMed

Yan, Junqing; Wu, Guangjun; Guan, Naijia; Li, Landong; Li, Zhuoxin; Cao, Xingzhong

2013-07-14

The sole effect of surface/bulk defects of TiO2 samples on their photocatalytic activity was investigated. Nano-sized anatase and rutile TiO2 were prepared by hydrothermal method and their surface/bulk defects were adjusted simply by calcination at different temperatures, i.e. 400-700 °C. High temperature calcinations induced the growth of crystalline sizes and a decrease in the surface areas, while the crystalline phase and the exposed facets were kept unchanged during calcination, as indicated by the characterization results from XRD, Raman, nitrogen adsorption-desorption, TEM and UV-Vis spectra. The existence of surface/bulk defects in calcined TiO2 samples was confirmed by photoluminescence and XPS spectra, and the surface/bulk defect ratio was quantitatively analyzed according to positron annihilation results. The photocatalytic activity of calcined TiO2 samples was evaluated in the photocatalytic reforming of methanol and the photocatalytic oxidation of α-phenethyl alcohol. Based on the characterization and catalytic results, a direct correlation between the surface specific photocatalytic activity and the surface/bulk defect density ratio could be drawn for both anatase TiO2 and rutile TiO2. The surface defects of TiO2, i.e. oxygen vacancy clusters, could promote the separation of electron-hole pairs under irradiation, and therefore, enhance the activity during photocatalytic reaction.

Study on Al2O3 extraction from activated coal gangue under different calcination atmospheres

NASA Astrophysics Data System (ADS)

Dong, Ling; Liang, Xinxing; Song, Qiang; Gao, Gewu; Song, Lihua; Shu, Yuanfeng; Shu, Xinqian

2017-12-01

Coal gangue was calcinated under air, nitrogen, carbon dioxide, air-hydrogen, and hydrogen atmospheres. The effects of different calcination temperatures and atmospheres on the mineral composition of activated coal gangue were investigated by X-ray diffraction. Moreover, the acid leaching kinetics of aluminum oxide from coal gangue was investigated with sulfuric acid. It showed that the air atmosphere promoted kaolinite decomposition during coal gangue calcination. The hydrogen atmosphere promoted the activation and decomposition of kaolinite at reaction temperatures exceeding 650°C. The carbon dioxide atmosphere eliminated the influence of residual carbon on coal gangue. When the ratio of acid/coal gangue was 1.5 and reaction temperature was 650°C, the sulfuric acid leaching rate under air, air-hydrogen, carbon dioxide, hydrogen and nitrogen atmospheres were 93.66%, 90.90%, 84.06%, 81.91% and 77.54% respectively. The acid leaching reaction process conformed to unreacted shrinking core model of particle unchanged, and was controlled by the interfacial chemical reaction. The reaction kinetic equation for the leaching process was 1-(1-x)1/3=kt with an apparent activation energy of 48.97 kJ/mol.

CuBi2O4 Prepared by the Polymerized Complex Method for Gas-Sensing Applications.

PubMed

Choi, Yun-Hyuk; Kim, Dai-Hong; Hong, Seong-Hyeon

2018-05-02

Multicomponent oxides can be extensively explored as alternative gas-sensing materials to binary oxides with their structural and compositional versatilities. In this work, the gas-sensing properties of CuBi 2 O 4 have been investigated toward various reducing gases (C 2 H 5 OH, NH 3 , H 2 , CO, and H 2 S) and oxidizing gas (NO 2 ) for the first time. For this, the powder synthesis has been developed using the polymerized complex method (Pechini method) to obtain a single-phase polycrystalline CuBi 2 O 4 . The defect, optical, and electronic properties in the prepared CuBi 2 O 4 powder were modulated by varying the calcination temperature from 500 to 700 °C. Noticeably, a high concentration of Cu + -oxygen vacancy ([Formula: see text]) defect complexes and isolated Cu 2+ ion clusters was found in the 500 °C-calcined CuBi 2 O 4 , where they were removed through air calcination at higher temperatures (up to 700 °C) while making the compound more stoichiometric. The change in the intrinsic defect concentration with the calcination temperature led to the variation of the electronic band gap energy and hole concentration in CuBi 2 O 4 with the polaronic hopping conduction (activation energy = 0.43 eV). The CuBi 2 O 4 sensor with 500 °C-calcined powder showed the highest gas responses (specifically, 10.4 toward 1000 ppm C 2 H 5 OH at the operating temperature of 400 °C) with the highest defect concentration. As a result, the gas-sensing characteristics of CuBi 2 O 4 are found to be dominantly affected by the intrinsic defect concentration, which is controlled by the calcination temperature. Toward reducing H 2 S and oxidizing NO 2 gases, the multiple reactions arising simultaneously on the surface of the CuBi 2 O 4 sensor govern its response behavior, depending on the gas concentration and the operating temperature. We believe that this work can be a cornerstone for understanding the effect of chemical defect on the gas-sensing characteristics in multicomponent oxides.

Wet calcining of trona (sodium sesquicarbonate) and bicarbonate in a mixed solvent

NASA Astrophysics Data System (ADS)

Gärtner, R. S.; Witkamp, G. J.

2002-04-01

Trona ore is used in large amounts for the production of soda ash. A key step in this process is the conversion of trona (sodium sesquicarbonate: Na 2CO 3·NaHCO 3·2H 2O) into soda (sodium carbonate anhydrate: Na 2CO 3). Currently, this conversion is done industrially by calcining of the raw ore in rotary calciners at ca. 120°C or higher (Natural Soda Ash—Occurrences, Processing, and Use, Van Nostrand Reinhold, New York, 1991, p. 267). Trona can however be converted at lower temperatures by using a "wet calcining" technique. In this technique, trona is contacted with an organic or mixed organic-aqueous solvent at a conversion temperature that depends on the water activity of the used solvent. In pure ethylene glycol this temperature can be as low as 55°C. The conversion by "wet calcining" occurs very similar to that in the regular dry calcining process via a solid phase conversion. The anhydrate crystals form directly from the solid trona. This produces pseudomorphs (J. Chem. Eng. Data 8(3) (1963) 301), i.e. agglomerates of fine anhydrate crystals (1-10 μm). At high temperatures, dense, finely pored agglomerates are formed, while the outer shape of the agglomerate retains the prism shape of the trona crystal. At low conversion temperatures, loosely packed or even unstable agglomerates are found.

Hydrogen Production by Steam Reforming of Ethanol over Nickel Catalysts Supported on Sol Gel Made Alumina: Influence of Calcination Temperature on Supports

PubMed Central

Yaakob, Zahira; Bshish, Ahmed; Ebshish, Ali; Tasirin, Siti Masrinda; Alhasan, Fatah H.

2013-01-01

Selecting a proper support in the catalyst system plays an important role in hydrogen production via ethanol steam reforming. In this study, sol gel made alumina supports prepared for nickel (Ni) catalysts were calcined at different temperatures. A series of (Ni/AlS.G.) catalysts were synthesized by an impregnation procedure. The influence of varying the calcination temperature of the sol gel made supports on catalyst activity was tested in ethanol reforming reaction. The characteristics of the sol gel alumina supports and Ni catalysts were affected by the calcination temperature of the supports. The structure of the sol gel made alumina supports was transformed in the order of γ → (γ + θ) → θ-alumina as the calcination temperature of the supports increased from 600 °C to 1000 °C. Both hydrogen yield and ethanol conversion presented a volcano-shaped behavior with maximum values of 4.3 mol/mol ethanol fed and 99.5%, respectively. The optimum values were exhibited over Ni/AlS.G800 (Ni catalyst supported on sol gel made alumina calcined at 800 °C). The high performance of the Ni/AlS.G800 catalyst may be attributed to the strong interaction of Ni species and sol gel made alumina which lead to high nickel dispersion and small particle size. PMID:28809270

Hydrogen Production by Steam Reforming of Ethanol over Nickel Catalysts Supported on Sol Gel Made Alumina: Influence of Calcination Temperature on Supports.

PubMed

Yaakob, Zahira; Bshish, Ahmed; Ebshish, Ali; Tasirin, Siti Masrinda; Alhasan, Fatah H

2013-05-30

Selecting a proper support in the catalyst system plays an important role in hydrogen production via ethanol steam reforming. In this study, sol gel made alumina supports prepared for nickel (Ni) catalysts were calcined at different temperatures. A series of (Ni/Al S.G. ) catalysts were synthesized by an impregnation procedure. The influence of varying the calcination temperature of the sol gel made supports on catalyst activity was tested in ethanol reforming reaction. The characteristics of the sol gel alumina supports and Ni catalysts were affected by the calcination temperature of the supports. The structure of the sol gel made alumina supports was transformed in the order of γ → (γ + θ) → θ-alumina as the calcination temperature of the supports increased from 600 °C to 1000 °C. Both hydrogen yield and ethanol conversion presented a volcano-shaped behavior with maximum values of 4.3 mol/mol ethanol fed and 99.5%, respectively. The optimum values were exhibited over Ni/Al S.G800 (Ni catalyst supported on sol gel made alumina calcined at 800 °C). The high performance of the Ni/Al S.G800 catalyst may be attributed to the strong interaction of Ni species and sol gel made alumina which lead to high nickel dispersion and small particle size.

Thermostable photocatalytically active TiO2 anatase nanoparticles

NASA Astrophysics Data System (ADS)

Qi, Fei; Moiseev, Anna; Deubener, Joachim; Weber, Alfred

2011-03-01

Anatase is the low-temperature (300-550 °C) crystalline polymorph of TiO2 and it transforms to rutile upon heating. For applications utilizing the photocatalytic properties of nanoscale anatase at elevated temperatures (over 600 °C) the issue of phase stabilisation is of major interest. In this study, binary TiO2/SiO2 particles were synthesized by a flame aerosol process with TiCl4 and SiCl4 as precursors. The theoretical Si/Ti ratio was varied in the range of 0.7-1.3 mol/mol. The synthesized TiO2/SiO2 samples were heat treated at 900 and 1,000 °C for 3 h to determine the thermostability of anatase. Pyrogenic TiO2 P25 (from Evonik/Degussa, Germany) widely applied as photocatalyst was used as non-thermostabilized reference material for comparison of photocatalytic activity of powders. Both the non-calcinated and calcinated powders were characterized by means of XRD, TEM and BET. Photocatalytic activity was examined with dichloroacetic acid (DCA) chosen as a model compound. It was found that SiO2 stabilized the material retarding the collapse of catalyst surface area during calcination. The weighted anatase content of 85% remains completely unchanged even after calcination at 1,000 °C. The presence of SiO2 layer/bridge as spacer between TiO2 particles freezes the grain growth: the average crystallite size increased negligibly from 17 to 18 nm even during the calcination at 1,000 °C. Due to the stabilizing effect of SiO2 the titania nanoparticles calcinated at 900 and 1,000 °C show significant photocatalytic activity. Furthermore, the increase in photocatalytic activity with calcination temperature indicates that the titania surface becomes more accessible either due to intensified cracking of the SiO2 layer or due to enhanced transport of SiO2 into the necks thus releasing additional titania surface.

Crystallite Size-Lattice Strain Estimation and Optical Properties of Mn0.5Zn0.5Fe2O4 Nanoparticles

NASA Astrophysics Data System (ADS)

Indrayana, I. P. T.; Suharyadi, E.

2018-04-01

In the present work, we performed William-Hall plot using uniform deformation model (UDM) to estimate the crystallite size and lattice strain of Mn0.5Zn0.5Fe2O4 with various calcination temperature. The calculated crystallite sizes are 25.86 nm, 29.55 nm and 24.97 nm for nanoparticles which were calcined at a temperature of 600°C, 800°C and 1000°C, consecutively. The strain of nanoparticles has value in the order of 10-3. Controlling the calcination temperature will facilitate a change in crystallinity of nanoparticles and influence their crystallite size and strain of the crystal lattice. The optical band gap energy of samples nanoparticles is in a range of 1.09 eV – 3.30 eV. Increasing calcination temperature increased the direct and indirect band gap energy. The Urbach energy was found to increase with increased of gap energy. These results demonstrated that higher structural and optical properties of Mn0.5Zn0.5Fe2O4 can be obtained from a higher calcination temperature.

The influence of temperature on a nutty-cake structural material: LiMn1-xFexPO4 composite with LiFePO4 core and carbon outer layer for lithium-ion battery

NASA Astrophysics Data System (ADS)

Huo, Zhen-Qing; Cui, Yu-Ting; Wang, Dan; Dong, Yue; Chen, Li

2014-01-01

The extremely low electronic conductivity, slow ion diffusion kinetics, and the Jahn-Teller effect of LiMnPO4 limit its electrochemical performance. In this work, a nutty-cake structural C-LiMn1-xFexPO4-LiFePO4 cathode material is synthesized by hydrothermal method and further calcined at different temperatures. The influence of calcination temperature on the electrochemical behavior is investigated by X-ray diffractometer, scanning electron microscope, field-emission high-resolution transmission electron microscope, energy-dispersive X-ray spectroscopy, electrochemical impedance spectroscopy and charge-discharge tests. And the performance of C-LiMn1-xFexPO4-LiFePO4 materials has a relationship with its crystal structure. The well-crystallized Sample-600 calcined at 600 °C shows the smallest charge transfer resistance, the largest lithium ion diffusion coefficient (DLi) and the best cycling stability. The discharge capacity of Sample-600 holds around 112 mAh g-1 after the 3rd cycle at 0.1 C rate. The performances improvement of C-LiMn1-xFexPO4-LiFePO4 material can be mainly attributed to the iron diffusion from the LiFePO4 core to the outer LiMnPO4 layer under appropriate calcination temperature.

Surface structural evolution of AuAg/TiO2 catalyst in the transformation of benzyl alcohol to sodium benzoate

NASA Astrophysics Data System (ADS)

Cui, Yuanyuan; Wang, Ying; Fan, Kangnian; Dai, Wei-Lin

2013-08-01

A series of AuAg/TiO2 catalysts calcined at different temperatures were used for single-pot, solvent-free synthesis of sodium benzoate and benzoic acid through the green oxidation of benzyl alcohol. The best catalytic performance, which produced a sodium benzoate yield of up to 85%, was obtained over the AuAg/TiO2 catalyst calcined at 623 K. Systematic characterizations including BET, XRD, TEM, XPS, and UV-vis DRS and ICP were carried out to investigate the influence of calcined temperature on the structural evolution of the bimetallic AuAg/TiO2 catalysts. TEM images showed that both low (473 K) and high calcinations temperatures (973 K) resulted in larger particles. The smallest particles (8.2 nm) were obtained at 623 K. This decrease in particle size may have been induced by the re-dispersion and interaction of the bimetallic species. XRD and XPS results showed that proper calcination temperature (623 K) could promote interactions between the bimetallic particles and the TiO2 support as well as the dispersion of active bimetallic species. The higher catalytic performance of the 623 K calcined catalyst could be attributed to the smaller particle size and the synergetic interaction between nano-bimetallic gold and silver species.

Hydrothermal synthesis and influence of later heat treatment on the structural evolution, optical and electrical properties of nanostructured α-MoO3 single crystals

NASA Astrophysics Data System (ADS)

Badr, A. M.; El-Anssary, E. H.; Elshaikh, H. A.; Afify, H. H.

2017-12-01

In the current study, α-MoO3 nanocrystals were successfully synthesized from ammonium heptamolybdate tetrahydrate using a simple hydrothermal route. The influence of calcination temperature on the structural, optical and electrical properties was systematically investigated for the MoO3 powder products. The XRD results were analyzed for these powders, revealing the formation of a mixed phase (β- and α-MoO3) at calcination temperatures ranging from 350 °C-450 °C, and hence a residual monoclinic phase still exists in the samples at the calcination temperature of 450 °C. Subsequently, the mixed phase was completely converted to a pure single phase of α-MoO3 at a calcination temperature of 500 °C. The optical properties of the MoO3 powders were investigated using the transformed diffuse reflectance technique according to Kubelka-Munk theory. For such a powder product, the results of the optical measurements demonstrated the realization of indirect and direct allowed transitions at the spectral ranges 3.31-3.91 eV and 3.66-4.27 eV, respectively. The indirect- and direct-allowed band-gaps of the MoO3 products were found to increase from 2.69-3.12 eV and from 3.43-3.64 eV, respectively, by increasing the calcination temperature from 350 °C-600 °C. The MoO3 powders calcined at different temperatures were converted into five dense tablets for performing the electrical measurements. These measurements were carried out at different working temperatures using a system operating under high vacuum conditions. The results revealed that the dc-conductivity of such a tablet typically increases by more than five orders of magnitude with an increase in the working temperature from 77-300 K. These results also demonstrated a high dependence of dc-conductivity on the calcination temperature for the MoO3 products. The dc-conductivity as a function of the operating temperature revealed the presence of at least three different electrical conduction mechanisms for the same MoO3 tablet.

Development of a low-pressure materials pre-treatment process for improved energy efficiency

NASA Astrophysics Data System (ADS)

Lee, Kwanghee; You, Byung Don

2017-09-01

Low pressure materials pre-treatment process has been developed as an alternative to the existing high-temperature sludge drying, limestone calcination, and limonite dehydroxylation. Using the thermodynamic equilibrium relationship between temperature and pressure represented by the Clausius-Clapeyron equation, the operational temperature of these reactions could be lowered at reduced pressure for increased energy efficiency. For industrial sludge drying, the evaporation rate was controlled by interfacial kinetics showing a constant rate with time and significant acceleration in the reaction could be observed with reduced pressure. At this modified reaction rate under low pressure, the rate was also partially controlled by mass transfer. Temperature of limestone calcination was lowered, but the reaction was limited at the calculated equilibrium temperature of the Clausius-Clapeyron equation and slightly higher temperatures were required. The energy consumption during limestone calcination and limonite dehydroxylation were evaluated, where lower processing pressures could enhance the energy efficiency for limestone calcination, but limonite dehydroxylation could not achieve energy-savings due to the greater power consumption of the vacuum pump under lower pressure and reduced temperatures.

The alcohol-sensing behaviour of SnO2 nanorods prepared by a facile solid state reaction

NASA Astrophysics Data System (ADS)

Gao, F.; Ren, X. P.; Wan, W. J.; Zhao, Y. P.; Li, Y. H.; Zhao, H. Y.

2017-02-01

SnO2 nanorods with the range of 12-85 nm in diameter were fabricated by a facile solid state reaction in the medium of NaCl-KCl mixture at room temperature and calcined at 600, 680, 760 and 840 oC, respectively. The XRD, TEM and XPS were employed to characterize the structure and morphology of the SnO2 nanorods. The influence of the calcination temperature on the gas sensing behaviour of the SnO2 nanorods with different diameter was investigated. The result showed that all the sensors had good response to alcohol. The response of the gracile nanorods prepared at a low calcined temperature demonstrated significantly better than the thick nanorods prepared at a high calcined temperature. The mechanism was attributed to the nonstoichiometric ratio of Sn/O and larger surface area of the gracile nanorods to enhance the oxygen surface adsorption.

Effects of calcining temperature on formation of hierarchical TiO2/g-C3N4 hybrids as an effective Z-scheme heterojunction photocatalyst

NASA Astrophysics Data System (ADS)

Lu, Lianying; Wang, Guohong; Zou, Min; Wang, Juan; Li, Jun

2018-05-01

Hierarchical TiO2/g-C3N4 heterojunction photocatalysts with well-defined multiscale porous TiO2 framework are synthesized by simply calcinating tetrabutyl titanate and melamine precursors. The samples have been characterized by XRD, XPS, SEM, TEM, FTIR, nitrogen absorption-desorption equipment and TGA. The photocatalytic activity of these samples has been investigated in photo-degradation of Rhodamine B (RhB). The results show that calcining temperature critically affects the microstructure, surface area, interface structure and catalytic properties of the prepared samples. At the optimal calcining temperature of 550 °C, the apparent reaction rate constant of the catalyst is 55.0 × 10-3 min-1, which is 16.2 fold of pure TiO2 (3.4 × 10-3 min-1) and 3.4 fold of pure g-C3N4 (16.4 × 10-3 min-1), respectively. The strengthened visible-light-driven photocatalytic activity is attributed to the formation of a unique Z-scheme TiO2/g-C3N4 heterojunction due to C- or N-doping at the surface of the porous TiO2 framework. This mechanism explains the observation in a series of radical trapping experiments that superoxide ions and photo-generated holes play major roles in the photo-decolorizing process while hydroxyl radicals are also involved with a minor role.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhao, Yajing; Chen, Yan; Chen, Kepi

In this study, the effects of doping with GeO 2 on the synthesis temperature, phase structure and morphology of (K 0.5Na 0.5)NbO 3 (KNN) ceramic powders were studied using XRD and SEM. The results show that KNN powders with good crystallinity and compositional homogeneity can be obtained after calcination at up to 900°C for 2 h. Introducing 0.5 mol.% GeO 2 into the starting mixture improved the synthesis of the KNN powders and allowed the calcination temperature to be decreased to 800°C, which can be ascribed to the formation of the liquid phase during the synthesis.

Adsorptive removal of arsenic by novel iron/olivine composite: Insights into preparation and adsorption process by response surface methodology and artificial neural network.

PubMed

Ghosal, Partha S; Kattil, Krishna V; Yadav, Manoj K; Gupta, Ashok K

2018-03-01

Olivine, a low-cost natural material, impregnated with iron is introduced in the adsorptive removal of arsenic. A wet impregnation method and subsequent calcination were employed for the preparation of iron/olivine composite. The major preparation process parameter, viz., iron loading and calcination temperature were optimized through the response surface methodology coupled with a factorial design. A significant variation of adsorption capacity of arsenic (measured as total arsenic), i.e., 63.15 to 310.85 mg/kg for arsenite [As(III) T ] and 76.46 to 329.72 mg/kg for arsenate [As(V) T ] was observed, which exhibited the significant effect of the preparation process parameters on the adsorption potential. The iron loading delineated the optima at central points, whereas a monotonous decreasing trend of adsorption capacity for both the As(III) T and As(V) T was observed with the increasing calcination temperature. The variation of adsorption capacity with the increased iron loading is more at lower calcination temperature showing the interactive effect between the factors. The adsorbent prepared at the optimized condition of iron loading and calcination temperature, i.e., 10% and 200 °C, effectively removed the As(III) T and As(V) T by more than 96 and 99%, respectively. The material characterization of the adsorbent showed the formation of the iron compound in the olivine and increase in specific surface area to the tune of 10 multifold compared to the base material, which is conducive to the enhancement of the adsorption capacity. An artificial neural network was applied for the multivariate optimization of the adsorption process from the experimental data of the univariate optimization study and the optimized model showed low values of error functions and high R 2 values of more than 0.99 for As(III) T and As(V) T . The adsorption isotherm and kinetics followed Langmuir model and pseudo second order model, respectively demonstrating the chemisorption in this study. Copyright © 2017 Elsevier Ltd. All rights reserved.

The influence of ozone on the photocatalytic degradation of phenol using TiO2 photocatalyst supported by Bayah natural zeolite

NASA Astrophysics Data System (ADS)

Sulaiman, Fatah; Sari, Denni Kartika; Kustiningsih, Indar

2017-05-01

Effect of ozone on the photocatalytic degradation of phenol using TiO2 photocatalyst which supported Bayah Natural Zeolite has been investigated. Phenol (merk Pro analys) was used as waste solution. TiO2 photocatalyst was obtained from Titanium isopropoxide using sol gel method which supported by Bayah Natural Zeolite. The influence of temperature of calcination and catalyst loading have been conducted. The calcination temperature of photocatalyst was 450°C, 500°C, 550°C dan 600°C while the catalyst loading of 0,1g/L; 0,3 g/L; 0,6 g/L; 1 g/L dan 1,2 g/L. Analysis of phenol concentration was used Hach Spechtrophotometer. To determine the effect of ozone on photocatalytic degradation during process ozone was flowed into reactor. The result showed the optimum calcination temperature was obtained at 500°C. The optimum catalyst loading to degrade the phenolic compounds was equal to 1g/L. In these optimum condition the conversion of phenol degradation was 87% after 5 hours. By adding ozone during the degradation process, the conversion reached 100% after 2 hours.

Preparation of highly active manganese oxides supported on functionalized MWNTs for low temperature NOx reduction with NH3

NASA Astrophysics Data System (ADS)

Pourkhalil, Mahnaz; Moghaddam, Abdolsamad Zarringhalam; Rashidi, Alimorad; Towfighi, Jafar; Mortazavi, Yadollah

2013-08-01

Manganese oxide catalysts (MnOx) supported on functionalized multi-walled carbon nanotubes (FMWNTs) for low temperature selective catalytic reduction (LTSCR) of nitrogen oxides (NOx) with NH3 in the presence of excess O2 were prepared by the incipient wetness impregnation method. These catalysts were characterized by N2 adsorption, Fourier transform infrared spectroscopy (FTIR), transmission electron microscope (TEM), X-ray diffraction (XRD), thermal gravimetric analysis (TGA) and H2-temperature programmed reduction (H2-TPR) methods. The effects of reaction temperature, MnOx loading, calcination temperature and calcination time were investigated. The presence of surface nitrate species under moderate calcination conditions may play a favorable role in the LTSCR of NOx with NH3. Under the reaction conditions of 200 °C, 1 bar, NO = NH3 = 900 ppm, O2 = 5 vol%, GHSV = 30,000 h-1 and 12 wt% MnOx, NOx conversion and N2 selectivity were 97% and 99.5%, respectively. The SCR activity was reduced in the presence of 100 ppm SO2 and 2.5 vol% H2O from 97% to 92% within 6 h at 200 °C, however such an effect was shown to be reversible by exposing the catalyst to a helium flow for 2 h at 350 °C due to thermal decomposition of ammonium sulphate salts.

Calcine Waste Storage at the Idaho Nuclear Technology and Engineering Center

DOE Office of Scientific and Technical Information (OSTI.GOV)

Staiger, Merle Daniel; M. C. Swenson

2005-01-01

This report documents an inventory of calcined waste produced at the Idaho Nuclear Technology and Engineering Center during the period from December 1963 to May 2000. The report was prepared based on calciner runs, operation of the calcined solids storage facilities, and miscellaneous operational information that establishes the range of chemical compositions of calcined waste stored at Idaho Nuclear Technology and Engineering Center. The report will be used to support obtaining permits for the calcined solids storage facilities, possible treatment of the calcined waste at the Idaho National Engineering and Environmental Laboratory, and to ship the waste to an off-sitemore » facility including a geologic repository. The information in this report was compiled from calciner operating data, waste solution analyses and volumes calcined, calciner operating schedules, calcine temperature monitoring records, and facility design of the calcined solids storage facilities. A compact disk copy of this report is provided to facilitate future data manipulations and analysis.« less

Effect of calcination temperature on the electrochemical properties of nickel-rich LiNi 0.76Mn 0.14Co 0.10O 2 cathodes for lithium-ion batteries

DOE PAGES

Zheng, Jianming; Yan, Pengfei; Estevez, Luis; ...

2018-05-01

High energy density, nickel (Ni)-rich, layered LiNi xMn yCo zO 2 (NMC, x ≥ 0.6) materials are promising cathodes for lithium-ion batteries. However, several technical challenges, such as fast capacity fading and high voltage instability, hinder their large-scale application. Herein, we identified an optimum calcining temperature range for the Ni-rich cathode LiNi 0.76Mn 0.14Co 0.10O 2 (NMC76). NMC76 calcined at 750–775 °C exhibits a high discharge capacity (~215 mAh g –1 when charged to 4.5 V) and retains ca. 79% of its initial capacity after 200 cycles. It also exhibits an excellent high-rate capability, delivering a capacity of more thanmore » 160 mAh g –1 even at a 10 C rate. The high performance of NMC76 is directly related to the optimized size of its primary particles (100–300 nm) (which onstitute the spherical secondary particles of >10 µm) and cation mixing. Higher calcination temperature (≥800 °C) leads to rapid increase of primary particle size, poor cycling stability, and inferior rate capability of NMC76 due to severe micro-strain and -crack formation upon repeated lithium-ion de/intercalations. Furthermore, NMC76 calcined at 750–775 °C is a very good candidate for the next generation of Li ion batteries.« less

Effect of calcination temperature on the electrochemical properties of nickel-rich LiNi 0.76Mn 0.14Co 0.10O 2 cathodes for lithium-ion batteries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zheng, Jianming; Yan, Pengfei; Estevez, Luis

High energy density, nickel (Ni)-rich, layered LiNi xMn yCo zO 2 (NMC, x ≥ 0.6) materials are promising cathodes for lithium-ion batteries. However, several technical challenges, such as fast capacity fading and high voltage instability, hinder their large-scale application. Herein, we identified an optimum calcining temperature range for the Ni-rich cathode LiNi 0.76Mn 0.14Co 0.10O 2 (NMC76). NMC76 calcined at 750–775 °C exhibits a high discharge capacity (~215 mAh g –1 when charged to 4.5 V) and retains ca. 79% of its initial capacity after 200 cycles. It also exhibits an excellent high-rate capability, delivering a capacity of more thanmore » 160 mAh g –1 even at a 10 C rate. The high performance of NMC76 is directly related to the optimized size of its primary particles (100–300 nm) (which onstitute the spherical secondary particles of >10 µm) and cation mixing. Higher calcination temperature (≥800 °C) leads to rapid increase of primary particle size, poor cycling stability, and inferior rate capability of NMC76 due to severe micro-strain and -crack formation upon repeated lithium-ion de/intercalations. Furthermore, NMC76 calcined at 750–775 °C is a very good candidate for the next generation of Li ion batteries.« less

Evolution of catalytic activity of Au-Ag bimetallic nanoparticles on mesoporous support for CO oxidation.

PubMed

Wang, Ai-Qin; Chang, Chun-Ming; Mou, Chung-Yuan

2005-10-13

We report a novel Au-Ag alloy catalyst supported on mesoporous aluminosilicate Au-Ag@MCM prepared by a one-pot synthesis procedure, which is very active for low-temperature CO oxidation. The activity was highly dependent on the hydrogen pretreatment conditions. Reduction at 550-650 degrees C led to high activity at room temperature, whereas as-synthesized or calcined samples did not show any activity at the same temperature. Using various characterization techniques, such as XRD, UV-vis, XPS, and EXAFS, we elucidated the structure and surface composition change during calcination and the reduction process. The XRD patterns show that particle size increased only during the calcination process on those Ag-containing samples. XPS and EXAFS data demonstrate that calcination led to complete phase segregation of the Au-Ag alloy and the catalyst surface is greatly enriched with AgBr after the calcination process. However, subsequent reduction treatment removed Br- completely and the Au-Ag alloy was formed again. The surface composition of the reduced Au-Ag@MCM (nominal Au/Ag = 3/1) was more enriched with Ag, with the surface Au/Ag ratio being 0.75. ESR spectra show that superoxides are formed on the surface of the catalyst and its intensity change correlates well with the trend of catalytic activity. A DFT calculation shows that CO and O2 coadsorption on neighboring sites on the Au-Ag alloy was stronger than that on either Au or Ag. The strong synergism in the coadsorption of CO and O2 on the Au-Ag nanoparticle can thus explain the observed synergetic effect in catalysis.

Effect of calcination environments and plasma treatment on structural, optical and electrical properties of FTO transparent thin films

NASA Astrophysics Data System (ADS)

Kafle, Madhav; Kapadi, Ramesh K.; Joshi, Leela Pradhan; Rajbhandari, Armila; Subedi, Deepak P.; Gyawali, Gobinda; Lee, Soo W.; Adhikari, Rajendra; Kafle, Bhim P.

2017-07-01

The dependence of the structural, optical and electrical properties of the FTO thin films on the film thickness (276 nm - 546 nm), calcination environment, and low temperature plasma treatment were examined. The FTO thin films, prepared by spray pyrolysis, were calcinated under air followed by either further heat treatment under N2 gas or treatment in low temperature atmospheric plasma. The samples before and after calcination under N2, and plasma treatment will be represented by Sair, SN2 and SPl, respectively, hereafter. The thin films were characterized by measuring the XRD spectra, SEM images, optical transmittance and reflectance, and sheet resistance of the films before and after calcination in N2 environment or plasma treatment. The presence of sharp and narrow multiple peaks in XRD spectra hint us that the films were highly crystalline (polycrystalline). The samples Sair with the thickness of 471 nm showed as high as 92 % transmittance in the visible range. Moreover, from the tauc plot, the optical bandgap Eg values of the Sair found to be noticeably lower than that of the samples SN2. Very surprisingly, the electrical sheet resistance (Rsh) found to decrease following the trend as Rshair > RshN2 > RshPl. The samples exposed to plasma found to possess the lowest RshPl (for film with thickness 546 nm, the RshPl was 17 Ω /sq.).

Effect of annealing temperature on titania nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Manikandan, K., E-mail: sanjaymani367@gmail.com; Arumugam, S., E-mail: sanjaymani367@gmail.com; Chandrasekaran, G.

2014-04-24

Titania polycrystalline samples are prepared by using sol-gel route hydrolyzing a alkoxide titanium precursor under acidic conditions. The as prepared samples are treated with different calcination temperatures. The anatase phase of titania forms when treated below 600°C, above that temperature the anatase phase tends to transform into the rutile phase of titania. The experimental determination of average grain size, phase formation, lattice parameters and the crystal structures of titania samples at different calcinations is done using X-ray diffraction (XRD). Fourier Transform Infra-red Spectroscopy (FTIR), UV-vis-NIR spectroscopy and Scanning Electron Microscopy (SEM) and Energy Dispersive Analysis X-ray are used to characterizemore » the samples to bring impact on the respective properties.« less

Oxidative desulfurization of benzothiophene and thiophene with WOx/ZrO2 catalysts: effect of calcination temperature of catalysts.

PubMed

Hasan, Zubair; Jeon, Jaewoo; Jhung, Sung Hwa

2012-02-29

Oxidative desulfurization (ODS) of model fuel containing benzothiophene (BT) or thiophene (Th) has been carried out with WO(x)/ZrO2 catalyst, which was calcined at various temperatures. Based on the conversion of BT in the model fuel, it can be shown that the optimum calcination temperature of WOx/ZrO2 catalyst is around 700 °C. The most active catalyst is composed of tetragonal zirconia (ZrO2) with well dispersed polyoxotungstate species and it is necessary to minimize the contents of the crystalline WO3 and monoclinic ZrO2 for a high BT conversion. The oxidation rate was interpreted with the first-order kinetics, and it demonstrated the importance of electron density since the kinetic constant for BT was higher than that for Th even though the BT is larger than Th in size. A WOx/ZrO2 catalyst, treated suitably, can be used as a reusable active catalyst in the ODS. Copyright © 2012 Elsevier B.V. All rights reserved.

Reduced graphene oxide modified NiFe-calcinated layered double hydroxides for enhanced photocatalytic removal of methylene blue

NASA Astrophysics Data System (ADS)

Zhao, Guoqing; Li, Caifeng; Wu, Xia; Yu, Jingang; Jiang, Xinyu; Hu, Wenjihao; Jiao, Feipeng

2018-03-01

Calcined layered double hydroxides (CLDH) are one of the remarkable photocatalysts passionately studied for photodecolorization of organic dyes. NiFe-CLDH was successfully modified by reduced graphene oxide (RGO) through a facile in situ crystallization technique. The obtained RGO/NiFe-CLDH composites were fully characterized by powder X-ray diffraction (XRD), Scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), Fourier transform infrared (FT-IR), and UV-vis diffuse reflectance spectroscopy (DRS). The results analysis indicated that RGO sheets could work as base course to prompt the growth of LDH crystallites and NiFe-LDH lamellar crystal promiscuously distributed on the sheets with a strong interplay between each other. The photocatalytic performance of RGO/NiFe-CLDH composites toward decolorization of methylene blue tightly depended on the mass fraction of RGO and calcinated temperature. At the RGO weight loading of 1%, calcination temperature of 500 °C, the photocatalytic degradation efficiency of RGO/NiFe-CLDH composites reached 93.0% within 5.0 h. The enhanced activity of RGO/NiFe-CLDH composites may be due to the concerted catalysis effect between two constituents of as-prepared composites.

Pore surface fractal analysis of palladium-alumina ceramic membrane using Frenkel-Halsey-Hill (FHH) model.

PubMed

Ahmad, A L; Mustafa, N N N

2006-09-15

The alumina ceramic membrane has been modified by the addition of palladium in order to improve the H(2) permeability and selectivity. Palladium-alumina ceramic membrane was prepared via a sol-gel method and subjected to thermal treatment in the temperature range 500-1100 degrees C. Fractal analysis from nitrogen adsorption isotherm is used to study the pore surface roughness of palladium-alumina ceramic membrane with different chemical composition (nitric acid, PVA and palladium) and calcinations process in terms of surface fractal dimension, D. Frenkel-Halsey-Hill (FHH) model was used to determine the D value of palladium-alumina membrane. Following FHH model, the D value of palladium-alumina membrane increased as the calcinations temperature increased from 500 to 700 degrees C but decreased after calcined at 900 and 1100 degrees C. With increasing palladium concentration from 0.5 g Pd/100 ml H(2)O to 2 g Pd/100 ml H(2)O, D value of membrane decreased, indicating to the smoother surface. Addition of higher amount of PVA and palladium reduced the surface fractal of the membrane due to the heterogeneous distribution of pores. However, the D value increased when nitric acid concentration was increased from 1 to 15 M. The effect of calcinations temperature, PVA ratio, palladium and acid concentration on membrane surface area, pore size and pore distribution also studied.

Photocatalytic Oxidation of Acetone Over High Thermally Stable TiO2 Nanosheets With Exposed (001) Facets.

PubMed

Shi, Ting; Duan, Youyu; Lv, Kangle; Hu, Zhao; Li, Qin; Li, Mei; Li, Xiaofang

2018-01-01

Anatase TiO 2 (A-TiO 2 ) usually exhibits superior photocatalytic activity than rutile TiO 2 (R-TiO 2 ). However, the phase transformation from A-TiO 2 to R-TiO 2 will inevitably happens when the calcination temperature is up to 600°C, which hampers the practical applications of TiO 2 photocatalysis in hyperthermal situations. In this paper, high energy faceted TiO 2 nanosheets (TiO 2 -NSs) with super thermal stability was prepared by calcination of TiOF 2 cubes. With increase in the calcination temperature from 300 to 600°C, TiOF 2 transforms into TiO 2 hollow nanoboxes (TiO 2 -HNBs) assembly from TiO 2 -NSs via Ostwald Rippening process. Almost all of the TiO 2 -HNBs are disassembled into discrete TiO 2 -NSs when calcination temperature is higher than 700°C. Phase transformation from A-TiO 2 to R-TiO 2 begins at 1000°C. Only when the calcination temperature is higher than 1200°C can all the TiO 2 -NSs transforms into R-TiO 2 . The 500°C-calcined sample (T500) exhibits the highest photoreactivity toward acetone oxidation possibly because of the production of high energy TiO 2 -NSs with exposed high energy (001) facets and the surface adsorbed fluorine. Surface oxygen vacancy, due to the heat-induced removal of surface adsorbed fluoride ions, is responsible for the high thermal stability of TiO 2 -NSs which are prepared by calcination of TiOF 2 cubes.

Synthesis and characterization of zeolite from coal fly ash

NASA Astrophysics Data System (ADS)

Liu, Yong; Luo, Qiong; Wang, Guodong; Li, Xianlong; Na, Ping

2018-05-01

Fly ash (FA) from coal-based thermal power plant was used to synthesize zeolite in NaOH solution with hydrothermal method in this work. Firstly, the effects of calcination and acid treatment on the removal of impurities in fly ash were studied. Then based on the pretreated FA, the effects of alkali concentration, reaction temperature and Si/Al ratio on the synthesis of zeolite were studied in detail. The mineralogy, morphology, thermal behavior, infrared spectrum and specific surface for the synthetic sample were investigated. The results indicated that calcination at 750 °C for 1.5 h can basically remove unburned carbon from FA, and 4 M hydrochloric acid treatment of calcined FA at 90 °C for 2 h will reduce the quality of about 34.3%wt, which are mainly iron, calcium and sulfur elements. The concentration of NaOH, reaction temperature and Si/Al ratio have important effect on the synthesis of zeolite. In this study, 0.5 M NaOH cannot obtain any zeolite. High temperature is beneficial to zeolite synthesis from FA, but easily lead to a variety of zeolites. The synthetic sample contains three kinds of zeolites such as zeolite P, sodalite and zeolite X, when the reaction conditions are 2 M NaOH and 120 °C for 24 h. In this research, quartz always exists in the synthetic sample, but will reduce with the increase of temperature. The synthetic zeolite has the specific surface area of about 42 m2 g‑1 and better thermal stability.

Photooxidative desulfurization for diesel using Fe / N - TiO2 photocatalyst

NASA Astrophysics Data System (ADS)

Khan, Muhammad Saqib; Kait, Chong Fai; Mutalib, Mohd Ibrahim Abdul

2014-10-01

A series of N - TiO2 with different mol% N was synthesized via sol-gel method and characterized using thermal gravimetric analyzer and raman spectroscopy. 0.2 wt% Fe was incorporated onto the calcined (200°C) N - TiO2 followed by calcination at 200°C, 250°C and 300°C. Photooxidative desulfurization was conducted in the presence of 0.2wt% Fe / N - TiO2 with different mol% N with and without oxidant (H2O2). Oxidative desulfurization was only achieved when H2O2 was used while without H2O2 no major effect on the sulfur removal. 0.2Fe -30N - H2O2 photocatalysts showed best performance at all calcination temperatures as compared to other mol% N - H2O2 photocatalysts. 16.45% sulfur removal was achieved using photocatalysts calcined at 300 °C.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bakel, Allen J.; Conner, Cliff; Quigley, Kevin

One of the missions of the Reduced Enrichment for Research and Test Reactors (RERTR) program (and now the National Nuclear Security Administrations Material Management and Minimization program) is to facilitate the use of low enriched uranium (LEU) targets for 99Mo production. The conversion from highly enriched uranium (HEU) to LEU targets will require five to six times more uranium to produce an equivalent amount of 99Mo. The work discussed here addresses the technical challenges encountered in the treatment of uranyl nitrate hexahydrate (UNH)/nitric acid solutions remaining after the dissolution of LEU targets. Specifically, the focus of this work is themore » calcination of the uranium waste from 99Mo production using LEU foil targets and the Modified Cintichem Process. Work with our calciner system showed that high furnace temperature, a large vent tube, and a mechanical shield are beneficial for calciner operation. One- and two-step direct calcination processes were evaluated. The high-temperature one-step process led to contamination of the calciner system. The two-step direct calcination process operated stably and resulted in a relatively large amount of material in the calciner cup. Chemically assisted calcination using peroxide was rejected for further work due to the difficulty in handling the products. Chemically assisted calcination using formic acid was rejected due to unstable operation. Chemically assisted calcination using oxalic acid was recommended, although a better understanding of its chemistry is needed. Overall, this work showed that the two-step direct calcination and the in-cup oxalic acid processes are the best approaches for the treatment of the UNH/nitric acid waste solutions remaining from dissolution of LEU targets for 99Mo production.« less

Arsenic removal from aqueous solutions using Fe3O4-HBC composite: effect of calcination on adsorbents performance.

PubMed

Baig, Shams Ali; Sheng, TianTian; Sun, Chen; Xue, XiaoQin; Tan, LiSha; Xu, XinHua

2014-01-01

The presence of elevated concentration of arsenic in water sources is considered to be health hazard globally. Calcination process is known to change the surface efficacy of the adsorbent. In current study, five adsorbent composites: uncalcined and calcined Fe3O4-HBC prepared at different temperatures (400°C and 1000°C) and environment (air and nitrogen) were investigated for the adsorptive removal of As(V) and As(III) from aqueous solutions determining the influence of solution's pH, contact time, temperature, arsenic concentration and phosphate anions. Characterizations from FTIR, XRD, HT-XRD, BET and SEM analyses revealed that the Fe3O4-HBC composite at higher calcination temperature under nitrogen formed a new product (fayalite, Fe2SiO4) via phase transformation. In aqueous medium, ligand exchange between arsenic and the effective sorbent site ( = FeOOH) was established from the release of hydroxyl group. Langmuir model suggested data of the five adsorbent composites follow the order: Fe3O4-HBC-1000°C(N2)>Fe3O4-HBC (uncalcined)>Fe3O4-HBC-400°C(N2)>Fe3O4-HBC-400°C(air)>Fe3O4-HBC-1000°C(air) and the maximum As(V) and As(III) adsorption capacities were found to be about 3.35 mg g(-1) and 3.07 mg g(-1), respectively. The adsorption of As(V) and As(III) remained stable in a wider pH range (4-10) using Fe3O4-HBC-1000°C(N2). Additionally, adsorption data fitted well in pseudo-second-order (R2>0.99) rather than pseudo-first-order kinetics model. The adsorption of As(V) and As(III) onto adsorbent composites increase with increase in temperatures indicating that it is an endothermic process. Phosphate concentration (0.0l mM or higher) strongly inhibited As(V) and As(III) removal through the mechanism of competitive adsorption. This study suggests that the selective calcination process could be useful to improve the adsorbent efficiency for enhanced arsenic removal from contaminated water.

Arsenic Removal from Aqueous Solutions Using Fe3O4-HBC Composite: Effect of Calcination on Adsorbents Performance

PubMed Central

Baig, Shams Ali; Sheng, TianTian; Sun, Chen; Xue, XiaoQin; Tan, LiSha; Xu, XinHua

2014-01-01

The presence of elevated concentration of arsenic in water sources is considered to be health hazard globally. Calcination process is known to change the surface efficacy of the adsorbent. In current study, five adsorbent composites: uncalcined and calcined Fe3O4-HBC prepared at different temperatures (400°C and 1000°C) and environment (air and nitrogen) were investigated for the adsorptive removal of As(V) and As(III) from aqueous solutions determining the influence of solution's pH, contact time, temperature, arsenic concentration and phosphate anions. Characterizations from FTIR, XRD, HT-XRD, BET and SEM analyses revealed that the Fe3O4-HBC composite at higher calcination temperature under nitrogen formed a new product (fayalite, Fe2SiO4) via phase transformation. In aqueous medium, ligand exchange between arsenic and the effective sorbent site ( = FeOOH) was established from the release of hydroxyl group. Langmuir model suggested data of the five adsorbent composites follow the order: Fe3O4-HBC-1000°C(N2)>Fe3O4-HBC (uncalcined)>Fe3O4-HBC-400°C(N2)>Fe3O4-HBC-400°C(air)>Fe3O4-HBC-1000°C(air) and the maximum As(V) and As(III) adsorption capacities were found to be about 3.35 mg g−1 and 3.07 mg g−1, respectively. The adsorption of As(V) and As(III) remained stable in a wider pH range (4–10) using Fe3O4-HBC-1000°C(N2). Additionally, adsorption data fitted well in pseudo-second-order (R 2>0.99) rather than pseudo-first-order kinetics model. The adsorption of As(V) and As(III) onto adsorbent composites increase with increase in temperatures indicating that it is an endothermic process. Phosphate concentration (0.0l mM or higher) strongly inhibited As(V) and As(III) removal through the mechanism of competitive adsorption. This study suggests that the selective calcination process could be useful to improve the adsorbent efficiency for enhanced arsenic removal from contaminated water. PMID:24967645

Thermal and structural characterization of synthetic and natural nanocrystalline hydroxyapatite.

PubMed

Sofronia, Ancuta M; Baies, Radu; Anghel, Elena M; Marinescu, Cornelia A; Tanasescu, Speranta

2014-10-01

The aim of this work was to study the thermal stability on heating and to obtain the processing parameters of synthetic and bone-derived hydroxyapatite over temperatures between room temperature and 1400°C by thermal analysis (thermogravimetry (TG)/differential scanning calorimetry (DSC) and thermo-mechanical analysis-TMA). Structural and surface modifications related to samples origin and calcination temperature were investigated by Fourier transformed infrared (FTIR) and Raman spectroscopy, X-ray diffraction (XRD) and BET method. FTIR spectra indicated that the organic constituents and carbonate are no longer present in the natural sample calcined at 800°C. Raman spectra highlighted the decomposition products of the hydroxyapatite. The calcination treatment modifies the processes kinetics of the synthetic samples, being able to isolate lattice water desorption processes of decarbonization and the dehydroxylation processes. Shrinkage of calcined synthetic sample increases by 10% compared to uncalcined synthetic powder. From the TMA correlated with TG analysis and heat capacity data it can be concluded that sintering temperature of the synthetic samples should be chosen in the temperature range of the onset of dehydroxylation and the temperature at which oxyapatite decomposition begins. Copyright © 2014 Elsevier B.V. All rights reserved.

Manufacture of barium hexaferrite (BaO3.98Fe2O3) from iron oxide waste of grinding process by using calcination process

NASA Astrophysics Data System (ADS)

Idayanti, N.; Dedi; Kristiantoro, T.; Mulyadi, D.; Sudrajat, N.; Alam, G. F. N.

2018-03-01

The utilization of iron oxide waste of grinding process as raw materials for making barium hexaferrite has been completed by powder metallurgy method. The iron oxide waste was purified by roasting at 800 °C temperature for 3 hours. The method used varying calcination temperature at 1000, 1100, 1200, and 1250 °C for 3 hours. The starting iron oxide waste (Fe2O3) and barium carbonate (BaCO3) were prepared by mol ratio of Fe2O3:BaCO3 from the formula BaO3.98Fe2O3. Some additives such as calcium oxide (CaO), silicon dioxide (SiO2), and polyvinyl alcohol (PVA) were added after calcination process. The samples were formed at the pressure of 2 ton/cm2 and sintered at the temperature of 1250 °C for 1 hour. The formation of barium hexaferrite compounds after calcination is determined by X-Ray diffraction. The magnetic properties were observed by Permagraph-Magnet Physik with the optimum characteristic at calcination temperature of 1250 °C with the induction of remanence (Br) = 1.38 kG, coercivity (HcJ) = 4.533 kOe, product energy maximum (BHmax) = 1.086 MGOe, and density = 4.33 g/cm3.

Biomimetic synthesis of hierarchical crystalline hydroxyapatite fibers in large-scale

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xing, Chaogang; Ge, Suxiang; Huang, Baojun

Highlights: ► Crystalline hierarchical hydroxyapatite (HAp) fibers are synthesized. ► We employ a biomimetic route by using cotton cloth as a natural bio-template. ► We study the effects of pH, ultrasonic cleaning time, and calcination temperature. ► We obtain an optimized reaction condition. ► This is a low cost method for production of hierarchical HAp fibers. -- Abstract: Crystalline hierarchical hydroxyapatite [Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}, HAp)] fibers were successfully synthesized via a biomimetic route by using cotton cloth as a natural bio-template. The effects of pH value, aging time, ultrasonic cleaning time, and calcination temperature on the purity andmore » morphology of the resulting hydroxyapatite (HAp) were monitored by scanning election microscope (SEM), X-ray diffraction (XRD), and infrared spectrophotometer (IR) to obtain an optimized reaction condition, namely, pH 9, ultrasonic cleaning for 1 min, aging for 24 h, and calcination at 600 °C for 4 h. We found that the natural cellulose could not only control the morphology of HAp but also lower its phase transformation temperature. The impact of this method lies in its low cost and successful production of large-scale patterning of three-dimensional hierarchical HAp fibers.« less

Effects of Calcination Temperature and Acid-Base Properties on Mixed Potential Ammonia Sensors Modified by Metal Oxides

PubMed Central

Satsuma, Atsushi; Katagiri, Makoto; Kakimoto, Shiro; Sugaya, Satoshi; Shimizu, Kenichi

2011-01-01

Mixed potential sensors were fabriated using yttria-stabilized zirconia (YSZ) as a solid electrolyte and a mixture of Au and various metal oxides as a sensing electrode. The effects of calcination temperature ranging from 600 to 1,000 °C and acid-base properties of the metal oxides on the sensing properties were examined. The selective sensing of ammonia was achieved by modification of the sensing electrode using MoO3, Bi2O3 and V2O5, while the use of WO3, Nb2O5 and MgO was not effective. The melting points of the former group were below 820 °C, while those of the latter group were higher than 1,000 °C. Among the former group, the selective sensing of ammonia was strongly dependent on the calcination temperature, which was optimum around melting point of the corresponding metal oxides. The good spreading of the metal oxides on the electrode is suggested to be one of the important factors. In the former group, the relative response of ammonia to propene was in the order of MoO3 > Bi2O3 > V2O5, which agreed well with the acidity of the metal oxides. The importance of the acidic properties of metal oxides for ammonia sensing was clarified. PMID:22319402

Effects of calcination temperature and acid-base properties on mixed potential ammonia sensors modified by metal oxides.

PubMed

Satsuma, Atsushi; Katagiri, Makoto; Kakimoto, Shiro; Sugaya, Satoshi; Shimizu, Kenichi

2011-01-01

Mixed potential sensors were fabriated using yttria-stabilized zirconia (YSZ) as a solid electrolyte and a mixture of Au and various metal oxides as a sensing electrode. The effects of calcination temperature ranging from 600 to 1,000 °C and acid-base properties of the metal oxides on the sensing properties were examined. The selective sensing of ammonia was achieved by modification of the sensing electrode using MoO(3), Bi(2)O(3) and V(2)O(5), while the use of WO(3,) Nb(2)O(5) and MgO was not effective. The melting points of the former group were below 820 °C, while those of the latter group were higher than 1,000 °C. Among the former group, the selective sensing of ammonia was strongly dependent on the calcination temperature, which was optimum around melting point of the corresponding metal oxides. The good spreading of the metal oxides on the electrode is suggested to be one of the important factors. In the former group, the relative response of ammonia to propene was in the order of MoO(3) > Bi(2)O(3) > V(2)O(5), which agreed well with the acidity of the metal oxides. The importance of the acidic properties of metal oxides for ammonia sensing was clarified.

Facile synthesis of both needle-like and spherical hydroxyapatite nanoparticles: effect of synthetic temperature and calcination on morphology, crystallite size and crystallinity.

PubMed

Wijesinghe, W P S L; Mantilaka, M M M G P G; Premalal, E V A; Herath, H M T U; Mahalingam, S; Edirisinghe, M; Rajapakse, R P V J; Rajapakse, R M G

2014-09-01

Synthetic hydroxyapatite (HA) nanoparticles, that mimic natural HA, are widely used as biocompatible coatings on prostheses to repair and substitute human bones. In this study, HA nanoparticles are prepared by precipitating them from a precursor solution containing calcium sucrate and ammonium dihydrogen orthophosphate, at a Ca/P mole ratio of 1.67:1, at temperatures, ranging from 10°C to 95°C. A set of products, prepared at different temperatures, is analyzed for their crystallinity, crystallite size, morphology, thermal stability and composition, by X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and Fourier transform infrared (FT-IR) spectroscopic techniques, while the other set is analyzed after calcining the respective products, soon after their synthesis, for 3h, at 700°C. The as-prepared products, after 2h of drying, without any calcination, are not crystalline, but they grow very slowly into needle-like morphologies, as they are ripened with time. The percentage crystallinity of the final products increases from 15% to 52%, with increasing the preparative temperature. The calcined samples always produce spherical nanoparticles of essentially the same diameter, between 90 nm and 100 nm, which does not change due to aging and preparative temperatures. Therefore, the same method can be utilized to synthesize both spherical and needle-like nanoparticles of hydroxyapatite, with well-defined sizes and shapes. The ability to use readily available cheap raw materials, for the synthesis of such well-defined crystallites of hydroxyapatite, is an added advantage of this method, which may be explored further for the scaling up of the procedures to suit to industrial scale synthesis of such hydroxyapatite nanoparticles. Copyright © 2014 Elsevier B.V. All rights reserved.

Effect of calcination temperature on the photodegradation efficiency of Ni/ZnO composite in removal of organic dye

NASA Astrophysics Data System (ADS)

Thein, Myo Thuya; Pung, Swee-Yong; Aziz, Azizan; Lockman, Zainovia; Itoh, Mitsuru

2017-07-01

ZnO based composite is an attractive UV light driven semiconductor photocatalyst to degrade organic compounds attributed to its wide bandgap (3.37 eV). In this study, Ni/ZnO composites were synthesized via solution precipitation method. The composites were calcinated at various temperature, i.e. from 250 °C to 700 °C and subsequently annealed at 500°C in reductive environment (hydrogen atmosphere). The diffraction peaks of all samples could be indexed to the hexagonal wurtzite ZnO. No diffraction peaks from Ni could be observed in all samples, suggesting that the amount of Ni in the composites were below the detection limit of X-ray diffraction (XRD). The field emission scanning electron microscope (FESEM) images confirm that all samples were rod-like structure with hexagonal tips. In addition, small Ni particles were homogeneously deposited on the surface of ZnO rods. This observation is supported by energy dispersive X-ray spectroscopy (EDX) analysis, showing present of Zn, O and Ni elements. It is noted that ZnO rods coupled with Ni experienced quenching of visible emission and enhancing of UV emission in room temperature photoluminescence (RTPL) analysis. The photodegradation efficiency of Ni/ZnO rods was improved when a higher calcination temperature was used. The removal of RhB dye under UV light (352 nm) by these photocatalysts followed pseudo first-order kinetic reaction. The Ni/ZnO composites synthesized at calcination temperature of 500 °C demonstrated the highest photodegradation efficiency of 37 % and the largest rate constant of 0.0053 min-1 after 75 min UV irradiation.

Electrochemical characterization for lithium vanadium phosphate with different calcination temperatures prepared by the sol–gel method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Yongchao; Wang, Shengping, E-mail: spwang@cug.edu.cn; Tao, Du

2015-09-15

Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C (LVP/C) composite materials were synthesized via a sol–gel method with oxalic acid as the chelating agent and polyethylene glycol (PEG) as the supplementary carbon source. The oxalic acid and PEG serve as double carbon sources. This study focused on the effect of different calcination temperatures on the electrochemical properties of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}. The diffraction peaks for all of the samples are well indexed to monoclinic Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} with a P2{sub 1}/n space group. The TGA data indicate that the residual carbon content of LVP/C-700 is the highest (i.e., 2.31more » wt.%), and as the calcination temperature increased, the residual carbon content of the material gradually decreased. SEM and TEM analyses indicated that the LVP particles that were calcined at 700 °C exhibit a uniform particle size distribution and the carbon coating exhibited a complete and orderly moderate thickness. The LVP/C-700 material exhibits the best electrochemical performance in the voltage range of 3.0 to 4.3 V and 0.1 C where the initial discharge capacity can reach 128.98 mAh g{sup −} {sup 1}. Even after 200 cycles, the discharge capacity was 119.31 mAh g{sup −} {sup 1}, and the capacity retention rate was 92.49%. - Highlights: • Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C composite materials have been synthesized via a sol–gel method with double carbon sources. • The different calcination temperatures affect the grain growth and crystallinity of the Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C materials. • The LVP/C-700 material exhibites the largest lithium ion diffusivity and electronic conductivity.« less

Electrochemical Properties of Graphene Oxide/Resol Composites as Electrode Materials for Supercapacitor Applications.

PubMed

Park, Geon Woo; Jeon, Sang Kwon; Yang, Jin Yong; Choi, Sung Dae; Kim, Geon Joong

2016-05-01

RGO/Resol carbon composites were prepared from a mixture of reduced GO and a low-molecular-weight phenolic resin (Resol) solution. The effects of the calcination temperature, amount of Resol added and KOH treatment on the electrochemical performance of the RGO/Resol composites were investigated. The physical and electrochemical properties of the composite materials were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Brunauer, Emmett and Teller (BET) surface areas measurements, and cyclic voltammetry (CV). The relationships between their physical properties and their electrochemical performance were examined for use as super-capacitors (SCs). The RGO/Resol composite calcined at 400 degrees C after the KOH loading showed dramatically improved electrochemical properties, showing a high BET surface and capacitance of 2190 m2/g and 220 F/g, respectively. The RGO/Resol composites calcined after the KOH treatment showed much better capacitor performance than those treated only thermally at the same temperature without KOH impregnation. The fabrication of high surface electrodes was essential for improving the SCs properties.

Study on the Growth Mechanism of K2Ti4O9 Crystal

NASA Astrophysics Data System (ADS)

Zhou, Xuesong; Fan, Jing; Wei, Xiaoli; Shen, Yi; Meng, Yanzhi

2018-04-01

Potassium hexatitanate (K2Ti4O9) whiskers were prepared by the kneading-drying-calcination method. After the preparation of products under different calcination temperatures and holding times, their morphology and structure were characterized by thermogravimetric and differential thermal, X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy. The XRD analysis showed that the reaction mixture was completely converted to K2Ti4O9 crystals at 800 °C when the T/K ratio was 3. Based on the analysis of LS (liquid-solid) growth mechanism, the corresponding transformation reaction mechanism during the roasting was elucidated. K2Ti4O9 whiskers grow mainly through the parallel action at a low temperature. With the increase in temperature, the series effect is obvious.

Preparation of Calcined Zirconia-Carbon Composite from Metal Organic Frameworks and Its Application to Adsorption of Crystal Violet and Salicylic Acid

PubMed Central

Hasan, Zubair; Cho, Dong-Wan; Nam, In-Hyun; Chon, Chul-Min; Song, Hocheol

2016-01-01

Zirconia-carbon (ZC) composites were prepared via calcination of Zr-based metal organic frameworks, UiO-66 and amino-functionalized UiO-66, under N2 atmosphere. The prepared composites were characterized using a series of instrumental analyses. The surface area of the ZC composites increased with the increase of calcination temperature, with the formation of a graphite oxide phase observed at 900 °C. The composites were used for adsorptive removal of a dye (crystal violet, CV) and a pharmaceutical and personal care product (salicylic acid, SA). The increase of the calcination temperature resulted in enhanced adsorption capability of the composites toward CV. The composite calcined at 900 °C exhibited a maximum uptake of 243 mg·g−1, which was much greater than that by a commercial activated carbon. The composite was also effective in SA adsorption (102 mg·g−1), and N-functionalization of the composite further enhanced its adsorption capability (109 mg·g−1). CV adsorption was weakly influenced by solution pH, but was more dependent on the surface area and pore volume of the ZC composite. Meanwhile, SA adsorption showed strong pH dependence, which implies an active role of electrostatic interactions in the adsorption process. Base-base repulsion and hydrogen bonding are also suggested to influence the adsorption of CV and SA, especially for the N-functionalized composite. PMID:28773387

Effects of calcining temperature on photocatalysis of g-C{sub 3}N{sub 4}/TiO{sub 2} composites for hydrogen evolution from water

DOE Office of Scientific and Technical Information (OSTI.GOV)

Qu, Ailan, E-mail: elainqal@163.com; Xu, Xinmei; Xie, Haolong

Highlights: • TiO{sub 2} promotes melon to form at 400 °C, whereas it forms at 500 °C for only melamine. • The highest photocatalytic activity was achieved when calcination was performed at 400 °C. • Coordinated N−Ti−N bonds were formed in MA/TiO{sub 2} (400) and disappeared at high temperature. • The surface area decreased and the pore size increased with increasing of temperature. • Only MA/TiO{sub 2} (400) has a narrower band gap than pure g-C{sub 3}N{sub 4}. - Abstract: A composite of graphitic carbon nitride and TiO{sub 2} (g-C{sub 3}N{sub 4}/TiO{sub 2}) with enhanced photocatalytic hydrogen evolution capacity wasmore » achieved by calcining melamine and TiO{sub 2} sol-gel precursor. Characterization results reveal that heating temperature had a great influence on the structure, surface area and properties of the composites. Compared with the polycondensation of pure melamine, the presence of TiO{sub 2} precursor can promote the formation of melon at a low temperature. The highest photocatalytic activity of g-C{sub 3}N{sub 4}/TiO{sub 2}(400) was achieved when the calcination was performed at 400 °C, exhibiting H{sub 2} production rate of 76.25 μmol/h under UV–vis light irradiation (λ > 320 nm) and 35.44 μmol/h under visible light irradiation (λ > 420 nm). The highest photocatalytic performance of g-C{sub 3}N{sub 4}/TiO{sub 2}(400) can be attributed to: (1) the strong UV–vis light absorption due to the narrow bandgap caused by synergic effect of TiO{sub 2} and g-C{sub 3}N{sub 4}, (2) high surface area and porosity, (3) the effective separation of photo-generated electron-holes owing to the favorable heterojunction between TiO{sub 2} and g-C{sub 3}N{sub 4}.« less

Structural morphology, upconversion luminescence and optical thermometric sensing behavior of Y2O3:Er(3+)/Yb(3+) nano-crystalline phosphor.

PubMed

Joshi, C; Dwivedi, A; Rai, S B

2014-08-14

Infrared-to-visible upconverting rare earths Er(3+)/Yb(3+) co-doped Y2O3 nano-crystalline phosphor samples have been prepared by solution combustion method followed by post-heat treatment at higher temperatures. A slight increase in average crystallite size has been found on calcinations verified by X-ray analysis. Transmission electron microscopy (TEM) confirms the nano-crystalline nature of the as-prepared and calcinated samples. Fourier transform infrared (FTIR) analysis shows the structural changes in as-prepared and calcinated samples. Upconversion and downconversion emission recorded using 976 and 532 nm laser sources clearly demonstrates a better luminescence properties in the calcinated samples as compared to as-prepared sample. Upconversion emission has been quantified in terms of standard chromaticity diagram (CIE) showing a shift in overall upconversion emission of as-prepared and calcinated samples. Temperature sensing behaviour of this material has also been investigated by measurement of fluorescence intensity ratio (FIR) of various signals in green emission in the temperature range of 315 to 555 K under 976 nm laser excitation. Copyright © 2014 Elsevier B.V. All rights reserved.

Nuclear forensics investigation of morphological signatures in the thermal decomposition of uranyl peroxide.

PubMed

Schwerdt, Ian J; Olsen, Adam; Lusk, Robert; Heffernan, Sean; Klosterman, Michael; Collins, Bryce; Martinson, Sean; Kirkham, Trenton; McDonald, Luther W

2018-01-01

The analytical techniques typically utilized in a nuclear forensic investigation often provide limited information regarding the process history and production conditions of interdicted nuclear material. In this study, scanning electron microscopy (SEM) analysis of the surface morphology of amorphous-UO 3 samples calcined at 250, 300, 350, 400, and 450°C from uranyl peroxide was performed to determine if the morphology was indicative of the synthesis route and thermal history for the samples. Thermogravimetic analysis-mass spectrometry (TGA-MS) and differential scanning calorimetry (DSC) were used to correlate transitions in the calcined material to morphological transformations. The high-resolution SEM images were processed using the Morphological Analysis for Material Attribution (MAMA) software. Morphological attributes, particle area and circularity, indicated significant trends as a result of calcination temperature. The quantitative morphological analysis was able to track the process of particle fragmentation and subsequent sintering as calcination temperature was increased. At the 90% confidence interval, with 1000 segmented particles, the use of Kolmogorov-Smirnov statistical comparisons allowed discernment between all calcination temperatures for the uranyl peroxide route. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

Improvement in synthesis of (K 0.5Na 0.5)NbO 3 powders by Ge 4+ acceptor doping

DOE PAGES

Zhao, Yajing; Chen, Yan; Chen, Kepi

2016-11-17

In this study, the effects of doping with GeO 2 on the synthesis temperature, phase structure and morphology of (K 0.5Na 0.5)NbO 3 (KNN) ceramic powders were studied using XRD and SEM. The results show that KNN powders with good crystallinity and compositional homogeneity can be obtained after calcination at up to 900°C for 2 h. Introducing 0.5 mol.% GeO 2 into the starting mixture improved the synthesis of the KNN powders and allowed the calcination temperature to be decreased to 800°C, which can be ascribed to the formation of the liquid phase during the synthesis.

Characteristics of nano-sized yttria powder synthesized by a polyvinyl alcohol solution route at low temperature.

PubMed

Lee, Sang-Jin; Jung, Choong-Hwan

2012-01-01

Nano-sized yttria (Y2O3) powders were successfully synthesized at a low temperature of 400 degrees C by a simple polymer solution route. PVA polymer, as an organic carrier, contributed to an atom-scale homogeneous precursor gel and it resulted in fully crystallized, nano-sized yttria powder with high specific surface area through the low temperature calcination. In this process, the content of PVA, calcination temperature and heating time affected the microstructure and crystallization behavior of the powders. The development of crystalline phase and the final particle size were strongly dependant on the oxidation reaction from the polymer burn-out step and the PVA content. In this paper, the PVA solution technique for the fabrication of nano-sized yttria powders is introduced. The effects of PVA content and holding time on the powder morphology and powder specific surface area are also studied. The characterization of the synthesized powders is examined by using XRD, DTA/TG, SEM, TEM and nitrogen gas adsorption. The yttria powder synthesized from the PVA content of 3:1 ratio and calcined at 400 degrees C had a crystallite size of about 20 nm or less with a high surface areas of 93.95-120.76 m2 g(-1).

A new in vivo screening model for posterior spinal bone formation: comparison of ten calcium phosphate ceramic material treatments.

PubMed

Wilson, Clayton E; Kruyt, Moyo C; de Bruijn, Joost D; van Blitterswijk, Clemens A; Oner, F Cumhur; Verbout, Abraham J; Dhert, Wouter J A

2006-01-01

This study presents a new screening model for evaluating the influence of multiple conditions on the initial process of bone formation in the posterior lumbar spine of a large animal. This model uses cages designed for placement on the decorticated transverse process of the goat lumbar spine. Five conduction channels per cage, each be defined by a different material treatment, are open to both the underlying bone and overlying soft tissue. The model was validated in ten adult Dutch milk goats, with each animal implanted with two cages containing a total of ten calcium phosphate material treatments according to a randomized complete block design. The ten calcium phosphate ceramic materials were created through a combination of material chemistry (BCP, TCP, HA), sintering temperature (low, medium, high), calcination and surface roughness treatments. To monitor the bone formation over time, fluorochrome markers were administered at 3, 5 and 7 weeks and the animals were sacrificed at 9 weeks after implantation. Bone formation in the conduction channels was investigated by histology and histomorphometry of non-decalcified sections using traditional light and epifluorescent microscopy. According to both observed and measured bone formation parameters, materials were ranked in order of increasing magnitude as follows: low sintering temperature BCP (rough and smooth) approximately medium sintering temperature BCP approximately = TCP > calcined low sintering temperature HA > non-calcined low sintering temperature HA > high sintering temperature BCP (rough and smooth) > high sintering temperature HA (calcined and non-calcined). These results agree closely with those obtained in previous studies of osteoconduction and bioactivity of ceramics thereby validating the screening model presented in this study.

Study on the mechanism of a manganese-based catalyst for catalytic NOX flue gas denitration

NASA Astrophysics Data System (ADS)

Zhang, Lei; Wen, Xin; Lei, Zhang; Gao, Long; Sha, Xiangling; Ma, Zhenhua; He, Huibin; Wang, Yusu; Jia, Yang; Li, Yonghui

2018-04-01

Manganese-based bimetallic catalysts were prepared with self-made pyrolysis coke as carrier and its denitration performance of low-temperature SCR (selective catalyst reduction) was studied. The effects of different metal species, calcination temperature, calcination time and the metal load quantity on the denitration performance of the catalyst were studied by orthogonal test. The denitration mechanism of the catalyst was analyzed by XRD (X-ray diffraction), SEM (scanning electron microscope), BET test and transient test. The experiments show that: * The denitration efficiency of Mn-based bimetallic catalysts mainly relates to the metal type, the metal load quantity and the catalyst adjuvant type. * The optimal catalyst preparation conditions are as follows: the load quantity of monometallic MnO2 is 10%, calcined at 300°C for 4h, and then loaded with 8% CeO2, calcined at 350°Cfor 3h. * The denitration mechanism of manganese-based bimetallic oxide catalysts is stated as: NH3 is firstly adsorbed by B acid center Mn-OH which nears Mn4+==O to form NH4+, NH4+ was then attacked by the gas phase NO to form N2, H2O and Mn3+-OH. Finally, Mn3+-OH was oxidized by O2 to regenerate Mn4+.

Extraction of caustic potash from spent tea for biodiesel Production

NASA Astrophysics Data System (ADS)

Sulaiman, Sarina; Faiz Che Fisol, Ahmad; Sharikh, Atikah Mohamed; Noraini Jimat, Dzun; Jamal, Parveen

2018-01-01

Biodiesel is an alternative to non-renewable fossil fuels due to its low gas emission and economical value. This study aims to extract caustic potash (KOH) from spent tea and to optimize the transesterfication process based on parameters such as amount of catalyst, reaction temperature and methanol to oil ratio. The spent tea was first dried at 60°C prior to calcination at 600°C for two hours. Caustic Potash were extracted from the calcined spent tea. The transesterification process was done based on Design of Experiments (DOE) to study the effects of amount of catalyst ranging from 0.5 wt % to 2.5 wt %, reaction temperature from 55°C to 65°C and methanol to oil ratio from 6:1 to 12:1 at a constant agitation rate of 300 rpm for three hours. The calcined spent tea produced was recorded the highest at 54.3 wt % and the extracted catalyst was 2.4 wt %. The optimized biodiesel yield recorded was 56.95% at the optimal conditions of 2.5 wt % amount of catalyst, 65°C reaction temperature and 9:1 methanol to oil ratio.

CALCINATION AND SINTERING MODELS FOR APPLICATION TO HIGH-TEMPERATURE, SHORT-TIME SULFATION OF CALCIUM-BASED SORBENTS

EPA Science Inventory

To simulate the staged availability of transient high surface area CaO observed in high-temperature flow-reactor data, the rate of calcination of CaCO3 or Ca(OH)2 is described by an empirical modification of the shrinking-core model. The physical model depicts particle decomposi...

Method of preparing porous, rigid ceramic separators for an electrochemical cell

DOEpatents

Bandyopadhyay, Gautam; Dusek, Joseph T.

1981-01-01

Porous, rigid separators for electrochemical cells are prepared by first calcining particles of ceramic material at temperatures above about 1200.degree. C. for a sufficient period of time to reduce the sinterability of the particles. A ceramic powder that has not been calcined is blended with the original powder to control the porosity of the completed separator. The ceramic blend is then pressed into a sheet of the desired shape and sintered at a temperature somewhat lower than the calcination temperature. Separator sheets of about 1 to 2.5 mm thickness and 30 to 70% porosity can be prepared by this technique. Ceramics such as yttria, magnesium oxide and magnesium-aluminum oxide have advantageously been used to form separators by this method.

Light Emission Intensities of Luminescent Y2O3:Eu and Gd2O3:Eu Particles of Various Sizes

PubMed Central

Adam, Jens; Metzger, Wilhelm; Koch, Marcus; Rogin, Peter; Coenen, Toon; Atchison, Jennifer S.; König, Peter

2017-01-01

There is great technological interest in elucidating the effect of particle size on the luminescence efficiency of doped rare earth oxides. This study demonstrates unambiguously that there is a size effect and that it is not dependent on the calcination temperature. The Y2O3:Eu and Gd2O3:Eu particles used in this study were synthesized using wet chemistry to produce particles ranging in size between 7 nm and 326 nm and a commercially available phosphor. These particles were characterized using three excitation methods: UV light at 250 nm wavelength, electron beam at 10 kV, and X-rays generated at 100 kV. Regardless of the excitation source, it was found that with increasing particle diameter there is an increase in emitted light. Furthermore, dense particles emit more light than porous particles. These results can be explained by considering the larger surface area to volume ratio of the smallest particles and increased internal surface area of the pores found in the large particles. For the small particles, the additional surface area hosts adsorbates that lead to non-radiative recombination, and in the porous particles, the pore walls can quench fluorescence. This trend is valid across calcination temperatures and is evident when comparing particles from the same calcination temperature. PMID:28336860

Catalytic dehydration of fructose to 5-hydroxymethylfurfural over Nb2O5 catalyst in organic solvent.

PubMed

Wang, Fenfen; Wu, Hai-Zhen; Liu, Chun-Ling; Yang, Rong-Zhen; Dong, Wen-Sheng

2013-03-07

The catalytic dehydration of fructose to 5-hydroxymethylfurfural (HMF) in DMSO was performed over Nb2O5 derived from calcination of niobic acid at various temperatures (300-700 °C). The catalysts were characterized by powder X-ray diffraction, N2 physical adsorption, temperature-programed desorption of NH3, n-butylamine titration using Hammett indicators, infrared spectroscopy of adsorbed pyridine, and X-ray photoelectron spectroscopy. It was found that both catalytic activity and surface acid sites decrease with increasing calcination temperatures. The Nb2O5 derived from calcination of niobic acid at 400 °C reveals the maximum yield of HMF among all the catalysts, although the amount of acid sites on the catalyst is lower than that on the sample calcined at 300 °C. The results suggest that the presence of larger amounts of strong acid sites on the surface of the Nb2O5 calcined at 300 °C may promote side reactions. The Nb2O5 prepared at 400 °C shows 100% fructose conversion with 86.2% HMF yield in DMSO at 120 °C after 2 h. The activity of the catalyst decreases gradually during recycle because of coke deposition; however, it can be fully recovered by calcination at 400 °C for 2 h, suggesting that this catalyst is of significance for practical applications. Copyright © 2012 Elsevier Ltd. All rights reserved.

Preparation of LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphors by a facile precursor method and their luminescent properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Xia; Liang, Pan; Huang, Hong-Sheng

2014-04-01

Graphical abstract: LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphor was obtained by calcining the precursor which was synthesized by boric acid melting method. It (a) exhibits much stronger PL intensity than that (b) prepared by conventional solid state reaction method. - Highlights: • A calcining precursor method was used for preparation of LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphor. • Precursor was prepared by boric acid melting method. • The luminescence intensity of LaB{sub 3}O{sub 6}:Eu{sup 3+} was enhanced by the present method. - Abstract: The LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphors were prepared by calcining the precursors which were synthesized by boric acid meltingmore » method using rare earth oxide and boric acid as raw materials, and they were characterized by EDS, XRD, IR, SEM and PL. The influences of reaction temperature for the preparation of precursor and subsequent calcination temperature and time of precursor on the luminescence properties of LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphor were investigated. The results showed that the LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphors with maximum luminescent intensity were obtained by calcining precursor at 1000 °C for 6 h, in which the precursor was prepared at 200 °C for 72 h. Compared with the conventional high temperature solid-state reaction method, the pure LaB{sub 3}O{sub 6}:Eu{sup 3+} phosphor can be obtained at relatively lower calcination temperature by the precursor method and exhibits much stronger emission intensity.« less

To study the effect of doping concentration of silver on structural and optical properties of cadmium oxide (CdO) nanostructure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Rajesh, E-mail: rkkaushik06@gmail.com; Dept. of Physics, Vaish College of Engineering, Rohtak-124001, Haryana; Sharma, Ashwani

The present work deals with study of structural and optical properties of Silver (Ag) doped Cadmium oxide (CdO) nanostructured synthesized by Chemical Co-precipitation Techniques followed by calcinations at small temperature. The doping concentrations were changing from 0.1 to 10 at% respectively. Structural analysis study of these calcined materials is carried out by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The optical properties of calcined samples were investigating by Fourier transformation infrared (FTIR)spectroscopy, UV-Visible Spectroscopy (UV-Vis). The structural properties analysis results revels that crystallite size are in the range of nano region and TEM results aremore » quite in accordance with XRD results.« less

Effect of calcination temperature on structure and photocatalytic activity under UV and visible light of nanosheets from low-cost magnetic leucoxene mineral

NASA Astrophysics Data System (ADS)

Charerntanom, Wissanu; Pecharapa, Wisanu; Pavasupree, Suttipan; Pavasupree, Sorapong

2017-07-01

This research has experimentally synthesized the nanosheets from the naturally-mineral magnetic leucoxene under the hydrothermal synthesis condition of 105 °C for 24 h. Magnetic leucoxene was utilized as the starting material due to its high TiO2 content (70-80%) and inexpensiveness. The characterization of the synthesized nanosheets was subsequently carried out: the crystalline structure, the chemical composition, the shape, the size and the specific surface area, by the X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Brunauer-Emmett-Teller (BET) specific surface area analysis. The analysis results indicated that the starting magnetic leucoxene is of rutile phase while the synthesized nanosheets are of titanate structure (H2TixO2x + 1). After calcination at the temperature range of 300 and 400 °C, the calcined samples demonstrated TiO2 (B). At 500 and 600 °C, the calcined nanosheets revealed a bi-crystalline mixture consisting of TiO2 (B) and anatase TiO2. At 700-1000 °C, the crystalline structure shows anatase and rutile phase. At 1100 °C, the prepared samples consisted of a mixture of anatase, rutile phase of TiO2, and Fe2O3 phase. The synthesized product also exhibited the flower-like morphology with 2-5 μm in diameter, and the nanosheets structure was slightly curved, with 100 nm to 2 μm in width and 1-3 nm in thickness. At 100-200 °C showed sheets-like structure. At 300-1100 °C, the calcined nanosheets became unstable and began to decompose and transform into nanoparticles. The increasing size of nanoparticle decreased the specific surface area of the nanosheets, caused by increasing calcination temperature. Furthermore, the BET specific surface area of the nanosheets was approximately 279.8 m2/g. More importantly, the synthesized nanosheets achieved the higher photocatalytic activity under UV and visible light than did the commercial TiO2 nanoparticles (JRC-01, JRC-03, ST-01 and P-25).

Effect of synthesis route on electrical and ethanol sensing characteristics for LaFeO3-δ nanoparticles by citric sol-gel method

NASA Astrophysics Data System (ADS)

Cao, Ensi; Yang, Yuqing; Cui, Tingting; Zhang, Yongjia; Hao, Wentao; Sun, Li; Peng, Hua; Deng, Xiao

2017-01-01

LaFeO3-δ nanoparticles were prepared by citric sol-gel method with different raw material choosing and calcination process. The choosing of polyethylene glycol instead of ethylene glycol as raw material and additional pre-calcination at 400 °C rather than direct calcination at 600 °C could result in the decrease of resistance due to the reduction of activation energy Ea. Meanwhile, the choosing of ethylene glycol as raw material and additional pre-calcination leads to the enhancement of sensitivity to ethanol. Comprehensive analysis on the sensitivity and XRD, SEM, TEM, XPS results indicates that the sensing performance of LaFeO3-δ should be mainly determined by the adsorbed oxygen species on Fe ions, with certain contribution from native active oxygen. The best sensitivity of 46.1-200 ppm ethanol at prime working temperature of 112 °C is obtained by the sample using ethylene glycol as raw material with additional pre-calcination, which originates from its uniformly-sized and well-dispersed particles as well as high atomic ratio of Fe/La at surface region.

Structural and Optical Properties of Ag Nanoparticles Synthesized by Thermal Treatment Method.

PubMed

Gharibshahi, Leila; Saion, Elias; Gharibshahi, Elham; Shaari, Abdul Halim; Matori, Khamirul Amin

2017-04-12

The modified thermal treatment method via alternate oxygen and nitrogen flow was successfully employed to synthesize very narrow and pure Ag nanoparticles. The structural and optical properties of the obtained metal nanoparticles at different calcination temperatures between 400 and 800 °C were studied using various techniques. The FTIR and EDX confirmed the formation of Ag nanoparticles without a trace of impurities. The XRD spectra revealed that the amorphous sample at 30 °C had transformed into the cubic crystalline nanostructures at the calcination temperature of 400 °C and higher. The TEM images showed the formation of spherical Ag nanoparticles in which the average particle size decreased with increasing calcination temperature from 7.88 nm at 400 °C to 3.29 nm at 800 °C. The optical properties were determined by UV-vis absorption spectrophotometer, which showed an increase in the conduction band of Ag nanoparticles with increasing calcination temperature from 2.75 eV at 400 °C to 3.04 eV at 800 °C. This was due to less attraction between conduction electrons and metal ions as the particle size decreases in corresponding to fewer numbers of atoms that made up the metal nanoparticles.

Structural and Optical Properties of Ag Nanoparticles Synthesized by Thermal Treatment Method

PubMed Central

Gharibshahi, Leila; Saion, Elias; Gharibshahi, Elham; Shaari, Abdul Halim; Matori, Khamirul Amin

2017-01-01

The modified thermal treatment method via alternate oxygen and nitrogen flow was successfully employed to synthesize very narrow and pure Ag nanoparticles. The structural and optical properties of the obtained metal nanoparticles at different calcination temperatures between 400 and 800 °C were studied using various techniques. The FTIR and EDX confirmed the formation of Ag nanoparticles without a trace of impurities. The XRD spectra revealed that the amorphous sample at 30 °C had transformed into the cubic crystalline nanostructures at the calcination temperature of 400 °C and higher. The TEM images showed the formation of spherical Ag nanoparticles in which the average particle size decreased with increasing calcination temperature from 7.88 nm at 400 °C to 3.29 nm at 800 °C. The optical properties were determined by UV-vis absorption spectrophotometer, which showed an increase in the conduction band of Ag nanoparticles with increasing calcination temperature from 2.75 eV at 400 °C to 3.04 eV at 800 °C. This was due to less attraction between conduction electrons and metal ions as the particle size decreases in corresponding to fewer numbers of atoms that made up the metal nanoparticles. PMID:28772762

Effect of the Mn oxidation state and lattice oxygen in Mn-based TiO2 catalysts on the low-temperature selective catalytic reduction of NO by NH3.

PubMed

Lee, Sang Moon; Park, Kwang Hee; Kim, Sung Su; Kwon, Dong Wook; Hong, Sung Chang

2012-09-01

TiO2-supported manganese oxide catalysts formed using different calcination temperatures were prepared by using the wet-impregnation method and were investigated for their activity in the low-temperature selective catalytic reduction (SCR) of NO by NH3 with respect to the Mn valence and lattice oxygen behavior. The surface and bulk properties of these catalysts were examined using Brunauer-Emmett-Teller (BET) surface area, X-ray diffraction (XRD), temperature-programmed reduction (TPR), and temperature-programmed desorption (TPD). Catalysts prepared using lower calcination temperatures, which contained Mn4+ displayed high SCR activity at low temperatures and possessed several acid sites and active oxygen. The TPD analysis determined that the Brönsted and Lewis acid sites in the Mn/TiO2 catalysts were important for the low-temperature SCR at 80-160 and 200-350 degrees C, respectively. In addition, the available lattice oxygen was important for attaining high NO to NO2 oxidation at low temperatures. Recently, various Mn catalysts have been evaluated as SCR catalysts. However, there have been no studies on the relationship of adsorption and desorption properties and behavior of lattice oxygen according to the valence state for manganese oxides (MnO(x)). Therefore, in this study, the catalysts were prepared by the wet-impregnation method at different calcination temperatures in order to show the difference of manganese oxidation state. These catalysts were then characterized using various physicochemical techniques, including BET, XRD, TPR, and TPD, to understand the structure, oxidation state, redox properties, and adsorption and desorption properties of the Mn/TiO2 catalysts.

Method of preparing porous, rigid ceramic separators for an electrochemical cell. [Patent application

DOEpatents

Bandyopadhyay, G.; Dusek, J.T.

Porous, rigid separators for electrochemical cells are prepared by first calcining particles of ceramic material at temperatures above about 1200/sup 0/C for a sufficient period of time to reduce the sinterability of the particles. A ceramic powder that has not been calcined is blended with the original powder to control the porosity of the completed separator. The ceramic blend is then pressed into a sheet of the desired shape and sintered at a temperature somewhat lower than the calcination temperature. Separator sheets of about 1 to 2.5 mm thickness and 30 to 70% porosity can be prepared by this technique. Ceramics such as yttria, magnesium oxide, and magnesium-aluminium oxide have advantageously been used to form separators by this method.

Preparation of Self-assembly Mesoporous TiO2 Using Block Copolymer Pluronic PE6200 Template

NASA Astrophysics Data System (ADS)

Septina, W.; Yuliarto, B.; Nugraha

2008-03-01

In this research, nanocrystal mesoporous TiO2 powders were synthesized by sol-gel method, with TiCl4 as a precursor in methanol solution. Block copolymer Pluronic PE 6200 was used as pores template. It was found that from the XRD measurements, both at 400 °C and 450 °C calcination temperatures, resulted in nanocrystal TiO2 with anatase phase. Based on N2 adsorption characterization (BET method), TiO2 samples have surface area 108 m2/g and 88 m2/g for 400 °C and 450 °C calcination temperatures respectively. From Small-angle Neutron Scattering (SANS) patterns, it is investigated that TiO2 samples have mesoporous structure where the pore order degree depend on the calcination temperature.

Co and Fe-catalysts supported on sepiolite: effects of preparation conditions on their catalytic behaviors in high temperature gas flow treatment of dye.

PubMed

Lin, Xiangfeng; Fang, Jian; Chen, Menglin; Huang, Zhi; Su, Chengyuan

2016-08-01

An efficient adsorbent/catalyst Co and Fe-catalysts loaded on sepiolite (Co-Fe/sepiolite) was successfully prepared for high temperature gas flow catalytic reaction by a simple impregnation method. The impact of preparation conditions (such as pH value of impregnation solution, impregnation time, calcination temperature, and time) on catalytic activity was studied. We found that the catalytic activity of Co-Fe/sepiolite was strongly influenced by all the investigated parameters. The regeneration efficiency (RE) was used to evaluate the catalytic activity. The RE is more noticeable at pH 5.0 of impregnation solution, impregnation time 18 h, calcination temperature 650 °C, and calcination time 3 h. This Co-Fe/sepiolite has great adsorption capacity in absorbing dye. It is used for an adsorbent to adsorb dye from wastewater solution under dynamic adsorption and saturated with dye, then regenerated with high temperature gas flow for adsorption/oxidation cycles. The Co-Fe/sepiolite acts as a catalyst to degrade the dye during regeneration under high temperature gas flow. Hence, the Co-Fe/sepiolite is not only an adsorbent but also a catalyst. The Co-Fe/sepiolite is more stable than sepiolite when applied in the treatment of plant's wastewater. The Co-Fe/sepiolite can be reused in adsorption-regeneration cycle. The results indicate the usability of the proposed combined process, dye adsorption on Co-Fe/sepiolite followed by the catalytic oxidation in high temperature gas flow.

Synthesis process and photocatalytic properties of BiOBr nanosheets for gaseous benzene.

PubMed

Liu, Yu; Yin, Yongquan; Jia, Xueqing; Cui, Xiangyu; Tian, Canrui; Sang, Yuanhua; Liu, Hong

2016-09-01

A series of nano-BiOBr were prepared by an effective hydrothermal method in the presence of cetyltrimethyl ammonium bromide (CTAB) and ethanol at different calcination temperatures. The as-prepared nano-BiOBr samples were characterized by measuring the specific area (S BET), UV-Vis diffuse reflectance spectrum, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD). The results show that the calcination temperature has an important impact on the morphology and microstructure of BiOBr. The nano-BiOBr calcined at 120 °C showed excellent photocatalytic degradation properties for benzene, with photocatalytic degradation rate of 75 % for benzene under UV irradiation for 90 min, and removal efficiency of benzene was significantly enhanced by using nano-BiOBr catalyst compared to UV irradiation alone. BiOBr catalyst possessed good photocatalytic activity even after three consecutive photocatalytic reaction cycles, illustrating its excellent stability. The photocatalytic degradation of benzene followed the first-order kinetics, and the good catalytic capability of nano-BiOBr catalyst can be attributed to its crystalline, hierarchical nanostructure and nanosheet thickness.

Structural and fractal characterization of tungstophosphoric acid modified titanium dioxide photocatalyst

NASA Astrophysics Data System (ADS)

Petrović, S.; Rožić, Lj; Vuković, Z.; Grbić, B.; Radić, N.; Stojadinović, S.; Vasilić, R.

2017-04-01

This article presents the comparison of structural and fractal properties of nanocrystalline titanium dioxide (TiO2) and TiO2 modified with tungstophosphoric acid (TiO2/HPW) and their impact on the photocatalytic degradation of hazardous water pollutants. TiO2 and TiO2/HPW samples were synthesized by a combined sol-gel and hydrothermal processing. The XRD analysis of pure TiO2 samples revealed that phase composition was mainly dependent on the calcination temperature, changing from amorphous TiO2 to crystalline anatase and rutile by increasing the temperature. On the other hand, the XRD of TiO2/HPW samples calcined at temperatures above 600 °C showed crystalline peaks associated to formation of WO3 and WO2.92 crystalline domains. The N2 adsorption-desorption isotherm and pore size distribution of TiO2/HPW samples detected the existence of mesoporous characteristic with very narrow bimodal pores in the mesoporous region. The structural heterogeneity of samples was analyzed by means of pore size distribution functions, while the variation in fractal dimension were determined from the nitrogen adsorption isotherms, using the modified Frenkel-Halsey-Hill method. The results demonstrate that the approach is capable of characterizing complex textures such as those present in the TiO2 and TiO2/HPW photocatalysts. Besides, the effect of calcinations condition on photocatalytic properties of the samples was also investigated. The highest efficiency with respect to methyl orange photodecomposition was observed for TiO2/HPW photocatalysts calcined at 700 °C.

Passivation of pigment particles for thermal control coatings

NASA Technical Reports Server (NTRS)

Farley, E. P.; Sancier, K. M.; Morrison, S. R.

1973-01-01

Five powders were received for plasma calcining during this report period. The particle size using a fluid energy mill, and obtained pigments that could be plasma calcined. Optimum results are obtained in the plasma calcining of zinc orthotitanate when finely dispersed particles are subjected to a calculated plasma temperature of 1670 C. Increasing the plasma calcining time by using multiple passes through the plasma stabilized the pigment to vacuum UV irradiation was evidenced by the resulting ESR spectra but slightly decreased the whiteness of the pigment. The observed darkening is apparently associated with the formation of Ti(+3) color centers.

Cordierite-supported metal oxide for non-methane hydrocarbon oxidation in cooking oil fumes.

PubMed

Huang, Yonghai; Yi, Honghong; Tang, Xiaolong; Zhao, Shunzheng; Gao, Fengyu; Wang, Jiangen; Yang, Zhongyu

2018-05-21

Cooking emission is an important reason for the air quality deterioration in the metropolitan area in China. Transition metal oxide and different loading of manganese oxide supported on cordierite were prepared by incipient wetness impregnation method and were used for non-methane hydrocarbon (NMHC) oxidation in cooking oil fumes (COFs). The effects of different calcination temperature and different Mn content were also studied. The SEM photographs and CO 2 temperature-programmed desorption revealed 5 wt% Mn/cordierite had the best pore structure and the largest number of the weak and moderate basic sites so it showed the best performance for NMHC oxidation. XRD analysis exhibited 5 wt% Mn/cordierite had the best dispersion of active phase and the active phase was MnO 2 when the calcination temperature was 400℃ which were good for the catalytic oxidation of NMHC.

Carbon dioxide capture from a cement manufacturing process

DOEpatents

Blount, Gerald C [North Augusta, SC; Falta, Ronald W [Seneca, SC; Siddall, Alvin A [Aiken, SC

2011-07-12

A process of manufacturing cement clinker is provided in which a clean supply of CO.sub.2 gas may be captured. The process also involves using an open loop conversion of CaO/MgO from a calciner to capture CO.sub.2 from combustion flue gases thereby forming CaCO.sub.3/CaMg(CO.sub.3).sub.2. The CaCO.sub.3/CaMg(CO.sub.3).sub.2 is then returned to the calciner where CO.sub.2 gas is evolved. The evolved CO.sub.2 gas, along with other evolved CO.sub.2 gases from the calciner are removed from the calciner. The reactants (CaO/MgO) are feed to a high temperature calciner for control of the clinker production composition.

Corn-like indium tin oxide nanostructures: fabrication, characterization and formation mechanism

NASA Astrophysics Data System (ADS)

Wu, Xu; Wang, Yihua; Yang, Bin

2015-11-01

Electrospinning is a simple but efficient procedure enabling the parallel fabrication of a multitude of inorganic fibers. But the precise control of the fiber's morphology, which seriously affects the electrical, optical and other important properties of such electrospun materials, is still less developed. The creation of nanoscale indium tin oxide fibers with corn-like geometry (corn-like ITO NFs) by our group has provided a good example to show how to modify the morphologies and properties of nanofibers by means of tailoring the fiber's compositions. Here we show that in the fabrication of corn-like ITO NFs, the usage of different solvents N, N-dimethylformamide (DMF) and deionized water, as well as the calcination temperature, can also lead to dramatic morphology changes, from ribbon-like to cylindrical and then to corn-like. The resultant nanoribbons and nanoscale corn-like fibers exhibit different photoluminescence properties. We find that the morphology of the as-spun fibers is closely related to the vapor pressure of the solvent we used, and the generation of ITO crystals sensitively depends on the calcination temperature, which both are critical for the morphology and properties of the final products. Thus, we demonstrate that the formation of this unprecedented nanostructure is determined by the combined effect of the precursor chemical composition, solvent and calcination temperature.

Effects of Coal Gangue on Cement Grouting Material Properties

NASA Astrophysics Data System (ADS)

Liu, J. Y.; Chen, H. X.

2018-05-01

The coal gangue is one of the most abundant industrial solid wastes and pollute source of air and water. The use of coal gangue in the production of cement grouting material comforms to the basic state policy of environment protection and the circular using of natural resources. Through coal gangue processing experiment, coal gangue cement grouting materials making test, properties detection of properties and theoretical analysis, the paper studied the effects of coal gangue on the properties of cement grouting materials. It is found that at the range of 600 to 700 °C, the fluidity and the compressive and flexural strengths of the cement grouting materials increase with the rising up of the calcination temperatures of coal gangue. The optimum calcination temperature is around 700 °C. The part substitution of cement by the calcined coal gangue in the cement grouting material will improve the mechanical properties of the cement grouting material, even thought it will decrease its fluidity. The best substitution amount of cement by coal gangue is about 30%. The fluidity and the long term strength of the ordinary silicate cement grouting material is obviously higher than that of the sulphoaluminate cement one as well as that of the silicate-sulphoaluminate complex cement one.

The Ca-looping process for CO2 capture and energy storage: role of nanoparticle technology

NASA Astrophysics Data System (ADS)

Valverde, Jose Manuel

2018-02-01

The calcium looping (CaL) process, based on the cyclic carbonation/calcination of CaO, has come into scene in the last years with a high potential to be used in large-scale technologies aimed at mitigating global warming. In the CaL process for CO2 capture, the CO2-loaded flue gas is used to fluidize a bed of CaO particles at temperatures around 650 °C. The carbonated particles are then circulated into a calciner reactor wherein the CaO solids are regenerated at temperatures near 950 °C under high CO2 concentration. Calcination at such harsh conditions causes a marked sintering and loss of reactivity of the regenerated CaO. This main drawback could be however compensated from the very low cost of natural CaO precursors such as limestone or dolomite. Another emerging application of the CaL process is thermochemical energy storage (TCES) in concentrated solar power (CSP) plants. Importantly, carbonation/calcination conditions to maximize the global CaL-CSP plant efficiency could differ radically from those used for CO2 capture. Thus, carbonation could be carried out at high temperatures under high CO2 partial pressure for maximum efficiency, whereas the solids could be calcined at relatively low temperatures in the absence of CO2 to promote calcination. Our work highlights the critical role of carbonation/calcination conditions on the performance of CaO derived from natural precursors. While conditions in the CaL process for CO2 capture lead to a severe CaO deactivation with the number of cycles, the same material may exhibit a high and stable conversion at optimum CaL-CSP conditions. Moreover, the type of CaL conditions influences critically the reaction kinetics, which plays a main role on the optimization of relevant operation parameters such as the residence time in the reactors. This paper is devoted to a brief review on the latest research activity in our group concerning these issues as well as the possible role of nanoparticle technology to enhance the activity of Ca-based materials at CaL conditions for CO2 capture and energy storage.

Growth of thin film containing high density ZnO nanorods with low temperature calcinated seed layer

NASA Astrophysics Data System (ADS)

Panda, Rudrashish; Samal, Rudranarayan; Khatua, Lizina; Das, Susanta Kumar

2018-05-01

In this work we demonstrate the growth of thin film containing high density ZnO nanorods by using drop casting of the seed layer calcinated at a low temperature of 132 °C. Chemical bath deposition (CBD) method is used to grow the nanorods. X-ray diffraction (XRD) analysis and Field Emission Scanning Electron Microscopy (FESEM) are performed for the structural and morphological characterizations of the nanorods. The average diameter and length of nanorods are found to be 33 nm and 270 nm respectively. The bandgap of the material is estimated to be 3.2 eV from the UV-Visible absorption spectroscopy. The reported method is much more cost-effective and can be used for growth of ZnO nanorods for various applications.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chudnovsky, Yaroslav; Kozlov, Aleksandr

Green petroleum coke (GPC) is an oil refining byproduct that can be used directly as a solid fuel or as a feedstock for the production of calcined petroleum coke. GPC contains a high amount of volatiles and sulfur. During the calcination process, the GPC is heated to remove the volatiles and sulfur to produce purified calcined coke, which is used in the production of graphite, electrodes, metal carburizers, and other carbon products. Currently, more than 80% of calcined coke is produced in rotary kilns or rotary hearth furnaces. These technologies provide partial heat utilization of the calcined coke to increasemore » efficiency of the calcination process, but they also share some operating disadvantages. However, coke calcination in an electrothermal fluidized bed (EFB) opens up a number of potential benefits for the production enhancement, while reducing the capital and operating costs. The increased usage of heavy crude oil in recent years has resulted in higher sulfur content in green coke produced by oil refinery process, which requires a significant increase in the calcinations temperature and in residence time. The calorific value of the process off-gas is quite substantial and can be effectively utilized as an “opportunity fuel” for combined heat and power (CHP) production to complement the energy demand. Heat recovered from the product cooling can also contribute to the overall economics of the calcination process. Preliminary estimates indicated the decrease in energy consumption by 35-50% as well as a proportional decrease in greenhouse gas emissions. As such, the efficiency improvement of the coke calcinations systems is attracting close attention of the researchers and engineers throughout the world. The developed technology is intended to accomplish the following objectives: - Reduce the energy and carbon intensity of the calcined coke production process. - Increase utilization of opportunity fuels such as industrial waste off-gas from the novel petroleum coke calcination process. - Increase the opportunity of heat (chemical and physical) utilization from process off-gases and solid product. - Develop a design of advanced CHP system utilizing off-gases as an “opportunity fuel” for petroleum coke calcinations and sensible heat of calcined coke. A successful accomplishment of the aforementioned objectives will contribute toward the following U.S. DOE programmatic goals: - Drive a 25% reduction in U. S. industrial energy intensity by 2017 in support of EPAct 2005; - Contribute to an 18% reduction in U.S. carbon intensity by 2012 as established by the Administration’s “National Goal to Reduce Emissions Intensity.” 8« less

Cobalt ferrite sphere-coated buckhorn-like barium titanate: Fabrication, characterization, its dielectric resonance, and microwave attenuation properties

NASA Astrophysics Data System (ADS)

Ji, Renlong; Cao, Chuanbao

2014-10-01

Barium titanate (BTO) with different morphology is prepared through hydrothermal method using titania spheres as precursor, then calcined at different temperatures and ultimately coated with cobalt ferrite (BTO/CFO). The dielectric dispersion of the composite containing BTO (75 wt. % ratio in paraffin wax) shows evidence of resonance behaviour in the microwave spectrum, rather than the usually observed relaxation mode. The imaginary part of permittivity (ɛ″) displays a strong peak in the 10-13 GHz frequency region, especially for buckhorn-like BTO (hydrothermally synthesized at 110 °C and calcined at 1100 °C). The dielectric response anomaly of BTO in special morphology is due to the emission of plane acoustic waves caused by electrostrictive and converse piezoelectric effects. An accepted model is adopted to simulate the resonance frequency. The minimum reflection loss of cauliflower-like BTO (hydrothermally synthesized at 110 °C, then calcined at 600 °C for 2 h, 75 wt. % ratio) in paraffin wax reaches -30.831 dB at 10.56 GHz with a matching thickness of 2 mm, lower than all the reported values. When the sintering temperature is changed to 1100 °C (buckhorn-like BTO), the minimum reflection loss value is -24.37 dB at 12.56 GHz under the thickness of 3 mm. After combination with CFO, the value reaches -42.677 dB when the thickness is 5.6 mm. The ginger-like BTO (hydrothermally synthesized at 200 °C and calcined at different temperatures) is inferior in microwave reflection reduction. The electromagnetic interference shielding effectiveness of buckhorn-like BTO composite is calculated to be -12.7 dB (94.6% shielding) at resonance frequency (2 mm, 11.52 GHz). This work clearly shows the potential to tune the dielectric property of ferroelectrics through control of morphology, facilitating new comprehension of the ferroelectrics in microwave regime.

Stabilization of As-, Pb-, and Cu-contaminated soil using calcined oyster shells and steel slag.

PubMed

Moon, Deok Hyun; Wazne, Mahmoud; Cheong, Kyung Hoon; Chang, Yoon-Young; Baek, Kitae; Ok, Yong Sik; Park, Jeong-Hun

2015-07-01

In this study, As-, Pb-, and Cu-contaminated soil was stabilized using calcined oyster shells (COS) and steel slag (SS). The As-contaminated soil was obtained from a timber mill site where chromate copper arsenate (CCA) was used as a preservative. On the other hand, Pb- and Cu-contaminated soil was obtained from a firing range. These two soils were thoroughly mixed to represent As-, Pb-, and Cu-contaminated soil. Calcined oyster shells were obtained by treating waste oyster shells at a high temperature using the calcination process. The effectiveness of stabilization was evaluated by 1-N HCl extraction for As and 0.1-N HCl extraction for Pb and Cu. The treatment results showed that As, Pb, and Cu leachability were significantly reduced upon the combination treatment of COS and SS. The sole treatment of SS (10 wt%) did not show effective stabilization. However, the combination treatment of COS and SS showed a significant reduction in As, Pb, and Cu leachability. The best stabilization results were obtained from the combination treatment of 15 wt% COS and 10 wt% SS. The SEM-EDX results suggested that the effective stabilization of As was most probably achieved by the formation of Ca-As and Fe-As precipitates. In the case of Pb and Cu, stabilization was most probably associated with the formation of pozzolanic reaction products such as CSHs and CAHs.

Laboratory study on the high-temperature capture of HCl gas by dry-injection of calcium-based sorbents.

PubMed

Shemwell, B; Levendis, Y A; Simons, G A

2001-01-01

This is a laboratory study on the reduction of combustion-generated hydrochloric acid (HCl) emissions by in-furnace dry-injection of calcium-based sorbents. HCl is a hazardous gaseous pollutant emitted in significant quantities by municipal and hazardous waste incinerators, coal-fired power plants, and other industrial furnaces. Experiments were conducted in a laboratory furnace at gas temperatures of 600-1000 degrees C. HCl gas diluted with N2, and sorbent powders fluidized in a stream of air were introduced into the furnace concurrently. Chlorination of the sorbents occurred in the hot zone of the furnace at gas residence times approximately 1 s. The sorbents chosen for these experiments were calcium formate (CF), calcium magnesium acetate (CMA), calcium propionate (CP), calcium oxide (CX), and calcium carbonate (CC). Upon release of organic volatiles, sorbents calcine to CaO at approximately 700 degrees C, and react with the HCl according to the reaction CaO + 2HCl <=> CaCl2 + H2O. At the lowest temperature case examined herein, 600 degrees C, direct reaction of HCl with CaCO3 may also be expected. The effectiveness of the sorbents to capture HCl was interpreted using the "pore tree" mathematical model for heterogeneous diffusion reactions. Results show that the thin-walled, highly porous cenospheres formed from the pyrolysis and calcination of CF, CMA, and CP exhibited high relative calcium utilization at the upper temperatures of this study. Relative utilizations under these conditions reached 80%. The less costly low-porosity sorbents, calcium carbonate and calcium oxide also performed well. Calcium carbonate reached a relative utilization of 54% in the mid-temperature range, while the calcium oxide reached an 80% relative utilization at the lowest temperature examined. The data matched theoretical predictions of sorbent utilization using the mathematical model, with activation energy and pre-exponential factors for the calcination reaction of 17,000 K and 300,000 (g gas/cm2/s/atm gas), respectively. Thus, the kinetics of the calcination reaction were found to be much faster (approximately 500 times) than those of the sulfation reaction examined previously in this laboratory.

Biodiesel synthesis using calcined layered double hydroxide catalysts

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schumaker, J. Link; Crofcheck, Czarena; TAckett, S. Adam

2008-01-01

The catalytic properties of calcined Li-Al, Mg-Al and Mg-Fe layered double hydroxides (LDHs) were examined in two transesterification reactions, namely, the reaction of glyceryl tributyrate with methanol, and the reaction of soybean oil with methanol. While the Li-Al catalysts showed high activity in these reactions at the reflux temperature of methanol, the Mg-Fe and Mg-Al catalysts exhibited much lower methyl ester yields. CO2 TPD measurements revealed the presence of sites of weak, medium and strong basicity on both Mg-Al and Li-Al catalysts, the latter showing higher concentrations of medium and strong base sites; by implication, these are the main sitesmore » active in transesterification catalyzed by calcined Li-Al LDHs. Maximum activity was observed for the Li-Al catalysts when a calcination temperature of 450-500 aC was applied, corresponding to decomposition of the layered double hydroxide to the mixed oxide without formation of crystalline lithium aluminate phases.« less

Electrochemical performance of LiV3O8 micro-rod at various calcination temperatures as cathode materials for lithium ion batteries

NASA Astrophysics Data System (ADS)

Noerochim, Lukman; Ginanjar, Edith Setia; Susanti, Diah; Prihandoko, Bambang

2018-04-01

Lithium vanadium oxide (LiV3O8) has been successfully synthesized by hydrothermal method followed by calcination via the reaction of Lithium hydroxide (LiOH) and ammonium metavanade (NH4VO3). The precursors were heated at hydrothermal at 200 °C and then calcined at different calcination temperature in 400, 450, and 500 °C. The characterization by X-ray diffraction (XRD) and scanning electron microscope (SEM) is indicated that LiV3O8 micro-rod have been obtained by this method. The cyclic voltammetry (CV) result showed that redox reaction occur in potential range between 2.42 - 3.57 V for the reduction reaction and oxidation reaction in potential range between 2.01 V-3.69 V. The highest result was obtained for sample 450 °C with specific discharge capacity of 138 mA/g. The result showed that LiV3O8 has a promising candidate as a cathode material for lithium ion batteries.

Well-dispersed NiO nanoparticles supported on nitrogen-doped carbon nanotube for methanol electrocatalytic oxidation in alkaline media

NASA Astrophysics Data System (ADS)

Wang, Pengcheng; Zhou, Yingke; Hu, Min; Chen, Jian

2017-01-01

Nitrogen-doped carbon nanotube supporting NiO nanoparticles were synthesized by a chemical precipitation process coupled with subsequent calcination. The morphology and structure of the composites were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), and the electrochemical performance was evaluated using cyclic voltammetry and chronoamperometric technique. The effects of nitrogen doping, calcination temperature and content of NiO nanoparticles on the electrocatalytic activity toward methanol oxidation were systematically studied. The results show that the uniformly dispersed ultrafine NiO nanoparticles supported on nitrogen-doped carbon nanotube are obtained after calcination at 400 °C. The optimized composite catalysts present high electrocatalytic activity, fast charge-transfer process, excellent accessibility and stability for methanol oxidation reaction, which are promising for application in the alkaline direct methanol fuel cells.

Effect of K3PO4 addition as sintering inhibitor during calcination of Y2O3 nanoparticles

NASA Astrophysics Data System (ADS)

Soga, K.; Okumura, Y.; Tsuji, K.; Venkatachalam, N.

2009-11-01

Erbium-doped yttrium oxide nanoparticle is one of the most important for fluorescence bioimaging under near infrared excitation. Particle size of it below 100 nm is an important requirement for a cellular bioimaging. However, the synthesis with such small particles is difficult at the calcination temperature above 1200 °C due to the sintering and crystal growth of the particles. In this study, yttrium oxide nanoparticles with average size of 30 nm were successfully synthesized by using K3PO4 as a sintering inhibitor during the calcination. A single phase of cubic Y2O3 as the resultant material was confirmed by XRD, which was also confirmed to emit a bright upconversion emission under 980-nm excitation. Improvement of chemical durability due to the introduction of phosphate group on the surface of the Y2O3 particles is also reported.

High field 27Al MAS NMR and TPD studies of active sites in ethanol dehydration using thermally treated transitional aluminas as catalysts

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hu, Jian Zhi; Xu, Suochang; Kwak, Ja Hun

High field quantitative 27Al MAS NMR and temperature programmed desorption (TPD) of ethanol are used to study the surface and phase transformation of gamma-Al2O3 during calcination in the temperature range of 500 to 1300 degrees C. Following ethanol adsorption, ethylene is generated during TPD with a desorption temperature > 200 degrees C. With increasing calcination temperature prior to TPD, the amount of ethylene produced decreases monotonically. Significantly, 27Al MAS NMR reveals that the amount of penta-coordinate Al3+ ions (Lewis acid sites) also decreases with increasing calcination temperature. In fact, a strong correlation between the amount of penta-coordinate Al3+ ions andmore » the amount of strongly adsorbed ethanol molecules (i.e., the ones that convert to ethylene during TPD) is obtained. This result indicates that the penta-coordinate aluminum sites are the catalytic active sites on alumina surfaces during ethanol dehydration reaction across the entire course of gamma- to alpha-Al2O3 phase transformations.« less

Surface hydrophobicity and acidity effect on alumina catalyst in catalytic methanol dehydration reaction

PubMed Central

Osman, Ahmed I; Thompson, Jillian; Halawy, Samih A; Mohamed, Mohamed A

2017-01-01

Abstract BACKGROUND Methanol to dimethyl ether (MTD) is considered one of the main routes for the production of clean bio‐fuel. The effect of copper loading on the catalytic performance of different phases of alumina that formed by calcination at two different temperatures was examined for the dehydration of methanol to dimethyl ether (DME). RESULTS A range of Cu loadings of (1, 2, 4, 6, 10 and 15% Cu wt/wt) on Al2O3 calcined at 350 and 550 °C were prepared and characterized by TGA, XRD, BET, NH3‐TPD, TEM, H2‐TPR, SEM, EDX, XPS and DRIFT‐Pyridine techniques. The prepared catalysts were used in a fixed bed reactor under reaction conditions in which the temperature ranged from 180–300 °C with weight hourly space velocity (WHSV) = 12.1 h‐1. It was observed that all catalysts calcined at 550 °C (γ‐Al2O3 support phase) exhibited higher activity than those calcined at 350 °C (γ‐AlOOH), and this is due to the phase support change. Furthermore, the optimum Cu loading was found to be 6% Cu/γ‐Al2O3 with this catalyst also showing a high degree of stability under steady state conditions and this is attributed to the enhancement in surface acidity and hydrophobicity. CONCLUSION The addition of copper to the support improved the catalyst properties and activity. For all the copper modified catalysts, the optimum catalyst with high degree of activity and stability was 6% copper loaded on gamma alumina. © 2017 The Authors. Journal of Chemical Technology & Biotechnology published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry. PMID:29200585

Structure, morphology and reducibility of ceria-doped zirconia

NASA Astrophysics Data System (ADS)

Aribi, Koubra; Soltani, Zohra; Ghelamallah, Madani; Granger, Pascal

2018-03-01

Zr1-xCexOx has been prepared by hydrolysis, in neutral medium, starting from rough ZrO2 and CeO2 materials as simple and cheaper synthesis method compared to sol-gel routes. The oxy-hydroxide precursors thus obtained were calcined under air at 450 °C, 900 °C and 1200 °C. The impact of those thermal treatments on the structure, texture and related redox properties has been investigated. Higher specific surface area than those observed on ceria were observed after calcination at low temperature, i.e., 450 °C. Above that temperature thermal sintering occurs having a detrimental effect on the specific surface area related to crystal growth more accentuated on CeO2. The formation of several Zrsbnd Ce mixed oxide phases formed by incorporation and substitution of Zr in the structure of ceria was characterized. A complete loss of specific surface area is noticeable after calcination at 1200 °C. XRD and SEM analysis revealed the formation of two mixed oxides structure, i.e. Ce2Zr2O7.04 and Ce2Zr2O7 corresponding to different redox behavior evidenced from H2-TPR experiments.

Microwave sintering of sol-gel derived abrasive grain

DOEpatents

Plovnick, Ross; Celikkaya, Ahmet; Blake, Rodger D.

1997-01-01

A method is provided for making microwave-sintered, free flowing alpha alumina-based ceramic abrasive grain, under conditions effective to couple microwaves with calcined alpha alumina-based abrasive gain precursor and sinter it at a temperature of at least about 1150.degree. C.

Magnetic and dielectric properties of Ca-substituted BiFeO3 nanoferrites by the sol-gel method.

PubMed

Lin, Jinpei; Guo, Zeping; Li, Mei; Lin, Qing; Huang, Kangling; He, Yun

2018-01-01

A multiferroic material can simultaneously show two or more basic magnetic properties, including ferromagnetism, antiferromagnetism, and ferroelectricity. BiFeO 3 is a multiferroic material with a rhombohedral distorted perovskite structure. Doping can reduce the volatility of Bi and greatly improve the magnetoelectric properties of BiFeO 3 . To investigate the influence of the doping content we used the following analytical methods: X-ray powder diffraction (XRD), scanning electron microscopy (SEM), microwave network analysis (PNA-N5244A), and the Superconducting Quantum Interference Device (Quantum Design MPMS) test. With the increase of Ca 2+ concentration in the solution, the grain size of Bi 1- x Ca x FeO 3 becomes smaller, showing the role of Ca 2+ ions as the dopant for fine grains. The calcination temperatures are the major causes for the saturated magnetization. The residual magnetization ( M r ) and the coercive force ( H c ) decrease linearly with the increase of x value, and due to the effect of Ca 2+ substitution at Bi 3+ sites, which causes the valence change of Fe and/or the oxygen vacancies. The XRD result indicates that the diffraction peak emerges with the increase of Ca 2+ and the main diffraction peak achieves a high angle. The best calcining temperature is 600 °C, and the morphology is very dependent on the calcining temperature.

Highly Visible Light Activity of Nitrogen Doped TiO2 Prepared by Sol-Gel Approach

NASA Astrophysics Data System (ADS)

Than, Le Dien; Luong, Ngo Sy; Ngo, Vu Dinh; Tien, Nguyen Manh; Dung, Ta Ngoc; Nghia, Nguyen Manh; Loc, Nguyen Thai; Thu, Vu Thi; Lam, Tran Dai

2017-01-01

A simple approach was explored to prepare N-doped anatase TiO2 nanoparticles (N-TiO2 NPs) from titanium chloride (TiCl4) and ammonia (NH3) via sol-gel method. The effects of important process parameters such as calcination temperatures, NH3/TiCl4 molar ratio ( R N) on crystallite size, structure, phase transformation, and photocatalytic activity of titanium dioxide (TiO2) were thoroughly investigated. The as-prepared samples were characterized by ultraviolet-visible spectroscopy, x-ray diffraction, transmission electron microscopy, energy dispersive x-ray spectroscopy, and x-ray photoelectron spectroscopy. The photocatalytic activity of the samples was evaluated upon the degradation of methylene blue aqueous solution under visible-light irradiation. The results demonstrated that both calcination temperatures and NH3/TiCl4 molar ratios had significant impacts on the formation of crystallite nanostructures, physicochemical, as well as catalytic properties of the obtained TiO2. Under the studied conditions, calcination temperature of 600°C and NH3/TiCl4 molar ratio of 4.2 produced N-TiO2 with the best crystallinity and photocatalytic activity. The high visible light activity of the N-TiO2 nanomaterials was ascribed to the interstitial nitrogen atoms within TiO2 lattice units. These findings could provide a practical pathway capable of large-scale production of a visible light-active N-TiO2 photocatalyst.

Super high energy density of Li3V2(PO4)3 as cathode materials for lithium ion batteries

NASA Astrophysics Data System (ADS)

Noerochim, Lukman; Amin, Mochammad Karim Al; Susanti, Diah; Triwibowo, Joko

2018-04-01

Lithium ion batteries have many advantages such as high energy density, no memory effect, long time cycleability and friendly environment. One type of cathode material that can be developed is Li3V2(PO4)3. In this study has been carried out the synthesis of Li3V2(PO4)3 with a hydrothermal temperature variation of 140, 160 and 180 °C and calcination temperature at 800 °C. SEM images show that the morphology of Li3V2(PO4)3 has irregular flakes with a size between 1-10 µm. CV results show redox reaction occurs in the range between 3 V to 4.8 V with the highest specific discharge capacity of 136 mAh/g for specimen with temperature hydrothermal and calcination are 180 °C and 800 °C. This result demonstrates that Li3V2(PO4)3 has a great potential as cathode material for lithium ion battery.

Preparation of TiO₂ nanocrystallite powders coated with 9 mol% ZnO for cosmetic applications in sunscreens.

PubMed

Ko, Horng-Huey; Chen, Hui-Ting; Yen, Feng-Ling; Lu, Wan-Chen; Kuo, Chih-Wei; Wang, Moo-Chin

2012-01-01

The preparation of TiO(2) nanocrystallite powders coated with and without 9 mol% ZnO has been studied for cosmetic applications in sunscreens by a co-precipitation process using TiCl(4) and Zn(NO(3))(2)·6H(2)O as starting materials. XRD results show that the phases of anatase TiO(2) and rutile TiO(2) coexist for precursor powders without added ZnO (T-0Z) and calcined at 523 to 973 K for 2 h. When the T-0Z precursor powders are calcined at 1273 K for 2 h, only the rutile TiO(2) appears. In addition, when the TiO(2) precursor powders contain 9 mol% ZnO (T-9Z) are calcined at 873 to 973 K for 2 h, the crystallized samples are composed of the major phase of rutile TiO(2) and the minor phases of anatase TiO(2) and Zn(2)Ti(3)O(8). The analyses of UV/VIS/NIR spectra reveal that the absorption of the T-9Z precursor powders after being calcined has a red-shift effect in the UV range with increasing calcination temperature. Therefore, the TiO(2) nanocrystallite powders coated with 9 mol% ZnO can be used as the attenuate agent in the UV-A region for cosmetic applications in sunscreens.

Preparation of TiO2 Nanocrystallite Powders Coated with 9 mol% ZnO for Cosmetic Applications in Sunscreens

PubMed Central

Ko, Horng-Huey; Chen, Hui-Ting; Yen, Feng-Ling; Lu, Wan-Chen; Kuo, Chih-Wei; Wang, Moo-Chin

2012-01-01

The preparation of TiO2 nanocrystallite powders coated with and without 9 mol% ZnO has been studied for cosmetic applications in sunscreens by a co-precipitation process using TiCl4 and Zn(NO3)2·6H2O as starting materials. XRD results show that the phases of anatase TiO2 and rutile TiO2 coexist for precursor powders without added ZnO (T-0Z) and calcined at 523 to 973 K for 2 h. When the T-0Z precursor powders are calcined at 1273 K for 2 h, only the rutile TiO2 appears. In addition, when the TiO2 precursor powders contain 9 mol% ZnO (T-9Z) are calcined at 873 to 973 K for 2 h, the crystallized samples are composed of the major phase of rutile TiO2 and the minor phases of anatase TiO2 and Zn2Ti3O8. The analyses of UV/VIS/NIR spectra reveal that the absorption of the T-9Z precursor powders after being calcined has a red-shift effect in the UV range with increasing calcination temperature. Therefore, the TiO2 nanocrystallite powders coated with 9 mol% ZnO can be used as the attenuate agent in the UV-A region for cosmetic applications in sunscreens. PMID:22408415

Process for preparing fine grain silicon carbide powder

DOEpatents

Wei, G.C.

Finely divided silicon carbide powder is obtained by mixing colloidal silica and unreacted phenolic resin in either acetone or methanol, evaporating solvent from the obtained solution to form a gel, drying and calcining the gel to polymerize the phenolic resin therein, pyrolyzing the dried and calcined gel at a temperature in the range of 500 to 1000/sup 0/C, and reacting silicon and carbon in the pyrolyzed gel at a temperature in the range of 1550 to 1700/sup 0/C to form the powder.

AlNbO oxides as new supports for hydrocarbon oxidation II. Catalytic properties of VO sub x -grafted AlNbO oxides

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oliveira, P.G. Pries de; Eon, J.G.; Volta, J.C.

1992-09-01

Vanadium oxides were immobilized by grafting VOCl{sub 3} on AlNbO oxides calcined between 500 and 750 C. Chemical analysis, XPS, and STEM measurements suggest an incomplete but homogeneous stoichiometric reaction between superficial hydroxyl groups and vanadyl oxychloride. By FTIR studies, it is observed that the interaction involves preferentially basic hydroxyl groups bonded to aluminium cations. UV-visible spectra show that mainly V{sup 5+} is present at the solid surface. Corresponding spectra are compatible with tetrahedral symmetry, in agreement with a previous {sup 51}V NMR investigation. The acido-basic properties of the catalyst were tested by isopropanol decomposition and compared with the correspondingmore » supports. It has been observed that basicity is higher for VO{sub x} grafted on AlBnO oxide calcined at high temperature and corresponding to the AlNbO{sub 4} structure. VO{sub x} grafted on AlNbO oxides calcined at intermediate temperatures and corresponding to a AlNbO disorganized structure present a good selectivity for the oxidative dehydrogenation of propane into propene. It has been observed that, for both reactions, the turnover number increases with the temperature of calcination of the catalysts. The reactivity of the aluminium niobiate support.« less

Synthesis and physical characterization of γ-Fe2O3 and (α+γ)-Fe2O3 nanoparticles

NASA Astrophysics Data System (ADS)

Bhavani, P.; Reddy, N. Ramamanohar; Reddy, I. Venkata Subba

2017-01-01

Magnetic nanoparticles were synthesized at different hydrothermal temperatures (HT; 100, 130, 160 and 190 °C) by using a facile hydrothermal route combined with a subsequent calcination process. The calcined materials were analyzed for phase, microstructure, and magnetic and dielectric properties through different characterization techniques. The structural analyses revealed that the material prepared at a HT of 100 °C and sequentially calcined at 300 °C for 3 h showed a high degree of the maghemite structure. On the other hand calcined materials showed a small additional peak belonging to the hematite structure. FESEM micrographs of the materials calcined at HT, of 100 °C and 190 °C showed spherical-like nanoparticles with diameters in range 30 - 54 nm. Materials prepared at a HT of 160 °C followed by calcination at 300 °C for 3 h exhibited the highest saturation magnetization, Ms = 67 emu/g, with a lower coercivity; all materials were in a single domain state. A high dielectric constant (105.54) was observed for the calcined material that had been prepared at a HT of 130 °C. The dielectric properties of synthesized materials showed an almost frequency-independent behavior.

Enhancement of structural and magnetic properties of M-type hexaferrite permanent magnet based on synthesis temperature

NASA Astrophysics Data System (ADS)

Anjum, Safia; Sehar, Fatima; Mustafa, Zeeshan; Awan, M. S.

2018-01-01

The main purpose of this research work is to develop the single domain magnetic particles of M-type barium hexaferrite (BaFe12O19) using oxide precursors employing conventional powder metallurgy technique. The phase formation and magnetic performance of the powders and magnets will be optimized by adjusting calcination and sintering temperatures. The synthesis of M-type barium hexaferrite was carried out in two sections. A series of four samples have been prepared by initial wet mixed powders calcined at different temperatures, i.e., 750, 850, 950 and 1050 °C. On the basis of structural analysis, the sample calcined at 950 °C has been selected and further divided into four parts to sintered them at 1100, 1150, 1200 and 1250 °C. The structural measurements depict the confirmation of M-type barium hexaferrite structure. SEM micrographs show the hexagonal-shaped grains. The abrupt decrease in coercivity for the sample sintered at 1250 °C has been seen which may be due to high sintering temperature, at which the particles have multi-domain properties.

Synthesis of octahedral like Cu-BTC derivatives derived from MOF calcined under different atmosphere for application in CO oxidation

NASA Astrophysics Data System (ADS)

Yang, Yiqiong; Dong, Han; Wang, Yin; He, Chi; Wang, Yuxin; Zhang, Xiaodong

2018-02-01

A series of octahedral structure Cu-BTC derivatives were successfully achieved through direct calcination of copper based metal organic framework Cu-BTC under different atmosphere (CO reaction gas, oxidizing gas O2, reducing gas H2, inert gas Ar). The Cu-BTC derivatives were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), laser Raman spectroscopy (LRS), N2 adsorption-desorption isotherm, element analysis, H2-temperature program reduction (H2-TPR) and X-ray photoelectron spectroscopic (XPS). It is found that Cu-BTC derivative derived from MOF calcined under reaction gas/O2 (Cu-BTC-CO/Cu-BTC-O) only retain Cu2O and CuO species. In addition, a weak Cu-BTC structure and Cu particles were observed on Cu-BTC derivative derived from MOF calcined under H2 (Cu-BTC-H). Obviously differently, Cu-BTC derivative derived from MOF calcined under Ar (Cu-BTC-Ar) still retains good MOF structure. The catalytic performance for CO oxidation over Cu-BTC derivatives was studied. It was found that Cu-BTC-CO showed a smaller specific surface area (8.0 m2/g), but presented an excellent catalytic performance, long-term stability and cycling stability with a complete CO conversion temperature (T100) of 140 °C, which was ascribed to the higher Cu2O/CuO ratio, good low temperature reduction behavior and a high quantity of surface active oxygen species.

Optimum Conditions for Preparation of High-Performance (Ba0.97Ca0.03)(Ti0.94Sn0.06)O3 Ceramics by Solid-State Combustion

NASA Astrophysics Data System (ADS)

Chootin, Suphornphun; Bongkarn, Theerachai

2017-08-01

The effects of calcination conditions (950°C to 1200°C for 2 h to 6 h) and sintering temperature (1300°C to 1500°C for 2 h) on phase formation, microstructure, and electrical behavior of lead-free piezoelectric (Ba0.97Ca0.03)(Ti0.94Sn0.06)O3 (BCTS) ceramics produced by solid-state combustion using glycine as fuel have been investigated. BCTS powder with pure perovskite structure was obtained by calcination at 1100°C for 4 h. The microstructure of the BCTS powders showed almost spherical shape with average particle size increasing from 184 nm to 320 nm as the calcination temperature and soaking time were increased. The XRD patterns of all ceramics exhibited single perovskite structure. Rietveld refinement analysis indicated that the BCTS ceramics exhibited coexistence of orthorhombic and tetragonal phase in all samples with increased tetragonal phase content with increasing sintering temperature. The average grain size, density, dielectric constants at room ( ɛ r) and Curie temperature ( ɛ C), remanent polarization ( P r), and piezoelectric constant ( d 33) increased as the sintering temperature was increased up to 1400°C, then decreased. BCTS ceramic sintered at 1400°C exhibited the highest relative density (98%), highest dielectric response ( ɛ r = 4951, ɛ C = 19,185), good ferroelectric behavior ( P r = 12.74 μC/cm2 and coercive field E c = 1.60 kV/cm), and highest d 33 value (528 pC/N). The large piezoelectricity of BCTS ceramics makes them good candidates for use in lead-free applications to replace Pb-based ceramics.

[Up-conversion luminescent materials of Y2O3: RE(RE=Er or Er/Yb) prepared by sol-gel combustion synthesis].

PubMed

Han, Peng-de; Zhang, Le; Huang, Xiao-gu; Wang, Li-xi; Zhang, Qi-tu

2010-11-01

Y2O3 powders doped with rare-earth ions were synthesized by sol-gel combustion synthesis. Effects of different calcinating temperatures, Er+ doping concentration and Yb3+ doping concentration were investigated. It was shown that the single well crystallized Y2O3 powders could be obtained at 800 degrees C; as the calcinating temperature increased, the crystallinity and upconversion luminescence intensity were higher; the particle size was uniform around 1 microm at 900 degrees C; when Er3+ doping concentration was 1 mol%, the green upconversion luminescence intensity reached the maximum, but for red upconversion luminescence, when Er3+ doping concentration was 4 mol%, its luminescence intensity reached the maximum; as the ratio of Yb3+ to Er3+ was 4:1, the green emission intensity reached the maximum, while the red emission intensity was always increasing as Yb3+ doping concentration increased.

Synthesis and characterization of LiFePO4/C cathode materials by sol-gel method.

PubMed

Liu, Shuxin; Yin, Hengbo; Wang, Haibin; Wang, Hong

2014-09-01

The carbon coated LiFePO4 cathode materials (LiFePO4/C) were successfully synthesized by sol-gel method with glucose, citric acid and PEG-4000 as dispersant and carbon source, respectively. The microstructure and grain size of LiFePO4/C composite were characterized by X-ray diffraction, Raman spectroscopy, transmission electron microscopy. The results showed that the carbon source and calcination temperature had important effect on the graphitization degree of carbon; the carbon decomposed by citric acid had higher graphitization degree; with calcination temperature rising, the graphitization degree of carbon increased and the particles size increased. The graphitization degree and grain size were very important for improving the electrochemical performance of LiFePO4 cathode materials, according to the experimental results, the sample LFP-700 (LFP-C) which was synthesized with citric acid as dispersant at 700 degree C had lower polarization and larger discharge capacity.

Study of phase transformation and microstructure of alcohol washed titania nanoparticles for thermal stability

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kaur, Manpreet, E-mail: manpreet.kaur@thapar.edu; Singh, Gaganjot; Bimbraw, Keshav

Nanostructured titania have been successfully synthesized by hydrolysis of alkoxide at calcination temperatures 500 °C, 600 °C and 700 °C. As the calcination temperature increases, alcohol washed samples show lesser rutile content as compared to water washed samples. Morphology and Particle sizes was determined by field emission scanning electron microscopy (FESEM), while thermogravimetric-differential scanning calorimetry (TG-DSC) was used to determine thermal stability. Alcohol washed samples undergo 30% weight loss whereas 16% in water washed samples was observed. The mean particle sizes were found to be increase from 37 nm to 100.9 nm and 35.3 nm to 55.2 nm for water and alcohol washed samplesmore » respectively. Hydrolysis of alkoxide was shown to be an effective means to prepare thermally stable titania by using alcohol washed samples as a precursor.« less

Natural manganese ore catalyst for low-temperature selective catalytic reduction of NO with NH3 in coke-oven flue gas.

PubMed

Zhu, Baozhong; Yin, Shoulai; Sun, Yunlan; Zhu, Zicheng; Li, Jiaxin

2017-11-01

Different types of manganese ore raw materials were prepared for use as catalysts, and the effects of different manganese ore raw materials and calcination temperature on the NO conversion were analyzed. The catalysts were characterized by XRF, XRD, BET, XPS, H 2 -TPR, NH 3 -TPD, and SEM techniques. The results showed that the NO conversion of calcined manganese ore with a Mn:Fe:Al:Si ratio of 1.51:1.26:0.34:1 at 450 °C reached 80% at 120 °C and 98% at 180~240 °C. The suitable proportions and better dispersibility of active ingredients, larger BET surface area, good reductibility, a lot of acid sites, contents of Mn 4+ and Fe 3+ , and surface-adsorbed oxygen played important roles in improving the NO conversion.

Biodiesel production from palm oil using calcined waste animal bone as catalyst.

PubMed

Obadiah, Asir; Swaroopa, Gnanadurai Ajji; Kumar, Samuel Vasanth; Jeganathan, Kenthorai Raman; Ramasubbu, Alagunambi

2012-07-01

Waste animal bones was employed as a cost effective catalyst for the transesterification of palm oil. The catalyst was calcined at different temperatures to transform the calcium phosphate in the bones to hydroxyapatite and 800 °C was found to give the best yield of biodiesel. The catalyst was characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive spectrometry (EDS) and Fourier transform infrared spectrometry (FT-IR). Under the optimal reaction conditions of 20 wt.% of catalyst, 1:18 oil to methanol molar ratio, 200 rpm of stirring of reactants and at a temperature of 65 °C, the methyl ester conversion was 96.78% and it was achieved in 4h. The catalyst performed equally well as the laboratory-grade CaO. Animal bone is therefore a useful raw material for the production of a cheap catalyst for transesterification. Copyright © 2012 Elsevier Ltd. All rights reserved.

Investigation of phase evolution of CaCu3Ti4O12 (CCTO) by in situ synchrotron high-temperature powder diffraction

NASA Astrophysics Data System (ADS)

Ouyang, Xin; Huang, Saifang; Zhang, Weijun; Cao, Peng; Huang, Zhaohui; Gao, Wei

2014-03-01

In situ synchrotron X-ray powder diffraction was used to study the high-temperature phase evolution of CaCu3Ti4O12 (CCTO) precursors prepared via solid-state and sol-gel methods. After the precursors are heated to 1225 °C, the CCTO phase is the main phase observed in the calcined powder, with the presence of some minor impurities. Comparing the two precursors, we found that the onset temperature for the CCTO phase formation is 800 °C in the sol-gel precursor, lower than that in the solid-state precursor (875 °C). Intermediate phases were only observed in the sol-gel precursor. Both precursors are able to be calcined to sub-micrometric sized powders. Based on the synchrotron data along with differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the phase formation sequence and mechanism during calcination are proposed in this study.

Evaluation of calcination temperature and phase composition ratio for new hyroxyapatite

NASA Astrophysics Data System (ADS)

Salimi, M. N. Ahmad; Chin, H. S.

2017-10-01

The demand of production of hydroxyapatite (HA) has been increasing for the purpose of medical and dental application. HA possesses the excellent properties leads to the priority choice for ceramic bone replacement. Synthesis route by wet chemical precipitation is commonly practised in industrial scale. Calcium hydroxide and Orthophosphoric acid are the precursors for production scale. The synthesis of HA is conducted by varying the synthetic condition: stirring rate, calcium-phosphate and calcination temperature. This paper is focused on the properties of HA produced by regulating the synthetic condition so that the qualities of HA can be well performed. Characterization studies were also carried out by Fourier Transform Infrared Spectroscopy (FT-IR) for functional group identification, Scanning Electron Microscope (SEM) for surface morphology analysis and X-Ray Diffraction (XRD) for phase composition and crystallinity respectively. Narrow particle size distribution contributed to better quality of hydroxyapatite for bone replacement. Both calcium-phosphate ratio and calcination temperature would affect the phase composition of calcium phosphate.

Magnetic properties of co-precipitated hexaferrite powders with Sm-Co substitutions optimized with the molten flux method

NASA Astrophysics Data System (ADS)

Serletis, C.; Litsardakis, G.; Pavlidou, E.; Efthimiadis, K. G.

2017-11-01

In this work, using the chemical coprecipitation method, Sr1-xSmxFe12-xCoxO19 (x = 0, 0.1, 0.2) hexaferrite powders were prepared. Major magnetization loops were recorded at room temperature in order to determine the correct calcination temperature for optimum hard magnetic properties. It is found that a small degree of substitution increases substantially the coercive field. Also, the use of the molten flux calcination method increases the remanent magnetization. SEM/EDXS and XRD measurements were performed at the calcined powders: the results show that a single hexaferrite phase is formed and that the substituted powders consist of an assembly of grains with a mean diameter of 40 nm. Measurements of minor magnetization loops and of the temperature and time dependence of the magnetization confirm that the powders consist of a non-oriented single domain magnetic particles assembly. The results indicate that Sm could be a viable replacement for La in the manufacturing of hexaferrites with a high-energy product.

Phase study of SiO2-ZrO2 composites prepared from polymorphic combination of starting powders via a ball-milling followed by calcination

NASA Astrophysics Data System (ADS)

Musyarofah; Nurlaila, R.; Muwwaqor, N. F.; Saukani, M.; Kuswoyo, A.; Triwikantoro; Pratapa, S.

2017-04-01

The effects of SiO2-ZrO2 polymorphic combinations as starting powders and calcination temperature on phase composition of the SiO2-ZrO2 composites were studied. Stoichiometric (1:1 mol%) mixtures of the SiO2-ZrO2 composites were mechanically activated using a ball-milling for 5 h followed by calcinations at 1000, 1100 and 1200 °C for 3 h. The composites used in the present study were a-SiO2+ a-ZrO2, a-SiO2+ t-ZrO2, c-SiO2+ a-ZrO2 and c-SiO2+ t-ZrO2 which were symbolized by AA, AT, CA and CT, respectively. Prefixes a, t and c denote amorphous, tetragonal and cristobalite, respectively. The phase composition was determined by Rietveld analysis of X-ray diffraction (XRD) data using Rietica software. The identified phases for all calcined samples were a combination among t-ZrO2, c-SiO2, m-ZrO2 and zircon (ZrSiO4). Amorphous zirconia formed a transient tetragonal zirconia phase during heating, which reacted with silica to form zircon. The zircon phase was not found to form even at 1200 °C in the AT and CT mixtures and at 1100 °C in the CA mixture. The AA mixture in particular crystallized to form zircon at a lower temperature with more composition fraction than the others, ca 82.9 (14) mol%.

Nuclear proliferomics: A new field of study to identify signatures of nuclear materials as demonstrated on alpha-UO3.

PubMed

Schwerdt, Ian J; Brenkmann, Alexandria; Martinson, Sean; Albrecht, Brent D; Heffernan, Sean; Klosterman, Michael R; Kirkham, Trenton; Tasdizen, Tolga; McDonald Iv, Luther W

2018-08-15

The use of a limited set of signatures in nuclear forensics and nuclear safeguards may reduce the discriminating power for identifying unknown nuclear materials, or for verifying processing at existing facilities. Nuclear proliferomics is a proposed new field of study that advocates for the acquisition of large databases of nuclear material properties from a variety of analytical techniques. As demonstrated on a common uranium trioxide polymorph, α-UO 3 , in this paper, nuclear proliferomics increases the ability to improve confidence in identifying the processing history of nuclear materials. Specifically, α-UO 3 was investigated from the calcination of unwashed uranyl peroxide at 350, 400, 450, 500, and 550 °C in air. Scanning electron microscopy (SEM) images were acquired of the surface morphology, and distinct qualitative differences are presented between unwashed and washed uranyl peroxide, as well as the calcination products from the unwashed uranyl peroxide at the investigated temperatures. Differential scanning calorimetry (DSC), UV-Vis spectrophotometry, powder X-ray diffraction (p-XRD), and thermogravimetric analysis-mass spectrometry (TGA-MS) were used to understand the source of these morphological differences as a function of calcination temperature. Additionally, the SEM images were manually segmented using Morphological Analysis for MAterials (MAMA) software to identify quantifiable differences in morphology for three different surface features present on the unwashed uranyl peroxide calcination products. No single quantifiable signature was sufficient to discern all calcination temperatures with a high degree of confidence; therefore, advanced statistical analysis was performed to allow the combination of a number of quantitative signatures, with their associated uncertainties, to allow for complete discernment by calcination history. Furthermore, machine learning was applied to the acquired SEM images to demonstrate automated discernment with at least 89% accuracy. Copyright © 2018 Elsevier B.V. All rights reserved.

Investigation of phase evolution of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) by in situ synchrotron high-temperature powder diffraction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ouyang, Xin; Huang, Saifang; School of Materials Science and Technology, China University of Geosciences

2014-03-15

In situ synchrotron X-ray powder diffraction was used to study the high-temperature phase evolution of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) precursors prepared via solid-state and sol–gel methods. After the precursors are heated to 1225 °C, the CCTO phase is the main phase observed in the calcined powder, with the presence of some minor impurities. Comparing the two precursors, we found that the onset temperature for the CCTO phase formation is 800 °C in the sol–gel precursor, lower than that in the solid-state precursor (875 °C). Intermediate phases were only observed in the sol–gel precursor. Both precursors are able to bemore » calcined to sub-micrometric sized powders. Based on the synchrotron data along with differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the phase formation sequence and mechanism during calcination are proposed in this study. -- Graphical abstract: The in situ synchrotron HT-XRD patterns of CCTO sol–gel and solid-state precursor. Highlights: • Phase formation sequence/mechanism in two CCTO precursors has been established. • Formation temperature of CCTO via sol–gel method is lower than solid-state method. • Intermediate phases are only observed in the sol–gel precursor. • Both precursors are able to be calcined into sub-micrometric sized powders.« less

Fabrication of solar light induced Fe-TiO{sub 2} immobilized on glass-fiber and application for phenol photocatalytic degradation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lin, Shaohua, E-mail: linsh75@163.com; Zhang, Xiwang; Sun, Qinju

2013-11-15

Graphical abstract: - Highlights: • Fe-doped TiO{sub 2} immobilized on glass-fiber net were prepared by sol–gel method. • Fe inhibited the phase transition of TiO{sub 2} from anatase to rutile. • The optimal Fe doping dose was around 0.005 wt%. • The optimal calcination temperature was around 600 °C. - Abstract: Iron-doped anatase titanium dioxide catalysts coated on glass-fiber were successfully synthesized by a dip-coating sol–gel method. The prepared catalysts were characterized by scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis, X-ray diffraction (XRD), UV-Vis diffuse reflectance spectroscopy to understand the synthesis mechanism, and their photocatalytic activities weremore » evaluated by photodegradation of phenol under simulated solar irradiation. EDX analysis confirmed the existence of iron in the immobilized catalysts. XRD suggested that the phase transition of the catalysts from anatase to rutile were restrained, and almost pure anatase TiO{sub 2} could retain even the calcination temperature reached 800 °C. The UV-Vis diffuse reflectance spectroscopy of the catalysts showed a red shift and increased photoabsorbance in the visible range for all the doped samples. Iron loading and calcination temperature have obvious influences on photocatalytic activity. In this study, the optimal doping dose and calcination temperature were around 0.005 wt% and 600 °C, respectively.« less

Preparation of Co-Zn ferrite nano-based materials and their enhanced magnetic performance via inverse miniemulsion method

NASA Astrophysics Data System (ADS)

Ji, Juejin; Zhang, Zhenqian; Fang, Bijun; Ding, Jianning

2017-11-01

The well dispersed CZF/PAM nanoparticles were prepared by the inverse miniemulsion method, which present high calcining and sintering activity for preparing Co0.875Zn0.125Fe2O4 (CZF) films, powders and ceramics at rather low temperatures. The prepared CZF/PAM inverse miniemulsion exhibits excellent film-formation performance, which is feasible for coating CZF films. XRD and FT-IR measurements confirmed that phase pure spinel structure and well crystalline CZF powders can be prepared calcined at the least temperature of 400 °C. The 450 °C-calcined CZF powders exhibit nearly spherical shape grains with average particle size 20-30 nm accompanied by apparent conglomeration. Improved external magnetic performance and electrical properties are obtained in the synthesized CZF powders and ceramics, which provide versatile promising applications.

Synthesis of porous nanocrystalline NiO with hexagonal sheet-like morphology by homogeneous precipitation method

NASA Astrophysics Data System (ADS)

Sharma, Ravi Kant; Ghose, Ranjana

2015-04-01

Porous nanocrystalline NiO has been synthesized by a simple homogeneous precipitation method in short time at low calcination temperature without using any surfactant, chelating or gelating agents. The porous nanocrystalline NiO with a hexagonal sheet-like morphology were obtained by calcination of Ni(OH)2 nanoflakes at 500 °C. The calcination temperature strongly influences the morphology, crystallite size, specific surface area, pore volume and optical band gap of the samples. The samples were characterized using powder X-ray diffraction, thermal gravimetric analysis, FT-IR spectroscopy, UV-Visible diffuse reflectance spectroscopy, surface area measurements, field emission scanning electron microscopy coupled with energy dispersive X-ray analysis and transmission electron microscopy. The chemical activity of the samples was tested by catalytic reduction of 4-nitrophenol with NaBH4.

To study the effect of calcinations durations and temperature on optical and structural properties of MgO-CuO nanocomposites

NASA Astrophysics Data System (ADS)

Kumar, Rajesh; Praveen, Sharma, Ashwani; Parmar, R.; Dahiya, S.; Kishor, N.

2016-05-01

The MgO-CuO nanocomposites has been synthesized by a sol-gel techniques based on precursor polyvinyl alcohol (PVA). In this work appropriate concentration of cupric nitrate, Magnisium nitrate and PVA are mixed with 50:50 ethanol water followed by heated to 80°C to form a homogeneous gel solution. The obtained gel was slowly heated at 100°C to evaporate the solvent to form a hard homogeneous gel. The hard gel was calcinated at temperature 600°C for 4 hrs and 6 hrs thereafter, crushed the material in agate-motar so that it is converted into fine powder form. The prepared nanocomposites have been characterized using X-Ray Diffraction (XRD), FTIR, UV-VIS spectroscopy, SEM etc. The size of MgO-CuO nanocomposites heated at 600°C for 4 hours and 6 hours evaluated by Debye Scherrer formula are 17.1 nm and 21.2 nm respectively and results show that Size of MgO-CuO nanocomposites increases with increase of calcinations durations. IR spectra is also used to determine purity of samples. Absorption spectra confirm the synthesis of nanomaterials. SEM images give the indication of morphology of the nanocomposites.

Magnetic Carbon Microspheres as a Reusable Adsorbent for Sulfonamide Removal from Water

NASA Astrophysics Data System (ADS)

Dai, Kewei; Wang, Fenghe; Jiang, Wei; Chen, Yajun; Mao, Jing; Bao, Jian

2017-09-01

Novel reusable magnetic carbon microspheres (MCMs) were prepared by hydrothermal method with glucose as carbon source and Fe3O4 nanoparticles as magnetic raw materials. And adsorption performance of MCMs for sulfonamide removal from water was investigated in detail. The results indicated that the calcination temperature and calcination time had significant effects on the surface area and its volume porous of MCMs. When MCMs were calcined in 600 °C for 1 h, the surface area and volume porous of MCMs were 1228 m2/g and 0.448 m3/g, respectively. The adsorption results showed that the adsorption data fitted well with the Langmuir isotherm model and followed pseudo-second-order kinetics. When the pH value was changed from 4.0 to 10.0, the adsorption capacity of MCMs for sulfonamide was decreased from 24.6 to 19.2 mg/g. The adsorption capacity of as-synthesized MCMs achieved 18.31 mg/g after it was reused four times, which exhibited a desirable adsorption capacity and reusability.

Comparison of the up-conversion photoluminescence for GAP, GAG and GAM phosphors

NASA Astrophysics Data System (ADS)

Deng, Taoli; Jiang, Xianbang

2018-04-01

GdAlO3:Er3+/Yb3+, Gd3Al5O12:Er3+/Yb3+ and Gd4Al2O9:Er3+/Yb3+ phosphors were prepared by co-precipitation. The effects for Gd2O3-Al2O3 composite oxides as the host materials with different crystal structures such as GdAlO3, Gd3Al5O12 and Gd4Al2O9 were investigated. It was found that the perovskite structured GdAlO3:Er3+/Yb3+ (GAP phosphor) could be obtained from the precursor when the calcination temperature was 1000 °C, while the garnet structured Gd3Al5O12:Er3+/Yb3+ (GAG phosphor) could be formed when the calcination temperature was 1300 °C, but the monoclinic-structured Gd4Al2O9:Er3+/Yb3+ (GAM phosphor) could be formed only when the calcination temperature was raised up to 1500 °C. The difference of the up-conversion photoluminescence (UCPL) spectra under 980 nm between the GAP, GAG and GAM phosphors was studied. The result showed that the UCPL intensity of the GAP phosphor was close to that of the GAM phosphor with much higher red-to-green intensity ratio than that of GAP phosphor. The UCPL intensity of GAG phosphor was the weakest among them. Finally, the factors which influenced on the UCPL of the GAP, GAG and GAM phosphors were discussed.

Iron active electrode and method of making same

DOEpatents

Jackovitz, John F.; Seidel, Joseph; Pantier, Earl A.

1982-10-26

An iron active electrode and method of preparing same in which iron sulfate is calcined in an oxidizing atmosphere at a temperature in the range of from about 600.degree. C. to about 850.degree. C. for a time sufficient to produce an iron oxide with a trace amount of sulfate. The calcined material is loaded into an electrically conductive support and then heated in a reducing atmosphere at an elevated temperature to produce activated iron having a trace amount of sulfide which is formed into an electrode plate.

Hydrophobicity of silica thin films: The deconvolution and interpretation by Fourier-transform infrared spectroscopy

NASA Astrophysics Data System (ADS)

Saputra, Riza Eka; Astuti, Yayuk; Darmawan, Adi

2018-06-01

This work investigated the synthesis of dimethoxydimethylsilane:tetraethoxysilane (DMDMS:TEOS) silica thin films as well as the effect of DMDMS:TEOS molar ratios and calcination temperature on hydrophobic properties of silica thin films and its correlation with the FTIR spectra behaviour. The silica thin films were synthesized by sol-gel method using combination of DMDMS and TEOS as silica precursors, ethanol as solvent and ammonia as catalyst, with DMDMS and TEOS molar ratio of 10:90, 25:75, 50:50, 75:25 and 90:10. The results showed that DMDMS:TEOS molar ratio had significant impact on the hydrophobic properties of silica thin films coated on a glass surface. Furthermore, the correlation between water contact angle (WCA) and DMDMS:TEOS molar ratio was found to be in a parabolic shape. Concurrently, the maximum apex of the parabola obtained was observed on the DMDMS:TEOS molar ratio of 50:50 for all calcination temperature. It was clearly observed that the silica xerogel exhibiting notable change in relative peak intensities showed FTIR peak splitting of υasymmetric Si-O-Si. To uncover what happened at the FTIR peak, the deconvolution was conducted in Gaussian approach. It was established that the changes in the Gaussian peak component were related to DMDMS:TEOS molar ratios and the calcination temperature that allowed us to tailor the DMDMS:TEOS silica polymer structure model based on the peak intensity ratios. With the increase of DMDMS:TEOS molar ratio, the ratio of (cyclic Si-O-Si)/(linear Si-O-Si) decreased, whilst the ratio of (C-H)/(linear Si-O-Si) increased. Both ratios intersected at DMDMS:TEOS molar ratio of 50:50 with contribution factor ratio of 1:16 and 1:50 for silica xerogel calcined at 300 °C and 500 °C respectively. The importance of this research is the DMDMS:TEOS molar ratio plays an important role in determining the hydrophobic properties of thin films.

Preparation of Heat Treated Titanium Dioxide (TiO2) Nanoparticles for Water Purification

NASA Astrophysics Data System (ADS)

Araoyinbo, A. O.; Abdullah, M. M. A. B.; Rahmat, A.; Azmi, A. I.; Vizureanu, P.; Rahim, W. M. F. Wan Abd

2018-06-01

Photocatalysis using the semiconductor titanium dioxide (TiO2) has proven to be a successful technology for waste water purification. The photocatalytic treatment is an alternative method for the removal of soluble organic compounds in waste water. In this research, titanium dioxide nanoparticles were synthesized by sol-gel method using titanium tetraisopropoxide (TTIP) as a precursor. The sol was dried in the oven at 120°C after aging for 24 hours. The dried powder was then calcined at 400°C and 700°C with a heating rate of 10°C/min. The phase transformation of the heat treated titanium dioxide nanoparticles were characterized by X-Ray Diffraction (XRD, and the surface morphology by Scanning Electron Microscopy (SEM). The photocatalytic activity of the heat treated titanium dioxide nanoparticles in the degradation of methyl orange (MO) dye under ultraviolet (UV) light irradiation has been studied. At calcination temperature of 400°C, only anatase phase was observed, as the calcination temperature increases to 700°C, the rutile phase was present. The SEM images show the irregular shape of titanium dioxide particles and the agglomeration which tends to be more significant at calcined temperature of 700°C. Degradation of methyl orange by 5 mg heat treated titanium dioxide nanoparticles gives the highest percentage of degradation after irradiation by UV lamp for 4 hours.

Dilithium dialuminium trisilicate Crystalline Phase Prepared from Coal Fly Ash

NASA Astrophysics Data System (ADS)

Yao, Zhitong; Xia, Meisheng; Ye, Ying

2012-06-01

The dilithium dialuminium trisilicate phase Li2Al2Si3O10 was prepared using coal fly ash and lithium hydroxide monohydrate LiOH·H2O as precursors. The influences of various preparation conditions on Li2Al2Si3O10 forming were investigated. The results showed that the optimum additive amount of LiOH·H2O was about 20%. The onset of calcining temperature and time was identified as 980 °C and 1 h, respectively. XRD analysis indicated that the content of Li2Al2Si3O10 phase increased at the expense of quartz and mullite, with calcining temperatures increasing and time extending. SEM observation revealed that the calcined samples were drastically interlocked together with the prolonging of time. The obtained Li2Al2Si3O10 phase was well crystallized and with small grain size.

Synthesis and Electrochemical Analyses of Manganese Oxides for Super-Capacitors.

PubMed

Kim, Taewoo; Hwang, Hyein; Jang, Jaeyong; Park, Inyeong; Shim, Sang Eun; Baeck, Sung-Hyeon

2015-11-01

δ-Phase and α-phase manganese oxides were prepared using a hydrothermal method and their electrochemical properties were characterized. The influence of calcination temperature on the properties of manganese oxides was studied. Crystallinities were studied by X-ray diffraction, and scanning and transmission electron microscopy were utilized to examine morphologies. Average pore sizes and specific surface areas of samples were analyzed using the Barret-Joyner-Halenda and Brunauer-Emmett-Teller methods, respectively. After calcination in the range 300 degrees C to 600 degrees C, changes in morphology and crystallinity were observed. The flower-like shape of as synthesized samples became nanorod-like and the δ-phase changed to the α-phase. These changes may have been due to the removal of water during calcination. Furthermore, a transition stage in which the two phases coexisted was observed. Synthesized manganese oxides were mixed with carbon by sonification, to increase electric conductivity and to induce a synergistic effect between pseudo-capacitor and electric double layer capacitor (EDLC). Specific capacitances and rate durability of each composite were investigated by cyclic voltammetry in 1 M Na2SO4 electrolyte at different scan rates. MnO2 calcined at 400 degrees C exhibited the highest capacitance, probably due to its high surface area and more porous structure.

Iron oxide particles in large pore zeolites

NASA Astrophysics Data System (ADS)

García, J. L.; López, A.; Lázaro, F. J.; Martínez, C.; Corma, A.

1996-05-01

The magnetic properties of iron-containing ETS-10 zeolite and its calcined variety have been studied by magnetic measurements. The results are consistent with the presence of paramagnetic ions and superparamagnetic clusters. Calcination results in a shift of the blocking temperatures, although their frequency dependence cannot be ascribed to non-interacting clusters. The hypothesis of cluster-glass like behaviour is discussed.

Development and characterisation of novel heterogeneous palm oil mill boiler ash-based catalysts for biodiesel production.

PubMed

Ho, Wilson Wei Sheng; Ng, Hoon Kiat; Gan, Suyin

2012-12-01

Novel heterogeneous catalysts from calcium oxide (CaO)/calcined calcium carbonate (CaCO(3)) loaded onto different palm oil mill boiler ashes were synthesised and used in the transesterification of crude palm oil (CPO) with methanol to yield biodiesel. Catalyst preparation parameters including the type of ash support, the weight percentage of CaO and calcined CaCO(3) loadings, as well as the calcination temperature of CaCO(3) were optimised. The catalyst prepared by loading of 15 wt% calcined CaCO(3) at a fixed temperature of 800°C on fly ash exhibited a maximum oil conversion of 94.48%. Thermogravimetric analysis (TGA) revealed that the CaCO(3) was transformed into CaO at 770°C and interacted well with the ash support, whereas rich CaO, Al(2)O(3) and SiO(2) were identified in the composition using X-ray diffraction (XRD). The fine morphology size (<5 μm) and high surface area (1.719 m(2)/g) of the fly ash-based catalyst rendered it the highest catalytic activity. Copyright © 2012 Elsevier Ltd. All rights reserved.

Characterization of SrFe0.75Mo0.25O3-δ-La0.9Sr0.1Ga0.8Mg0.2O3-δ composite cathodes prepared by infiltration

NASA Astrophysics Data System (ADS)

Meng, Xie; Han, Da; Wu, Hao; Li, Junliang; Zhan, Zhongliang

2014-01-01

This paper describes the structure and electrochemical properties of composite cathodes for solid oxide fuel cells fabricated by infiltration of aqueous solutions corresponding to SrFe0.75Mo0.25O3-δ (SFMO) into porous La0.9Sr0.1Ga0.8Mg0.2O3-δ (LSGM) backbones. XRD measurement confirms the predominance of the perovskite SFMO oxides in the infiltrates together with some minor impurities of SrMoO4 after calcinations at 850-1100 °C. The cathode polarization resistance as obtained from impedance measurement on symmetric cathode fuel cells exhibits a pronounced increase as a function of calcinations temperature due to increased SFMO particle sizes, e.g., 0.04 Ω cm2 for 70 nm-sized catalysts calcinated at 850 °C versus 0.11 Ω cm2 for 400 nm-sized catalysts calcinated at 1100 °C. Oxygen partial pressure and temperature dependence of impedance data shows that oxygen reduction kinetics is largely determined by ionization of adsorbed oxygen atoms on the SFMO catalysts.

Alumosilicate ceramic proppants based on natural refractory raw materials

NASA Astrophysics Data System (ADS)

Vakalova, T. V.; Devyashina, L. P.; Burihina, M. A.; Kisner, A. S.; Pashenko, N. V.

2017-12-01

The sintering-strengthening effect of the additions of the highly ferrous bauxite (with Fe2O3 content of 20-25 % in the calcined state) in the compositions with refractory clays was established. It was found that in the temperature range 1350-1500°C the additions of bauxite in amounts of 10-40% have a fluxing effect due to the iron oxide introduced with bauxite in compositions with clay. An increasing the bauxite additive in the amount of 50-70% ensures its strengthening effect by increasing the total content of the mullite of the prismatic habit in the firing products of composites with clay. Preliminary clay and bauxite calcination at 900 °C and an increase in the content of bauxite additive up to 50-70% in compositions with clay allow to produce aluminosilicate proppants with a bulk density of 1.62-1.65 g/cm3 and compressive strength up to 52 MPa.

Dual-Templated Cobalt Oxide for Photochemical Water Oxidation.

PubMed

Deng, Xiaohui; Bongard, Hans-Josef; Chan, Candace K; Tüysüz, Harun

2016-02-19

Mesoporous Co3 O4 was prepared using a dual templating approach whereby mesopores inside SiO2 nanospheres, as well as the void spaces between the nanospheres, were used as templates. The effect of calcination temperature on the crystallinity, morphology, and textural parameters of the Co3 O4 replica was investigated. The catalytic activity of Co3 O4 for photochemical water oxidation in a [Ru(bpy)3 ](2+) [S2 O8 ](2-) system was evaluated. The Co3 O4 replica calcined at the lowest temperature (150 °C) exhibited the best performance as a result of the unique nanostructure and high surface area arising from the dual templating. The performance of Co3 O4 with highest surface area was further examined in electrochemical water oxidation. Superior activity over high temperature counterpart and decent stability was observed. Furthermore, CoO with identical morphology was prepared from Co3 O4 using an ethanol reduction method and a higher turnover-frequency number for photochemical water oxidation was obtained. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A thermal study on the structural changes of bimetallic ZrO2-modified TiO2 nanotubes synthesized using supercritical CO2.

PubMed

Lucky, R A; Charpentier, P A

2009-05-13

In this study the thermal behavior of bimetallic ZrO(2)-TiO(2) (10/90 mol/mol) nanotubes are discussed which were synthesized via a sol-gel process in supercritical carbon dioxide (scCO(2)). The effects of calcination temperature on the morphology, phase structure, mean crystallite size, specific surface area and pore volume of the nanotubes were investigated by using a variety of physiochemical techniques. We report that SEM and TEM images showed that the nanotubular structure was preserved at up to 800 degrees C calcination temperature. When exposed to higher temperatures (900-1000 degrees C) the ZrO(2)-TiO(2) tubes deformed and the crystallites fused together, forming larger crystallites, and a bimetallic ZrTiO(4) species was detected. These results were further examined using TGA, FTIR, XRD and HRTEM analysis. The BET textural properties demonstrated that the presence of a small amount of Zr in the TiO(2) matrix inhibited the grain growth, stabilized the anatase phase and increased the thermal stability.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Peigong; Fan, Caimei, E-mail: fancm@163.com; Wang, Yawen

Graphical abstract: The cubic phase BaTiO{sub 3} nanoparticles can be obtained at 600 °C and changed into tetragonal phase at 900 °C by a dual chelating sol–gel method, and the photocatalytic activities of the photocatalysts calcined at different temperatures were investigated by the removal of humic acid (HA) from water under UV light irradiation. Highlights: ► The humic acid in water was firstly degradated by BaTiO{sub 3} photocatalyst. ► The cubic BaTiO{sub 3} was obtained and changed into tetragonal phase at lower temperature. ► The chelating agents had an important influence on the phase formation of BaTiO{sub 3}. ► Themore » tetragonal phase BaTiO{sub 3} calcined at 900 °C exhibited higher photocatalytic activity under UV irradiation. -- Abstract: In this paper, a dual chelating sol–gel method was used to synthesize BaTiO{sub 3} nanoparticles by using acetylacetone and citric acid as chelating agents. The samples calcined at different temperatures were analyzed by thermogravimetric and differential thermal analysis (TG-DTA), X-ray diffraction (XRD), X-ray photoelectron spectra (XPS), scanning electron microscope (SEM) and UV–vis diffuse reflectance spectra (UV–vis). The results indicated that cubic phase BaTiO{sub 3} nanoparticles about 19.6 nm can be obtained at 600 °C and changed into tetragonal phase at 900 °C about 97.1 nm. All the BaTiO{sub 3} nanoparticles showed effective photocatalytic activities on the removal of humic acid (HA) under UV light irradiation. A comparison of single (acetylacetone or citric acid) and dual chelating (acetylacetone and citric acid) synthetic processes was also studied and the results demonstrated that the dual chelating agents indeed reduced phase transformation temperature from cubic to tetragonal BaTiO{sub 3}.« less

Synthesis and characterization of Co3O4 prepared from atmospheric pressure acid leach liquors of nickel laterite ores

NASA Astrophysics Data System (ADS)

Meng, Long; Guo, Zhan-cheng; Qu, Jing-kui; Qi, Tao; Guo, Qiang; Hou, Gui-hua; Dong, Peng-yu; Xi, Xin-guo

2018-01-01

A chemical precipitation-thermal decomposition method was developed to synthesize Co3O4 nanoparticles using cobalt liquor obtained from the atmospheric pressure acid leaching process of nickel laterite ores. The effects of the precursor reaction temperature, the concentration of Co2+, and the calcination temperature on the specific surface area, morphology, and the electrochemical behavior of the obtained Co3O4 particles were investigated. The precursor basic cobaltous carbonate and cobaltosic oxide products were characterized and analyzed by Fourier transform infrared spectroscopy, thermogravimetric differential thermal analysis, X-ray diffraction, field-emission scanning electron microscopy, specific surface area analysis, and electrochemical analysis. The results indicate that the specific surface area of the Co3O4 particles with a diameter of 30 nm, which were obtained under the optimum conditions of a precursor reaction temperature of 30°C, 0.25 mol/L Co2+, and a calcination temperature of 350°C, was 48.89 m2/g. Electrodes fabricated using Co3O4 nanoparticles exhibited good electrochemical properties, with a specific capacitance of 216.3 F/g at a scan rate of 100 mV/s.

LiMn2O4–yBryNanoparticles Synthesized by a Room Temperature Solid-State Coordination Method

PubMed Central

2009-01-01

LiMn2O4–yBrynanoparticles were synthesized successfully for the first time by a room temperature solid-state coordination method. X-ray diffractometry patterns indicated that the LiMn2O4–yBrypowders were well-crystallized pure spinel phase. Transmission electron microscopy images showed that the LiMn2O4–yBrypowders consisted of small and uniform nanosized particles. Synthesis conditions such as the calcination temperature and the content of Br−were investigated to optimize the ideal condition for preparing LiMn2O4–yBrywith the best electrochemical performances. The optimized synthesis condition was found in this work; the calcination temperature is 800 °C and the content of Br−is 0.05. The initial discharge capacity of LiMn2O3.95Br0.05obtained from the optimized synthesis condition was 134 mAh/g, which is far higher than that of pure LiMn2O4, indicating introduction of Br−in LiMn2O4is quite effective in improving the initial discharge capacity. PMID:20628635

Effects of local structure of Ce3+ ions on luminescent properties of Y3Al5O12:Ce nanoparticles

PubMed Central

He, Xiaowu; Liu, Xiaofang; Li, Rongfeng; Yang, Bai; Yu, Kaili; Zeng, Min; Yu, Ronghai

2016-01-01

Ce3+-doped yttrium aluminum garnet (YAG:Ce) nanocrystals were successfully synthesized via a facile sol-gel method. Multiple characterization techniques were employed to study the structure, morphology, composition and photoluminescence properties of YAG:Ce nanophosphors. The YAG:Ce0.0055 sintered at 1030 °C exhibited a typical 5d1-4f1 emission band with the maximum peak located at 525 nm, and owned a short fluorescence lifetime τ1 (~28 ns) and a long fluorescence lifetime τ2 (~94 ns). Calcination temperature and Ce3+ doping concentration have significant effects on the photoluminescence properties of the YAG:Ce nanophosphors. The emission intensity was enhanced as the calcination temperature increased from 830 to 1030 °C, but decreased dramatically with the increase of Ce3+ doping concentration from 0.55 to 5.50 at.% due to the concentration quenching. By optimizing the synthesized condition, the strongest photoluminescence emission intensity was achieved at 1030 °C with Ce3+ concentration of 0.55 at.%. PMID:26935980

Effect of microwave-assisted sintering on dielectric properties of CaCu3Ti4O12 ceramic

NASA Astrophysics Data System (ADS)

Rani, Suman; Ahlawat, Neetu; Punia, R.; Kundu, R. S.; Ahlawat, N.

2016-05-01

In this present work, CaCu3Ti4O12 (CCTO) was synthesized by conventional solid-state reaction technique. The synthesis process was carried out in two phases; by conventional process (calcination and sintering at 1080°C for 10 hours) and phase II involves the micro assisted pre sintering of conventionally calcined CCTO for very short soaking time of 30 min at 1080°C in a microwave furnace followed by sintering at 1080°C for 10 hours in conventional furnace. X-ray diffraction (XRD) patterns confirmed the formation of single phase ceramic. Dielectric properties were studied over the frequency range from 50Hz -5MHz at temperatures (273K-343K). It was observed that pre- microwave sintering enhance the dielectric constant values from 10900 to 11893 and respectively reduces the dielectric loss values from 0.49 to 0.34 at room temperature(1 KHz). CCTO ceramics which are found desirable for many technological applications. The effect is more pronounced at low frequencies of applied electric field.

Effect of the calcination temperature on the photocatalytic efficiency of acidic sol-gel synthesized TiO2 nanoparticles in the degradation of alprazolam.

PubMed

Romeiro, Andreia; Freitas, Diana; Emília Azenha, M; Canle, Moisés; Burrows, Hugh D

2017-06-14

We report a comparative study on the photodegradation of the widely used benzodiazepine psychoactive drug alprazolam (8-chloro-1-methyl-6-phenyl-4H-[1,2,4]triazolo[4,3-a][1,4]benzodiazepine, ALP) using direct photolysis, and titanium dioxide photocatalyzed reaction. Titanium dioxide photocatalysts were prepared as nanoparticles by acidic sol-gel methods, calcined at two different temperatures, and their behavior compared with P25 (Degussa type) TiO 2 . Efficient photodegradation was observed in the photocatalytic process, with over 90% degradation after 90 minutes under optimized conditions. Triazolaminoquinoline, 5-chloro-(5-methyl-4H-1,2,4-triazol-4-yl)benzophenone, triazolbenzophenone, and α-hydroxyalprazolam were identified as the degradation products by fluorescence spectroscopy and HPLC-MS. A comparison with the literature suggests that 8H-alprazolam may also be formed. Good mineralization was observed with TiO 2 photocatalysts. ALP photodegradation with TiO 2 follows pseudo-first order kinetics, with rates depending on the photocatalyst used. The effects of the quantity of the photocatalyst and concentration of alprazolam were studied.

Anatase vs. rutile efficiency on the photocatalytic degradation of clofibric acid under near UV to visible irradiation.

PubMed

Silva, Cláudia Gomes; Faria, Joaquim Luís

2009-05-01

Titanium dioxide (TiO(2)) powder, a semiconductor material typically used as a photocatalyst, is prepared following an acid-catalyzed sol-gel method starting from titanium isopropoxide. The xerogel calcination temperature is used to control surface and morphological properties of the material. Materials are extensively characterized by spectroscopic, micrographic and calorimetric techniques. The different TiO(2) catalysts are used in the visible-light-driven photocatalytic degradation of clofibric acid, a lipid regulator drug. The photoefficiency of TiO(2) catalysts, quantified in terms of kinetic rate constant, total organic carbon removal and initial quantum yield, increases with calcination temperature up to 673 K. A further increase in the calcination temperature leads to a decline in the photoefficiency of the catalysts, which is associated with the phase transformation from anatase to rutile concomitant with an increase in crystallite dimensions. The photochemical and photocatalytic oxidation of clofibric acid follows a pseudo-first order kinetic rate law. 4-Chlorophenol, isobutyric acid, hydroquinone, benzoquinone and 4-chlorocatechol are detected as main intermediates.

The influence of calcination temperatures on the acid-based properties and catalytic activity for the 1,3-butadiene synthesis from ethanol/acetaldehyde mixture

NASA Astrophysics Data System (ADS)

Gao, Meixiang; Jiang, Haoxi; Zhang, Minhua

2018-05-01

The influences of the calcination temperature on the catalysts' acid-based properties and catalytic activity for the 1,3-butadiene synthesis from ethanol are investigated. The results show that the 2 wt% ZrO2/Nano-SiO2 calcined at 773 K shows the best performance with the selectivity of 93.18% and conversion of 58.52% when reacted at 593 K, a WHSV of 1.8 h-1 and 3.5:1 volume ratio ethanol-to-acetaldehyde in an atmospheric fixed-bed reactor. Prepared catalysts were characterized by N2 adsorption-desorption, XRD, temperature-programmed desorption of NH3 and CO2, FTIR spectroscopy of adsorbed pyridine and CO2. Based on the relationship between the catalyst activity and its properties, the fact can be presumed that the formation and strength of Zrsbnd Osbnd Si bond determines the acid-based properties of the catalyst. In addition, moderate-intensity weak acid-basic sites are more suitable for ethanol conversion to BD with the amount of acid and basic sites as close as possible.

Removal of acid blue 062 on aqueous solution using calcinated colemanite ore waste.

PubMed

Atar, Necip; Olgun, Asim

2007-07-19

Colemanite ore waste (CW) has been employed as adsorbent for the removal of acid blue 062 anionic dye (AB 062) from aqueous solution. The adsorption of AB 062 onto CW was examined with respect to contact time, calcination temperature, particle size, pH, adsorbent dosage and temperature. The physical and chemical properties of the CW, such as particle sizes and calcinations temperature, play important roles in dye adsorption. The dye adsorption largely depends on the initial pH of the solution with maximum uptake occurring at pH 1. Three simplified kinetics models, namely, pseudo-first order, pseudo-second order, and intraparticle diffusion models were tested to investigate the adsorption mechanisms. The kinetic adsorption of AB 062 on CW follows a pseudo-second order equation. The adsorption data have been analyzed using Langmuir and Freundlich isotherms. The results indicate that the Langmuir model provides the best correlation of the experimental data. Isotherms have also been used to obtain the thermodynamic parameters such as free energy, enthalpy and entropy of the adsorption of dye onto CW.

Low temperature molten-salt synthesis of nanocrystalline cubic Sr{sub 2}SbMnO{sub 6}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Baral, Antara; Varma, K.B.R., E-mail: kbrvarma@mrc.iisc.ernet.i

2009-12-15

Sr{sub 2}SbMnO{sub 6} (SSM) powders were successfully synthesized at reasonably low temperatures via molten-salt synthesis (MSS) method using eutectic composition of 0.635 Li{sub 2}SO{sub 4}-0.365 Na{sub 2}SO{sub 4} (flux). High-temperature cubic phase SSM was stabilized at room temperature by calcining the as-synthesized powders at 900 deg. C/10 h. The phase formation and morphology of these powders were characterized via X-ray powder diffraction and scanning electron microscopy, respectively. The SSM phase formation associated with {approx}60 nm sized crystallites was also confirmed by transmission electron microscopy. The activation energy associated with the particle growth was found to be 95+-5 kJ mol{sup -1}.more » The dielectric constant of the tetragonal phase of the ceramic (fabricated using this cubic phase powder) with and without the flux (sulphates) has been monitored as a function of frequency (100 Hz-1 MHz) at room temperature. Internal barrier layer capacitance (IBLC) model was invoked to rationalize the dielectric properties. - Graphical abstract: The as synthesized powders of Sr{sub 2}SbMnO{sub 6} calcined at 900 deg. C/10 h yielded a cubic phase ({approx}60 nm sized crystallites). Centrosymmetric tetragonal (I4/mcm) phase was obtained by increasing the calcination temperature to 1000 deg. C. Display Omitted« less

Optical properties of β-Ga2O3 nanorods synthesized by a simple and cost-effective method using egg white solution

NASA Astrophysics Data System (ADS)

Phumying, Santi; Labauyai, Sarawut; Chareonboon, Wirat; Phokha, Sumalin; Maensiri, Santi

2015-06-01

In this paper, we report on the optical properties of gallium oxide (β-Ga2O3) nanorods synthesized by a simple, cost-effective and environment-friendly method using gallium(III) nitrate hydrate and freshly extracted egg white (ovalbumin) in an aqueous medium. The extracted egg white acted as a matrix for the entrapment of gallium ions to generate a gelled precursor. The structure of the prepared samples was studied by X-ray diffraction and Raman spectroscopy to confirm the formation of β-Ga2O3 with a monoclinic structure after calcination of the precursor in air at 750, 850, and 950 °C for 3 h. Scanning electron microscopy images revealed the morphology and formation of nanorods with different sizes and shapes in the samples, resulting from the effect of the calcination temperature. All the samples showed a strong UV absorption with the band gap in the range of 3.87-3.97 eV. Room-temperature photoluminescence spectra of all the samples also showed a strong UV emission. The UV emission results were discussed based on the basis of charge recombination.

Surface chemistry and catalytic performance of amorphous NiB/Hβ catalyst for n-hexane isomerization

NASA Astrophysics Data System (ADS)

Chen, Jinshe; Cai, Tingting; Jing, Xiaohui; Zhu, Lijun; Zhou, Yulu; Xiang, Yuzhi; Xia, Daohong

2016-12-01

The amorphous NiB nanoparticles were synthesized and a novel type of NiB/Hβ catalyst was prepared for the isomerization of n-hexane. The optimum preparation conditions were investigated and the effect of preparation conditions on the surface chemistry information of catalysts was characterized by XRD, N2 sorption studies, XPS, TPD and other related means. It was demonstrated that the loading amounts of NiB have effect on textural properties and the acid properties of surface. The loading amounts of NiB were also related to the amount of strong Lewis acid sites and the ratios of weak acid to strong acid of samples. Meanwhile, calcination temperatures of samples were closely associated with the structure of active components that function as metal centers. When the loading amount of NiB was 5 wt.% and calcination temperature was 200 °C, the catalyst had proper surface acidity sites and metal active sites to provide suitable synergistic effects. The mechanism for n-hexane isomerization was also investigated and the existence of unique structure of Bsbnd Nisbnd H was proved, which could provide good hydrogenation-dehydrogenation functions.

Preparation of erbium ion-doped TiO2 films and the study of their photocatalytic activity under simulated solar light

NASA Astrophysics Data System (ADS)

Lin, Hongfei; Huang, Yujiao; Li, Shaoni; Luan, Chunhui; Huang, Wei; Wang, Xiaodong; Feng, Xianshe

2017-11-01

A series of erbium ion-doped TiO2 (Er3+-TiO2) films were prepared by a sol-gel dip/spin coating method, and the effect of the dosage of erbium ion (0-2.0 mol%), the films coating layers (1-5 layers), and calcination temperature (400-700 °C) on the film structure and photocatalytic activity were investigated in detail. The films were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), thermal analysis (TG-DTG) and UV-Vis diffusive reflectance spectra (DRS). The results showed that the films were composed of anatase, and no other TiO2 phases (rutile and brookite). With the increase of the erbium ion dosage, the crystal size decreased. Erbium ion doping could enhance the thermal stability of TiO2 and inhibit the increase of the crystallite size. Meanwhile doping of erbium ions gave rise to three typical absorption peaks within the range of visible light (400-700 nm), locating at 490, 523, and 654 nm, attributed to the transition of 4f electrons. The higher calcination temperature led to higher crystallinity and bigger crystal grains. The photocatalytic performance of the films was evaluated by degradation of methyl orange solution under simulated solar light. The highest quality film we prepared was with 4 layers, 1.0 mol% dosage of erbium ion, and the calcination temperature of 500 °C. With this film, the degradation percentage of 7.8 mg/L methyl orange solution was up to 53.3% under simulated solar light after 6 h photoreaction.

Facile hydrothermal crystallization of NaLn(WO4)2 (Ln=La-Lu, and Y), phase/morphology evolution, and photoluminescence

NASA Astrophysics Data System (ADS)

Shi, Xiaofei; Li, Ji-Guang; Wang, Xuejiao; Zhu, Qi; Kim, Byung-Nam; Sun, Xudong

2017-12-01

Hydrothermal reaction of Ln nitrate and Na2WO4 at pH=8 and 200 °C for 24 hours, in the absence of any additive, has directly produced the scheelite-type sodium lanthanide tungstate of NaLn(WO4)2 for the larger Ln3+ of Ln=La-Dy (including Y, Group I) and an unknown compound that can be transformed into NaLn(WO4)2 by calcination at the low temperature of 600 °C for the smaller Ln3+ of Ln=Ho-Lu (Group II). With the successful synthesis of NaLn(WO4)2 for the full spectrum of Ln, the effects of lanthanide contraction on the structural features, crystal morphology, and IR responses of the compounds were clarified. The temperature- and time-course phase/morphology evolutions and the phase conversion upon calcination were thoroughly studied for the Group I and Group II compounds with Ln=La and Lu for example, respectively. Unknown intermediates were characterized by elemental analysis, IR absorption, thermogravimetry, and differential scanning calorimetry to better understand their chemical composition and coordination. The photoluminescence properties of NaEu(WO4)2 and NaTb(WO4)2, including excitation, emission, fluorescence decay, and quantum efficiency of luminescence, were also comparatively studied for the as-synthesized and calcination products.

Synthesis and characterization of C-doped TiO2 thin films for visible-light-induced photocatalytic degradation of methyl orange

NASA Astrophysics Data System (ADS)

Hassan, Mohamed Elfatih; Cong, Longchao; Liu, Guanglong; Zhu, Duanwei; Cai, Jianbo

2014-03-01

C-TiO2 thin films were synthesized by a modified sol-gel route based on the self-assembly technique exploiting Tween80 (T80) as a pore directing agent and carbon source. The effect of calcination time on the photocatalytic activity of C-doped TiO2 catalyst was studied. The samples were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transforms infrared (FTIR), UV-vis diffuse reflectance spectroscopy, and photoluminescence spectra (PL). The XRD results showed that C-TiO2 sample calcined at 400 °C for various times exhibited anatase phase and no other crystal phase was identified. C-TiO2 exhibited a shift in an absorption edge of samples in the visible region than that of conventional or reference TiO2. The XPS results showed an existence of C in the TiO2 catalysts and C might be existed as Csbnd Osbnd Ti group. Moreover, the C-TiO2 thin film calcined at 400 °C for 30 min showed the lowest PL intensity due to a decrease in the recombination rate of photogenerated electrons and holes under UV light irradiation. Also the photocatalytic activity of synthesized catalyst was evaluated by decomposition of methyl orange (MO) under visible light irradiation. The results showed that the optimum preparations of C-TiO2 thin films were found to be under calcination temperature of 400, calcination time of 30 min, and with preparation 9 layers film.

Structural and surface properties of CuO-ZnO-Cr{sub 2}O{sub 3} catalysts and their relationship with selectivity to higher alcohol synthesis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Campos-Martin, J.M.; Fierro, J.L.G.; Guerrero-Ruiz, A.

1995-10-01

A series of copper-zinc-chromium catalysts of different compositions and calcination temperatures has been prepared, characterized by several techniques (BET specific surface area, XRD, gravimetric TPR, TPD-CO, and XPS), and tested under high alcohol synthesis (HAS) conditions. CO hydrogenation was carried out at reaction temperatures of 523-598 K and 50 bar total pressure. The influence of catalyst composition, calcination temperature, and surface characteristics on the HAS selectivity was studied. The optimum HAS yields were found in the low Cr content region, but chromium was needed. Although chromium oxide does not seem to be involved in the catalytic site, its presence inmore » the catalyst composition is essential, owing to the larger specific surfaces and catalyst stability obtained at the highest reaction temperatures. For low Cr content composition, the temperature-programmed reduction (TPR) profiles were shifted to higher temperatures and simultaneously larger CO{sub 2} amounts were found in the temperature-programmed desorption profiles of adsorbed CO (TPD-CO). Photoelectron spectra (XPS) revealed that the oxidation state of copper is Cu{sup 2+} in the calcined catalysts and Cu{sup O} in the reduced ones; Cu{sup +} was only stabilized in a CuCr{sub 2}O{sub 4} spinel in the Cr-rich catalysts. These features derived from catalyst characterization are discussed in the framework of the catalytic behaviour for HAS synthesis. 53 refs., 7 figs., 4 tabs.« less

Quantifying Morphological Features of α-U3O8 with Image Analysis for Nuclear Forensics.

PubMed

Olsen, Adam M; Richards, Bryony; Schwerdt, Ian; Heffernan, Sean; Lusk, Robert; Smith, Braxton; Jurrus, Elizabeth; Ruggiero, Christy; McDonald, Luther W

2017-03-07

Morphological changes in U 3 O 8 based on calcination temperature have been quantified enabling a morphological feature to serve as a signature of processing history in nuclear forensics. Five separate calcination temperatures were used to synthesize α-U 3 O 8 , and each sample was characterized using powder X-ray diffraction (p-XRD) and scanning electron microscopy (SEM). The p-XRD spectra were used to evaluate the purity of the synthesized U-oxide; the morphological analysis for materials (MAMA) software was utilized to quantitatively characterize the particle shape and size as indicated by the SEM images. Analysis comparing the particle attributes, such as particle area at each of the temperatures, was completed using the Kolmogorov-Smirnov two sample test (K-S test). These results illustrate a distinct statistical difference between each calcination temperature. To provide a framework for forensic analysis of an unknown sample, the sample distributions at each temperature were compared to randomly selected distributions (100, 250, 500, and 750 particles) from each synthesized temperature to determine if they were statistically different. It was found that 750 particles were required to differentiate between all of the synthesized temperatures with a confidence interval of 99.0%. Results from this study provide the first quantitative morphological study of U-oxides, and reveals the potential strength of morphological particle analysis in nuclear forensics by providing a framework for a more rapid characterization of interdicted uranium oxide samples.

Facile Synthesis of Wormhole-Like Mesoporous Tin Oxide via Evaporation-Induced Self-Assembly and the Enhanced Gas-Sensing Properties

NASA Astrophysics Data System (ADS)

Li, Xiaoyu; Peng, Kang; Dou, Yewei; Chen, Jiasheng; Zhang, Yue; An, Gai

2018-01-01

Wormhole-like mesoporous tin oxide was synthesized via a facile evaporation-induced self-assembly (EISA) method, and the gas-sensing properties were evaluated for different target gases. The effect of calcination temperature on gas-sensing properties of mesoporous tin oxide was investigated. The results demonstrate that the mesoporous tin oxide sensor calcined at 400 °C exhibits remarkable selectivity to ethanol vapors comparison with other target gases and has a good performance in the operating temperature and response/recovery time. This might be attributed to their high specific surface area and porous structure, which can provide more active sites and generate more chemisorbed oxygen spices to promote the diffusion and adsorption of gas molecules on the surface of the gas-sensing material. A possible formation mechanism of the mesoporous tin oxide and the enhanced gas-sensing mechanism are proposed. The mesoporous tin oxide shows prospective detecting application in the gas sensor fields.

Lewis acid properties of alumina based catalysts: study by paramagnetic complexes of probe molecules

NASA Astrophysics Data System (ADS)

Fionov, Alexander V.

2002-06-01

Lewis acid properties of LiAl 5O 8/Al 2O 3 (2 wt.% Li) and MgAl 2O 4/Al 2O 3 (3 wt.% Mg) catalysts were studied by EPR of adsorbed probe molecules--anthraquinone and 2,2,6,6-tetramethylpiperidine- N-oxyl (TEMPO). The lesser (in comparison with γ-Al 2O 3) concentration and the strength of Lewis acid sites (LAS) formed on the surface of aluminate layer has been shown. The stability of this layer plays important role in the change of Lewis acid properties during the calcination of modified alumina. The lithium aluminate layer was stable at used calcination temperature, 773 K, meanwhile magnesium aluminate layer observed only at calcination temperature below 723 K. The increase of the calcination temperature to 773 K caused the segregation of MgAl 2O 4 on the surface resulted in the release of alumina surface and recovery of the Lewis acid properties. The differences in the LAS manifestations towards TEMPO and anthraquinone was discussed. The mechanism of the formation of anthraquinone paramagnetic complexes with LAS--three-coordinated aluminum ions--was proposed. This mechanism includes the formation of anthrasemiquinone, and then--anthrasemiquinone ion pair or triple ion. Fragments like -O-Al +-O- play the role of cations in these ion pairs and triple ions. Proposed mechanism can also be applied for the consideration of similar anthraquinone paramagnetic complexes on the surface of gallium oxide containing systems.

Studies on photocatalytic activity of the synthesised TiO2 and Ag/TiO2 photocatalysts under UV and sunlight irradiations.

PubMed

Vaithiyanathan, R; Sivakumar, T

2011-01-01

Photocatalytic decolorisation and degradation of Reactive Red 120 (RR 120) has been investigated under UV (365 nm) and solar light as radiation sources using synthesised nano titania catalyst prepared via sol-gel method. The study encompassed calcination of synthesised titania catalyst at a range of temperature up to 1,000°C. The effects of calcination temperature on titania catalyst have been evaluated on the decolorisation of RR 120. The analysis revealed complete decolorisation of dye solution in 100 min under UV light with the TiO2 catalyst calcined at 200°C. Only a maximum of 47% dye decolorisation was achieved under sunlight in 4 h with no improvement even after prolonged irradiation. In an endeavour to improve the catalytic activity, bare titania was modified with silver metal and a comprehensive study on the characteristics of silver modified catalyst was made. The result was an enhancement of the rate of decolorisation of dye under both UV and solar light sources. All the catalysts were characterised by XRD and BET analyses. Optimisation of the degradation of RR 120 has been carried out using the unmodified catalyst by varying the amount of catalyst, substrate concentration, pH of dye solution. Effects of addition of small amounts of various oxidants such as H2O2, KBrO3 and (NH4)2S2O8 have also been studied. Pseudo first order kinetics was observed in the photocatalytic decolorisation of dye. The mineralisation of RR 120 was monitored by TOC analysis.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lu, D.Y.; Hughes, R.W.; Anthony, E.J.

Sintering during calcination/carbonation may introduce substantial economic penalties for a CO{sub 2} looping cycle using limestone/dolomite-derived sorbents. Cyclic carbonation and calcination reactions were investigated for CO{sub 2} capture under fluidized bed combustion (FBC) conditions. The cyclic carbonation characteristics of CaCO{sub 3}-derived sorbents were compared at various calcination temperatures (700-925{sup o} C) and different gas stream compositions: pure -2 and a realistic calciner environment where high concentrations of CO{sub 2}>80-90% are expected. The conditions during carbonation were 700 {sup o}C and 15% CO{sub 2} in N{sub 2} and 0.18% or 0.50% SO{sub 2} in selected tests. Up to 20 calcination/carbonation cyclesmore » were conducted using a thermogravimetric analyzer (TGA) apparatus. Three Canadian limestones were tested: Kelly Rock, Havelock, and Cadomin, using a prescreened particle size range of 400-650 {mu} m. Calcined Kelly Rock and Cadomin samples were hydrated by steam and examined. Sorbent reactivity was reduced whenever SO{sub 2} was introduced to either the calcining or carbonation streams. The multicyclic capture capacity of CaO for CO{sub 2} was substantially reduced at high concentrations of CO{sub 2} during the sorbent regeneration process and carbonation conversion of the Kelly Rock sample obtained after 20 cycles was only 10.5%. Hydrated sorbents performed better for CO{sub 2} capture but showed deterioration following calcination in high CO{sub 2} gas streams indicating that high CO{sub 2} and SO{sub 2} levels in the gas stream lead to lower CaO conversion because of enhanced sintering and irreversible formation of CaSO{sub 4}.« less

The effect of heating on mineral composition and grain size distribution of flux calcined porcelanites from the Gafsa-Metlaoui basin, southwestern Tunisia

NASA Astrophysics Data System (ADS)

Saidi, Raja; Tlili, Ali; Jamoussi, Fakher

2016-12-01

The porcelanite rock of Ypresian phosphatic series of the Gafsa-Metlaoui basin (south-western Tunisia), is composed mainly of opal CT, and presents a variable percentage of carbonates and fibrous clays. This rock is treated with flux calcination at different temperatures in order to prepare a specific filter aid for cleaning melting sulfur which can be used for the production of sulfuric acid. This work presents the effect of heating on the mineralogy and grain size distribution of carbonate-rich porcelanite (Tm1) and clay-rich porcelanite (Gh) compared to flux calcined silica-rich porcelanite (CHM3) and diatomaceous filtration aids. The porcelanite samples used in this work come from three localities of the Gafsa-Metlaoui basin: Kef El Ghis (Gh), Tamarza (Tm1) and Mides (CHM3). Flux calcination at 1000 °C provokes a mineralogical transformation on carbonate-rich porcelanite samples. The opal CT transforms to opal C and becomes neater and more stable. The Thermal treatment of porcelanite (Tm1) incites also the apparition of new peaks of wollastonite. However, the structural change of opal CT to opal C by heat treatment is blocked for flux calcination of clay-rich porcelanite. The opal CT of fluxing clay-rich porcelanite becomes more ordered without significant change to opal C. The difference between fluxing carbonate-rich porcelanite (Tm1) and fluxing clay-rich porcelanite (Gh) appears also with granulometric distribution histogram of the tow heated samples. All raw samples have unimodal granulometric distribution (1-100 μm). After calcination with alkaline flux at 1000 °C fluxing carbonate-rich porcelanite displays bimodal granulometric distribution and a new mode appears systematically, between 0.1 μm and 1 μm. This occurs for fluxing silica-riche porcelanite and diatomaceous filtration aids as well and corresponds to the opal C formed after heat treatment. Whereas fluxing clay-rich porcelanite present trimodal granulometric distribution and a third mode appears (100-300 μm), which due to silica glass phase. Since, the granulometric rearrangement of porcelanite during thermal treatment may due to mineralogical transformation of opal CT to opal C and crystal grow.

40 CFR 60.733 - Reconstruction.

Code of Federal Regulations, 2014 CFR

2014-07-01

... § 60.733 Reconstruction. The cost of replacement of equipment subject to high temperatures and abrasion... facility” under § 60.15. Calciner and dryer equipment subject to high temperatures and abrasion are: end...

40 CFR 60.733 - Reconstruction.

Code of Federal Regulations, 2012 CFR

2012-07-01

... § 60.733 Reconstruction. The cost of replacement of equipment subject to high temperatures and abrasion... facility” under § 60.15. Calciner and dryer equipment subject to high temperatures and abrasion are: end...

40 CFR 60.733 - Reconstruction.

Code of Federal Regulations, 2011 CFR

2011-07-01

... § 60.733 Reconstruction. The cost of replacement of equipment subject to high temperatures and abrasion... facility” under § 60.15. Calciner and dryer equipment subject to high temperatures and abrasion are: end...

40 CFR 60.733 - Reconstruction.

Code of Federal Regulations, 2013 CFR

2013-07-01

... § 60.733 Reconstruction. The cost of replacement of equipment subject to high temperatures and abrasion... facility” under § 60.15. Calciner and dryer equipment subject to high temperatures and abrasion are: end...

Combustion synthesis and structural analysis of nanocrystalline nickel ferrite at low temperature regime

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shanmugavel, T., E-mail: gokulrajs@hotmail.com, E-mail: shanmugavelnano@gmail.com; Raj, S. Gokul, E-mail: gokulrajs@hotmail.com, E-mail: shanmugavelnano@gmail.com; Rajarajan, G.

2015-06-24

Combustion synthesis of single phase Nickel ferrite was successfully achieved at low temperature regime. The obtained powders were calcinated to increase the crystallinity and their characterization change due to calcinations is investigated in detail. Citric acid used as a chelating agent for the synthesis of nickel ferrite. Pure single phase nickel ferrites were found at this low temperature. The average crystalline sizes were measured by using powder XRD measurements. Surface morphology was investigated through Transmission Electron Microscope (TEM). Particle size calculated in XRD is compared with TEM results. Magnetic behaviour of the samples is analyzed by using Vibrating Sample Magnetometermore » (VSM). Saturation magnetization, coercivity and retentivity are measured and their results are discussed in detail.« less

Conversion of Conventional Rotary Kiln Into Effective Sandy Alumina Calciner

NASA Astrophysics Data System (ADS)

Ishihara, M.; Hirano, T.; Yajima, H.

Using conventional rotary kiln for calcining sandy alumina in potlines, remakable heat-saving and capacity-improving can be achieved. 83 liters of oil per tonne of alumina (3200MJ/tonne) were required for calcining 800 m.t.p.d. of sandy alumina in the rotary kiln at Shimizu Works. The kiln is installed with two stages of flash dryers and planetary coolers, and was originally designed for calcining floury alumina at 550 m.t.p.d. This improvement in capacity and unit oil consumption was achieved mainly through shortening the flame by using a special burner and effective heat recovery. The quality of sandy alumina calcined by the kiln is good enough for potlines.

Sol-Gel Synthesis of La(0.6)Sr(0.4)CoO(3-x) and Sm(0.5)Sr(0.5)CoO(3-x) Cathode Nanopowders for Solid Oxide Fuel Cells

NASA Technical Reports Server (NTRS)

Bansal, Narottam P.; Wise, Brent

2011-01-01

Nanopowders of La(0.6)Sr(0.4)CoO(3-x) (LSC) and Sm(0.5)Sr(0.5)CoO(3-x) (SSC) compositions, which are being investigated as cathode materials for intermediate temperature solid oxide fuel cells (IT-SOFC) 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. Solgel powders calcined at 550 to 1000 C consisted of a number of phases. Single perovskite phase La(0.6)Sr(0.4)CoO(3-x) or Sm(0.5)Sr(0.5)CoO(3-x) powders were obtained at 1200 and 1300 C, respectively. Morphological analysis of the powders calcined at various temperatures was done by scanning electron microscopy. The average particle size of the powders was approx.15 nm after 700 C calcinations and slowly increased to 70 to 100 nm after heat treatments at 1300 to 1400 C.

Nanostructure investigation of magnetic nanomaterial Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4} synthesized by sol-gel method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pransisco, Prengki, E-mail: prengkipransisco@gmail.com; Badan Lingkungan Hidup Derah Kabupaten Empat Lawang South of Sumatera; Shafie, Afza, E-mail: afza@petronas.com.my

2015-07-22

Magnetic nanomaterial Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4} was successfully prepared by using sol-gel method. Heat treatment on material is always giving defect on properties of material. This paper investigates the effect of heat treatment on nanostructure of magnetic nanomaterial Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4}. According to thermo gravimetric analysis (TGA) that after 600°C there is no more weight loss detected and it was decided as minimum calcination temperature. Intensity, crystallite size, structure, lattice parameter and d-spacing of the material were investigated by using X-ray diffraction (XRD). High resolution transmission electron microscope (HRTEM) was used to examine nanostructure, nanosize,more » shape and distribution particle of magnetic material Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4} and variable pressure field emission scanning electron microscope (VP-FESEM) was used to investigate the surface morphology and topography of the material. The XRD result shows single-phase cubic spinel structure with average crystallite size in the range of 25.6-95.9 nm, the value of the intensity of the material was increased with increasing temperature, and followed by lattice parameter was increased with increasing calcination temperature, value of d-spacing was relatively decreased with accompanied increasing temperature. From HRTEM result the distribution of particles was tend to be agglomerates with particle size of 7.8-17.68 nm. VP-FESEM result shows that grain size of the material increases with increasing calcination temperature and the surface morphology shows that the material is in hexagonal shape and it was also proved by mapping result which showing the presence each of constituents inside the compound.« less

Structural, magnetic and optical properties of ZnO nanostructures converted from ZnS nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patel, Prayas Chandra; Ghosh, Surajit; Srivastava, P.C., E-mail: pcsrivastava50@gmail.com

Graphical abstract: The phase conversion of ZnS to highly crystalline hexagonal ZnO was done by heat treatment. - Highlights: • Phase change of cubic ZnS to hexagonal ZnO via heat treatment. • Band gap was found to decrease with increasing calcinations temperature. • ZnO samples have higher magnetic moment than ZnS. • Blocking Temperature of the samples is well above room temperature. • Maximum negative%MR with saturation value ∼38% was found for sample calcined at 600° C. - Abstract: The present work concentrates on the synthesis of cubic ZnS and hexagonal ZnO semiconducting nanoparticle from same precursor via co-precipitation method.more » The phase conversion of ZnS to highly crystalline hexagonal ZnO was done by heat treatment. From the analysis of influence of calcination temperature on the structural, optical and vibrational properties of the samples, an optimum temperature was found for the total conversion of ZnS nanoparticles to ZnO. Role of quantum confinement due to finite size is evident from the blue shift of the fundamental absorption in UV–vis spectra only in the ZnS nanoparticles. The semiconducting nature of the prepared samples is confirmed from the UV–vis, PL study and transport study. From the magnetic and transport studies, pure ZnO phase was found to be more prone to magnetic field.« less

Green synthesis and characterization of ANbO3 (A = Na, K) nanopowders fabricated using a biopolymer

NASA Astrophysics Data System (ADS)

Khorrami, Gh. H.; Mousavi, M.; Khayatian, S. A.; Kompany, A.; Khorsand Zak, A.

2017-10-01

Lead-free sodium niobate (NaNbO3, NN) and potassium niobate (KNbO3, KN) nanopowders were successfully synthesized by a simple and green synthesis process in gelatin media. Gelatin, which is a biopolymer, was used as stabilizer. In order to determine the lowest calcination temperature needed to obtain pure NN and KN nanopowders, the produced gels were analyzed by thermogravometric analyzer (TGA). The produced gels were calcined at 500∘C and 600∘C. The structural and optical properties of the prepared powders were examined using X-ray diffraction (XRD) technique, transmission electron microscopy (TEM), and UV-Vis spectroscopy. The XRD results revealed that pure phase NN and KN nanopowders were formed at low temperature calcination of 500∘C and 600∘C, respectively. The Scherrer formula and size-strain plot (SSP) method were employed to estimate crystallite size and lattice strain of the samples. The TEM images show that the NN and KN samples calcined at 600∘C have cubic shape with an average particle size of 60.95 and 39.29 nm, respectively. The optical bandgap energy of the samples was calculated using UV-Vis diffused reflectance spectra of the samples and Kubelka-Munck relation.

High-surface-area mesoporous TiO2 microspheres via one-step nanoparticle self-assembly for enhanced lithium-ion storage

NASA Astrophysics Data System (ADS)

Wang, Hsin-Yi; Chen, Jiazang; Hy, Sunny; Yu, Linghui; Xu, Zhichuan; Liu, Bin

2014-11-01

Mesoporous TiO2 microspheres assembled from TiO2 nanoparticles with specific surface areas as high as 150 m2 g-1 were synthesized via a facile one-step solvothermal reaction of titanium isopropoxide and anhydrous acetone. Aldol condensation of acetone gradually releases structural H2O, which hydrolyzes and condenses titanium isopropoxide, forming TiO2 nanocrystals. Simultaneous growth and aggregation of TiO2 nanocrystals leads to the formation of high-surface-area TiO2 microspheres under solvothermal conditions. After a low-temperature post-synthesis calcination, carbonate could be incorporated into TiO2 as a dopant with the carbon source coming from the organic byproducts during the synthesis. Carbonate doping modifies the electronic structure of TiO2 (e.g., Fermi level, Ef), and thus influences its electrochemical properties. Solid electrolyte interface (SEI) formation, which is not common for titania, could be initiated in carbonate-doped TiO2 due to elevated Ef. After removing carbonate dopants by high-temperature calcination, the mesoporous TiO2 microspheres showed much improved performance in lithium insertion and stability at various current rates, attributed to a synergistic effect of high surface area, large pore size and good anatase crystallinity.Mesoporous TiO2 microspheres assembled from TiO2 nanoparticles with specific surface areas as high as 150 m2 g-1 were synthesized via a facile one-step solvothermal reaction of titanium isopropoxide and anhydrous acetone. Aldol condensation of acetone gradually releases structural H2O, which hydrolyzes and condenses titanium isopropoxide, forming TiO2 nanocrystals. Simultaneous growth and aggregation of TiO2 nanocrystals leads to the formation of high-surface-area TiO2 microspheres under solvothermal conditions. After a low-temperature post-synthesis calcination, carbonate could be incorporated into TiO2 as a dopant with the carbon source coming from the organic byproducts during the synthesis. Carbonate doping modifies the electronic structure of TiO2 (e.g., Fermi level, Ef), and thus influences its electrochemical properties. Solid electrolyte interface (SEI) formation, which is not common for titania, could be initiated in carbonate-doped TiO2 due to elevated Ef. After removing carbonate dopants by high-temperature calcination, the mesoporous TiO2 microspheres showed much improved performance in lithium insertion and stability at various current rates, attributed to a synergistic effect of high surface area, large pore size and good anatase crystallinity. Electronic supplementary information (ESI) available. See DOI: 10.1039/c4nr04729j

DOE Office of Scientific and Technical Information (OSTI.GOV)

Richard D. Boardman; B. H. O'Brien; N. R. Soelberg

About one million gallons of acidic, hazardous, and radioactive sodium-bearing waste are stored in stainless steel tanks at the Idaho Nuclear Technology and Engineering Center (INTEC), which is a major operating facility of the Idaho National Engineering and Environmental Laboratory. Calcination at high-temperature conditions (600 C, with alumina nitrate and calcium nitrate chemical addition to the feed) is one of four options currently being considered by the Department of Energy for treatment of the remaining tank wastes. If calcination is selected for future processing of the sodium-bearing waste, it will be necessary to install new off-gas control equipment in themore » New Waste Calcining Facility (NWCF) to comply with the Maximum Achievable Control Technology (MACT) standards for hazardous waste combustors and incinerators. This will require, as a minimum, installing a carbon bed to reduce mercury emissions from their current level of up to 7,500 to <45 {micro}g/dscm, and a staged combustor to reduce unburned kerosene fuel in the off-gas discharge to <100 ppm CO and <10 ppm hydrocarbons. The staged combustor will also reduce NOx concentrations of about 35,000 ppm by 90-95%. A pilot-plant calcination test was completed in a newly constructed 15-cm diameter calciner vessel. The pilot-plant facility was equipped with a prototype MACT off-gas control system, including a highly efficient cyclone separator and off-gas quench/venturi scrubber for particulate removal, a staged combustor for unburned hydrocarbon and NOx destruction, and a packed activated carbon bed for mercury removal and residual chloride capture. Pilot-plant testing was performed during a 50-hour system operability test January 14-16, followed by a 100-hour high-temperature calcination pilot-plant calcination run January 19-23. Two flowsheet blends were tested: a 50-hour test with an aluminum-to-alkali metal molar ratio (AAR) of 2.25, and a 50-hour test with an AAR of 1.75. Results of the testing indicate that sodium-bearing waste can be successfully calcined at 600 C with an AAR of 1.75. Unburned hydrocarbons are reduced to less than 10 ppm (7% O2, dry basis), with >90% reduction of NOx emissions. Mercury removal by the carbon bed reached 99.99%, surpassing the control efficiency needed to meet MACT emissions standards. No deleterious impacts on the carbon bed were observed during the tests. The test results imply that upgrading the NWCF calciner with a more efficient cyclone separator and the proposed MACT equipment can process the remaining tanks wastes in 3 years or less, and comply with the MACT standards.« less

Summary of Calcine Disposal Development Using Hot Isostatic Pressing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bateman, Ken; Wahlquist, Dennis; Hart, Edward

2015-03-01

Battelle Energy Alliance, LLC, has demonstrated the effectiveness of the hot isostatic press (HIP) process for treatment of hazardous high-level waste known as calcine that is stored at the Idaho Nuclear Technology and Engineering Center (INTEC) at Idaho National Laboratory. HIP trials performed with simulated calcines at Idaho National Laboratory’s Materials and Fuels Complex and an Australian Nuclear Science and Technology Organization facility from 2007 to 2010 produced a dense, monolithic waste form with increased chemical durability and effective (storage) volume reductions of ~10 to ~70% compared to granular calcine forms. In December 2009, the U.S. Department of Energy signedmore » an amended Record of Decision selecting HIP technology as the treatment method for the 4,400 m3 of granular zirconia and alumina calcine stored at INTEC. Testing showed that HIP treatment reduces the risks associated with radioactive and hazardous constituent release, post-production handling, and long-term (repository) storage of calcines and would result in estimated storage cost savings in the billions of dollars. Battelle Energy Alliance has the ability to complete pilot-scale HIP processing of INTEC calcine, which is the next necessary step in implementing HIP processing as a calcine treatment method.« less

Morphology and crystalline phase study of electrospun TiO2 SiO2 nanofibres

NASA Astrophysics Data System (ADS)

Ding, Bin; Kim, Hakyong; Kim, Chulki; Khil, Myungseob; Park, Soojin

2003-05-01

Nanofibres of TiO2-SiO2 (Ti:Si = 50: 50 mol%) with diameters of 50-400 nm were prepared by calcining electrospun nanofibres of polyvinyl acetate (PVac)/titania-silica composite as precursor. These PVac/titania-silica hybrid nanofibres were obtained from a homogenous solution of PVac with a sol-gel of titanium isopropoxide (TiP) and tetraethoxysilane by using the electrospinning technique. The nanofibres were characterized by scanning electron microscopy (SEM), wide-angle x-ray diffraction (WAXD), Fourier transform infrared (FTIR) spectroscopy and Brunauer-Emmett-Teller (BET) surface area. SEM, WAXD and FTIR results indicated that the morphology and crystalline phase of TiO2-SiO2 nanofibres were strongly influenced by the calcination temperature and the content of titania and silica in the nanofibres. Additionally, the BET results showed that the surface area of TiO2-SiO2 nanofibres was decreased with increasing calcination temperature and the content of titania and silica in nanofibres.

[Catalytic combustion of soot on combined oxide catalysts].

PubMed

He, Xu-wen; Yu, Jun-jie; Kang, Shou-fang; Hao, Zheng-ping; Hu, Chun

2005-01-01

Combined oxide catalysts are prepared for catalytic combustion of soot and regeneration from diesel emissions. Thermo-gravimetric analysis(TGA) and temperature programmed oxidation(TPO)are used to evaluate the activity of catalysts under the influence of composition,atomic ration, H2O, calcinations temperature and mass ration between catalysts and soot. Results show that Cu-Mo-O had high activity among double metal oxide catalysts. Among multicomponent metal oxide catalysts, Cu-K-Mo-O had high activity when atomic ratio Cu: K: Mo = 1:1:2 and mass ration between catalysts and soot equals 5: 1. Under this condition, soot ignition temperature of Cu-K-Mo-O catalyst was 327 degrees C. H2O addition and calcinations temperature had little influence on it,which is one kind of compatible catalyst for soot control and catalytic regeneration from diesel emissions.

Biodiesel production via the transesterification of soybean oil using waste starfish (Asterina pectinifera).

PubMed

Jo, Yong Beom; Park, Sung Hoon; Jeon, Jong-Ki; Ko, Chang Hyun; Ryu, Changkook; Park, Young-Kwon

2013-07-01

Calcined waste starfish was used as a base catalyst for the production of biodiesel from soybean oil for the first time. A batch reactor was used for the transesterification reaction. The thermal characteristics and crystal structures of the waste starfish were investigated by thermo-gravimetric analysis and X-ray diffraction. The biodiesel yield was determined by measuring the content of fatty acid methyl esters (FAME). The calcination temperature appeared to be a very important parameter affecting the catalytic activity. The starfish-derived catalyst calcined at 750 °C or higher exhibited high activity for the transesterification reaction. The FAME content increased with increasing catalyst dose and methanol-over-oil ratio.

Synthesis, structural and semiconducting properties of Ba(Cu1/3 Sb2/3)O3-PbTiO3 solid solutions

NASA Astrophysics Data System (ADS)

Singh, Chandra Bhal; Kumar, Dinesh; Prashant, Verma, Narendra Kumar; Singh, Akhilesh Kumar

2018-05-01

We report the synthesis and properties of a new solid solution 0.05Ba(Cu1/3Sb2/3)O3-0.95PbTiO3 (BCS-PT) which shows the semiconducting properties. In this study, we have designed new perovskite-type (ABO3) solid solution of BCS-PT that have tunable optical band gap. BCS-PT compounds were prepared by conventional solid-state reaction method and their structural, micro-structural and optical properties were analyzed. The calcination temperature for BCS-PT solid solutions has been optimized to obtain a phase pure system. The Reitveld analysis of X-ray data show that all samples crystallize in tetragonal crystal structure with space group P4mm. X-ray investigation revealed that increase in calcination temperature led to increase of lattice parameter `a' while `c' parameter value lowered. The band gap of PbTiO3 is reduced from 3.2 eV to 2.8 eV with BCS doping and with increasing calcination temperature it further reduces to 2.56 eV. The reduced band gap indicated that the compounds are semiconducting and can be used for photovoltaic device applications.

Preparation and characterization of nanosilica from oil shale ash.

PubMed

Li, Jinhong; Qian, Tingting; Tong, Lingxin; Shen, Jie

2014-05-01

Nano-sized silica powders was prepared using oil shale ash (OSA) as starting materials. A combined process was proposed for the utilization of OSA in the production of the nanosilica, including three stages: calcination, alkaline leaching and carbon dioxide separation. Effects of the calcining temperature, sodium hydroxide concentration and holding time on the desilication ratio were investigated. The microstructure and morphologies of the nano-sized silica were characterized by X-ray diffraction, transmission electron microscopy, and Brunauer-Emmett-Teller nitrogen-gas adsorption method. The results indicated that the obtained powders with particle size of about 40 nm are homegeneously dispersed and its specific surface area is 387 m2/g. The properties of the nano-sized silica powder meet the requirements of the Chinese Chemical Industry Standard HG/T 3061-1999.

In-situ X-ray diffraction activation study on an Fe/TiO2 pre-catalyst.

PubMed

Rayner, Matthew K; Billing, David G; Coville, Neil J

2014-06-01

This study focuses on the use of in situ powder X-ray diffraction (PXRD) and quantitative phase analysis using the Rietveld method to monitor the structural properties of a titania-supported iron (10% Fe/TiO2) pre-catalyst during calcination (oxidation) and activation (reduction) in the temperature range 25-900°C. The TiO2 oxidation study revealed an increase in anatase particle size before the anatase to rutile phase transformation, lending credibility to the bridging mechanism proposed by Kim et al. [(2007), Mater. Sci. Forum, 534-536, 65-68]. Pre-catalyst oxidation experiments allowed for the determination of a suitable calcination temperature (450°C) of the pre-catalyst in terms of maximum hematite concentration and appropriate particle size. These experiments also confirmed that the anatase to rutile phase transformation occurred at higher temperatures after Fe addition and that anatase was the sole donor of Ti(4+) ions, which are known to migrate into hematite (Gennari et al., 1998), during the formation of pseudobrookite (Fe2TiO5) at temperatures above 690°C. Using the results from the oxidation experiments, two pre-catalyst samples were calcined at different temperatures; one to represent the preferred case and one to represent a case where the pre-catalyst had been excessively heated. Samples of the excessively heated catalysts were exposed to different reducing gas atmospheres (5, 10 and 100% H2/N2) and heated in the in situ PXRD reactor, so that diffraction data could be collected during the activation process. The results show that reduction with gases containing low concentrations of H2 (5 and 10%) led to the formation of ilmenite (FeTiO3) and we were able to show that both anatase and rutile are consumed in the reaction. Higher concentrations of H2 led to the formation of magnetite (Fe3O4) and metallic iron (Fe(0)). We also noted a decrease in the anatase to rutile transformation temperature under reducing atmospheres when compared with the pre-catalyst heat-treatment experiment. A reduced calcination temperature prior to reduction allowed more facile Fe reduction.

Synthesis and Thermodynamic Stability of Ba2B‧B″O6 and Ba3B*B″2O9 Perovskites Using the Molten Salt Method

NASA Astrophysics Data System (ADS)

Meng, Wei; Virkar, Anil V.

1999-12-01

A number of mixed perovskites of the types Ba2B‧B″O6 (BaB‧1/2B″1/2O3) and Ba3B*B″2O9 (BaB*1/3B″2/3O3) where B‧=Gd, La, Nd, Sm, or Y; B″=Nb and B*=Ca were synthesized by a conventional calcination process, as well as by the molten salt method. The former consists of calcining appropriate mixtures of oxide or carbonate precursors in air at elevated temperatures (∼1250°C). The latter method consists of adding appropriate mixtures of oxide or carbonate precursors to a molten salt bath at relatively low temperatures (on the order of 300 to 500°C) so that the requisite compound is formed by dissolution-reprecipitation. X-ray diffraction confirmed the formation of a single-phase perovskite in each case with calcination at 1250°C. In a molten salt bath, however, all except Ba2LaNbO6 and Ba2NdNbO6 formed the perovskite structure. On the contrary, powders of Ba2LaNbO6 and Ba2NdNbO6 formed by a high-temperature calcination process readily decomposed when introduced into the molten salt bath. The formation of the requisite perovskite at a temperature as low as 350°C in a molten salt suggests that: (a) The perovskite is stable at 350°C. (b) The molten salt exhibits sufficient precursor solubility for the dissolution-reprecipitation process to occur in a reasonable time. Similarly, the decomposition of Ba2LaNbO6 and Ba2NdNbO6 in a molten salt bath shows that these materials are thermodynamically unstable at the temperature of the molten salt bath.

Effects of B2O3 content and sintering temperature on crystallization and microstructure of CBS glass-ceramic coatings

NASA Astrophysics Data System (ADS)

Li, Pengyang; Wang, Shubin; Liu, Jianggao; Feng, Mengjie; Yang, Xinwang

2015-11-01

Borosilicate glass-ceramics precursors with varying compositional ratios in the CaO-SiO2-B2O3 (CBS) system were synthesized by sol-gel method. The precursors were calcined at 1200 °C for 2 h to form glass powders. The glass-ceramics were prepared by overlaying glass slurries on the substrates before sintering at different temperatures. The as-prepared glasses and glass-ceramics were characterized by differential scanning calorimetry and X-ray diffraction. The crystallization activation energies (Ec) were calculated using the Kissinger method from DSC results. The morphology and crystallization behavior of the glass-ceramics were monitored by scanning electron microscopy. Both glass transition and crystallization temperatures decreased, however, the metastable zone increased. The Ec values of CBS glasses and glass-ceramics were 254.1, 173.2 and 164.4 kJ/mol with increasing B2O3 content, whereas that of the calcined G3 glass was 104.9 kJ/mol. Finally, the coatings were prepared at a low temperature (700 °C). The crystals that grew on the surface of multilayer coatings demonstrated heterogeneous surface nucleation and crystallization after heat-treatment from 700 °C to 850 °C for 4 h.

Obtention of low oxidation states of copper from Cu 2+-Al 3+ layered double hydroxides containing organic sulfonates in the interlayer

NASA Astrophysics Data System (ADS)

Trujillano, Raquel; Holgado, María Jesús; Rives, Vicente

2009-03-01

A series of hydrotalcite-type compounds containing Cu(II) and Al(III) in the layers, and carbonate or different alkylsulfonates in the interlayer, have been prepared and studied. Calcination of these solids gives rise to formation of metallic copper and Cu 2+ and Cu + oxides or sulfates, depending on the calcination temperature and on the precise nature of the interlayer alkylsulfonate.

Investigation of the influence of vanadium, iron and nickel dopants on the morphology, and crystal structure and photocatalytic properties of titanium dioxide based nanopowders.

PubMed

Shao, Godlisten N; Jeon, Sun-Jeong; Haider, M Salman; Abbass, Nadir; Kim, Hee Taik

2016-07-15

Photoactive V, Fe and Ni doped TiO2 (M-TiO2) nanopowders were synthesized by a modified two-step sol-gel process in the absence of additives. Titanium oxychloride, which is a rarely-used TiO2 precursor was used to yield M-TiO2 photocatalysts with preferential photochemical performance in the presence of natural solar irradiation. The obtained samples were calcined at different calcination temperatures ranging from 450 to 800°C to evaluate the influence of the sintering on the physicochemical properties. The properties of the obtained samples were examined by XRF, XRD, Raman spectroscopy, UV-visible DRS, XPS, nitrogen gas physisorption studies, SEM-EDAX and HRTEM analyses. Structural characterization of the samples revealed the incorporation of these transition metal element into TiO2. It was also depicted that the morphology, crystal structure, optical and photochemical properties of the obtained samples were largely dependent on the calcination temperature and the type of dopant used during the preparation process. The photochemical performance of the samples was investigated in the photodegradation of methylene blue in the presence of natural sunlight. The experimental results indicated that the VT600 sample possessed the highest activity due to its superior properties. This study provides a systematic preparation and selection of the precursor, dopant and calcination temperature that are suitable for the formation of TiO2-based heterogeneous photocatalysts with appealing morphology, crystal structure, optical and photochemical properties for myriad of applications. Copyright © 2016 Elsevier Inc. All rights reserved.

Modified inverse micelle synthesis for mesoporous alumina with a high D4 siloxane adsorption capacity

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhong, Wei; Jiang, Ting; Jafari, Tahereh

In this work, mesoporous aluminas (MAs) with uniform and monomodal pores were fabricated via a modified inverse micelle synthesis method, using a non-polar solvent (to minimize the effect of water content) and short reaction time (for a fast evaporation process). The effects of reaction times (4–8 h), surfactant chain lengths (non-ionic surfactants), and calcination temperatures and hold times (450–600 °C; 1–4 h) on the textural properties of MA were studied. Additionally, the targeted pore sizes of MA were obtained in the range of 3.1–5.4 nm by adjusting the surfactant and reaction time. The surface area and pore volume were controlledmore » by the calcination temperature and hold time while maintaining the thermal stability of the materials. The tuned MA of the large mesopore volume achieved 168 mg/g octamethylcyclotetrasiloxane (D4 siloxane) adsorption capacity, a 32% improvement compared to commercially activated alumina. Finally, after three adsorption recycles, the synthesized MA still maintained approximate 85% of its original adsorption capacity, demonstrating a sustainable adsorption performance and high potential for related industrial applications.« less

Modified inverse micelle synthesis for mesoporous alumina with a high D4 siloxane adsorption capacity

DOE PAGES

Zhong, Wei; Jiang, Ting; Jafari, Tahereh; ...

2016-10-18

In this work, mesoporous aluminas (MAs) with uniform and monomodal pores were fabricated via a modified inverse micelle synthesis method, using a non-polar solvent (to minimize the effect of water content) and short reaction time (for a fast evaporation process). The effects of reaction times (4–8 h), surfactant chain lengths (non-ionic surfactants), and calcination temperatures and hold times (450–600 °C; 1–4 h) on the textural properties of MA were studied. Additionally, the targeted pore sizes of MA were obtained in the range of 3.1–5.4 nm by adjusting the surfactant and reaction time. The surface area and pore volume were controlledmore » by the calcination temperature and hold time while maintaining the thermal stability of the materials. The tuned MA of the large mesopore volume achieved 168 mg/g octamethylcyclotetrasiloxane (D4 siloxane) adsorption capacity, a 32% improvement compared to commercially activated alumina. Finally, after three adsorption recycles, the synthesized MA still maintained approximate 85% of its original adsorption capacity, demonstrating a sustainable adsorption performance and high potential for related industrial applications.« less

Photocatalytic and electrochemical performance of three-Dimensional reduced graphene Oxide/WS2/Mg-doped ZnO composites

NASA Astrophysics Data System (ADS)

Yu, Weiwei; Chen, Xi'an; Mei, Wei; Chen, Chuansheng; Tsang, Yuenhong

2017-04-01

To improve the dispersion of reduced graphene oxide and enhance the photocatalytic property of reduced graphene oxide/Mg-doped ZnO composites (rGMZ), the reduced graphene oxide/WS2/Mg-doped ZnO composites (rGWMZ) were prepared by electrostatic self-assembly and coprecipitation methods. The effects of mass ratio of WS2 nanosheets to reduced graphene oxide (WS2/rGO wt.%) and calcination temperature on the photocatalytic and electrochemical property of rGWMZ composites were investigated. Experimental results showed that the photocatalytic efficiency of rGWMZ composites is three-fold compared with that of rGMZ composites when the WS2/rGO wt.% is 20.8% and calcination temperature is 500 °C, in which the degradation ratio Rhodamin B (RhB) can reach 95% within 15 min under the UV light and 90% within 90 min under simulated solar light. In addition, the rGWMZ show larger capacitance and smaller resistance than rGMZ. The enhancement for photocatalytic activity and electrochemical performance of rGWMZ is ascribed to improving the specific surface area, electrical conductivity and electronic storage capability because of the synergistic effect of rGO and WS2 nanosheets.

Enhanced piezoelectricity and high temperature poling effect in (1-x)Pb(Mg1/3Nb2/3)O3-xPbTiO3 ceramics via an ethylene glycol route

NASA Astrophysics Data System (ADS)

Tailor, H. N.; Ye, Z.-G.

2010-05-01

A solution chemical method utilizing ethylene glycol as solvent has been developed to prepare the ceramics of (1-x)Pb(Mg1/3Nb2/3)O3-xPbTiO3[(1-x)PMN-xPT] from a precursor powder that can be pressed and fired in one step to produce high quality ceramics with excellent piezoelectric properties. The ceramics reach a relative density of up to 97% of the theoretical value after direct calcinations. This high density is achieved without the need of additional sintering after calcination which is usually required in conventional solid state syntheses to produce ceramics. The ceramics exhibit a unipolar piezoelectric coefficient d33 of 848 pC/N, which is one of the highest values for any unmodified/untextured binary systems reported to date. Since the piezoelectric properties depend on composition and electric field, the effect of poling conditions was investigated. A critical temperature limit has been found, above which poling can dramatically impair the piezoelectric properties due to a field-induced increase in the monoclinic phase component around the morphotropic phase boundary.

Effect of microwave-assisted sintering on dielectric properties of CaCu{sub 3}Ti{sub 4}O{sub 12} ceramic

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rani, Suman, E-mail: sumanranigju@gmail.com; Ahlawat, Neetu; Punia, R.

2016-05-23

In this present work, CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) was synthesized by conventional solid-state reaction technique. The synthesis process was carried out in two phases; by conventional process (calcination and sintering at 1080°C for 10 hours) and phase II involves the micro assisted pre sintering of conventionally calcined CCTO for very short soaking time of 30 min at 1080°C in a microwave furnace followed by sintering at 1080°C for 10 hours in conventional furnace. X-ray diffraction (XRD) patterns confirmed the formation of single phase ceramic. Dielectric properties were studied over the frequency range from 50Hz -5MHz at temperatures (273K-343K). It wasmore » observed that pre- microwave sintering enhance the dielectric constant values from 10900 to 11893 and respectively reduces the dielectric loss values from 0.49 to 0.34 at room temperature(1 KHz). CCTO ceramics which are found desirable for many technological applications. The effect is more pronounced at low frequencies of applied electric field.« less

Synthesis and catalytic activity of Birnessite-Type Manganese Oxide synthesized by solvent-free method

NASA Astrophysics Data System (ADS)

Siregar, S. S.; Awaluddin, A.

2018-04-01

Redox reaction between KMnO4 and glucose usingsolvent-free method produces the octahedral layer birnessite-type manganese oxide. The effects of mole ratios, temperatures, and calcinations time on the structures and crystallinity of the oxides were studied throughthe X-ray powder diffraction analysis. The mole ratio of KMnO4/glucose (1:3) produces the purebirnessite with low crystallinity, whereas the mole ratio of KMnO4/glucose (3:1) yields high crystalline birnessite with minor components of hausmannite-type manganese oxide.The increasing of the temperature and calcinations times (300-700 °C and 3-7 h, respectively) willimprove the crystallinity and the purity of the as-synthesized oxide. Further experiments also showed that the as-syntesized octahedral layer birnessite-type manganese oxides have catalytic activity on the degradation of methylene blue (MB) dye with H2O2 as oxidant. The results revealed that the effective degradation could be achieved only in the presence of both the birnessite and H2O2, whereas without the addition of catalyst (H2O2only) or addition of H2O2 (catalyst only), the 3.5% and 15.5% of MB removal were obtained, respectively.

Influences of synthesis methods and modifier addition on the properties of Ni-based catalysts supported on reticulated ceramic foams

NASA Astrophysics Data System (ADS)

Nikolić, Vesna; Kamberović, Željko; Anđić, Zoran; Korać, Marija; Sokić, Miroslav; Maksimović, Vesna

2014-08-01

A method of synthesizing Ni-based catalysts supported on α-Al2O3-based foams was developed. The foams were impregnated with aqueous solutions of metal chlorides under an air atmosphere using an aerosol route. Separate procedures involved calcination to form oxides and drying to obtain chlorides on the foam surface. The synthesized samples were subsequently reduced with hydrogen. With respect to the Ni/Al2O3 catalysts, the chloride reduction route enabled the formation of a Ni coating without agglomerates or cracks. Further research included catalyst modification by the addition of Pd, Cu, and Fe. The influences of the additives on the degree of reduction and on the low-temperature reduction effectiveness (533 and 633 K) were examined and compared for the catalysts obtained from oxides and chlorides. Greater degrees of reduction were achieved with chlorides, whereas Pd was the most effective modifier among those investigated. The reduction process was nearly complete at 533 K in the sample that contained 0.1wt% Pd. A lower reduction temperature was utilized, and the calcination step was avoided, which may enhance the economical and technological aspects of the developed catalyst production method.

The influence of Ca substitution on LaFeO3 nanoparticles in terms of structural and magnetic properties.

PubMed

Lin, Qing; Xu, Jianmei; Yang, Fang; Yang, Xingxing; He, Yun

2018-01-01

The nanocrystalline structure of La 1 -x Ca x FeO 3 was prepared by a sol-gel method involving an auto-combustion process. The incorporation of rare-earths in LaFeO 3 induces strain in magnetic properties, especially in terms of the following parameters: replacement amount, oxygen partial pressure, and calcination temperature. To determine the effects of the amount of Ca 2+ ion doping agent and the calcination temperature on the microstructure, particle morphology, and magnetic properties of LaFeO 3 crystal, we performed the following respective analytical methods: X-ray powder diffraction, Fourier-transform infrared (FT-IR) spectroscopy, scanning electron microscopy, and vibrating sample magnetometer tests. The orthorhombic structure of LaFeO 3 perovskite did not change even when it was doped with Ca 2+ ions, and its space group continued to be Pnma (No.62). FT-IR spectra confirmed that the main band appearing at 568 cm -1 is due to the antisymmetric stretching vibration of Fe-O-Fe bonds in FeO 6 . The introduction of Ca inhibits the growth of grains but the morphology of particles is improved. With an increasing concentration of Ca 2+ ions, magnetic behavior of the samples also witnessed an increasing trend in a proportionate manner. With an increase in calcination temperature, the enclosed area of the magnetic hysteresis curve of the sample reduced remarkably. The growth of nanoparticles can be restrained with an increase of Ca content that is used as doping agent. The magnetic behavior of La 1 -x Ca x FeO 3 tilts towards G-type antiferromagnetism; the magnetic orientation is achieved from the super exchange interaction of Fe 3+ ions with oxygen ions.

Enhanced photocatalytic performance of mesoporous TiO{sub 2} coated SBA-15 nanocomposites fabricated through a novel approach: supercritical deposition aided by liquid-crystal template

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Chen; Lin, Xiao; Li, Youji, E-mail: bcclyj@163.com

2016-03-15

Highlights: • Highly uniform mesoporous TiO{sub 2} nanopartices were coated SBA-15. • MT showed smaller crystallite size, higher hydroxyl content and surface area. • MT/SBA-15 show enhanced photocatalytic activity and high reused activity. • The optimum MT loading rate and calcination temperature were obtained to be 15% and 400 °C, respectively. • Photocatalytic behaviors are discussed in terms of the Langmuir–Hinshelwood model. - Abstract: Mesoporous TiO2 coated SBA-15 (MT@S) nanocomposites were fabricated through supercritical CO{sub 2} deposition aided by liquid-crystal template. The as-prepared samples were characterized by transmission electron microscopy, X-ray photoelectron spectroscopy, diffuse reflectance spectroscopy and so on. Themore » results reveal that MT uniformly deposited onto silica with titania incorporated in SBA-15 channels, showed smaller crystallite size, higher hydroxyl content and surface area than nonporous TiO{sub 2} coated SBA-15 (NT@S) obtained by a similar route without template. With TiO{sub 2} loading ratio of 15 wt% and calcination temperature of 400 °C, 15%MT@S-400 showed the enhanced degradation efficiency for azo dyes (methylene blue, methyl orange, and rhodamine B) and phenol in comparsion with 15%NT@S-400, due to those improved textural and physicochemical properties. Meanwhile, the reused MT@S also showed high photoactivity. Additionally, the effects of MT content and calcination temperature have been examined as operational parameters. Photocatalytic reactions followed pseudo-first-order kinetics and are discussed in terms of the Langmuir–Hinshelwood model.« less

Low temperature synthesis of nano alpha-alumina powder by two-step hydrolysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yan, Ting; Guo, Xiaode, E-mail: guoxiaodenj@sina.com; Zhang, Xiang

Highlights: • The nano α-Al{sub 2}O{sub 3} with good dispersion was prepared by two-step hydrolysis. • α-Al{sub 2}O{sub 3} powders were added as seed particles in the hydrolysis. • This article indicated that the glucose could impel the γ-Al{sub 2}O{sub 3} transformed to α-Al{sub 2}O{sub 3} directly. • This article indicated that the addictive of α-Al{sub 2}O{sub 3} seed could improve the phase transformation rate of γ-Al{sub 2}O{sub 3} to α-Al{sub 2}O{sub 3}. • In this article, the pure α-Al{sub 2}O{sub 3} could be obtained by calcining at 1000 °C for 1.5 h. - Abstract: The ultral fine alpha-alumina powdermore » has been successfully synthesized via two-step hydrolysis of aluminum isopropoxide. Glucose and polyvinyl pyrrolidone were used as surfactants during the appropriate processing step. The alpha-alumina powder was used as seed particles. Several synthesis parameters, such as the amount of seeds, surfactants, and calcination temperature, were studied by X-ray diffraction (XRD), Fourier transform infrared spectra (FTIR), Thermogravimetry-differential scanning calorimetry (TG-DSC), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The experimental results showed that glucose greatly lower the phase transformation temperature of alpha-alumina by impelling the gamma-alumina transformed to alpha-alumina directly, and the seed could improve the phase transformation rate of alpha-alumina, the polyvinylpyrrolidone have an effect on preventing excessive grain growth and agglomeration of alpha-alumina powder. Comparatively well dispersed alpha-alumina powder with particle size less than 50 nm can be synthesized through this method after calcinations at 1000 °C for 2 h.« less

Magnetically separable maghemite/montmorillonite composite as an efficient heterogeneous Fenton-like catalyst for phenol degradation.

PubMed

Jin, Mingjie; Long, Mingce; Su, Hanrui; Pan, Yue; Zhang, Qiuzhuo; Wang, Juan; Zhou, Baoxue; Zhang, Yanwu

2017-01-01

To develop highly efficient and conveniently separable iron containing catalysts is crucial to remove recalcitrant organic pollutants in wastewater through a heterogeneous Fenton-like reaction. A maghemite/montmorillonite composite was synthesized by a coprecipitation and calcination method. The physiochemical properties of catalysts were characterized by XRD, TEM, nitrogen physisorption, thermogravimetric analysis/differential scanning calorimetry (TG/DSC), zeta potential, and magnetite susceptibility measurements. The influence of calcination temperatures and reaction parameters was investigated. The calcined composites retain magnetism because the presence of montmorillonite inhibited the growth of γ-Fe 2 O 3 nanoparticles, as well as their phase transition. The catalytic activities for phenol degradation were significantly enhanced by calcinations, which strengthen the interaction between iron oxides and aluminosilicate framework and result in more negatively charged surface. The composite (73 m 2 /g) calcined at 350 °C had the highest catalytic activities, with more than 99 % phenol reduction after only 35 min reaction at pH 3.6. Simultaneously, this catalyst exhibited high stability, low iron leaching, and magnetically separable ability for consecutive usage, making it promising for the removal of recalcitrant organic pollutants in wastewater.

Calcination of calcium carbonate and blend therefor

DOEpatents

Mallow, William A.; Dziuk, Jr., Jerome J.

1989-01-01

A method for calcination of a calcium carbonate material comprising heating the calcium carbonate material to a temperature and for a time sufficient to calcine the material to the degree desired while in the presence of a catalyst; said catalyst comprising at least one fused salt having the formula MCO.sub.3.CaCO.sub.3.CaO.H.sub.2 O.sub.x, wherein M is an alkali metal and x is 0 to 1 and formed by fusing MCO.sub.3 and CaCO.sub.3 in a molar ratio of about 1:2 to 2:1, and a blend adapted to be heated to CaO comprising a calcium carbonate material and at least one such fused salt.

Synthesis and characterization of binary (CuO)0.6(CeO2)0.4 nanoparticles via a simple heat treatment method

NASA Astrophysics Data System (ADS)

Baqer, Anwar Ali; Matori, Khamirul Amin; Al-Hada, Naif Mohammed; Shaari, Abdul Halim; Kamari, Halimah Mohamed; Saion, Elias; Chyi, Josephine Liew Ying; Abdullah, Che Azurahanim Che

2018-06-01

A binary (CuO)0.6 (CeO2)0.4 nanoparticles were prepared via thermal treatment method, using copper nitrate, cerium nitrate as precursors, PVP as capping agent and de-ionized water as a solvent. The structures, morphology, composition of the element and optical properties of these nanoparticles have been studied under different temperatures using various techniques. The XRD spectrum of the samples at 500 °C and above confirmed the existence of both monoclinic (CuO) and cubic fluorite (CeO2) structures. The findings of FESEM and TEM exhibited the average practical size and agglomeration increment with an elevation in the calcination temperature. The synthesized nanoparticles were also characterized by FTIR, which indicated the formation of binary Cu-O and Ce-O bonds. The EDX analysis was performed to indicate the chemical composition of the sample. The double energy band gaps of (CuO)0.6(CeO2)0.4 reduction with rising calcination temperature, can be referred to the enhancement of the crystallinity of the samples. PL intensity of (CuO)0.6(CeO2)0.4 nanoparticles peaks, which increased with the elevation of the calcination temperature to 800 °C was observed from the PL spectrum; this was due to the increment of the particle size that occurred.

Adsorption of phosphate from seawater on calcined MgMn-layered double hydroxides.

PubMed

Chitrakar, Ramesh; Tezuka, Satoko; Sonoda, Akinari; Sakane, Kohji; Ooi, Kenta; Hirotsu, Takahiro

2005-10-01

Adsorptive properties of MgMn-3-300 (MgMn-type layered double hydroxide with Mg/Mn mole ratio of 3, calcined at 300 degrees C) for phosphate were investigated in phosphate-enriched seawater with a concentration of 0.30 mg-P/dm3. It showed the highest phosphate uptake from the seawater among the inorganic adsorbents studied (hydrotalcite, calcined hydrotalcite, activated magnesia, hydrous aluminum oxide, manganese oxide (delta-MnO2)). The phosphate uptake by MgMn-3-300 reached 7.3 mg-P/g at an adsorbent/solution ratio of 0.05 g/2 dm3. The analyses of the uptakes of other constituents (Na+, K+, Ca(+, Cl-, and SO(2-)4) of seawater showed that the adsorbent had a markedly high selectivity for the adsorption of phosphate ions. Effects of initial phosphate concentration, temperature, pH, and salinity on phosphate uptake were investigated in detail by a batch method. The phosphate uptake increased slightly with an increase in the adsorption temperature. The adsorption isotherm followed Freundlich's equation with constants of logK(F)=1.25 and 1/n=0.65, indicating that it could effectively remove phosphate even from a solution of markedly low phosphate concentration as well as with large numbers of coexisting ions. The pH dependence showed a maximum phosphate uptake around pH 8.5. The pH dependence curve suggested that selective phosphate adsorption progresses mainly by the ion exchange of HPO(2-)4. The study on the effect of salinity suggested the presence of two kinds of adsorption sites in the adsorbent: one nonspecific site with weak interaction and one specific site with strong interaction. The effective desorption of phosphate could be achieved using a mixed solution of 5 M NaCl + 0.1 M NaOH (1 M = 1 mol/dm3), with negligible dissolution of adsorbent. The adsorbent had high chemical stability against the adsorption/desorption cycle; it kept a good phosphate uptake even after the repetition of the seventh cycle.

Experimental study on the effect of calcination on the volcanic ash activity of diatomite

NASA Astrophysics Data System (ADS)

Xiao, Liguang; Pang, Bo

2017-09-01

The volcanic ash activity of diatomite was studied under the conditions of aerobic calcination and vacuum calcination by the combined water rate method, it was characterized by XRD, BET and SEM. The results showed that the volcanic ash activity of diatomite under vacuum conditions was higher than that of aerobic calcination, 600°C vacuum calcination 2h, the combined water rate of diatomite-Ca(OH)2-H2O system was increased from 6.24% to 71.43%, the volcanic ash activity reached the maximum value, the specific surface

Porous acicular mullite obtained by controlled oxidation of waste molybdenum disilicide

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bučevac, Dušan, E-mail: bucevac@vinca.rs; Dapčević, Aleksandra; Maksimović, Vesna

2014-02-01

Highlights: • Waste MoSi{sub 2} heating elements were used as starting material for fabrication of porous acicular mullite. • Calcined MoSi{sub 2} powder was source of SiO{sub 2} and pore former at the same time. • Porous acicular mullite is promising material for filtration of diesel engine exhaust. • Samples with decent mechanical integrity and porosity of more than 60% were fabricated. - Abstract: Porous acicular mullite was fabricated by using waste MoSi{sub 2} heating element and Al{sub 2}O{sub 3}. Careful calcination of the pulverized heating element led to the formation of a mixture of MoO{sub 3} and amorphous SiO{submore » 2}. This mixture was employed as both SiO{sub 2} precursor and pore former. The oxidation of MoSi{sub 2} and mullite formation were studied. The effect of fabrication temperature on phase composition, porosity, grain morphology, and compressive strength of sintered mullite was examined. Pure mullite with porosity of more than 60% and compressive strength of ∼20 MPa was obtained at temperature as low as 1300 °C. The microstructure consisted of elongated, rectangular, prism-like grains which are known to be effective in filtration of diesel engine exhaust. The increase in sintering temperature caused the change of grain morphology and reduction in compressive strength.« less

Study and Fabrication of Super Low-Cost Solar Cell (SLC-SC) Based on Counter Electrode from Animal’s Bone

NASA Astrophysics Data System (ADS)

Fadlilah, D. R.; Fajar, M. N.; Aini, A. N.; Haqqiqi, R. I.; Wirawan, P. R.; Endarko

2018-04-01

The synthesized carbon from bones of chicken, cow, and fish with the calcination temperature at 450 and 600°C have been successfully fabricated for counter electrode in the Super Low-Cost Solar Cell (SLC-LC) based the structure of Dye-Sensitized Solar Cells (DSSC). The main proposed study was to fabricate SLC-SC and investigate the influence of the synthesized carbon from animal’s bone for counter electrode towards to photovoltaic performance of SLC-SC. X-Ray Diffraction and UV-Vis was used to characterize the phase and the optical properties of TiO2 as photoanode in SLC-SC. Meanwhile, the morphology and particle size distribution of the synthesized carbon in counter electrodes were investigated by Scanning Electron Microscopy (SEM) and Particle Size Analyzer (PSA). The results showed that the TiO2 has anatase phase with the absorption wavelength of 300 to 550 nm. The calcination temperature for synthesizing of carbon could affect morphology and particle size distribution. The increasing temperature gave the effect more dense in morphology and increased the particle size of carbon in the counter electrode. Changes in morphology and particle size of carbon give effect to the performance of the SLC-SC where the increased morphology’s compact and particle size make decreased in the performance of the SLC-SC.

In-situ XAFS study for calcination process of Cr catalyst supported on γ-Al2O3 and SiO2

NASA Astrophysics Data System (ADS)

Watanabe, T.; Ikeda, K.; Katayama, M.; Inada, Y.

2016-05-01

The catalytic performance is largely affected by the oxidation state of supported Cr species, and its control changes the activity of Cr catalysts and the selectivity of products. In this study, the calcination process of the supported Cr catalysts on γ-Al2O3 and SiO2 was investigated by in-situ XAFS spectroscopy. The hydrate species was first supported by the impregnation method and was converted to CrO3 via Cr2O3 during the calcination process on both supporting materials. It was found that the temperature to complete the oxidation from Cr2O3 to CrO3 on SiO2 was higher than that on γ-Al2O3. The similarity of the interatomic distance between the surface oxygen atoms of the intermediate Cr2O3 species to that of SiO2 contributes to the stabilization of Cr2O3 on SiO2 during the calcination process.

(Bi, Pb){sub 2}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub x} superconductor and method of making same utilizing sinter-forging

DOEpatents

Chen, N.; Goretta, K.C.; Lanagan, M.T.

1998-10-13

A (BiPb){sub 2}Sr{sub 2}Ca{sub 2}Cu{sub 3}O{sub x}(Bi223) superconductor with high J{sub c}, phase purity, density and mechanical strength is formed from Bi2223 powder which is synthesized from a mixture of Bi{sub 2}O{sub 3}, PbO, SrCO{sub 3}, CaCo{sub 3} and CuO. The mixture is milled, then dried and calcined to synthesize the Bi2223 powder with the desired phase purity. The calcination is performed by heating the dried mixture for 50 hours at 840 C. The partially synthesized powder is then milled for 1--4 hours before calcining further for another 50 hours at 855 C to complete the synthesis. After calcination, the Bi2223 powder is cold pressed to a predetermined density and sinter forged under controlled temperature and time to form a Bi2223 superconductor with the desired superconducting properties. 5 figs.

(Bi, Pb).sub.2, Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x superconductor and method of making same utilizing sinter-forging

DOEpatents

Chen, Nan; Goretta, Kenneth C.; Lanagan, Michael T.

1998-01-01

A (BiPb).sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x (Bi223) superconductor with high J.sub.c, phase purity, density and mechanical strength is formed from Bi2223 powder which is synthesized from a mixture of Bi.sub.2 O.sub.3, PbO, SrCO.sub.3, CaCo.sub.3 and CuO. The mixture is milled, then dried and calcined to synthesize the Bi2223 powder with the desired phase purity. The calcination is performed by heating the dried mixture for 50 hours at 840.degree. C. The partially synthesized powder is then milled for 1-4 hours before calcining further for another 50 hours at 855.degree. C. to complete the synthesis. After calcination, the Bi2223 powder is cold pressed to a predetermined density and sinter forged under controlled temperature and time to form a Bi2223 superconductor with the desired superconducting properties.

Nanograin Ceramic Optical Composite Window

DTIC Science & Technology

2005-07-15

parts are sintered in air at 1100 C̊. Table 1: Carbon content of the calcined Alumina- Zirconia powders analyzed by LECO Calcination Temperature Carbon...estimated particle size of the Alumina and Zirconia powders Material name Surface area (m2/g) Estimated particle size (nm) Alumina 315.7 4.7 Zirconia...200 300 400 500 600 700 800 900 1000 2-Theta - Scale 20 30 40 50 60 70 80 Figure 3: XRD patterns of zirconia powder prepared by sonochemical method

Fluidized bed calciner apparatus

DOEpatents

Owen, Thomas J.; Klem, Jr., Michael J.; Cash, Robert J.

1988-01-01

An apparatus for remotely calcining a slurry or solution feed stream of toxic or hazardous material, such as ammonium diurante slurry or uranyl nitrate solution, is disclosed. The calcining apparatus includes a vertical substantially cylindrical inner shell disposed in a vertical substantially cylindrical outer shell, in which inner shell is disposed a fluidized bed comprising the feed stream material to be calcined and spherical beads to aid in heat transfer. Extending through the outer and inner shells is a feed nozzle for delivering feed material or a cleaning chemical to the beads. Disposed in and extending across the lower portion of the inner shell and upstream of the fluidized bed is a support member for supporting the fluidized bed, the support member having uniform slots for directing uniform gas flow to the fluidized bed from a fluidizing gas orifice disposed upstream of the support member. Disposed in the lower portion of the inner shell are a plurality of internal electric resistance heaters for heating the fluidized bed. Disposed circumferentially about the outside length of the inner shell are a plurality of external heaters for heating the inner shell thereby heating the fluidized bed. Further, connected to the internal and external heaters is a means for maintaining the fluidized bed temperature to within plus or minus approximately 25.degree. C. of a predetermined bed temperature. Disposed about the external heaters is the outer shell for providing radiative heat reflection back to the inner shell.

Preparation of extrusions of bulk mixed oxide compounds with high macroporosity and mechanical strength

DOEpatents

Flytzani-Stephanopoulos, Maria; Jothimurugesan, Kandaswami

1990-01-01

A simple and effective method for producing bulk single and mixed oxide absorbents and catalysts is disclosed. The method yields bulk single oxide and mixed oxide absorbent and catalyst materials which combine a high macroporosity with relatively high surface area and good mechanical strength. The materials are prepared in a pellet form using as starting compounds, calcined powders of the desired composition and physical properties these powders are crushed to broad particle size distribution, and, optionally may be combined with an inorganic clay binder. The necessary amount of water is added to form a paste which is extruded, dried and heat treated to yield and desired extrudate strength. The physical properties of the extruded materials (density, macroporosity and surface area) are substantially the same as the constituent powder is the temperature of the heat treatment of the extrudates is approximately the same as the calcination temperature of the powder. If the former is substantially higher than the latter, the surface area decreases, but the macroporosity of the extrusions remains essentially constant.

Data on calcium oxide and cow bone catalysts used for soybean biodiesel production.

PubMed

Ayodeji, Ayoola A; Blessing, Igho E; Sunday, Fayomi O

2018-06-01

Biodiesel was produced from soybean oil using calcium oxide and cow bone as heterogeneous catalysts, through transesterification process. The soybean oil used was characterized using gas chromatography mass spectrometer (GCMS) and the cow bone catalyst produced was characterized X-ray fluorescence (XRF) spectrometer. The effects of the variation of methanol/oil mole ratio, catalyst concentration and reaction temperature on biodiesel yield during the transesterification of soybean oil were investigated. Reaction time of 3 h and stirring rate of 500 rpm were kept constant. Using Response Optimizer (Minitab 17), the optimum conditions for biodiesel production were established. It was observed that the calcination of cow bone catalyst enhanced its conversion to apatite-CaOH. Also, the results obtained showed that the performance trends of calcined cow bone catalyst and the conventional CaO catalyst were similar.

Optical and dielectric properties of poly(vinyl-alcohol) - Cobalt oxide nanocomposite film

NASA Astrophysics Data System (ADS)

Das, Amit Kumar; Tripathi, Himadri Sekhar; Meikap, Ajit Kumar

2018-04-01

Highly crystalline cobalt oxide (Co3O4) have been synthesized via calcination method. The crystallite size of the nanoparticles is 28.5 nm. Two direct band gap of Co3O4 is observed. The temperature dependent dielectric spectroscopy of PVA-Co3O4 composite film shows ferroelectric behavior. The dielectric constant of the composite film is almost 2.5 times compare to pure PVA at a 1kHz frequency and room temperature. From the Nyquist plot grain and grain boundary effects are identified.

Synthesis of TiO2 Nanoparticle and its phase Transition

NASA Astrophysics Data System (ADS)

Mangrola, M. H.; Joshi, V. G.; Parmar, B. H.

2011-12-01

Here we report the synthesis of titanium dioxide (TiO2) nanoparticles and study of its phase transition from anataze to rutile. Titanium dioxide (TiO2) nanoparticles have been prepared by hydrolysis of Titanium isopropoxide an aqueous solution with constant value of pH 2 and peptizing the resultant suspension gel(white-Blue) and calcinate gel at different temperature. Structures of synthetic samples of TiO2 have been examined by X-ray diffraction (XRD) and scanning electron microscope (SEM). The anatase-rutile transition has been a popular topic due to its interest to scientific and engineering fields. . Here we have seen that the 100 °C calcinate powder consist of anatase fine crystalline phase with a particle size 14 to 15 nm. The prepared TiO2 nanoparticles have uniform size and morphology, and the phase transformation kinetics of obtained material was studied by interpretation of the X-ray diffraction patterns peaks. The phase transform occurred from anatase to rutile at calcinate temperature up to 600 °C. A very fine network texture made from uniform nanoparticles was revealed by scanning electron microscopy (SEM) analyses.

[Preparation and photocatalytic activity of boron doped CeO2/TiO2 mixed oxides].

PubMed

Tang, Xin-hu; Wei, Chao-hai; Liang, Jie-rong; Wang, Bo-guang

2006-07-01

Boron doped CeO2/TiO2 mixed oxides photocatalysts were prepared by adding boric acid and cerous nitrate during the hydrolyzation of titanium trichloride and tetrabutyl titanate. XRD, UV-Vis DRS and XPS techniques were used to characterize the crystalline structure, light absorbing ability and the chemical state of Boron element in the photocatalyst sample. The photocatalytic activities were evaluated by monitoring the degradation of acid red B under UV irradiation. These results indicate that the wavelengths at adsorbing edge are affected by the content of cerous nitrate and the maximum absorption wavelength is about 481 nm when the mole ratio of Ce/Ti is 1.0. For higher dosage of Cerium, the absorbance edge shifts to blue slightly. The prepared photocatalyst is composed of anatase TiO2 and cubic CeO2 when calcined at 500 degrees C. An increase in the calcination temperature transforms the crystalline structure of the titanium oxides from anatase to rutile, and has no obvious influence on crystalline structure of CeO2 but crystallites growth up. The absorbance edge decreases drastically with the increase of calcination temperature. With a view to the stability of photocatalyst and utilization of sun energy, 500 degrees C of calcination temperature is recommended. The XP spectrum for B1s exhibits that only a few boron ions dope into titania and ceria matrix, others exist in B2O3. The photocatalytic activity increases with increase of cerous nitrate dosage, and decreases drastically due to higher dosage (the mol ratio of Ce/Ti > 0.5). After 10 min UV irradiation, 96% of acid red B is degraded completely over photocatalyst under optimum reaction condition.

Titanium dioxide-based carbon monoxide gas sensors: Effects of crystallinity and chemistry on sensitivity

NASA Astrophysics Data System (ADS)

Seeley, Zachary Mark

Among metal-oxide gas sensors which change electrical resistive properties upon exposure to target gasses, titanium dioxide (TiO2) has received attention for its sensitivity and stability during high temperature (>500°C) operation. However, due to the sensing mechanism sensitivity, selectivity, and stability remain as critical deficiencies to be resolved before these sensors reach commercial use. In this study, TiO2 thick films of approximately 30mum and thin films of approximately 1mum thick were fabricated to assess the influence of their material properties on gas sensing mechanism. Increased calcination temperature of TiO2 thick films led to grain growth, reduction in specific surface area, and particle-particle necking. These properties are known to degrade sensitivity; however the measured carbon monoxide (CO) gas response improved with increasing calcination temperature up to 800°C. It was concluded that the sensing improvement was due to increased crystallinity within the films. Sensing properties of TiO2 thin films of were also dependent on crystallization, however; due to the smaller volume of material, they reached optimized crystallization at lower temperatures of 650°C, compared to 800°C for thick films. Incorporation of tungsten (W) and nickel (Ni) ions into the films created donor and acceptor defect sites, respectively, within the electronic band gap of TiO2. The additional n-type defects in W-doped TiO 2 improved n-type CO response, while p-type defects in Ni-doped TiO 2 converted the gas response to p-type. Chemistry of thin films had a more significant impact on the electrical properties and gas response than did microstructure or crystallinity. Doped films could be calcined at higher temperatures and yet remain highly sensitive to CO. Thin films with p-n bi-layer structure were fabricated to determine the influence of a p-n junction on gas sensing properties. No effect of the junction was observed and the sensing response neared the average of the layers; however, electrical and gas response studies revealed that the majority of the conductivity and gas-surface reactions took place on the outer layer of the film. Further research is necessary to understand the influence of p-n junctions on the gas sensing behavior.

[Preparation and photoluminescence study of Er3+ : Y2O3 transparent ceramics].

PubMed

Luo, Jun-ming; Li, Yong-xiu; Deng, Li-ping

2008-10-01

Y2O3 acted as the matrix material, which was doped with different concentrations of Er3+, Er3+ : Y2O3 nanocrystalline powder was prepared by co-precipitation method, and Er3+ : Y2O3 transparent ceramics was fabricated by vacuum sintering at 1700 degrees C, 1 x 10(-3) Pa for 8 h. By using the X-ray diffraction (D/MAX-RB), transmission electron microscopy(Philips EM420), automatic logging spectrophotometer(DMR-22), fluorescence analyzer (F-4500) and 980 nm diode laser, the structural, morphological and luminescence properties of the sample were investigated. The results show that Er3+ dissolved completely in the Y2O3 cubic phase, the precursor was amorphous, weak diffraction peaks appeared after calcination at 400 degrees C, and if calcined at 700 degrees C, the precursor turned to pure cubic phase. With increasing the calcining temperature, the diffraction peaks became sharp quickly, and when the calcining temperature reached 1100 degrees C, the diffraction peaks became very sharp, indicating that the grains were very large. The particles of Er+ : Y2O3 is homogeneous and nearly spherical, the average diameter of the particles is in the range of 40-60 nm after being calcined at 1000 degrees C for 2 h. The relative density of Er3+ : Y2O3 transparent ceramics is 99.8%, the transmittance of the Er2+ : Y2O3 transparent ceramics is markedly lower than the single crystal at the short wavelength, but the transmittance is improved noticeably with increasing the wavelength, and the transmittance exceeds 60% at the wavelength of 1200 nm. Excited under the 980 nm diode laser, there are two main up-conversion emission bands, green emission centers at 562 nm and red emission centers at 660 nm, which correspond to (4)S(3/2) / (2)H(11/2) - (4)I(15/2) and (4)F(9/2) - (4)I(15/2) radiative transitions respectively. By changing the doping concentrations of Er3+, the color of up-conversion luminescence can be tuned from green to red gradually. The luminescence intensity is not reinforce with the increase in the concentration, so the doping concentration of Er3+ should not exceed 2%. If the doping concentration of Er3+ exceeds the range, the concentration has very small effect on the improvement of luminescence intensity.

Preparation and properties of calcium oxide from eggshells via calcination

NASA Astrophysics Data System (ADS)

Tangboriboon, N.; Kunanuruksapong, R.; Sirivat, A.

2012-12-01

Duck eggs are one of the most versatile cooking ingredients in which residue eggshells are discarded. Raw duck eggshells were calcined at temperatures between 300 to 900 °C, for 1, 3, and 5 h. Both the raw and calcined duck eggshells were characterized by FTIR, STA, XRD, XRF, TEM, BET, a particle size analyzer, and an impedance analyzer. The proper calcination conditions are: 900 °C and 1 h, yielding calcium oxide with a purity of 99.06 % w/w. The calcium carbonate of the rhombohedral form (CaCO3) transforms completely into the calcium oxide or lime of the face centered cubic form (CaO) at 900 °C, as shown by XRD diffraction patterns. The transmission electron microscopy (TEM) images of the calcium oxide reveal a moderately good dispersion of nearly uniform particles. The calcium oxide has a white color, a spherical shape, high porosity, and narrow particles size distribution. The percentage of ceramic yield of the calcium oxide is 53.53, as measured by STA (TG-DTA-DTG). The calcium oxide has a N2 adsorption-desorption isotherm indicating the meso-porosity range. The dielectric constant and the electrical conductivity of the calcined calcium oxide are 35 and 1:0×10-6(Ω·m)-1, respectively, at the frequency of 500 Hz.

Effects of TiO2 crystal structure on the luminescence quenching of [Ru(bpy)2(dppz)]2 +-intercalated into DNA

NASA Astrophysics Data System (ADS)

Chen, Linlin; Wang, Yi; Huang, Minggao; Li, Xiaodan; Zhu, Licai; Li, Hong

2017-06-01

The intercalation of [Ru(bpy)2(dppz)]2 + labeled as Ru(II) (bpy = 2,2‧-bipyridine and dppz = dipyrido[3,2,-a:2‧,3‧-c]phenazine) into herring sperm DNA leads to the formation of emissive Ru(II)-DNA dyads, which can be quenched by TiO2 nanoparticles (NPs) and sol-gel silica matrices at heterogeneous interfaces. The calcinations temperature exhibits a remarkable influence on the luminescence quenching of the Ru(II)-DNA dyads by TiO2 NPs. With increasing calcinations temperature in the range from 200 to 850 °C, the anatase-to-rutile TiO2 crystal structure transformation increases the average particle size and hydrodynamic diameter of TiO2 and DNA@TiO2. The anatase TiO2 has the stronger ability to unbind the Ru(II)-DNA dyads than the rutile TiO2 at room temperature. The TiO2 NPs and sol-gel silica matrices can quench the luminescence of the Ru(II) complex intercalated into DNA by selectively capturing the negatively DNA and positively charged Ru(II) complex to unbind the dyads, respectively. This present results provide new insights into the luminescence quenching and competitive binding of dye-labeled DNA dyads by inorganic NPs.

Bioactive glasses containing Au nanoparticles. Effect of calcination temperature on structure, morphology, and surface properties.

PubMed

Lusvardi, Gigliola; Malavasi, Gianluca; Aina, Valentina; Bertinetti, Luca; Cerrato, Giuseppina; Magnacca, Giuliana; Morterra, Claudio; Menabue, Ledi

2010-06-15

Bioactive glasses containing gold nanoparticles (AuNPs) have been synthesized via the sol-gel route using HAuCl(4) x 3 H(2)O as gold precursor. The formation process of AuNPs was studied as a function of the thermal treatment, which induces nucleation of Au particles and influences their nature, optical properties, shape, size, and distribution. The physicochemical characterization indicates that the sample treated at 600 degrees C presents the best characteristics to be used as a bioactive material, namely high surface area, high amount of AuNPs located at the glass surface, presence of micropores, and abundant surface OH groups. In the case of samples either aged at 60 degrees C or calcined at 150 degrees C, AuNPs just begin their formation, and at this stage the gel is not completely polymerized and dried yet. A thermal treatment at higher temperatures (900 degrees C) causes the aggregation of AuNPs, forming "AuMPs" (i.e., Au microparticles) in a densified glass-ceramic material with low surface area, absence of pores, and low number of surface OH groups. These features induce in the glass-ceramic materials treated at high-temperatures a lower bioactivity (evidenced by SBF reaction), as compared with that exhibited by the glass samples treated at 600 degrees C.

Synthesis, photoelectrochemical properties and solar light-induced photocatalytic activity of bismuth ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Pattnaik, Sambhu Prasad; Behera, Arjun; Martha, Satyabadi; Acharya, Rashmi; Parida, Kulamani

2018-01-01

Bismuth ferrite (BFO) nanoparticles prepared by solid state reaction route were characterized by various characterization techniques such as XRD, FESEM, HRTEM, UV-Vis DRS, PL etc., and their photocatalytic activities were evaluated by decolorization of aqueous solution of Congo red (CR) under solar light. The photocatalytic activity of BFO was increased by increasing the preparation temperature from 350 to 500 °C and then decreased with rise in temperature. The results of electrochemical measurements such as linear sweep voltammetry (LSV), electrochemical impedence (EIS), and Mott-Schottky analysis of BFO nanoparticles corroborated the findings of their photocatalytic activity. The enhanced photocatalytic response of the sample prepared at 500 °C is attributed to its smallest band gap, minimum crystallite size (30 nm), efficient separation, and lowest possible recombination of photo-generated charge carriers. The effects of amount of nano-BFO, irradiation time, initial CR concentration, and BFO calcination temperature on the decolorization of CR were examined. It was observed that 1 g/L nano-BFO calcined at 500 °C can decolorize up to 77% a 10-ppm CR dye solution under solar irradiation for 60 min. The studies included scavenger tests for identification of reactive species and a possible mechanism of dye decolorization.

Low-temperature growth of nitrogen-doped carbon nanofibers by acetonitrile catalytic CVD using Ni-based catalysts

NASA Astrophysics Data System (ADS)

Iwasaki, Tomohiro; Makino, Yuri; Fukukawa, Makoto; Nakamura, Hideya; Watano, Satoru

2016-11-01

To synthesize nitrogen-doped carbon nanofibers (N-CNFs) at high growth rates and low temperatures less than 673 K, nickel species (metallic nickel and nickel oxide) supported on alumina particles were used as the catalysts for an acetonitrile catalytic chemical vapor deposition (CVD) process. The nickel:alumina mass ratio in the catalysts was fixed at 0.05:1. The catalyst precursors were prepared from various nickel salts (nitrate, chloride, sulfate, acetate, and lactate) and then calcined at 1073 K for 1 h in oxidative (air), reductive (hydrogen-containing argon), or inert (pure argon) atmospheres to activate the nickel-based catalysts. The effects of precursors and calcination atmosphere on the catalyst activity at low temperatures were studied. We found that the catalysts derived from nickel nitrate had relatively small crystallite sizes of nickel species and provided N-CNFs at high growth rates of 57 ± 4 g-CNF/g-Ni/h at 673 K in the CVD process using 10 vol% hydrogen-containing argon as the carrier gas of acetonitrile vapor, which were approximately 4 times larger than that of a conventional CVD process. The obtained results reveal that nitrate ions in the catalyst precursor and hydrogen in the carrier gas can contribute effectively to the activation of catalysts in low-temperature CVD. The fiber diameter and nitrogen content of N-CNFs synthesized at high growth rates were several tens of nanometers and 3.5 ± 0.3 at.%, respectively. Our catalysts and CVD process may lead to cost reductions in the production of N-CNFs.

Synthesis of highly efficient α-Fe{sub 2}O{sub 3} catalysts for CO oxidation derived from MIL-100(Fe)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cui, Lifeng; Zhao, Di; Yang, Yang

Mesoporous hollow α-Fe{sub 2}O{sub 3} bricks were synthesized via a hydrothermal method to create a precursor MIL-100(Fe) and a subsequent calcination process was applied to prepare the Fe{sub 2}O{sub 3} phase. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) results showed the morphology of hollow α-Fe{sub 2}O{sub 3} bricks which inherited from the MIL-100(Fe) template. The catalytic activities of hollow α-Fe{sub 2}O{sub 3} bricks for CO oxidation are studied in this work. Due to better low temperature reduction behavior, mesoporous hollow α-Fe{sub 2}O{sub 3} bricks obtained at calcination temperature of 430 °C displayed high catalytic activity and excellent stabilitymore » with a complete CO conversion temperature (T{sub 100}) of 255 °C. - Graphical abstract: Synthesis of highly efficient α-Fe{sub 2}O{sub 3} catalysts for CO oxidation derived from MIL-100(Fe). - Highlights: • α-Fe{sub 2}O{sub 3} is prepared by the thermolysis of a MIL-100(Fe) template. • The morphology of hollow α-Fe{sub 2}O{sub 3} bricks is inherited from MIL-100(Fe) template. • α-Fe{sub 2}O{sub 3} obtained at calcined temperature of 430 °C displays high activity • Enhanced activity is attributed to crystal plane and reduction behavior.« less

Two-step oxalate approach for the preparation of high performance LiNi0.5Mn1.5O4 cathode material with high voltage

NASA Astrophysics Data System (ADS)

Liu, Zushan; Jiang, Yangmei; Zeng, Xiaoyuan; Xiao, Guan; Song, Huiyu; Liao, Shijun

2014-02-01

A high voltage cathode material, LiNi0.5Mn1.5O4, is synthesized with a two-step approach, in which the nickel-manganese oxalate precipitate is firstly obtained by adding oxalic acid to the solution of nickel and manganese ions precursors, followed by calcining the oxalates to obtain spinel nickel-manganese oxide, incorporating lithium ions with ball milling and calcining at 900 °C for 15 h. The materials are characterized with TG, XRD, SEM, BET and FTIR; it is revealed that both nickel-manganese oxide and final LiNi0.5Mn1.5O4 have well defined spinel structure. The LiNi0.5Mn1.5O4 spinel materials exhibit high capacities and good cyclic stability, the capacity of the materials is in the range from 126 to 136 mAh -1, depending on the calcining temperatures. The sample calcined at an optimal temperature of 900 °C exhibits best performance, the capacity is high up to 136 mAh g-1 at tenth cycle and the capacity retention after 50 cycles is 93%. For the sample prepared by mixing and milling oxalate with lithium salt, the discharge capacity is only 115 mAh g-1. We suggest that the spinel oxide derived from oxalate may play an important role for the high performance and high stability of the final cathode materials.

TiO2-V2O5 nanocomposites as alternative energy storage substances for photocatalysts.

PubMed

Ngaotrakanwiwat, Pailin; Meeyoo, Vissanu

2012-01-01

TiO2-V2O5 was prepared and evaluated as an energy storage material for photocatalysts with high capacity and initial charging rate. The compound was successfully obtained by sol-gel technique and effects of compound composition and calcination temperature on the energy storage ability were investigated. The synthesized compounds were characterized by means of X-ray powder diffraction (XRD), scanning electron microscopy equipped with energy-dispersive X-ray analysis (SEM-EDX) and transmission electron microscopy (TEM). The results reveals that the compound of Ti:V molar ratio equal to 1:0.11 calcined at 550 degrees C exhibited superior energy storage ability than parent substances and 1.7-times higher capacity and 2.3-times higher initial charging rate compared to WO3, indicating that the compound is a remarkable alternative to conventional energy storage substances.

The influence of coating solution and calcination condition on the durability of Ir1-xSnxO2/Ti anodes for oxygen evolution

NASA Astrophysics Data System (ADS)

Kato, Zenta; Kashima, Ryo; Tatsumi, Kohei; Fukuyama, Shinnosuke; Izumiya, Koichi; Kumagai, Naokazu; Hashimoto, Koji

2016-12-01

For oxygen formation without forming chlorine in seawater electrolysis for hydrogen production we have been using the anode consisting of three layers of MnO2-type multiple oxide catalyst, intermediate layer and titanium substrate. The intermediate layer was used for prevention of oxidation of the titanium substrate during anodic polarization for oxygen evolution and was prepared by calcination of butanol solutions of H2IrCl6 and SnCl4 coated on titanium. The protectiveness of Ir1-xSnxO2 layer formed was directly examined using Ir1-xSnxO2/Ti anodes in H2SO4 solution changing the preparation conditions of the layer. When the sum of Ir4+ and Sn4+ was 0.1 M, the highest protectiveness was observed at 0.06 M Sn4+. Although an increase in calcination temperature led to the formation of Ir1-x-ySnxTiyO2 triple oxide with a slightly lower catalytic activity for oxygen evolution, the anode calcined at 450 °C showed the highest protectiveness.

Photoemission and energy gap of MgWO4 particles connecting as nanofibers synthesized by electrospinning-calcination combinations

NASA Astrophysics Data System (ADS)

Wannapop, Surangkana; Thongtem, Titipun; Thongtem, Somchai

2012-03-01

Mixtures of magnesium acetate tetrahydrate ((CH3COO)2Mg·4H2O), ammonium tungstate tetrahydrate ((NH4)6W7O24·4H2O), and poly(vinyl alcohol) with the molecular weight of 72,000 were electrospun through a +15 kV direct voltage to form fibers on ground flat aluminum foils. The electrospun fibers of 1.5, 3.0, and 4.5 mmol of each starting material containing 1.3 g poly(vinyl alcohol) were further calcined at 500-700 °C for 3 h constant length of time. At 500 and 600 °C calcination, both monoclinic and anorthic phases of MgWO4 particles with different sizes connecting as fibrous assemblies were detected. Upon increasing the calcination temperature to 700 °C, only monoclinic phase of facet nanoparticles interconnecting along the fibrous axes with 4.19 eV indirect band gap and 461 nm photoemission was synthesized. In the present research, formation of MgWO4 molecules as well as nucleation and growth of nanoparticles was also proposed.

Effects of graphene oxide concentration on optical properties of ZnO/RGO nanocomposites and their application to photocurrent generation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Azarang, Majid, E-mail: azarangmajid@gmail.com, E-mail: azarang@phys.usb.ac.ir; Department of Physics, University of Sistan and Baluchestan, 98135-674 Zahedan; Shuhaimi, Ahmad

2014-08-28

The effects of different concentrations of graphene oxide (GO) on the structure and optical properties of ZnO nanoparticles (NPs) were investigated. The nanocomposites were synthesized via the sol-gel method in a gelatin medium. X-ray diffraction patterns (XRD) and Fourier transform infrared spectroscopy indicated that the GO sheets were reduced and changed to reduced GO (RGO) during the calcination of the nanocomposites at 400 °C. In addition, the XRD patterns of the NPs indicated a hexagonal (wurtzite) structure for all the products. Microscopic studies showed that the NPs were decorated and dispersed on the RGO sheets very well. However, these studies revealedmore » that the RGO concentration had an effect on the crystal growth process for the ZnO NPs. Furthermore, these studies showed that the NPs could be grown with a single crystal quality in an optimum RGO concentration. According to the XRD results that were obtained from pure ZnO NPs, the calcinations temperature was decreased by the RGO. UV–vis and room temperature photoluminescence studies showed that the optical properties of the ZnO/RGO nanocomposite were affected by the RGO concentration. Finally, the obtained ZnO/RGO nanocomposite was used to generate a photocurrent. Observations showed that the photocurrent intensity of the nanocomposite was significantly increased by increasing the RGO, with an optimum RGO concentration.« less

Toward Stabilizing Co 3O 4 Nanoparticles as an Oxygen Reduction Reaction Catalyst for Intermediate-Temperature SOFCs

DOE PAGES

Ren, Yaoyu; Cheng, Yuan; Gorte, Raymond J.; ...

2017-04-05

The oxygen reduction reaction (ORR) activity of a series of composite cathodes consisting of a porous Gd 0.20Ce 0.80O 2-δ (GDC) scaffold infiltrated with Sr-, Co-, and Y-nitrate solutions has been systematically investigated in this study. The results show that such infiltrated cathodes if calcined at low temperatures such as 350°C exhibit low polarization resistance (RP) in the temperature range of 450–700°C, even though XRD analysis reveals that the calcined product is virtually a mixture of Co 3O 4 and SrCO 3. A further study by design-of-experiment suggests that the true ORR-active species is Co 3O 4, whereas SrCO 3more » serves as a sintering inhibitor to preserve the high surface area of Co 3O 4. The findings and understanding in this study present a new strategy for future development of active cathodes for intermediate-temperature solid oxide fuel cells (SOFCs).« less

Low temperature synthesis & characterization of lead-free BCZT ceramics using molten salt method

NASA Astrophysics Data System (ADS)

Jai Shree, K.; Chandrakala, E.; Das, Dibakar

2018-04-01

Piezoelectric properties are greatly influenced by the synthesis route, microstructure, stoichiometry of the chemical composition, purity of the starting materials. In this study, molten salt method was used to prepare lead-free BCZT ceramics. Molten salt method is one of the simplestmethods to prepare chemically-purified, single phase powders in high yield often at lower temperatures and shorten reaction time. Calcination of the molten salt synthesized powders resulted in asingle-phase perovskite structure at 1000 °C which is ˜ 350 °C less than the conventional solid-sate reaction method. With increasing calcination temperature the average template size was increased (˜ 0.5-2 µm). Formation of well dispersive templates improves the sinterability at lower temperatures. Lead-free BCZT ceramics sintered at 1500 °C for 2 h resulted in homogenous and highly dense microstructure with ˜92% of the theoretical density and a grain size of ˜ 35 µm. This highly dense microstructure could enhance the piezoelectric properties of the system.

Toward Stabilizing Co 3O 4 Nanoparticles as an Oxygen Reduction Reaction Catalyst for Intermediate-Temperature SOFCs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ren, Yaoyu; Cheng, Yuan; Gorte, Raymond J.

The oxygen reduction reaction (ORR) activity of a series of composite cathodes consisting of a porous Gd 0.20Ce 0.80O 2-δ (GDC) scaffold infiltrated with Sr-, Co-, and Y-nitrate solutions has been systematically investigated in this study. The results show that such infiltrated cathodes if calcined at low temperatures such as 350°C exhibit low polarization resistance (RP) in the temperature range of 450–700°C, even though XRD analysis reveals that the calcined product is virtually a mixture of Co 3O 4 and SrCO 3. A further study by design-of-experiment suggests that the true ORR-active species is Co 3O 4, whereas SrCO 3more » serves as a sintering inhibitor to preserve the high surface area of Co 3O 4. The findings and understanding in this study present a new strategy for future development of active cathodes for intermediate-temperature solid oxide fuel cells (SOFCs).« less

Photocatalytic characteristic and photodegradation kinetics of toluene using N-doped TiO2 modified by radio frequency plasma.

PubMed

Shie, Je-Lueng; Lee, Chiu-Hsuan; Chiou, Chyow-San; Chen, Yi-Hung; Chang, Ching-Yuan

2014-01-01

This study investigates the feasibility of applications of the plasma surface modification of photocatalysts and the removal of toluene from indoor environments. N-doped TiO2 is prepared by precipitation methods and calcined using a muffle furnace (MF) and modified by radio frequency plasma (RF) at different temperatures with light sources from a visible light lamp (VLL), a white light-emitting diode (WLED) and an ultraviolet light-emitting diode (UVLED). The operation parameters and influential factors are addressed and prepared for characteristic analysis and photo-decomposition examination. Furthermore, related kinetic models are established and used to simulate the experimental data. The characteristic analysis results show that the RF plasma-calcination method enhanced the Brunauer Emmett Teller surface area of the modified photocatalysts effectively. For the elemental analysis, the mass percentages of N for the RF-modified photocatalyst are larger than those of MF by six times. The aerodynamic diameters of the RF-modifiedphotocatalyst are all smaller than those of MF. Photocatalytic decompositions of toluene are elucidated according to the Langmuir-Hinshelwood model. Decomposition efficiencies (eta) of toluene for RF-calcined methods are all higher than those of commercial TiO2 (P25). Reaction kinetics ofphoto-decomposition reactions using RF-calcined methods with WLED are proposed. A comparison of the simulation results with experimental data is also made and indicates good agreement. All the results provide useful information and design specifications. Thus, this study shows the feasibility and potential use of plasma modification via LED in photocatalysis.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zheng Jun; Liu Jing; Lv Dongping

The porous hierarchical spherical Co{sub 3}O{sub 4} assembled by nanosheets have been successfully fabricated. The porosity and the particle size of the product can be controlled by simply altering calcination temperature. SEM, TEM and SAED were performed to confirm that mesoporous Co{sub 3}O{sub 4} nanostructures are built-up by numerous nanoparticles with random attachment. The BET specific surface area and pore size of the product calcined at 280 deg. C are 72.5 m{sup 2} g{sup -1} and 4.6 nm, respectively. Our experiments further demonstrated that electrochemical performances of the synthesized products working as an anode material of lithium-ion battery are stronglymore » dependent on the porosity. - Graphical abstract: The flower-like Co{sub 3}O{sub 4} porous spheres with hierarchical structure have been successfully prepared via a simple calcination process using cobalt hydroxide as precursor.« less

Preparation and application of zirconium sulfate supported on SAPO-34 molecular sieve as solid acid catalyst for esterification

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xu, Dongyan, E-mail: xdy0156@sina.com; Ma, Hong; Cheng, Fei

2014-05-01

Graphical abstract: - Highlights: • SAPO-34 supported zirconium sulfate solid acid catalyst was prepared. • Esterification of acetic acid with ethanol can be catalyzed by ZS/SAPO-34. • The hydration of ZS is vital to the acidic property and catalytic performance. • The ZS/SAPO-34 catalyst treated at 200 °C shows good reusability. - Abstract: Zirconium sulfate (ZS) was supported on SAPO-34 molecular sieve by using an incipient wetness impregnation method with zirconium sulfate as the precursor. The as-prepared catalysts were used as solid acid catalyst for esterification reaction of acetic acid with ethanol. The influence of calcination temperature on the acidicmore » property, catalytic activity, and reusability of ZS/SAPO-34 catalysts were mainly investigated. FT-IR, SEM, EDS and TG analysis have been carried out to demonstrate the characteristics of ZS/SAPO-34 catalysts. It was found that the 30 wt%ZS/SAPO-34 catalysts display the property of superacid irrespective of calcination temperature. The ZS/SAPO-34 catalyst treated at 200 °C can enhance the interaction between the supported ZS and SAPO-34 and keep the catalyst remaining substantially active after several reaction cycles. However, further increasing calcination temperature will cause the transfer of ZS from hydrate to anhydrous phase, and thus the decrease of activity.« less

Understanding microstrain anisotropy in yttrium oxide synthesized by sol-gel route

NASA Astrophysics Data System (ADS)

Murugesan, S.; Thirumurugesan, R.; Parameswaran, P.

2018-04-01

Yttrium oxide was synthesized by wet chemical route and calcined at various temperatures. On x-ray diffraction analysis of the material using Williamson-Hall analysis followed by Rietveld analysis indicates that the powder exists in nano crystallite size with lattice strain. The spherical harmonics analysis model of microstrain indicates the presence of strain anisotropy. The change in crystal structure lattice parameter, atomic coordinates of Y, O in yttria and the bond length analysis of the calcined powder reveals the presence of oxygen vacancies in the system.

Impact of support calcination and competitive adsorbate in Fe/Mo-Al2O3 catalyst for synthesis of carbon nanotubes by V-flame

NASA Astrophysics Data System (ADS)

Sun, Ya-Ping; Sun, Bao-Min; Zhai, Gang; Guo, Yong-Hong; Jia, Xiao-Wei; Kang, Zhi-Zhong

2018-05-01

Carbon nanotubes (CNTs) were synthesized via carbon monoxide decomposition with aid of various Fe/Mo-Al2O3 catalysts by V-type flame method. The influences of support calcination and competitive adsorbates on the morphology and properties of CNTs were studied. SEM, HRTEM, TPO and Raman spectroscopy were applied to investigate the morphology and microstructure of CNT products. XRD, H2-TPR were employed to characterize catalysts. The obtained results indicate that calcinated support can increase production and promote the formation of CNTs with small diameter. Utilizing citric acid as a competitive adsorbate is successful in improving the quality of CNTs. Besides, the addition of citric acid and calcinated support in catalyst enhances the catalytic growth activity. The obtained CNTs have a diameter around 4–6 nm within a narrow diameter distribution range. Raman spectrum analysis also illustrates that highly graphitized CNTs are produced on the catalyst with calcinated support and citric acid. These results suggest that support calcination and competitive adsorbate have pronounced effect on the average diameter, diameter distribution, and graphitization of CNTs, which provides a simple and effective way to tune the properties of CNTs.

Synthesis of strontium hexaferrite nanoparticles prepared using co-precipitation method and microemulsion processing

NASA Astrophysics Data System (ADS)

Drmota, A.; Žnidaršič, A.; Košak, A.

2010-01-01

Strontium hexaferrite (SrFe12O19) nanoparticles have been prepared with co-precipitation in aqueous solutions and precipitation in microemulsion system water/SDS/n-butanol/cyclohexane, using iron and strontium nitrates in different molar rations as a starting materials. The mixed Sr2+, Fe3+ hydroxide precursors obtained during the reaction between corresponding metal nitrates and tetramethylammonium hydroxide (TMAH), which served as a precipitating reagent, were calcined in a wide temperature range, from 350 °C to 1000 °C in a static air atmosphere. The influence of the Sr2+/Fe3+ molar ratio and the calcination temperature to the chemistry of the product formation, its crystallite size, morphology and magnetic properties were investigated. It was found that the formation of single phase SrFe12O19 with relatively high specific magnetization (54 Am2/kg) was achieved at the Sr2+/Fe3+ molar ration of 6.4 and calcination at 800 °C for 3h with heating/cooling rate 5 °C/min. The prepared powders were characterized using X-ray diffractometry (XRD) and specific surface area measurements (BET). The specific magnetization (DSM-10, magneto-susceptometer) of the prepared samples was measured.

Preparation and photocatalytic performance of fibrous Tb3+-doped TiO2 using collagen fiber as template

NASA Astrophysics Data System (ADS)

Luo, Ting; Wan, Xiang-Jun; Jiang, Shang-Xuan; Zhang, Li-Yuan; Hong, Zheng-Qu; Liu, Jiao

2018-04-01

Fibrous Tb3+-doped TiO2 were prepared using collagen fiber as template. Morphology, crystalline structure, surface area, element content, chemical composition and elemental chemical status, microstructure and element distribution of the prepared samples were characterized by using scanning electron microscopy, X-ray diffraction, specific surface area analysis, inductively coupled plasma atomic emission spectrometer, X-ray photoelectron spectroscopy, transmission electron microscope and element mapping, respectively. The photocatalytic activities were evaluated by following degradation of methyl orange. The results showed that the fiber structure of collagen template was fully preserved when the calcination temperature was 500-800 °C. However, with the increase of calcination temperature, crystallinity and average particle size were increased, and the photocatalytic performance was decreased. For 2% Tb3+-TiO2 calcined at 500 °C, the degradation rate of methyl orange reached 93.87% after 6 h when a high-pressure mercury lamp (150 W) was used as the light source for photocatalytic degradation. Titanium tanning agent performance was excellent, the yield of TiO2 was high, and the fiber structure was presented when 0.2 mol/L citric acid/sodium citrate buffer solution was used.

Fabrication of Tb3Al5O12 transparent ceramics using co-precipitated nanopowders

NASA Astrophysics Data System (ADS)

Dai, Jiawei; Pan, Yubai; Wang, Wei; Luo, Wei; Xie, Tengfei; Kou, Huamin; Li, Jiang

2017-11-01

Terbium aluminum garnet (TAG) precursor was synthesized by a co-precipitation method from a mixed solution of terbium and aluminum nitrates using ammonium hydrogen carbonate (AHC) as the precipitant. The powders calcined at different temperatures were investigated by XRD, FTIR and FESEM in order to choose the optimal calcination temperature. Fine and low-agglomerated TAG powders with average particle size of 88 nm were obtained by calcining the precursor at 1100 °C for 4 h. Using this powder as starting material, TAG transparent ceramics were fabricated by vacuum sintering combined with hot isostatic pressing (HIP) sintering. For the sample pre-sintered at 1700 °C for 20 h with HIP post-treated at 1700 °C for 3 h, the average grain size is about 3.9 μm and the in-line transmittance is beyond 55% in the region of 500-1600 nm, reaching a maximum transmittance of 64.2% at the wavelength of 1450 nm. The Verdet constant at 633 nm is measured to be -178.9 rad T-1 m-1, which is 33% larger than that of the commercial TGG single crystal (-134 rad T-1 m-1).

Development of high T(sub c) (greater than 110 K) Bi, Tl, and Y-based materials as superconducting circuit elements

NASA Technical Reports Server (NTRS)

Haertling, Gene H.; Grabert, Gregory; Gilmour, Phillip

1992-01-01

Experimental work has continued on the development and characterization of bulk and hot pressed powders and tapecast materials in the Bi-Sr-Ca-Cu-O and Tl-Ba-Ca-Cu-O systems. A process for producing warp-free, sintered, superconducting tapes of Bi composition Bi2Sr2Ca2Cu3O(x) with a mixed oxide process was established. This procedure required a triple calcination at 830 C for 24 hours and sintering at 845 C from 20 to 200 hours. Hot pressing the triple calcined powder at 845 C for 6 hours at 5000 psi yielded a dense material which on further heat treatment at 845 C for 24 hours exhibited a Tc of 108.2 K. A further improvement in the processing of the bismuth materials was achieved via a chemical coprecipitation process wherein the starting nitrate materials were coprecipitated with oxalic acid, thus yielding a more chemically homogeneous, more reactive powder. With the coprecipitated powders, only one calcine at 830 C for 12 hours and a final sinter at 845 C for 30 hours was sufficient to produce a bulk superconducting material with a Tc of 108.4 K. SAFIRE-type grounding links were successfully fabricated from sintered, tapecast, coprecipitated BSCCO 2223 powders. Compositional and processing investigations were continued on the Tl-based superconductors. Manganese and lithium additions and sintering temperature and time were examined to determine their influence on superconducting properties. It was found that lithium substitutions for copper enhance the transition temperatures while manganese additions produced deleterious effects on the superconducting properties. A suitable procedure for producing reproducible bulk and tapecast material of Tl composition Tl2Ba2Ca2Cu3O(x) was developed and used in fabricating uniform superconducting tapes. The highest transition temperature for Tl-based tapes was measured at 110.2 K. Thallium superconducting SAFIRE-type grounding links were fabricated from the tapes.

Solution-Based Approaches to Fabrication of YBa2Cu3O7-δ (YBCO): Precursors of Tri-Fluoroacetate (TFA) and Nanoparticle Colloids

NASA Astrophysics Data System (ADS)

Mukhopadhyay, S. M.; Su, J.; Chintamaneni, V.

2007-10-01

Detailed investigation of superconducting films of YBa2Cu3O7-δ (YBCO) prepared from solution-based precursors have been performed. Two precursors have been compared in this study: the presently used trifluoroacetate (TFA) solution and a recently developed colloidal suspension containing nanoparticles of mixed oxide. Detailed analyses of the evolution of microstructure and chemistry of the films have been performed, and process parameters have been correlated with final superconducting properties. Both films need two heating steps: a low temperature calcination and a higher temperature crystallization step. For TFA films, it was seen that the heating rate during calcination needs to be carefully optimized and is expected to be slow. For the alternate process using a nanoparticle precursor, a significantly faster calcination rate is possible. In the TFA process, the Ba ion remains as fluoride and the Y remains as oxyfluoride after calcination. This implies that, during the final crystallization stage to form YBCO, fluorine-containing gases will evolve, resulting in residual porosity. On the other hand, the film from the nanoparticle process is almost fully oxidized after calcination. Therefore, no gases evolve at the final firing (crystallization) stage, and the film has much lower porosity. The superconducting properties of both types of films are adequate, but the nanoparticle films appear to have persistently higher J c values. Moreover, they show improved flux pinning in higher magnetic fields, probably due to nanoscale precipitates of a Cu-rich phase. In addition, the nanocolloid films seem to show additionally enhanced flux pinning when doped with minute amounts of second phase precipitates. It therefore appears that, whereas the TFA process is already quite successful, the newly developed nanoparticle process has significant scope for additional improvement. It can be scaled-up with ease, and can be easily adapted to incorporate nanoscale flux pinning defects for in-field performance.

Synthesis of porous sheet-like Co{sub 3}O{sub 4} microstructure by precipitation method and its potential applications in the thermal decomposition of ammonium perchlorate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lu Shanshan; Jing Xiaoyan; Liu Jingyuan

2013-01-15

Porous sheet-like cobalt oxide (Co{sub 3}O{sub 4}) were successfully synthesized by precipitation method combined with calcination of cobalt hydroxide precursors. The structure, morphology and porosity properties of the products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and nitrogen adsorption-desorption measurement. The as-prepared sheet-like microstructures were approximately 2-3 {mu}m in average diameter, and the morphology of the cobalt hydroxide precursors was retained after the calcination process. However, it appeared a large number of uniform pores in the sheets after calcination. In order to calculate the potential catalytic activity, the thermal decomposition of ammoniummore » perchlorate (AP) has been analyzed, in which cobalt oxide played a role of an additive and the porous sheet-like Co{sub 3}O{sub 4} microstructures exhibited high catalytic performance and considerable decrease in the thermal decomposition temperature of AP. Moreover, a formation mechanism for the sheet-like microstructures has been discussed. - Graphical abstract: Porous sheet-like Co{sub 3}O{sub 4} were synthesized by facile precipitation method combined with calcination of {beta}-Co(OH){sub 2} precursors. Thermogravimetric-differential scanning calorimetric analysis indicates potential catalytic activity in the thermal decomposition of ammonium perchlorate. Highlights: Black-Right-Pointing-Pointer Synthesis of sheet-like {beta}-Co(OH){sub 2} precursors by precipitation method. Black-Right-Pointing-Pointer Porous sheet-like Co{sub 3}O{sub 4} were obtained by calcining {beta}-Co(OH){sub 2} precursors. Black-Right-Pointing-Pointer The possible formation mechanism of porous sheet-like Co{sub 3}O{sub 4} has been discussed. Black-Right-Pointing-Pointer Porous sheet-like Co{sub 3}O{sub 4} decrease the thermal decomposition temperature of ammonium perchlorate.« less

Structural, magnetic and gas sensing properties of nanosized copper ferrite powder synthesized by sol gel combustion technique

NASA Astrophysics Data System (ADS)

Sumangala, T. P.; Mahender, C.; Barnabe, A.; Venkataramani, N.; Prasad, Shiva

2016-11-01

Stoichiometric nano sized copper ferrite particles were synthesized by sol gel combustion technique. They were then calcined at various temperatures ranging from 300-800 °C and were either furnace cooled or quenched in liquid nitrogen. A high magnetisation value of 48.2 emu/g signifying the cubic phase of copper ferrite, was obtained for sample quenched to liquid nitrogen temperature from 800 °C. The ethanol sensing response of the samples was studied and a maximum of 86% response was obtained for 500 ppm ethanol in the case of a furnace cooled sample calcined at 800 °C. The chemical sensing is seen to be correlated with the c/a ratio and is best in the case of tetragonal copper ferrite.

[Removal Kinetics and Mechanism of Aniline by Manganese-oxide-modified Diatomite].

PubMed

Xiao, Shao-dan; Liu, Lu; Jiang, Li-ying; Chen, Jian-meng

2015-06-01

A novel rapid green one-step method was developed for the preparation of manganese modified diatomite (Mn-D) by treating roasted diatomite with an acidic permanganate solution. The effects of calcination temperature and mass ratio of KMnO4 and diatomite (p) on aniline removal efficiency of Mn-D were investigated. The removal kinetics and mechanism of aniline by Mn-D were also discussed. The results showed that when the optimal calcination temperature was 450 degrees C, p was 1.6, and the loading amounts of δ-MnO2 was 0.82 g x g(-1), Mn-D had a great performance for aniline removal, and more than 80% of aniline was adsorbed within 10 minutes, accompanied with the release of Mn2+. In acidic conditions, the adsorption process on Mn-D followed pseudo-second-order and was mainly controlled by intra-particle diffusion. The best fitting of the experimental adsorption data was given by the Freundlich equation. Gas chromatograph-mass spectrometer was applied to identify the reaction intermediates at different times, and azobenzene was found to be the main reaction intermediate in the degradation system. Based on the above observations, the possible degradation pathway of aniline by Mn-D was proposed.

Preparation of ZnO Photocatalyst for the Efficient and Rapid Photocatalytic Degradation of Azo Dyes.

PubMed

Chen, Xiaoqing; Wu, Zhansheng; Liu, Dandan; Gao, Zhenzhen

2017-12-01

Zinc oxide (ZnO) photocatalysts were synthesized by sol-gel method using zinc acetate as precursor for degradation of azo dyes under UV irradiation. The resultant samples were characterized by different techniques, such as XRD, SEM, and EDX. The influence of preparation conditions such as calcination temperature and composite ratio on the degradation of methyl orange (MO) was investigated. ZnO prepared with a composite ratio of 4:1 and calcination temperature of 400 °C exhibited 99.70% removal rate for MO. The effect of operation parameters on the degradation was also studied. Results showed that the removal rate of azo dyes increased with the increased dosage of catalyst and decreased initial concentration of azo dyes and the acidic condition is favorable for degradation. Furthermore, the kinetics and scavengers of the reactive species during the degradation were also investigated. It was found that the degradation of azo dyes fitted the first-order kinetics and superoxide ions were the main species. The proposed photocatalyst can efficiently and rapidly degrade azo dyes; thus, this economical and environment-friendly photocatalyst can be applied to the treatment of wastewater contaminated with synthetic dyes.

Synthesis of ZnFe2O4/SiO2 composites derived from a diatomite template.

PubMed

Liu, Zhaoting; Fan, Tongxiang; Zhou, Han; Zhang, Di; Gong, Xiaolu; Guo, Qixin; Ogawa, Hiroshi

2007-03-01

A novel porous ZnFe2O4/SiO2 composite product has been generated with a template-directed assembly method from porous diatomite under different synthesis conditions, such as precursor concentrations (metallic nitrates), calcination temperature and diatomite type. The phase composition and morphology of all the materials were examined by x-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). The results indicated that an inherited hierarchical porous structure from the diatomite template can be obtained, and the synthesis conditions were found to have clear effects on the formation of the ZnFe2O4/SiO2 composite. The ideal composite of ZnFe2O4/SiO2 can be obtained through optimization of diatomite template type, precursor solution and calcination temperature. Furthermore, the adsorption abilities of two types of diatomites were analyzed in detail using FTIR spectra and nitrogen adsorption measurements etc, which proved that A-diatomite (Shengzhou-diatomite) is better than B-diatomite (Changbai-diatomite) on the aspect of adsorbing Zn and Fe ions, and of forming the ZnFe2O4.

Effects of temperature, pressure, and carrier gas on the cracking of coal tar over a char-dolomite mixtures and calcined dolomite in a fixed-bed reactor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Seshadri, K.; Shamsi, A.

1998-10-01

A distillation fraction of a coal-derived liquid (tar) was cracked over a char-dolomite mixture, calcined dolomite, and silicon carbide in a fixed-bed reactor. The char-dolomite mixture (FWC) was produced from Pittsburgh No. 8 coal and dolomite in a Foster Wheeler carbonizer. The experiments were conducted under nitrogen and simulated coal gas (SCG), which was a mixture of CO, CO{sub 2}, H{sub 2}S, CH{sub 4}, N{sub 2}, and steam, at 1 and 17 atm. The conversion over these materials under nitrogen was much higher at 17 atm than at 1 atm. At higher pressures, tar molecules were trapped in the poresmore » of the bed material and underwent secondary reactions, resulting in the formation of excess char. However, when nitrogen was replaced by SCG, the reactions that induce char formation were suppressed, thus increasing the yield of gaseous products. The analysis of the gaseous products and the spent bed materials for organic and inorganic carbons suggested that the product distribution can be altered by changing the carrier gas, temperature, and pressure.« less

Phase progression of γ-Al2O3 nanoparticles synthesized in a solvent-deficient environment.

PubMed

Smith, Stacey J; Amin, Samrat; Woodfield, Brian F; Boerio-Goates, Juliana; Campbell, Branton J

2013-04-15

Our simple and uniquely cost-effective solvent-deficient synthetic method produces 3-5 nm Al2O3 nanoparticles which show promise as improved industrial catalyst-supports. While catalytic applications are sensitive to the details of the atomic structure, a diffraction analysis of alumina nanoparticles is challenging because of extreme size/microstrain-related peak broadening and the similarity of the diffraction patterns of various transitional Al2O3 phases. Here, we employ a combination of X-ray pair-distribution function (PDF) and Rietveld methods, together with solid-state NMR and thermogravimetry/differential thermal analysis-mass spectrometry (TG/DTA-MS), to characterize the alumina phase-progression in our nanoparticles as a function of calcination temperature between 300 and 1200 °C. In the solvent-deficient synthetic environment, a boehmite precursor phase forms which transitions to γ-Al2O3 at an extraordinarily low temperature (below 300 °C), but this γ-Al2O3 is initially riddled with boehmite-like stacking-fault defects that steadily disappear during calcination in the range from 300 to 950 °C. The healing of these defects accounts for many of the most interesting and widely reported properties of the γ-phase.

Calcinations effect on the grain size distributions Al2O3 powder

NASA Astrophysics Data System (ADS)

Issa, Tarik Talib; Mohammed, Awattif A.; Kamil, Dunia

2012-09-01

Fine of Al2O3 Powder was calcined at 200°C, 400°C, 600°C, and 800°C respectively for 2 hours under static air, x-ray diffraction, optical microscope and grain size distribution were done to analysis the resulting data after calcinations process. Batter particle size was achieved at 800°C of value (0.486) μm, while batter particles mean value of size 7.18 μm was found at 400°C. SEM micrographs shows that the agglomerate particles were vanished due to the calcinations process.

Preparation of hydroxyapatite-titania hybrid coatings on titanium alloy.

PubMed

Un, Serhat; Durucan, Caner

2009-08-01

Hydroxypapatite-titania hybrid films on Ti6Al4V alloys were prepared by sol-gel technique by incorporating presynthesized hydroxypapatite (Ca(10)(PO(4))(6)(OH)(2) or HAp) powders into a titanium-alkoxide dip coating solution. Titania network was formed by the hydrolysis and condensation of Ti-isopropoxide Ti[OCH(CH(3))(2)](4)-based sols. The effect of titania sol formulation, specifically the effect of organic solvents on the microstructure of the dip coated films calcined at 500 degrees C has been investigated. The coatings exhibit higher tendency for cracking when a high vapor pressure solvent, such as ethanol (C(2)H(5)OH) is used causing development of higher macroscopic stresses during evaporation of the sol. Titania sol formulations replacing the solvent with n-proponal (CH(3)(CH(2))(2)OH) and acetly-acetone (C(5)H(8)O) combinations enhanced the microstructural integrity of the coating during evaporation and calcination treatments. Sol-gel processing parameters, such as multilayer coating application and withdrawal rate, can be employed to change the titania thickness in the range of 0.120-1.1 microm and to control the microstructure of HAp-titania hybrid coatings. A high-calcination temperature in the range of 400-600 degrees C does not cause a distinct change in crystals nature of the titania matrix or HAp, but results in more cracking due to the combined effect of densification originated stresses and thermal stresses upon cooling. Slower withdraw rates and multilayer dip coating lead to coatings more vulnerable to microcracking.

Characterization of LaRhO3 perovskites for dry (CO2) reforming of methane (DRM)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Johansson, Ted; Pakhare, Devendra; Haynes, Daniel

2014-01-01

Abstract This work reports on the characterization of LaRhO3 perovskite as a catalyst for dry reforming of methane. The catalyst was studied using CH4-temperature programmed reduction (TPR), H2-TPR, and temperature programmed surface reaction (TPSR), and the changes in the crystal structure of the catalyst due to these treatments were studied by X-ray diffraction (XRD). XRD pattern of the freshly calcined perovskites showed the formation of highly crystalline LaRhO3 and La2O3 phases. H2-TPR of the fresh calcined catalyst showed a shoulder at 342°C and a broad peak at 448°C, suggesting that the reduction of Rh in perovskite occurs in multiple steps.more » XRD pattern of the reduced catalyst suggests complete reduction of the LaRhO3 phase and the formation of metallic Rh and minor amounts of La(OH)3. The CH4-TPR data show qualitatively similar results as H2-TPR, with a shoulder and a broad peak in the same temperature range. Following the H2-TPR up to 950°C, the same batch of catalyst was oxidized by flowing 5 vol. % O2/He up to 500°C and a second H2-TPR (also up to 950°C) was conducted. This second H2-TPR differed significantly from that of the fresh calcined catalyst. The single sharp peak at 163°C in the second H2-TPR suggests a significant change in the catalyst, probably causedby the transformation of about 90 % of the perovskite into Rh/La2O3. This was confirmed by the XRD studies of the catalyst reduced after the oxidation at 500°C. TPSR of the dry reforming reaction on the fresh calcined catalyst showed CO and H2 formation starting at 400°C, with complete consumption of the reactants at 650°C. The uneven consumption of reactants between 400°C and 650°C suggests that reactions other than DRM occur, including reverse water gas shift (RWGS) and the Boudouard reaction (BR), probably as a result of in-situ changes in the catalyst, consistent with the H2-TPR results. TPSR, after a H2-TPR up to 950°C, showed that the dry reforming reaction did not light off until 570°C, which is much higher temperature than the one observed using fresh calcined catalyst. This shows that the uniform sites produced during the 950°C H2-TPR are catalytically less active than those of the fresh calcined catalyst, and that no significant side reactions such as RWGS or the Boudouard reaction occur. This suggests that reduction leads to the formation of a single type of sites which do not catalyze simultaneous side reactions.« less

A new method of preparation of AgBr/TiO2 composites and investigation of their photocatalytic activity

NASA Astrophysics Data System (ADS)

Xing, Yangyang; Li, Rui; Li, Qiuye; Yang, Jianjun

2012-12-01

Silver bromide/titanium dioxide composites were first prepared using titanic acid nanobelts (TAN) as the TiO2 source. First, TAN reacted with AgNO3 to prepare Ag-incorporated TAN by the ion-exchange method, and then AgBr/TAN was obtained after adding NaBr. Finally, AgBr/TAN was transformed to AgBr/TiO2 composites by calcination. The post-treated calcination would not only convert TAN to TiO2 (H2Ti2O4(OH)2 → 2H2O + 2TiO2), but also increase the effective contact between AgBr and TiO2, further to improve the separation of photo-generated electron-holes. The advantage of this preparation method is the small particle size (ca. 10-20 nm) and well dispersion of AgBr on the surface of TiO2, and close contact between AgBr and TiO2. The effect of the different calcination temperature on the morphology, structure, and properties of AgBr/TiO2 composites was investigated in detail. The AgBr/TiO2 composites were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), and ultraviolet-visible diffuse reflectance spectra (UV-Vis DRS). Comparing with pure TAN, AgBr, and AgBr/P25 mixture, the AgBr/TiO2 composites exhibited enhanced photocatalytic activity in decomposition of methyl orange (MO) under visible light irradiation.

Preparation and photo Fenton-like activities of high crystalline CuO fibers

NASA Astrophysics Data System (ADS)

Zhang, Yan; He, Jing; Shi, Ruixia; Yang, Ping

2017-11-01

CuO fibers were successfully fabricated by a simple electrospinning method, followed by calcination. Some experimental parameters such as the content of Cu(NO3)2•3H2O, the content of PVP, the stirring time, the applied voltage, as well the calcination temperature were investigated, respectively, and their influences on the morphologies of fibers and the spinnability of precursor solution were analyzed. The CuO fibers calcined at 550 °C consisted of numerous CuO grains exhibited a well-crystalline structure. Furthermore, the CuO fibers demonstrated effective photo-Fenton degradation to methyl orange with the assist of H2O2 and the adding volume of H2O2 affects the degradation activities greatly. The degradation rate of methyl orange by the CuO fibers in the presence of 238.8 mmol/L H2O2 is 3.8 times as much as one by P25 alone under the irradiation of Xe lamp. The degradation ratio of methyl orange could achieve 83% in 180 min. The enhanced photocatalytic activities of the CuO fibers were attributed to two aspects: one is the well-crystalline of CuO fibers; the other is that H2O2 accepted the photogenerated electrons and holes effectively, which not only prevented the recombination of charge carriers but also produced additional rad OH. In this work, the formation and photocatalysis mechanisms of CuO fibers were also investigated.

Kinetics of NiO and NiCl2 Hydrogen Reduction as Precursors and Properties of Produced Ni/Al2O3 and Ni-Pd/Al2O3 Catalysts

PubMed Central

Sokić, Miroslav; Kamberović, Željko; Nikolić, Vesna; Marković, Branislav; Korać, Marija; Anđić, Zoran; Gavrilovski, Milorad

2015-01-01

The objects of this investigation were the comparative kinetic analysis of the NiO and NiCl2 reduction by hydrogen during an induction period and elimination of the calcination during the synthesis of Ni/Al2O3 catalysts. The effect of temperature and time on NiO and NiCl2 reduction degrees was studied. Avrami I equation was selected as the most favorable kinetic model and used to determine activation energy of the NiO and NiCl2 reduction for the investigated temperature range (623–923 K) and time intervals (1–5 minutes). The investigation enabled reaching conclusions about the reaction ability and rate of the reduction processes. Afterward, Ni/Al2O3 catalysts were obtained by using oxide and chloride precursor for Ni. The catalysts were supported on alumina-based foam and prepared via aerosol route. Properties of the samples before and after low-temperature hydrogen reduction (633 K) were compared. Obtained results indicated that the synthesis of Ni/Al2O3 catalysts can be more efficient if chloride precursor for Ni is directly reduced by hydrogen during the synthesis process, without the calcination step. In addition, Ni-Pd/Al2O3 catalysts with different metal content were prepared by using chloride precursors. Lower reduction temperature was utilized and the chlorides were almost completely reduced at 533 K. PMID:25789335

Alcoa Pressure Calcination Process for Alumina

NASA Astrophysics Data System (ADS)

Sucech, S. W.; Misra, C.

A new alumina calcination process developed at Alcoa Laboratories is described. Alumina is calcined in two stages. In the first stage, alumina hydrate is heated indirectly to 500°C in a decomposer vessel. Released water is recovered as process steam at 110 psig pressure. Partial transformation of gibbsite to boehmite occurs under hydrothermal conditions of the decomposer. The product from the decomposer containing about 5% LOI is then calcined by direct heating to 850°C to obtain smelting grade alumina. The final product is highly attrition resistant, has a surface area of 50-80 m2/g and a LOI of less than 1%. Accounting for the recovered steam, the effective fuel consumption for the new calcination process is only 1.6 GJ/t A12O3.

Oil shale retorting and combustion system

DOEpatents

Pitrolo, Augustine A.; Mei, Joseph S.; Shang, Jerry Y.

1983-01-01

The present invention is directed to the extraction of energy values from l shale containing considerable concentrations of calcium carbonate in an efficient manner. The volatiles are separated from the oil shale in a retorting zone of a fluidized bed where the temperature and the concentration of oxygen are maintained at sufficiently low levels so that the volatiles are extracted from the oil shale with minimal combustion of the volatiles and with minimal calcination of the calcium carbonate. These gaseous volatiles and the calcium carbonate flow from the retorting zone into a freeboard combustion zone where the volatiles are burned in the presence of excess air. In this zone the calcination of the calcium carbonate occurs but at the expense of less BTU's than would be required by the calcination reaction in the event both the retorting and combustion steps took place simultaneously. The heat values in the products of combustion are satisfactorily recovered in a suitable heat exchange system.

21 CFR 73.2725 - Ultramarines.

Code of Federal Regulations, 2012 CFR

2012-04-01

..., ultramarines (blue, green, pink, red, and violet) are pigments obtained by calcining at temperatures above 700... cosmetics, including cosmetics intended for use in the area of the eye, in amounts consistent with good...

21 CFR 73.2725 - Ultramarines.

Code of Federal Regulations, 2013 CFR

2013-04-01

..., ultramarines (blue, green, pink, red, and violet) are pigments obtained by calcining at temperatures above 700... cosmetics, including cosmetics intended for use in the area of the eye, in amounts consistent with good...

21 CFR 73.2725 - Ultramarines.

Code of Federal Regulations, 2014 CFR

2014-04-01

..., ultramarines (blue, green, pink, red, and violet) are pigments obtained by calcining at temperatures above 700... cosmetics, including cosmetics intended for use in the area of the eye, in amounts consistent with good...

21 CFR 73.2725 - Ultramarines.

Code of Federal Regulations, 2010 CFR

2010-04-01

..., ultramarines (blue, green, pink, red, and violet) are pigments obtained by calcining at temperatures above 700... cosmetics, including cosmetics intended for use in the area of the eye, in amounts consistent with good...

Poorly crystalline hydroxyapatite: A novel adsorbent for enhanced fulvic acid removal from aqueous solution

NASA Astrophysics Data System (ADS)

Wei, Wei; Yang, Lei; Zhong, Wenhui; Cui, Jing; Wei, Zhenggui

2015-03-01

In this study, poorly crystalline hydroxyapatite (HAP) was developed as an efficient adsorbent for the removal of fulvic acid (FA) from aqueous solution. Surface functionality, crystallinity, and morphology of the synthetic adsorbent were studied by Fourier-transformation infrared (FT-IR) spectroscopy, powder X-ray diffraction (XRD) and transmission electron microscopy (TEM). The effects of various parameters such as crystallinity of adsorbent, contact time, adsorbent dosage, pH, initial adsorbate concentration, temperature, ionic strength and the presence of alkaline earth metal ions on FA adsorption were investigated. Results indicated that the nanosized HAP calcined at lower temperature was poorly crystalline (Xc = 0.23) and had better adsorption capacity for FA than those (Xc = 0.52, 0.86) calcined at higher temperature. FA removal was increased with increases of adsorbent dosage, temperature, ionic strength and the presence of alkali earth metal ions, but decreased as the pH increased. Kinetic studies showed that pseudo-second-order kinetic model better described the adsorption process. Equilibrium data were best described by Sips models, and the estimated maximum adsorption capacity of poorly crystalline HAP was 90.20 mg/g at 318 K, displaying higher efficiency for FA removal than previously reported adsorbents. FT-IR results revealed that FA adsorption over the adsorbent could be attributed to the surface complexation between the oxygen atom of functional groups of FA and calcium ions of HAP. Regeneration studies indicated that HAP could be recyclable for a long term. Findings of the present work highlight the potential for using poorly crystalline HAP nanoparticles as an effective and recyclable adsorbent for FA removal from aqueous solution.

Calcination does not remove all carbon from colloidal nanocrystal assemblies

DOE PAGES

Mohapatra, Pratyasha; Shaw, Santosh; Mendivelso-Perez, Deyny; ...

2017-12-11

Removing organics from hybrid nanostructures is a crucial step in many bottom-up materials fabrication approaches. It is usually assumed that calcination is an effective solution to this problem, especially for thin films. This assumption has led to its application in thousands of papers. Here in this paper, we show that this general assumption is incorrect by using a relevant and highly controlled model system consisting of thin films of ligand-capped ZrO 2 nanocrystals. After calcination at 800 °C for 12 h, while Raman spectroscopy fails to detect the ligands after calcination, elastic backscattering spectrometry characterization demonstrates that ~18% of themore » original carbon atoms are still present in the film. By comparison plasma processing successfully removes the ligands. Our growth kinetic analysis shows that the calcined materials have significantly different interfacial properties than the plasma-processed counterparts. Calcination is not a reliable strategy for the production of single-phase all-inorganic materials from colloidal nanoparticles.« less

Silicon-based microfabricated tin oxide gas sensor incorporating use of Hall effect measurement

NASA Astrophysics Data System (ADS)

Hammond, Joseph Wilson

2000-10-01

Characterization of a microfabricated sol-gel derived nano-particle tin oxide thin film on a silicon substrate, through simultaneous measurement of conductivity, Hall mobility and electron density, had not been accomplished before this study. Conductivity is a function of carrier density and Hall mobility. Therefore, a full understanding of the sensing mechanism of tin oxide requires knowledge of the sensor conductivity, electron density and Hall mobility. A tin oxide thin film (1100A thick), derived by the sol-gel method, was deposited on a Si/SiO2 substrate by means of spin coating method. The sol-gel method produces films of porous interconnected nano-sized particles and is relatively inexpensive and easy to produce compared to existing methods of tin oxide thin film deposition. A goal of this study was to determine the compatibility of sol-gel derived tin oxide thin films with silicon based microfabrication procedures. It was determined that conductivity sensitivity is strongly dependant on electron density level and shows very weak dependence on Hall mobility. Lack of Hall mobility sensitivity to H2 concentration suggests that conduction is grain control limited. In this regime, in which the grain size (D) is less than twice the characteristic Debye length (LD), a change in reducing gas concentration results in a nearly simultaneous change in carrier density throughout the entire grain, while the Hall mobility remains unchanged. The sensor calcined at 500°C and operated at 250°C showed maximum conductivity sensitivity to H2 in air. The sensor exhibited a high conductivity sensitivity of 10.6 to 100ppm H2 in air with response time of (˜1) minute and recovery time of (˜4) minutes. Images of the thin film surface, obtained by SEM, were used to study the effects of calcination temperature and operating conditions on the tin oxide structure. Sensitivity decreased as average grain size increased from 7.7nm to 14.7nm, with increasing calcination temperature from 500°C to 800°C. The sensors displayed slight drift in long term baseline stability and good long term sensitivity stability (14 days). Long term operation (30 days) at elevated temperatures had no noticeable effect on the thin film structure.

Effect of different alcohols, gelatinizing times, calcination and microwave on characteristics of TiO2 nanoparticles synthesized by sol-gel method

NASA Astrophysics Data System (ADS)

Bahar, Mahmoud; Mozaffari, Masoud; Esmaeili, Sahar

2017-03-01

In this work, nanoparticles of titanium dioxide (TiO2) were synthesized by means of TiCl4 as precursor. Effects of alcohol type, calcination, gelatinizing time and microwave exposure on the particle size, morphology, crystallinity and particle phase are studied using XRD patterns and SEM images. Results showed that alcohols such as ethanol increased the particle size; calcination increased the particle size and improved the crystallinity of particles. Microwave exposure of particles resulted in smaller particles; adding water increased the impact of microwave. Effect of microwave exposure in rutile phase formation is also observed during this study.

Iron Oxide Silica Derived from Sol-Gel Synthesis

PubMed Central

Darmawan, Adi; Smart, Simon; Julbe, Anne; Diniz da Costa, João Carlos

2011-01-01

In this work we investigate the effect of iron oxide embedded in silica matrices as a function of Fe/Si molar ratio and sol pH. To achieve homogeneous dispersion of iron oxide particles, iron nitrate nonahydrate was dissolved in hydrogen peroxide and was mixed with tetraethyl orthosilicate and ethanol in a sol-gel synthesis method. Increasing the calcination temperature led to a reduction in surface area, although the average pore radius remained almost constant at about 10 Å, independent of the Fe/Si molar ratio or sol pH. Hence, the densification of the matrix was accompanied by similar reduction in pore volume. However, calcination at 700 °C resulted in samples with similar surface area though the iron oxide content increased from 5% to 50% Fe/Si molar ratio. As metal oxide particles have lower surface area than polymeric silica structures, these results strongly suggest that the iron oxides opposed the silica structure collapse. The effect of sol pH was found to be less significant than the Fe/Si molar ratio in the formation of molecular sieve structures derived from iron oxide silica. PMID:28879999

Usage of immobilized porcine pancreas lipase in the hydrolysis of roselle (Hibiscus sabdariffa L.) seed oil

NASA Astrophysics Data System (ADS)

Ai, Chau Tran Diem; Linh, Vo Thi Hong; Yen, Tran Thi Ngoc; Nguyen, Nguyen Thi; Hoa, Phan Ngoc

2017-09-01

This study focused on the comparison among the usage of immobilized porcine pancreas lipase (PPL) on different hydrotalcite carriers (uncalcined and calcined hydrotalcite - like compound Mg /Al) and free lipase as the catalysts to hydrolyze of roselle (Hibiscus sabdariffa L.) seed oil. The reaction conditions were investigated including the ratio of oil to buffer, ratio of enzyme to substrate, the temperature of the hydrolysis, pH. The calcined hydrotalcite showed a higher lipase immobilization yield and a better reusability than the uncalcined hydrotalcite (87.15% and 86.78%, respectively).

Synthesis, characterization and effect of calcination temperature on phase transformation and photocatalytic activity of Cu,S-codoped TiO 2 nanoparticles

NASA Astrophysics Data System (ADS)

Hamadanian, M.; Reisi-Vanani, A.; Majedi, A.

2010-01-01

A novel copper and sulfur codoped TiO 2 photocatalyst was synthesized by modified sol-gel method using titanium(IV) isopropoxide, CuCl 2·2H 2O and thiourea as precursors. The samples were characterized by X-ray diffraction (XRD), diffuse reflectance spectroscopy (DRS), scanning electron microscopy equipped with energy dispersive X-ray micro-analysis (SEM-EDX), transmission electron microscopy (TEM) and Fourier transform infrared (FT-IR) analysis. The XRD results showed undoped and Cu,S-codoped TiO 2 nanoparticles only include anatase phase. Effect of calcination temperature showed rutile phase appears in 650 and 700 °C for undoped and 0.1% Cu,S-codoped TiO 2, respectively. The SEM analysis revealed the doping of Cu and S does not leave any change in morphology of the catalyst surface. The increase of copper doping enhanced "red-shift" in the UV-vis absorption spectra. The TEM images confirmed the dopants suppressed the growth of TiO 2 grains. The photocatalytic activity of samples was tested for degradation of methyl orange (MO) solutions. The results showed photocatalytic activity of the catalysts with 0.05% Cu,0.05% S and 0.1% Cu,0.05% S were higher than that of other catalysts under ultraviolet (UV) and visible irradiation, respectively. Because of synergetic effect of S and Cu, the Cu,S-codoped TiO 2 catalyst has higher activity than undoped and Cu or S doped TiO 2 catalysts.

Hydrothermal synthesis and tunable luminescence of CaSiO{sub 3}:RE{sup 3+}(RE{sup 3+} = Eu{sup 3+}, Sm{sup 3+}, Tb{sup 3+}, Dy{sup 3+}) nanocrystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fu, Linlin; Yang, Xingxing; Fu, Zuoling, E-mail: zlfu@jlu.edu.cn

2015-05-15

Highlights: • Near-spherical CaSiO{sub 3} nanocrystals were synthesized via a hydrothermal method. • The effect of calcination temperature on crystalline phase formation was discussed. • Optical properties of trivalent ions doped CaSiO{sub 3} nanocrystals were investigated. • Tunable luminescence of CaSiO{sub 3}:Tb{sup 3+}, Eu{sup 3+} can be achieved by a simple method. - Abstract: CaSiO{sub 3}:RE{sup 3+} (RE{sup 3+} = Eu{sup 3+}, Sm{sup 3+}, Tb{sup 3+}, Dy{sup 3+}) nanocrystals were prepared by facile hydrothermal method with further calcinations. The crystal structure and the effects of annealing temperature on phase transition have been characterized by X-ray diffraction (XRD). The photoluminescence (PL)more » and PL excitation (PLE) spectra were used to characterize the optical properties of all samples. The effect of Eu{sup 3+} and Sm{sup 3+} doping concentrations on the luminescent intensity were also investigated in details, respectively. Moreover, the luminescence colors of the Tb{sup 3+} and Eu{sup 3+} co-doped CaSiO{sub 3} samples can be tuned by simply adjusting the relative doping concentrations of the rare earth ions under a single wavelength excitation, which might find potential applications in the fields of light display systems and optoelectronic devices.« less

Facile and rapid auto-combustion synthesis of nano-porous γ-Al2O3 by application of hexamethylenetetramine in fuel composition

NASA Astrophysics Data System (ADS)

Salem, Shiva; Salem, Amin; Parni, Mohammad Hosein; Jafarizad, Abbas

2018-06-01

In this article, urea, glycine and hexamethylenetetramine were blended in accordance with the mixture design algorithm to prepare γ-Al2O3 by auto-combustion technique. Aluminum nitrate was then mixed with the stoichiometric contents of prepared fuel solutions to obtain gel systems. The gels exhibited a typical self-propagating combustion behavior at low temperature, directly resulting amorphous materials. The precursors were calcined at various temperatures ranging from 700 to 900 °C. The treated powders were evaluated by determining the methylene blue (MB) adsorption efficiency. The production condition to obtain γ-Al2O3 with maximum surface area depends on fuel composition and calcination temperature. The alumina powder fabricated by this procedure was uniformly distributed and contains nano-sized secondary particles with diameter about 10-30 nm in which the average pore size is 3.2 nm induced large surface area, 240 m2g-1. The employment of hexamethylenetetramine provides a potential for synthesis of γ-Al2O3 at lower temperature, 700 °C, with maximum MB removal efficiency.

Lithium ion conduction in sol-gel synthesized LiZr2(PO4)3 polymorphs

NASA Astrophysics Data System (ADS)

Kumar, Milind; Yadav, Arun Kumar; Anita, Sen, Somaditya; Kumar, Sunil

2018-04-01

Safety issue associated with the high flammability and volatility of organic electrolytes used in commercial rechargeable lithium ion batteries has led to significant attention to ceramic-based solid electrolytes. In the present study, lithium ion conduction in two polymorphs of LiZr2(PO4)3 synthesized via the sol-gel route has been investigated. Rietveld refinement of room temperature X-ray diffraction data of LiZr2(PO4)3 powders calcined at 900 °C and 1300 °C confirmed these to be the monoclinic phase with P21/n structure and rhombohedral phase with R3¯c structure, respectively. Increase in calcination temperature and resultant phase transformation improved the room temperature conductivity from 2.27×10-6 ohm-1m-1 for the monoclinic phase to 1.41×10-4 ohm-1m-1 for rhombohedral phase. Temperature dependence of conductivity was modeled using Arrhenius law and activation energy of ˜ 0.59 eV (for monoclinic phase) and ˜0.50 eV (for rhombohedral phase) were obtained.

Induced emission cross section of a possible laser line in Nd:Y2O3 ceramics at 1.095 μm

NASA Astrophysics Data System (ADS)

Fukabori, Akihiro; Sekita, Masami; Ikegami, Takayasu; Iyi, Nobuo; Komatsu, Toshiki; Kawamura, Masayuki; Suzuki, Makoto

2007-02-01

In this study, we measured the change of the optical transmittance for calcination temperatures, in steps of 10°, at two different sintering temperatures. It was found that the optical transmittance is highly dependent on the calcination temperature. The highest optical transmittance obtained was 70% for the transparent Y2O3 (yttria) ceramics produced without the use of additives and high injection presure in this study, higher than the highest reported value of 65%. Optical absorption and emission spectra of Nd :Y2O3 obtained from a low temperature synthesis process were measured. The energy level structure of Nd3+ in the Y2O3 ceramics was determined for a 1mol% Nd concentration. The induced emission cross section was calculated to be in the range of 3.2×10-19-1.1×10-17cm2 for the 1mol% Nd-doped Y2O3 ceramics. Furthermore, a laser line possibly has been identified in this study, in the Nd :Y2O3 ceramic at 1.095μm.

Combustion Synthesis of Sm0.5Sr0.5CoO3-x and La0.6Sr0.4CoO3-x Nanopowders for Solid Oxide Fuel Cell Cathodes

NASA Technical Reports Server (NTRS)

Bansal, Narottam P.; Zhong, zhimin

2005-01-01

Nanopowders of Sm0.5Sr0.5CoO(3-x) (SSC) and La0.6Sr0.4CoO(3-x) (LSC) compositions, which are being investigated as cathode materials for intermediate temperature solid oxide fuel cells, were synthesized by a solution-combustion method using metal nitrates and glycine as fuel. Development of crystalline phases in the as-synthesized powders after heat treatments at various temperatures was monitored by x-ray diffraction. Perovskite phase in LSC formed more readily than in SSC. Single phase perovskites were obtained after heat treatment of the combustion synthesized LSC and SSC powders at 1000 and 1200 C, respectively. The as-synthesized powders had an average particle size of 12 nm as determined from x-ray line broadening analysis using the Scherrer equation. Average grain size of the powders increased with increase in calcination temperature. Morphological analysis of the powders calcined at various temperatures was done by scanning electron microscopy.

Study of KOH/Al2O3 as heterogeneous catalyst for biodiesel production via in situ transesterification from microalgae.

PubMed

Ma, Guixia; Hu, Wenrong; Pei, Haiyan; Jiang, Liqun; Ji, Yan; Mu, Ruimin

2015-01-01

Heterogeneous KOH/Al2O3 catalysts, synthesized by the wet impregnation method with different KOH loadings (20-40 wt%) and calcination temperatures from 400°C to 800°C, were used to produce biodiesel from Chlorella vulgaris biomass by in situ transesterification. The highest yield of biodiesel of 89.53±1.58% was achieved at calcination temperature of 700°C for 2 h and 35 wt% loading of KOH, and at the optimal reaction condition of 10 wt% of catalyst content, 8 mL/g of methanol to biomass ratio and at 60°C for 5 h. The characteristics of the catalysts were analysed by X-ray diffraction, scanning electron microscopy and Brunauer-Emmett-Teller.

Adsorption of vitamin E on mesoporous titania nanocrystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shih, C.J., E-mail: cjshih@kmu.edu.tw; Lin, C.T.; Wu, S.M.

2010-07-15

Tri-block nonionic surfactant and titanium chloride were used as starting materials for the synthesis of mesoporous titania nanocrystallite powders. The main objective of the present study was to examine the synthesis of mesoporous titania nanocrystals and the adsorption of vitamin E on those nanocrystals using X-ray diffraction (XRD), transmission electron microscopy, and nitrogen adsorption and desorption isotherms. When the calcination temperature was increased to 300 {sup o}C, the reflection peaks in the XRD pattern indicated the presence of an anatase phase. The crystallinity of the nanocrystallites increased from 80% to 98.6% with increasing calcination temperature from 465 {sup o}C tomore » 500 {sup o}C. The N{sub 2} adsorption data and XRD data taken after vitamin E adsorption revealed that the vitamin E molecules were adsorbed in the mesopores of the titania nanocrystals.« less

Re-cycling of sugar-ash: a raw feed material for rotary kilns.

PubMed

Kantiranis, Nikolaos

2004-01-01

Large amounts of sugar-ash, a material rich in calcium carbonate, are produced as a by-product in the Greek Sugar Industry. This work explores the possibility of re-cycling sugar-ash for use in the lime industry. A representative sample of sugar-ash from the Plati Imathias sugar plant was studied by PXRD, TG/DTG, calcination experiments at temperatures between 650 and 1150 degrees C and experiments to determine the quality of the quicklime produced at temperatures between 850 and 1150 degrees C following methods described in ASTM C110 standard. The sugar-ash was found to consist of 90 wt% calcium rich minerals (calcite and monohydrocalcite) and 10 wt% amorphous material. Traces of quartz were also detected. The quicklime of highest quality was produced at 950 degrees C. It is concluded that this "useless" material (sugar-ash) can be re-cycled for use in rotary kilns in the lime industry at calcination temperatures up to 950-1000 degrees C.

Fast and Simple Microwave Synthesis of TiO2/Au Nanoparticles for Gas-Phase Photocatalytic Hydrogen Generation.

PubMed

May-Masnou, Anna; Soler, Lluís; Torras, Miquel; Salles, Pol; Llorca, Jordi; Roig, Anna

2018-01-01

The fabrication of small anatase titanium dioxide (TiO 2 ) nanoparticles (NPs) attached to larger anisotropic gold (Au) morphologies by a very fast and simple two-step microwave-assisted synthesis is presented. The TiO 2 /Au NPs are synthesized using polyvinylpyrrolidone (PVP) as reducing, capping and stabilizing agent through a polyol approach. To optimize the contact between the titania and the gold and facilitate electron transfer, the PVP is removed by calcination at mild temperatures. The nanocatalysts activity is then evaluated in the photocatalytic production of hydrogen from water/ethanol mixtures in gas-phase at ambient temperature. A maximum value of 5.3 mmol·[Formula: see text]h -1 (7.4 mmol·[Formula: see text]h -1 ) of hydrogen is recorded for the system with larger gold particles at an optimum calcination temperature of 450°C. Herein we demonstrate that TiO 2 -based photocatalysts with high Au loading and large Au particle size (≈50 nm) NPs have photocatalytic activity.

Size dependent anomalous dielectric behavior in nanoparticle Gd2 O 3 : SiO2 glass composite system

NASA Astrophysics Data System (ADS)

Mukherjee, Sudip; Lin, Yu-Hsing; Kao, Ting-Hui; Chou, C. C.; Yang, H. D.

2011-03-01

Gd 2 O3 (0.5 mol%) nanoparticles have been synthesized in a silica glass matrix by the sol-gel method at calcination temperatures of 700& circ; C and above. Compared with the parent material Si O2 , this nano-glass composite system shows enhancement of dielectric constant and diffuse phase transition along with magnetodielectric effect around room temperature. Observed conduction mechanism is found to be closely related to the thermally activated oxygen vacancies. Magnetodielectric behavior is strongly associated with magnetoresistance changes, depending on the nanoparticle size and separation. Such a material might be treated as a potential candidate for device miniaturization.

The Preparation and Characterization of Natrolite Synthetized by Purified Attapulgite

NASA Astrophysics Data System (ADS)

Li, H. J.; Zhou, X. D.; Zhang, J. M.; Wu, X. Y.; Gao, H. B.

2017-06-01

This paper mainly researched the hydrothermal synthesis of Natrolite, using amorphous silicon source from the purified attapulgite. The effects of silicon source, silicon aluminum ratio, crystallization time and crystallization temperature on the synthesis of natrolite were investigated. The results showed that the optimal synthesis condition of natrolite was: Hydrothermal activated ATP with NaOH was silicon source, silicon aluminum ratio was 10:1, crystallization time lasted to 72h and crystallization temperature was 150°C, the template was removed by calcining 8 hours at 550°C. The structural formula of obtained natrolite is Na2Al2Si3O10•2H2O.

Reactivity improvement of Ca(OH)2 sorbent using diatomaceous earth (DE) from Aceh Province

NASA Astrophysics Data System (ADS)

Mariana, M.; Mahidin, M.; Mulana, F.; Agam, T.; Hafdiansyah, F.

2018-04-01

In this study, the diatomaceous earth (DE) from Aceh Province was used to increase the reactivity of Ca(OH)2sorbent. The high silica (SiO2) content of about 97% in the diatomaceous earth allows the increasing reactivity of Ca(OH)2sorbent by forming calcium silicate hydrate (CSH). The CSH improved the porosity characteristic of the sorbent. The improvement process was performed by mixing Ca(OH)2sorbent, diatomaceous earth and water in a beaker glass at the Ca(OH)2/DE weight ratio of 1:10 for 2 hand then dried at 120 °C for 24 h. The dried sorbent was calcined at 500 °C and 800 °C for 2 h. The activated sorbent was characterized using Scanning Electron Microscopy (SEM) for the morphological properties; X- Ray Diffraction (XRD) for the materials characteristics. The adsorption capacity of thesorbent was tested by methylene blue adsorption. The results showed that the Ca(OH)2/DEsorbent had a higher porosity than the Ca(OH)2 adsorbent.The results also showed that Ca(OH)2/DE which was calcined at higher temperature of 800 °C had a higher adsorption capacity compared to Ca(OH)2/DE which was calcined at lower temperature of 500 °C.

A systematic investigation into the extraction of aluminum from coal spoil through kaolinite.

PubMed

Qiao, X C; Si, P; Yu, J G

2008-11-15

This research has applied kaolin and active carbon (AC) to the investigation of the recovery of aluminum from coal spoil (CS). The kaolin, AC-containing kaolin mixture, and CS have been calcined at 500, 600, 700, 800, and 900 degrees C for 15, 30, 60, and 120 min. The transformation of kaolinite and aluminum extraction that occurred in each calcined sample have been characterized using XRD, TG, IR, and hydrochloric acid leaching methods. The dehydroxylation of kaolinite and the decomposition of metakaolin were influenced by thermal treatment temperature and time. The metakaolin had kept a portion of OH- in its structure until it was calcined at a temperature of 800 degrees C. Under 60 min treatment, new SiO2 phase was able to be formed at 500 degrees C, kaolinite was totally converted to metakaolin at 600 degrees C, and the SiO2 rejoined the reaction at 800 degrees C. The decompositions of CS were similar to those of kaolin mixture containing 20 wt % AC (MKC). The combustion of combustible matter accelerated the decomposition of kaolinite in the CS and MKC. Higher AC content led to lower aluminum extraction. The treatment at 600 degrees C was optimal for both CS and MKC.

Boron sorption from aqueous solution by hydrotalcite and its preliminary application in geothermal water deboronation.

PubMed

Guo, Qinghai; Zhang, Yin; Cao, Yaowu; Wang, Yanxin; Yan, Weide

2013-11-01

Hydrotalcite and its calcination product were used to treat pure water spiked with various concentrations of boron and geothermal water containing boron as a major undesirable element. The kinetics process of boron sorption by uncalcined hydrotalcite is controlled by the diffusion of boron from bulk solution to sorbent-solution boundary film and its exchange with interlayer chloride of hydrotalcite, whereas the removal rate of boron by calcined hydrotalcite rests with the restoration process of its layered structure. The results of isotherm sorption experiments reveal that calcined hydrotalcite generally has much stronger ability to lower solution boron concentration than uncalcined hydrotalcite. The combination of adsorption of boron on the residue of MgO-Al2O3 solid solution and intercalation of boron into the reconstructed hydrotalcite structure due to "structural memory effect" is the basic mechanism based on which the greater boron removal by calcined hydrotalcite was achieved. As 15 geothermal water samples were used to test the deboronation ability of calcined hydrotalcite at 65 °C, much lower boron removal efficiencies were observed. The competitive sorption of the other anions in geothermal water, such as HCO3-, SO4(2-), and F-, is the reason why calcined hydrotalcite could not remove boron from geothermal water as effectively as from pure boron solution. However, boron removal percents ranging from 89.3 to 99.0% could be obtained if 50 times of sorbent were added to the geothermal water samples. Calcined hydrotalcite is a good candidate for deboronation of geothermal water.

Effects of Carbonization Temperature on Nature of Nanostructured Electrode Materials Derived from Fe-MOF for Supercapacitors

NASA Astrophysics Data System (ADS)

Sui, Yanwei; Zhang, Dongling; Han, Yongpeng; Sun, Zhi; Qi, Jiqiu; Wei, Fuxiang; He, Yezeng; Meng, Qingkun

2018-05-01

This work successfully demonstrates various temperature carbonization of iron based metal organic framework to derive electrode materials for supercapacitors. Furthermore, impacts of calcined temperatures on the nature of as-prepared products are reported, and samples obtained at 300, 400, 500, 600 and 700 °C were investigated respectively. The products reveals excellent electrochemical performance. Carbonized at 600 °C, the composite materials display the highest specific capacitance of 972 F/g at a current density of 1 A/g. Carbonized at 500 °C, the capacitance retention of materials reach up to 93%. The high specific capacitance and excellent cyclic stability of the developed materials would exhibit nice prospect for the practical utilization of electrode materials.

Iron-oxide Aerogel and Xerogel Catalyst Formulations: Characterization by 57Fe Mössbauer and XAFS Spectroscopies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huggins, F.; Bali, S; Huffman, G

2010-01-01

Iron in various iron-oxide aerogel and xerogel catalyst formulations ({ge}85% Fe{sub 2}O{sub 3}; {le}10% K, Co, Cu, or Pd) developed for possible use in Fischer-Tropsch synthesis (FTS) or the water-gas-shift (WGS) reaction has been examined by {sup 57}Fe Moessbauer spectroscopy. The seventeen samples consisted of both as-prepared and calcined aerogels and xerogels and their products after use as catalysts for FTS or the WGS reaction. Complementary XAFS spectra were obtained on the occurrence of the secondary elements in some of the same materials. A broad, slightly asymmetric, two-peak Moessbauer spectrum was obtained from the different as-prepared and calcined catalyst formulationsmore » in the majority of cases. Such spectra could only be satisfactorily fit with three quadrupole doublet components, but no systematic trends in the isomer shift and quadrupole splitting parameters and area ratios of the individual components could be discerned that reflected variations in the composition or preparation of the aerogel or xerogel materials. However, significant reductions were noted in the Moessbauer effective thickness (recoilless absorption effect per unit mass of iron) parameter, {chi}{sub eff}/g, determined at room temperature, for aerogels and xerogels compared to bulk iron oxides, reflecting the openness and lack of rigidity of the aerogel and xerogel structures. Moessbauer measurements for two aerogels over the range from 15 to 292 K confirmed the greatly diminished nature of this parameter at room temperature. Major increases in the effective thickness parameter were observed when the open structure of the aerogel or xerogel collapsed during calcination resulting in the formation of iron oxides (hematite, spinel ferrite). Similar structural changes were indicated by increases in this parameter after use of iron-oxide aerogels as catalysts for FTS or the WGS reaction, during which the iron-oxide aerogel was converted to a mixture of nonstoichiometric magnetite and the Haegg carbide, {chi}-Fe{sub 5}C{sub 2}, or nonstoichiometric magnetite, respectively.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mohapatra, Pratyasha; Shaw, Santosh; Mendivelso-Perez, Deyny

Removing organics from hybrid nanostructures is a crucial step in many bottom-up materials fabrication approaches. It is usually assumed that calcination is an effective solution to this problem, especially for thin films. This assumption has led to its application in thousands of papers. Here in this paper, we show that this general assumption is incorrect by using a relevant and highly controlled model system consisting of thin films of ligand-capped ZrO 2 nanocrystals. After calcination at 800 °C for 12 h, while Raman spectroscopy fails to detect the ligands after calcination, elastic backscattering spectrometry characterization demonstrates that ~18% of themore » original carbon atoms are still present in the film. By comparison plasma processing successfully removes the ligands. Our growth kinetic analysis shows that the calcined materials have significantly different interfacial properties than the plasma-processed counterparts. Calcination is not a reliable strategy for the production of single-phase all-inorganic materials from colloidal nanoparticles.« less

Green Synthesis of ZnO Nanoparticles by an Alginate Mediated Ion-Exchange Process and a case study for Photocatalysis of Methylene Blue Dye

NASA Astrophysics Data System (ADS)

Keong, Choo Cheng; Sunitha Vivek, Yamini; Salamatinia, Babak; Amini Horri, Bahman

2017-04-01

In this study, zinc oxide (ZnO) was prepared via extrusion-dripping method through an ion exchange mediated process using sodium alginate. The samples were synthesized at 500 °C and 600 °C to study the effect of calcination temperature. The morphology, microstructure and optical activity of the calcined ZnO nanoparticles were analyzed by TGA, FESEM and XRD. It was found that ZnO nanoparticles synthesized at 600 °C was of higher purity with high crystallinity. To enhance the photocatalytic efficiency of zinc oxide, ZnO/NCC films were synthesized at varying ZnO loading fractions of 10 wt%, 15 wt%, 20 wt% and 25 wt% and were evaluated by photodegradation of Methylene blue dye and the highest dye percentage removal is found to be 96% which is obtained at ZnO loadings of 25 wt%. The usage of ion-exchange process has shown promising results in producing ZnO of desirable characteristics.

Short belt-like Ca 2 B 2 O 5 ·H 2 O nanostructures: Hydrothermal formation, FT-IR, thermal decomposition, and optical properties

NASA Astrophysics Data System (ADS)

Zhu, Wancheng; Zhang, Xiao; Wang, Xiaoli; Zhang, Heng; Zhang, Qiang; Xiang, Lan

2011-10-01

Uniform high crystallinity short belt-like Ca 2B 2O 5·H 2O nanostructures (nanobelts) were facilely synthesized through a room temperature coprecipitation of CaCl 2, H 3BO 3, and NaOH solutions, followed by a mild hydrothermal treatment (180 °C, 12.0 h). By a preferential growth parallel to the (1 0 0) planes, Ca 2B 2O 5·H 2O nanobelts with a length of 1-5 μm, a width of 100-400 nm, and a thickness of 55-90 nm were obtained. The calcination of the nanobelts at 500 °C for 2.0 h led to short Ca 2B 2O 5 nanobelts with well preserved 1D morphology. Calcination at 800 °C led to a mixture of Ca 2B 2O 5 and Ca 3B 2O 6. The products were with belt-like and quasi-polyhedron morphology, while they turned into pore-free micro-rod like and polyhedron morphology when the calcination was taken in the presence of NaCl. NaCl assisted high temperature calcination at 900 °C promoted the formation of Ca 3B 2O 6 in the products. When dispersed in deionized water or absolute ethanol, the Ca 2B 2O 5·H 2O nanobelts and Ca 2B 2O 5 nanobelts showed good transparency from the ultraviolet to the visible region. The as-synthesized Ca 2B 2O 5·H 2O and Ca 2B 2O 5 nanobelts can be employed as novel metal borate nanomaterials for further potential applications in the area of glass fibers, antiwear additive, ceramic coatings, and so on.

Hierarchically 3D assembled strontium titanate nanomaterials for water splitting application

NASA Astrophysics Data System (ADS)

Moniruddin, Md; Afroz, Khurshida; Shabdan, Yerkin; Bizri, Baraa; Nuraje, Nurxat

2017-10-01

Water splitting is an important technique to store solar energy in the simple form of chemical energy, such as hydrogen. Strontium titanate (SrTiO3) is one of the most promising photocatalysts to produce hydrogen gas from water splitting. In this research, an electrospinning technique in combination with sol-gel method was developed to synthesize 3D porous SrTiO3 nanostructures. Different crystallite sizes of SrTiO3-nanofibers (STO-NFs) were produced by varying the synthesis parameters including precursor concentration and calcination temperature. The synthesized nanofibers were characterized using DSC, TGA, XRD, SEM, and TEM. The crystallite size of STO-NFs decreases with increasing precursor concentration (3.03-15.78 vol.%) and gradually increases as the calcination temperature increases within the range of 600-800 °C. The photocatalytic activity of different STO-NFs (based on crystallite size) was also evaluated by the amount of H2 production from water splitting under UV irradiation. The H2 evolution study demonstrated that the photocatalytic activity of the STO-NFs strongly depends on the crystallite size of the nanofibers, precursor concentration, and calcination temperature. The H2 production rate increases with increasing crystallite size and temperature, whereas it decreases with increasing precursor concentration. The photocatalytic performance of the STO-NFs was also compared with the commercial SrTiO3 nanoparticles (STO-NPs) after Pt addition as a cocatalyst, where the synthesized nanofibers showed 2 times higher H2 production rate (1.14 mmol/g-h) than that of the nanoparticles. This synthesis technique provides a good example to produce other inorganic photocatalytic 3D porous structure materials.

Electrochemical Performance of Ni-MOFs for Supercapacitors

NASA Astrophysics Data System (ADS)

Li, Yujuan; Song, Lili; Han, Yinghui; Wang, Guangyou

2018-03-01

In this work, the Ni-MOFs of electrode material has been synthesized, characterized and studied for the electrochemical properties of electrode materials. The effects of the doping amount of Ni, calcination temperature and time were studied in detail. The results suggested that the electrochemical properties were obviously improved by the Ni-MOFs of electrode material and the best preparation conditions can also improve the electrochemical properties of electrode materials. These results open a way for the design of tailored MOFs as electrode materials for supercapacitors.

Effect of SiO2 addition on photocatalytic activity, water contact angle and mechanical stability of visible light activated TiO2 thin films applied on stainless steel by a sol gel method

NASA Astrophysics Data System (ADS)

Momeni, Mansour; Saghafian, Hasan; Golestani-Fard, Farhad; Barati, Nastaran; Khanahmadi, Amirhossein

2017-01-01

Nanostructured N doped TiO2/20%SiO2 thin films were developed on steel surface via sol gel method using a painting airbrush. Thin films then were calcined at various temperatures in a range of 400-600 °C. The effect of SiO2 addition on phase composition and microstructural evolution of N doped TiO2 films were studied using XRD and FESEM. Optical properties, visible light photocatalytic activity, hydrophilic behavior, and mechanical behavior of the films were also investigated by DRS, methylene blue degradation, water contact angle measurements, and nanoscratch testing. Results indicated that the band gap energy of N doped TiO2/SiO2 was increased from 2.93 to 3.09 eV. Crack formation during calcination was also significantly promoted in the composite films. All composite films demonstrated weaker visible light photocatalytic activities and lower mechanical stability in comparison with N doped TiO2 films. Moreover, the N doped TiO2/SiO2 film calcined at 600 °C showed undesirable hydrophilic behavior with a water contact angle of 57° after 31 h of visible light irradiation. Outcomes of the present study reveal some different results to previous reports on TiO2/SiO2 films. In general, we believe the differences in substrate material as well as application in visible light are the main reasons for the above mentioned contradiction.

Nanostructure of aluminium (Al) - Doped zinc oxide (AZO) thin films

NASA Astrophysics Data System (ADS)

Hussin, Rosniza; Husin, M. Asri

2017-12-01

Aluminium (Al)-doped Zinc Oxide (ZnO) was deposited on glass substrates by using the sol-gel dip coating technique. Next, AZO sol-gel solution was produced via sol-gel method. Al was used as doped element with molar ratios of 1%, 2%, and 3%, while the calcination temperatures were set at 400°C, 500°C, and 600°C for 2 hours. In fact, characterization was carried out in order to determine the effect of calcination temperature and molar ratio of doping by using several techniques, such as X-Ray Diffraction (XRD), Atomic Force Microscopy (AFM), Field Emission Scanning Electron Microscopy (FESEM), and Ultraviolet-Visible spectroscopy (UV-Vis). XRD was performed to investigate the crystal structure in which the ZnO was in wurtzite hexagonal form. Next, Energy Dispersive Spectroscopy (EDS) was used to determine the composition of thin films where the result revealed the existence of zinc, oxygen, and aluminium. The roughness of the deposited film was later measured by using the AFM approach where the findings indicated increment in RMS from 8.496 nm to 35.883 nm as the temperature was increased. Additionally, FESEM was carried out to look into the microstructure surfaces of the deposited AZO thin film for increased temperature caused the particle to grow bigger for all molar ratio of dopant. Lastly, UV-Vis was conducted to study the optical properties of AZO, in which the result demonstrated that AZO thin film possessed the highest transmittance percentage among all samples above 90% with band gap value that ranged from 3.25 eV to 3.32 eV.

Transformation Toughening of Composite Ceramics

DTIC Science & Technology

1992-12-31

Ca 2SiO 4 ) entiwickelt. Als Sili:ium-haltiger Prekursor i’urde has been well studied ’ 2 because of the considerable Siliziumdioxid veruiendet. Diese ...of carbon diffraction (XRD). This was after calcination for formed during the pyrolysis . The thermal decompo- I min at temperatures in the range...ques respectively. Some of the powders were also temperature for 1 min and cooled. At temperatures examined by SEM. below the pyrolysis stage the

Crystalline maricite NaFePO4 as a positive electrode material for sodium secondary batteries operating at intermediate temperature

NASA Astrophysics Data System (ADS)

Hwang, Jinkwang; Matsumoto, Kazuhiko; Orikasa, Yuki; Katayama, Misaki; Inada, Yasuhiro; Nohira, Toshiyuki; Hagiwara, Rika

2018-02-01

Maricite NaFePO4 (m-NaFePO4) was investigated as a positive electrode material for intermediate-temperature operation of sodium secondary batteries using ionic liquid electrolytes. Powdered m-NaFePO4 was prepared by a conventional solid-state method at 873 K and subsequently fabricated in two different conditions; one is ball-milled in acetone and the other is re-calcined at 873 K after the ball-milling. Electrochemical properties of the electrodes prepared with the as-synthesized m-NaFePO4, the ball-milled m-NaFePO4, and the re-calcined m-NaFePO4 were investigated in Na[FSA]-[C2C1im][FSA] (C2C1im+ = 1-ethyl-3-methylimidazolium, FSA- = bis(fluorosulfonyl)amide) ionic liquid electrolytes at 298 K and 363 K to assess the effects of temperature and particle size on their electrochemical properties. A reversible charge-discharge capacity of 107 mAh g-1 was achieved with a coulombic efficiency >98% from the 2nd cycle using the ball-milled m-NaFePO4 electrode at a C-rate of 0.1 C and 363 K. Electrochemical impedance spectroscopy using m-NaFePO4/m-NaFePO4 symmetric cells indicated that inactive m-NaFePO4 becomes an active material through ball-milling treatment and elevation of operating temperature. X-ray diffraction analysis of crystalline m-NaFePO4 confirmed the lattice contraction and expansion upon charging and discharging, respectively. These results indicate that the desodiation-sodiation process in m-NaFePO4 is reversible in the intermediate-temperature range.

Solid state microwave synthesis of highly crystalline ordered mesoporous hausmannite Mn 3 O 4 films

DOE PAGES

Xia, Yanfeng; Qiang, Zhe; Lee, Byeongdu; ...

2017-06-23

Microwave calcination of ordered micelle templated manganese carbonate films leads to highly crystalline, ordered mesoporous manganese oxide, while similar temperatures in a furnace lead to disordered, amorphous manganese oxide.

Photocatalytic Degradation of DIPA Using Bimetallic Cu-Ni/TiO2 Photocatalyst under Visible Light Irradiation

PubMed Central

Bustam, Mohamad Azmi; Chong, Fai Kait; Man, Zakaria B.; Khan, Muhammad Saqib; Shariff, Azmi M.

2014-01-01

Bimetallic Cu-Ni/TiO2 photocatalysts were synthesized using wet impregnation (WI) method with TiO2 (Degussa-P25) as support and calcined at different temperatures (180, 200, and 300°C) for the photodegradation of DIPA under visible light. The photocatalysts were characterized using TGA, FESEM, UV-Vis diffuse reflectance spectroscopy, fourier transform infrared spectroscopy (FTIR) and temperature programmed reduction (TPR). The results from the photodegradation experiments revealed that the Cu-Ni/TiO2 photocatalysts exhibited much higher photocatalytic activities compared to bare TiO2. It was found that photocatalyst calcined at 200°C had the highest photocatalyst activities with highest chemical oxygen demand (COD) removal (86.82%). According to the structural and surface analysis, the enhanced photocatalytic activity could be attributed to its strong absorption into the visible region and high metal dispersion. PMID:25105158

Structural study of VO {sub x} doped aluminium fluoride and aluminium oxide catalysts

DOE Office of Scientific and Technical Information (OSTI.GOV)

Scheurell, Kerstin; Scholz, Gudrun; Kemnitz, Erhard

The structural properties of vanadium doped aluminium oxyfluorides and aluminium oxides, prepared by a modified sol-gel synthesis route, were thoroughly investigated. The influence of the preparation technique and the calcination temperature on the coordination of vanadium, aluminium and fluorine was analysed by different spectroscopic methods such as Raman, MAS NMR and ESR spectroscopy. In all samples calcined at low temperatures (350 deg. C), vanadium coexists in two oxidation states V{sup IV} and V{sup V}, with V{sup IV} as dominating species in the vanadium doped aluminium oxyfluorides. In the fluoride containing solids aluminium as well as vanadium are coordinated by fluorinemore » and oxygen. Thermal annealing of 800 deg. C leads to an extensive reorganisation of the original matrices and to the oxidation of V{sup IV} to V{sup V} in both systems. - Graphical abstract: Structure model for VO {sub x} doped aluminium oxide.« less

Highly transparent, flexible, and thermally stable superhydrophobic ORMOSIL aerogel thin films.

PubMed

Budunoglu, Hulya; Yildirim, Adem; Guler, Mustafa O; Bayindir, Mehmet

2011-02-01

We report preparation of highly transparent, flexible, and thermally stable superhydrophobic organically modified silica (ORMOSIL) aerogel thin films from colloidal dispersions at ambient conditions. The prepared dispersions are suitable for large area processing with ease of coating and being directly applicable without requiring any pre- or post-treatment on a variety of surfaces including glass, wood, and plastics. ORMOSIL films exhibit and retain superhydrophobic behavior up to 500 °C and even on bent flexible substrates. The surface of the films can be converted from superhydrophobic (contact angle of 179.9°) to superhydrophilic (contact angle of <5°) by calcination at high temperatures. The wettability of the coatings can be changed by tuning the calcination temperature and duration. The prepared films also exhibit low refractive index and high porosity making them suitable as multifunctional coatings for many application fields including solar cells, flexible electronics, and lab on papers.

Positron annihilation lifetime spectroscopy (PALS) study of the as prepared and calcined MFI zeolites

NASA Astrophysics Data System (ADS)

Bosnar, Sanja; Vrankić, Martina; Bosnar, Damir; Ren, Nan; Šarić, Ankica

2017-11-01

The synthesis of high silica zeolites in many cases implies the usage of organic structural direction agents (SDA). However, to manifest their functionalities, the SDA occluded inside the channels of the as-synthesized structure should be removed, usually by a high temperature treatment (calcination). In this paper, the positron annihilation lifetime spectroscopy (PALS) was used to monitor the development of accessible spaces, their sizes and distributions in MFI zeolites, ZSM-5 and silicalite-1 in order to give an additional insight in the process of the SDA removal. For that purpose, a conventional PALS setup with 22Na positron source was applied. It was established that there is a pronounced difference between positron annihilation data for these two zeolites of the same structural type. The samples were additionally analysed by X-ray powder diffraction at room temperature with a crystal structure refinement and thermogravimetry.

Sol gel method for synthesis of semiconducting ferrite and the study of FTIR, DTA, SEM and CV

NASA Astrophysics Data System (ADS)

Alva, Sagir; Hua, Tang Ing; Kalmar Nizar, Umar; Wahyudi, Haris; Sundari, Rita

2018-03-01

In this study, a sol gel method using citric acid as anionic surfactant is used for synthesis of magnesium ferrite. Calcinations of magnesium ferrite at temperature (300°C, 600°C and 800°C) have been conducted after sol gel process. Characterization study of the prepared magnesium ferrite related to calcinations using Fourier transform infrared spectrometry (FTIR), Differential thermogravic analysis (DTA), and Scanning electron microscope (SEM) has been discussed. The study of Cyclic voltammetry (CV) of the prepared magnesium ferrite has been examined to assay the semiconducting behavior of magnesium ferrite in relation to its electrochemical behavior.

Synthesis of alumina ceramic encapsulation for self-healing materials on thermal barrier coating

NASA Astrophysics Data System (ADS)

Golim, O. P.; Prastomo, N.; Izzudin, H.; Hastuty, S.; Sundawa, R.; Sugiarti, E.; Thosin, K. A. Z.

2018-03-01

Durability of Thermal Barrier Coating or TBC can be optimized by inducing Self-Healing capabilities with intermetallic materials MoSi2. Nevertheless, high temperature operation causes the self-healing materials to become oxidized and lose its healing capabilities. Therefore, a method to introduce ceramic encapsulation for MoSi2 is needed to protect it from early oxidation. The encapsulation process is synthesized through a simple precipitation method with colloidal aluminum hydroxide as precursor and variations on calcination process. Semi-quantitative analysis on the synthesized sample is done by using X-ray diffraction (XRD) method. Meanwhile, qualitative analysis on the morphology of the encapsulation was carried out by using Scanning Electron Microscope (SEM) and Field Emission Scanning Electron Microscope (FESEM) equipped with dual Focus Ion Beam (FIB). The result of the experiment shows that calcination process significantly affects the final characteristic of encapsulation. The optimum encapsulation process was synthesized by colloidal aluminum hydroxide as a precursor, with a double step calcination process in low pressure until 900 °C.

Synthesis and Characterization Materials M-Barium Hexaferrite Doping Ions Co-Mn Nano Particle

NASA Astrophysics Data System (ADS)

Susilawati; Doyan, A.; Sahlam

2017-05-01

This research has been success in the synthesis of M-Barium hexaferrite (BaM) doping Co-Mn ions using coprecipitation method are expected to be applied as a base material in the coating RADAR. M-Barium hexaferrite (BaM) are BaFe12-2xCoxMnxO19 synthesized with various concentrations (x = 0.0, 0.1, 0.2, 0.3) and the calcinations temperature (T = 400°C, 600°C, 800°C). The materials characterization using a X-Ray Diffraction (XRD), Transmission Electron Microscope (TEM), Inductance Capacitance and resistance (LCR) meter, and Vibrating Sample Magnetometer (VSM) Instruments. The measurement results using XRD shows the material has a hexagonal crystalline structure. The measurement results using a TEM show a sample of nano crystal materials with grain diameters up to 40 nm and spacing of the crystal lattice. The measurement results using a LCR-meter shows the electric conductivity of 1.15 × 10-6 S/cm to BaM without doping, 3.75 × 10-6 S/cm to 0.1 doping concentration calcination temperature of 400 °C, and 1,23 × 10-5 S/cm to 0.3 doping concentration calcination temperature of 800 °C, thus including semiconductor materials. The magnetic properties of materials using a VSM test results show the value of coercivity of 0.1 T; remanence value of 0.06 emu/g; and the saturation value of 0.42 emu/g. The results above show BaM Co-Mn metal doping potential as anti-radar material.

Thermal decomposition of dolomite under CO2: insights from TGA and in situ XRD analysis.

PubMed

Valverde, Jose Manuel; Perejon, Antonio; Medina, Santiago; Perez-Maqueda, Luis A

2015-11-28

Thermal decomposition of dolomite in the presence of CO2 in a calcination environment is investigated by means of in situ X-ray diffraction (XRD) and thermogravimetric analysis (TGA). The in situ XRD results suggest that dolomite decomposes directly at a temperature around 700 °C into MgO and CaO. Immediate carbonation of nascent CaO crystals leads to the formation of calcite as an intermediate product of decomposition. Subsequently, decarbonation of this poorly crystalline calcite occurs when the reaction is thermodynamically favorable and sufficiently fast at a temperature depending on the CO2 partial pressure in the calcination atmosphere. Decarbonation of this dolomitic calcite occurs at a lower temperature than limestone decarbonation due to the relatively low crystallinity of the former. Full decomposition of dolomite leads also to a relatively low crystalline CaO, which exhibits a high reactivity as compared to limestone derived CaO. Under CO2 capture conditions in the Calcium-Looping (CaL) process, MgO grains remain inert yet favor the carbonation reactivity of dolomitic CaO especially in the solid-state diffusion controlled phase. The fundamental mechanism that drives the crystallographic transformation of dolomite in the presence of CO2 is thus responsible for its fast calcination kinetics and the high carbonation reactivity of dolomitic CaO, which makes natural dolomite a potentially advantageous alternative to limestone for CO2 capture in the CaL technology as well as SO2in situ removal in oxy-combustion fluidized bed reactors.

Development of Highly Durable and Reactive Regenerable Magnesium-Based Sorbents for CO2 Separation in Coal Gasification Process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Javad Abbasian; Armin Hassanzadeh Khayyat; Rachid B. Slimane

The specific objective of this project was to develop physically durable and chemically regenerable MgO-based sorbents that can remove carbon dioxide from raw coal gas at operating condition prevailing in IGCC processes. A total of sixty two (62) different sorbents were prepared in this project. The sorbents were prepared either by various sol-gel techniques (22 formulations) or modification of dolomite (40 formulations). The sorbents were prepared in the form of pellets and in granular forms. The solgel based sorbents had very high physical strength, relatively high surface area, and very low average pore diameter. The magnesium content of the sorbentsmore » was estimated to be 4-6 % w/w. To improve the reactivity of the sorbents toward CO{sub 2}, The sorbents were impregnated with potassium salts. The potassium content of the sorbents was about 5%. The dolomite-based sorbents were prepared by calcination of dolomite at various temperature and calcination environment (CO{sub 2} partial pressure and moisture). Potassium carbonate was added to the half-calcined dolomite through wet impregnation method. The estimated potassium content of the impregnated sorbents was in the range of 1-6% w/w. In general, the modified dolomite sorbents have significantly higher magnesium content, larger pore diameter and lower surface area, resulting in significantly higher reactivity compared to the sol-gel sorbents. The reactivities of a number of sorbents toward CO{sub 2} were determined in a Thermogravimetric Analyzer (TGA) unit. The results indicated that at the low CO{sub 2} partial pressures (i.e., 1 atm), the reactivities of the sorbents toward CO{sub 2} are very low. At elevated pressures (i.e., CO{sub 2} partial pressure of 10 bar) the maximum conversion of MgO obtained with the sol-gel based sorbents was about 5%, which corresponds to a maximum CO{sub 2} absorption capacity of less than 1%. The overall capacity of modified dolomite sorbents were at least one order of magnitude higher than those of the sol-gel based sorbents. The results of the tests conducted with various dolomite-based sorbent indicate that the reactivity of the modified dolomite sorbent increases with increasing potassium concentration, while higher calcination temperature adversely affects the sorbent reactivity. Furthermore, the results indicate that as long as the absorption temperature is well below the equilibrium temperature, the reactivity of the sorbent improves with increasing temperature (350-425 C). As the temperature approaches the equilibrium temperature, because of the significant increase in the rate of reverse (i.e., regeneration) reaction, the rate of CO{sub 2} absorption decreases. The results of cyclic tests show that the reactivity of the sorbent gradually decreases in the cyclic process. To improve long-term durability (i.e., reactivity and capacity) of the sorbent, the sorbent was periodically re-impregnated with potassium additive and calcined. The results indicate that, in general, re-treatment improves the performance of the sorbent, and that, the extent of improvement gradually decreases in the cyclic process. The presence of steam significantly enhances the sorbent reactivity and significantly decreases the rate of decline in sorbent deactivation in the cyclic process.« less

Synthesis, characterization and photocatalytic properties of Mg1-xZnxAl2O4 spinel nanoparticles

NASA Astrophysics Data System (ADS)

Li, Hui; Liu, Yuqin; Tang, Junkai; Deng, Yanxi

2016-08-01

Mg1-xZnxAl2O4 spinel nanoparticles with x = 0, 0.05, 0.10, 0.15 and 0.20 were prepared via the chemical coprecipitation method. The obtained samples were characterised by thermal gravimetric and differential scanning calorimetry, X-ray diffraction, Fourier transform infrared spectroscopy, UV-Vis diffuse reflection spectrum, transmission electron microscopy and 27Al MAS-NMR spectroscopy. Mg1-xZnxAl2O4 spinel powders with the mean crystallite size of around 11 nm-14 nm were obtained. The crystallinity of the MgAl2O4 samples increases with the increase in the calcination temperature. At the same calcination temperature, higher amount of Zn2+ substitution leads to the higher level of crystallinity, but has no apparent influence on the mean crystallite size of the samples. The photocatalytic activity of the obtained Mg1-xZnxAl2O4 spinel nanoparticles was evaluated by monitoring the degradation of methylene blue under UV light. The degradation rates of methylene blue using the MgAl2O4 nanoparticles prepared at the calcination temperatures of 700 °C and 800 °C are much higher than those prepared at 900 °C and 1000 °C. The photocatalytic activities of the spinel powders with lower level of Zn2+ substitution such as Mg0.95Zn0.05Al2O4 are inferior to that of MgAl2O4. Results of 27Al MAS-NMR spectroscopy analysis and the first principle total density of state calculations reveal that this is probably due to the substitutions of Zn2+ decreasing the degree of Al3+ ions inversion over the sites of tetrahedral and octahedral coordination. With the increase in the amounts of Zn2+ substitution, the effects of Zn2+ additions on the photocatalytic activities become gradually predominant, leading to the increases in the degradation rates. The methylene blue degraded by 99% within 4 h using the Mg0.8Zn0.2Al2O4 spinel powders.

Anomalous dielectric behavior in nanoparticle Eu2O3 : SiO2 glass composite system

NASA Astrophysics Data System (ADS)

Mukherjee, S.; Chen, C. H.; Chou, C. C.; Yang, H. D.

2010-12-01

Eu2O3 (0.5 mol%) nanoparticles have been synthesized in a silica glass matrix by the sol-gel method at calcination temperatures of 700 °C and above. Compared with the parent material SiO2, this nano-glass composite system shows enhancement of dielectric constant and diffuse phase transition along with magnetodielectric effect around room temperature (~270 K). The observed conduction mechanism is found to be closely related to the thermally activated oxygen vacancies. Magnetodielectric behavior is strongly associated with magnetoresistance changes, depending on the nanoparticle size and separation. Such a material might be treated as a potential candidate for device miniaturization.

The Microscopic Magnetic Properties of W-type Hexaferrite Powder Prepared by A Sol-Gel Route

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jotania, Rajshree; Chauhan, Chetna; Sharma, Pooja

2010-12-01

Magnetic particles of W-type barium-calcium hexaferrite (BaCa{sub 2}Fe{sub 16}O{sub 27}) have been synthesized using a Stearic acid gel route. The gel precursors were dried at 100 deg. C for 2 hrs and then calcinated at 650 deg. C, 750 deg. C, 850 deg. C and 950 deg. C for 4 hrs in a furnace and slowly cooled to room temperature in order to obtain barium-calcium hexaferrite particles. The microscopic magnetic properties of prepared samples studying using Moessbauer spectroscopy. Moessbauer spectra of all samples were recorded at room temperature. Mossbauer parameters like Isomer shift, Quadruple splitting etc. were calculated with respectmore » to iron foil. Barium calcium hexaferrite samples heated at 650 deg. C, 750 deg. C, 850 deg. C show relaxation type Moessbauer spectra along with paramagnetic doublet. The intensity of paramagnetic doublet increases with temperature confirm the presence of ferrous ions in the samples, where as sample calcinated at 950 deg. C confirm the presence of ferrimagnetic phase with partial super paramagnetic nature of prepared hexaferrite sample.« less

Fast and simple microwave synthesis of TiO2/Au nanoparticles for gas-phase photocatalytic hydrogen generation

NASA Astrophysics Data System (ADS)

May-Masnou, Anna; Soler, Lluís; Torras, Miquel; Salles, Pol; Llorca, Jordi; Roig, Anna

2018-04-01

The fabrication of small anatase titanium dioxide (TiO2) nanoparticles (NPs) attached to larger anisotropic gold (Au) morphologies by a very fast and simple two-step microwave-assisted synthesis is presented. The TiO2/Au NPs are synthesized using polyvinylpyrrolidone (PVP) as reducing, capping and stabilizing agent through a polyol approach. To optimize the contact between the titania and the gold and facilitate electron transfer, the PVP is removed by calcination at mild temperatures. The nanocatalysts activity is then evaluated in the photocatalytic production of hydrogen from water/ethanol mixtures in gas-phase at ambient temperature. A maximum value of 5.3 mmol·gcat-1·h-1 (7.4 mmol·gTiO2-1·h-1) of hydrogen is recorded for the system with larger gold particles at an optimum calcination temperature of 450 °C. Herein we demonstrate that TiO2-based photocatalysts with high Au loading and large Au particle size (≈ 50 nm) NPs have photocatalytic activity.

Room temperature ferromagnetism in non-magnetic doped TiO2 nanoparticles

NASA Astrophysics Data System (ADS)

Gómez-Polo, C.; Larumbe, S.; Pastor, J. M.

2013-05-01

Room-temperature ferromagnetism in non-magnetic doped TiO2 semiconductor nanoparticles is analyzed in the present work. Undoped and N-doped TiO2 nanoparticles were obtained employing sol-gel procedure using urea as the nitrogen source. The obtained gels were first dried at 70 °C and afterwards calcined in air at 300 °C. A residual carbon concentration was retained in the samples as a consequence of the organic decomposition process. Post-annealing treatments at 300 °C under air and vacuum conditions were also performed. The crystallographic structure of nanoparticles was analyzed by X-ray diffraction, obtaining a single anatase crystalline phase after the calcinations (mean nanoparticle diameters around 5-8 nm). SQUID magnetometry was employed to analyze the magnetic response of the samples. Whereas for the undoped samples synthesized with hydrolysis rate h = 6, paramagnetic like behavior is observed at room temperature, the N-doped nanoparticles (h = 3) show a weak ferromagnetic response (saturation magnetization ≈10-3 emu/g). Moreover, a clear reinforcement of the room-temperature ferromagnetism response is found with the post-annealing treatments, in particular that performed in vacuum. Thus, the results indicate the dominant role of the oxygen stoichiometry and the oxygen vacancies in the room temperature ferromagnetic response of these TiO2 nanoparticles.

Calcinated tea and cellulose composite films and its dielectric and lead adsorption properties.

PubMed

Jayaramudu, Tippabattini; Varaprasad, Kokkarachedu; Kim, Hyun Chan; Kafy, Abdullahil; Kim, Jung Woong; Kim, Jaehwan

2017-09-01

In this paper, calcinated tea and cellulose composite (CTCC) films were fabricated via solution casting method. Chemical structure, morphology, crystallinity and thermal stability of the fabricated films were characterized by using Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction and thermogravimetric analysis. The effect of calcinated tea loading on the properties of the prepared CTCC films was studied. The results suggest that the prepared CTCC films show higher mechanical properties, thermal stability and dielectric constant than the neat cellulose film. In addition, the CTCC films adsorb Pb 2+ ions and its adsorption performance depends on the calcinated tea content and pH level. The CTCC films are useful for sensors, flexible capacitor as well as lead adsorption applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Phase equilibrium and preparation, crystallization and viscous sintering of glass in the alumina-silica-lanthanum phosphate system

NASA Astrophysics Data System (ADS)

He, Feng

The phase equilibrium, viscosity of melt-quenched glasses, and processing of sol-gel glasses of the alumina-silica-lanthanum phosphate system were studied. These investigations were directed towards serving the objective of synthesizing nano-structured ceramic-matrix-composites via controlled crystallization of glass precursors. The thermal stability, phase equilibrium, and liquidus temperatures of the alumina- and mullite-lanthanum phosphate systems are determined. An iridium wire heater was constructed to anneal samples up to 2200°C. Phosphorus evaporation losses were significant at high temperatures, especially over 1800°C. The tentative phase diagrams of the two quasi-binary systems were presented. The viscosity of the melt-quenched mullite-lanthanum phosphate glasses was measured by three different methods, including viscous sintering of glass powder compacts, neck formation between two Frenkel glass beads, and thermal analysis of the glass transition. Improved methodologies were developed for applying the interpretative mathematical models to the results of the sintered powder and thermal analytical experiments. Good agreement was found between all three methods for both absolute values and temperature dependence. A sol-gel process was developed as a low temperature route to producing glasses. A unique, single phase mullite gel capable of low temperature (575°C) mullitization was made from tetraethoxysilane and aluminum isopropoxide at room temperature in three days. Low temperature crystallization was attributed to the avoidance of phase segregation during gel formation and annealing. This was greatly enhanced by a combination of low temperature preheating in the amorphous state, a high heating rate during crystallization and low water content. The Al2O3 content in mullite (61-68 mol%) depended on the highest annealing temperature. Two mullite-lanthanum phosphate gels were made based upon modifying the chemical procedures used for the homogeneous single phase and heterogeneous diphasic mullite gels from same starting chemicals. Amorphous powders were obtained after optimized calcinations. Their different crystallization routes and sintering behavior were investigated and correlated with the different homogeneities of precursor gels. Structurally stable open, porous ceramics (up to 80% porosity) were produced from the single-phase gel derived powder, where gases exsolved during calcination caused foaming coincident with sintering. Translucent, dense glass ceramic was made from the calcined diphasic gel by hot-pressing.

Alumina Calcination in the Fluid-Flash Calciner

NASA Astrophysics Data System (ADS)

Fish, William M.

In the mid 40's, Alcoa turned to fluidized solids techniques as a means of improving the efficiency of the alumina calcining process. This paper traces calciner development from the first pilot operation in 1946 through the first plant fluid-bed unit in 1952, the early "fluid-flash" calciner designs in 1960, the first 300 ton/day fluid-flash calciner at Alcoa's Bauxite, Arkansas plant in 1963, the 600 ton/day calciners installed in Suriname and Australia in 1965 and 1966, up to the 1500 ton/day Mark III calciners now operating in Jamaica, Australia and the United States. These Mark III fluid-flash calciners have provided a 30 to 40 percent fuel saving in addition to major savings in capital investment and maintenance costs.

The preparation and characterization of La doped TiO 2 nanoparticles and their photocatalytic activity

NASA Astrophysics Data System (ADS)

Liqiang, Jing; Xiaojun, Sun; Baifu, Xin; Baiqi, Wang; Weimin, Cai; Honggang, Fu

2004-10-01

In this paper, pure and La doped TiO2 nanoparticles with different La content were prepared by a sol-gel process using Ti (OC4H9)4 as raw material, and also were characterized by XRD, TG-DTA, TEM, XPS, DRS and Photoluminescence (PL) spectra. We mainly investigated the effects of calcining temperature and La content on the properties and the photocatalytic activity for degrading phenol of as-prepared TiO2 samples, and also discussed the relationships between PL spectra and photocatalytic activity as well as the mechanisms of La doping on TiO2 phase transformation. The results showed that La3+ did not enter into the crystal lattices of TiO2 and was uniformly dispersed onto TiO2 as the form of La2O3 particles with small size, which possibly made La dopant have a great inhibition on TiO2 phase transformation; La dopant did not give rise to a new PL signal, but it could improve the intensity of PL spectra with a appropriate La content, which was possibly attributed to the increase in the content of surface oxygen vacancies and defects after doping La; La doped TiO2 nanoparticles calcined at 600°C exhibited higher photocatalytic activity, indicating that 600°C was an appropriate calcination temperature. The order of photocatalytic activity of La doped TiO2 samples with different La content was as following: 1>1.5>3>0.5>5>0 mol%, which was the same as the order of their PL intensity, namely, the stronger the PL intensity, the higher the photocatalytic activity, demonstrating that there were certain relationships between PL spectra and photocatalytic activity. This could be explained by the points that PL spectra mainly resulted from surface oxygen vacancies and defects during the process of PL, while surface oxygen vacancies and defects could be favorable in capturing the photoinduced electrons during the process of photocatalytic reactions.

Preparation of a new Fenton-like catalyst from red mud using molasses wastewater as partial acidifying agent.

PubMed

Wei, Guangtao; Shao, Luhua; Mo, Jihua; Li, Zhongmin; Zhang, Linye

2017-06-01

Using molasses wastewater as partial acidifying agent, a new Fenton-like catalyst (ACRM sm ) was prepared through a simple process of acidification and calcination using red mud as main material. With molasses wastewater, both the free alkali and the chemically bonded alkali in red mud were effectively removed under the action of H 2 SO 4 and molasses wastewater, and the prepared ACRM sm was a near-neutral catalyst. The ACRM sm preparation conditions were as follows: for 3 g of red mud, 9 mL of 0.7 mol/L H 2 SO 4 plus 2 g of molasses wastewater as the acidifying agent, calcination temperature 573 K, and calcination time 1 h. Iron phase of ACRM sm was mainly α-Fe 2 O 3 and trace amount of carbon existed in ACRM sm . The addition of molasses wastewater not only effectively reduced the consumption of H 2 SO 4 in acidification of red mud but also resulted in the generation of carbon and significantly improved the distribution of macropore in prepared ACRM sm . It was found that near-neutral pH of catalyst, generated carbon, and wide distribution of macropore were the main reasons for the high catalytic activity of ACRM sm . The generated carbon and wide distribution of macropore were entirely due to the molasses wastewater added. In degradation of orange II, ACRM sm retained most of its catalytic stability and activity after five recycling times, indicating ACRM sm had an excellent long-term stability in the Fenton-like process. Furthermore, the performance test of settling showed ACRM sm had an excellent settleability. ACRM sm was a safe and green catalytic material used in Fenton-like oxidation for wastewater treatment.

Process parameters in the manufacture of ceramic ZnO nanofibers made by electrospinning

NASA Astrophysics Data System (ADS)

Nonato, Renato C.; Morales, Ana R.; Rocha, Mateus C.; Nista, Silvia V. G.; Mei, Lucia H. I.; Bonse, Baltus C.

2017-01-01

Zinc oxide (ZnO) nanofibers were prepared by electrospinning under different conditions using a solution of poly(vinyl alcohol) and zinc acetate as precursor. A 23 factorial design was made to study the influence of the process parameters in the electrospinning (collector distance, flow rate and voltage), and a 22 factorial design was made to study the influence of the calcination process (time and temperature). SEM images were made to analyze the fiber morphology before and after calcination process, and the images were made to measure the nanofiber diameter. X-ray diffraction was made to analyze the total precursor conversion to ZnO and the elimination of the polymeric carrier.

Modification of the ECAS reference steam power generating plant to comply with the EPA 1979 new source performance standards

NASA Technical Reports Server (NTRS)

Fogelson, S. A.; Chait, I. L.; Bradley, W. J.; Benson, W.

1980-01-01

Detailed capital cost estimates for the ECAS and modified reference plants in mid-1978 dollars for both 250 and 175 F (394 and 353 K) stack gas reheat temperatures based on the cost estimates developed for the ECAS study are presented. The scope of the work included technical assessment of sulfur dioxide scrubber system design, on site calcination versus purchased lime, reheat of stack gas, effect of sulfur dioxide scrubber on particulate emission, and control of nitrogen oxides.

Geochemistry of highly basic calcium hydroxide groundwater in Jordan

USGS Publications Warehouse

Barnes, I.; Presser, T.S.; Saines, M.; Dickson, P.; Van Groos, A. F. K.

1982-01-01

Highly-alkaline (pH > 12.5) meteoric waters of a Ca2+OH--type issue from naturally calcined bituminous marl. The cold (16.5 ??? T(??C) ??? 19.1) waters are super-saturated with minerals thought to be of high-temperature origin. ?? 1982.

Ambient temperature NO oxidation over Cr-based amorphous mixed oxide catalysts: effects from the second oxide components

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Aiyong; Lin, Bo; Zhang, Hanlei

2017-01-01

Three series of Cr-based mixed oxides (Cr-Co, Cr-Fe, and Cr-Ni oxides) with high specific surface areas and amorphous textures were synthesized using a novel sol-gel method. These mixed oxides, in comparison to their pure metal oxide (CrOx, Co3O4, FeOx and NiO) counterparts, display enhanced performance for catalytic oxidation of low-concentration NO at room temperature. The best performing catalysts achieve 100% NO conversion for ~30 h of operation at a high space velocity of 45,000 ml g-1 h-1. The amorphous structure was found to be critical for these catalysts to maintain high activity and durability. Control of Cr/M (M=Co, Fe andmore » Ni) molar ratio, nitrate precursor decomposition temperature and catalyst calcination temperature was key to the synthesis of these highly active catalysts.« less

Evaluation of Vitrification Processing Step for Rocky Flats Incinerator Ash

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wigent, W.L.; Luey, J.K.; Scheele, R.D.

In 1997, Pacific Northwest National Laboratory (PNNL) staff developed a processing option for incinerator ash at the Rocky Flats Environmental Technology Sites (RFETS). This work was performed with support from Los Alamos National Laboratory (LANL) and Safe Sites of Colorado (SSOC). A description of the remediation needs for the RFETS incinerator ash is provided in a report summarizing the recommended processing option for treatment of the ash (Lucy et al. 1998). The recommended process flowsheet involves a calcination pretreatment step to remove carbonaceous material followed by a vitrification processing step for a mixture of glass tit and calcined incinerator ash.more » Using the calcination pretreatment step to remove carbonaceous material reduced process upsets for the vitrification step, allowed for increased waste loading in the final product, and improved the quality of the final product. Figure 1.1 illustrates the flow sheet for the recommended processing option for treatment of RFETS incinerator ash. In 1998, work at PNNL further developed the recommended flow sheet through a series of studies to better define the vitrification operating parameters and to address secondary processing issues (such as characterizing the offgas species from the calcination process). Because a prototypical rotary calciner was not available for use, studies to evaluate the offgas from the calcination process were performed using a benchtop rotary calciner and laboratory-scale equipment (Lucy et al. 1998). This report focuses on the vitrification process step after ash has been calcined. Testing with full-scale containers was performed using ash surrogates and a muffle furnace similar to that planned for use at RFETS. Small-scale testing was performed using plutonium-bearing incinerator ash to verify performance of the waste form. Ash was not obtained from RFETS because of transportation requirements to calcine the incinerator ash prior to shipment of the material. Because part of PNNL's work was to characterize the ash prior to calcination and to investigate the effect of calcination on product quality, representative material was obtained from LANL. Ash obtained from LANL was selected based on its similarity to that currently stored at RFETS. The plutonium-bearing ashes obtained from LANL are likely from a RFETS incinerator, but the exact origin was not identified.« less

Fabrication of nano structural biphasic materials from phosphogypsum waste and their in vitro applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mohamed, Khaled R., E-mail: Kh_rezk966@yahoo.com; Mousa, Sahar M.; Inorganic Chemistry Department, National Research Centre, Dokki, P.O. Box 12622, 11787 Cairo

2014-02-01

Graphical abstract: (a) Schema of the process, (b) TEM of nano particles of biphasic materials and (c) SEM of post-immersion. - Highlights: • Ratio of HA and β-TCP phases were controlled by thermal treatment. • HA partially decomposed into β-TCP with other bioactive phases. • Calcined HA at 900 °C is the best for the bioactivity behavior. - Abstract: In this study, a novel process of preparing biphasic calcium phosphate (BCP) is proposed. Also its bioactivity for the utilization of the prepared BCP as a biomaterial is studied. A mixture of calcium hydroxyapatite (HAP) and tricalcium phosphate (β-TCP) could bemore » obtained by thermal treatment of HAP which was previously prepared from phosphogypsum (PG) waste. The chemical and phase composition, morphology and particle size of prepared samples was characterized by X-ray diffraction (XRD), Infrared spectroscopy (IR), Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM). The bioactivity was investigated by soaking of the calcined samples in simulated body fluid (SBF). Results confirmed that the calcination temperatures played an important role in the formation of calcium phosphate (CP) materials. XRD results indicated that HAP was partially decomposed into β-TCP. The in vitro data confirmed that the calcined HAP forming BCP besides other phases such as pyrophosphate and silica are bioactive materials. Therefore, BCP will be used as good biomaterials for medical applications.« less

Human health risk characterization of petroleum coke calcining facility emissions.

PubMed

Singh, Davinderjit; Johnson, Giffe T; Harbison, Raymond D

2015-12-01

Calcining processes including handling and storage of raw petroleum coke may result in Particulate Matter (PM) and gaseous emissions. Concerns have been raised over the potential association between particulate and aerosol pollution and adverse respiratory health effects including decrements in lung function. This risk characterization evaluated the exposure concentrations of ambient air pollutants including PM10 and gaseous pollutants from a petroleum coke calciner facility. The ambient air pollutant levels were collected through monitors installed at multiple locations in the vicinity of the facility. The measured and modeled particulate levels in ambient air from the calciner facility were compared to standards protective of public health. The results indicated that exposure levels were, on occasions at sites farther from the facility, higher than the public health limit of 150 μg/m(3) 24-h average for PM10. However, the carbon fraction demonstrated that the contribution from the calciner facility was de minimis. Exposure levels of the modeled SO2, CO, NOx and PM10 concentrations were also below public health air quality standards. These results demonstrate that emissions from calcining processes involving petroleum coke, at facilities that are well controlled, are below regulatory standards and are not expected to produce a public health risk. Copyright © 2015 Elsevier Inc. All rights reserved.

40 CFR 98.86 - Data reporting requirements.

Code of Federal Regulations, 2012 CFR

2012-07-01

...) Monthly fraction of total CaO, total MgO, non-calcined CaO and non-calcined MgO in clinker for each kiln (as wt-fractions). (7) Method used to determine non-calcined CaO and non-calcined MgO in clinker. (8) Quarterly fraction of total CaO, total MgO, non-calcined CaO and non-calcined MgO in CKD not recycled to the...

Retrieval System for Calcined Waste for the Idaho Cleanup Project - 12104

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eastman, Randy L.; Johnston, Beau A.; Lower, Danielle E.

This paper describes the conceptual approach to retrieve radioactive calcine waste, hereafter called calcine, from stainless steel storage bins contained within concrete vaults. The retrieval system will allow evacuation of the granular solids (calcine) from the storage bins through the use of stationary vacuum nozzles. The nozzles will use air jets for calcine fluidization and will be able to rotate and direct the fluidization or displacement of the calcine within the bin. Each bin will have a single retrieval system installed prior to operation to prevent worker exposure to the high radiation fields. The addition of an articulated camera armmore » will allow for operations monitoring and will be equipped with contingency tools to aid in calcine removal. Possible challenges (calcine bridging and rat-holing) associated with calcine retrieval and transport, including potential solutions for bin pressurization, calcine fluidization and waste confinement, are also addressed. The Calcine Disposition Project has the responsibility to retrieve, treat, and package HLW calcine. The calcine retrieval system has been designed to incorporate the functions and technical characteristics as established by the retrieval system functional analysis. By adequately implementing the highest ranking technical characteristics into the design of the retrieval system, the system will be able to satisfy the functional requirements. The retrieval system conceptual design provides the means for removing bulk calcine from the bins of the CSSF vaults. Top-down vacuum retrieval coupled with an articulating camera arm will allow for a robust, contained process capable of evacuating bulk calcine from bins and transporting it to the processing facility. The system is designed to fluidize, vacuum, transport and direct the calcine from its current location to the CSSF roof-top transport lines. An articulating camera arm, deployed through an adjacent access riser, will work in conjunction with the retrieval nozzle to aid in calcine fluidization, remote viewing, clumped calcine breaking and recovery from off-normal conditions. As the design of the retrieval system progresses from conceptual to preliminary, increasing attention will be directed toward detailed design and proof-of- concept testing. (authors)« less

Biotemplated synthesis of high specific surface area copper-doped hollow spherical titania and its photocatalytic research for degradating chlorotetracycline

NASA Astrophysics Data System (ADS)

Bu, Dan; Zhuang, Huisheng

2013-01-01

Copper-doped titania (Cu/TiO2) hollow microspheres were fabricated using the rape pollen as biotemplates via an improved sol-gel method and a followed calcinations process. In the fabricated process, a titanium(IV)-isopropoxide-based sol directly coated onto the surface of rape pollen. Subsequently, after calcinations, rape pollen was removed by high temperature and the hollow microsphere structure was retained. The average diameter of as-obtained hollow microspheres is 15-20 μm and the thickness of shell is approximately 0.6 μm. Knowing from XRD results, the main crystal phase of microspheres is anatase, coupled with rutile. The specific surface area varied between 141.80 m2/g and 172.51 m2/g. This hollow sphere photocatalysts with high specific surface area exhibited stronger absorption ability and higher photoactivity, stimulated by visible light. The degradation process of chlortetracycline (CTC) solution had been studied. The degradated results indicate that CTC could be effective degradated by fabricated hollow spherical materials. And the intermediate products formed in the photocatalytic process had been identified.

Preparation of InYO3 catalyst and its application in photodegradation of molasses fermentation wastewater.

PubMed

Qin, Zuzeng; Liang, Yi; Liu, Zili; Jiang, Weiqing

2011-01-01

An InYO3 photocatalyst was prepared through a precipitation method and used for the degradation of molasses fermentation wastewater. The InYO3 photocatalyst characterized by X-ray diffraction (XRD), UV-Vis diffuse reflectance spectroscopy, surface area and porosimetry. Energy band structures and density of states were achieved using the Cambridge Serial Total Energy package (CASTEP). The results indicated that the photodegradation of molasses fermentation wastewater was significantly enhanced in the presence of InYO3 when compared with PbWO4. The calcination temperature was found to have a significant effect on the photocatalytic activity of InYO3. Specifically, InYO3 calcined at 700 degrees C had a considerably larger surface area and lower reflectance intensity and showed higher photocatalytic activity. The mathematical simulation results indicated that InYO3 is a direct band gap semiconductor, and its conduction band is composed of In 5p and Y 4d orbitals, whereas its valence band is composed of O 2p and In 5s orbitals.

Effect of boron on enhancing infrared emissivity of Ni-Cr system coating

NASA Astrophysics Data System (ADS)

Li, Yongjia; Ouyang, Taoyuan; Wang, Xiaohuan; Li, Shuhao; Mao, Jiawei; Cheng, Xudong

2018-03-01

High infrared emissivity coating possesses great value in practical application, whether in the military or civilian areas. In this study, B-NiCr precursor powder containing NiO, Cr2O3 and ZrB2 was calcined at 1300 °C and then used to prepare a high infrared emissivity B-NiCr coating via atmospheric plasma spraying. A large number of test methods were employed to analyze the powder and coating, including TG-DSC, XRD, FE-SEM, infrared spectrometer and so on. The result of infrared emissivity measurement indicates that the coating possesses maximum infrared emissivity of 0.908 at 1000 °C while the infrared emissivity is 0.901 after thermal shock test. Comparing with NiCr coating, Ni2CrO2(BO3) formed during calcination may be the main factor to improve the infrared emissivity of B-NiCr coating. The B-NiCr coating possesses good thermal shock resistance and can withstand 50 times thermal shock at least without falling off, from 800 °C to room temperature.

Isotopic Variability of Mercury in Ore, Mine-Waste Calcine, and Leachates of Mine-Waste Calcine from Areas Mined for Mercury

PubMed Central

2009-01-01

The isotopic composition of mercury (Hg) was determined in cinnabar ore, mine-waste calcine (retorted ore), and leachates obtained from water leaching experiments of calcine from two large Hg mining districts in the U.S. This study is the first to report significant mass-dependent Hg isotopic fractionation between cinnabar ore and resultant calcine. Data indicate that δ202Hg values relative to NIST 3133 of calcine (up to 1.52‰) in the Terlingua district, Texas, are as much as 3.24‰ heavier than cinnabar (−1.72‰) prior to retorting. In addition, δ202Hg values obtained from leachates of Terlingua district calcines are isotopically similar to, or as much as 1.17‰ heavier than associated calcines, most likely due to leaching of soluble, byproduct Hg compounds formed during ore retorting that are a minor component in the calcines. As a result of the large fractionation found between cinnabar and calcine, and because calcine is the dominant source of Hg contamination from the mines studied, δ202Hg values of calcine may be more environmentally important in these mined areas than the primary cinnabar ore. Measurement of the Hg isotopic composition of calcine is necessary when using Hg isotopes for tracing Hg sources from areas mined for Hg, especially mine water runoff. PMID:19848142

Isotopic variability of mercury in ore, mine-waste calcine, and leachates of mine-waste calcine from areas mined for mercury

USGS Publications Warehouse

Stetson, S.J.; Gray, J.E.; Wanty, R.B.; Macalady, D.L.

2009-01-01

The isotopic composition of mercury (Hg) was determined in cinnabar ore, mine-waste calcine (retorted ore), and leachates obtained from water leaching experiments of calcine from two large Hg mining districts in the U.S. This study is the first to report significant mass-dependent Hg isotopic fractionation between cinnabar ore and resultant calcine. Data indicate that ??202Hg values relative to NIST 3133 of calcine (up to 1.52???) in the Terlingua district, Texas, are as much as 3.24??? heavier than cinnabar (-1.72???) prior to retorting. In addition, ??202Hg values obtained from leachates of Terlingua district calcines are isotopically similar to, or as much as 1.17??? heavier than associated calcines, most likely due to leaching of soluble, byproduct Hg compounds formed during ore retorting that are a minor component in the calcines. As a result of the large fractionation found between cinnabar and calcine, and because calcine is the dominant source of Hg contamination from the mines studied, ??202Hg values of calcine may be more environmentally important in these mined areas than the primary cinnabar ore. Measurement of the Hg isotopic composition of calcine is necessary when using Hg isotopes for tracing Hg sources from areas mined for Hg, especially mine water runoff. ?? 2009 American Chemical Society.

Dispersed-nanoparticle loading synthesis for monodisperse Au-titania composite particles and their crystallization for highly active UV and visible photocatalysts.

PubMed

Sakamoto, Takeshi; Nagao, Daisuke; Noba, Masahiro; Ishii, Haruyuki; Konno, Mikio

2014-06-24

Submicrometer-sized amorphous titania spheres incorporating Au nanoparticles (NPs) were prepared in a one-pot synthesis consisting of a sol-gel reaction of titanium(IV) isopropoxide in the presence of chloroauric acid and a successive reduction with sodium borohydride in a mixed solvent of ethanol/acetonitrile. The synthesis was allowed to prepare monodisperse titania spheres that homogeneously incorporated Au NPs with sizes of ca. 7 nm. The Au NP-loaded titania spheres underwent different crystallization processes, including 500 °C calcination in air, high-temperature hydrothermal treatment (HHT), and/or low-temperature hydrothermal treatment (LHT). Photocatalytic experiments were conducted with the Au NP-loaded crystalline titania spheres under irradiation of UV and visible light. A combined process of LHT at 80 °C followed by calcination at 500 °C could effectively crystallize titania spheres maintaining the dispersion state of Au NPs, which led to photocatalytic activity higher than that of commercial P25 under UV irradiation. Under visible light irradiation, the Au NP-titania spheres prepared with a crystallization process of LHT at 80 °C for 6 h showed photocatalytic activity much higher than a commercial product of visible light photocatalyst. Structure analysis of the visible light photocatalysts indicates the importance of prevention of the Au NPs aggregation in the crystallization processes for enhancement of photocatalytic activity.

Easily recycled Bi2O3 photocatalyst coatings prepared via ball milling followed by calcination

NASA Astrophysics Data System (ADS)

Cheng, Lijun; Hu, Xumin; Hao, Liang

2017-06-01

Bi2O3 photocatalyst coatings derived from Bi coatings were first prepared by a two-step method, namely ball milling followed by the calcination process. The as-prepared samples were characterized by XRD, SEM, XPS and UV-Vis spectra, respectively. The results showed that monoclinic Bi2O3 coatings were obtained after sintering Bi coatings at 673 or 773 K, while monoclinic and triclinic mixed phase Bi2O3 coatings were obtained at 873 or 973 K. The topographies of the samples were observably different, which varied from flower-like, irregular, polygonal to nanosized particles with the increase in calcination temperature. Photodegradation of malachite green under simulated solar irradiation for 180 min showed that the largest degradation efficiency of 86.2% was achieved over Bi2O3 photocatalyst coatings sintered at 873 K. The Bi2O3 photocatalyst coatings, encapsulated with Al2O3 ball with an average diameter around 1 mm, are quite easily recycled, which provides an alternative visible light-driven photocatalyst suitable for practical water treatment application.

Synthesis-microstructure-performance relationship of layered transition metal oxides as cathode for rechargeable sodium batteries prepared by high-temperature calcination.

PubMed

Xie, Man; Luo, Rui; Lu, Jun; Chen, Renjie; Wu, Feng; Wang, Xiaoming; Zhan, Chun; Wu, Huiming; Albishri, Hassan M; Al-Bogami, Abdullah S; El-Hady, Deia Abd; Amine, Khalil

2014-10-08

Research on sodium batteries has made a comeback because of concern regarding the limited resources and cost of lithium for Li-ion batteries. From the standpoint of electrochemistry and economics, Mn- or Fe-based layered transition metal oxides should be the most suitable cathode candidates for affordable sodium batteries. Herein, this paper reports a novel cathode material, layered Na1+x(Fey/2Niy/2Mn1-y)1-xO2 (x = 0.1-0.5), synthesized through a facile coprecipitation process combined with subsequent calcination. For such cathode material calcined at 800 °C for 20 h, the Na/Na1+x(Fey/2Niy/2Mn1-y)1-xO2 (x = 0.4) electrode exhibited a good capacity of 99.1 mAh g(-1) (cycled at 1.5-4.0 V) and capacity retention over 87% after 50 cycles. Optimization of this material would make layered transition metal oxides a strong candidate for the Na-ion battery cathode.

Up-conversion monodispersed spheres of NaYF4:Yb3+/Er3+: green and red emission tailoring mediated by heating temperature, and greatly enhanced luminescence by Mn2+ doping.

PubMed

Zhu, Qi; Song, Caiyun; Li, Xiaodong; Sun, Xudong; Li, Ji-Guang

2018-04-09

Submicron sized, monodispersed spheres of Mn2+, Yb3+/Er3+ and Mn2+/Yb3+/Er3+ doped α-NaYF4 were easily autoclaved from mixed solutions of the component nitrates and ammonium fluoride (NH4F), in the presence of EDTA-2Na. Detailed characterizations of the resultant phosphors were obtained using XRD, Raman spectroscopy, FE-SEM, HR-TEM, STEM, PLE/PL spectroscopy, and fluorescence decay analysis. Finer structure and better crystal perfection was observed at a higher calcination temperature, and the spherical shape and excellent dispersion of the original particles was retained at temperatures up to 600 °C. Under the 980 nm infrared excitation, the Yb3+/Er3+-doped sample (calcined at 400 °C) exhibits a stronger green emission centered at ∼524 nm (2H11/2 → 4I15/2 transition of Er3+) and a weaker red emission centered at ∼657 nm (4F9/2 → 4I15/2 transition of Er3+). A 200 °C increase in the temperature from 400 °C to 600 °C resulted in the dominant red emission originating from the 4F9/2 → 4I15/2 transition of Er3+, instead of the previously dominant green one. Mn2+ doping induced a remarkable more enhanced intensity at ∼657 nm and ∼667 nm (red emission area) than that at ∼524 nm and ∼546 nm (green emission area), because of the non-radiative energy transfer between Mn2+ and Er3+. However, a poor thermal stability was induced by Mn2+ doping. The observed upconversion luminescence of the samples calcined at 400 °C and 600 °C followed the two photon process and the four photon process, respectively.

Synthesis and characterization of novel Ce{sub 0.8}Sm{sub 0.2}Fe{sub 0.9}Ir{sub 0.03}Co{sub 0.07}O{sub 3−δ} perovskite material and possible application as a cathode for low–intermediate temperature SOFCs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Njoku, Chima Benjamin; Ndungu, Patrick Gathura, E-mail: ndungup@ukzn.ac.za

2015-08-15

Highlights: • Ce{sub 0.8}Sm{sub 0.2}Fe{sub 0.9}Ir{sub 0.03}Co{sub 0.07}O{sub 3−δ} was synthesized using sol–gel methods. • Material was thoroughly characterized using Raman, FTIR, XRD, HRTEM, SEM, and TGA. • Electrochemical performance showed the materials are a promising new cathode material for low temperature SOFC. - Abstract: A novel perovskite material, Ce{sub 0.8}Sm{sub 0.2}Fe{sub 0.9}Ir{sub 0.03}Co{sub 0.07}O{sub 3−δ} was synthesized using a sol–gel technique. The materials were calcined at temperatures of 800 °C, 900 °C, and 1000 °C and then characterized using X-ray diffraction, Raman and infrared spectroscopy, high resolution transmission electron microscopy and scanning electron microscopy (SEM). The particle sizes andmore » crystallite sizes increased with increasing calcination temperature and formed perovskite type materials with some separate magnetite and iridium oxide. The powders were used to assemble button cells using samarium doped ceria as the electrolyte and NiO/SDC as the anode materials. The electrochemical properties were investigated using a Fiaxell open flanges test set-up and a Nuvant™ Powerstat-05 potentiostat/galvanostat. The Ce{sub 0.8}Sm{sub 0.2}Fe{sub 0.9}Ir{sub 0.03}Co{sub 0.07}O{sub 3−δ} cathode material calcined at 1000 °C exhibited the most promising performance, with a maximum power density of 0.400 W/cm{sup 2}, a current density of 0.8 A/cm{sup 2}, and a corresponding area specific resistance of 0.247 Ωcm{sup 2} at 500 °C. The button cells were reasonably stable over15 h.« less

Influence of high-temperature steam on the reactivity of CaO sorbent for CO₂ capture.

PubMed

Donat, Felix; Florin, Nicholas H; Anthony, Edward J; Fennell, Paul S

2012-01-17

Calcium looping is a high-temperature CO(2) capture technology applicable to the postcombustion capture of CO(2) from power station flue gas, or integrated with fuel conversion in precombustion CO(2) capture schemes. The capture technology uses solid CaO sorbent derived from natural limestone and takes advantage of the reversible reaction between CaO and CO(2) to form CaCO(3); that is, to achieve the separation of CO(2) from flue or fuel gas, and produce a pure stream of CO(2) suitable for geological storage. An important characteristic of the sorbent, affecting the cost-efficiency of this technology, is the decay in reactivity of the sorbent over multiple CO(2) capture-and-release cycles. This work reports on the influence of high-temperature steam, which will be present in flue (about 5-10%) and fuel (∼20%) gases, on the reactivity of CaO sorbent derived from four natural limestones. A significant increase in the reactivity of these sorbents was found for 30 cycles in the presence of steam (from 1-20%). Steam influences the sorbent reactivity in two ways. Steam present during calcination promotes sintering that produces a sorbent morphology with most of the pore volume associated with larger pores of ∼50 nm in diameter, and which appears to be relatively more stable than the pore structure that evolves when no steam is present. The presence of steam during carbonation reduces the diffusion resistance during carbonation. We observed a synergistic effect, i.e., the highest reactivity was observed when steam was present for both calcination and carbonation.

Synthesis and characterization of nanostructured strontium hexaferrite thin films by the sol-gel method

NASA Astrophysics Data System (ADS)

Masoudpanah, S. M.; Seyyed Ebrahimi, S. A.

2012-07-01

Nanostructured single phase strontium hexaferrite, SrFe12O19, thin films have been synthesized on the (100) silicon substrate using a spin coating sol-gel process. The thin films with various Fe/Sr molar ratios of 8-12 were calcined at different temperatures from 500 to 900 °C. The composition, microstructure and magnetic properties of the SrFe12O19 thin films were characterized using Fourier transform infrared spectroscopy, differential thermal analysis, thermogravimetry, X-ray diffraction, electron microscopy and vibrating sample magnetometer. The results showed that the optimum molar ratio for Fe/Sr was 10 at which the lowest calcination temperature to obtain the single phase strontium hexaferrite thin film was 800 °C. The magnetic measurements revealed that the sample with Fe/Sr molar ratio of 10, exhibited higher saturation magnetization (267.5 emu/cm3) and coercivity (4290 Oe) in comparison with those synthesized under other Fe/Sr molar ratios.

Preparation and characterization of ultrafine nanoparticles of Cu doped lithium tetraborate

NASA Astrophysics Data System (ADS)

Khalilzadeh, Nasrin; Saion, Elias Bin; Mirabolghasemi, Hamed; Crouse, Karen A.; Shaari, Abdul Halim Bin; Hashim, Mansor Bin

This study details an innovative single-step thermal synthesis of nano-sized lithium tetraborate doped with 0.1 %wt copper and its characterization. The heating temperature for the synthesis of the nanoparticle material was optimized by variation between 200 and 850 °C. The optimum amount of polyvinyl pyrrolidone (PVP) the capping agent was determined to be 0.027 mol per 1 g LTB-Cu. The calcination time was 2 h. Characterization of the samples was carried out using Thermogravimetry Analysis (TGA), Derivative Thermogravimetry (DTG), Differential Scanning Calorimetry (DSC), Fourier Transform Infrared (FTIR) Spectroscopy, X-ray diffractometer (XRD), transmission electron microscopy (TEM) and Ultraviolet-Visible (UV-Vis) spectroscopy. The product was thermally stable above 450 °C. FTIR, XRD and TEM results confirmed the formation of pure nano-crystalline copper doped lithium tetraborate between 450 and 750 °C. The optical bandgap was estimated to be 5.02-6.05 eV in the presence of different amounts of PVP at various calcination temperatures.

Low temperature pyrolysis of coal or oil shale in the presence of calcium compounds

DOEpatents

Khan, M. Rashid

1988-01-01

A coal pyrolysis technique or process is described in which particulate coal is pyrolyzed in the presence of about 5 to 21 wt. % of a calcium compound selected from calcium oxide, calcined (hydrate) dolomite, or calcined calcium hydrate to produce a high quality hydrocarbon liquid and a combustible product gas which are characterized by low sulfur content. The pyrolysis is achieved by heating the coal-calcium compound mixture at a relatively slow rate at a temperature of about 450.degree. to 700.degree. C. over a duration of about 10 to 60 minutes in a fixed or moving bed reactor. The gas exhibits an increased yield in hydrogen and C.sub.1 -C.sub.8 hydrocarbons and a reduction in H.sub.2 S over gas obtainable by pyrolyzing cola without the calcium compound. The liquid product obtained is of a sufficient quality to permit its use directly as a fuel and has a reduced sulfur and oxygen content which inhibits polymerization during storage.

Thermal characteristic of limonite ore upon calcination and reduction

NASA Astrophysics Data System (ADS)

Febriana, Eni; Manaf, Azwar; Prasetyo, A. B.; Mayangsari, W.

2018-05-01

Thermal characteristics of the limonite laterite ore types have been studied using TG / DTA. There are four endothermic peaks at 250, 646, 900, and 1023 °C with a total mass loss of 10.07wt%. These four peaks correspond to the XRD results on samples calcined at 600-1000 °C. Analysis of TG / DTA to the mixture of limonite and graphite showed two endothermic reaction peaks at 641 and 900 °C and an exothermic peak at 1180 °C. Reduction of the limonite-graphite mixture was done by heating at 800-1100 °C for 1 hour, and the reduced samples were analyzed using XRD. The results indicate that the reduction process proceed completely at higher temperatures, indicated by the increasing intensity of kamacite and Fe metal phase, and the decrease of peak intensity of carbon due to reaction with metal oxides. At 1100 °C, intensity of Fe-metal decreased due to sintering of Fe which may occur because the temperature was too high.

Preparation of silver nanoparticles at low temperature

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mishra, Mini, E-mail: mishramini5@gmail.com; Chauhan, Pratima, E-mail: mangu167@yahoo.co.in

Silver from ancient time is used as antimicrobial agent in the bulk form but now with the advancement in nanotechnology silver in the form of nanoparticles shown potential effect against microbes which make us easy to fight with many diseases plants and animals. In this work silver nanoparticles were synthesized by chemical routes using sodium borohydride as reducing agent at low temperature. The particles were characterized through UV-Visible spectroscopy as well as X-Ray Diffraction. The UV-visible spectra of silver nanoparticles exhibited absorption at 425 cm; the crystallite size of the particles is between 19nm to 39nm. EDAX graph shows two peaksmore » of silver and oxygen. Water absorbed by silver nanoparticles was removed by the calcinations.« less

Attrition resistant Fischer-Tropsch catalyst and support

DOEpatents

Singleton, Alan H.; Oukaci, Rachid; Goodwin, James G.

2004-05-25

A catalyst support having improved attrition resistance and a catalyst produced therefrom. The catalyst support is produced by a method comprising the step of treating calcined .gamma.-alumina having no catalytic material added thereto with an acidic aqueous solution having an acidity level effective for increasing the attrition resistance of the calcined .gamma.-alumina.

Immobilization of plutonium from solutions on porous matrices by the method of high temperature sorption

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nardova, A.K.; Filippov, E.A.; Glagolenko, Y.B.

1996-05-01

This report presents the results of investigations of plutonium immobilization from solutions on inorganic matrices with the purpose of producing a solid waste form. High-temperature sorption is described which entails the adsorption of radionuclides from solutions on porous, inorganic matrices, as for example silica gel. The solution is brought to a boil with additional thermal process (calcination) of the saturated granules.

(100) facets of γ-Al2O3: the active surfaces for alcohol dehydration reactions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kwak, Ja Hun; Mei, Donghai; Peden, Charles HF

2011-05-01

Temperature programmed desorption (TPD) of ethanol, and methanol dehydration reaction were studied on γ-Al2O3 in order to identify the catalytic active sites for alcohol dehydration reactions. Two high temperature (> 473 K) desorption features were observed following ethanol adsorption. Samples calcined at T≤473 K displayed a desorption feature in the 523-533 K temperature range, while those calcined at T ≥ 673 K showed a single desorption feature at 498 K. The switch from the high to low temperature ethanol desorption correlated well with the dehydroxylation of the (100) facets of γ-Al2O3 that was predicted at 550 K DFT calculations. Theoreticalmore » DFT simulations of the mechanism of dehydration. on clean and hydroxylated γ-Al2O3(100) surfaces, find that a concerted elimination of ethylene from an ethanol molecule chemisorbed at an Al3+ pentacoordinated site is the rate limiting step for catalytic cycle on both surfaces. Furthermore, titration of the pentacoordinate Al3+ sites on the (100) facets of γ-Al2O3 by BaO completely turned off the methanol dehydration reaction activity. These results unambiguously demonstrate that only the (100) facets on γ-Al2O3 are the catalytic active surfaces for alcohol dehydration.« less

Electrochemical performance of Fe3O4 micro flower as anode for lithium ion batteries

NASA Astrophysics Data System (ADS)

Noerochim, Lukman; Anggara, Dika; Susanti, Diah; Subhan, Achmad; Sudaryanto

2018-04-01

Graphite is generally employed in commercial lithium ion batteries which has a specific capacity of 372 mAh/g. In this study, graphite is replaced with carbon-coated magnetite (Fe3O4/C) which has large theoretical specific capacity of 926 mAh/g, environmental friendly, and low cost production. The synthesis of Fe3O4/C is carried out by hydrothermal method with reacting FeCl3 and hexamethylenetetramine (HMT) at temperature variation of 160, 170 and 180°C. The following process is heated by calcination at temperature variations 450, 500 and 550°C. XRD and SEM results show that the as-prepared Fe3O4/C powder has a single phase of Fe3O4 and morphology micro-flowers like with size between 700 nm - 3 µm. CV test results show redox reaction occurs in the voltage range between 0.21-0.85 V and 1.68-1.81 V. The highest specific discharge capacity is obtained 644 mAh/g for specimen with temperature hydrothermal of 170°C and temperature calcination of 550°C. This result shows that Fe3O4/C has a high potential as anode material for lithium ion battery.

Synthesis and Characterization of Yttria-Stabilized Zirconia Nanoparticles Doped with Ytterbium and Gadolinium: ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3

NASA Astrophysics Data System (ADS)

Bahamirian, M.; Hadavi, S. M. M.; Rahimipour, M. R.; Farvizi, M.; Keyvani, A.

2018-06-01

Defect cluster thermal barrier coatings (TBCs) are attractive alternatives to Yttria-stabilized zirconia (YSZ) in advanced applications. In this study, YSZ nanoparticles doped with ytterbium and gadolinium (ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3 (ZGYbY)) were synthesized through a chemical co-precipitation and calcination method, and characterized by in situ high-temperature X-ray diffraction analysis in the temperature range of 25 °C to 1000 °C (HTK-XRD), thermogravimetric analysis, differential thermal analysis, Fourier transform infrared spectroscopy, Raman spectroscopy, and field emission scanning electron microscopy (FE-SEM). Precise cell parameters of t-prime phase and the best zirconia phase for TBC applications were calculated by Cohen's and Rietveld refinement methods. Optimum crystallization temperature of the precursor powder was found to be 1000 °C. Furthermore, FE-SEM results for the calcined ZGYbY powders indicated orderly particles of uniform shape and size with a small tendency toward agglomeration. Average lattice thermal expansion coefficient in the temperature range of 25 °C to 1000 °C was determined to be 31.71 × 10-6 K-1.

Synthesis and Characterization of Yttria-Stabilized Zirconia Nanoparticles Doped with Ytterbium and Gadolinium: ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3

NASA Astrophysics Data System (ADS)

Bahamirian, M.; Hadavi, S. M. M.; Rahimipour, M. R.; Farvizi, M.; Keyvani, A.

2018-03-01

Defect cluster thermal barrier coatings (TBCs) are attractive alternatives to Yttria-stabilized zirconia (YSZ) in advanced applications. In this study, YSZ nanoparticles doped with ytterbium and gadolinium (ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3 (ZGYbY)) were synthesized through a chemical co-precipitation and calcination method, and characterized by in situ high-temperature X-ray diffraction analysis in the temperature range of 25 °C to 1000 °C (HTK-XRD), thermogravimetric analysis, differential thermal analysis, Fourier transform infrared spectroscopy, Raman spectroscopy, and field emission scanning electron microscopy (FE-SEM). Precise cell parameters of t-prime phase and the best zirconia phase for TBC applications were calculated by Cohen's and Rietveld refinement methods. Optimum crystallization temperature of the precursor powder was found to be 1000 °C. Furthermore, FE-SEM results for the calcined ZGYbY powders indicated orderly particles of uniform shape and size with a small tendency toward agglomeration. Average lattice thermal expansion coefficient in the temperature range of 25 °C to 1000 °C was determined to be 31.71 × 10-6 K-1.

Effect of metal cation ratio on chemical properties of ZnFe2O4/AC composite and adsorption of organic contaminant

NASA Astrophysics Data System (ADS)

Meilia, Demara; Misbah Khunur, Mochamad; Setianingsih, Tutik

2018-01-01

Porous woody char is biochar prepared through pyrolisis. The biochar can be used as adsorbent. In this research, ZnFe2O4/AC composite was synthesized through imregnation of the woody biochar with ZnFe2O4 to study effect of mol ratio of Fe(III) and Zn(II) toward their physicochemistry and adsorption of drug wastewater. Paracetamol was used as adsorbate model. This research was conducted in several steps, including activation of the woody biochar using KOH activator at temperatur 500 °C for 15 min to produce the activated carbon, fungsionalization of the carbon using H2SO4 oxidator (6M) at temperature of 80 °C for 3 h, impregnation of the oxidized activated carbon with Zn-Fe-LDH (Layered Double Hydroxide) at various mol ratio of Fe(III) and Zn(III), including 1:2, 1:3 and 1:4 using NaOH solution (5M) for coprecipitation, and calcination of Zn-Fe-LDH/AC at 950 °C for 5 min to produce ZnFe2O4/AC. FTIR diffraction characterization indicated existence of M-O (M = Zn(II), Fe(III)) and OH functional groups. FTIR spectra showed increasing of bands connected to -OH by increasing of the ratio till the ratio was achieved at 1:4, then decreased again. The ratio mol showed effect on the adsorption of paracetamol. Profile of adsorption value was fit with changing of functional groups. The highest adsorption was achieved at the ratio of 1:4. After calcination it gave the adsorption value of 17,66 mg/g.

Biologically synthesized titanium oxide nanostructures combined with morphogenetic protein as wound healing agent in the femoral fracture after surgery.

PubMed

Zhang, Yushu; Zhang, Chuanlian; Liu, Kemiao; Zhu, Xia; Liu, Fang; Ge, Xiaofen

2018-05-01

The aim of the present study is to develop novel approach for the green synthesis of titanium oxide nanoparticles (TiO 2 NPs) using Eichhornia crassipes extract and calcined at different temperatures for evaluate the wound healing activity in the femoral fracture. The synthesized TiO 2 are formed different (plate and rod-like) nanostructures at various calcination temperatures. These samples were characterized by X-ray diffraction (XRD), Fourier transform-infrared spectroscopy (FTIR), Field emission scanning electron microscope (FE-SEM) and transmission electron microscope (TEM). Microscopic studies of TiO 2 NPs revealed that the synthesized TiO 2 NPs are formed well-defined rod-like structures at 400 °C with size ranged from 200 nm to 500 nm. The characterized plate and rod-like TiO 2 NPs are combined with human morphogenetic protein (HbMP) to improving its wound healing activity and osteoblast properties on femoral fractures. The biocompatibility was tested by using human bone marrow mesenchymal stem cells (BMSC) cells and antibacterial efficacy analyzed using human pathogenica bacteria Staphylococcus aureus and Escherichia coli through agar well diffusion assay. The green synthesized rod-like TiO 2 NPs combined with HbMP has been exhibited effective bone fusion behaviors with biomechanical properties and also improved antibacterial activity against pathogenic bacteria. From this study results, it is suggested that green synthesized TiO 2 NPs could be used effectively in biomedical application. Copyright © 2018. Published by Elsevier B.V.

Synthesis of Hydroxyapatite through Ultrasound and Calcination Techniques

NASA Astrophysics Data System (ADS)

Akindoyo, John O.; Beg, M. D. H.; Ghazali, Suriati; Akindoyo, Edward O.; Jeyaratnam, Nitthiyah

2017-05-01

There is a growing demand for hydroxyapatite (HA) especially in medical applications, production of HA which is totally green is however a challenge. In this research, HA was produced from biowaste through ultrasound followed by calcination techniques. Pre-treatment of the biowaste was effectively achieved through the help of ultrasound. After calcination at 950°C, the obtained HA was characterized through Thermogravimetric (TGA) analysis, X-ray diffraction analysis (XRD) and Fourier transform infrared spectroscopy (FTIR). Spectrum of the produced HA was compared with standard HA index. The spectrum is in agreement with the standard HA as confirmed through FTIR, XRD and TGA result. Furthermore, morphological study of the HA through Field emission scanning electron microscope (FESEM) shows almost uniform spherical shape for the HA as expected. Based on the results obtained herein, combining ultrasound with calcination can help to produce pure HA with potential medical applications without the use of any organic solvent.

Templated synthesis of nickel nanoparticles: Toward heterostructured nanocomposites for efficient hydrogen storage

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nelson, Nicholas Cole

2013-01-01

The world is currently facing an energy and environmental crisis for which new technologies are needed. Development of cost-competitive materials for catalysis and hydrogen storage on-board motor vehicles is crucial to lead subsequent generations into a more sustainable and energy independent future. This thesis presents work toward the scalable synthesis of bimetallic heterostructures that can enable hydrogen to compete with carbonaceous fuels by meeting the necessary gravimetric and volumetric energy densities and by enhancing hydrogen sorption/desorption kinetics near ambient temperatures and pressures. Utilizing the well-known phenomenon of hydrogen spillover, these bimetallic heterostructures could work by lowering the activation energy for hydrogenation and dehydrogenation of metals. Herein, we report a novel method for the scalable synthesis of silica templated zero-valent nickel particles (Nimore » $$\\subset$$ SiO 2) that hold promise for the synthesis of nickel nanorods for use in bimetallic heterostructures for hydrogen storage. Our synthesis proceeds by chemical reduction of a nickel-hydrazine complex with sodium borohydride followed by calcination under hydrogen gas to yield silica encapsulated nickel particles. Transmission electron microscopy and powder X-ray diffraction were used to characterize the general morphology of the resultant nanocapsules as well as the crystalline phases of the incorporated Ni 0 nanocrystals. The structures display strong magnetic behavior at room temperature and preliminary data suggests nickel particle size can be controlled by varying the amount of nickel precursor used in the synthesis. Calcination under different environments and TEM analysis provides evidence for an atomic migration mechanism of particle formation. Ni$$\\subset$$SiO 2 nanocapsules were used as seeds to induce heterogeneous nucleation and subsequent growth within the nanocapsule via electroless nickel plating. Nickel nanoparticle growth occurs under high temperature alkaline conditions, however silica nanocapsule integrity is not maintained due to the incompatibility of silica with the growth conditions. Silica nanocapsule integrity is maintained under low temperature neutral conditions, but nickel particle growth is not observed. Through FTIR and UV/Vis analysis, we show the degree of crosslinking and condensation increases in calcined silica compared to as-synthesized silica. We propose the increased density of the silica nanocapsule hinders mass transfer of the bulky nickel precursor complex from solution and onto the surface of the “catalytic” zero-valent nickel seed within the nanocapsule cavity. Decreasing the density of the silica nanocapsule can be achieved through co-condensation of tetraethylorthosilicate with an alkyl functionalized silane followed by calcination to remove the organic component or by chemical etching in alkaline solution, but will not be addressed in this thesis.« less

Nano-crystalline porous tin oxide film for carbon monoxide sensing

NASA Technical Reports Server (NTRS)

Liu, Chung-Chiun (Inventor); Savinell, Robert F. (Inventor); Jin, Zhihong (Inventor)

2000-01-01

A tin oxide sol is deposited on platinum electrodes (12) of a sensor (10). The sol is calcined at a temperature of 500 to 800.degree. C. to produce a thin film of tin oxide with a thickness of about 150 nm to 2 .mu. and having a nano-crystalline structure with good stability. The sensor rapidly detects reducing gases, such as carbon monoxide, or hydrocarbons and organic vapors. Sensors using films calcined at around 700.degree. C. have high carbon monoxide selectivity with a response time of around 4 minutes and a recovery time of 1 minute, and therefore provide good detection systems for detection of trace amounts of pollutants such as toxic and flammable gases in homes, industrial settings, and hospitals.

Methane adsorption capacity on graphene derived from glucose and ferric chloride

NASA Astrophysics Data System (ADS)

Ismail, M. S.; Yusof, N.; Yusop, M. Zamri; Ismail, A. F.; Nasri, N. S.; Othman, F. E. Che

2018-05-01

This study examines the methane adsorption capacity using graphene derived from glucose and ferric chloride (FeCl3). The graphene was prepared via simple method by dissolution of glucose and FeCl3 in water, vaporization of water in oven, and calcination process in quartz furnace. Graphene was successfully produced with impregnation ratio of glucose and FeCl3 at 1:1 and calcination temperature of 650 °C. The prepared graphene subsequently underwent a volumetric adsorption setup, to measure the adsorption capacity of methane (CH4). The highest CH4 adsorption capacity obtained was 6.37 mmol/g at 3.5 bar and 298 K for 40 minutes. These result shows that the prepared graphene displayed good adsorption characteristic for CH4.

Calcination and solid state reaction of ceramic-forming components to provide single-phase superconducting materials having fine particle size

DOEpatents

Balachandran, Uthamalingam; Poeppel, Roger B.; Emerson, James E.; Johnson, Stanley A.

1992-01-01

An improved method for the preparation of single phase, fine grained ceramic materials from precursor powder mixtures where at least one of the components of the mixture is an alkali earth carbonate. The process consists of heating the precursor powders in a partial vacuum under flowing oxygen and under conditions where the partial pressure of CO.sub.2 evolved during the calcination is kept to a very low level relative to the oxygen. The process has been found particularly suitable for the preparation of high temperature copper oxide superconducting materials such as YBa.sub.2 Cu.sub.3 O.sub.x "123" and YBa.sub.2 Cu.sub.4 O.sub.8 "124".

Synthesis and characterization of mesoporous NaY zeolite from natural Blitar’s kaolin

NASA Astrophysics Data System (ADS)

Khalifah, S. N.; aini, Z. N.; Hayati, E. K.; Aini, N.; Prasetyo, A.

2018-03-01

Mesoporous NaY Zeolite has been synthesized from calcined natural Blitar’s kaolin with the addition of NaOH and CTABr surfactant as mesoporous template by hydrothermal method. Natural kaolin was calcinated with different time and temperature to change kaolin to metakaolin. X-ray diffraction data showed that mesoporous NaY zeolite was formed with impurities compound of sodalite, kaolin and quartz phases. The BET analysis resulted that the pore of NaY Zeolite belongs to mesoporous type with pore size 9,421 nm. Characterization from FTIR confirmed about the functional group of zeolites (988, 776, 663, 464 cm-1). Scanning electron microscopy characterization showed that the morphological of mesoporous NaY zeolites have uniform and crystalline particles formed.

Evaluation of blends bauxite-calcination-method red mud with other industrial wastes as a cementitious material: properties and hydration characteristics.

PubMed

Zhang, Na; Liu, Xiaoming; Sun, Henghu; Li, Longtu

2011-01-15

Red mud is generated from alumina production, and its disposal is currently a worldwide problem. In China, large quantities of red mud derived from bauxite calcination method are being discharged annually, and its utilization has been an urgent topic. This experimental research was to evaluate the feasibility of blends red mud derived from bauxite calcination method with other industrial wastes for use as a cementitious material. The developed cementitious material containing 30% of the bauxite-calcination-method red mud possessed compressive strength properties at a level similar to normal Portland cement, in the range of 45.3-49.5 MPa. Best compressive strength values were demonstrated by the specimen RSFC2 containing 30% bauxite-calcination-method red mud, 21% blast-furnace slag, 10% fly ash, 30% clinker, 8% gypsum and 1% compound agent. The mechanical and physical properties confirm the usefulness of RSFC2. The hydration characteristics of RSFC2 were characterized by XRD, FTIR, (27)Al MAS-NMR and SEM. As predominant hydration products, ettringite and amorphous C-S-H gel are principally responsible for the strength development of RSFC2. Comparing with the traditional production for ordinary Portland cement, this green technology is easier to be implemented and energy saving. This paper provides a key solution to effectively utilize bauxite-calcination-method red mud. Copyright © 2010 Elsevier B.V. All rights reserved.

Method for calcining radioactive wastes

DOEpatents

Bjorklund, William J.; McElroy, Jack L.; Mendel, John E.

1979-01-01

This invention relates to a method for the preparation of radioactive wastes in a low leachability form by calcining the radioactive waste on a fluidized bed of glass frit, removing the calcined waste to melter to form a homogeneous melt of the glass and the calcined waste, and then solidifying the melt to encapsulate the radioactive calcine in a glass matrix.

Synthesis and LPG sensing properties of nano-sized cadmium oxide.

PubMed

Waghulade, R B; Patil, P P; Pasricha, Renu

2007-04-30

This paper reports the synthesis and liquid petroleum gas (LPG) sensing properties of nano-sized cadmium oxide (CdO). The nano-sized CdO powder was successfully synthesized by using a chemical co-precipitation method using cadmium acetate and the ammonium hydroxide, as starting materials and water as a carrier. The resulting nano-sized powder was characterized by X-ray diffraction (XRD) measurements and the transmission electron microscopy (TEM). The LPG sensing properties of the synthesized nano-sized CdO were investigated at different operating temperatures and LPG concentrations. It was found that the calcination temperature and the operating temperature significantly affect the sensitivity of the nano-sized CdO powder to the LPG. The sensitivity is found to be maximum when the calcination temperature was 400 degrees C. The sensitivity to 75ppm of LPG is maximum at an operating temperature 450 degrees C and it was found to be approximately 341%. The response and recovery times were found to be nearly 3-5s and 8-10s, respectively. The synthesized nano-sized CdO powder is able to detect up to 25ppm for LPG with reasonable sensitivity at an operating temperature 450 degrees C and it can be reliably used to monitor the concentration of LPG over the range (25-75ppm). The experimental results of the LPG sensing studies reveal that the nano-sized CdO powder synthesized by a simple co-precipitation method is a suitable material for the fabrication of the LPG sensor.

pH sensitive silica nanotubes as rationally designed vehicles for NSAIDs delivery.

PubMed

Sousa, Célia T; Nunes, Cláudia; Proença, Mariana P; Leitão, Diana C; Lima, José L F C; Reis, Salette; Araújo, João P; Lúcio, Marlene

2012-06-01

A novel pH-sensitive drug delivery system based on functionalized silica nanotubes was developed for the incorporation of non-steroidal anti-inflammatory drugs (NSAIDs), aimed at a tailored drug release in acidic conditions characteristic of inflamed tissues. Silica nanotubes (SNTs) were synthesized by a nanoporous alumina template assisted sol-gel method. Inner surfaces were physically and chemically modified to improve both the functionalization and subsequent incorporation of the drug. Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and transmission electron microscopy (TEM) were used to characterize the designed nanocarriers and their functionalization. To achieve the highest degree of functionalization, three types of aminosilanes were tested and calcination conditions were optimized. APTES was shown to be the most effective aminosilane regarding the functionalization of the SNTs' inner surface and an adequate calcination temperature (220°C) was found to attain mechanical stability without compromising functionalization efficiency. Finally, the incorporation of naproxen into the nanotubes was accessed by fluorescence measurements and drug release studies were performed, revealing that the electrostatic linkage ensures effective release of the drug in the acidic pH typical of inflamed cells, while maintaining the SNT-drug conjugates stable at the typical bloodstream pH. Copyright © 2012 Elsevier B.V. All rights reserved.

Effect of molarity on sol-gel routed nano TiO2 thin films

NASA Astrophysics Data System (ADS)

Lourduraj, Stephen; Williams, Rayar Victor

The nanostructured titanium dioxide (TiO2) thin films have been prepared for the molar concentrations of titanium tetra isopropoxide (TTIP) 0.05M, 0.1M, 0.15M and 0.2M by sol-gel routed spin coating technique with calcination at 450∘C. The processing parameters such as, pH value (8), catalyst HCl (0.1ml), spin speed (3000rpm) and calcination temperature (450∘C) are optimized. The crystalline nature and surface morphology were analyzed by XRD, SEM and AFM analysis. The XRD results confirm that the films are crystalline with anatase phase, and are nanostructured. The SEM micrographs of the TiO2 film reveal the spherical nature of the particle. AFM analysis establishes that the uniformity of the TiO2 thin film was optimized at 0.2M. The optical measurements show that the transmittance depends on the molarity, and the optical band gap energy of TiO2 films is found to be inversely proportional to molarity. The I-V characteristics exhibit that the molarity strongly influences the electrical conductivity of the film. The results indicate that the significant effect of molarity on structural, optical and electrical properties of the nanostructured TiO2 thin films will be useful to photovoltaic application.

Modification of waste coal gangue and its application in the removal of Mn(2+) from aqueous solution.

PubMed

Qiu, Ruifang; Cheng, Fangqin

We developed a new calcination method to convert coal gangue (CG), a common waste generated from coal production process, into a modified form, which could be used as an adsorbent to remove Mn(2+) from aqueous solution. Sodium tetraborate (Na2B4O7·10H2O) was added into the CG calcination process as an additive, and the concentrations of Na2B4O7·10H2O were optimized along with the calcination temperature to obtain the best adsorbent capacity of modified coal gangue (MCG). We applied multiple analytical methods such as scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy and Brunauer-Emmett-Teller analysis to characterize the MCG. The results showed it had a smaller particle size and a larger specific surface area and pore volume after modification. It also indicated that the phase of CG transformed from kaolinite to metakaolinite after calcination. Moreover, a new substance was generated with two new peaks at 1,632 cm(-1) and 799 cm(-1). The Mn(2+) absorption capacity of MCG was evaluated using a series of experiments with different adsorbent doses, pH values and initial Mn(2+) concentrations during the adsorption process. We found that Mn(2+) adsorbent capacity of MCG increased by more than seven-fold compared to that of CG. The Langmuir isotherm model and the pseudo-second-order kinetic model provided the best fit to the adsorption processes.

46 CFR 148.04-17 - Petroleum coke, calcined, at 130 °F or above.

Code of Federal Regulations, 2010 CFR

2010-10-01

... flashpoint under 200 °F, a two-to-three foot layer of the material at a temperature not greater than 110 °F..., the loading of the two-to-three foot layer of the material at a temperature not greater than 110 °F... described in paragraph (e)(1) of this section, a two-to-three foot layer of the material at 130 °F or above...

Influence of the physico-chemical properties of CeO 2-ZrO 2 mixed oxides on the catalytic oxidation of NO to NO 2

NASA Astrophysics Data System (ADS)

Atribak, Idriss; Guillén-Hurtado, Noelia; Bueno-López, Agustín; García-García, Avelina

2010-10-01

Commercial and home-made Ce-Zr catalysts prepared by co-precipitation were characterised by XRD, Raman spectroscopy, N 2 adsorption at -196 °C and XPS, and were tested for NO oxidation to NO 2. Among the different physico-chemical properties characterised, the surface composition seems to be the most relevant one in order to explain the NO oxidation capacity of these Ce-Zr catalysts. As a general trend, Ce-Zr catalysts with a cerium-rich surface, that is, high XPS-measured Ce/Zr atomic surface ratios, are more active than those with a Zr-enriched surface. The decrease in catalytic activity of the Ce-Zr mixed oxided upon calcinations at 800 °C with regard to 500 °C is mainly attributed to the decrease in Ce/Zr surface ratio, that is, to the surface segregation of Zr. The phase composition (cubic or t'' for Ce-rich compositions) seems not to be a direct effect on the catalytic activity for NO oxidation in the range of compositions tested. However, the formation of a proper solid solution prevents important surface segregation of Zr upon calcinations at high temperature. The effect of the BET surface area in the catalytic activity for NO oxidation of Ce-Zr mixed oxides is minor in comparison with the effect of the Ce/Zr surface ratio.

A new photocatalyst of LuFeO3 for the dye degradation

NASA Astrophysics Data System (ADS)

Zhou, M.; Yang, H.; Xian, T.; Zhang, C. R.

2015-08-01

A polyacrylamide gel route was introduced to synthesize LuFeO3 particles, where the effects of calcination temperature, calcination time and chelating agent on the products were investigated. By varying the experimental conditions, several LuFeO3 samples with sphere-, ellipsoid- and worm-like morphologies and average particle sizes of 200-270 nm were prepared. The photocatalytic activity of LuFeO3 samples was evaluated by degrading rhodamine B (RhB) under simulated-sunlight irradiation, revealing that they exhibit a pronounced photocatalytic activity. The effects of p-benzoquinone (BQ), ethanol and oxalic acid (OA) on the photocatalytic efficiency were investigated. It is observed that BQ has almost no effect on the photocatalytic degradation of RhB, ethanol exhibits a substantial suppression of RhB degradation, while OA significantly enhances the photocatalytic efficiency. Hydroxyl (•OH) radicals were examined by fluorimetry using terephthalic acid as a probe molecule, and are found to be produced over the simulated-sunlight irradiated LuFeO3 particles. The addition of ethanol leads to a quenching of •OH radicals, whereas the yield of •OH radicals is highly increased on addition of OA. Based on the experimental results, •OH radicals are suggested to be the dominant active species responsible for the dye degradation, while superoxide (•O2-) radicals play a negligible role in the photocatalysis.

Electrical, Magnetic and Microwave Absorption Properties of M-type Barium Hexaferrites (BaFe12-2x CoxNixO19)

NASA Astrophysics Data System (ADS)

Susilawati; Doyan, A.; Khair, H.; Taufik, M.; Wahyudi

2018-04-01

M-type barium hexaferrites synthesis with Co-Ni doping ion (BaFe12-2x CoxNixO19) based on natural iron sand of Loang Balok beach, Lombok, Indonesia, to be applied as a microwave absorbent material using co-precipitation method. The materials used in the synthesis process are magnetite minerals (Fe2O3 and Fe3O4), 12M HCl, NH4OH 37%, CoCl2.6H2O and NiCl2.6H2O. This research to investigate the effect of doping ion concentration variation (x = 0.0, 0.6 and 1.0) and calcination temperature (T = 80, 600, and 800°C) on electrical and magnetic properties and microwave absorption as well. The samples were characterized using Vibrating Sample Magnetometer (VSM) and Network Vector Analyzer (VNA). The result from VSM showed that the coercivity value decreased when doping ion concentration and calcination temperature increased (0.151 Tesla at 600°C for x = 0.0 and 0.044 Tesla at 800°C for x = 1.0. The value of magnetic saturation and the magnetic remanence increased with increasing ion concentration (Ms = 0.327 emu/g at x = 0.0 increased to 35.4 emu/g at x = 1.0) and Mr = 0.148 emu/g for x = 0.0 increased to 15.6 emu/g at x=1.0, this indicates that the sample has been soft magnetic. The result from VNA showed that the electrical conductivity values measured in the range 8.0-15.0 GHz indicate that the sample is a semiconductor (6.149 x 10-6 -5.975 x 10-4 S/cm). It also showed that the microwave absorption properties increased at higher concentration of doping ions and the calcination temperature would increase the value of Reflection Loss (RL). The maximum RL value of the sample is -14.47 dB at 12.38 GHz, and the absorption coefficient of 96.43%. These results indicate that the BaFe12-2x CoxNixO19 sample can be applied as a microwave absorbent material on X-band to Ku-band frequency.

Chlorination of alumina in kaolinitic clay

NASA Astrophysics Data System (ADS)

Grob, B.; Richarz, W.

1984-09-01

The chlorination of alumina in kaolinitic clay with Cl2 and CO gas mixtures was studied gravimetrically. The effects of the calcination method and of NaCl addition on the reactivity of the clay were examined. Fast reaction rates were achieved only with samples previously exposed to a sulfating treatment. Optimum conditions, with maximum yield and selectivity to A1C13 and minimum SiO2 conversion, were found between 770 and 970 K. At higher temperatures the SiCl4 formed poisons the reactive alumina surface by selective chemisorption with a marked decrease of the reaction rate.

Study of variation grain size in desulfurization process of calcined petroleum coke

NASA Astrophysics Data System (ADS)

Pintowantoro, Sungging; Setiawan, Muhammad Arif; Abdul, Fakhreza

2018-04-01

Indonesia is a country with abundant natural resources, such as mineral mining and petroleum. In petroleum processing, crude oil can be processed into a source of fuel energy such as gasoline, diesel, oil, petroleum coke, and others. One of crude oil potentials in Indonesia is petroleum coke. Petroleum coke is a product from oil refining process. Sulfur reducing process in calcined petroleum cokes can be done by desulfurization process. The industries which have potential to become petroleum coke processing consumers are industries of aluminum smelting (anode, graphite block, carbon mortar), iron riser, calcined coke, foundry coke, etc. Sulfur reducing process in calcined petroleum coke can be done by thermal desulfurization process with alkaline substance NaOH. Desulfurization of petroleum coke process can be done in two ways, which are thermal desulfurization and hydrodesulphurization. This study aims to determine the effect of various grain size on sulfur, carbon, and chemical bond which contained by calcined petroleum coke. The raw material use calcined petroleum coke with 0.653% sulfur content. The grain size that used in this research is 50 mesh, then varied to 20 mesh and 100 mesh for each desulfurization process. Desulfurization are tested by ICP, UV-VIS, and FTIR to determine levels of sulfur, carbon, chemical bonding and sulfur dissolved water which contained in the residual washing of calcined petroleum coke. From various grain size that mentioned before, the optimal value is on 100 mesh grain size, where the sulfur content in petroleum coke is 0.24% and carbon content reaches the highest level of 97.8%. Meanwhile for grain size 100 mesh in the desulfurization process is enough to break the chemical bonds of organic sulfur in petroleum coke.

Preparation of α-Fe2O3 nanotubes via electrospinning and research on their catalytic properties

NASA Astrophysics Data System (ADS)

Shao, Hao; Zhang, Xuebin; Chen, Fanyan; Liu, Shasha; Ji, Yi; Zhu, Yajun; Feng, Yi

2012-09-01

In this paper, smooth α-Fe2O3 nanotubes have been successfully synthesized by electrospinning of ferric nitrate-polyvinyl alcohol solution followed by calcination in air. The morphologies and structures of the samples were characterized by transmission electron microscopy, scanning electron microscopy and X-ray diffraction. The catalytic properties were studied by differential thermal analysis and thermogravimetric analysis. The results indicated that the as-prepared α-Fe2O3 nanotubes showed a continuous morphology and an extremely high degree of crystallization. The average inner and outer diameters of the obtained α-Fe2O3 nanotubes were about 60 nm and 100 nm, respectively. The obtained α-Fe2O3 nanotubes were able to lower the temperature of the high-temperature thermal decomposition of ammonium perchlorate, while they had little effect on the crystallographic phase transformation and the low-temperature thermal decomposition.

The influence of temperature on limestone sulfation and attrition under fluidized bed combustion conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Montagnaro, Fabio; Salatino, Piero; Dipartimento di Ingegneria Chimica - Universita degli Studi di Napoli Federico II, Piazzale Vincenzo Tecchio 80, 80125 Napoli

2010-04-15

The influence of temperature on attrition of two limestones during desulfurization in a fluidized bed reactor was investigated. Differences in the microstructure of the two limestones were reflected by a different thickness of the sulfate shell formed upon sulfation and by a different value of the ultimate calcium conversion degree. Particle attrition and fragmentation were fairly small under moderately bubbling fluidization conditions for both limestones. An increase of temperature from 850 C to 900 C led to an increase of the attrition rate, most likely because of a particle weakening effect caused by a faster CO{sub 2} evolution during calcination.more » This weakening effect, however, was not sufficiently strong to enhance particle fragmentation in the bed. The progress of sulfation, associated to the build-up of a hard sulfate shell around the particles, led in any case to a decrease of the extent of attrition. Sulfation at 900 C was less effective than at 850 C, and this was shown to be related to the porosimetric features of the different samples. (author)« less

In Vitro Studies Evaluating Leaching of Mercury from Mine Waste Calcine Using Simulated Human Body Fluids

PubMed Central

2010-01-01

In vitro bioaccessibility (IVBA) studies were carried out on samples of mercury (Hg) mine-waste calcine (roasted Hg ore) by leaching with simulated human body fluids. The objective was to estimate potential human exposure to Hg due to inhalation of airborne calcine particulates and hand-to-mouth ingestion of Hg-bearing calcines. Mine waste calcines collected from Hg mines at Almadén, Spain, and Terlingua, Texas, contain Hg sulfide, elemental Hg, and soluble Hg compounds, which constitute primary ore or compounds formed during Hg retorting. Elevated leachate Hg concentrations were found during calcine leaching using a simulated gastric fluid (as much as 6200 μg of Hg leached/g sample). Elevated Hg concentrations were also found in calcine leachates using a simulated lung fluid (as much as 9200 μg of Hg leached/g), serum-based fluid (as much as 1600 μg of Hg leached/g), and water of pH 5 (as much as 880 μg of Hg leached/g). The leaching capacity of Hg is controlled by calcine mineralogy; thus, calcines containing soluble Hg compounds contain higher leachate Hg concentrations. Results indicate that ingestion or inhalation of Hg mine-waste calcine may lead to increased Hg concentrations in the human body, especially through the ingestion pathway. PMID:20491469

In vitro studies evaluating leaching of mercury from mine waste calcine using simulated human body fluids.

PubMed

Gray, John E; Plumlee, Geoffrey S; Morman, Suzette A; Higueras, Pablo L; Crock, James G; Lowers, Heather A; Witten, Mark L

2010-06-15

In vitro bioaccessibility (IVBA) studies were carried out on samples of mercury (Hg) mine-waste calcine (roasted Hg ore) by leaching with simulated human body fluids. The objective was to estimate potential human exposure to Hg due to inhalation of airborne calcine particulates and hand-to-mouth ingestion of Hg-bearing calcines. Mine waste calcines collected from Hg mines at Almaden, Spain, and Terlingua, Texas, contain Hg sulfide, elemental Hg, and soluble Hg compounds, which constitute primary ore or compounds formed during Hg retorting. Elevated leachate Hg concentrations were found during calcine leaching using a simulated gastric fluid (as much as 6200 microg of Hg leached/g sample). Elevated Hg concentrations were also found in calcine leachates using a simulated lung fluid (as much as 9200 microg of Hg leached/g), serum-based fluid (as much as 1600 microg of Hg leached/g), and water of pH 5 (as much as 880 microg of Hg leached/g). The leaching capacity of Hg is controlled by calcine mineralogy; thus, calcines containing soluble Hg compounds contain higher leachate Hg concentrations. Results indicate that ingestion or inhalation of Hg mine-waste calcine may lead to increased Hg concentrations in the human body, especially through the ingestion pathway.

In vitro studies evaluating leaching of mercury from mine waste calcine using simulated human body fluids

USGS Publications Warehouse

Gray, John E.; Plumlee, Geoffrey S.; Morman, Suzette A.; Higueras, Pablo L.; Crock, James G.; Lowers, Heather A.; Witten, Mark L.

2010-01-01

In vitro bioaccessibility (IVBA) studies were carried out on samples of mercury (Hg) mine-waste calcine (roasted Hg ore) by leaching with simulated human body fluids. The objective was to estimate potential human exposure to Hg due to inhalation of airborne calcine particulates and hand-to-mouth ingestion of Hg-bearing calcines. Mine waste calcines collected from Hg mines at Almadén, Spain, and Terlingua, Texas, contain Hg sulfide, elemental Hg, and soluble Hg compounds, which constitute primary ore or compounds formed during Hg retorting. Elevated leachate Hg concentrations were found during calcine leaching using a simulated gastric fluid (as much as 6200 μg of Hg leached/g sample). Elevated Hg concentrations were also found in calcine leachates using a simulated lung fluid (as much as 9200 μg of Hg leached/g), serum-based fluid (as much as 1600 μg of Hg leached/g), and water of pH 5 (as much as 880 μg of Hg leached/g). The leaching capacity of Hg is controlled by calcine mineralogy; thus, calcines containing soluble Hg compounds contain higher leachate Hg concentrations. Results indicate that ingestion or inhalation of Hg mine-waste calcine may lead to increased Hg concentrations in the human body, especially through the ingestion pathway.

Optimization of an innovative approach involving mechanical activation and acid digestion for the extraction of lithium from lepidolite

NASA Astrophysics Data System (ADS)

Vieceli, Nathália; Nogueira, Carlos A.; Pereira, Manuel F. C.; Durão, Fernando O.; Guimarães, Carlos; Margarido, Fernanda

2018-01-01

The recovery of lithium from hard rock minerals has received increased attention given the high demand for this element. Therefore, this study optimized an innovative process, which does not require a high-temperature calcination step, for lithium extraction from lepidolite. Mechanical activation and acid digestion were suggested as crucial process parameters, and experimental design and response-surface methodology were applied to model and optimize the proposed lithium extraction process. The promoting effect of amorphization and the formation of lithium sulfate hydrate on lithium extraction yield were assessed. Several factor combinations led to extraction yields that exceeded 90%, indicating that the proposed process is an effective approach for lithium recovery.

Cubic phase stability, optical and magnetic properties of Cu-stabilized zirconia nanocrystals

NASA Astrophysics Data System (ADS)

Pramanik, Prativa; Singh, Sobhit; Joshi, Deep Chandra; Mallick, Ayan; Pisane, Kelly; Romero, Aldo H.; Thota, Subhash; Seehra, M. S.

2018-06-01

By means of experimental and ab initio investigations, we report on the cubic phase stability of Cu doped zirconia (ZrO2) at room temperature, and further characterize its structural, optical and magnetic properties. Various compositions of Zr1‑x Cu x O2 (0.01  ⩽  x  ⩽  0.25) nanocrystallites of average size  ∼16 nm were synthesized using co-precipitation technique. Thermal analysis and kinetics of crystallization revealed that the cubic phase at ambient temperature can be stabilized by using a critical calcination temperature of 500 °C for 8 h in air and a critical composition of . For x  <  x c , some undigested monoclinic phase of ZrO2 exists together with the cubic structure. However, for x  >  x c , the monoclinic CuO emerges as a secondary phase with shrinkage of unit-cell volume with increasing the Cu content. At x  =  0.05 and 500 °C calcination temperature, we observe a high degree of cubic crystallinity which breaks down into monoclinic phase with increasing calcination temperature beyond 550 °C. Electron magnetic resonance studies provide evidence for the substitution of Cu2+ (2D5/9,3d9) ions at Zr4+ sites with g, g and average g a   =  (  +  2)/3  ∼  2.1. The temperature dependence of magnetic susceptibility measurements from 2 K to 300 K exhibits Curie–Weiss behaviour whose analysis using g a   =  2.1 and spin S  =  1/2 yields x  =  0.028 and x  =  0.068 for the nominal x  =  0.05 and x  =  0.20 samples, respectively. This magnetic analysis confirms the findings from x-ray diffraction that only a part of Cu is successfully doped into cubic phase of Cu-doped ZrO2. The optical bandgap decreases with increasing x, which is due to the emergence of Cu-d states at Fermi-level near the valence bands, thus making Cu-doped zirconia a hole doped (p-type) semiconductor.

Facile solution-precipitation assisted synthesis and luminescence property of greenish-yellow emitting Ca{sub 6}Ba(PO{sub 4}){sub 4}O:Eu{sup 2+} phosphor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ji, Haipeng; Huang, Zhaohui, E-mail: huang118@cugb.edu.cn; Xia, Zhiguo, E-mail: xiazg@ustb.edu.cn

2016-03-15

Highlights: • Ca{sub 6}Ba(PO{sub 4}){sub 4}O:Eu{sup 2+} phosphor was prepared by the solution-precipitation assisted route. • The phosphors have satisfactory smooth grain surface and particle size. • It shows greenish-yellow color emission (maximum at 540 nm) upon blue light excitation. • Eu{sup 2+} is coordinated with isolated oxygen atoms and those from PO{sub 4} polyhedra. - Abstract: Greenish-yellow emitting microcrystalline Ca{sub 6}Ba(PO{sub 4}){sub 4}O:Eu{sup 2+} phosphor was successfully prepared by a solution-precipitation assisted high temperature reaction method. Phase structure, morphology and/or luminescence properties of the precursor and the as-prepared phosphors were characterized. The phase-pure Ca{sub 6}Ba(PO{sub 4}){sub 4}O:Eu{sup 2+} phosphorsmore » were obtained with smooth grain surface and particle size of 2–8 μm. Ca{sub 6}Ba(PO{sub 4}){sub 4}O:Eu{sup 2+} exhibits bright greenish-yellow color emission with its maximum at 540 nm upon UV-blue light excitation. The maximum position of the broad emission band is independent on the calcination temperature. The emission intensity increases with increasing calcination temperature due to improved crystallinity. Besides, the presence of two Eu{sup 2+} emission centers in the Ca{sub 6}Ba(PO{sub 4}){sub 4}O crystal lattice was confirmed and the coordination effects are considered concerning the roles of isolated O atoms and those from the PO{sub 4} tetrahedra.« less

Frequency dependent dielectric properties of Sr doped NiO nanostructures

NASA Astrophysics Data System (ADS)

Siddique, M. Naseem; Ahmed, Ateeq; Ali, T.; Tripathi, P.

2018-05-01

Ni1-xSrxO (x=0.0, 0.02) nanoparticles have been synthesized using sol-gel method calcined at temperature 600 °C. The XRD analysis result revealed that the calcined sample has a cubic structure with single phase structure. We have calculated crystallite size of samples using both Debye-Sherrer and William Hall (W-H) method which are found to be 19.69 nm, 22.39 nm and 28.50 nm, 33.27 nm, respectively. TEM image reveals the formation of spherical shaped particles. In addition, dielectric properties have been studied using LCR measurement and found that ɛ', ɛ″ and tan δ are decreases with increase in frequency whereas ac conductivity increases with increase in frequency. This behavior may be explained using Maxwell-Wagner and Koop theory.

Synthesis of In2O3nanoparticles by thermal decomposition of a citrate gel precursor

NASA Astrophysics Data System (ADS)

Rey, J. F. Q.; Plivelic, T. S.; Rocha, R. A.; Tadokoro, S. K.; Torriani, I.; Muccillo, E. N. S.

2005-06-01

This paper describes the synthesis of indium oxide by a modified sol-gel method, and the study of thermal decomposition of the metal complex in air. The characterization of the intermediate as well as the final compounds was carried out by thermogravimetry, differential thermal analysis, Fourier transform infrared spectroscopy, X-ray diffraction, transmission electron microscopy, and small angle X-ray scattering. The results show that the indium complex decomposes to In2O3 with the formation of an intermediate compound. Nanoparticles of cubic In2O3 with crystallite sizes in the nanosize range were formed after calcination at temperatures up to 900°C. Calcined materials are characterized by a polydisperse distribution of spherical particles with sharp and smooth surfaces.

ZnO-based regenerable sulfur sorbents for fluid-bed/transport reactor applications

DOEpatents

Slimane, Rachid B.; Abbasian, Javad; Williams, Brett E.

2004-09-21

A method for producing regenerable sulfur sorbents in which a support material precursor is mixed with isopropanol and a first portion of deionized water at an elevated temperature to form a sol mixture. A metal oxide precursor comprising a metal suitable for use as a sulfur sorbent is dissolved in a second portion of deionized water, forming a metal salt solution. The metal salt solution and the sol mixture are mixed with a sol peptizing agent while heating and stirring, resulting in formation of a peptized sol mixture. The metal oxide precursor is dispersed substantially throughout the peptized sol mixture, which is then dried, forming a dry peptized sol mixture. The dry peptized sol mixture is then calcined and the resulting calcined material is then converted to particles.

Removal of oxytetracycline from aqueous solutions by hydroxyapatite as a low-cost adsorbent

NASA Astrophysics Data System (ADS)

Harja, Maria; Ciobanu, Gabriela

2017-11-01

The present paper involved a study of the adsorption process of the oxytetracycline drug from aqueous medium by using the hydroxyapatite nanopowders as adsorbent materials. The batch adsorption experiments were performed by monitoring the solution pH, contact time, adsorbent dosage and drug solution concentration. At pH 8 and ambient temperature, high oxytetracycline removal rates of about 97.58% and 89.95% for the uncalcined and calcined nanohydroxyapatites, respectively, were obtained. The kinetic studies indicate that the oxytetracycline adsorption onto nanohydroxyapatite samples follows a pseudo-second order kinetic model. The maximum adsorption capacities of 291.32 mg/g and 278.27 mg/g for uncalcined and calcined nanohydroxyapatite samples, respectively, have been found. So, the conclusion can be drawn that the hydroxyapatite shows good adsorption ability towards oxytetracycline.

Synergistic effects between TiO2 and carbon nanotubes (CNTs) in a TiO2/CNTs system under visible light irradiation.

PubMed

Wu, Chung-Hsin; Kuo, Chao-Yin; Chen, Shih-Ting

2013-01-01

This study synthesized a TiO2/carbon nanotubes (CNTs) composite via the sol-gel method. The surface characteristics of the TiO2/CNTs composite were determined by X-ray diffraction, transmission electron microscopy, specific surface area analyser, ultraviolent (UV)-vis spectroscopy, X-ray photoelectron spectroscopy and Raman spectrometer. The photocatalytic activity ofthe TiO2/CNTs composite was evaluated by decolourizing C.I. Reactive Red 2 (RR2) under visible light irradiation. Furthermore, the effects of calcination temperature, pH, RR2 concentration, and the TiO2/CNTs composite dosage on RR2 decolourization were determined simultaneously. The optimal calcination temperature to generate TiO2 and the TiO2/CNTs composite was 673 K, as the percentage of anatase crystallization at this temperature was highest. The specific surface area of the TiO2/CNTs composite and TiO2 were 45 and 42 m2/g, respectively. The band gap of TiO2 and the TiO2/CNTs composite was 2.97 and 2.71 eV by UV-vis measurements, respectively. Experimental data indicate that the Ti-O-C bond formed in the TiO2/CNTs composite. The RR2 decolourization rates can be approximated by pseudo-first-order kinetics; moreover, only the TiO2/CNTs composite had photocatalytic activity under visible light irradiation. At pH 7, the RR2 decolourization rate constant of 0.5, 1 and 2 g/L TiO2/CNTs addition was 0.005, 0.0015, and 0.0047 min(-1), respectively. Decolourization rate increased as pH and the RR2 concentration decreased. The CNTs functioned as electron acceptors, promoting separation of photoinduced electron-hole pairs to retard their recombination; thus, photocatalytic activity of the TiO2/CNTs composite exceeded that of TiO2.

Photoluminescence and photocatalytic properties of rhombohedral CuGaO2 nanoplates

PubMed Central

Shi, Linlin; Wang, Fei; Wang, Yunpeng; Wang, Dengkui; Zhao, Bin; Zhang, Ligong; Zhao, Dongxu; Shen, Dezhen

2016-01-01

Rhombohedral phase CuGaO2 nanoplates with a diameter of about 10 μm were synthesized via low temperature hydrothermal method. Room temperature and low temperature photoluminescence of the obtained CuGaO2 nanoplates were characterized. CuGaO2 nanoplates exhibited blue emission at room temperature and free exciton emission were appeared at low temperature. The blue emission is originated from defects such as Cu vacancies, which is the possible origin of p-type conductivity. The appearance of free exciton emission can demonstrate the direct bandgap transition behavior of CuGaO2 nanoplates. The as-prepared p-type CuGaO2 nanoplates were further decorated by n-type ZnO nanoparticles via calcination method to fabricate p-n junction nanocomposites. The nanocomposites exhibited enhanced photocatalytic activity which can be ascribed to the effective separation of photogenerated carriers by the internal electrostatic field in the p-n junction region, and the enhanced light absorption properties resulted from sub-bandgap absorption effect of p-n junction. This work has offered a new insight into the design of p-n junction devices using p-type CuGaO2 nanoplates. PMID:26887923

Agarose encapsulated mesoporous carbonated hydroxyapatite nanocomposites powder for drug delivery.

PubMed

Kolanthai, Elayaraja; Abinaya Sindu, P; Thanigai Arul, K; Sarath Chandra, V; Manikandan, E; Narayana Kalkura, S

2017-01-01

The powder composites are predominantly used for filling of voids in bone and as drug delivery carrier to prevent the infection or inflammatory reaction in the damaged tissues. The objective of this work was to study the synthesis of agarose encapsulation on carbonated hydroxyapatite powder and their biological and drug delivery properties. Mesoporous, nanosized carbonated hydroxyapatite/agarose (CHAp/agarose) powder composites were prepared by solvothermal method and subsequently calcined to study the physico-chemical changes, if it subjected to thermal exposure. The phase of the as-synthesized powder was CHAp/agarose whereas the calcinated samples were non-stoichiometric HAp. The CHAp/agarose nanorods were of length 10-80nm and width 40-190nm for the samples synthesized at temperatures 120°C (ST120) and 150°C (ST150). The calcination process produced spheres (10-50nm) and rods with reduced size (40-120nm length and 20-30nm width). Composites were partially dissolved in SBF solution followed by exhibited better bioactivity than non-stoichiometric HAp confirmed by gravimetric method. Hemo and biocompatibility remained unaffected by presence of agarose or carbonate in the HAp. Specific surface area of the composites was high and exhibited an enhanced amoxicillin and 5-fluorouracil release than the calcined samples. The composites demonstrated a strong antimicrobial activity against E. coli, S. aureus and S. epidermidis. The ST120 showed prolonged drug (AMX and 5-Fcil) release and antimicrobial efficacy than ST150 and calcined samples. This technique would be simple and rapid for composites preparation, to produce high quality crystalline, resorbable, mesoporous and bioactive nanocomposite (CHAp/agarose) powders. This work provides new insight into the role of agarose coated on bioceramics by solvothermal technique and suggests that CHAp/agarose composites powders are promising materials for filling of void in bone and drug delivery applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Development of Al2O3 electrospun fibers prepared by conventional sintering method or plasma assisted surface calcination

NASA Astrophysics Data System (ADS)

Mudra, E.; Streckova, M.; Pavlinak, D.; Medvecka, V.; Kovacik, D.; Kovalcikova, A.; Zubko, P.; Girman, V.; Dankova, Z.; Koval, V.; Duzsa, J.

2017-09-01

In this paper, the electrospinning method was used for preparation of α-Al2O3 microfibers from PAN/Al(NO3)3 precursor solution. The precursor fibers were thermally treated by conventional method in furnace or low-temperature plasma induced surface sintering method in ambient air. The four different temperatures of PAN/Al(NO3)3 precursors were chosen for formation of α-Al2O3 phase by conventional sintering way according to the transition features observed in the TG/DSC analysis. In comparison, the low-temperature plasma treatment at atmospheric pressure was used as an alternative sintering method at the exposure times of 5, 10 and 30 min. FTIR analysis was used for evaluation of residual polymer after plasma induced calcination and for studying the mechanism of polymer degradation. The polycrystalline alumina fibers arranged with the nanoparticles was created continuously throughout the whole volume of the sample. On the other side the low temperature approach, high density of reactive species and high power density of plasma generated at atmospheric pressure by used plasma source allowed rapid removal of polymer in preference from the surface of fibers leading to the formation of composite ceramic/polymer fibers. This plasma induced sintering of PAN/Al(NO3)3 can have obvious importance in industrial applications where the ceramic character of surface with higher toughness of the fibers are required.

The Leaching of Aluminium In Spanish Clays, Coal Mining Wastes and Coal Fly Ashes by Sulphuric Acid.

NASA Astrophysics Data System (ADS)

Fernández, A. M.; Ibáñez, J. L.; Llavona, M. A.; Zapico, R.

The acid leaching of aluminium from several non traditional ores, bayerite, kaolinite, different clays, coal mining wastes and coal fly ashes, and the kinetic of their dissolution are described. The effects of time, temperature, acid concentration, sample calcination, particle size were examined. The leaching of aluminium is dependent on acid concentration and strongly on temperature. Generally, the time to reach a fixed percentage of dissolution decreases with increasing acid concentration in the range 6% to 40% acid by weight. On clays and coal mining wastes a good relation between Al removal and ratio kaolinite/illite was also observed at all temperatures and acid concentration tested. Coal fly ashes are particles that were heated at very high temperatures in the power station and Al compounds were transformed into mullite and so Al recovery was minor. Several rate equations describing the kinetics of the leach reaction were discussed and Kinetic parameters and activation energy values of samples are presented.

Preparation of ordered mesoporous alumina-doped titania films with high thermal stability and their application to high-speed passive-matrix electrochromic displays.

PubMed

Jiang, Xiangfen; Bastakoti, Bishnu Prasad; Weng, Wu; Higuchi, Tetsuya; Oveisi, Hamid; Suzuki, Norihiro; Chen, Wei-Jung; Huang, Yu-Tzu; Yamauchi, Yusuke

2013-08-12

Ordered mesoporous alumina-doped titania thin films with anatase crystalline structure were prepared by using triblock copolymer Pluronic P123 as structure-directing agent. Uniform Al doping was realized by using aluminum isopropoxide as a dopant source which can be hydrolyzed together with titanium tetraisopropoxide. Aluminum doping into the titania framework can prevent rapid crystallization to the anatase phase, thereby drastically increasing thermal stability. With increasing Al content, the crystallization temperatures tend to increase gradually. Even when the Al content doped into the framework was increased to 15 mol %, a well-ordered mesoporous structure was obtained, and the mesostructural ordering was still maintained after calcination at 550 °C. During the calcination process, large uniaxial shrinkage occurred along the direction perpendicular to the substrate with retention of the horizontal mesoscale periodicity, whereby vertically oriented nanopillars were formed in the film. The resulting vertical porosity was successfully exploited to fabricate a high-speed and high-quality passive-matrix electrochromic display by using a leuco dye. The vertical nanospace in the films can effectively prevent drifting of the leuco dye. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ceramic-like open-celled geopolymer foam as a porous substrate for water treatment catalyst

NASA Astrophysics Data System (ADS)

Kovářík, T.; Křenek, T.; Pola, M.; Rieger, D.; Kadlec, J.; Franče, P.

2017-02-01

This paper presents results from experimental study on microstructural and mechanical properties of geopolymer-based foam filters. The process for making porous ceramic-like geopolymer body was experimentally established, consists of (a) geopolymer paste synthesis, (b) ceramic filler incorporation, (c) coating of open-celled polyurethane foam with geopolymer mixture, (d) rapid setting procedure, (e) thermal treatment. Geopolymer paste was based on potassium silicate solution n(SiO2)/n(K2O)=1.6 and powder mixture of calcined kaolin and precipitated silica. Various types of ceramic granular filler (alumina, calcined schistous clay and cordierite) were tested in relation to aggregate gradation design and particle size distribution. The small amplitude oscillatory rheometry in strain controlled regime 0.01% with angular frequency 10 rad/s was applied for determination of rheology behavior of prepared mixtures. Thermal treatment conditions were applied in the temperature range 1100 - 1300 °C. The developed porous ceramic-like foam effectively served as a substrate for highly active nanoparticles of selected Fe+2 spinels. Such new-type of nanocomposite was tested as a heterogeneous catalyst for technological process of advanced oxidative degradation of resistive antibiotics occurring in waste waters.

Phase transformations of α-alumina made from waste aluminum via a precipitation technique.

PubMed

Matori, Khamirul Amin; Wah, Loy Chee; Hashim, Mansor; Ismail, Ismayadi; Zaid, Mohd Hafiz Mohd

2012-12-07

We report on a recycling project in which α-Al(2)O(3) was produced from aluminum cans because no such work has been reported in literature. Heated aluminum cans were mixed with 8.0 M of H(2)SO(4) solution to form an Al(2)(SO(4))(3) solution. The Al(2)(SO(4))(3) salt was contained in a white semi-liquid solution with excess H(2)SO(4); some unreacted aluminum pieces were also present. The solution was filtered and mixed with ethanol in a ratio of 2:3, to form a white solid of Al(2)(SO(4))(3)·18H(2)O. The Al(2)(SO(4))(3)·18H(2)O was calcined in an electrical furnace for 3 h at temperatures of 400-1400 °C. The heating and cooling rates were 10 °C /min. XRD was used to investigate the phase changes at different temperatures and XRF was used to determine the elemental composition in the alumina produced. A series of different alumina compositions, made by repeated dehydration and desulfonation of the Al(2)(SO(4))(3)·18H(2)O, is reported. All transitional alumina phases produced at low temperatures were converted to α-Al(2)O(3) at high temperatures. The X-ray diffraction results indicated that the α-Al(2)O(3) phase was realized when the calcination temperature was at 1200 °C or higher.

Phase Transformations of α-Alumina Made from Waste Aluminum via a Precipitation Technique

PubMed Central

Matori, Khamirul Amin; Wah, Loy Chee; Hashim, Mansor; Ismail, Ismayadi; Zaid, Mohd Hafiz Mohd

2012-01-01

We report on a recycling project in which α-Al2O3 was produced from aluminum cans because no such work has been reported in literature. Heated aluminum cans were mixed with 8.0 M of H2SO4 solution to form an Al2(SO4)3 solution. The Al2(SO4)3 salt was contained in a white semi-liquid solution with excess H2SO4; some unreacted aluminum pieces were also present. The solution was filtered and mixed with ethanol in a ratio of 2:3, to form a white solid of Al2(SO4)3·18H2O. The Al2(SO4)3·18H2O was calcined in an electrical furnace for 3 h at temperatures of 400–1400 °C. The heating and cooling rates were 10 °C/min. XRD was used to investigate the phase changes at different temperatures and XRF was used to determine the elemental composition in the alumina produced. A series of different alumina compositions, made by repeated dehydration and desulfonation of the Al2(SO4)3·18H2O, is reported. All transitional alumina phases produced at low temperatures were converted to α-Al2O3 at high temperatures. The X-ray diffraction results indicated that the α-Al2O3 phase was realized when the calcination temperature was at 1200 °C or higher. PMID:23222685

Visible light activity of Ag-loaded and guanidine nitrate-doped nano-TiO2: Degradation of dichlorophenol and antibacterial properties

EPA Science Inventory

To utilize visible light, co-doped nano-TiO2 was prepared via “one pot” synthesis using mild reaction conditions and benign precursors. Synthesis was optimized using an appropriate experimental design taking into account silver content and calcination temperature. The optimized ...

HIGH-TEMPERATURE, SHORT-TIME SULFATION OF CALCIUM- BASED SORBENTS. 1. THEORETICAL SULFATION MODEL

EPA Science Inventory

A mathematical model for the sulfation of CaO is developed around the overlapping grain concept. The potential influence of high mass-transfer rates from simultaneous calcination of CaCO3 or Ca(OH)2 is incorporated in the mass-transfer coefficient for SO2 diffusion to the partic...

METHOD FOR PREPARATION OF SINTERABLE BERYLLIUM OXIDE

DOEpatents

Sturm, B.J.

1963-08-13

High-purity beryllium oxide for nuclear reactor applications can be prepared by precipitation of beryllium oxalate monohydrate from aqueous solution at a temperature above 50 deg C and subsequent calcination of the precipitate. Improved purification with respect to metallic impurities is obtained, and the product beryllium oxide sinters reproducibly to a high density. (AEC)

A Novel Gas Sensor Based on MgSb2O6 Nanorods to Indicate Variations in Carbon Monoxide and Propane Concentrations

PubMed Central

Guillén-Bonilla, Héctor; Flores-Martínez, Martín; Rodríguez-Betancourtt, Verónica-María; Guillen-Bonilla, Alex; Reyes-Gómez, Juan; Gildo-Ortiz, Lorenzo; de la Luz Olvera Amador, María; Santoyo-Salazar, Jaime

2016-01-01

Bystromite (MgSb2O6) nanorods were prepared using a colloidal method in the presence of ethylenediamine, after a calcination step at 800 °C in static air. From X-ray powder diffraction analyses, a trirutile-type structure with lattice parameters a = 4.64 Å and c = 9.25 Å and space group P42/mnm was identified. Using scanning electron microscopy (SEM), microrods with sizes from 0.2 to 1.6 μm were observed. Transmission electron microscopy (TEM) analyses revealed that the nanorods had a length of ~86 nm and a diameter ~23.8 nm. The gas-sensing properties of these nanostructures were tested using pellets elaborated with powders of the MgSb2O6 oxide (calcined at 800 °C) at temperatures 23, 150, 200, 250 and 300 °C. The pellets were exposed to different concentrations of carbon monoxide (CO) and propane (C3H8) at these temperatures. The results showed that the MgSb2O6 nanorods possess excellent stability and high sensitivity in these atmospheres. PMID:26840318

A Novel Gas Sensor Based on MgSb2O6 Nanorods to Indicate Variations in Carbon Monoxide and Propane Concentrations.

PubMed

Guillén-Bonilla, Héctor; Flores-Martínez, Martín; Rodríguez-Betancourtt, Verónica-María; Guillen-Bonilla, Alex; Reyes-Gómez, Juan; Gildo-Ortiz, Lorenzo; de la Luz Olvera Amador, María; Santoyo-Salazar, Jaime

2016-01-30

Bystromite (MgSb2O6) nanorods were prepared using a colloidal method in the presence of ethylenediamine, after a calcination step at 800 °C in static air. From X-ray powder diffraction analyses, a trirutile-type structure with lattice parameters a = 4.64 Å and c = 9.25 Å and space group P4₂/mnm was identified. Using scanning electron microscopy (SEM), microrods with sizes from 0.2 to 1.6 μm were observed. Transmission electron microscopy (TEM) analyses revealed that the nanorods had a length of ~86 nm and a diameter ~23.8 nm. The gas-sensing properties of these nanostructures were tested using pellets elaborated with powders of the MgSb2O6 oxide (calcined at 800 °C) at temperatures 23, 150, 200, 250 and 300 °C. The pellets were exposed to different concentrations of carbon monoxide (CO) and propane (C3H8) at these temperatures. The results showed that the MgSb2O6 nanorods possess excellent stability and high sensitivity in these atmospheres.

Synthesis, characterization and magnetic properties of MFe2O4 (M=Co, Mg, Mn, Ni) nanoparticles using ricin oil as capping agent

NASA Astrophysics Data System (ADS)

Gherca, Daniel; Pui, Aurel; Cornei, Nicoleta; Cojocariu, Alina; Nica, Valentin; Caltun, Ovidiu

2012-11-01

We focused on obtaining MFe2O4 nanoparticles using ricin oil solution as surfactant and on their structural characterization and magnetic properties. The annealed samples at 500 °C in air for 6 h were analyzed for the crystal phase identification by powder X-ray diffraction using CuKα radiation. The particle size, the chemical composition and the morphology of the calcinated powders were characterized by scanning electron microscopy. All sintered samples contain only one phase, which has a cubic structure with crystallite sizes of 12-21 nm. From the infrared spectra of all samples were observed two strong bands around 600 and 400 cm-1, which correspond to the intrinsic lattice vibrations of octahedral and tetrahedral sites of the spinel structure, respectively, and characteristic vibration for capping agent. The magnetic properties of fine powders were investigated at room temperature by using a vibrating sample magnetometer. The room temperature M-H hysteresis loops show ferromagnetic behavior of the calcined samples, with specific saturation magnetization (Ms) values ranging between 11 and 53 emu/g.

Fabrication and application of mesoporous TiO2 film coated on Al wire by sol-gel method with EISA

NASA Astrophysics Data System (ADS)

Zhao, Linkang; Lu, Jianjun

2017-04-01

Mesoporous TiO2 film on Al wire was fabricated by sol-gel method with evaporation induced self assembly (EISA) process using F127 as templating agent in the mixed solution of ethanol and Tetra-n-butyl Titanate. The Ni/TiO2 film catalyst supported on Al wire was prepared by impregnation and the catalytic performance on methanation was carried out in a titanium alloy micro-reactor tube. It was shown that anatase mesoporous TiO2 film was prepared in this conditions (1 g F127,calcined at 400 °C and aged for 24 h), which has specific surface area of 127 m2 g-1 and narrow pore size distribution of 5.3 nm. Low calcined temperature (300 °C) cannot transfer film to anatase and decompose F127 completely. Ni/TiO2 film on Al wire catalyst was proved to be active in CO methanation reaction. And the CO conversion reaches 99% and CH4 selectivity close is to 80% when the reaction temperature is higher 360 °C.

Synthesis of adsorbent with zeolite structure from red mud and rice husk ash and its properties

NASA Astrophysics Data System (ADS)

Quyen, Dinh Thi Ngoc; Loc, Luu Cam; Ha, Huynh Ky Phuong; Nga, Dang Thi Hang; Tri, Nguyen; Van, Nguyen Thi Thuy

2017-09-01

There are many researches in the modification of red mud as adsorbent for treatment of wastewater or waste gases. Yet, most of them have to face up with a thorny problem caused by remaining alkali in red mud. In this study, the material with zeolite structure was synthesized by fusion method using red mud with the remaining alkali and rice husk ash as raw materials. It comprised alkaline fusion followed by hydrothermal treatment with step - change of synthesis temperature. The synthesized materials were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), BET and CO2 adsorption capacity. The influences on the quality of these materialswere investigated under various calcination temperatures, calcination times and the ratios of raw materials (based on SiO2/Al2O3 ratio). The optimum reaction parameters were determined. The results depicted that the sample treated at 600 °C for 2 hours with the ratio of SiO2/Al2O3 of 1.8 had the best adsorption capacity and total specific surface area compared with the others.

Thermal and Surface Evaluation on The Process of Forming a Cu2O/CuO Semiconductor Photocatalyst on a Thin Copper Plate

NASA Astrophysics Data System (ADS)

Zainul, R.; Oktavia, B.; Dewata, I.; Efendi, J.

2018-04-01

This research aims to investigate the process of forming a multi-scale copper oxide semiconductor (CuO/Cu2O) through a process of calcining a copper plate. The changes that occur during the formation of the oxide are thermally and surface evaluated. Evaluation using Differential Thermal Analysis (DTA) obtained by surface change of copper plate happened at temperature 380°C. Calcination of oxide formation was carried out at temperature 380°C for 1 hour. Surface evaluation process by using Scanning Electron Microscope (SEM) surface and cross-section, to determine diffusion of oxide formation on copper plate. The material composition is monitored by XRF and XRD to explain the process of structural and physical changes of the copper oxide plate formed during the heating process. The thickness of Cu plates used is 200-250 μm. SEM analysis results, the oxygen atom interruption region is in the range of 20-30 μm, and diffuses deeper during thermal oxidation process. The maximum diffusion depth of oxygen atoms reaches 129 μm.

Effect of sulfuric acid concentration of bentonite and calcination time of pillared bentonite

NASA Astrophysics Data System (ADS)

Mara, Ady; Wijaya, Karna; Trisunaryati, Wega; Mudasir

2016-04-01

An activation of natural clay has been developed. Activation was applied by refluxing the natural bentonite in variation of the sulfuric acid concentration and calcination time of pillared bentonite (PLC). Calcination was applied using oven in microwave 2,45 GHz. Determination of acidity was applied by measuring the amount of adsorbed ammonia and pyridine. Morphological, functional groups and chrystanility characterizations were analyzed using SEM, TEM, FTIR and XRD. Porosity was analyzed using SSA. The results showed that the greater of the concentration of sulfuric acid and calcination time was, the greater the acidity of bentonite as well as the pore diameter were. FTIR spectra showed no fundamental changes in the structure of the natural bentonite, SEM, and TEM images were showing an increase in space or field due to pillarization while the XRD patterns showed a shift to a lower peak. Optimization was obtained at a concentration of 2 M of sulfuric acid and calcination time of 20 minutes, keggin ion of 2.2 and suspension of 10 mmol, respectively each amounted to 11.7490 mmol/gram of ammonia and 2.4437 mmol/gram of pyridine with 154.6391 m2/gram for surface area, 0.130470 m3/gram of pore volume and 3.37484 nm of pore diameter.

Sorption-desorption of antimony species onto calcined hydrotalcite: Surface structure and control of competitive anions.

PubMed

Constantino, Leonel Vinicius; Quirino, Juliana Nunes; Abrão, Taufik; Parreira, Paulo Sérgio; Urbano, Alexandre; Santos, Maria Josefa

2018-02-15

Calcined hydrotalcite can be applied to remove anionic contaminants from aqueous systems such as antimony species due to its great anion exchange capacity and high surface area. Hence, this study evaluated antimonite and antimonate sorption-desorption processes onto calcined hydrotalcite in the presence of nitrate, sulfate and phosphate. Sorption and desorption experiments of antimonite and antimonate were carried out in batch equilibrium and the post-sorption solids were analyzed by X-ray fluorescence (EDXRF). Sorption data were better fitted by dual-mode Langmuir-Freundlich model (R 2 >0.99) and desorption data by Langmuir model. High maximum sorption capacities were found for the calcined hydrotalcite, ranging from 617 to 790meqkg -1 . The competing anions strongly affected the antimony sorption. EDXRF analysis and mathematical modelling showed that sulfate and phosphate presented higher effect on antimonite and antimonate sorption, respectively. High values for sorption efficiency (SE=99%) and sorption capacity were attributed to the sorbent small particles and the large surface area. Positive hysteresis indexes and low mobilization factors (MF>3%) suggest very low desorption capacity to antimony species from LDH. These calcined hydrotalcite characteristics are desirable for sorption of antimony species from aqueous solutions. Copyright © 2017. Published by Elsevier B.V.

Effects of chlorine on the volatilization of heavy metals during the co-combustion of sewage sludge.

PubMed

Yu, Shengrong; Zhang, Bin; Wei, Jiangxiong; Zhang, Tongsheng; Yu, Qijun; Zhang, Wensheng

2017-04-01

To clarify the volatilization of heavy metals (Cu, Ni, Pb, and Zn) in sewage sludge during co-combustion in cement kiln, effects of addition and types of four chlorides and temperature on the volatilization of heavy metals in raw meal with 25wt.% sewage sludge were investigated. The results showed that the volatilization of Cu, Ni, and Pb increased significantly with increase of chlorides addition, while no obvious change in the volatilization of Zn was observed. The effectiveness of chlorides on the volatilization of heavy metals depended on their release capacity of chlorine radicals and the chlorine combined capacity of heavy metals. Higher calcination temperature resulted in dramatically increase in the volatilization of heavy metals due to easier formation of volatile heavy metal chlorides. The results will provide a guideline for co-combusting heavy metals contained solid wastes in cement kiln on the basis of security. Copyright © 2017 Elsevier Ltd. All rights reserved.

[Preparation of porous ceramics based on waste ceramics and its Ni2+ adsorption characteristics].

PubMed

Zhang, Yong-Li; Wang, Cheng-Zhi; Shi, Ce; Shang, Ling-Ling; Ma, Rui; Dong, Wan-Li

2013-07-01

The preparation conditions of porous ceramics were determined by SEM, XRD and FT-IR characterizations as well as the nickel removal ability of porous ceramics to be: the mass fraction w of sesbania powder doped was 4%, and the calcination temperature was 800 degrees C. SEM and pore structure characterization illustrated that calcination caused changes in the structure and morphology of waste ceramics. With the increase of calcination temperature, the specific surface area and pore volume decreased, while the aperture increased. EDS analyses showed that the main elements of both the original waste porcelain powder and the porous ceramics were Si, Al and O. The SEM, XRD and FT-IR characterization of porous ceramics illustrated that the structure of porous ceramics was stable before and after adsorption. The series of experiments of Ni2+ adsorption using these porous ceramics showed that when the dosage of porous ceramics was 10 g x L(-1), the adsorption time was 60 min, the pH value was 6.32, and the concentration of nickel-containing wastewater was below 100 mg x L(-1), the Ni2+ removal of wastewater reached 89.7%. Besides, the porous ceramics showed higher removal efficiency on nickel in the wastewater. The Ni(2+)-containing wastewater was processed by the porous ceramics prepared, and the adsorption dynamics and adsorption isotherms of Ni2+ in wastewater by porous ceramics were investigated. The research results showed that the Ni2+ adsorption process of porous ceramics was in accordance with the quasi second-order kinetic model (R2 = 0.999 9), with Q(e) of 9.09 mg x g(-1). The adsorption process can be described by the Freundlich equation and Langmuir equation, and when the temperature increased from 20 degrees C to 40 degrees C, the maximum adsorption capacity Q(m) increased from 14.49 mg x g(-1) to 15.38 mg x g(-1).

Advanced Ceramic Technology for Space Applications at NASA MSFC

NASA Technical Reports Server (NTRS)

Alim, Mohammad A.

2003-01-01

The ceramic processing technology using conventional methods is applied to the making of the state-of-the-art ceramics known as smart ceramics or intelligent ceramics or electroceramics. The sol-gel and wet chemical processing routes are excluded in this investigation considering economic aspect and proportionate benefit of the resulting product. The use of ceramic ingredients in making coatings or devices employing vacuum coating unit is also excluded in this investigation. Based on the present information it is anticipated that the conventional processing methods provide identical performing ceramics when compared to that processed by the chemical routes. This is possible when sintering temperature, heating and cooling ramps, peak temperature (sintering temperature), soak-time (hold-time), etc. are considered as variable parameters. In addition, optional calcination step prior to the sintering operation remains as a vital variable parameter. These variable parameters constitute a sintering profile to obtain a sintered product. Also it is possible to obtain identical products for more than one sintering profile attributing to the calcination step in conjunction with the variables of the sintering profile. Overall, the state-of-the-art ceramic technology is evaluated for potential thermal and electrical insulation coatings, microelectronics and integrated circuits, discrete and integrated devices, etc. applications in the space program.

Calcination process for radioactive wastes

DOEpatents

Kilian, Douglas C.

1976-05-04

The present invention provides a method for minimizing the volatilization of chlorides during solidification in a fluidized-bed calciner of liquids containing sodium, nitrate and chloride ions. Zirconium and fluoride are introduced into the liquid, and one-half mole of calcium nitrate is added per mole of fluoride present in the liquid mixture. The mixture is calcined in the fluidized-bed calciner at about 500.degree.C., producing a high bulk density calcine product containing the chloride, thus tying up the chloride in the solid product and minimizing chloride volatilization.

Synthesis, characterization and sonocatalytic applications of nano-structured carbon based TiO2 catalysts.

PubMed

Choi, Jongbok; Cui, Mingcan; Lee, Yonghyeon; Kim, Jeonggwan; Yoon, Yeomin; Jang, Min; Khim, Jeehyeong

2018-05-01

In order to enhance sonocatalytic oxidation of a recalcitrant organic pollutant, rhodamine B (RhB), it is necessary to study the fundamental aspects of sonocatalysis. In this study, TiO 2 -incorporated nano-structured carbon (i.e., carbon nanotubes (CNTs) or graphene (GR)) composites were synthesized by coating TiO 2 on CNTs or GR of different mass percentages (0.5, 1, 5, and 10 wt%) by a facile hydrothermal method. The sonocatalytic degradation rates of RhB were examined for the effect of ultrasound (US) frequency and calcination temperature by using the prepared TiO 2 -NSC composites. Since US frequency affected the sonoluminescence (SL) intensities, it was proposed that there exists a correlation between the surface area or band-gap of the sonocatalysts and the degradation kinetic constants of RhB. In addition, the reusability of TiO 2 -GR composites was also investigated. Overall, the performance of TiO 2 -GRs prepared by the hydrothermal method was better than that of calcined TiO 2 -CNTs. Among TiO 2 -GRs, 5% GR incorporated media (TiO 2 -GR-5) showed the best performance. Interestingly, the kinetic constants of sonocatalysts prepared under hydrothermal conditions had a negative linear relationship with the band-gap energy for the corresponding media. Furthermore, the strongest SL intensity and highest degradation rates of RhB for both carbonaceous composites were observed at 500 kHz. The kinetic constants of calcined media decreased linearly as the specific area of the media decreased, while the band-gap energy could not be correlated with the kinetic constants. The GR combined TiO 2 composite might be a good sonocatalyst in wastewater treatment using ultrasound-based oxidation because of its high stability. Copyright © 2018 Elsevier B.V. All rights reserved.

Low-temperature synthesis and investigations on photocatalytic activity of nanoparticles BiFeO3 for methylene blue and methylene orange degradation and some toxic organic compounds

NASA Astrophysics Data System (ADS)

Nhiem Dao, Ngoc; Luu, Minh Dai; Chuc Pham, Ngoc; Dung Doan, Trung; Nguyen, Thi Ha Chi; Bac Nguyen, Quang; Lim Duong, Thi

2016-12-01

The photocatalytic BiFeO3 perovskite nanoparticles were fabricated by gel combustion method using polyvinyl alcohol and corresponding metal nitrate precursors under the optimum mild conditions such as pH 2, gel formation temperature of 80 °C, metal/polyvinyl alcohol molar ratio of 1/3, metal molar ratio Bi/Fe of 1/1 and calcination temperature at 500 °C for 2 h. The prepared sample was characterized by x-ray diffraction, field scanning electron microscopy, transmission electron microscopy, Brunauer-Emmetl-Teller nitrogen adsorption method at 77 K, energy dispersive x-ray spectroscopy, ultraviolet-visible light spectrophotometry, and thermal analysis. The effects of molar ratios of starting material and calcination temperature on phase formation and morphology were investigated. The degradation of methylene blue, methylene orange and some toxic organic compounds such as phenol and diazinon under visible light irradiation by photocatalytic BiFeO3 nanoparticles were evaluated at different parameters and conditions such as the light intensity determined from the light source to the measured sample, the addition H2O2, reaction time and the regeneration performance. Obtained results showed that the synthesized perovskite BiFeO3 nanoparticles for the optimized sample have a size smaller than 50 nm and the high mean surface area of 50 m2 g-1. Degradation efficiency was almost 90.0% for methylene blue and 80.0% for methylene orange with added H2O2 after 30 min of reaction. After the 3rd time of regeneration, the BiFeO3 nanoparticles still have 92.8% of the degradation performance for removing methylene blue. Phenol and diazinon toxic compound were degraded with the performance of 92.42% and 85.7%, respectively, for 150 min

10. VIEW OF CALCINER IN ROOM 146148. THE CALCINER HEATED ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

10. VIEW OF CALCINER IN ROOM 146-148. THE CALCINER HEATED PLUTONIUM PEROXIDE TO CONVERT IT TO PLUTONIUM OXIDE. THE PROCESS REMOVED RESIDUAL WATER AND NITRIC ACID LEAVING A DRY, POWDERED PRODUCT. (4/29/65) - Rocky Flats Plant, Plutonium Recovery & Fabrication Facility, North-central section of plant, Golden, Jefferson County, CO

Influence of calcinated and non calcinated nanobioglass particles on hardness and bioactivity of sol-gel-derived TiO2-SiO2 nano composite coatings on stainless steel substrates.

PubMed

Dadash, Mohammad Saleh; Karbasi, Saeed; Esfahani, Mojtaba Nasr; Ebrahimi, Mohammad Reza; Vali, Hojatollah

2011-04-01

Thick films of calcinated and non calcinated nanobioglass (NBG)-titania composite coatings were prepared on stainless steel substrates by alkoxide sol-gel process. Dip-coating method was used for the films preparation. The morphology, structure and composition of the nano composite films were evaluated using environmental scanning electron microscope, X-ray diffraction and Fourier transform infrared spectroscope. The SEM investigation results showed that prepared thick NBG-titania films are smooth and free of macrocracking, fracture or flaking. The grain size of these films was uniform and nano scale (50-60 nm) which confirmed with TEM. Also FTIR confirmed the presence of Si-O-Si bands on the calcinated NBG-titania films. The hardness of the prepared films (TiO(2)-calcinated NBG and TiO(2)-Non calcinated NBG) was compared by using micro hardness test method. The results verified that the presence of calcinated NBG particles in NBG-titania composite enhanced gradually the mechanical data of the prepared films. The in vitro bioactivity of these films was discussed based on the analysis of the variations of Ca and P concentrations in the simulated body fluid (SBF) and their surface morphologies against immersion time. Surface morphology and Si-O-Si bands were found to be of great importance with respect to the bioactivity of the studied films. The results showed that calcinated NBG-titania films have better bioactivity than non calcinated NBG-titania films.

Role of annealing temperature on microstructural and electro-optical properties of ITO films produced by sputtering

NASA Astrophysics Data System (ADS)

Senol, Abdulkadir; Gulen, Mahir; Yildirim, Gurcan; Ozturk, Ozgur; Varilci, Ahmet; Terzioglu, Cabir; Belenli, Ibrahim

2013-03-01

In this study, we investigate the effect of annealing temperature on electrical, optical and microstructural properties of indium tin oxide (ITO) films deposited onto Soda lime glass substrates by conventional direct current (DC) magnetron reactive sputtering technique at 100 watt using an ITO ceramic target (In2O3:SnO2, 90:10 wt. %) in argon atmosphere at room temperature. The films obtained are exposed to the calcination process at different temperature up to 700 ° C. Resistivity, Hall Effect, X-ray diffractometer (XRD), ultra violet-visible spectrometer (UV-vis) and atomic force microscopy (AFM) measurements are performed to characterize the samples. Moreover, phase purity, surface morphology, optical and photocatalytic properties of the films are compared with each other. Furthermore, mobility, carrier density and conductivity characteristics of the samples prepared are carried out as function of temperature in the range of 80-300 K at the magnetic field of 0.550 T. The results obtained show that all the properties depend strongly on the annealing temperature and in fact the film annealed at 400 ° C obtains the better optical properties due to the high refractive index while the film produced at 100 °C exhibits much better photoactivity than the other films as a result of the large optical energy band gap.

Nuclear waste solidification

DOEpatents

Bjorklund, William J.

1977-01-01

High level liquid waste solidification is achieved on a continuous basis by atomizing the liquid waste and introducing the atomized liquid waste into a reaction chamber including a fluidized, heated inert bed to effect calcination of the atomized waste and removal of the calcined waste by overflow removal and by attrition and elutriation from the reaction chamber, and feeding additional inert bed particles to the fluidized bed to maintain the inert bed composition.

Effect of hydroxyapatite on the biodegradation and biomechanical stability of polyester nanocomposites for orthopaedic applications.

PubMed

Jayabalan, M; Shalumon, K T; Mitha, M K; Ganesan, K; Epple, M

2010-03-01

The effect of hydroxyapatite (HAP) on the performance of nanocomposites of an unsaturated polyester, i.e., hydroxy-terminated high molecular weight poly(proplyene fumarate) (HT-PPFhm), was investigated. A thermoset nanocomposite was prepared with nanoparticles of calcined HAP (<100 nm, rod-like shape, filler content 30 wt.%), HT-PPFhm and N-vinyl pyrrolidone, dibenzoyl peroxide and N,N-dimethyl aniline. Two more nanocomposites were prepared with precipitated HAP nanoparticles (<100 nm rod-like shape) and commercially available HAP nanoparticles (<200 nm spherical shape), respectively. Calcined HAP nanoparticles resulted in very good crosslinking in the resin matrix with high crosslinking density and interfacial bonding with the polymer, owing to the rod-like shape of the nanoparticles; this gave improved biomechanical strength and modulus and also controlled degradation of the nanocomposite for scaffold formation. The tissue compatibility and osteocompatibility of the nanocomposite containing calcined HAP nanoparticles was evaluated. The tissue compatibility was studied by intramuscular implantation in a rabbit animal model for 3 months as per ISO standard 10993/6. The in vivo femoral bone repair was also carried out in the rabbit animal model as per ISO standard 10993/6. The nanocomposite containing calcined HAP nanoparticles is both biocompatible and osteocompatible. Copyright 2009 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Elucidation of reaction mechanism involved in the formation of LaNiO3 from XRD and TG analysis

NASA Astrophysics Data System (ADS)

Dharmadhikari, Dipti V.; Athawale, Anjali A.

2013-06-01

The present work is focused on the synthesis and elucidation of reaction mechanism involved in the formation of LaNiO3 with the help of X-ray diffraction (XRD) and thermogravimetric (TG) analysis. LaNiO3 was synthesized by hydrothermal method by heating at 160°C under autogenous pressure for 6h. Pure phase product was obtained after calcining the hydrothermally activated product for 6h at 700°C. The various phases of the product obtained after hydrothermal treatment and calcination followed by the formation of pure phase nanocrystalline lanthanum nickel oxide could be determined from XRD analysis of the samples. The reaction mechanism and phase formation temperature has been interpreted by thermogravimetric analysis of the hydrothermally synthesized product and XRD analysis.

Neodymium cobalt oxide as a chemical sensor

NASA Astrophysics Data System (ADS)

Abdel-Latif, I. A.; Rahman, Mohammed M.; Khan, Sher Bahadar

2018-03-01

Chemical sensing and electrical transport properties of neodymium coblate, NdCoO3, was investigated in this work. It was prepared by using co-precipitation method. Pure neodymium chloride and cobalt chloride were mixing in the presence of sodium hydroxide and the obtained co-precipitated powder was calcined at 850 and 1000 °C. The synthesized composites, as-grown (NdCoO3-I), calcined at 850 °C (NdCoO3-II), and calcined at 1000 °C (NdCoO3-III) were studied in details in terms of their morphological and structural properties. The X-ray analysis confirmed that the synthesized products are well crystalline possessing single phase orthorhombic crystal system of space group Pbnm(62). The crystallite size of NdCoO3-I, NdCoO3-II, and NdCoO3-III is 22, 111, and 338 nm, respectively which reflect that crystallite size is increasing with increase in firing temperature. The DC resistivity was measured as a function of temperature in the temperature range from room temperature up to 200 °C. All NdCoO3 are semiconductor in this range of temperature but showed different activation energy which strongly depends on the crystallite size of the products. The activation energy decreased with increase in crystallite size, 0.798, 0.414 and 0.371 eV for NdCoO3-I, NdCoO3-II, and NdCoO3-III, respectively. Thus resistivity increases with increase in crystallite size of NdCoO3. All NdCoO3 products were tested as chemical sensor for acetone by electrochemical approaches and showed excellent sensitivity. Among the NdCoO3 samples, NdCoO3-III showed the highest sensitivity (3.4722 μAcm-2 mM-1) compared to other compositions and gradually decreased to 3.2407 μAcm-2 mM-1 with decreasing the crystallite size of NdCoO3-II. It is also observed that the sensitivity drastically decreased to 0.76253 μAcm-2 mM-1 in the case of NdCoO3-I. It is introduced an efficient route for the detection of environmental unsafe chemicals by electrochemical approach for the safety of healthcare and environmental fields in broad scales.

Steam Reforming of CH4 Using Ni- Substituted Pyrochlore Catalysts

NASA Astrophysics Data System (ADS)

Haynes, Daniel J.

The steam reforming of methane (SMR) continues to remain an important industrial reaction for large-scale production of H2 as well as synthesis gas mixtures which can be used for the production of useful chemicals (e.g. methanol). Although SMR is a rather mature technology, traditional nickel based catalysts used industrially are subjected to severe temperatures and reaction conditions, which lead to irreversible activity loss through sintering, support collapse, and carbon formation. Pyrochlore-based mixed oxide have been identified as refractory materials that can be modified through the substitution of catalytic metals and other promoting species into the structure to mitigate these issues causing deactivation. For this study, a lanthanum zirconate pyrochlore catalyst was substituted with Ni to determine whether the oxide structure could effectively stabilize the activity of the catalytic metal during the SMR. The effect of different variables including calcination temperature, a comparison of a substituted versus supported Ni pyrochlore catalyst, Ni weight loading, and Sr promotion have been evaluated to determine the location of the Ni in the structure, and their effect on catalytic behavior. It was revealed that the effect of calcination temperature on a 6wt% Ni substituted pyrochlore produced by the Pechini method demonstrated very little Ni was soluble in the pyrochlore lattice. It was further revealed that by XRD, TEM, and atom probe tomography that, despite the metal loading, Ni exsolves from the structure upon crystallization of the pyrochlore at 700°C, and forms NiO at the surface and grain boundaries. An additional separate La2ZrNiO6 perovskite phase also began to form at higher temperatures (>800°C). Increasing calcination temperature was found to lead to slight sintering of the NiO at the surface, which made the NiO more reducible. Meanwhile decreasing the Ni weight loading was found to produce a lower reduction temperature due to the presence of less lanthanum at the surface. Comparing the XANES and EXAFS profiles for the supported and substituted Ni catalysts showed no detectable difference between the spectra, further confirming the Ni to be present as NiO after substitution. Activity testing found the NiO on the surface to be the active catalytic form. However, the Ni proved to be highly sensitive to sintering and oxidation by steam, especially under high pressures (1.8 MPa), which caused all catalysts to suffer irreversible activity loss. Low reaction pressures (0.23 MPa) elicited an activation effect in which the Ni initially lost activity, but then recovered to near equilibrium yields after nearly 10 hours time on stream. The activation was correlated with an increase in Ni particle size, as observed by XRD. It is speculated from similar behavior reported in the literature that ability to recovery activity was linked to a redox cycling of the Ni particles under reaction conditions, in which a small amount of the Ni was redistributed over the surface through the volatilization with steam, as well as the exsolution of the Sr from the structure which helped stabilize the Ni. A comparison of the supported and substituted forms of Ni showed the substituted form to have a weaker interaction with the pyrochlore surface, which is the likely cause for the rapid sintering and deactivation by steam. It was also found that the substitution of more Sr into the structure produced only strong basic sites, which resulted in a lower degree of activity loss and more stable activity under high pressure conditions (1.8 MPa) compared to the catalyst with less Sr. Carbon formation was not an issue for these materials, due to the rapid sintering and oxidation of the metal in-situ. Fitting the Ni particle size growth with time showed a parabolic relationship with growth proportional to time by the power 0.28. This value is close to results observed in the literature which indicates the Ni agglomerates via atomic migration.

Synthesis of Hollow Sphere and 1D Structural Materials by Sol-Gel Process.

PubMed

Li, Fa-Liang; Zhang, Hai-Jun

2017-08-25

The sol-gel method is a simple and facile wet chemical process for fabricating advanced materials with high homogeneity, high purity, and excellent chemical reactivity at a relatively low temperature. By adjusting the processing parameters, the sol-gel technique can be used to prepare hollow sphere and 1D structural materials that exhibit a wide application in the fields of catalyst, drug or gene carriers, photoactive, sensors and Li-ion batteries. This feature article reviewed the development of the preparation of hollow sphere and 1D structural materials using the sol-gel method. The effects of calcination temperature, soaking time, pH value, surfactant, etc., on the preparation of hollow sphere and 1D structural materials were summarized, and their formation mechanisms were generalized. Finally, possible future research directions of the sol-gel technique were outlined.

Synthesis of Hollow Sphere and 1D Structural Materials by Sol-Gel Process

PubMed Central

Li, Fa-Liang; Zhang, Hai-Jun

2017-01-01

The sol-gel method is a simple and facile wet chemical process for fabricating advanced materials with high homogeneity, high purity, and excellent chemical reactivity at a relatively low temperature. By adjusting the processing parameters, the sol-gel technique can be used to prepare hollow sphere and 1D structural materials that exhibit a wide application in the fields of catalyst, drug or gene carriers, photoactive, sensors and Li-ion batteries. This feature article reviewed the development of the preparation of hollow sphere and 1D structural materials using the sol-gel method. The effects of calcination temperature, soaking time, pH value, surfactant, etc., on the preparation of hollow sphere and 1D structural materials were summarized, and their formation mechanisms were generalized. Finally, possible future research directions of the sol-gel technique were outlined. PMID:28841188

Characterization and thermal behavior of PrMO{sub 3} (M = Co or Ni) ceramic materials obtained from gelatin

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aquino, F.M., E-mail: flavyma@hotmail.com; Melo, D.M.A.; Pimentel, P.M.

2012-09-15

Graphical abstract: The micrograph in figure shows sample calcined at temperature 900 °C. The sample exhibits morphology with considerable porosity and the formation of agglomerated nanometric particles. Gelatin provides the system with a large amount of organic matter, which is then removed during calcinations, favoring the appearance of pores in the material. Highlights: ► Oxides with PrNiO{sub 3} and PrCoO{sub 3} were prepared by new method synthesis. ► The gelatin, through its carboxylate groups and amine, is an efficient director. ► The obtained materials have magnetic properties and application in catalysis. ► The decomposition kinetic study of bonding groups ofmore » gelatin with metallic ions that takes part in the synthesis of PrMO{sub 3}. -- Abstract: Metal oxides with perovskite-type structure have attracted considerable interest in recent years due to their magnetic and electrical properties, as well as their catalytic activity. In this study, oxides with PrNiO{sub 3} and PrCoO{sub 3} composition were prepared by using gelatin powder as a precursor agent for its use as a catalyst. The powders obtained were calcined at 700 °C and 900 °C and characterized using the X-ray diffraction, thermal analysis (thermogravimetry and differential thermal analysis), infrared spectroscopy, temperature programed reduction and scanning electron microscopy techniques. Thermogravimetric data using the non-isothermal kinetic models of Flynn and Wall and “Model-free Kinetics” were used to determine the activation energy to study the decomposition kinetics of the ligand groups with system's metallic ions that takes part in the synthesis of PrMO{sub 3} (M = Ni or Co).« less

Development of Bioactive Ceramic Coating on Titanium Alloy substrate for Biomedical Application Using Dip Coating Method

NASA Astrophysics Data System (ADS)

Asmawi, R.; Ibrahim, M. H. I.; Amin, A. M.; Mustafa, N.; Noranai, Z.

2017-08-01

Bioactive apatite, such as hydroxyapatite ceramic (HA), [Ca10(PO4)6(OH)2] has been extensively investigated for biomedical applications due to its excellent biocompatibility and tissue bioactivity properties. Its bioactivity provides direct bonding to the bone tissue. Because of its similarity in chemical composition to the inorganic matrix of bone, HA is widely used as implant materials for bone. Unfortunately, because of its poor mechanical properties,. this bioactive material is not suitable for load bearing applications. In this study, by the assistance of dip-coating technique, HA coatings were deposited on titanium alloy substrates by employing hydrothermal derived HA powder. The produced coatings then were oven-dried at 130°C for 1 hour and calcined at various temperature over the range of 200-800°C for 1 hour. XRD measurement showed that HA was the only phase present in the coatings. However coatings calcined at 800°C comprised a mixture of HA and tri-calcium phosphate (TCP). FTIR measurement showed the existence of hydroxyl, phosphate, and carbonate bands. PO4 - band became sharper and narrower with the increased of calcination temperature. FESEM observation showed that the coating is polycrystalline with individual particles of nano to submicron size and has an average particle size of 35 nm. The thickness of the coating are direcly propotional with the viscosity of coating slurry. It was shown that the more viscous coating slurry would produce a thicker ceramic coating. Mechanical properties of the coating were measured in term of adhesion strength using a Micro Materials Nano Test microscratch testing machine. The result revealed that the coating had a good adhesion to the titanium alloy substrate.

Calcined Waste Storage at the Idaho Nuclear Technology and Engineering Center

DOE Office of Scientific and Technical Information (OSTI.GOV)

M. D. Staiger

2007-06-01

This report provides a quantitative inventory and composition (chemical and radioactivity) of calcined waste stored at the Idaho Nuclear Technology and Engineering Center. From December 1963 through May 2000, liquid radioactive wastes generated by spent nuclear fuel reprocessing were converted into a solid, granular form called calcine. This report also contains a description of the calcine storage bins.

UV-vis-DR study of VO x/SiO 2 catalysts prepared by sol-gel method

NASA Astrophysics Data System (ADS)

Moussa, N.; Ghorbel, A.

2008-12-01

Vanadia-silica catalysts with different vanadium loadings were prepared by sol-gel process. UV-vis diffuse-reflectance spectroscopy was used to elucidate the effect of drying mode (i.e., xerogel vs. aerogel), vanadium loading and calcination on the molecular structure of supported vanadium species. The results indicate that for vanadium loading ranging from 2.8 to 11.2 wt.%, the band-gap energies of all catalysts varying from 2.28 to 2.68 eV which demonstrate that vanadium oxides are predominantly in octahedral structure with the presence of tetrahedral species. The discrimination of different surface VO x species has been based on their characteristic Ligand to Metal Charge Transfer (LMCT) O → V(V) and d-d transition. It was found that the LMCT band position of V dbnd O bond is not affected by calcination either in xerogels or in aerogels but the position and the shape of bands relative to bridging V sbnd O sbnd V bonds are affected by vanadium loading, calcination and drying mode. For the same V/Si ratio, band-gap energy of xerogel is lower than that of aerogel which indicate that vanadium species are more dispersed in aerogels than in xerogels. Drying and calcination led to rearrangement, dehydration, cleavage and crystallization of vanadium species which explain the presence of some amount of crystalline V 2O 5 in calcined samples.

Micro Structural, Optical and Magnetic Properties of Co-SiO2 Nanocomposite Synthesized by Sol-Gel Technique

NASA Astrophysics Data System (ADS)

Saha, Mrinal; Mukherjee, Soumya; Gayen, Arup; Mukherjee, Siddhartha

2017-04-01

Co-SiO2 nano composite has been synthesized via sol-gel technique using dextrose [C6H12O6] as a reducer and tetraethyl orthosilicate [Si(OCH2CH3)4] as oxide forming agent, respectively. The dried gel has been subsequently calcined at different temperature (850 and 900 °C) for 30 min in an inert atmosphere by N2 purging. The synthesized materials have been characterized by X-ray diffraction, high resolution transmission microscope, Fourier transform infrared spectroscopy, UV-Vis spectroscopy, scanning electron microscope, field emission microscope, atomic force microscope and physical property measurement system. The crystallite sizes of the face centered cubic cobalt nano composite materials have been found to be in the range of 14-28 nm. The crystallite size of the material found to be increased at higher calcination temperature due to the grain growth. The surface morphology of the obtained material has been found to be agglomerated but spherical in nature. This agglomeration tendency could be attributed to magnetic interaction between particles, large surface area as well as high surface energy. The band gap value of the obtained material has been determined to be 1.92 eV. The saturation magnetization (Ms) and the coercivity (Hc) of the composite material were found to be 29.45 emu g-1and 23.2 Oe, respectively. This technique has thus been found to be a convenient and effective method to prepare pure metallic cobalt nanoparticles with uniform size and homogeneous distribution throughout the matrix.

A novel approach for the synthesis of SnO2 nanoparticles and its application as a catalyst in the reduction and photodegradation of organic compounds.

PubMed

Bhattacharjee, Archita; Ahmaruzzaman, M; Sinha, Tanur

2015-02-05

Tin oxide (SnO2) nanoparticles of sizes ∼4.5, ∼10 and ∼30 nm were successfully synthesized by a simple chemical precipitation method using amino acid, glycine which acts as a complexing agent and surfactant, namely sodium dodecyl sulfate (SDS) as a stabilizing agent, at various calcination temperatures of 200, 400 and 600°C. This method resulted in the formation of spherical SnO2 nanoparticles and the size of the nanoparticles was found to be a factor of calcination temperature. The spherical SnO2 nanoparticles show a tetragonal rutile crystalline structure. A dramatic increase in band gap energy (3.8-4.21 eV) was observed with a decrease in grain size (30-4.5 nm) due to three dimensional quantum confinement effect shown by the synthesized SnO2 nanoparticles. SnO2 nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and fourier transformed infrared spectroscopy (FT-IR). The optical properties were investigated using UV-visible spectroscopy. These SnO2 nanoparticles were employed as catalyst for the reduction of p-nitro phenol to p-amino phenol in aqueous medium for the first time. The synthesized SnO2 nanoparticles act as an efficient photocatalyst in the degradation of methyl violet 6B dye under direct sunlight. For the first time, methyl violet 6B dye was degraded by SnO2 nanoparticles under direct sunlight. Copyright © 2014 Elsevier B.V. All rights reserved.

Nanoblast synthesis and consolidation of (La0.8Sr0.2)(Ga0.9Mg0.1)O(3-delta) under Spark plasma sintering conditions.

PubMed

Vasylkiv, Oleg; Borodianska, Hanna; Badica, Petre; Zhen, Yongda; Tok, Alfred

2009-01-01

Four-cation nanograined strontium and magnesium doped lanthanum gallate (La0.8Sr0.2) (Ga0.9Mg0.1)O(3-delta) (LSGM) and its composite with 2 wt% of ceria (LSGM-Ce) were prepared. Morphologically homogeneous nanoreactors, i.e., complex intermediate metastable aggregates of desired composition were assembled by spray atomization technique, and subsequently loaded with nanoparticles of highly energetic C3H6N6O6. Rapid nanoblast calcination technique was applied and the final composition was synthesized within the preliminary localized volumes of each single nanoreactor on the first step of spark plasma treatment. Subsequent SPS consolidations of nanostructured extremely active LSGM and LSGM-Ce powders were achieved by rapid treatment under pressures of 90-110 MPa. This technique provided the heredity of the final structure of nanosize multimetal oxide, allowed the prevention of the uncontrolled agglomeration during multicomponent aggregates assembling, subsequent nanoblast calcination, and final ultra-rapid low-temperature SPS consolidation of nanostructured ceramics. LaSrGaMgCeO(3-delta) nanocrystalline powder consisting of approximately 11 nm crystallites was consolidated to LSGM-Ce nanoceramic with average grain size of approximately 14 nm by low-temperature SPS at 1250 degrees C. Our preliminary results indicate that nanostructured samples of (La0.8Sr0.2)(Ga0.9Mg0.1)O(3-delta) with 2 wt% of ceria composed of approximataley 14 nm grains can exhibit giant magnetoresistive effect in contrast to the usual paramagnetic properties measured on the samples with larger grain size.

Synthesis and modification of nano-sized TiO{sub 2} for photo-degradation process under visible light irradiation; a Placket–Burman experimental design

DOE Office of Scientific and Technical Information (OSTI.GOV)

Izadyar, Soheila; Fatemi, Shohreh, E-mail: shfatemi@ut.ac.ir; Mousavand, Tahereh

2013-09-01

Graphical abstract: - Highlights: • Nanosized TiO{sub 2} doped with nitrogen and iron was produced by sol-gel method. • Linear models were derived to relate the phase and particle size to synthesis factors. • High photocatalytic activity was observed for acetaldehyde degradation. - Abstract: In this research, nitrogen and iron (III) co-doped nano TiO{sub 2} (N-Fe-TiO{sub 2}) was prepared by sol-gel method using ammonium chloride and iron chloride solutions as nitrogen and iron sources, respectively. The effect of synthesis parameters (weight ratios of N/TiO{sub 2} and Fe/TiO{sub 2}, synthesis temperature, calcination time and temperature) was simultaneously investigated on the qualitymore » of the N-Fe-TiO{sub 2} product by a two-level Placket–Burman experimental design. The synthesized powders were characterized by XRD, XPS and UV–Vis spectroscopy techniques. The mean crystal size and anatase content were determined and evaluated as the linear functions of so-called synthesis parameters by the statistical analysis and regression. The 2%N-1%Fe-TiO{sub 2} product by 11 nm mean crystal size and 78% anatase content, synthesized at 35 °C and calcined at 500 °C during 2 h, exhibited the most significant activity during the photo-degradation of acetaldehyde under visible light irradiation and its efficiency was obtained about four times more than photocatalytic activity of Degussa TiO{sub 2}-P25.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, Dan; Yang, Ping, E-mail: mse_yangp@ujn.edu.cn; Huang, Baibiao

Graphical abstract: The iron alkoxide precursors are calcined into α-Fe{sub 2}O{sub 3}, Fe{sub 3}O{sub 4} microstructures with different morphologies by changing calcination atmosphere, reaction time of precursors and calcination temperature simply. The Fe{sub 2}O{sub 3}/Ag hybrid composites prepared through aqueous synthesis and light irradiation. - Highlights: • α-Fe{sub 2}O{sub 3} and Fe{sub 3}O{sub 4} microstructures with different morphologies were created. • Solvents play an important role for the solvothermal treatment of precursors. • The α-Fe{sub 2}O{sub 3} microstructures show excellent adsorption properties. • Fe{sub 2}O{sub 3}/Ag hybrid composites were prepared to improve their properties. - Abstract: The flower-like precursors ofmore » Fe alkoxide constructed by the self-assembly of nanoflakes were prepared. Time-dependent experiments confirmed the formation mechanism of flower-like precursors. After calcination, α-Fe{sub 2}O{sub 3} and Fe{sub 3}O{sub 4} nanostructures with different morphologies were created. Fe{sub 3}O{sub 4} nanostructures containing blocks with a truncated octahedron structure were obtained under N{sub 2} protection. α-Fe{sub 2}O{sub 3} nanostructures were prepared in an air atmosphere. The values of maximum adsorption capacity of α-Fe{sub 2}O{sub 3} nanostructures for Cr{sup 6+} ions were much higher than that of commercial bulk α-Fe{sub 2}O{sub 3}. Ag NPs were deposited on α-Fe{sub 2}O{sub 3} nanostructures through an aqueous synthesis and light irradiation using L-cysteine as a linker. Such procedure is utilizable for the preparation of the composites of noble metals and magnetic materials.« less

Gold nanoparticles-decorated electrospun poly(N-vinyl-2-pyrrolidone) nanofibers with tunable size and coverage density for nanomolar detection of single and binary component dyes by surface-enhanced raman spectroscopy

NASA Astrophysics Data System (ADS)

Kurniawan, Alfin; Wang, Meng-Jiy

2017-09-01

The application of the electrospun nanomaterials to surface-enhanced Raman spectroscopy (SERS) is a rapidly evolving field which holds potential for future developments in the generation of portable plasmonic-based detection platforms. In this study, a simple approach to fabricate electrospun poly(N-vinylpyrrolidone) (PVP) mats decorated with gold nanoparticles (AuNPs) by combining electrospinning and calcination was presented. AuNPs were decorated on the fiber mat surface through electrostatic interactions between positively charged aminosilane groups and negatively charged AuNPs. The size and coverage density of AuNPs on the fiber mats could be tuned by varying the calcination temperature. Calcination of AuNPs-decorated PVP fibers at 500 °C-700 °C resulted in the uniform decoration of high density AuNPs with very narrow gaps on every single fiber, which in turn contribute to strong electromagnetic SERS enhancement. The robust free-standing AuNPs-decorated mat which calcined at 500 °C (500/AuNPs-F) exhibited high SERS activity toward cationic (methylene blue, MB) and anionic (methyl orange, MO) dyes in single and binary systems with a detection range from tens of nM to a few hundred μM. The fabricated SERS substrate demonstrated high reproducibility with the spot-to-spot variation in SERS signal intensities was ±10% and ±12% for single and binary dye systems, respectively. The determination of MB and MO in spiked river water and tap water with 500/AuNPs-F substrate gave satisfactory results in terms of the percent spike recoveries (ranging from 92.6%-96.6%) and reproducibility (%RSD values less than 15 for all samples).

Use of Raman spectroscopy to assess the efficiency of MgAl mixed oxides in removing cyanide from aqueous solutions

NASA Astrophysics Data System (ADS)

Cosano, Daniel; Esquinas, Carlos; Jiménez-Sanchidrián, César; Ruiz, José Rafael

2016-02-01

Calcining magnesium/aluminium layered double hydroxides (Mg/Al LDHs) at 450 °C provides excellent sorbents for removing cyanide from aqueous solutions. The process is based on the "memory effect" of LDHs; thus, rehydrating a calcined LDH in an aqueous solution restores its initial structure. The process, which conforms to a first-order kinetics, was examined by Raman spectroscopy. The metal ratio of the LDH was found to have a crucial influence on the adsorption capacity of the resulting mixed oxide. In this work, Raman spectroscopy was for the first time use to monitor the adsorption process. Based on the results, this technique is an effective, expeditious choice for the intended purpose and affords in situ monitoring of the adsorption process. The target solids were characterized by using various instrumental techniques including X-ray diffraction spectroscopy, which confirmed the layered structure of the LDHs and the periclase-like structure of the mixed oxides obtained by calcination.

Preparation and Characteristics of Porous Ceramics by a foaming Technology at Low Temperature

NASA Astrophysics Data System (ADS)

Zhang, H. Q.; Wang, S. P.; Wen, J.; Wu, N.; Xu, S. H.

2017-12-01

Recycling and converting coal gangue and red mud into porous ceramics with good performance is a feasible disposal route. In this present work, porous foam ceramics was prepared using coal gangue and red mud as main raw materials at low sintering temperature, The amount of coal gangue and red mud were up to 70 wt%. To regulate the forming and sintering performance of the product, quartz sands and clay material were added to the formula. The green body was formed by a foaming technology using aluminum powders as foaming agents at room temperature. After foamed, the specimens were dried at 60-80 °C, and then calcined at 1060°C. Effects of concentration of NaOH and amount of aluminum powders on the phase, mechanical properties and microstructure were investigated here. Such study is expected to provide a new utilization route of the coal gangue and red mud, and brings both intensive environmental and economic benefits.

Conventional and two step sintering of PZT-PCN ceramics

NASA Astrophysics Data System (ADS)

Keshavarzi, Mostafa; Rahmani, Hooman; Nemati, Ali; Hashemi, Mahdieh

2018-02-01

In this study, PZT-PCN ceramic was made via sol-gel seeding method and effects of conventional sintering (CS) as well as two-step sintering (TSS) were investigated on microstructure, phase formation, density, dielectric and piezoelectric properties. First, high quality powder was achieved by seeding method in which the mixture of Co3O4 and Nb2O5 powder was added to the prepared PZT sol to form PZT-PCN gel. After drying and calcination, pyrochlore free PZT-PCN powder was synthesized. Second, CS and TSS were applied to achieve dense ceramic. The optimum temperature used for 2 h of conventional sintering was obtained at 1150 °C; finally, undesired ZrO2 phase formed in CS procedure was removed successfully with TSS procedure and dielectric and piezoelectric properties were improved compared to the CS procedure. The best electrical properties obtained for the sample sintered by TSS in the initial temperature of T 1 = 1200 °C and secondary temperature of T 2 = 1000 °C for 12 h.

Preparation and characterization of CuO catalyst for the thermolysis treatment of distillery wastewater.

PubMed

Sharma, Deepak; Prajapati, Abhinesh Kumar; Choudhary, Rumi; Kaushal, Rajesh Kumar; Pal, Dharm; Sawarkar, Ashish N

2017-08-16

CuO catalyst was prepared from copper sulfate by alkali precipitation method followed by drying and calcination. Characterization of CuO catalyst using X-ray diffraction, Brunauer-Emmett-Teller, and Barrett-Joyner-Halenda surface area analysis envisaged the effectiveness of CuO as a catalyst for the treatment of biodigester effluent (BDE) emanated from distilleries. The catalytic thermolysis is an efficient advance treatment method for distillery biodigester effluent (BDE). CT treatment of BDE was carried out in a 0.5 dm 3 thermolytic batch reactor using CuO as a catalyst at different pH (1-9), temperatures (80-110°C), and catalyst loadings (1-4 kg/m 3 ). With CuO catalyst, a temperature of 110°C, catalyst loading of 4 kg/m 3 , and pH of 2 was found to be optimal, providing a maximum reduction in chemical oxygen demand of 65%. The settling characteristics at different temperatures of CT-treated sludge were also presented.

Method for producing refractory nitrides

DOEpatents

Quinby, Thomas C.

1989-01-24

A process for making fine, uniform metal nitride powders that can be hot pressed or sintered. A metal salt is placed in a solvent with Melamine and warmed until a metal-Melamine compound forms. The solution is cooled and the metal-Melamine precipitate is calcined at a temperature below 700.degree. C. to form the metal nitrides and to avoid formation of the metal oxide.

Synthesis of methyl esters from relevant palm products in near-critical methanol with modified-zirconia catalysts.

PubMed

Laosiripojana, N; Kiatkittipong, W; Sutthisripok, W; Assabumrungrat, S

2010-11-01

The transesterification and esterification of palm products i.e. crude palm oil (CPO), refined palm oil (RPO) and palm fatty acid distillate (PFAD) under near-critical methanol in the presence of synthesized SO(4)-ZrO(2), WO(3)-ZrO(2) and TiO(2)-ZrO(2) (with various sulfur- and tungsten loadings, Ti/Zr ratios, and calcination temperatures) were studied. Among them, the reaction of RPO with 20%WO(3)-ZrO(2) (calcined at 800 degrees C) enhanced the highest fatty acid methyl ester (FAME) yield with greatest stability after several reaction cycles; furthermore, it required shorter time, lower temperature and less amount of methanol compared to the reactions without catalyst. These benefits were related to the high acid-site density and tetragonal phase formation of synthesized WO(3)-ZrO(2). For further improvement, the addition of toluene as co-solvent considerably reduced the requirement of methanol to maximize FAME yield, while the addition of molecular sieve along with catalyst significantly increased FAME yield from PFAD and CPO due to the inhibition of hydrolysis reaction. Copyright 2010 Elsevier Ltd. All rights reserved.

A laboratory scale study on arsenic(V) removal from aqueous medium using calcined bauxite ore.

PubMed

Mohapatra, Debasish; Mishra, Debaraj; Park, Kyung Ho

2008-01-01

The present work deals with the As(V) removal from an aqueous medium by calcined refractory grade bauxite (CRB) as a function of solution pH, time, As(V) concentration and temperature. The residual As(V) was lowered from 2 mg/L to below 0.01 mg/L in the optimum pH range 4.0-7.0 using a 5 g/L CRB within 3 h contact time. The adsorption data fits well with Langmuir isotherm and yielded Langmuir monolayer capacity of 1.78 mg As(V)/g of CRB at pH 7.0. Presence of anions such as silicate and phosphate decreased As(V) adsorption efficiency. An increase temperature resulted a decrease in the amount of As(V) adsorbed by 6%. The continuous fixed bed column study showed that at the adsorbent bed depth of 30 cm and residence time of 168 min, the CRB was capable of treating 340 bed volumes of As(V) spiked water (C0 = 2 mg/L) before breakthrough (Ce = 0.01 mg/L). This solid adsorbent, although not reusable, can be considered for design of adsorption columns as an efficiency arsenic adsorption media.

Optimization of sol-gel technique for coating of metallic substrates by hydroxyapatite using the Taguchi method

NASA Astrophysics Data System (ADS)

Pourbaghi-Masouleh, M.; Asgharzadeh, H.

2013-08-01

In this study, the Taguchi method of design of experiment (DOE) was used to optimize the hydroxyapatite (HA) coatings on various metallic substrates deposited by sol-gel dip-coating technique. The experimental design consisted of five factors including substrate material (A), surface preparation of substrate (B), dipping/withdrawal speed (C), number of layers (D), and calcination temperature (E) with three levels of each factor. An orthogonal array of L18 type with mixed levels of the control factors was utilized. The image processing of the micrographs of the coatings was conducted to determine the percentage of coated area ( PCA). Chemical and phase composition of HA coatings were studied by XRD, FT-IR, SEM, and EDS techniques. The analysis of variance (ANOVA) indicated that the PCA of HA coatings was significantly affected by the calcination temperature. The optimum conditions from signal-to-noise ( S/N) ratio analysis were A: pure Ti, B: polishing and etching for 24 h, C: 50 cm min-1, D: 1, and E: 300 °C. In the confirmation experiment using the optimum conditions, the HA coating with high PCA of 98.5 % was obtained.

Water-based sol-gel synthesis of hydroxyapatite: process development.

PubMed

Liu, D M; Troczynski, T; Tseng, W J

2001-07-01

Hydroxyapatite (HA) ceramics were synthesized using a sol-gel route with triethyl phosphite and calcium nitrate as phosphorus and calcium precursors, respectively. Two solvents, water and anhydrous ethanol, were used as diluting media for HA sol preparation. The sols were stable and no gelling occurred in ambient environment for over 5 days. The sols became a white gel only after removal of the solvents at 60 degrees C. X-ray diffraction showed that apatitic structure first appeared at a temperature as low as 350 degrees C. The crystal size and the HA content in both gels increase with increasing calcination temperature. The type of initial diluting media (i.e., water vs. anhydrous ethanol) did not affect the microstructural evolution and crystallinity of the resulting HA ceramic. The ethanol-based sol dip-coated onto a Ti substrate, followed by calcination at 450 degrees C, was found to be porous with pore size ranging from 0.3 to 1 microm. This morphology is beneficial to the circulation of physiological fluid when the coating is used for biomedical applications. The satisfactory adhesion between the coating and substrate suggests its suitability for load-bearing uses.

46 CFR 148.295 - Petroleum coke, calcined or uncalcined, at 55 °C (131 °F) or above.

Code of Federal Regulations, 2013 CFR

2013-10-01

... 46 Shipping 5 2013-10-01 2013-10-01 false Petroleum coke, calcined or uncalcined, at 55 °C (131 Â... Requirements for Certain Materials § 148.295 Petroleum coke, calcined or uncalcined, at 55 °C (131 °F) or above. (a) This part does not apply to shipments of petroleum coke, calcined or uncalcined, on any vessel...

46 CFR 148.295 - Petroleum coke, calcined or uncalcined, at 55 °C (131 °F) or above.

Code of Federal Regulations, 2012 CFR

2012-10-01

... 46 Shipping 5 2012-10-01 2012-10-01 false Petroleum coke, calcined or uncalcined, at 55 °C (131 Â... Requirements for Certain Materials § 148.295 Petroleum coke, calcined or uncalcined, at 55 °C (131 °F) or above. (a) This part does not apply to shipments of petroleum coke, calcined or uncalcined, on any vessel...

46 CFR 148.295 - Petroleum coke, calcined or uncalcined, at 55 °C (131 °F) or above.

Code of Federal Regulations, 2014 CFR

2014-10-01

... 46 Shipping 5 2014-10-01 2014-10-01 false Petroleum coke, calcined or uncalcined, at 55 °C (131 Â... Requirements for Certain Materials § 148.295 Petroleum coke, calcined or uncalcined, at 55 °C (131 °F) or above. (a) This part does not apply to shipments of petroleum coke, calcined or uncalcined, on any vessel...

46 CFR 148.295 - Petroleum coke, calcined or uncalcined, at 55 °C (131 °F) or above.

Code of Federal Regulations, 2011 CFR

2011-10-01

... 46 Shipping 5 2011-10-01 2011-10-01 false Petroleum coke, calcined or uncalcined, at 55 °C (131 Â... Requirements for Certain Materials § 148.295 Petroleum coke, calcined or uncalcined, at 55 °C (131 °F) or above. (a) This part does not apply to shipments of petroleum coke, calcined or uncalcined, on any vessel...

1. CONTEXTUAL VIEW OF WASTE CALCINING FACILITY. CAMERA FACING NORTHEAST. ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

1. CONTEXTUAL VIEW OF WASTE CALCINING FACILITY. CAMERA FACING NORTHEAST. ON RIGHT OF VIEW IS PART OF EARTH/GRAVEL SHIELDING FOR BIN SET. AERIAL STRUCTURE MOUNTED ON POLES IS PNEUMATIC TRANSFER SYSTEM FOR DELIVERY OF SAMPLES BEING SENT FROM NEW WASTE CALCINING FACILITY TO THE CPP REMOTE ANALYTICAL LABORATORY. INEEL PROOF NUMBER HD-17-1. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

Fabrication of photonic band gap materials

DOEpatents

Constant, Kristen; Subramania, Ganapathi S.; Biswas, Rana; Ho, Kai-Ming

2002-01-15

A method for forming a periodic dielectric structure exhibiting photonic band gap effects includes forming a slurry of a nano-crystalline ceramic dielectric or semiconductor material and monodisperse polymer microspheres, depositing a film of the slurry on a substrate, drying the film, and calcining the film to remove the polymer microspheres therefrom. The film may be cold-pressed after drying and prior to calcining. The ceramic dielectric or semiconductor material may be titania, and the polymer microspheres may be polystyrene microspheres.

Synthesis of nano-sized lithium cobalt oxide via a sol-gel method

NASA Astrophysics Data System (ADS)

Li, Guangfen; Zhang, Jing

2012-07-01

In this study, nano-structured LiCoO2 thin film were synthesized by coupling a sol-gel process with a spin-coating method using polyacrylic acid (PAA) as chelating agent. The optimized conditions for obtaining a better gel formulation and subsequent homogenous dense film were investigated by varying the calcination temperature, the molar mass of PAA, and the precursor's molar ratios of PAA, lithium, and cobalt ions. The gel films on the silicon substrate surfaces were deposited by multi-step spin-coating process for either increasing the density of the gel film or adjusting the quantity of PAA in the film. The gel film was calcined by an optimized two-step heating procedure in order to obtain regular nano-structured LiCoO2 materials. Both atomic force microscopy (AFM) and scanning electron microscopy (SEM) were utilized to analyze the crystalline and the morphology of the films, respectively.

Optimization of mechanical strength of titania fibers fabricated by direct drawing

NASA Astrophysics Data System (ADS)

Hanschmidt, Kelli; Tätte, Tanel; Hussainova, Irina; Part, Marko; Mändar, Hugo; Roosalu, Kaspar; Chasiotis, Ioannis

2013-11-01

Nanostructured polycrystalline titania (TiO2) microfibers were produced by direct drawing from visco-elastic alkoxide precursors. The fiber crystallinity and grain size were shown to depend on post-treatment calcination temperature. Tensile tests with individual fibers showed strong sensitivity of the elastic modulus and the tensile strength to microstructural details of the fibers. The elastic modulus of as-fabricated fibers increased about 10 times after calcination at 700 ∘C, while the strain at failure remained almost the same at ˜1.4 %. The highest tensile strength of more than 800 MPa was exhibited by nanoscale grained fibers with a bimodal grain size distribution consisting of rutile grains embedded into an anatase matrix. This structure is believed to have reduced the critical defect size, and thus increased the tensile strength. The resultant fibers showed properties that were appropriate for reinforcement of different matrixes.

Dynamic Diffraction Studies on the Crystallization, Phase Transformation, and Activation Energies in Anodized Titania Nanotubes.

PubMed

Albetran, Hani; Vega, Victor; Prida, Victor M; Low, It-Meng

2018-02-23

The influence of calcination time on the phase transformation and crystallization kinetics of anodized titania nanotube arrays was studied using in-situ isothermal and non-isothermal synchrotron radiation diffraction from room temperature to 900 °C. Anatase first crystallized at 400 °C, while rutile crystallized at 550 °C. Isothermal heating of the anodized titania nanotubes by an increase in the calcination time at 400, 450, 500, 550, 600, and 650 °C resulted in a slight reduction in anatase abundance, but an increase in the abundance of rutile because of an anatase-to-rutile transformation. The Avrami equation was used to model the titania crystallization mechanism and the Arrhenius equation was used to estimate the activation energies of the titania phase transformation. Activation energies of 22 (10) kJ/mol for the titanium-to-anatase transformation, and 207 (17) kJ/mol for the anatase-to-rutile transformation were estimated.

Room temperature ferromagnetism in Fe-doped CeO2 nanoparticles.

PubMed

Maensiri, Santi; Phokha, Sumalin; Laokul, Paveena; Seraphin, Supapan

2009-11-01

RT ferromagnetism was observed in nanoparticles of Fe-doped CeO2 (i.e., Ce(0.97)Fe(0.03)O2) synthesized by a sol-gel method. The undoped and Fe-doped CeO2 were characterized by XRD, Raman spectroscopy, TEM, and VSM. The undoped samples and Ce(0.97)Fe(0.03)O2 precursor exhibit a diamagnetic behavior. The 673 K-calcined Ce(0.97)Fe(0.03)O2 sample is paramagnetic whereas 773 and 873 K-calcined Ce(0.97)Fe(0.03)O2 samples are ferromagnetism having the magnetizations of 4.65 x 10(-3) emu/g and 6.20 x 10(-3) emu/g at 10 kOe, respectively. Our results indicate that the ferromagnetic property is intrinsic to the Fe-doped CeO2 system and is not a result of any secondary magnetic phase or cluster formation.

STUDY ON SYNTHESIS AND EVOLUTION OF NANOCRYSTALLINE Mg4Ta2O9 BY AQUEOUS SOL-GEL PROCESS

NASA Astrophysics Data System (ADS)

Wu, H. T.; Yang, C. H.; Wu, W. B.; Yue, Y. L.

2012-06-01

Nanosized and highly reactive Mg4Ta2O9 were successfully synthesized by aqueous sol-gel method compared with conventional solid-state method. Ta-Mg-citric acid solution was first formed and then evaporated resulting in a dry gel for calcination in the temperature ranging from 600°C to 800°C for crystallization in oxygen atmosphere. The crystallization process from the gel to crystalline Mg4Ta2O9 was identified by thermal analysis and phase evolution of powders was studied using X-ray diffraction (XRD) technique during calcinations. Particle size and morphology were examined by transmission electron microscopy (TEM) and high resolution scanning electron microscopy (HR-SEM). The results revealed that sol-gel process showed great advantages over conventional solid-state method and Mg4Ta2O9 nanopowders with the size of 20-30 nm were obtained at 800°C.

21. CONSTRUCTION PROGRESS VIEW OF CALCINER VESSEL ON LOW BOY ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

21. CONSTRUCTION PROGRESS VIEW OF CALCINER VESSEL ON LOW BOY EN ROUTE TO FACILITY. INEEL PHOTO NUMBER NRTS-60-2487. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

22. CONSTRUCTION PROGRESS PHOTO SHOWING WORKERS LOWERING CALCINER VESSEL INTO ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

22. CONSTRUCTION PROGRESS PHOTO SHOWING WORKERS LOWERING CALCINER VESSEL INTO CELL THROUGH THE HATCH. INEEL PHOTO NUMBER NRTS-60-2485. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

Novel Montmorillonite/TiO₂/MnAl-Mixed Oxide Composites Prepared from Inverse Microemulsions as Combustion Catalysts.

PubMed

Napruszewska, Bogna D; Michalik-Zym, Alicja; Rogowska, Melania; Bielańska, Elżbieta; Rojek, Wojciech; Gaweł, Adam; Wójcik-Bania, Monika; Bahranowski, Krzysztof; Serwicka, Ewa M

2017-11-19

A novel design of combustion catalysts is proposed, in which clay/TiO₂/MnAl-mixed oxide composites are formed by intermixing exfoliated organo-montmorillonite with oxide precursors (hydrotalcite-like in the case of Mn-Al oxide) obtained by an inverse microemulsion method. In order to assess the catalysts' thermal stability, two calcination temperatures were employed: 450 and 600 °C. The composites were characterized with XRF (X-ray fluorescence), XRD (X-ray diffraction), HR SEM (high resolution scanning electron microscopy, N₂ adsorption/desorption at -196 °C, and H₂ TPR (temperature programmed reduction). Profound differences in structural, textural and redox properties of the materials were observed, depending on the presence of the TiO₂ component, the type of neutralization agent used in the titania nanoparticles preparation (NaOH or NH₃ (aq)), and the temperature of calcination. Catalytic tests of toluene combustion revealed that the clay/TiO₂/MnAl-mixed oxide composites prepared with the use of ammonia showed excellent activity, the composites obtained from MnAl hydrotalcite nanoparticles trapped between the organoclay layers were less active, but displayed spectacular thermal stability, while the clay/TiO₂/MnAl-mixed oxide materials obtained with the aid of NaOH were least active. The observed patterns of catalytic activity bear a direct relation to the materials' composition and their structural, textural, and redox properties.

Griffiths-like phase in high TC perovskite La2FeReO6 prepared in a controlled reducing atmosphere

NASA Astrophysics Data System (ADS)

Kaipamagalath, Aswathi; Palakkal, Jasnamol P.; Varma, Manoj R.

2018-05-01

The perovskite La2FeReO6 is prepared by solid-state reaction method. Calcination was done in a controlled reducing atmosphere. The structure of the compound is found to be orthorhombic with Pbnm space group. From the DC magnetic studies, the transition temperature (TC) of La2FeReO6 is found to be at 729 K. A Griffiths-like phase is present in the material with ferromagnetic short-range correlations above TC up to the Griffiths temperature TG = 863 K.

25. CONSTRUCTION PROGRESS AERIAL VIEW OF WASTE CALCINING FACILITY TAKEN ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

25. CONSTRUCTION PROGRESS AERIAL VIEW OF WASTE CALCINING FACILITY TAKEN WHEN STRUCTURE WAS 99 PERCENT COMPLETE. INEEL PHOTO NUMBER NRTS-60-5409. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

Diatomite releases silica during spirit filtration.

PubMed

Gómez, J; Gil, M L A; de la Rosa-Fox, N; Alguacil, M

2014-09-15

The purpose of this study was to ascertain whether diatomite is an inert filter aid during spirit filtration. Surely, any compound with a negative effect on the spirit composition or the consumer's health could be dissolved. In this study different diatomites were treated with 36% vol. ethanol/water mixtures and the amounts and structures of the extracted compounds were determined. Furthermore, Brandy de Jerez was diatomite- and membrane-filtered at different temperatures and the silicon content was analysed. It was found that up to 0.36% by weight of diatomite dissolved in the aqueous ethanol and amorphous silica, in the form of hollow spherical microparticles, was the most abundant component. Silicon concentrations in Brandy de Jerez increased by up to 163.0% after contact with diatomite and these changes were more marked for calcined diatomite. In contrast, reductions of more than 30% in silicon concentrations were achieved after membrane filtration at low temperatures. Copyright © 2014 Elsevier Ltd. All rights reserved.

Fe2O3 hollow sphere nanocomposites for supercapacitor applications

NASA Astrophysics Data System (ADS)

Zhao, Yu; Wen, Yang; Xu, Bing; Lu, Lu; Ren, Reiming

2018-02-01

Nanomaterials have attracted increasing interest in electrochemical energy storage and conversion. Hollow sphere Fe2O3 nanocomposites were successfully prepared through facile low temperature water-bath method with carbon sphere as hard template. The morphology and microstructure of samples were characterized by X-ray diffraction (XRD) and Scanning electron microscope (SEM), respectively. Through hydrolysis mechanism, using ferric chloride direct hydrolysis, iron hydroxide coated on the surface of carbon sphere, after high temperature calcination can form the hollow spherical iron oxide materials. Electrochemical performances of the hollow sphere Fe2O3 nanocomposites electrodes were investigated by cyclic voltammery (CV) and galvanostatic charge/discharge. The Pure hollow sphere Fe2O3 nanocomposites achieves a specific capacitance of 125 F g-1 at the current density of 85 mA g-1. The results indicate that the uniform dispersion of hollow ball structure can effectively reduce the particle reunion in the process of charging and discharging.

Synthesis and optical properties of Tb-doped pentazinc dimolybdate pentahydrate

NASA Astrophysics Data System (ADS)

Zhai, Bao-gai; Ma, Qing-lan; Yang, Long; Huang, Yuan Ming

Tb3+ doped pentazinc bimolybdate pentahydrate (Zn5Mo2O11·5H2O) was synthesized via the precipitation method. Thermal gravimetric analysis and differential scanning calorimetric analysis indicate that Zn5Mo2O11·5H2O is decomposed into ZnMoO4 at the phase transition temperature 267 °C. The photoluminescence characterization shows that the characteristic emissions of Tb3+ at 488, 544, 586 and 613 nm are superimposed over a broad emission band of Zn5Mo2O11·5H2O. The characteristic emissions of Tb3+ ions get weakened in intensity as the calcination temperature increases from 150 to 267 °C. Our results have demonstrated that Tb3+ can be used as an effective and direct probe in the spectroscopic studies on the phase transition of Zn5Mo2O11·5H2O.

Evaluation of Type I cement sorbent slurries in the U.C. pilot spray dryer facility. Final report, November 1, 1994--February 28, 1996

DOE Office of Scientific and Technical Information (OSTI.GOV)

Keener, T.C.; Khang, S.J.

1996-07-31

This research was focused on evaluating hydrated cement sorbents in the U. C. pilot spray dryer. The main goal of this work was to determine the hydration conditions resulting in reactive hydrated cement sorbents. Hydration of cement was achieved by stirring or by grinding in a ball mill at either room temperature or elevated temperatures. Also, the effects of several additives were studied. Additives investigated include calcium chloride, natural diatomite, calcined diatomaceous earth, and fumed silica. The performance of these sorbents was compared with conventional slaked lime. Further, the specific surface area and pore volume of the dried SDA sorbentsmore » were measured and compared to reactivity. Bench-scale tests were performed to obtain a more detailed picture of the development of the aforementioned physical properties as a function of hydration time.« less

Immobilization of lead in a Korean military shooting range soil using eggshell waste: an integrated mechanistic approach.

PubMed

Ahmad, Mahtab; Hashimoto, Yohey; Moon, Deok Hyun; Lee, Sang Soo; Ok, Yong Sik

2012-03-30

This study evaluated the effectiveness of eggshell and calcined eggshell on lead (Pb) immobilization in a shooting range soil. Destructive and non-destructive analytical techniques were employed to determine the mechanism of Pb immobilization. The 5% additions of eggshell and calcined eggshell significantly decreased the TCLP-Pb concentration by 68.8% due mainly to increasing soil pH. Eggshell and calcined-eggshell amendments decreased the exchangeable Pb fraction to ≈ 1% of the total Pb in the soil, while the carbonate-associated Pb fraction was increased to 40.0-47.1% at >15% application rates. The thermodynamic modeling on Pb speciation in the soil solution predicted the precipitation of Pb-hydroxide [Pb(OH)(2)] in soils amended with eggshell and calcined eggshell. The SEM-EDS, XAFS and elemental dot mapping revealed that Pb in soil amended with calcined eggshell was associated with Si and Ca, and may be immobilized by entrapping into calcium-silicate-hydrate. Comparatively, in the soil amended with eggshell, Pb was immobilized via formation of Pb-hydroxide or lanarkite [Pb(2)O(SO(4))]. Applications of amendments increased activities of alkaline phosphatase up to 3.7 times greater than in the control soil. The use of eggshell amendments may have potential as an integrated remediation strategy that enables Pb immobilization and soil biological restoration in shooting range soils. Copyright © 2012 Elsevier B.V. All rights reserved.

Novel erbia-yttria co-doped zirconia fluorescent thermal history sensor

NASA Astrophysics Data System (ADS)

Copin, E. B.; Massol, X.; Amiel, S.; Sentenac, T.; Le Maoult, Y.; Lours, P.

2017-01-01

Thermochromic pigments are commonly used for off-line temperature mapping on components from systems operating at a temperature higher than 1073 K. However, their temperature resolution is often limited by the discrete number of color transitions they offer. This paper investigates the potential of erbia-yttria co-doped zirconia as a florescent thermal history sensor alternative to thermochromic pigments. Samples of yttria-stabilized zirconia powder (YSZ, 8.3 mol% YO1.5) doped with 1.5 mol% ErO1.5 and synthesized by a sol-gel route are calcined for 15 minutes under isothermal conditions between 1173 and 1423 K. The effects of temperature on their crystal structure and room temperature fluorescence properties are then studied. Results show a steady increase of the crystallinity of the powders with temperature, causing a significant and permanent increase of the emission intensity and fluorescence lifetime which could be used to determine temperature with a calculated theoretical resolution lower than 1 K for intensity. The intensity ratio obtained using a temperature insensitive YSZ:Eu3+ reference phosphor is proposed as a more robust parameter regarding experimental conditions for determining thermal history. Finally, the possibilities for integrating this fluorescent marker into sol-gel deposited coatings for future practical thermal history sensing applications is also discussed.

Enhancement of acid treated g-C3N4sbnd Cu2O photocatalytic activity by PEG under visible light irradiation

NASA Astrophysics Data System (ADS)

Zuo, Shiyu; Xu, Haiming; Liao, Wei; Sun, Lei; Li, Qiang; Zan, Jie; Zhang, Binyang; Li, Dongya; Xia, Dongsheng

2018-05-01

In this study, g-C3N4sbnd Cu2O was successfully synthesized in the presence of PEG-400 surfactant via an acid treatment hydrothermal method and a high-temperature calcination method. The structures and properties of as-synthesized samples were characterized using a range of techniques, such as XPS, TEM, PL and BET. The g-C3N4sbnd Cu2O heterojunction exhibits the enhanced photocatalytic performance and high stability. It is revealed that the addition of PEG can promote the heterojunction effect of g-C3N4sbnd Cu2O, effectively improving the crystallinity and specific surface area of the photocatalyst, separation efficiency of photocarriers, and light absorption, thus enhancing the photocatalytic performance.

Humate-assisted Synthesis of MoS2/C Nanocomposites via Co-Precipitation/Calcination Route for High Performance Lithium Ion Batteries

NASA Astrophysics Data System (ADS)

Geng, Qin; Tong, Xin; Wenya, Gideon Evans; Yang, Chao; Wang, Jide; Maloletnev, A. S.; Wang, Zhiming M.; Su, Xintai

2018-04-01

A facile, cost-effective, non-toxic, and surfactant-free route has been developed to synthesize MoS2/carbon (MoS2/C) nanocomposites. Potassium humate consists of a wide variety of oxygen-containing functional groups, which is considered as promising candidates for functionalization of graphene. Using potassium humate as carbon source, two-dimensional MoS2/C nanosheets with irregular shape were synthesized via a stabilized co-precipitation/calcination process. Electrochemical performance of the samples as an anode of lithium ion battery was measured, demonstrating that the MoS2/C nanocomposite calcinated at 700 °C (MoS2/C-700) electrode showed outstanding performance with a high discharge capacity of 554.9 mAh g- 1 at a current density of 100 mA g- 1 and the Coulomb efficiency of the sample maintained a high level of approximately 100% after the first 3 cycles. Simultaneously, the MoS2/C-700 electrode exhibited good cycling stability and rate performance. The success in synthesizing MoS2/C nanocomposites via co-precipitation/calcination route may pave a new way to realize promising anode materials for high-performance lithium ion batteries.

The effect of microwave and conventional heating on a modified sol-gel derived biphasic calcium phosphate

NASA Astrophysics Data System (ADS)

Herradi, S.; Bouhazma, S.; Khaldi, M.; El Hachadi, A.; El Bali, B.; Lachkar, M.

2018-03-01

A facile sol-gel method was used to synthesize either hydroxyapatite (HA) or beta-tricalcium phosphate (β-TCP) as the major phase. Herein, we report, on the one hand, the effect of a very low maturation temperature on the final powder composition after drying step, and on the other hand, we compare the effect of calcination of this powder by microwave or electric furnace. It was found that microwave heating has led to the formation of hydroxyapatite phase upon 180°C for 20 minutes, however, XRD patterns show that the powder becomes less crystallized upon 220°C and amorphous upon 230°C. In contrast, furnace heating at 600°C and 700°C converts the as-synthesized powder to β-TCP as the major phase together with HA as the minor phase. This work shows the possibility to obtain the as-prepared BCP at much lower maturation temperature; it also gives an insight into the role, of either microwave or conventional heating, in controlling the ratio between HA and β-TCP in the sintered powder.