Effect of fly ash calcination in geopolymer synthesis

NASA Astrophysics Data System (ADS)

Samadhi, Tjokorde Walmiki; Jatiningrum, Mirna; Arisiani, Gresia

2015-12-01

Geopolymer, a largely amorphous class of inorganic polymer consisting of aluminosilicate repeat units, is an environmentally attractive engineering material due to its ability to consume aluminosilicate waste as raw materials. This work studies the effect of the calcination temperature of a coal fly ash generated by a low-efficiency boiler on the mechanical strength of geopolymer mortar synthesized using a mixture of the fly ash, potassium hydroxide as the alkali activator, and locally available sand as the filler aggregate. The calcination temperature is varied between 500-700 °C, with a calcination period of 2 hours in an electric furnace. Two sand samples with different particle size distributions are used. The key response variable is the compressive strength at room temperature, measured after curing at 80 °C for 7 and 14 days. Uncalcined ash, with a carbon content of approximately 31.0%, is not amenable for geopolymer synthesis. Analysis of experimental data using the ANOVA method for general factorial design identifies significant main effects for all three experimental variables. Two-way interactions are significant, except that between sand type and curing period. Higher calcination temperature significantly improves the strength of the mortar. However, the strength of the obtained geopolymer mortars are still significantly lower than that of ordinary Portland cement mortar.

29. FLOOR PLAN OF WASTE CALCINATION FACILITY SHOWING MAIN ABOVEGRADE ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

29. FLOOR PLAN OF WASTE CALCINATION FACILITY SHOWING MAIN ABOVE-GRADE FLOOR LEVEL. INEEL DRAWING NUMBER 200-0633-00-287-106354. FLUOR NUMBER 5775-CPP-633-A-4. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

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.

3. CONTEXTUAL VIEW OF WASTE CALCINING FACILITY, CAMERA FACING NORTHEAST. ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

3. CONTEXTUAL VIEW OF WASTE CALCINING FACILITY, CAMERA FACING NORTHEAST. SHOWS RELATIONSHIP BETWEEN DECONTAMINATION ROOM, ADSORBER REMOVAL HATCHES (FLAT ON GRADE), AND BRIDGE CRANE. INEEL PROOF NUMBER HD-17-2. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

31. FLOOR PLANS OF WASTE CALCINATION FACILITY. SHOWS ACCESS CORRIDOR ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

31. FLOOR PLANS OF WASTE CALCINATION FACILITY. SHOWS ACCESS CORRIDOR AT MEZZANINE AND LOWER LEVELS. INEEL DRAWING NUMBER 200-0633-00-287-106352. FLUOR NUMBER 5775-CPP-633-A-2. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

30. FLOOR PLANS OF WASTE CALCINATION FACILITY. SHOWS LEVELS ABOVE ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

30. FLOOR PLANS OF WASTE CALCINATION FACILITY. SHOWS LEVELS ABOVE GRADE AND AT LEVEL OF OPERATING CORRIDOR. INEEL DRAWING NUMBER 200-0633-00-287-106351. FLUOR NUMBER 5775-CPP-633-A-1. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

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.

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.

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

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.

Removal of Dissolved Silica using Calcinated Hydrotalcite in Real-life Applications.

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

Sasan, Koroush; Brady, Patrick Vane.; Krumhansl, James L.

Water shortages are a growing global problem. Reclamation of industrial and municipal wastewater will be necessary in order to mitigate water scarcity. However, many operational challenges, such as silica scaling, prevent large scale water reuse. Previously, our team at Sandia has demonstrated the use of selective ion exchange materials, such as calcinated hydrotalcite (HTC, (Mg 6 Al 2 (OH) 16 (CO 3 )*4H 2 O)), for the low cost removal of silica from synthetic cooling tower water. However, it is not currently know if calcinated HTC has similar capabilities in realistic applications. The purpose of this study was to investigatemore » the ability of calcinated HTC to remove silica from real cooling tower water. This was investigated under both batch and continuous conditions, and in the presence of competing ions. It was determined that calcinated HTC behaved similarly in real and synthetic cooling tower water; the HTC is highly selective for the silica even in the presence of competing cations. Therefore, the data concludes that calcinated HTC is a viable anti-scaling pretreatment for the reuse of industrial wastewaters.« less

32. SECTIONS AA, BB, CC, DD, AND EE WASTE CALCINATION ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

32. SECTIONS A-A, B-B, C-C, D-D, AND E-E WASTE CALCINATION FACILITY SHOWING RELATIONSHIPS OF DIFFERENT FLOOR LEVELS TO ONE ANOTHER. INEEL DRAWING NUMBER 200-0633-00-287-106353. FLUOR NUMBER 5775-CPP-633-A-3. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

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.

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

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.

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.

The effect of calcination conditions on the graphitizability of novel synthetic and coal-derived cokes

NASA Astrophysics Data System (ADS)

Bennett, Barbara Ellen

The effects of calcination heating rate and ultimate calcination temperature upon calcined coke and subsequent graphitic material microstructures were studied for materials prepared from three different precursors. The pitch precursors used were Mitsubishi AR pitch (a synthetic, 100% mesophase pitch), the NMP-extracted portion of a raw coal, and the NMP-extracted fraction of a coal liquefaction residue obtained from an HTI pilot plant. These materials were all green-coked under identical conditions. Optical microscopy confirmed that the Mitsubishi coke was very anisotropic and the HTI coke was nearly as anisotropic. The coke produced from the direct coal extract was very isotropic. Crystalline development during calcination heating was verified by high-temperature x-ray diffraction. Experiments were performed to ascertain the effects of varying calcination heating rate and ultimate temperature. It was determined that calcined coke crystallite size increased with increasing temperature for all three materials but was found to be independent of heating rate. The graphene interplanar spacing decreased with increasing temperature for the isotropic NMP-extract material but increased with increasing temperature for the anisotropic materials---Mitsubishi and HTI cokes. Graphene interplanar spacing was also found to be independent of heating rate. Calcined coke real densities were, likewise, found to be independent of heating rate. The anisotropic cokes (Mitsubishi and HTI) exhibited increasing real density with increasing calcination temperature. The NMP-extract coke increased in density up to 1050°C and then suffered a dramatic reduction in real density when heated to 1250°C. This is indicative of puffing. Since there was no corresponding disruption in the crystalline structure, the puffing phenomena was determined to be intercrystalline rather than intracrystalline. After the calcined cokes were graphitized (under identical conditions), the microstructures were re

7. WASTE CALCINING FACILITY, LOOKING AT NORTH END OF BUILDING. ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

7. WASTE CALCINING FACILITY, LOOKING AT NORTH END OF BUILDING. CAMERA FACING SOUTH. TENT-ROOFED COVER IN RIGHT OF VIEW IS A TEMPORARY WEATHER-PROOFING SHELTER OVER THE BLOWER PIT IN CONNECTION WITH DEMOLITION PROCEDURES. SMALL BUILDING CPP-667 IN CENTER OF VIEW WAS USED FOR SUPPLEMENTARY OFFICE SPACE BY HEALTH PHYSICISTS AND OTHERS. INEEL PROOF SHEET NOT NUMBERED. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

Effect of calcination temperature on the photocatalytic reduction and oxidation processes of hydrothermally synthesized titania nanotubes.

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

Viayan, B.; Dimitrijevic, N. M.; Rajh, T.

Titania nanotubes having diameters 8 to 12 nm and lengths of 50-300 nm were prepared using a hydrothermal method. Further, the titania nanotubes were calcined over the temperature range 200-800 C in order to enhance their photocatalytic properties by altering their morphology. The calcined titania nanotubes were characterized by using X-ray diffraction and surface area analysis and their morphological features were studied by scanning and transmission electron microscopy. Nanotubes calcined at 400 C showed the maximum extent of photocatalyitc reduction of carbon dioxide to methane, whereas samples calcined at 600 C produced maximum photocatalytic oxidation of acetaldehyde. Electron paramagnetic resonancemore » (EPR) spectroscopy was used to interrogate the effects of nanotube structure on the charge separation and trapping as a function of calcination temperature. EPR results indicated that undercoordinated titania sites are associated with maximum CO{sub 2} reduction occurring in nanotubes calcined at 400 C. Despite the collapse of the nantube structure to form nanorods and the concomitant loss of surface area, the enhanced charge separation associated with increased crystallinity promoted high rates of oxidation of acetaldehyde in titania materials calcined at 600 C. These results illustrate that calcination temperature allows us to tune the morphological and surface features of the titania nanostructures for particular photocatalytic reactions.« less

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.

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.

40. CALCINER CELL SECTIONS. TOGETHER WITH HAER ID33C37 ILLUSTRATES COMPLEXITY ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

40. CALCINER CELL SECTIONS. TOGETHER WITH HAER ID-33-C-37 ILLUSTRATES COMPLEXITY OF PIPING. INEEL DRAWING NUMBER 200-0633-00-287-106446. FLUOR NUMBER 5775-CPP-P-51. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

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.

39. CALCINER CELL PLANS. TOGETHER WITH HAER ID33C37 ILLUSTRATES COMPLEXITY ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

39. CALCINER CELL PLANS. TOGETHER WITH HAER ID-33-C-37 ILLUSTRATES COMPLEXITY OF PIPING. INEEL DRAWING NUMBER 200-0633-00-287-106445. FLUOR NUMBER 5775-CPP-633-P-50 - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

Silica-associated limited systemic sclerosis after occupational exposure to calcined diatomaceous earth.

PubMed

Moisan, Stéphanie; Rucay, Pierre; Ghali, Alaa; Penneau-Fontbonne, Dominique; Lavigne, Christian

2010-10-01

Silica-associated systemic sclerosis can occur in persons using calcined diatomaceous earth for filtration purpose. A limited systemic sclerosis was diagnosed in a 52-year-old male winegrower who had a combination of Raynaud's phenomenon, oesophageal dysfunction, sclerodactyly and telangectasia. The anti-centromere antibodies titre was 1/5000. The patient was frequently exposed to high atmospheric concentrations of calcined diatomaceous earth when performing the filtration of wines. Calcined diatomaceous earth is almost pure crystalline silica under the cristobalite form. The diagnosis of silica-associated limited systemic sclerosis after exposure to calcined diatomaceous earth was made. The patient's disease met the medical, administrative and occupational criteria given in the occupational diseases list 22 bis of the agriculture Social Security scheme and thence was presumed to be occupational in origin, without need to be proved. The diagnosis of occupational disease had been recognized by the compensation system of the agricultural health insurance. Copyright © 2010 Société française de rhumatologie. Published by Elsevier SAS. All rights reserved.

Effect of calcination temperatures on microstructures and photocatalytic activity of tungsten trioxide hollow microspheres.

PubMed

Yu, Jiaguo; Qi, Lifang; Cheng, Bei; Zhao, Xiufeng

2008-12-30

Tungsten trioxide hollow microspheres were prepared by immersing SrWO4 microspheres in a concentrated HNO3 solution, and then calcined at different temperatures. The prepared tungsten oxide samples were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectra, differential thermal analysis-thermogravimetry, UV-visible spectrophotometry, scanning electron microscopy, N2 adsorption/desorption measurements. The photocatalytic activity of the samples was evaluated by photocatalytic decolorization of rhodamine B aqueous solution under visible-light irradiation. It was found that with increasing calcination temperatures, the average crystallite size and average pore size increased, on the contrary, Brunauer-Emmett-Teller-specific surface areas decreased. However, pore volume and porosity increased firstly, and then decreased. Increasing calcination temperatures resulted in the changes of surface morphology of hollow microspheres. The un-calcined and 300 degrees C-calcined samples showed higher photocatalytic activity than other samples. At 400 degrees C, the photocatalytic activity decreased greatly due to the decrease of specific surface areas. At 500 degrees C, the photocatalytic activity of the samples increased again due to the junction effect of two phases.

CALCINATION AND SINTERING OF SORBENTS DURING BOILER INJECTION FOR DRY SULFUR DIOXIDE CONTROL

EPA Science Inventory

The paper discusses the calcination and sintering of sorbents during boiler injection for dry sulfur dioxide (S02) control, with emphasis on calcium hydroxide--Ca(OH)2--because of its superior reactivity with S02 and its wide commercial availability. Calcination and sintering are...

Effect of calcination temperature on phase transformation and crystallite size of copper oxide (CuO) powders

NASA Astrophysics Data System (ADS)

Ratnawulan, Fauzi, Ahmad; AE, Sukma Hayati

2017-08-01

Copper oxide powder was prepared from Copper iron from South Solok, Indonesia. The samples was dried and calcined for an hour at temperatures of 145°C, 300°C,850°C, 1000°C. Phase transformation and crystallite size of the calcined powders have been investigated as a function of calcination temperature by room-temperature X-ray diffraction (XRD). It was seen that the tenorite, CuO was successfully obtained. With increasing calcining temperature, CuO transformed from malachite Cu2(CO3)(OH)2 to tenorite phase (CuO) and crystallite size of prepared samples increased from 36 nm to 76 nm.

The effect of precipitation and calcination parameters on oxalate derived ThO2 pellets

NASA Astrophysics Data System (ADS)

Wangle, Tadeas; Tyrpekl, Vaclav; Cagno, Simone; Delloye, Thierry; Larcher, Olivier; Cardinaels, Thomas; Vleugels, Jozef; Verwerft, Marc

2017-11-01

Thorium oxalate is easy to prepare, but the derived oxide powders retain the platelet morphology of the primary oxalate. This negatively impacts packing and sintering. If powder milling is to be avoided, powder synthesis needs to be optimized. That is the goal of this paper, where different precipitation strategies were used and their effect on powder characteristics and pellet synthesis was investigated. Oxalates prepared by adding a thorium nitrate solution to an oxalic acid solution proved most promising. Further optimizing of the calcination temperature revealed that with increasing calcination temperature the packing density improved significantly. This came at the cost of decreased early stage sintering and a higher frequency of end-capping during compaction. The calcination temperature at which the highest final density can be reached was dependent on the sintering cycle. Furthermore, the ThO2 powders had less surface area and thus adsorbed less gases during storage when calcined at higher temperatures.

Effect of calcination routes on phase formation of BaTiO3 and their electronic and magnetic properties

NASA Astrophysics Data System (ADS)

Majumder, Supriyo; Choudhary, R. J.; Tripathi, M.; Phase, D. M.

2018-05-01

We have investigated the phase formation and correlation between electronic and magnetic properties of oxygen deficient BaTiO3 ceramics, synthesized by solid state reaction method, following different calcination paths. The phase analysis divulge that a higher calcination temperature above 1000° C is favored for tetragonal phase formation than the cubic phase. The core level X-ray photo electron spectroscopy measurements confirm the presence of oxygen vacancies and oxygen vacancy mediated Ti3+ states. As the calcination temperature and calcination time increases these oxygen vacancies and hence Ti3+ concentrations reduce in the sample. The temperature dependent magnetization curves suggest unexpected magnetic ordering, which may be due to the presence of unpaired electron at the t2g state (d1) of nearest-neighbor Ti atoms. In magnetization vs magnetic field isotherms, the regular decrease of saturation moment value with increasing calcination temperature and calcination time, can be discussed considering the amount of oxygen deficiency induced Ti3+ concentrations, present in the sample.

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

SPRAY CALCINATION REACTOR

DOEpatents

Johnson, B.M.

1963-08-20

A spray calcination reactor for calcining reprocessin- g waste solutions is described. Coaxial within the outer shell of the reactor is a shorter inner shell having heated walls and with open regions above and below. When the solution is sprayed into the irner shell droplets are entrained by a current of gas that moves downwardly within the inner shell and upwardly between it and the outer shell, and while thus being circulated the droplets are calcined to solids, whlch drop to the bottom without being deposited on the walls. (AEC) H03 H0233412 The average molecular weights of four diallyl phthalate polymer samples extruded from the experimental rheometer were redetermined using the vapor phase osmometer. An amine curing agent is required for obtaining suitable silver- filled epoxy-bonded conductive adhesives. When the curing agent was modified with a 47% polyurethane resin, its effectiveness was hampered. Neither silver nor nickel filler impart a high electrical conductivity to Adiprenebased adhesives. Silver filler was found to perform well in Dow-Corning A-4000 adhesive. Two cascaded hot-wire columns are being used to remove heavy gaseous impurities from methane. This purified gas is being enriched in the concentric tube unit to approximately 20% carbon-13. Studies to count low-level krypton-85 in xenon are continuing. The parameters of the counting technique are being determined. The bismuth isotopes produced in bismuth irradiated for polonium production are being determined. Preliminary data indicate the presence of bismuth207 and bismuth-210m. The light bismuth isotopes are probably produced by (n,xn) reactions bismuth-209. The separation of uranium-234 from plutonium-238 solutions was demonstrated. The bulk of the plutonium is removed by anion exchange, and the remainder is extracted from the uranium by solvent extraction techniques. About 99% of the plutonium can be removed in each thenoyltrifluoroacetone extraction. The viscosity, liquid density, and

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.

Characterization of Offgas Generated During Calcination of Incinerator Ash Surrogates

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

Wigent, H.L.; Vienna, J.D.; Darab, J.G.

1999-01-28

The Pacific Northwest National Laboratory (PNNL), in cooperation with the Los Alamos National Laboratory (LANL) and Safe Sites of Colorado (SSOC), developed a recommended flowsheet for the processing of plutonium-bearing incinerator ash stored at the Rocky Flats Environmental Technology Site (RFETS) (Lucy et al. 1998). This flowsheet involves a calcination pretreatment step, the purpose of which is to remove carbonaceous material from the incinerator ash. Removal of this material reduced the probability of process upsets, improved product quality, and increases ash waste loading. As part of the continued development of the recommended flowsheet, PNNL performed a series of tests tomore » characterize the offgas generated during the calcination process.« less

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.

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...

Phosphorous removal from aqueous solution can be enhanced through the calcination of lime sludge.

PubMed

Bal Krishna, K C; Niaz, Mohamed R; Sarker, Dipok C; Jansen, Troy

2017-09-15

Water treatment plants generate an enormous amount of the sludge which is normally treated as waste. In the recent past, many investigations have been focused on developing an economical adsorbent using water treatment sludge to remove phosphorous (P) from aqueous solutions. However, the great extents of the studies have been limited in the use of alum- and iron-based sludges. This study, therefore, investigated the P removal performance of the calcined lime sludge. Calcined lime sludge at 700 °C significantly enhanced the P removal efficiency whereas marginal improvement was noted when the sludge calcined at 400 °C was tested. With increase P removal efficiency, final pH values of the solution also significantly increased. P removal efficiency of the calcined sludge decreased with increasing the initial P concentrations. However, the removal efficiency could be improved by increasing the weight of the sludge. Further analysis demonstrated that P removal trend followed both pseudo-second order and diffusion-chemisorption kinetics signifying the P removal is potentially due to a multi-mechanistic reaction in which, the process is controlled by intra-particle diffusion followed by chemisorptions. Copyright © 2017 Elsevier Ltd. All rights reserved.

Effects of pH and calcination temperature on structural and optical properties of alumina nanoparticles

NASA Astrophysics Data System (ADS)

Amirsalari, A.; Farjami Shayesteh, S.

2015-06-01

In this study, we describe the synthesis of alumina nanoparticles using a chemical wet method in at varying pH. The optimized prepared particles with pH equals to 9 were calcined at various temperatures. For characterization of structural and optical properties of nanoparticles had been used X-ray diffraction, Infrared Fourier transform spectroscopy, field effect-scanning electron microscopy, photoluminescence and ultraviolet-visible spectroscopy. The results revealed that the nanoparticles calcined at 500 °C consist of an Al2O3 tetragonal structure and tetragonal distortion decreases with increasing calcination temperature up to 750 °C then increased with increasing temperature. Another phase similar to γ-Al2O3 was formed instead of δ-Al2O3 in the transition sequence from the γ to θ phase. FT-IR analysis; suggests that there are a few different types of functional groups on the surface of the alumina nanoparticles such as hydroxy groups and oxy groups. The transmittance spectra showed that the absorption bands in the UV region strongly depend on the calcination temperature. Moreover, the results showed that alumina has an optical direct band gap and that the energy gap decreases with increasing the calcination temperature and pH of the reaction. Luminescence spectra showed that some luminescent centers such as OH-related radiative centers and oxygen vacancies (F, F22+ and F2 centers) centers exist in the nanoparticles.

Effect of calcination temperature on structural and photocatalyst properties of nanofibers prepared from low-cost natural ilmenite mineral by simple hydrothermal method

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

Simpraditpan, Athapon; Wirunmongkol, Thanakorn; Pavasupree, Sorapong, E-mail: sorapongp@yahoo.com

2013-09-01

Graphical abstract: - Highlights: • Nanofibers were prepared from low-cost ilmenite mineral via simple hydrothermal. • High photocatalyst nanofibers were prepared via post heat treatment method. • The nanofibers calcined at 100–700 °C for 2 h maintained nanofiber structure. • The calcined nanofibers at 400 °C showed the highest photocatalytic activity. - Abstract: Titanate nanofibers were synthesized via the hydrothermal method (120 °C for 72 h) using natural ilmenite mineral (FeTiO{sub 3}) as the starting material. The samples were characterized by X-ray diffraction (XRD), X-ray fluorescent (XRF), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Brunauer–Emmett–Teller (BET) for specificmore » surface area. The nanofibers were 20–90 nm in diameter and 2–7 μm in length. The as-synthesized nanofibers calcined at 300–400 °C showed TiO{sub 2} (B) whereas the nanofibers calcined at 500 °C revealed a mixture of two phases of TiO{sub 2} (B) and anatase. The nanofibers calcined at high temperature of 600–1000 °C showed a mixture of tri-crystalline of anatase, rutile, and Fe{sub 2}O{sub 3}. The rutile phase increased with increasing calcination temperature. The nanofibers calcined at 300–700 °C maintained their structure while the morphology of the nanofibers calcined at 800–1000 °C transformed into submicron rod-like structure. This increase of calcination temperature led to the phase transformation from thermodynamically metastable anatase to the most stable form of rutile phase. The crystallite size of prepared samples increased with increasing calcination temperature. Interestingly, with increasing calcination temperature, the absorption edge of the prepared samples shows an obvious shift to visible light region due to the change of crystallite phase and increased crystallite size. Therefore, the band gap energy of the prepared samples became narrower with increasing calcination temperature. Furthermore

[Based on Curing Age of Calcined Coal Gangue Fine Aggregate Mortar of X-Ray Diffraction and Scanning Electron Microscopy Analysis].

PubMed

Dong, Zuo-chao; Xia, Jun-wu; Duan, Xiao-mu; Cao, Ji-chang

2016-03-01

By using X-ray diffraction (XRD) and environmental scanning electron microscope (SEM) analysis method, we stud- ied the activity of coal gangue fine aggregate under different calcination temperature. In view of the activity of the highest-700 degrees C high temperature calcined coal gangue fine aggregate mortar of hydration products, microstructure and strength were discussed in this paper, and the change laws of mortar strength with curing age (3, 7, 14, 28, 60 and 90 d) growth were analyzed. Test results showed that coal gangue fine aggregate with the increase of calcination temperature, the active gradually increases. When the calcination temperature reaches 700 degrees C, the activity of coal gangue fine aggregate is the highest. When calcining temperature continues to rise, activity falls. After 700 degrees C high temperature calcined coal gangue fine aggregate has obvious ash activity, the active components of SiO2 and Al2 O3 can be with cement hydration products in a certain degree of secondary hydration reaction. Through on the top of the activity of different curing age 700 degrees C high temperature calcined coal gangue fine aggregate mortar, XRD and SEM analysis showed that with the increase of curing age, secondary hydration reaction will be more fully, and the amount of hydration products also gradually increases. Compared with the early ages of the cement mortar, the products are more stable hydration products filling in mortar microscopic pore, which can further improve the microstructure of mortar, strengthen the interface performance of the mortar. The mortar internal structure is more uniform, calcined coal gangue fine aggregate and cement mortar are more of a strong continuous whole, which increase the later strength of hardened cement mortar, 700 degrees C high temperature calcined coal gangue fine aggregate pozzolanic effect is obvious.

Additional Effects of Silver Nanoparticles on Bactericidal Efficiency Depend on Calcination Temperature and Dip-Coating Speed▿

PubMed Central

Le, Nhung Thi Tuyet; Nagata, Hirofumi; Aihara, Mutsumi; Takahashi, Akira; Okamoto, Toshihiro; Shimohata, Takaaki; Mawatari, Kazuaki; Kinouchi, Yhosuke; Akutagawa, Masatake; Haraguchi, Masanobu

2011-01-01

There is an increasing interest in the application of photocatalytic properties for disinfection of surfaces, air, and water. Titanium dioxide is widely used as a photocatalyst, and the addition of silver reportedly enhances its bactericidal action. However, the synergy of silver nanoparticles and TiO2 is not well understood. The photocatalytic elimination of Bacillus atrophaeus was examined under different calcination temperatures, dip-coating speeds, and ratios of TiO2, SiO2, and Ag to identify optimal production conditions for the production of TiO2- and/or TiO2/Ag-coated glass for surface disinfection. Photocatalytic disinfection of pure TiO2 or TiO2 plus Ag nanoparticles was dependent primarily on the calcination temperature. The antibacterial activity of TiO2 films was optimal with a high dip-coating speed and high calcination temperature (600°C). Maximal bacterial inactivation using TiO2/Ag-coated glass was also observed following high-speed dip coating but with a low calcination temperature (250°C). Scanning electron microscopy (SEM) showed that the Ag nanoparticles combined together at a high calcination temperature, leading to decreased antibacterial activity of TiO2/Ag films due to a smaller surface area of Ag nanoparticles. The presence of Ag enhanced the photocatalytic inactivation rate of TiO2, producing a more pronounced effect with increasing levels of catalyst loading. PMID:21724887

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.

Calcined polyaniline-iron composite as a high efficient cathodic catalyst in microbial fuel cells.

PubMed

Lai, Bin; Wang, Peng; Li, Haoran; Du, Zhuwei; Wang, Lijuan; Bi, Sichao

2013-03-01

A new type of carbon-nitrogen-metal catalyst, PANI-Fe-C, was synthesized by calcination process. According to the results of FT-IR and XPS analysis, polyaniline chain was broken by calcination. Small nitrogen-contained molecular fragments were gasified during calcination process, while the remaining nitrogen atoms were enchased in the new produced multiple carbon rings by C-N and CN bonds and performed as the catalytic active sites and the covalent centers for soluble iron components. Calculated from the polarization curves, a maximum power density of 10.17W/m(3) for the MFC with the synthetic catalyst was obtained, which was slightly higher than the MFC with Pt/C catalyst of 9.56W/m(3). All the results obtained in this paper proved that the newly synthetic nitrogen-carbon-metal catalyst would be a potential alternative to the expensive Pt/C catalyst in the field of MFC. Copyright © 2012 Elsevier Ltd. All rights reserved.

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.

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.

The effect of calcination temperature on the formation and magnetic properties of ZnMn2O4 spinel

NASA Astrophysics Data System (ADS)

Hermanto, B.; Ciswandi; Afriani, F.; Aryanto, D.; Sudiro, T.

2018-03-01

The spinel based on transition-metal oxides has a typical composition of AB2O4. In this study, the ZnMn2O4 spinel was synthesized using a powder metallurgy technique. The Zn and Mn metallic powders with an atomic ratio of 1:2 were mechanically alloyed for 3 hours in aqueous solution. The mixed powder was then calcined in a muffle furnace at elevated temperature of 400, 500 and 600 °C. The X-ray Diffractometer (XRD) was used to evaluate the formation of a ZnMn2O4 spinel structure. The magnetic properties of the sample at varying calcination temperatures were characterized by a Vibrating Sample Magnetometer (VSM). The results show that the fraction of ZnMn2O4 spinel formation increases with the increase of calcination temperature. The calcination temperature also affects the magnetic properties of the samples.

Synthesis and Study of Gel Calcined Cd-Sn Oxide Nanocomposites

NASA Astrophysics Data System (ADS)

De, Arijit; Kundu, Susmita

2016-07-01

Cd-Sn oxide nanocomposites were synthesized by sol-gel method from precursor sol containing Cd:Sn = 2:1 and 1:1 mol ratio. Instead of coprecipitation, a simple novel gel calcination route was followed. Cd (NO3)2. 4H2O and SnCl4. 5H2O were used as starting materials. Gel was calcined at 1050 °C for 2 h to obtain nanocomposites. XRD analysis reveals the presence of orthorhombic, cubic Cd2SnO4 along with orthorhombic, hexagonal CdSnO3 phases in both the composites. SEM and TEM studies indicate the development of nanocomposites of different shapes suggesting different degrees of polymerization in precursor sol of different composition. UV-Vis absorption spectra show a blue shift for both the composites compared to bulk values. Decrease of polarization with frequency, dipole contribution to the polarization, and more sensitivity to ethanol vapor were observed for the nanocomposite derived from precursor sol containing Cd:Sn = 2:1 mol ratio.

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

Method for calcining nuclear waste solutions containing zirconium and halides

DOEpatents

Newby, Billie J.

1979-01-01

A reduction in the quantity of gelatinous solids which are formed in aqueous zirconium-fluoride nuclear reprocessing waste solutions by calcium nitrate added to suppress halide volatility during calcination of the solution while further suppressing chloride volatility is achieved by increasing the aluminum to fluoride mole ratio in the waste solution prior to adding the calcium nitrate.

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.

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.

The calcination temperature dependence of microstructural, vibrational spectra and magnetic properties of nanocrystalline Mn0.5Zn0.5Fe2O4

NASA Astrophysics Data System (ADS)

Indrayana, I. P. T.; Siregar, N.; Suharyadi, E.; Kato, T.; Iwata, S.

2016-11-01

Effect of calcination temperature on microstructural, vibrational, and magnetic properties of Mn0.5Zn0.5Fe2O4 nanoparticles have been successfully investigated. The nanoparticles were synthesized via coprecipitation method and calcined at different temperatures varying from 400, 600, 800, and 1000°C. The X-ray diffraction (XRD) pattern confirmed the formation of cubic spinel structure Mn0.5Zn0.5Fe2O4 with crystallite size ranging from 18.3 nm to 24.8 nm. The TEM micrograph showed the morphology of nanoparticles change from nearly spherical to cubic form after calcination. The FTIR spectra confirmed the existence of vibrations at 416.6 cm-1 - 455.2 cm-1 and 555.5 cm-1 -578.6 cm-1 which corresponds to the intrinsic stretching vibration of metal-oxygen at octahedral and tetrahedral sites, respectively. The maximum specific magnetization and coercivity increase with increasing calcination temperature. The maximum specific magnetization value of 54.7emu/gram was obtained for sample calcined at 1000°C. The results showed that calcination treatment will facilitate the tunability of microstructural and magnetic properties of nanoparticles for expanding the field of application.

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.

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.

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.

Synthesis and antibacterial evaluation of calcinated Ag-doped nano-hydroxyapatite with dispersibility.

PubMed

Furuzono, Tsutomu; Motaharul, Mazumder; Kogai, Yasumichi; Azuma, Yoshinao; Sawa, Yoshiki

2015-05-01

Dispersible hydroxyapatite (HAp) nanoparticles are very useful for applying a monolayer to implantable medical devices using the nano-coating technique. To improve tolerance to infection on implanted medical devices, silver-doped HAp (Ag-HAp) nanoparticles with dispersiblity and crystallinity were synthesized, avoiding calcination-induced sintering, and evaluated for antibacterial activity. The Ca10-xAgx(PO4)6(OH)2 with x = 0 and 0.2 were prepared by wet chemical processing at 100°C. Before calcination at 700°C for 2 h, two kinds of anti-sintering agents, namely a Ca(NO3)2 (Ca salt) and a polyacrylic acid/Ca salt mixture (PAA-Ca), were used. Escherichia coli was used to evaluate the antibacterial activity of the nanopowder. When PAA-Ca was used as an anti-sintering agent in calcination to prepare the dispersible nanoparticles, strong metallic Ag peaks were observed at 38.1° and 44.3° (2θ) in the X-ray diffraction (XRD) profile. However, the Ag peak was barely observed when Ca salt was used alone as the anti-sintering agent. Thus, using Ca salt alone was more effective for preparation of dispersible Ag-HAp than PAA-Ca. The particle average size of Ag-HAp with 0.5 mol% of Ag content was found to be 325 ± 70 nm when the formation of large particleaggregations was prevented, as determined by dynamic light scattering instrument. The antibacterial activity of the Ag-HAp nanoparticles possessing 0.5 mol% against E. coli was greater than 90.0%. Dispersible and crystalline nano Ag-HAp can be obtained by using Ca salt alone as an anti-sintering agent. The nanoparticles showed antibacterial activity.

Effect of calcinations temperature of CuO nanoparticle on the kinetics of decontamination and decontamination products of sulphur mustard.

PubMed

Mahato, T H; Singh, Beer; Srivastava, A K; Prasad, G K; Srivastava, A R; Ganesan, K; Vijayaraghavan, R

2011-09-15

Present study investigates the potential of CuO nanoparticles calcined at different temperature for the decontamination of persistent chemical warfare agent sulphur mustard (HD) at room temperature (30 ± 2 °C). Nanoparticles were synthesized by precipitation method and characterized by using SEM, EDAX, XRD, and Raman Spectroscopy. Synthesized nanoparticles were tested as destructive adsorbents for the degradation of HD. Reactions were monitored by GC-FID technique and the reaction products characterized by GC-MS. It was observed that the rate of degradation of HD decreases with the increase in calcination temperature and there is a change in the percentage of product of HD degradation. GC-MS data indicated that the elimination product increases with increase in calcination temperature whereas the hydrolysis product decreases. Copyright © 2011 Elsevier B.V. All rights reserved.

Evaluation and Testing of IONSIV IE-911 for the Removal of Cesium-137 from INEEL Tank Waste and Dissolved Calcines

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

N. R. Mann; T. A. Todd; K. N. Brewer

1999-04-01

Development of waste treatment processes for the remediation of radioactive wastes is currently underway. A number of experiments were performed at the Idaho Nuclear Technology and Environmental Center (INTEC) located at the Idaho National Engineering and Environmental Laboratory (INEEL) with the commercially available sorbent material, IONSIV IE-911, crystalline silicotitanate (CST), manufactured by UOP LLC. The purpose of this work was to evaluate the removal efficiency, sorbent capacity and selectivity of CST for removing Cs-137 from actual and simulated acidic tank waste in addition to dissolved pilot-plant calcine solutions. The scope of this work included batch contact tests performed with non-radioactivemore » dissolved Al and Run-64 pilot plant calcines in addition to simulants representing the average composition of tank waste. Small-scale column tests were performed with actual INEEL tank WM-183 waste, tank waste simulant, dissolved Al and Run-64 pilot plant calcine solutions. Small-scale column experiments using actual WM-183 tank waste resulted in fifty-percent Cs-137 breakthrough at approximately 589 bed volumes. Small-scale column experiments using the tank waste simulant displayed fifty-percent Cs-137 breakthrough at approximately 700 bed volumes. Small-scale column experiments using dissolved Al calcine simulant displayed fifty-percent Cs-137 breakthrough at approximately 795 bed volumes. Column experiments with dissolved Run-64, pilot plant calcine did not reach fifty-percent breakthrough throughout the test.« less

Mercury and methylmercury contents in mine-waste calcine, water, and sediment collected from the Palawan Quicksilver mine, Philippines

USGS Publications Warehouse

Gray, J.E.; Greaves, I.A.; Bustos, D.M.; Krabbenhoft, D.P.

2003-01-01

The Palawan Quicksilver mine, Philippines, produced about 2,900 t of mercury during mining of cinnabar ore from 1953 to 1976. More than 2,000,000 t of mine-waste calcines (retorted ore) were produced during mining, much of which were used to construct a jetty in nearby Honda Bay. Since 1995, high Hg contents have been found in several people living near the mine, and 21 of these people were treated for mercury poisoning. Samples of mine-waste calcine contain high total Hg concentrations ranging from 43-660 ??g/g, whereas total Hg concentrations in sediment samples collected from a mine pit lake and local stream vary from 3.7-400 ??g/g. Mine water flowing through the calcines is acidic, pH 3.1-4.3, and total Hg concentrations ranging from 18-31 ??g/l in this water significantly exceed the 1.0-??g/l drinking water standard for Hg recommended by the World Health Organization (WHO). Total Hg contents are generally lower in water samples collected from surrounding domestic wells, the mine pit lake, Honda Bay, and the nearby stream, varying from 0.008-1.4 ??g/l. Methylmercury concentrations in water draining mine calcines range from <0.02-1.4 ng/l, but methylmercury is highest in the pit lake water, ranging from 1.7-3.1 ng/l. Mercury methylation at the Palawan mine is similar to or higher than that found in other mercury mines worldwide. Much of the methylmercury generated in Palawan mine-waste calcines and those in Honda Bay is transferred to water, and then to marine fish and seafood. A food source pathway of Hg to humans is most likely in this coastal, high fish-consuming population.

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.).

Interfacial interactions between calcined hydroxyapatite nanocrystals and substrates.

PubMed

Okada, Masahiro; Furukawa, Keiko; Serizawa, Takeshi; Yanagisawa, Yoshihiko; Tanaka, Hidekazu; Kawai, Tomoji; Furuzono, Tsutomu

2009-06-02

Interfacial interactions between calcined hydroxyapatite (HAp) nanocrystals and surface-modified substrates were investigated by measuring adsorption behavior and adhesion strength with a quartz crystal microbalance (QCM) and a contact-mode atomic force microscope (AFM), respectively. The goal was to develop better control of HAp-nanocrystal coatings on biomedical materials. HAp nanocrystals with rodlike or spherical morphology were prepared by a wet chemical process followed by calcination at 800 degrees C with an antisintering agent to prevent the formation of sintered polycrystals. The substrate surface was modified by chemical reaction with a low-molecular-weight compound, or graft polymerization with a functional monomer. QCM measurement showed that the rodlike HAp nanocrystals adsorbed preferentially onto anionic COOH-modified substrates compared to cationic NH2- or hydrophobic CH3-modified substrates. On the other hand, the spherical nanocrystals adsorbed onto NH2- and COOH-modified substrates, which indicates that the surface properties of the HAp nanocrystals determined their adsorption behavior. The adhesion strength, which was estimated from the force required to move the nanocrystal in contact-mode AFM, on a COOH-grafted substrate prepared by graft polymerization was almost 9 times larger than that on a COOH-modified substrate prepared by chemical reaction with a low-molecular-weight compound, indicating that the long-chain polymer grafted on the substrate mitigated the surface roughness mismatch between the nanocrystal and the substrate. The adhesion strength of the nanocrystal bonded covalently by the coupling reaction to a Si(OCH3)-grafted substrate prepared by graft polymerization was approximately 1.5 times larger than that when adsorbed on the COOH-grafted substrate.

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.

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.

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.

Calcined Eggshell Waste for Mitigating Soil Antibiotic-Resistant Bacteria/Antibiotic Resistance Gene Dissemination and Accumulation in Bell Pepper.

PubMed

Ye, Mao; Sun, Mingming; Feng, Yanfang; Li, Xu; Schwab, Arthur P; Wan, Jinzhong; Liu, Manqiang; Tian, Da; Liu, Kuan; Wu, Jun; Jiang, Xin

2016-07-13

The combined accumulation of antibiotics, heavy metals, antibiotic-resistant bacteria (ARB)/antibiotic resistance genes (ARGs) in vegetables has become a new threat to human health. This is the first study to investigate the feasibility of calcined eggshells modified by aluminum sulfate as novel agricultural wastes to impede mixed contaminants from transferring to bell pepper (Capsicum annuum L.). In this work, calcined eggshell amendment mitigated mixed pollutant accumulation in bell pepper significantly, enhanced the dissipation of soil tetracycline, sulfadiazine, roxithromycin, and chloramphenicol, decreased the water-soluble fractions of antibiotics, and declined the diversity of ARB/ARGs inside the vegetable. Moreover, quantitative polymerase chain reaction analysis detected that ARG levels in the bell pepper fruits significantly decreased to 10(-10) copies/16S copies, indicating limited risk of ARGs transferring along the food chain. Furthermore, the restoration of soil microbial biological function suggests that calcined eggshell is an environmentally friendly amendment to control the dissemination of soil ARB/ARGs in the soil-vegetable system.

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.

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.

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.

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.

Limestone calcination under calcium-looping conditions for CO2 capture and thermochemical energy storage in the presence of H2O: an in situ XRD analysis.

PubMed

Valverde, Jose Manuel; Medina, Santiago

2017-03-15

This work reports an in situ XRD analysis of whether the calcination/carbonation behavior of natural limestone (CaCO 3 ) is affected by the addition of H 2 O to the calciner at a very low concentration under relevant Calcium-Looping (CaL) conditions for CO 2 capture in coal fired power plants (CFPP) and Thermochemical Energy Storage (TCES) in Concentrated Solar Power plants (CSP). Previous studies have demonstrated that the presence of steam in the calciner at a high concentration yields a significant increase in the reaction rate. However, a further undesired consequence is the serious deterioration of the CaO mechanical strength, which would lead to particle attrition and mass loss in any CaL process based on the use of circulating fluidized beds. The results presented in this manuscript on the time evolution of the wt% and crystallite size of the phases involved in the calcination/carbonation reactions indicate that the calcination rate is still notably increased by the presence of H 2 O at very low concentrations whereas the reactivity toward carbonation and crystal structure of the formed CaO are not essentially affected, which suggests that the CaO mechanical strength is not impaired. Thus, the benefit of using steam for calcination in the CaL process could be still retained while at the same time particle attrition would not be promoted.

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.

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.

46 CFR 148.04-15 - Petroleum coke, uncalcined; petroleum coke, uncalcined and calcined (mixture).

Code of Federal Regulations, 2010 CFR

2010-10-01

... 46 Shipping 5 2010-10-01 2010-10-01 false Petroleum coke, uncalcined; petroleum coke, uncalcined and calcined (mixture). 148.04-15 Section 148.04-15 Shipping COAST GUARD, DEPARTMENT OF HOMELAND... Requirements for Certain Material § 148.04-15 Petroleum coke, uncalcined; petroleum coke, uncalcined and...

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

Development of a SREX Flowsheet for the Separation of Strontium from Dissolved INEEL Zirconium Calcine

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

Law, Jack Douglas; Wood, David James; Todd, Terry Allen

1999-02-01

Laboratory experimentation has indicated that the SREX process is effective for partitioning 90 Sr from acidic radioactive waste solutions located at the Idaho Nuclear Technology and Engineering Center. These laboratory results were used to develop a flowsheet for countercurrent testing of the SREX process with dissolved pilot plant calcine. Testing was performed using 24 stages of 2-cm diameter centrifugal contactors which are installed in the Remote Analytical Laboratory hot cell. Dissolved Run #64 pilot plant calcine spiked with 85 Sr was used as feed solution for the testing. The flowsheet tested consisted of an extraction section (0.15 M 4',4'(5')-di-(tert-butylcyclohexo)-18-crown-6 andmore » 1.5 M TBP in Isopar-L.), a 1.0 M NaNO3 scrub section to remove extracted K from the SREX solvent, a 0.01 M HNO3 strip section for the removal of Sr from the SREX solvent, a 0.25 M Na2CO3 wash section to remove degradation products from the solvent, and a 0.1 M HNO3 rinse section. The behavior of 85 Sr, Na, K, Al, B, Ca, Cr, Fe, Ni, and Zr was evaluated. The described flowsheet successfully extracted 85 Sr from the dissolved pilot plant calcine with a removal efficiency of 99.6%. Distribution coefficients for 85 Sr ranged from 3.6 to 4.5 in the extraction section. With these distribution coefficients a removal efficiency of approximately >99.99% was expected. It was determined that the lower than expected removal efficiency can be attributed to a stage efficiency of only 60% in the extraction section. Extracted K was effectively scrubbed from the SREX solvent with the 1.0 M NaNO3 resulting in only 6.4% of the K in the HLW strip product. Sodium was not extracted from the dissolved calcine by the SREX solvent; however, the use of a 1.0 M NaNO3 scrub solution resulted in a Na concentration of 70 mg/L (12.3% of the feed concentration) in the HLW strip product. Al, B, Ca, Cr, Fe, Ni, and Zr were determined to be essentially inextractable.« less

40 CFR Table Aa-2 to Subpart Aa of... - Kraft Lime Kiln and Calciner Emissions Factors for CH4 and N2O

Code of Federal Regulations, 2014 CFR

2014-07-01

... 40 Protection of Environment 21 2014-07-01 2014-07-01 false Kraft Lime Kiln and Calciner Emissions Factors for CH4 and N2O AA Table AA-2 to Subpart AA of Part 98 Protection of Environment ENVIRONMENTAL... Manufacturing Pt. 98, Subpt. AA, Table AA -2 Table AA-2 to Subpart AA of Part 98—Kraft Lime Kiln and Calciner...

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.

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 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

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.

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

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.

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.

Photocatalytic hydrogen evolution of palladium nanoparticles decorated black TiO2 calcined in argon atmosphere

NASA Astrophysics Data System (ADS)

Wu, Ming-Chung; Hsiao, Kai-Chi; Chang, Yin-Hsuan; Chan, Shun-Hsiang

2018-02-01

Black TiO2 nanoparticles (BTN) was prepared by sol-gel derived precursor calcined in an argon atmosphere. The synthesized BTN with trivalent titanium ion, structural defect, and oxygen vacancy shows a remarkably high absorbance in the visible light spectrum. BTN thus behaves a higher visible-active nanoreactor than white TiO2 nanoparticles (WTN) in the aqueous solution for organic pollutant degradation. Moreover, palladium decoration on the BTN surface (Pd-BTN) demonstrates a fascinating clean energy application. The obtained Pd-BTN fulfills a satisfied green material demand in the photocatalytic hydrogen production application. Pd-BTN calcined at 400 °C (Pd-BTN-400) shows the high photocatalytic hydrogen generation rate of 5200 μmol/g h under UV-A irradiation and 9300 μmol/g h under UV-B irradiation, respectively. The well-developed material, Pd-BTN-400, could be one of the best solutions in the concern of clean energy and water-purification with regard to the continuous environmental issue.

Calcined Mg-Fe layered double hydroxide as an absorber for the removal of methyl orange

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

Peng, Chao; State Key Laboratory of Silicate Materials for Architectures, Wuhan University of Technology, Wuhan 430070; Dai, Jing

2015-05-15

In this work, methyl orange (MO) was effectively removed from aqueous solution with the calcined product of hydrothermal synthesized Mg/Fe layered double hydroxide (Mg/Fe-LDH). The structure, composition, morphology and textural properties of the Mg/Fe-LDH before and after adsorption were characterized by X-ray diffraction, Fourier transformation infrared spectroscopy, transmission electron microscopy, nitrogen adsorption apparatus and X-ray photoelectron spectroscopy. It was confirmed that MO had been absorbed by calcined Mg/Fe-LDH which had strong interactions with MO. The adsorption of MO onto the Mg/Fe-LDH was systematically investigated by batch tests. The adsorption capacity of the Mg/Fe-LDH toward MO was found to be 194.9more » mg • g{sup −1}. Adsorption kinetics and isotherm studies revealed that the adsorption of MO onto Mg/Fe-LDH was a spontaneous and endothermic process. These results indicate that Mg/Fe-LDH is a promising material for the removal of MO.« less

Development of a SREX flowsheet for the separation of strontium from dissolved INEEL zirconium calcine

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

Law, J.D.; Wood, D.J.; Todd, T.A.

1999-01-01

Laboratory experimentation has indicated that the SREX process is effective for partitioning {sup 90}Sr from acidic radioactive waste solutions located at the Idaho Nuclear Technology and Engineering Center. These laboratory results were used to develop a flowsheet for countercurrent testing of the SREX process with dissolved pilot plant calcine. Testing was performed using 24 stages of 2-cm diameter centrifugal contactors which are installed in the Remote Analytical Laboratory hot cell. Dissolved Run No.64 pilot plant calcine spiked with {sup 85}Sr was used as feed solution for the testing. The flowsheet tested consisted of an extraction section (0.15 M 4{prime},4{prime}(5{prime})-di-(tert-butylcyclohexo)-18-crown-6 andmore » 1.5 M TBP in Isopar-L.), a 1.0 M NaNO{sub 3} scrub section to remove extracted K from the SREX solvent, a 0.01 M HNO{sub 3} strip section for the removal of Sr from the SREX solvent, a 0.25 M Na2CO{sub 3} wash section to remove degradation products from the solvent, and a 0.1 M HNO{sub 3} rinse section. The behavior of {sup 85}Sr, Na, K, Al, B, Ca, Cr, Fe, Ni, and Zr was evaluated. The described flowsheet successfully extracted {sup 85}Sr from the dissolved pilot plant calcine with a removal efficiency of 99.6%. Distribution coefficients for {sup 85}Sr ranged from 3.6 to 4.5 in the extraction section. With these distribution coefficients a removal efficiency of approximately >99.99% was expected. It was determined that the lower than expected removal efficiency can be attributed to a stage efficiency of only 60% in the extraction section. Extracted K was effectively scrubbed from the SREX solvent with the 1.0 M NaNO{sub 3} resulting in only 6.4% of the K in the HLW strip product. Sodium was not extracted from the dissolved calcine by the SREX solvent; however, the use of a 1.0 M NaNO{sub 3} scrub solution resulted in a Na concentration of 70 mg/L (12.3% of the feed concentration) in the HLW strip product. Al, B, Ca, Cr, Fe, Ni, and Zr were

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.

Operation of a 25 KWth Calcium Looping Pilot-plant with High Oxygen Concentrations in the Calciner.

PubMed

Erans, María; Jeremias, Michal; Manovic, Vasilije; Anthony, Edward J

2017-10-25

Calcium looping (CaL) is a post-combustion CO2 capture technology that is suitable for retrofitting existing power plants. The CaL process uses limestone as a cheap and readily available CO2 sorbent. While the technology has been widely studied, there are a few available options that could be applied to make it more economically viable. One of these is to increase the oxygen concentration in the calciner to reduce or eliminate the amount of recycled gas (CO2, H2O and impurities); therefore, decreasing or removing the energy necessary to heat the recycled gas stream. Moreover, there is a resulting increase in the energy input due to the change in the combustion intensity; this energy is used to enable the endothermic calcination reaction to occur in the absence of recycled flue gases. This paper presents the operation and first results of a CaL pilot plant with 100% oxygen combustion of natural gas in the calciner. The gas coming into the carbonator was a simulated flue gas from a coal-fired power plant or cement industry. Several limestone particle size distributions are also tested to further explore the effect of this parameter on the overall performance of this operating mode. The configuration of the reactor system, the operating procedures, and the results are described in detail in this paper. The reactor showed good hydrodynamic stability and stable CO2 capture, with capture efficiencies of up to 70% with a gas mixture simulating the flue gas of a coal-fired power plant.

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.

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.

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.

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...

Feasibility of sulfate-calcined eggshells for removing pathogenic bacteria and antibiotic resistance genes from landfill leachates.

PubMed

Ye, Mao; Sun, Mingming; Chen, Xu; Feng, Yanfang; Wan, Jinzhong; Liu, Kuan; Tian, Da; Liu, Manqiang; Wu, Jun; Schwab, Arthur P; Jiang, Xin

2017-05-01

High abundance of human pathogen and antibiotic resistance genes (ARGs) in landfill leachate has become an emerging threat against human health. Therefore, sulfate- and calcination-modified eggshells as green agricultural bioresource were applied to test the feasibility of removing pathogenic bacteria and ARGs from leachate. The highest removal of Escherichia coli (E. coil) and gentamycin resistant gene (gmrA) from artificial contaminated landfill leachate was achieved by the application of eggshell with combined treatment of sulfate and calcination. The 16S and gmrA gene copies of E. coil declined significantly from 1.78E8±8.7E6 and 4.12E8±5.9E6 copies mL -1 to 1.32E7±2.6E6 and 2.69E7±7.2E6 copies mL -1 , respectively, within 24h dynamic adsorption equilibrium process (p<0.05). Moreover, according to the Langmuir kinetic model, the greatest adsorption amount (1.56×10 9 CFU E. coil per gram of modified eggshells) could be obtained at neutral pH of 7.5. The optimal adsorption eggshells were then screened to the further application in three typical landfill leachates in Nanjing, eastern China. Significant decrease in species and abundance of pathogenic bacteria and ARGs (tet, sul, erm, qnr, and ampC) indicated its great efficiency to purify landfill leachates. This study demonstrated that sulfate-calcined eggshells can be an environmentally-friendly and highly efficient bioadsorbent to the management of reducing dissemination risk of pathogen and ARGs in landfill leachate. Copyright © 2017 Elsevier Ltd. All rights reserved.

Surface complexation modeling calculation of Pb(II) adsorption onto the calcined diatomite

NASA Astrophysics Data System (ADS)

Ma, Shu-Cui; Zhang, Ji-Lin; Sun, De-Hui; Liu, Gui-Xia

2015-12-01

Removal of noxious heavy metal ions (e.g. Pb(II)) by surface adsorption of minerals (e.g. diatomite) is an important means in the environmental aqueous pollution control. Thus, it is very essential to understand the surface adsorptive behavior and mechanism. In this work, the Pb(II) apparent surface complexation reaction equilibrium constants on the calcined diatomite and distributions of Pb(II) surface species were investigated through modeling calculations of Pb(II) based on diffuse double layer model (DLM) with three amphoteric sites. Batch experiments were used to study the adsorption of Pb(II) onto the calcined diatomite as a function of pH (3.0-7.0) and different ionic strengths (0.05 and 0.1 mol L-1 NaCl) under ambient atmosphere. Adsorption of Pb(II) can be well described by Freundlich isotherm models. The apparent surface complexation equilibrium constants (log K) were obtained by fitting the batch experimental data using the PEST 13.0 together with PHREEQC 3.1.2 codes and there is good agreement between measured and predicted data. Distribution of Pb(II) surface species on the diatomite calculated by PHREEQC 3.1.2 program indicates that the impurity cations (e.g. Al3+, Fe3+, etc.) in the diatomite play a leading role in the Pb(II) adsorption and dominant formation of complexes and additional electrostatic interaction are the main adsorption mechanism of Pb(II) on the diatomite under weak acidic conditions.

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

40 CFR Table Aa-2 to Subpart Aa of... - Kraft Lime Kiln and Calciner Emissions Factors for Fossil Fuel-Based CH4 and N2O

Code of Federal Regulations, 2012 CFR

2012-07-01

... 40 Protection of Environment 22 2012-07-01 2012-07-01 false Kraft Lime Kiln and Calciner Emissions Factors for Fossil Fuel-Based CH4 and N2O AA Table AA-2 to Subpart AA of Part 98 Protection of Environment... and Calciner Emissions Factors for Fossil Fuel-Based CH4 and N2O Fuel Fossil fuel-based emissions...

40 CFR Table Aa-2 to Subpart Aa of... - Kraft Lime Kiln and Calciner Emissions Factors for Fossil Fuel-Based CH4 and N2O

Code of Federal Regulations, 2011 CFR

2011-07-01

... 40 Protection of Environment 21 2011-07-01 2011-07-01 false Kraft Lime Kiln and Calciner Emissions Factors for Fossil Fuel-Based CH4 and N2O AA Table AA-2 to Subpart AA of Part 98 Protection of Environment... and Calciner Emissions Factors for Fossil Fuel-Based CH4 and N2O Fuel Fossil fuel-based emissions...

40 CFR Table Aa-2 to Subpart Aa of... - Kraft Lime Kiln and Calciner Emissions Factors for Fossil Fuel-Based CH4 and N2O

Code of Federal Regulations, 2013 CFR

2013-07-01

... 40 Protection of Environment 22 2013-07-01 2013-07-01 false Kraft Lime Kiln and Calciner Emissions Factors for Fossil Fuel-Based CH4 and N2O AA Table AA-2 to Subpart AA of Part 98 Protection of Environment... and Calciner Emissions Factors for Fossil Fuel-Based CH4 and N2O Fuel Fossil fuel-based emissions...

Feasibility of CO₂/SO₂ uptake enhancement of calcined limestone modified with rice husk ash during pressurized carbonation.

PubMed

Chen, Huichao; Zhao, Changsui; Ren, Qiangqiang

2012-01-01

The calcination/carbonation cycle using calcium-based sorbents appears to be a viable method for carbon dioxide (CO₂) capture from combustion gases. Recent attempts to improve the CO₂/SO₂ uptake of a calcium-based sorbent modified by using rice husk ash (RHA) in the hydration process have succeeded in enhancing its effectiveness. The optimal mole ratio of RHA to calcined limestone (M(Si/Ca)) was adjusted to 0.2. The cyclic CO₂ capture characteristics and the SO₂ uptake activity of the modified sorbent were evaluated in a calcination/pressurized carbonation reactor system. Scanning electron microscope (SEM) images and X-ray diffraction (XRD) spectrum of the sorbent were also taken to supplement the study. The results showed that the carbonation conversion was greatly increased for the sorbent with M(Si/Ca) ratio of 0.2. For this sorbent formulation the optimal operating conditions were 700-750 °C and 0.5-0.7 MPa. CO₂ absorption was not proportional to CO₂ concentration in the carbonation atmosphere, but was directly related to reaction time. The CO₂ uptake decreased in the presence of SO₂. SO₂ uptake increased, and the total calcium utilization was maintained over multiple cycles. Analysis has shown that the silicate component is evenly or well distributed, and this serves as a framework to prevent sintering, thus preserving the available microstructure for reaction. The sorbent also displayed high activity to SO₂ absorption and could be used to capture CO₂ and SO₂ simultaneously. Copyright © 2011 Elsevier Ltd. All rights reserved.

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.

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 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.

Mesoporous Titania Powders: The Role of Precursors, Ligand Addition and Calcination Rate on Their Morphology, Crystalline Structure and Photocatalytic Activity

PubMed Central

Masolo, Elisabetta; Meloni, Manuela; Garroni, Sebastiano; Mulas, Gabriele; Enzo, Stefano; Baró, Maria Dolors; Rossinyol, Emma; Rzeszutek, Agnieszka; Herrmann-Geppert, Iris; Pilo, Maria

2014-01-01

We evaluate the influence of the use of different titania precursors, calcination rate, and ligand addition on the morphology, texture and phase content of synthesized mesoporous titania samples, parameters which, in turn, can play a key role in titania photocatalytic performances. The powders, obtained through the evaporation-induced self-assembly method, are characterized by means of ex situ X-Ray Powder Diffraction (XRPD) measurements, N2 physisorption isotherms and transmission electron microscopy. The precursors are selected basing on two different approaches: the acid-base pair, using TiCl4 and Ti(OBu)4, and a more classic route with Ti(OiPr)4 and HCl. For both precursors, different specimens were prepared by resorting to different calcination rates and with and without the addition of acetylacetone, that creates coordinated species with lower hydrolysis rates, and with different calcination rates. Each sample was employed as photoanode and tested in the water splitting reaction by recording I-V curves and comparing the results with commercial P25 powders. The complex data framework suggests that a narrow pore size distribution, due to the use of acetylacetone, plays a major role in the photoactivity, leading to a current density value higher than that of P25. PMID:28344237

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.

Integrated photooxidative-extractive desulfurization system for fuel oil using Cu, Fe and Cu-Fe/TiO2 and eutectic based ionic liquids: Effect of calcination temperature and duration

NASA Astrophysics Data System (ADS)

Zaid, Hayyiratul Fatimah Mohd; Kait, Chong Fai; Mutalib, Mohamed Ibrahim Abdul

2014-10-01

Photocatalyts TiO2 doped with Cu, Fe and Cu-Fe metal at different calcination temperature and duration were successfully prepared and characterized. Photocatalytic oxidative desulfurization of model oil containing dibenzothiophene as the sulfur compound (100 ppm) using the prepared photocatalyst was investigated. The photocatalyst calcined at 500°C and duration of 1 h showed the best performance.

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

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.

Standardization and quality control parameters for Muktā Bhasma (calcined pearl)

PubMed Central

Joshi, Namrata; Sharma, Khemchand; Peter, Hema; Dash, Manoj Kumar

2015-01-01

Background: Muktā Bhasma (MB) is a traditional Ayurvedic preparation for cough, breathlessness, and eye disorders and is a powerful cardiac tonic, mood elevator, and known to promote strength, intellect, and semen production. Objectives: The present research work was conducted to generate fingerprint for raw and processed MB for quality assessment and standardization using classical and other techniques. Setting and Design: Three samples of MB were prepared by purification (śodhana) of Muktā (pearl) followed by repeated calcinations (Māraṇa). Resultant product was subjected to organoleptic tests and Ayurvedic tests for quality control such as rekhāpūrṇatā, vāritaratva, and nirdhūmatva. Materials and Methods: For quality control, physicochemical parameters such as loss on drying, total ash value, acid insoluble ash, specific gravity, pH value, and other tests using techniques such as elemental analysis with energy dispersive X-ray analysis (EDAX), Structural study with powder X-ray diffraction, particle size with scanning electron microscopy (SEM) were carried out on raw Muktā, Śodhita Muktā, and triplicate batches of MB. Results: The study showed that the raw material Muktā was calcium carbonate in aragonite form, which on repeated calcinations was converted into a more stable calcite form. SEM studies revealed that in raw and purified materials the particles were found scattered and unevenly arranged in the range of 718.7–214.7 nm while in final product, uniformly arranged, stable, rod-shaped, and rounded particles with more agglomerates were observed in the range of 279.2–79.93 nm. EDAX analysis revealed calcium as a major ingredient in MB (average 46.32%) which increased gradually in the stages of processing (raw 34.11%, Śodhita 37.5%). Conclusion: Quality control parameters have been quantified for fingerprinting of MB prepared using a particular method. PMID:26600667

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

LAB-SCALE DEMONSTRATION OF PLUTONIUM PURIFICATION BY ANION EXCHANGE, PLUTONIUM (IV) OXALATE PRECIPITATION, AND CALCINATION TO PLUTONIUM OXIDE TO SUPPORT THE MOX FEED MISSION

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

Crowder, M.; Pierce, R.

2012-08-22

H-Canyon and HB-Line are tasked with the production of PuO{sub 2} from a feed of plutonium metal. The PuO{sub 2} will provide feed material for the MOX Fuel Fabrication Facility. After dissolution of the Pu metal in H-Canyon, the solution will be transferred to HB-Line for purification by anion exchange. Subsequent unit operations include Pu(IV) oxalate precipitation, filtration and calcination to form PuO{sub 2}. This report details the results from SRNL anion exchange, precipitation, filtration, calcination, and characterization tests, as requested by HB-Line1 and described in the task plan. This study involved an 80-g batch of Pu and employed testmore » conditions prototypical of HB-Line conditions, wherever feasible. In addition, this study integrated lessons learned from earlier anion exchange and precipitation and calcination studies. H-Area Engineering selected direct strike Pu(IV) oxalate precipitation to produce a more dense PuO{sub 2} product than expected from Pu(III) oxalate precipitation. One benefit of the Pu(IV) approach is that it eliminates the need for reduction by ascorbic acid. The proposed HB-Line precipitation process involves a digestion time of 5 minutes after the time (44 min) required for oxalic acid addition. These were the conditions during HB-line production of neptunium oxide (NpO{sub 2}). In addition, a series of small Pu(IV) oxalate precipitation tests with different digestion times were conducted to better understand the effect of digestion time on particle size, filtration efficiency and other factors. To test the recommended process conditions, researchers performed two nearly-identical larger-scale precipitation and calcination tests. The calcined batches of PuO{sub 2} were characterized for density, specific surface area (SSA), particle size, moisture content, and impurities. Because the 3013 Standard requires that the calcination (or stabilization) process eliminate organics, characterization of PuO{sub 2} batches monitored

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.

Vitrification of radioactive high-level waste by spray calcination and in-can melting

NASA Astrophysics Data System (ADS)

Hanson, M. S.; Bjorklund, W. J.

1980-07-01

After several nonradioactive test runs, radioactive waste from the processing of 1.5 t of spent, light water reactor fuel was successfully concentrated, dried and converted to a vitreous product. A total of 97 L of waste glass (in two stainless steel canisters) was produced. The spray calcination process coupled to the in-can melting process, as developed at Pacific Northwest Labortory, was used to vitrify the waste. An effluent system consisting of a variety of condensation of scrubbing steps more than adequately decontaminated the process off gas before it was released to the atmosphere.

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.

Calcination/dissolution chemistry development Fiscal year 1995

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

Delegard, C.H.

1995-09-01

The task {open_quotes}IPC Liaison and Chemistry of Thermal Reconstitution{close_quotes} is a $300,000 program that was conducted in Fiscal Year (FY) 1995 with U.S. Department of Energy (DOE) Office of Research and Development (EM-53) Efficient Separations and Processing Crosscutting Program supported under technical task plan (TTP) RL4-3-20-04. The principal investigator was Cal Delegard of the Westinghouse Hanford Company (WHC). The task encompassed the following two subtasks related to the chemistry of alkaline Hanford Site tank waste: (1) Technical Liaison with the Institute of Physical Chemistry of the Russian Academy of Science (IPC/RAS) and its research into the chemistry of transuranic elementsmore » (TRU) and technetium (Tc) in alkaline media. (2) Laboratory investigation of the chemistry of calcination/dissolution (C/D) (or thermal reconstitution) as an alternative to the present reference Hanford Site tank waste pretreatment flowsheet, Enhanced Sludge Washing (ESW). This report fulfills the milestone for the C/D subtask to {open_quotes}Provide End-of-Year Report on C/D Laboratory Test Results{close_quotes} due 30 September 1995. A companion report, fulfilling the milestone to provide an end-of-year report on the IPC/RAS liaison, also has been prepared.« less

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.

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.

Biomass Potential of Virgin and Calcined Tapioca (Cassava Starch) for the Removal of Sr(II) and Cs(I) from Aqueous Solutions.

PubMed

Ogata, Fumihiko; Nagai, Noriaki; Ueta, Erimi; Nakamura, Takehiro; Kawasaki, Naohito

2018-01-01

In this study, we prepared novel adsorbents containing virgin and calcined tapioca products for removing strontium (Sr(II)) and cesium (Cs(I)) from aqueous solutions. The characteristics of tapioca, along with its capacity to adsorb Sr(II) and Cs(I), were evaluated. Multiple tapioca products were prepared and tested. The adsorbent prepared by boiling the tapioca followed by calcination at 300°C (BTP300) was the most effective. In addition, adsorption was affected by the adsorbent's surface properties. The Sr(II) and Cs(I) adsorbed onto BTP300 could be recovered through desorption by hydrochloric acid at different concentrations, which indicates that BTP300 can be used several times for adsorption/desorption. The results of this study suggest that BTP300, which was produced from tapioca biomass, can remove Sr(II) and Cs(I) from aqueous solutions.

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.

Genesis of Cr(VI) in Sri Lankan soils and its adsorptive removal by calcined gibbsite

NASA Astrophysics Data System (ADS)

Rajapaksha, A. U.; Wijesundara, D. M.; Vithanage, M. S.; Ok, Y. S.

2012-12-01

Hexavalent chromium is highly toxic to biota and considered as a priority pollutant. Industrial sources of Cr(VI) include leather tanning, plating, electroplating, anodizing baths, rinse waters, etc. In addition, weathering of ultramafic rocks rich in chromium, such as serpentine, is known to Cr(VI) sources into natural water. The Cr(III) is the most stable in the environment, however, conversion of Cr(III) into Cr(VI) occurs in soil due to presence of naturally occurring minerals such as manganese dioxides. We investigated the amount of Cr(VI) recorded from the soils from anthropogenically and naturally contaminated soils (serpentine soils) in Sri Lanka and the removal efficacy of Cr(VI) by calcined gibbsite (Al oxides). The effect of pH on Cr(VI) adsorption was determined by adjusting the pH in the range of 4-10. In the experiments, the adsorbent concentration was kept at 1 g/l of solution containing 10 mg/l Cr(VI) at 25 0C. Total chromium recorded were around 11,000 mg kg-1 and 6,000 mg kg-1 for serpentine soil and tannery waste-contaminated soil, respectively. Although total Cr was high in the contaminated soils, Cr(VI) concentration was only about 28 mg kg-1 and 210 mg kg-1 in the serpentine and tannery soils, respectively. The calcined gibbsite has maximum adsorption of 85 % around pH 4 and adsorption generally decreased with increase of pH.

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.

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

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.

Transesterification of edible, non-edible and used cooking oils for biodiesel production using calcined layered double hydroxides as reusable base catalysts.

PubMed

Sankaranarayanan, Sivashunmugam; Antonyraj, Churchil A; Kannan, S

2012-04-01

Fatty acid methyl esters (FAME) were produced from edible, non-edible and used cooking oils with different fatty acid contents by transesterification with methanol using calcined layered double hydroxides (LDHs) as solid base catalysts. Among the catalysts, calcined CaAl2-LDH (hydrocalumite) showed the highest activity with >90% yield of FAME using low methanol:oil molar ratio (<6:1) at 65 °C in 5 h. The activity of the catalyst was attributed to its high basicity as supported by Hammett studies and CO(2)-TPD measurements. The catalyst was successfully reused in up to four cycles. Some of the properties such as density, viscosity, neutralization number and glycerol content of the obtained biodiesel matched well with the standard DIN values. It is concluded that a scalable heterogeneously catalyzed process for production of biodiesel in high yields from a wide variety of triglyceride oils including used oils is possible using optimized conditions. Copyright © 2012 Elsevier Ltd. All rights reserved.

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.

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.

SOx removal by calcined MgAlFe hydrotalcite-like materials: effect of the chemical composition and the cerium incorporation method.

PubMed

Cantú, Manuel; López-Salinas, Esteban; Valente, Jaime S; Montiel, Ramon

2005-12-15

Sulfur oxides are one of the most hazardous atmospheric pollutants since they contribute directly to acid rain formation. Consequently, stringent environmental regulations limit atmospheric SOx emissions, motivating research on efficient ways to reduce them. To supply an alternative to reduce these emissions in fluid catalytic cracking units, this study discloses efficient SOx reducing materials based on calcined MgAlFe hydrotalcite-like compounds (HT's). Thus, HT materials were synthesized by several methods including cerium addition. The adsorption of SO2 was carried out by contacting the calcined solid with a mixture of SO2 (1%) in air at 650 degrees C. It was demonstrated that the isomorphic incorporation of iron increased its reduction capability which was reflected in higher reduction rates and metal sulfate reduction grade at 550 degrees C. Moreover, when cerium was present in the iron-containing materials the saturation rate was improved, because cerium oxide promotes the oxidation of SO2 to SO3. The way cerium is incorporated influences the SO2 adsorption capacity.

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.

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.

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%.

One-pot synthesis of carbon supported calcined-Mg/Al layered double hydroxides for antibiotic removal by slow pyrolysis of biomass waste

PubMed Central

Tan, Xiaofei; Liu, Shaobo; Liu, Yunguo; Gu, Yanling; Zeng, Guangming; Cai, Xiaoxi; Yan, ZhiLi; Yang, Chunping; Hu, Xinjiang; Chen, Bo

2016-01-01

A biochar supported calcined-Mg/Al layered double hydroxides composite (CLDHs/BC) was synthesized by a one-pot slow pyrolysis of LDHs preloaded bagasse biomass. Multiple characterizations of the product illustrated that the calcined-Mg/Al layered double hydroxides (CLDHs) were successfully coated onto the biochar in slow pyrolysis of pre-treated biomass. The as-synthesized CLDHs/BC could efficiently remove antibiotic tetracycline from aqueous solutions. The coating of CLDHs significantly increased the adsorption ability of biochar, and CLDHs/BC exhibited more than 2 times higher adsorption capacity than that of the pristine biochar (BC) in the tested pH range. The maximum adsorption capacity of CLDHs/BC for tetracycline was 1118.12 mg/g at 318 K. The experimental results suggested that the interaction with LDHs on biochar played a dominant role in tetracycline adsorption, accompanied with π–π interaction and hydrogen bond. This study provides a feasible and simple approach for the preparation of high-performance material for antibiotics contaminated wastewater treatment in a cost-effective way. PMID:28000759

One-pot synthesis of carbon supported calcined-Mg/Al layered double hydroxides for antibiotic removal by slow pyrolysis of biomass waste

NASA Astrophysics Data System (ADS)

Tan, Xiaofei; Liu, Shaobo; Liu, Yunguo; Gu, Yanling; Zeng, Guangming; Cai, Xiaoxi; Yan, Zhili; Yang, Chunping; Hu, Xinjiang; Chen, Bo

2016-12-01

A biochar supported calcined-Mg/Al layered double hydroxides composite (CLDHs/BC) was synthesized by a one-pot slow pyrolysis of LDHs preloaded bagasse biomass. Multiple characterizations of the product illustrated that the calcined-Mg/Al layered double hydroxides (CLDHs) were successfully coated onto the biochar in slow pyrolysis of pre-treated biomass. The as-synthesized CLDHs/BC could efficiently remove antibiotic tetracycline from aqueous solutions. The coating of CLDHs significantly increased the adsorption ability of biochar, and CLDHs/BC exhibited more than 2 times higher adsorption capacity than that of the pristine biochar (BC) in the tested pH range. The maximum adsorption capacity of CLDHs/BC for tetracycline was 1118.12 mg/g at 318 K. The experimental results suggested that the interaction with LDHs on biochar played a dominant role in tetracycline adsorption, accompanied with π-π interaction and hydrogen bond. This study provides a feasible and simple approach for the preparation of high-performance material for antibiotics contaminated wastewater treatment in a cost-effective way.

Infrared detection of the mineralogical aspects that influence the processing of calcined kaolin

NASA Astrophysics Data System (ADS)

Groenheide, Stefan; Guatame-Garcia, Adriana; Buxton, Mike; van der Werff, Harald

2017-04-01

Calcined kaolin is an industrial minerals product used in the production of paper, paint, rubber and other specialty applications. It is produced from kaolinite through a series of refinement steps and final calcination at temperatures of above 900°C, with the aim of generating a whiter and more abrasive material. The raw kaolin ore is a mixture of clay minerals, quartz and feldspars, where kaolinite is the main constituent. The optimal kaolin ores to feed the processing plant should ideally have high kaolinite abundance, be free in Fe-bearing mineralogy (to avoid influence in the colour of the product), and the kaolinite itself should be of high crystallinity (to ensure the correct abrasiveness after calcination). This work presents a case study from the kaolin deposits in the St. Austell Granite (South-West England), which are known for their high quality and world-class size. In this area, the kaolin is of primary-hydrothermal origin, with mineral associations that are related to the genetic history. The eventual depletion of the high-quality reserves is bringing now the attention to the lower grade zones, where the amount of impurities increases. As a consequence, it is critical to developing strategies that ensure the supply of high-quality ore to the processing plant. For this, it is necessary to acquire a thorough knowledge of the ore, including relative abundance of the minerals and their textural relationships. Hyperspectral images in the visible-near infrared (VNIR) and short-wave infrared (SWIR) ranges were collected from drill cores and run-off-mine (ROM) samples, obtained from one of the kaolin pits in the St. Austell area, where the kaolin quality is known to be lower than in the rest of the deposit. A series of mineral maps were generated to assess the distribution, texture and abundance of the Fe-bearing mineralogy and the other kaolin-associated minerals, as well as the variations in the crystallinity of kaolinite. The mineral maps enabled the

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.

Synthesis of zeolites Na-A and Na-X from tablet compressed and calcinated coal fly ash

NASA Astrophysics Data System (ADS)

Hu, Tao; Gao, Wenyan; Liu, Xin; Zhang, Yifu; Meng, Changgong

2017-10-01

Zeolites Na-A and Na-X are important synthetic zeolites widely used for separation and adsorption in industry. It is of great significance to develop energy-efficient routines that can synthesize zeolites Na-A and Na-X from low-cost raw materials. Coal fly ash (CFA) is the major residue from the combustion of coal and biomass containing more than 85% SiO2 and Al2O3, which can readily replace the conventionally used sodium silicate and aluminate for zeolite synthesis. We used Na2CO3 to replace the expensive NaOH used for the calcination of CFA and showed that tablet compression can enhance the contact with Na2CO3 for the activation of CFA through calcination for the synthesis of zeolites Na-A and Na-X under mild conditions. We optimized the control variables for zeolite synthesis and showed that phase-pure zeolite Na-A can be synthesized with CFA at reactant molar ratio, hydrothermal reaction temperature and reaction time of 1.3Na2O: 0.6Al2O3: 1SiO2: 38H2O at 80°C for 6 h, respectively, while phase-pure zeolite Na-X can be synthesized at 2.2Na2O: 0.2Al2O3: 1SiO2: 88H2O at 100°C for 8 h, respectively. The composition, morphology, specific surface area, vibration spectrum and thermogravimetry of synthesized Na-A and Na-X were further characterized.

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.

Calcinated egg shell as a candidate of biosecurity enhancement material

PubMed Central

OTA, Mari; TOYOFUKU, Chiharu; THAMMAKARN, Chanathip; SANGSRIRATANAKUL, Natthanan; YAMADA, Masashi; NAKAJIMA, Katsuhiro; KITAZAWA, Minori; HAKIM, Hakimullah; ALAM, Md. Shahin; SHOHAM, Dany; TAKEHARA, Kazuaki

2016-01-01

Calcinated egg shell (Egg-CaO), of which the main component is calcium oxide, was evaluated in the forms of powder and aqueous solutions for their efficacies as disinfectants against avian influenza virus (AIV), Newcastle disease virus (NDV), infectious bursal disease virus (IBDV), Salmonella Infantis and Escherichia coli. Egg-CaO powder inactivated these viruses within 3 min in the presence of 33% of fetal bovine serum (FBS). In Egg-CaO solutions, except AIV, all pathogens were inactivated within 1 hr, even in the presence of 5% of FBS. Without FBS, all pathogens, except AIV, were inactivated within 3 min, and AIV within 1 hr. In addition, persistence of virucidal activity against AIV and NDV of Egg-CaO powder was confirmed after exposure to sunlight for 2 weeks or resuspension with water for 7 times, simulating field harsh environments. Chick growth test was conducted to ensure the safety of the use of Egg-CaO powder in chicken cages and showed that it is safe to add Egg-CaO in litter or feed. In conclusion, Egg-CaO can be useful for the enhancement of biosecurity at farms. PMID:26854110

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.

Experimental study of the combined calcination and hydrodesulfurization of high-sulfur green petroleum coke

NASA Astrophysics Data System (ADS)

Kilic, Saliha Meltem

The primary production of aluminum is done by means of the Hall-Heroult process where large amounts of carbon anodes are required and consumed. The quality of carbon anodes used in electrolysis is one of the most important parameters affecting the production of primary aluminum. The anode quality widely depends on the raw materials, one of which is the petroleum coke. Green petroleum coke is produced from the heavy residual fractions of petroleum. Petroleum cokes produced from sour crude oil sources contain high quantity of sulfur. A certain level of sulfur is needed to reduce the anode reactivities; however, the demand for anode-grade coke with acceptable sulfur content is increasing faster than the available supply. High sulfur levels in carbon anodes would have an adverse effect on environment; hence, the desulfurization of high sulfur green petroleum cokes is necessary. There are different ways of desulfurizing green petroleum cokes: solvent extraction, thermal desulfurization, and hydrodesulfurization. Coke produced by solvent extraction is prone to contamination. The thermal approach requires greater energy consumption and causes an increase in coke porosity. The global objective of this master project is to find an alternative solution for desulfurization that will produce quality calcined coke with minimum impact on environment. Hydrodesulfurization seems to be a viable option and was investigated in this study. Water was used for the hydrodesulfurization of commercially available high sulfur green petroleum coke. Different experimental systems were tried during the hydrodesulfurization experiments. A systematic approach was used to investigate the influence of hydrodesulfurization parameters including water injection temperature, duration, and water flow rate as well as coke particle size on the hydrodesulfurization of green petroleum coke. In addition to hydrodesulfurization, a number of thermal desulfurization experiments were carried out with the same

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.

Enhanced removal of natural organic matters by calcined Mg/Al layered double hydroxide nanocrystalline particles: Adsorption, reusability and mechanism studies

NASA Astrophysics Data System (ADS)

Fang, Liping; Hou, Jingwei; Xu, Cuihong; Wang, Yaru; Li, Ji; Xiao, Feng; Wang, Dongsheng

2018-06-01

Natural organic matters (NOMs) can generate disinfection by-products during water treatment process, threatening to human health. However, the removal of NOM is still unsatisfactory in water treatment. Hence, this work investigated the removal efficiency of humic and fulvic acids (HA and FA) by layered double hydroxide (LDH) and its calcined forms under different conditions. Our results show that calcination of LDH at 500 °C can effectively enhance the NOM removal with adsorption capacities of 98.8 mg/g for HA and 97.6 mg/g for FA at pH 9.5. The removal efficiency of HA and FA notably increases by decreasing pH. The presence of SO42- and CO32- significantly suppresses the removal of HA or FA by CLDHs. The release of Al from LDH and CLDH is negligible and safe to aquatic organisms at pH > 6.5. Moreover, CLDH shows a good reusability for NOM removal in water treatment. The removal of HA and FA by CLDH is governed through electrostatic interactions and intercalation into the interlayers of LDH was not observed. Fluorescence and molecular weight analyses show that the microbial by-products with mid-molecular weight are more difficult to be removed than HA and FA. This study provides a new insight into the NOM removal using LDH and CLDH.

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.

Well-crystallized mesoporous TiO2 shells for enhanced photocatalytic activity: prepared by carbon coating and silica-protected calcination.

PubMed

Zhang, Zewu; Zhou, Yuming; Zhang, Yiwei; Zhou, Shijian; Shi, Junjun; Kong, Jie; Zhang, Sicheng

2013-04-14

Mesoporous anatase-phase TiO2 hollow shells were successfully fabricated by the solvothermal and calcination process. This method involves preparation of SiO2@TiO2 core-shell colloidal templates, sequential deposition of carbon and then silica layers through solvothermal and sol-gel processes, crystallization of TiO2 by calcination and finally removal of the inner and outer silica to produce hollow anatase TiO2 shells. The prepared samples were characterized by transmission electron microscopy, X-ray diffraction, N2 adsorption-desorption isotherms and UV-vis absorption spectroscopy. The results show that a uniform carbon layer is coated on the core-shell particles through the solvothermal process. The combustion of carbon offers the space for the TiO2 to further grow into large crystal grains, and the outer silica layer serves as a barrier against the excessive growth of anatase TiO2 nanocrystals. Furthermore, the initial crystallization of TiO2 generated in the carbon coating step and the heat generated by the combustion of the carbon layer allow the crystallization of TiO2 at a relatively low temperature without changing the uniform structure. When used as photocatalysts for the oxidation decomposition of Rhodamine B in aqueous solution under UV irradiation, the hollow TiO2 shells showed enhanced catalytic activity. Moreover, the TiO2 hollow shells prepared with optimal crystallinity by this method showed a higher performance than commercial P25 TiO2.

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.

Thermophilic bio-hydrogen production from corn-bran residue pretreated by calcined-lime mud from papermaking process.

PubMed

Zhang, Jishi; Zhang, Junjie; Zang, Lihua

2015-12-01

This study investigated the use of calcined-lime mud from papermaking process (CLMP) pretreatment to improve fermentative hydrogen yields from corn-bran residue (CBR). CBR samples were pretreated with different concentrations (0-15 g/L) of CLMP at 55°C for 48 h, prior to the thermophilic fermentation with heat-treated anaerobic sludge inoculum. The maximum hydrogen yield (MHY) of 338.91 ml/g-VS was produced from the CBR pretreated with 10 g/L CLMP, with the corresponding lag-phase time of 8.24h. Hydrogen yield increments increased from 27.76% to 48.07%, compared to the control. The CLMP hydrolyzed more cellulose, which provided adequate substrates for hydrogen production. Copyright © 2015 Elsevier Ltd. All rights reserved.

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.

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

Alizarin red S dye removal from contaminated water on calcined [Mg/Al, Zn/Al and MgZn/Al]-LDH

NASA Astrophysics Data System (ADS)

Aissat, Miloud; Hamouda, Sara; Benhadria, Naceur; Chellali, Rachid; Bettahar, Noureddine

2018-05-01

The waste water rejected by the textile industries is loaded with organic dyes, responsible for the high color present in the effluents. Some dyes and / or their degradation products could be carcinogenic and may have mutagenic properties. The rapid growth of the global economy has caused many environmental problems with a huge pollution problem. The abuse use of chemicals product is an environmental toxicological problem. The consequences can be serious for water resources. In this perspective, our study comes to participate with new means of depollution using new materials with interesting properties in the treatment of pollution. Among these materials, LDHs whose synthesis is easy and inexpensive can be a tool in the treatment of water Polluted [1]. Our contribution consists in using HDL as a means of sorption of dyes which are considered as polluting agents of waters especially for the industry textile. This study considers the removal of the Alizarine Red S (AR) from water on calcined MgAl,ZnAL and MgZnAL-layered double hydroxides. The different LDH was prepared by copreprecipation method. The materials was obtained for molar ratios R =2 for the different LDH. The carbonated layered Calcination of these solids leads to the formation of mixed oxides which have the property of being able to be regenerated by adsorbing new anionic entities. Adsorbents and adsorption products were characterized by physicochemical techniques. The structural characterization of the material was carried out by X-ray diffraction, infrared spectroscopy (FTIR). Dosages of the polluted solutions were monitored by UV-Visible spectrometry.

Enhanced Removal of Arsenic and Antimony in the Mining Site by Calcined γ-Fe2O3/Layered Double Hydroxide Nanocomposite

NASA Astrophysics Data System (ADS)

Lee, Sang-Ho; Choi, Heechul; Kim, Kyoung-Woong

2016-04-01

Arsenic (As) and Antimony (Sb) have been recognized as harmful contaminants in aquatic environment due to its high toxicity and carcinogenicity. Especially, the contamination of arsenic in the mining areas is considered as a serious emerging environmental issue in Korea. Due to the hazardous effect of arsenic, the United States Environmental Protection Agency (US EPA) regulated maximum contamination level of arsenic to 10 μg/L in drinking water. The harmful effect on human health by excessive intake of antimony was also reported by previous studies, and severe contamination level (100 - 7,000 μg/L) of antimony reported in surface and groundwater of abandoned mining area in China and Slovakia. Therefore, US EPA regulated maximum contaminants level of antimony in drinking water to 6 μg/L. In order to remove anionic contaminants in drinking water, various type of nanomaterials have been developed. Layered double hydroxide (LDH) is the artificial anionic clay that is based on the layered structure of positively charged brucite-like layers with interlayers of anions. The LDH is one of the promising nanomaterials for the removal of anionic contaminants because it has high selectivity for arsenic, phosphate, chromium and antimony. However, the biggest problem of LDH for wastewater treatment is that the particles cannot be easily separated after the removal of contaminants. In this study, magnetic nanoparticles (γ-Fe2O3) supported LDH nanocomposite (γ-Fe2O3/LDH) was investigated to enhance magnetic particle recovery and removal efficiency for arsenic and antimony. The calcined γ-Fe2O3/LDH nanocomposites synthesized by co-precipitation method, and the crystallographic properties of maghemite (γ-Fe2O3) and layered structure of LDH were confirmed by X-ray diffraction. The nano-sized γ-Fe2O3 (30 to 50 nm) was stably attached on the surface of LDH (100 to 150 nm) and O1s spectrum by X-ray photoelectron spectroscopy (XPS) explained that there are both physical and

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

In situ fabrication of ZnO@N-doped nanoporous carbon core-shell heterostructures with high photocatalytic and adsorption capacity by a calcination of ZnO@MOF strategy

NASA Astrophysics Data System (ADS)

Qi, Qi; Liu, Sujuan; Li, Xing; Kong, Chunlong; Guo, Zhiyong; Chen, Liang

2017-11-01

This report describes the controllable encapsulation of ZnO nanoparticles with N-doped nanoporous carbon (N-NpC) via a simple fabrication and calcination of ZnO@ZIF-8 (zeolitic imidazolate framework). In the fabrication of ZnO@ZIF-8, ZnO was used both as the support and Zn source for the formation of ZIF-8. After calcination under N2 atmosphere, the ZnO@N-NpC core-shell heterostructures were formed and characterized by IR, UV-vis, XRD, XPS, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). As expected, the well-defined ZnO@N-NpC core-shell nanospheres demonstrated distinct photocatalytic activity and adsorption capacity in response to the dye methylene blue (MB) in aqueous solution, and the degradation efficiency of MB is up to 99% under UV irradiation for 20 min after catalysts were reused for 5 cycles and stored for two months. Therefore, it is reasonable to believe that the ZnO@N-NpC core-shell heterostructures are new-type nanomaterials for photodegradation of the organic pollutants from wastewater.

Efficacy of chlorine and calcinated calcium treatment of alfalfa seeds and sprouts to eliminate Salmonella.

PubMed

Gandhi, Megha; Matthews, Karl R

2003-11-01

The efficacy of a 20,000 ppm calcium hypochlorite treatment of alfalfa seeds artificially contaminated with Salmonella was studied. Salmonella populations reached >7.0 log on sprouts grown from seeds artificially contaminated with Salmonella and then treated with 20,000 ppm Ca(OCl)(2). The efficacy of spray application of chlorine (100 ppm) to eliminate Salmonella during germination and growth of alfalfa was assessed. Alfalfa seed artificially contaminated with Salmonella was treated at germination, on day 2 or day 4, or for the duration of the growth period. Spray application of 100 ppm chlorine at germination, day 2, or day 4 of growth was minimally effective resulting in approximately a 0.5-log decrease in population of Salmonella. Treatment on each of the 4 days of growth reduced populations of Salmonella by only 1.5 log. Combined treatment of seeds with 20,000 ppm Ca(OCl)(2) and followed by 100 ppm chlorine or calcinated calcium during germination and sprout growth did not eliminate Salmonella.

Behavior of radioactive iodine and technetium in the spray calcination of high-level waste

NASA Astrophysics Data System (ADS)

Knox, C. A.; Farnsworth, R. K.

1981-08-01

The Remote Laboratory-Scale Waste Treatment Facility (RLSWTF) was designed and built as a part of the High-Level Waste Immobilization Program (now the High-Level Waste Process Development Program) at the Pacific Northwest Laboratory. In facility, installed in a radiochemical cell, is described in which installed in a radiochemical cell is described in which small volumes of radioactive liquid wastes can be solidified, the process off gas can be analyzed, and the methods for decontaminating this off gas can be tested. During the spray calcination of commercial high-level liquid waste spiked with Tc-99 and I-131 and 31 wt% loss of I-131 past the sintered-metal filters. These filters and venturi scrubber were very efficient in removing particulates and Tc-99 from the the off-gas stream. Liquid scrubbers were not efficient in removing I-131 as 25% of the total lost went to the building off-gas system. Therefore, solid adsorbents are needed to remove iodine. For all future operations where iodine is present, a silver zeolite adsorber is to be used.

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".

An acetylcholinesterase biosensor based on graphene-gold nanocomposite and calcined layered double hydroxide.

PubMed

Zhai, Chen; Guo, Yemin; Sun, Xia; Zheng, Yuhe; Wang, Xiangyou

2014-05-10

In this study, a novel acetylcholinesterase-based biosensor was fabricated. Acetylcholinesterase (AChE) was immobilized onto a glassy carbon electrode (GCE) with the aid of Cu-Mg-Al calcined layered double hydroxide (CLDH). CLDH can provide a bigger effective surface area for AChE loading, which could improve the precision and stability of AChE biosensor. However, the poor electroconductibility of CLDHs could lead to the low sensitivity of AChE biosensor. In order to effectively compensate the disadvantages of CLDHs, graphene-gold nanocomposites were used for improving the electron transfer rate. Thus, the graphene-gold nanocomposite (GN-AuNPs) was firstly modified onto the GCE, and then the prepared CLDH-AChE composite was immobilized onto the modified GCE to construct a sensitive AChE biosensor for pesticides detection. Relevant parameters were studied in detail and optimized, including the pH of the acetylthiocholine chloride (ATCl) solution, the amount of AChE immobilized on the biosensor and the inhibition time governing the analytical performance of the biosensor. The biosensor detected chlorpyrifos at concentrations ranging from 0.05 to 150μg/L. The detection limit for chlorpyrifos was 0.05μg/L. Copyright © 2014 Elsevier Inc. 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.

Tuning the porosity of mesoporous NiO through calcining isostructural Ni-MOFs toward supercapacitor applications

NASA Astrophysics Data System (ADS)

Hou, Xiang-Yang; Yan, Xiao-Li; Wang, Xiao; Zhai, Quan-Guo

2018-07-01

NiO has an unusually high theoretical specific capacitance and possess relatively high electrical conductivity compared to other metal oxides. However, the reported specific capacitance of the NiO-based electrodes is far below the theoretical value up to now. In this paper, three porous NiO materials with different specific surface area were synthesized simply by calcining iso-structural Ni-based MOFs templates. The formation mechanism of NiO was discussed by taking into account the thermal behavior and intrinsic structural features of the Ni-MOFs. Taking advantages of the Ni-MOFs precursors, all prepared NiO compounds are mesoporous and their porosity can be tuned by the structure of MOFs. Specially, due to the high porosity, three NiO exhibited an improved electrochemical performance and the specific discharge capacitances are of 102, 105, and 116 F g-1 at the current density of 1 A g-1, respectively. The specific capacitance of 1-NiO-450 is approximately 93.2% of its maximum value after 3000 cycles, which obviously superior to most of the previously reported NiO electrode materials and suggests their promising applications in supercapacitors.

Evolution of porous structure and texture in nanoporous SiO2/Al2O3 materials during calcination

NASA Astrophysics Data System (ADS)

Glazkova, Elena A.; Bakina, Olga V.

2016-11-01

The study focuses on the evolution of porous structure and texture of silica/alumina xerogels during calcination in the temperature range from 500 to 1200°C. The xerogel was prepared via sol-gel method using subcritical drying. The silica/alumina xerogels were examined using transmission electron microscopy-energy dispersive spectroscopy (TEM-EDS), Brunauer Emmett Teller-Barrett Joyner Halenda (BET-BJH), differential scanning calorimetry (DSC), and Fourier transform infrared (FTIR) spectroscopy. SiO2 primary particles of size about 10 nm are connected with each other to form a porous xerogel structure. Alumina is uniformly distributed over the xerogel volume. The changes of textural characteristics under heat treatment of samples are radical; the specific surface area and pore size attain their maximum at 500-700°C. The heat treatment of samples causes dehydroxylation of the xerogel surface, and at 1200°C the sample is sintered, loses mesoporosity, and its specific surface area reduces considerably down to 78 m2/g.

Surface modification of calcined kaolin with toluene diisocyanate based on high energy ball milling

NASA Astrophysics Data System (ADS)

Yuan, Yongbing; Chen, Hongling; Lin, Jinbin; Ji, Yan

2013-11-01

The surface of calcined kaolin particle was modified with toluene diisocyanate (TDI) by using high energy ball milling. The prepared hybrids were characterized by FT-IR, MAS NMR, thermal analysis (TGA-DSC), static water contact angle (CA), apparent viscosity and transmission electron microscopy (TEM). FT-IR and MAS NMR spectra demonstrated that TDI molecules were chemically anchored to kaolin surface after modification. The results of thermal analysis showed that the maximum grafting ratio reached up to 446.61% when the mass ratio of TDI/kaolin was 0.5:1.0, and CA measurements revealed that the resultant hybrids exhibited strong hydrophobicity (148.82°). Apparent viscosity and TEM were employed to examine the dispersion properties of blank and modified kaolin particles in poly (dimenthylsiloxane) matrix. The results illustrated that the dispersion stability depended strongly on the grafting ratio of TDI, neither too low nor too high achieved uniform and stable dispersion, and the favorable grafting ratio was obtained when the mass ratio of TDI/kaolin was 0.2:1.0. Further modification of TDI/kaolin (mass ration of TDI/kaolin, 1.0:1.0) particles with bis(aminopropyl)-terminated-poly(dimethylsiloxane) (APS) was also investigated. TEM evidenced that the dispersion properties of the obtained TDI/APS/kaolin particles were remarkably improved in octamethyl cyclotetrasiloxane compared with the original TDI/kaolin particles.

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.

Regeneration of Waste Edible Oil by the Use of Virgin and Calcined Magnesium Hydroxide as Adsorbents.

PubMed

Ogata, Fumihiko; Kawasaki, Naohito

2016-01-01

In this study, we prepared virgin (S, L) and calcined (S-380, S-1000, L-380, L-1000) magnesium hydroxide for regeneration of waste edible oil. Deterioration of soybean oil, rapeseed oil, and olive oil was achieved by heat and aeration treatment. The properties of the different adsorbents were investigated using specific surface area measurements, scanning electron microscopy, X-ray diffraction analysis, thermogravimetric-differential thermal analysis, and surface pH measurement. Moreover, the relationship between the changes in acid value (AV) and carbonyl value (CV) and the adsorbent properties were evaluated. The specific surface areas of S-380 and L-380 were greater than that of other adsorbents. In addition, the XRD results show that S-380 and L-380 contain both magnesium hydroxide and magnesium oxide structures. The decreases in AV and CV using S-380 and L-380 were greater than achieved using other adsorbents. The correlation coefficients between the decrease in AV and CV and specific surface area were 0.947 for soybean oil, 0.649 for rapeseed oil, and 0.773 for olive oil, respectively. The results obtained in this study suggest that a physical property of the adsorbent, namely specific surface area, was primarily responsible for the observed decreases in AV and CV. Overall, the results suggest that S-380 and L-380 are useful for the regeneration of waste edible oil.

Luminescence properties and color identification of Eu doped Ca3(PO4)2 phosphors calcined in air

NASA Astrophysics Data System (ADS)

Tong, Chao; Zhu, Yangguang; Xu, Chuanyan; Yang, Lei; Li, Yadong

2017-09-01

The Ca3(PO4)2：Eu (TCP) phosphor was synthesized by a high-temperature solid-state reaction in air atmosphere. X-ray powder diffraction(XRD) analysis indicates that the α-TCP↔β-TCP phase transition takes place under different calcination and cooling conditions. The luminescence properties of the two different phases of TCP were discussed according to the luminescence spectra during the heating and cooling transition. The CIE chromaticity coordinates of β-TCP phase located at the red region, α-TCP phase at bluish-green region because of the coexistence of Eu2+ and Eu3+ ions. The color-tunable emission of the products could also be directly observed under UV lamp. Pure red and bluish-green-emitting particles were observed respectively for the pure β-TCP phase and α-TCP phase samples whereas bluish-green and red mixture emitting particles were traced for the α-TCP /β-TCP phase co-existence samples. Therefore, results of this study suggested that Eu ion could be used as a spectroscopic probe to qualitatively identify the crystalline phase of TCP by a simple and convenient way to observe the color-tunable emission of the samples when irradiating it under 365 nm UV lamp.

Characterizing the correlation between dephosphorization and solution pH in a calcined water treatment plant sludge.

PubMed

Zhou, Zhenming; Liu, Qidi; Li, Shuwen; Li, Fei; Zou, Jing; Liao, Xiaobin; Yuan, Baoling; Sun, Wenjie

2018-04-26

This study focused on characterizing the correlation between the dephosphorization process of calcined water treatment plant sludge (C-WTPS) and the solution initial pH in batch experiments. The specific aim was to illustrate the effect of different initial pH on the adsorption and desorption of phosphorous in C-WTPS. In addition, the effects of solution initial pH on the release of ammonia nitrogen and total organic carbon (TOC) from C-WTPS and the change of pH after adsorption were also investigated. The results demonstrated that the initial pH significantly influenced the adsorption of phosphorus on C-WTPS. When initial pH was increased from 3 to 10, the phosphorous absorption capacity reduced by 76.5%. Especially, when the initial pH reached to 11, the phosphorus adsorption capacity became a negative value, indicating that C-WTPS released phosphorus into the solution. The addition of C-WTPS to the solution had little impact on the initial pH of the solution. The absorbed phosphorous on C-WTPS was relatively stable in the pH range of 3 to 10. Nevertheless, when the solution pH was higher than 11, it can be easily released into the solution. Furthermore, by comparison with WTPS, C-WTPS released less ammonia nitrogen and TOC into the solution and adsorbed more phosphorus from the solution in the experimental pH range. Therefore, C-WTPS is more suitable to serve as a cost-effective sorbent for phosphorus removal.

Semiconducting and quartz microbalance (QCM) humidity sensor properties of TiO2 by sol gel calcination method

NASA Astrophysics Data System (ADS)

Yakuphanoglu, Fahrettin

2012-06-01

Titanium dioxide (TiO2) material was synthesized using the sol gel calcination method. The structural properties of the TiO2 semiconductor were investigated by atomic force microscopy. The electrical conductivity of the TiO2 was measured as a function of temperature and TiO2 exhibits a conductivity of 2.55 × 10-6 S/m at room temperature with activation energy of 104 meV. The electrical conductivity of the TiO2 at room temperature is higher than that of nanocrystalline TiO2 (3 × 10-7 S/m) and TiO2 thin film in air (5 × 10-9 S/m) and in vacuum (8.8 × 10-10 S/m). It was found that the electrical transport mechanism of the TiO2 is controlled by thermally activated mechanism. The optical band gap of the TiO2 powder sample was determined to be 3.17 eV, which is good in agreement with the bulk TiO2 (Eg = 3.2 eV). Up to our knowledge, there is no any reported data about the band gap of TiO2 nanopowder based on the diffused reflectance calculation. Quartz crystal microbalance (QCM) TiO2 humidity sensor was prepared. The sensor indicates a large frequency change with an interaction occurred between TiO2 and humidity molecules. The sensor exhibits a good repeatability when it was exposed to the moist air of 65% RH.

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.

Morphology and structure features of ZnAl{sub 2}O{sub 4} spinel nanoparticles prepared by matrix-isolation-assisted calcination

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

Du, Xuelian, E-mail: xueliandu@126.com; Li, Liqiang; Zhang, Wenxing

2015-01-15

Graphical abstract: The substrate ZnO as the isolation medium is effective in preventing the sintering and agglomeration of ZnAl{sub 2}O{sub 4} nanoparticles, and it also prevents their contamination. High purity, well-dispersed, and single-crystal ZnAl{sub 2}O{sub 4} nanoparticles with 3.72 eV band gap were obtained. - Abstract: Well-dispersed ZnAl{sub 2}O{sub 4} spinel nanoparticles with an average crystalline size of 25.7 nm were synthesized successfully and easily by polymer-network and matrix-isolation-assisted calcination. The product microstructure and features were investigated by X-ray diffractometry, thermogravimetric and differential thermal analysis, Fourier transform-infrared spectroscopy, N{sub 2} adsorption–desorption isotherms, and energy dispersive X-ray spectra. The morphology andmore » optical performance of the as-prepared ZnAl{sub 2}O{sub 4} nanoparticles were characterized by scanning electron microscope, transmission electron microscopy, and photoluminescence spectrometer. Experimental results indicate that excess ZnO acted as the isolation medium is effective in preventing the sintering and agglomeration of ZnAl{sub 2}O{sub 4} nanoparticles, and it also prevents their contamination. Then, high purity and well-dispersed ZnAl{sub 2}O{sub 4} nanoparticles with single-crystal structure were obtained.« less

Micro-structural characterization of the hydration products of bauxite-calcination-method red mud-coal gangue based cementitious materials.

PubMed

Liu, Xiaoming; Zhang, Na; Yao, Yuan; Sun, Henghu; Feng, Huan

2013-11-15

In this research, the micro-structural characterization of the hydration products of red mud-coal gangue based cementitious materials has been investigated through SEM-EDS, (27)Al MAS NMR and (29)Si MAS NMR techniques, in which the used red mud was derived from the bauxite calcination method. The results show that the red mud-coal gangue based cementitious materials mainly form fibrous C-A-S-H gel, needle-shaped/rod-like AFt in the early hydration period. With increasing of the hydration period, densification of the pastes were promoted resulting in the development of strength. EDS analysis shows that with the Ca/Si of red mud-coal gangue based cementitious materials increases, the average Ca/Si and Ca/(Si+Al) atomic ratio of C-A-S-H gel increases, while the average Al/Si atomic ratio of C-A-S-H gel decreases. MAS NMR analysis reveals that Al in the hydration products of red mud-coal gangue based cementitious materials exists in the forms of Al(IV) and Al(VI), but mainly in the form of Al(VI). Increasing the Ca/Si ratio of raw material promotes the conversion of [AlO4] to [AlO6] and inhibits the combination between [AlO4] and [SiO4] to form C-A-S-H gel. Meanwhile, the polymerization degree of [SiO4] in the hydration products declines. Published by Elsevier B.V.

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.

Calcination Method Synthesis of SnO2/g-C3N4 Composites for a High-Performance Ethanol Gas Sensing Application

PubMed Central

Cao, Jianliang; Qin, Cong; Wang, Yan; Zhang, Bo; Gong, Yuxiao; Zhang, Huoli; Sun, Guang; Bala, Hari; Zhang, Zhanying

2017-01-01

The SnO2/g-C3N4 composites were synthesized via a facile calcination method by using SnCl4·5H2O and urea as the precursor. The structure and morphology of the as-synthesized composites were characterized by the techniques of X-ray diffraction (XRD), the field-emission scanning electron microscopy and transmission electron microscopy (SEM and TEM), energy dispersive spectrometry (EDS), thermal gravity and differential thermal analysis (TG-DTA), and N2-sorption. The analysis results indicated that the as-synthesized samples possess the two dimensional structure. Additionally, the SnO2 nanoparticles were highly dispersed on the surface of the g-C3N4nanosheets. The gas-sensing performance of the as-synthesized composites for different gases was tested. Moreover, the composite with 7 wt % g-C3N4 content (SnO2/g-C3N4-7) SnO2/g-C3N4-7 exhibits an admirable gas-sensing property to ethanol, which possesses a higher response and better selectivity than that of the pure SnO2-based sensor. The high surface area of the SnO2/g-C3N4 composite and the good electronic characteristics of the two dimensional graphitic carbon nitride are in favor of the elevated gas-sensing property. PMID:28468245

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

Stabilization of Pb²⁺ and Cu²⁺ contaminated firing range soil using calcined oyster shells and waste cow bones.

PubMed

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

2013-05-01

Pb(2+) and Cu(2+) contamination at army firing ranges poses serious environmental and health risks to nearby communities necessitating an immediate and prompt remedial action. In this study, a novel mixture of calcined oyster shells (COSs) and waste cow bones (WCBs) was utilized to immobilize Pb(2+) and Cu(2+) in army firing range soils. The effectiveness of the treatment was evaluated based on the Korean Standard leaching test. The treatment results showed that Pb(2+) and Cu(2+) immobilization in the army firing range soil was effective in significantly reducing Pb(2+) and Cu(2+) leachability upon the combined treatment with COS and WCB. A drastic reduction in Pb(2+) (99%) and Cu(2+) leachability (95%) was obtained as compared to the control sample, upon treatment with 5 wt.% COS and 5 wt.% WCB. The combination treatment of COS and WCB was more effective for Pb immobilization, than the treatment with COS or WCB alone. The 5 wt.% COS alone treatment resulted in 95% reduction in Cu(2+) leachability. The SEM-EDX results suggested that Pb(2+) and Cu(2+) immobilization was most probably associated with the formation of ettringite, pozzolanic reaction products and pyromorphite-like phases at the same time. Copyright © 2013 Elsevier Ltd. 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...

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.

An ingenious strategy of preparing TiO2/g-C3N4 heterojunction photocatalyst: In situ growth of TiO2 nanocrystals on g-C3N4 nanosheets via impregnation-calcination method

NASA Astrophysics Data System (ADS)

Zhang, Guanghui; Zhang, Tianyong; Li, Bin; Jiang, Shuang; Zhang, Xia; Hai, Li; Chen, Xingwei; Wu, Wubin

2018-03-01

An ingenious method was employed to design and fabricate the TiO2/g-C3N4 heterojunction photocatalysts in this study. The thermal oxidation etching of g-C3N4 nanosheets and the in situ growth of TiO2 nanocrystal on the surface of g-C3N4 nanosheets were completed simultaneously by the calcination process. The g-C3N4 nanosheets played a crucial role in regulating and assembling the structures and morphologies of TiO2. Furthermore, the thickness and content of g-C3N4, and the crystallinity of TiO2 in TiO2/g-C3N4 composites could be regulated and controlled by the calcination temperature. Among the resultant TiO2/g-C3N4 samples, the TiO2/g-C3N4 sample with 41.6 wt% g-C3N4 exhibited the highest photocatalytic activity. It could degrade almost all MO molecules under visible light irradiation within 3 h. Moreover, it displayed higher visible light photocatalytic performance for degrading MO solution than pure g-C3N4 and D-TiO2. The synergistic effect between TiO2 and g-C3N4 makes significant contributions to the enhancement of the visible light photocatalytic activity. In addition, the favorable photocatalytic performance of TiO2/g-C3N4 nanocomposites is also attributed to the porous structures and uniform morphologies, and large surface area. Furthermore, the resultant TiO2/g-C3N4 exhibits excellent photocatalytic stability. Radical trapping experiments indicated that rad O2- and h+ were the main reactive species during the photodegradation process under visible light irradiation. Hopefully, the results can offer new design and strategy for preparing other g-C3N4-based nanocomposites for environmental and energy applications.

Transition metal modified and partially calcined inorganic-organic pillared clays for the adsorption of salicylic acid, clofibric acid, carbamazepine, and caffeine from water.

PubMed

Cabrera-Lafaurie, Wilman A; Román, Félix R; Hernández-Maldonado, Arturo J

2012-11-15

Pharmaceutical and Personal Care Products (PPCPs) are considered emerging contaminants, and their efficient removal from water is going to be a challenging endeavor. Microporous adsorbent materials, including pillared clays, could offer a potential solution if tailored properly. Although pillared clays have been employed previously for the removal of organics, the effective removal of PPCPs will only be possible if their surface and textural properties are manipulated from the bottom-up. This work presents the use of modified inorganic-organic pillared clays (IOCs) for the adsorption of salicylic acid, clofibric acid, carbamazepine, and caffeine. The IOCs have been modified with Co(2+), Cu(2+), or Ni(2+) to induce complexation-like adsorbate-adsorbent interactions at ambient conditions, in an attempt to provide an efficient and yet reversible driving force in the sub-ppm concentration range. Furthermore, the IOCs were partially calcined to increase effective surface area by an order of magnitude while preserving some hydrophobicity. In general, the Ni(2+) IOCs exhibited the greatest interaction with salicylic and clofibric acids, respectively, while the Co(2+) adsorbents excelled at adsorbing caffeine at low concentrations. All of the metal-modified IOCs showed comparable adsorption capacities for the case of carbamazepine, probably due to the lack of availability of particular functional groups in this adsorbate. Copyright © 2012 Elsevier Inc. All rights reserved.

Impact of natural and calcined starfish (Asterina pectinifera) on the stabilization of Pb, Zn and As in contaminated agricultural soil.

PubMed

Lim, Jung Eun; Sung, Jwa Kyung; Sarkar, Binoy; Wang, Hailong; Hashimoto, Yohey; Tsang, Daniel C W; Ok, Yong Sik

2017-04-01

Metal stabilization using soil amendments is an extensively applied, economically viable and environmentally friendly remediation technique. The stabilization of Pb, Zn and As in contaminated soils was evaluated using natural starfish (NSF) and calcined starfish (CSF) wastes at different application rates (0, 2.5, 5.0 and 10.0 wt%). An incubation study was conducted over 14 months, and the efficiency of stabilization for Pb, Zn and As in soil was evaluated by the toxicity characteristic leaching procedure (TCLP) test. The TCLP-extractable Pb was reduced by 76.3-100 and 91.2-100 % in soil treated with NSF and CSF, respectively. The TCLP-extractable Zn was also reduced by 89.8-100 and 93.2-100 % in soil treated with NSF and CSF, respectively. These reductions could be associated with the increased metal adsorption and the formation of insoluble metal precipitates due to increased soil pH following application of the amendments. However, the TCLP-extractable As was increased in the soil treated with NSF, possibly due to the competitive adsorption of phosphorous. In contrast, the TCLP-extractable As in the 10 % CSF treatment was not detectable because insoluble Ca-As compounds might be formed at high pH values. Thermodynamic modeling by visual MINTEQ predicted the formation of ettringite (Ca 6 Al 2 (SO 4 ) 3 (OH) 12 ·26H 2 O) and portlandite (Ca(OH) 2 ) in the 10 % CSF-treated soil, while SEM-EDS analysis confirmed the needle-like structure of ettringite in which Pb was incorporated and stabilized in the 10 % CSF treatment.

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

Reduction of Acute Inflammatory Effects of Fumed Silica Nanoparticles in the Lung by Adjusting Silanol Display through Calcination and Metal Doping

PubMed Central

Sun, Bingbing; Pokhrel, Suman; Dunphy, Darren R.; Zhang, Haiyuan; Ji, Zhaoxia; Wang, Xiang; Wang, Meiying; Liao, Yu-Pei; Chang, Chong Hyun; Dong, Juyao; Li, Ruibin; Mädler, Lutz; Brinker, C. Jeffrey; Nel, André E.; Xia, Tian

2015-01-01

The production of pyrogenic (fumed) silica is increasing worldwide at a 7% annual growth rate, including expanded use in food, pharmaceuticals and other industrial products. Synthetic amorphous silica, including fumed silica, has been generally recognized as safe (GRAS) for use in food products by the Food and Drug Administration (FDA). However, emerging evidence from experimental studies now suggests that fumed silica could be hazardous due to its siloxane ring structure, high silanol density, and “string-of-pearl-like” aggregate structure, which could combine to cause membrane disruption, generation of reactive oxygen species, pro-inflammatory effects, and liver fibrosis. Based on this structure-activity analysis (SAA), we investigated whether calcination and rehydration of fumed silica changes its hazard potential in the lung due to an effect on silanol density display. This analysis demonstrated that the accompanying change in surface reactivity could indeed impact cytokine production in macrophages and acute inflammation in the lung, in a manner that is dependent on siloxane ring reconstruction. Confirmation of this SAA in vivo, prompted us to consider safer design of fumed silica properties by titanium (Ti) and aluminum (Al) doping (0–7%), using flame spray pyrolysis (FSP). Detailed characterization revealed that increased Ti and Al doping could reduce surface silanol density and expression of three-membered siloxane rings, leading to dose-dependent reduction in hydroxyl radical generation, membrane perturbation, potassium efflux, NLRP3 inflammasome activation and cytotoxicity in THP-1 cells. The reduction of NLRP3 inflammasome activation was also confirmed in bone marrow-derived macrophages (BMDMs). Ti- and to a lesser extent Al-doping, also ameliorated acute pulmonary inflammation, demonstrating the possibility of a safer design approach for fumed silica, should that be required for specific use circumstances. PMID:26200133

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

Single and multi-component adsorption of salicylic acid, clofibric acid, carbamazepine and caffeine from water onto transition metal modified and partially calcined inorganic-organic pillared clay fixed beds.

PubMed

Cabrera-Lafaurie, Wilman A; Román, Félix R; Hernández-Maldonado, Arturo J

2015-01-23

Fixed-beds of transition metal (Co(2+), Ni(2+) or Cu(2+)) inorganic-organic pillared clays (IOCs) were prepared to study single- and multi-component non-equilibrium adsorption of a set of pharmaceutical and personal care products (PPCPs: salicylic acid, clofibric acid, carbamazepine and caffeine) from water. Adsorption capacities for single components revealed that the copper(II) IOCs have better affinity toward salicylic and clofibric acid. However, multi-component adsorption tests showed a considerable decrease in adsorption capacity for the acids and an unusual selectivity toward carbamazepine depending on the transition metal. This was attributed to a combination of competition between PPCPs for adsorption sites, adsorbate-adsorbate interactions, and plausible pore blocking caused by carbamazepine. The cobalt(II) IOC bed that was partially calcined to fractionate the surfactant moiety showcased the best selectivity toward caffeine, even during multi-component adsorption. This was due to a combination of a mildly hydrophobic surface and interaction between the PPCP and cobalt(II). In general, the tests suggest that these IOCs may be a potential solution for the removal of PPCPs if employed in a layered-bed configuration, to take care of families of adsorbates in a sequence that would produce sharpened concentration wavefronts. Copyright © 2014 Elsevier B.V. All rights reserved.

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

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.

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.

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

Cryolite process for the solidification of radioactive wastes

DOEpatents

Wielang, Joseph A.; Taylor, Larry L.

1976-01-01

An improved method is provided for solidifying liquid wastes containing significant quantities of sodium or sodium compounds by calcining in a fluidized-bed calciner. The formation of sodium nitrate which will cause agglomeration of the fluidized-bed particles is retarded by adding aluminum and a fluoride to the waste in order to produce cryolite during calcination. The off-gas of the calciner is scrubbed with a solution containing aluminum in order to complex any fluoride which may be liberated by subsequent dissolution of cryolite and prevent corrosion in the off-gas cleanup system.

Effect of thermal treatment on the nano-structure and phase transformation of metakaolin-based geopolymers.

PubMed

Kim, Yongsung; Kang, Seunggu

2014-11-01

Enhancement of the mechanical strength of metakaolin-based geopolymers activated with NaOH was attempted by calcining metakaolin at a higher temperature than that commonly reported. Increasing the calcination temperature from 750 degrees C to 1150 degrees C promoted the recrystallization of mullite. Two type of zeolite of sodium aluminum silicate hydrates were found in the geopolymers made of metakaolin calcined at 750 degrees C-1050 degrees C. The h-zeolite [Na6(AlSiO4)6 x H2O] was not found in the geopolymer made of metakaolin calcined above 900 degrees C, while Z-zeolite [Na2O x Al2O3 x SiO2 x H2O] remained in specimens calcined at up to 1050 degrees C, All zeolite disappeared above 1150 degrees C. The pozzolanic reaction generates very small particles of 10-30 nm on the surface of metakaolin grains of 0.2-0.6 μm, rendering the matrix denser by binding the grains. The maximum compressive strength was revealed with the geopolymer made of metakaolin calcined at 1050 degrees C. The reason for the increased strength of the geopolymer obtained using higher calcination temperature is thought to be the combined effects of matrix hardening by geopolymeric reaction and reinforcement by mullite crystal phases.

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.

40 CFR 98.213 - Calculating GHG emissions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... calcination fractions with Equation U-1 of this section. ER30OC09.077 Where: ECO2 = Annual CO2 mass emissions... ton carbonate consumed. Fi = Fraction calcination achieved for each particular carbonate type i (decimal fraction). As an alternative to measuring the calcination fraction, a value of 1.0 can be used. n...

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.

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

Preparation and electrochemical properties of NiO-Co3O4 composite as electrode materials for supercapacitors

NASA Astrophysics Data System (ADS)

Wang, X. W.; Zheng, D. L.; Yang, P. Z.; Wang, X. E.; Zhu, Q. Q.; Ma, P. F.; Sun, L. Y.

2017-01-01

The precursor of NiO-Co3O4 composites was synthesized via a simple hydrothermal process. After that, the precursor was calcined at 300 °C for 3 h to obtain the composite powders. The powders calcined at 300 °C showed amorphous, and the powders calcined at 400 °C and 500 °C for comparison showed the composite phase of NiO and Co3O4. The composite products showed a microstructure of micro-spheres. For the samples calcined at 300 °C for 3 h, the specific capacitance reached 801 F g-1 at a current density of 1 A g-1.

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

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.

The effect of heat treatment on superhydrophilicity of TiO2 nano thin films

NASA Astrophysics Data System (ADS)

Ashkarran, A. A.; Mohammadizadeh, M. R.

2007-11-01

TiO2 thin films were synthesized by the sol-gel method and spin coating process. The calcination temperature was changed from 100 to 550°C. XRD patterns show increasing the content of polycrystalline anatase phase with increasing the calcination temperature. The AFM results indicate granular morphology of the films, which particle size changes from 22 to 166nm by increasing the calcination temperature. The RBS, EDX and Raman spectroscopy of the films show the ratio of Ti:O ~0.5, and diffusion of sodium ions from substrate into the layer, by increasing the calcination temperature. The UV-vis spectroscopy of the films indicates a red shift by increasing the calcination temperature. The contact angle meter experiment shows that superhydrophilicity of the films depends on the formation of anatase crystal structure and diffused sodium content from substrate to the layer. The best hydrophilicity property was observed at 450°C calcination temperature, where the film is converted to a superhydrophilic surface after 10min under 2mW/cm2 UV irradiation. Water droplet on TiO2 thin film on Si(111), Si(100), and quartz substrates is spread to smaller angles rather than glass and polycrystalline Si substrates under UV irradiation.

Effects of biomass reducing agent on magnetic properties and phase transformation of Baotou low-grade limonite during magnetizing-roasting

PubMed Central

Guo, Wen chao; Luo, Hui juan; Gong, Zhi jun; Li, Bao wei; Wu, Wen fei

2017-01-01

Biomass was used as reducing agent to roast the Baotou low-grade limonite in a high temperature vacuum atmosphere furnace. The effect of calcination temperature, time and ratio of reducing agent on the magnetic properties of calcined ore was studied by VSM. The phase and microstructure changes of limonite before and after calcination were analyzed by XRD and SEM. The results show that in the roasting process the phase transition process of the ferrous material in limonite is first dehydrated at high temperature to formα-Fe2O3, and then it is converted into Fe3O4 by the reduction of biomass. With the increase of calcination temperature, the magnetic properties of the calcined ore first increase and then decrease. When the temperature is higher than 650°C, Fe3O4 will become Fe2SiO4, resulting in reduced the magnetic material in calcined ore and the magnetic weakened. The best magnetization effect was obtained when the roasting temperature is 550°C, the percentage of biomass was 15% and the roasting time was 30min. The saturation magnetization can reach 60.13emu·g-1, the recovery of iron was 72% and the grade of iron was 58%. PMID:29040307

Effects of biomass reducing agent on magnetic properties and phase transformation of Baotou low-grade limonite during magnetizing-roasting.

PubMed

Zhang, Kai; Chen, Xiu Li; Guo, Wen Chao; Luo, Hui Juan; Gong, Zhi Jun; Li, Bao Wei; Wu, Wen Fei

2017-01-01

Biomass was used as reducing agent to roast the Baotou low-grade limonite in a high temperature vacuum atmosphere furnace. The effect of calcination temperature, time and ratio of reducing agent on the magnetic properties of calcined ore was studied by VSM. The phase and microstructure changes of limonite before and after calcination were analyzed by XRD and SEM. The results show that in the roasting process the phase transition process of the ferrous material in limonite is first dehydrated at high temperature to formα-Fe2O3, and then it is converted into Fe3O4 by the reduction of biomass. With the increase of calcination temperature, the magnetic properties of the calcined ore first increase and then decrease. When the temperature is higher than 650°C, Fe3O4 will become Fe2SiO4, resulting in reduced the magnetic material in calcined ore and the magnetic weakened. The best magnetization effect was obtained when the roasting temperature is 550°C, the percentage of biomass was 15% and the roasting time was 30min. The saturation magnetization can reach 60.13emu·g-1, the recovery of iron was 72% and the grade of iron was 58%.

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.

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.

77 FR 12491 - Revisions to the California State Implementation Plan, Antelope Valley Air Quality Management...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-03-01

... Coke Calcining Operations-- 01/18/11 06/20/11 Oxides of Sulfur. SJVUAPCD Synthesized Pharmaceutical.... (a) * * * (6) * * * (ix) Petroleum Coke Calcining Operations--Oxides of Sulfur submitted on June 20...

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.

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.

Sodium Bearing Waste Processing Alternatives Analysis

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

Murphy, James Anthony; Palmer, Brent J; Perry, Keith Joseph

2003-12-01

A multidisciplinary team gathered to develop a BBWI recommendation to DOE-ID on the processing alternatives for the sodium bearing waste in the INTEC Tank Farm. Numerous alternatives were analyzed using a rigorous, systematic approach. The data gathered were evaluated through internal and external peer reviews for consistency and validity. Three alternatives were identified to be top performers: Risk-based Calcination, MACT to WIPP Calcination and Cesium Ion Exchange. A dual-path through early Conceptual design is recommended for MACT to WIPP Calcination and Cesium Ion Exchange since Risk-based Calcination does not require design. If calcination alternatives are not considered based on givingmore » Type of Processing criteria significantly greater weight, the CsIX/TRUEX alternative follows CsIX in ranking. However, since CsIX/TRUEX shares common uncertainties with CsIX, reasonable backups, which follow in ranking, are the TRUEX and UNEX alternatives. Key uncertainties must be evaluated by the decision-makers to choose one final alternative. Those key uncertainties and a path forward for the technology roadmapping of these alternatives is provided.« less

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.

Assessment of the use of red mud as a catalyst for photodegradation of bisphenol A in wastewater treatment.

PubMed

Busto, Raquel Vieira; Gonçalves, Maraisa; Coelho, Lúcia Helena Gomes

2016-09-01

This study aimed to investigate the use of red mud (RM) - a byproduct of aluminum production, as a photocatalyst, which was characterized physical-chemically and used in the photodegradation of the target compound bisphenol A (BPA). Chemical processing was performed in the RM (acid treatment, chemical reduction and calcination) to verify the most active catalyst. From the results obtained, a complete degradation kinetics of BPA was carried out using a synthetic matrix (BPA in deionized water) and a real matrix (BPA in wastewater) using natural RM/calcined and TiO 2 for comparison. The results indicated the potential use of the RM/calcined, which was able to degrade between 88 and 100% of the pollutant in a synthetic sample. Tests on a real effluent sample resulted in degradation rates that ranged from 59 to 100% with chemical oxygen demand reductions of up to 23% using natural RM/calcined in comparison to TiO 2 . The blank system (irradiation of the solution without the use of a photocatalyst) and the natural RM/calcined one, resulted in reductions of the toxicity in the effluent sample (measured by EC 20 using the marine bacteria Vibrio fischeri) of about 12 times, whereas the same treatment using TiO 2 resulted in a toxicity reduction of only seven times. Within these results, the RM/calcined showed potential to be used in wastewater treatment in polishing processes.

40 CFR 60.734 - Monitoring of emissions and operations.

Code of Federal Regulations, 2014 CFR

2014-07-01

... fuller's earth rotary dryer, a gypsum rotary dryer, a gypsum flash calciner, gypsum kettle calciner, an... water column gauge pressure at the level of operation. The liquid flow rate monitoring device must be...

40 CFR 60.734 - Monitoring of emissions and operations.

Code of Federal Regulations, 2013 CFR

2013-07-01

... fuller's earth rotary dryer, a gypsum rotary dryer, a gypsum flash calciner, gypsum kettle calciner, an... water column gauge pressure at the level of operation. The liquid flow rate monitoring device must be...

40 CFR 60.734 - Monitoring of emissions and operations.

Code of Federal Regulations, 2012 CFR

2012-07-01

... fuller's earth rotary dryer, a gypsum rotary dryer, a gypsum flash calciner, gypsum kettle calciner, an... water column gauge pressure at the level of operation. The liquid flow rate monitoring device must be...

40 CFR 60.734 - Monitoring of emissions and operations.

Code of Federal Regulations, 2011 CFR

2011-07-01

... fuller's earth rotary dryer, a gypsum rotary dryer, a gypsum flash calciner, gypsum kettle calciner, an... water column gauge pressure at the level of operation. The liquid flow rate monitoring device must be...

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.

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.

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.

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

Screen-printed SnO2/CNT quasi-solid-state gel-electrolyte supercapacitor

NASA Astrophysics Data System (ADS)

Kuok, Fei-Hong; Liao, Chen-Yu; Chen, Chieh-Wen; Hao, Yu-Chuan; Yu, Ing-Song; Chen, Jian-Zhang

2017-11-01

This study investigates a quasi-solid-state gel-electrolyte supercapacitor fabricated with nanoporous SnO2/CNT nanocomposite electrodes and a polyvinyl alcohol/sulfuric acid (PVA/H2SO4) gel electrolyte. First, pastes containing SnO2 nanoparticles, CNTs, ethyl cellulose, and terpineol are screen-printed onto carbon cloth. A tube furnace is then used for calcining the SnO2/CNT electrodes on carbon cloth. After furnace-calcination, the wettability of SnO2/CNT significantly improved; furthermore, the XPS analysis shows that number of C-O bond and oxygen content significantly decrease after furnace-calcination owing to the burnout of the ethyl cellulose by the furnace calcination processes. The furnace-calcined SnO2/CNT electrodes sandwich the PVA/H2SO4 gel electrolyte to form a supercapacitor. The fabricated supercapacitor exhibits an areal capacitance of 5.61 mF cm-2 when flat and 5.68 mF cm-2 under bending with a bending radius (R) of 1.0 cm. After a 1000 cycle stability test, the capacitance retention rates of the supercapacitor are 96% and 97% when flat and under bending (R  =  1.0 cm), respectively.

Conductivity dependence of lithium diffusivity and electrochemical performance for electrospun TiO2 fibers

NASA Astrophysics Data System (ADS)

Qing, Rui; Liu, Li; Bohling, Christian; Sigmund, Wolfgang

2015-01-01

TiO2 is one of the most exciting anode candidates for safe application in lithium ion batteries. However, its low intrinsic electronic conductivity limits application. In this paper, a simple sol-gel based route is presented to produce nanosize TiO2 fibers with 119 ± 27 nm diameters via electrospinning. Subsequent calcination in various atmospheres was applied to achieve anatase and anatase-rutile mixed phase crystallites with and without carbon coating. The crystallite size was 5 nm for argon calcined fibers and 13-20 nm for air calcined fibers. Argon calcined TiO2 nanofibers exhibited electronic conductivity orders of magnitude higher than those of air-calcined samples. Lithium diffusivity was increased by one time and specific capacity by 26.9% due to the enhanced conductivity. It also had a different intercalation mechanism of lithium. Hydrogen post heat-treatment was found to benefit electronic conductivity (by 3-4.5 times), lithium diffusivity (1.5-2 times) and consequently the high rate performance of the TiO2 nanofibers (over 80%). The inner mechanism and structure-property relations among these parameters were also discussed.

Formation and morphology of Zn(2)Ti(3)O(8) powders using hydrothermal process without dispersant agent or mineralizer.

PubMed

Wang, Cheng-Li; Hwang, Weng-Sing; Chang, Kuo-Ming; Ko, Horng-Huey; Hsi, Chi-Shiung; Huang, Hong-Hsin; Wang, Moo-Chin

2011-01-28

Synthesis of Zn(2)Ti(3)O(8) powders for attenuating UVA using TiCl(4), Zn(NO(3))(2)·6H(2)O and NH(4)OH as precursor materials by hydrothermal process has been investigated. The X-ray diffractometry (XRD) results show the phases of ZnO, anatase TiO(2) and Zn(2)Ti(3)O(8) coexisted when the zinc titanate powders were calcined at 600 °C for 1 h. When calcined at 900 °C for 1 h, the XRD results reveal the existence of ZnO, Zn(2)TiO(4), rutile TiO(2) and ZnTiO(3). Scanning electron microscope (SEM) observations show extensive large agglomeration in the samples. Transmission electron microscope (TEM) and electron diffraction (ED) examination results indicate that ZnTiO(3) crystallites formed with a size of about 5 nm on the matrix of plate-like ZnO when calcined at 700 °C for 1 h. The calcination samples have acceptable absorbance at a wavelength of 400 nm, indicating that the zinc titanate precursor powders calcined at 700 °C for 1 h can be used as an UVA-attenuating agent.

Formation and Morphology of Zn2Ti3O8 Powders Using Hydrothermal Process without Dispersant Agent or Mineralizer

PubMed Central

Wang, Cheng-Li; Hwang, Weng-Sing; Chang, Kuo-Ming; Ko, Horng-Huey; Hsi, Chi-Shiung; Huang, Hong-Hsin; Wang, Moo-Chin

2011-01-01

Synthesis of Zn2Ti3O8 powders for attenuating UVA using TiCl4, Zn(NO3)2·6H2O and NH4OH as precursor materials by hydrothermal process has been investigated. The X-ray diffractometry (XRD) results show the phases of ZnO, anatase TiO2 and Zn2Ti3O8 coexisted when the zinc titanate powders were calcined at 600 °C for 1 h. When calcined at 900 °C for 1 h, the XRD results reveal the existence of ZnO, Zn2TiO4, rutile TiO2 and ZnTiO3. Scanning electron microscope (SEM) observations show extensive large agglomeration in the samples. Transmission electron microscope (TEM) and electron diffraction (ED) examination results indicate that ZnTiO3 crystallites formed with a size of about 5 nm on the matrix of plate-like ZnO when calcined at 700 °C for 1 h. The calcination samples have acceptable absorbance at a wavelength of 400 nm, indicating that the zinc titanate precursor powders calcined at 700 °C for 1 h can be used as an UVA-attenuating agent. PMID:21541035

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.

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.

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

Preparation of ZrO II/nano-TiO II composite powder by sol-gel method

NASA Astrophysics Data System (ADS)

Baharvandi, H. R.; Mohammadi, E.; Abdizadeh, H.; Hadian, A. M.; Ehsani, N.

2007-07-01

The effects of concentration of TTIP, amount of distilled water, and calcination temperature on morphology and particle size distribution of ZrO II/nano-TiO II catalysts were investigated. Mixed ZrO II/nano-TiO II powders were prepared by a modified sol-gel method by varying the mole fraction of TTIP from 0.002 to 0.01, H IIO/TTIP fraction from 2 to 8, and various stirring time (2, 4, and 10 h). The prepared ZrO II/nano-TiO II powders have been characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and TG/DTA. Each oxide was calcined at the temperature between 110 and 1000°C. The results showed that the calcinations temperature has a pronounced effect on the phase formation and particle size of the calcined zirconium titanate (ZT) powders.

12. PHOTOGRAPH OF A PHOTOGRAPH OF A SCALE MODEL OF ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

12. PHOTOGRAPH OF A PHOTOGRAPH OF A SCALE MODEL OF THE WASTE CALCINER FACILITY, SHOWING WEST ELEVATION. (THE ORIGINAL MODEL HAS BEEN LOST.) INEEL PHOTO NUMBER 95-903-1-3. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

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.

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.

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

In vitro cytotoxicity and quantitative silica analysis of diatomaceous earth products.

PubMed

Bye, E; Davies, R; Griffiths, D M; Gylseth, B; Moncrieff, C B

1984-05-01

Mouse peritoneal macrophages were used to evaluate the relative cytotoxicity of a series of diatomaceous earth products in vitro. The amorphous and crystalline silica content of the products was determined by a combination of infrared spectroscopy and x ray powder diffraction techniques. The cytotoxicities of the high cristobalite content flux calcined materials were similar to that of the standard cristobalite ; both the natural and straight calcined materials had significantly greater activities than the flux calcined materials. Thus within the limitations of the macrophage cytotoxicity test the hypothesis that crystalline content is the only determinant of fibrogenicity of diatomaceous earth is not supported.

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

40 CFR 98.314 - Monitoring and QA/QC requirements.

Code of Federal Regulations, 2011 CFR

2011-07-01

... requirements. (a) You must measure your consumption of calcined petroleum coke using plant instruments used for accounting purposes including direct measurement weighing the petroleum coke fed into your process (by belt... used to ensure the accuracy of monthly calcined petroleum coke consumption measurements. (c) You must...

40 CFR 98.314 - Monitoring and QA/QC requirements.

Code of Federal Regulations, 2013 CFR

2013-07-01

... requirements. (a) You must measure your consumption of calcined petroleum coke using plant instruments used for accounting purposes including direct measurement weighing the petroleum coke fed into your process (by belt... used to ensure the accuracy of monthly calcined petroleum coke consumption measurements. (c) You must...

40 CFR 98.314 - Monitoring and QA/QC requirements.

Code of Federal Regulations, 2012 CFR

2012-07-01

... requirements. (a) You must measure your consumption of calcined petroleum coke using plant instruments used for accounting purposes including direct measurement weighing the petroleum coke fed into your process (by belt... used to ensure the accuracy of monthly calcined petroleum coke consumption measurements. (c) You must...

40 CFR 98.314 - Monitoring and QA/QC requirements.

Code of Federal Regulations, 2014 CFR

2014-07-01

... requirements. (a) You must measure your consumption of calcined petroleum coke using plant instruments used for accounting purposes including direct measurement weighing the petroleum coke fed into your process (by belt... used to ensure the accuracy of monthly calcined petroleum coke consumption measurements. (c) You must...

Direct cementitious waste option study report

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

Dafoe, R.E.; Losinski, S.J.

A settlement agreement between the Department of Energy (DOE) and the State of Idaho mandates that all high-level radioactive waste (HLW) now stored at the Idaho Chemical Processing Plant (ICPP) will be treated so that it is ready to be moved out of Idaho for disposal by a target data of 2035. This study investigates the direct grouting of all ICPP calcine (including the HLW dry calcine and those resulting from calcining sodium-bearing liquid waste currently residing in the ICPP storage tanks) as the treatment method to comply with the settlement agreement. This method involves grouting the calcined waste andmore » casting the resulting hydroceramic grout into stainless steel canisters. These canisters will be stored at the Idaho National Engineering and Environmental Laboratory (INEEL) until they are sent to a national geologic repository. The operating period for grouting treatment will be from 2013 through 2032, and all the HLW will be treated and in interim storage by the end of 2032.« less

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.

Phase analysis of ZrO2-SiO2 systems synthesized through Ball milling mechanical activations

NASA Astrophysics Data System (ADS)

Nurlaila, Rizka; Musyarofah, Muwwaqor, Nibras Fuadi; Triwikantoro, Kuswoyo, Anton; Pratapa, Suminar

2017-01-01

Zircon powders have been produced from raw materials of amorphous zirconia and amorphous silica powders obtained from natural zircon sand of Kalimantan Tengah, Indonesia. Synthesis process was started with the extraction of zircon powder to produce sodium silicate solution and pure zircon powder. The amorphous zirconia and silica powders were prepared by alkali fusion and co-precipitation techniques. The powders were mixed using a planetary ball mill, followed by a calcination of various holding time of 3, 10, and 15 h. Phase characterization was done using X-Ray Diffraction (XRD) technique and analysis of the diffraction data was carried out using Rietica and MAUD software. The identified phases after the calcination were zircon, tetragonal zirconia, and cristobalite. The highest zircon content was obtained in the sample calcinated for15 hours - reaching 99.66 %wt. Crystallite size analysis revealed that the samples calcinated for 3, 10, and 15 h exhibited zircon crystal size of 176 (1) nm, 191 (1) nm and 233 (1) nm respectively.

(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.

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.

40 CFR 98.317 - Records that must be retained.

Code of Federal Regulations, 2012 CFR

2012-07-01

... coke purchases. (2) Annual operating hours for each titanium dioxide process line. (b) If a CEMS is not... paraghraph: (1) Records of all calcined petroleum coke purchases (tons). (2) Records of all analyses and... content of consumed calcined petroleum coke (percent by weight expressed as a decimal fraction). (4...

40 CFR 98.317 - Records that must be retained.

Code of Federal Regulations, 2011 CFR

2011-07-01

... coke purchases. (2) Annual operating hours for each titanium dioxide process line. (b) If a CEMS is not... paraghraph: (1) Records of all calcined petroleum coke purchases (tons). (2) Records of all analyses and... content of consumed calcined petroleum coke (percent by weight expressed as a decimal fraction). (4...

40 CFR 98.317 - Records that must be retained.

Code of Federal Regulations, 2014 CFR

2014-07-01

... coke purchases. (2) Annual operating hours for each titanium dioxide process line. (b) If a CEMS is not... paraghraph: (1) Records of all calcined petroleum coke purchases (tons). (2) Records of all analyses and... content of consumed calcined petroleum coke (percent by weight expressed as a decimal fraction). (4...

40 CFR 98.317 - Records that must be retained.

Code of Federal Regulations, 2013 CFR

2013-07-01

... coke purchases. (2) Annual operating hours for each titanium dioxide process line. (b) If a CEMS is not... paraghraph: (1) Records of all calcined petroleum coke purchases (tons). (2) Records of all analyses and... content of consumed calcined petroleum coke (percent by weight expressed as a decimal fraction). (4...

Cements for Structural Concrete in Cold Regions.

DTIC Science & Technology

1977-10-01

ability to reduce the early evolu- tion of heat: slag and obsidian, pumicite and calcined shale, fly-ash , tuff and calcined diatomite , natural cement...and uncalcined diatomite . Variations in initial set times of cements can be controlled ‘cy varying the percentages of different cement mixtures . Wh it

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

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.

Energy Efficient Microwave Hybrid Processing of Lime for Cement, Steel, and Glass Industries

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

Fall, Morgana L; Yakovlev, Vadim; Sahi, Catherine

2012-02-10

In this study, the microwave materials interactions were studied through dielectric property measurements, process modeling, and lab scale microwave hybrid calcination tests. Characterization and analysis were performed to evaluate material reactions and energy usage. Processing parameters for laboratory scale and larger scale calcining experiments were developed for MAT limestone calcination. Early stage equipment design concepts were developed, with a focus on microwave post heating treatment. The retrofitting of existing rotary calcine equipment in the lime industry was assessed and found to be feasible. Ceralink sought to address some of the major barriers to the uptake of MAT identified as themore » need for (1) team approach with end users, technology partners, and equipment manufacturers, (2) modeling that incorporates kiln materials and variations to the design of industrial microwave equipment. This project has furthered the commercialization effort of MAT by working closely with an industrial lime manufacturer to educate them regarding MAT, identifying equipment manufacturer to supply microwave equipment, and developing a sophisticated MAT modeling with WPI, the university partner. MAT was shown to enhance calcining through lower energy consumption and faster reaction rates compared to conventional processing. Laboratory testing concluded that a 23% reduction in energy was possible for calcining small batches (5kg). Scale-up testing indicated that the energy savings increased as a function of load size and 36% energy savings was demonstrated (22 kg). A sophisticated model was developed which combines simultaneous microwave and conventional heating. Continued development of this modeling software could be used for larger scale calcining simulations, which would be a beneficial low-cost tool for exploring equipment design prior to actual building. Based on these findings, estimates for production scale MAT calcining benefits were calculated, assuming

In vitro cytotoxicity and quantitative silica analysis of diatomaceous earth products.

PubMed Central

Bye, E; Davies, R; Griffiths, D M; Gylseth, B; Moncrieff, C B

1984-01-01

Mouse peritoneal macrophages were used to evaluate the relative cytotoxicity of a series of diatomaceous earth products in vitro. The amorphous and crystalline silica content of the products was determined by a combination of infrared spectroscopy and x ray powder diffraction techniques. The cytotoxicities of the high cristobalite content flux calcined materials were similar to that of the standard cristobalite ; both the natural and straight calcined materials had significantly greater activities than the flux calcined materials. Thus within the limitations of the macrophage cytotoxicity test the hypothesis that crystalline content is the only determinant of fibrogenicity of diatomaceous earth is not supported. Images PMID:6326795

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.

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.

Process and equipment development for hot isostatic pressing treatability study

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

Bateman, Ken; Wahlquist, Dennis; Malewitz, Tim

2015-03-01

Battelle Energy Alliance (BEA), LLC, has developed processes and equipment for a pilot-scale hot isostatic pressing (HIP) treatability study to stabilize and volume reduce radioactive calcine stored at Idaho National Laboratory (INL). In 2009, the U. S. Department of Energy signed a Record of Decision with the state of Idaho selecting HIP technology as the method to treat 5,800 yd^3 (4,400 m^3) of granular zirconia and alumina calcine produced between 1953 and 1992 as a waste byproduct of spent nuclear fuel reprocessing. Since the 1990s, a variety of radioactive and hazardous waste forms have been remotely treated using HIP withinmore » INL hot cells. To execute the remote process at INL, waste is loaded into a stainless-steel or aluminum can, which is evacuated, sealed, and placed into a HIP furnace. The HIP simultaneously heats and pressurizes the waste, reducing its volume and increasing its durability. Two 1 gal cans of calcine waste currently stored in a shielded cask were identified as candidate materials for a treatability study involving the HIP process. Equipment and materials for cask-handling and calcine transfer into INL hot cells, as well as remotely operated equipment for waste can opening, particle sizing, material blending, and HIP can loading have been designed and successfully tested. These results demonstrate BEA’s readiness for treatment of INL calcine.« less

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.

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

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.

Mercury isotope fractionation during ore retorting in the Almadén mining district, Spain

USGS Publications Warehouse

Gray, John E.; Pribil, Michael J.; Higueras, Pablo L.

2013-01-01

Almadén, Spain, is the world's largest mercury (Hg) mining district, which has produced over 250,000 metric tons of Hg representing about 30% of the historical Hg produced worldwide. The objective of this study was to measure Hg isotopic compositions of cinnabar ore, mine waste calcine (retorted ore), elemental Hg (Hg0(L)), and elemental Hg gas (Hg0(g)), to evaluate potential Hg isotopic fractionation. Almadén cinnabar ore δ202Hg varied from − 0.92 to 0.15‰ (mean of − 0.56‰, σ = 0.35‰, n = 7), whereas calcine was isotopically heavier and δ202Hg ranged from − 0.03‰ to 1.01‰ (mean of 0.43‰, σ = 0.44‰, n = 8). The average δ202Hg enrichment of 0.99‰ between cinnabar ore and calcines generated during ore retorting indicated Hg isotopic mass dependent fractionation (MDF). Mass independent fractionation (MIF) was not observed in any of the samples in this study. Laboratory retorting experiments of cinnabar also were carried out to evaluate Hg isotopic fractionation of products generated during retorting such as calcine, Hg0(L), and Hg0(g). Calcine and Hg0(L) generated during these retorting experiments showed an enrichment in δ202Hg of as much as 1.90‰ and 0.67‰, respectively, compared to the original cinnabar ore. The δ202Hg for Hg0(g) generated during the retorting experiments was as much as 1.16‰ isotopically lighter compared to cinnabar, thus, when cinnabar ore was roasted, the resultant calcines formed were isotopically heavier, whereas the Hg0(g) generated was isotopically lighter in Hg isotopes.

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

Cryochemical method for forming spherical metal oxide particles from metal salt solutions

DOEpatents

Tinkle, M.C.

1973-12-01

A method is described of preparing small metal oxide spheres cryochemically utilizing metal salts (e.g., nitrates) that cannot readily be dried and calcined without loss of sphericity of the particles. Such metal salts are cryochemically formed into small spheres, partially or completely converted to an insoluble salt, and dried and calcined. (Official Gazette)

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.

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.

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.

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.

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

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

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

Recycling Lithium Carbonate/Lithium Hydroxide Waste

NASA Technical Reports Server (NTRS)

Flowers, J.; Flowers, J.

1983-01-01

Hazardous waste disposal problem eliminated by regeneration. Li2CO3/ LiOH recycling process relies on low solubility of alkali carbonates in corresponding hydroxides. Li2CO3 precipitate calcined to LI2O, then rehydrated LiOH. Regeneration eliminates need to dispose caustic waste and uses less energy than simple calcination of entire waste mass.

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.

Synthesis and characterization of mesoporous ceria/alumina nanocomposite materials via mixing of the corresponding ceria and alumina gel precursors.

PubMed

Khalil, Kamal M S

2007-03-01

Mesoporous ceria/alumina, CeO(2)/Al(2)O(3), composites containing 10, 20 and 30% (w/w) ceria were prepared by a novel gel mixing method. In the method, ceria gel (formed via hydrolysis of ammonium cerium(IV) nitrate by aqueous ammonium carbonate solution) and alumina gel (formed via controlled hydrolysis of aluminum tri-isopropoxide) were mixed together. The mixed gel was subjected to subsequent drying and calcination for 3 h at 400, 600, 800 and 1000 degrees C. The uncalcined (dried at 110 degrees C) and the calcined composites were investigated by different techniques including TGA, DSC, FTIR, XRD, SEM and nitrogen adsorption/desorption isotherms. Results indicated that composites calcined for 3 h at 800 degrees C mainly kept amorphous alumina structure and gamma-alumina formed only upon calcinations at 1000 degrees C. On the other hand, CeO(2) was found to crystallize in the common ceria, cerinite, phase and it kept this structure over the entire calcination range (400-1000 degrees C). Therefore, high surface areas, stable surface textures, and non-aggregated nano-sized ceria dispersions were obtained. A systematic texture change based on ceria ratio was observed, however in all cases mesoporous composite materials exposing thermally stable texture and structure were obtained. The presented method produces composite ceria/alumina materials that suit different applications in the field of catalysis and membranes technology, and throw some light on physicochemical factors that determine textural morphology and thermal stability of such important composite.

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.

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.

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.

Characterization and morphology of prepared titanium dioxide nanofibers by electrospinning.

PubMed

Park, Ju-Young; Lee, In-Hwa

2010-05-01

Dispersed titanium dioxide in polymer nanofibers were prepared by sol-gel processing and electrospinning techniques using titanium isopropoxide (TiP)/polyvinylpyrrolidone (PVP) solution. The prepared titanium dioxide nanofibers were characterized by FE-SEM, TEM, XRD, and FT-IR. Pure titanium dioxide nanofibers were obtained from calcination of inorganic-organic composite fiber. The diameter of titanium oxide nanofibers were in the range of 70 nm to 150 nm. Prepared titanium dioxide nanofibers show rough surface and rather small diameter compare with TiP/PVP composite nanofibers. After calcined at 500 degrees C, TiO2 nanofibers convert into anatase and rutile mixed phased from amorphous structure. Calcination of these composite fibers above 600 degrees C resulted in pure rutile TiO2 nanofibers.

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.

Synthesis and characterization of Ni doped ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Tamgadge, Y. S.; Gedam, P. P.; Ganorkar, R. P.; Mahure, M. A.; Pahurkar, V. G.; Muley, G. G.

2018-05-01

In this paper, we present synthesis of L-valine assisted surface modification of Ni doped ZnO nanoparticles (NPs) using chemical precipitation method. Samples were calcined at 500oC for 2h. Uncalcined and calcined samples were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and ultraviolet-visible (UV-vis) spectroscopy. Ni doped ZnO NPs with average particle size of 8 nm have been successfully obtained using L-valine as surface modifying agent. Increase in the particle size was observed after the calcination. XRD and TEM studies confirmed the purity, surface morphology and hexagonal wurtzite crystal structure of ZnO NPs. UV-vis spectroscopy indicated the blue shift of excitons absorption wavelength and surface modification by L-valine.

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.

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.

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.

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.

One-step rapid synthesis of ultrafine γ-Ga2O3 nanocrystals by microwave hydrothermal method in ammonium hydroxide medium

NASA Astrophysics Data System (ADS)

Cui, Lu; Wang, Hong; Xin, Baifu; Mao, Guijie

2017-10-01

Ultrafine nanocrystals of γ-gallium oxide (γ-Ga2O3) were rapidly synthesized via microwave hydrothermal method at 140 °C, in which Ga(NO3)3 was used as the gallium source and urea was the precipitant. The samples were characterized by X-ray diffraction (XRD), ultraviolet-visible absorption spectroscopy (UV-Vis), transmission electron microscopy (TEM), nitrogen physisorption and photoluminescence spectroscopy (PL). The crystallite size of ultrafine spinel γ-Ga2O3 was in the range from 4 to 5 nm and the optical bandgap was 4.61 eV. To improve the crystallinity, the ultrafine γ-Ga2O3 nanocrystals were calcined at 300-700 °C further. The ultrafine γ-Ga2O3 calcined at 500 °C (calcined-γ-Ga2O3) still remained the metastable γ-phase with relatively high crystallinity and the crystallite size around 5-7 nm. Photocatalytic performances of the synthesized samples were also evaluated by the degradation of rhodamine B (RhB). Results revealed that the ultrafine γ-Ga2O3 and the calcined-γ-Ga2O3 samples exhibited high photocatalytic efficiencies of 68.2 and 90.7%, respectively.

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.

Preparation, characterizations and photocatalytic activity of a ZnO/TiO2 nanocomposite

NASA Astrophysics Data System (ADS)

Lachom, Vichuda; Poolcharuansin, Phitsanu; Laokul, Paveena

2017-03-01

Nanoparticles of TiO2, ZnO and nanocomposite ZnO/TiO2 were prepared via a co-precipitation method. The precursor powders were calcined in air at 400 and 500 °C for 2 h. Crystallite sizes of the calcined samples ranged from 11-43 nm. The XRD patterns of ZnO/TiO2 powder showed two phases of anatase and wurtzite, with no ZnTiO3 impurity phase. TEM images showed three types of particles in the ZnO/TiO2 samples: a fine particle type of TiO2 and submicron ellipsoidal and rod-like particles of ZnO. The energy gap (E g) of the calcined powders was evaluated using UV-vis absorption spectra and found to be in the range of 3.15-3.60 eV. Photodegradation efficiencies of the prepared samples in methyl orange aqueous solution were investigated under UVA irradiation. The results showed that nanocomposite ZnO/TiO2 calcined at 400 °C exhibited the highest apparent rate constant (k), and a higher capacity for methyl orange removal than TiO2 and ZnO nanoparticles.

Is there lattice contraction in multicomponent metal oxides? Case study for GdVO4:Eu3+ nanoparticles.

PubMed

Yang, Liusai; Li, Liping; Zhao, Minglei; Fu, Chaochao; Li, Guangshe

2013-08-02

Metal oxide nanomaterials have been found to have great potential for diverse applications due to their unique relationships between structure and properties. Lattice expansion as particle size reduces was previously considered to be general for metal oxide nanomaterials. It is now a great challenge to see if lattice contraction could be induced by the size effect for metal oxide nanomaterials. ABO4 metal oxides (e.g., CaWO4, GdVO4, and CdWO4) are some of the most important functional materials with many applications, while such oxides at the nanoscale are never reported to show a lattice contraction. This work presents a first report on the variation from lattice expansion to lattice contraction by tuning the microstructures of GdVO4:Eu(3+) nanocrystals. A hydrothermal method was adopted to synthesize GdVO4:Eu(3+) nanocrystals, and then these nanoparticles were calcined at 600 ° C in air. It is found that particle size reduction led to a lattice contraction for the calcined samples, which is in contrast to the lattice expansion observed for the hydrothermally synthesized counterparts or many other metal oxide nanomaterials. In addition, the lattice symmetry of the calcined samples remained almost a constant. The results indicate that the negative surface stress was eliminated by calcination treatment, leading to a homogeneous compression process in the lattice structure of the calcined GdVO4:Eu(3+) nanocrystals. Furthermore, Eu(3+) was taken as a structural probe and a luminescence center to study the local environments pertinent to these structural changes and to optimize the photoluminescence performance.

Is there lattice contraction in multicomponent metal oxides? Case study for GdVO4:Eu3+ nanoparticles

NASA Astrophysics Data System (ADS)

Yang, Liusai; Li, Liping; Zhao, Minglei; Fu, Chaochao; Li, Guangshe

2013-08-01

Metal oxide nanomaterials have been found to have great potential for diverse applications due to their unique relationships between structure and properties. Lattice expansion as particle size reduces was previously considered to be general for metal oxide nanomaterials. It is now a great challenge to see if lattice contraction could be induced by the size effect for metal oxide nanomaterials. ABO4 metal oxides (e.g., CaWO4, GdVO4, and CdWO4) are some of the most important functional materials with many applications, while such oxides at the nanoscale are never reported to show a lattice contraction. This work presents a first report on the variation from lattice expansion to lattice contraction by tuning the microstructures of GdVO4:Eu3+ nanocrystals. A hydrothermal method was adopted to synthesize GdVO4:Eu3+ nanocrystals, and then these nanoparticles were calcined at 600 ° C in air. It is found that particle size reduction led to a lattice contraction for the calcined samples, which is in contrast to the lattice expansion observed for the hydrothermally synthesized counterparts or many other metal oxide nanomaterials. In addition, the lattice symmetry of the calcined samples remained almost a constant. The results indicate that the negative surface stress was eliminated by calcination treatment, leading to a homogeneous compression process in the lattice structure of the calcined GdVO4:Eu3+ nanocrystals. Furthermore, Eu3+ was taken as a structural probe and a luminescence center to study the local environments pertinent to these structural changes and to optimize the photoluminescence performance.

Structural and Magnetic Properties Evolution of Co-Nd Substituted M-type Hexagonal Strontium Ferrites Synthesized by Ball-Milling-Assisted Ceramic Process

NASA Astrophysics Data System (ADS)

Chen, Wen; Wu, Wenwei; Zhou, Chong; Zhou, Shifang; Li, Miaoyu; Ning, Yu

2018-03-01

M-type hexagonal Sr1- x Co x Nd x Fe12- x O19 ( x = 0, 0.08, 0.16, and 0.24) has been synthesized by ball milling, followed by calcination in air. The calcined products have been characterized by x-ray powder diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectra, and vibrating sample magnetometry. XRD and SEM analyses confirm the formation of M-type Sr hexaferrite with platelet-like morphology when Sr1- x Co x Nd x Fe12- x O19 ( x = 0, 0.08, 0.16, and 0.24) precursors are calcined at 950°C in air for 2.5 h. Lattice parameters " a" and " c" values of Sr1- x Co x Nd x Fe12- x O19 reflect a very small variation after doping of Nd3+ and Co2+ ions. Average crystallite size of Sr1- x Co x Nd x Fe12- x O19 sample, calcined at 1150°C, decreased obviously after doping of Co2+ and Nd3+ ions. This is because the bond energy of Nd3+-O2- is much larger than that of Sr2+-O2-. Magnetic characterization indicates that all the samples exhibit good magnetic properties. Substitution of Sr2+ and Fe3+ ions by Nd3+ and Co2+ ions can improve the specific saturation magnetizations and remanence of Sr1- x Co x Nd x Fe12- x O19. Sr0.84Co0.16Nd0.16Fe11.84O19, calcined at 1050°C, has the highest specific saturation magnetization value (74.75 ± 0.60 emu/g), remanence (45.15 ± 0.32 emu/g), and magnetic moment (14.34 ± 0.11 μ B); SrFe12O19, calcined at 1150°C, has the highest coercivity value (4037.01 ± 42.39 Oe). These magnetic parameters make this material a promising candidate for applications such as high-density magnetic recording and microwave absorbing materials.

Macroscopic and microscopic observations of particle-facilitated mercury transport from New Idria and Sulphur Bank mercury mine tailings

USGS Publications Warehouse

Lowry, G.V.; Shaw, S.; Kim, C.S.; Rytuba, J.J.; Brown, Gordon E.

2004-01-01

Mercury (Hg) release from inoperative Hg mines in the California Coast Range has been documented, but little is known about the release and transport mechanisms. In this study, tailings from Hg mines located in different geologic settings-New Idria (NI), a Si-carbonate Hg deposit, and Sulphur Bank (SB), a hot-spring Hg deposit-were characterized, and particle release from these wastes was studied in column experiments to (1) investigate the mechanisms of Hg release from NI and SB mine wastes, (2) determine the speciation of particle-bound Hg released from the mine wastes, and (3) determine the effect of calcinations on Hg release processes. The physical and chemical properties of tailings and the colloids released from them were determined using chemical analyses, selective chemical extractions, XRD, SEM, TEM, and X-ray absorption spectroscopy techniques. The total Hg concentration in tailings increased with decreasing particle size in NI and SB calcines (roasted ore), but reached a maximum at an intermediate particle size in the SB waste rock (unroasted ore). Hg in the tailings exists predominantly as low-solubility HgS (cinnabar and metacinnabar), with NI calcines having >50% HgS, SB calcines having >89% HgS, and SB waste rock having ???100% HgS. Leaching experiments with a high-ionic-strength solution (0.1 M NaCl) resulted in a rapid but brief release of soluble and particulate Hg. Lowering the ionic strength of the leach solution (0.005 M NaCl) resulted in the release of colloidal Hg from two of the three mine wastes studied (NI calcines and SB waste rock). Colloid-associated Hg accounts for as much as 95% of the Hg released during episodic particle release. Colloids generated from the NI calcines are produced by a breakup and release mechanism and consist of hematite, jarosite/alunite, and Al-Si gel with particle sizes of 10-200 nm. ATEM and XAFS analyses indicate that the majority (???78%) of the mercury is present in the form of HgS. SB calcines also

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

Comparison of the biological H2S removal characteristics among four inorganic packing materials.

PubMed

Hirai, M; Kamamoto, M; Yani, M; Shoda, M

2001-01-01

Four inorganic packing materials were evaluated in terms of their availability as packing materials of a packed tower deodorization apparatus (biofilter) from the viewpoints of biological H2S removal characteristics and some physical properties. Among porous ceramics (A), calcinated cristobalite (B), calcinated and formed obsidian (C), granulated and calcinated soil (D), the superiority of these packing materials determined based on the values of non-biological removal per unit weight or unit volume of packing material, complete removal capacity of H2S per unit weight of packing material per day or unit volume of packing material per day and pressure drop of the packed bed was in the order of A approximately equal to C > D approximately equal to B, which is correlated with the maximum water content, porosity, and mean pore diameter.

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.

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.

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.

METHOD AND APPARATUS FOR CALCINING SALT SOLUTIONS

DOEpatents

Lawroski, S.; Jonke, A.A.; Taecker, R.G.

1961-10-31

A method is given for converting uranyl nitrate solution into solid UO/ sub 3/, The solution is sprayed horizontally into a fluidized bed of UO/sub 3/ particles at 310 to 350 deg C by a nozzle of the coaxial air jet type at about 26 psig, Under these conditions the desired conversion takes place, and caking in the bed is avoided.

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.

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.

High speed production of YBCO precursor films by advanced TFA-MOD process

NASA Astrophysics Data System (ADS)

Ichikawa, H.; Nakaoka, K.; Miura, M.; Sutoh, Y.; Nakanishi, T.; Nakai, A.; Yoshizumi, M.; Izumi, T.; Shiohara, Y.

2009-10-01

YBa 2Cu 3O 7-y (YBCO) long tapes derived from the metal-organic deposition (MOD) method using the starting solution containing trifluoroacetate (TFA) have been developed with high critical currents ( I c) over 200 A/cm-width. However, high speed production of YBCO films is simultaneously necessary to satisfy the requirements of electric power device applications in terms of cost and the amounts of the tapes. In this work, we developed a new TFA-MOD starting solution using F-free salt of Y, TFA salt of Ba and Cu-Octylate for application to the coating/calcination process and discussed several issues by using the Multi-turn (MT) Reel-to-Reel (RTR) system calcination furnace for the purpose of high throughput without degradation of the properties. The coating system was improved for uniform deposition qualities in both longitudinal and transversal directions. YBCO films using the new starting solution at the traveling rate of 10 m/h in coating/calcination by the MT-RTR calcination furnace showed the values of the critical current density of 1.6 MA/cm 2 as thick as 1.5 μm at 77 K under the self fields after firing at the high heating rate in the crystallization.

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

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.

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+.

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.

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.

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

Bauxite and alumina

USGS Publications Warehouse

Bray, E. Lee

2013-01-01

The United States is reliant upon imports for nearly all of the bauxite that it consumes. Small amounts of bauxite and bauxitic clays are produced in Alabama, Arkansas and Georgia for nonmetallurgical uses. Metallurgical-grade bauxite (crude dry) imports in 2012 totaled 10.3 Mt (11.3 million st), 8 percent more than the quantity imported in 2011. Jamaica (46 percent), Guinea (27 percent) and Brazil (25 percent) were the leading suppliers to the United States in 2012. In 2012, 84 kt (92,600 st) of refractory-grade calcined bauxite was imported, an 8-percent decrease compared with imports in 2011. Although domestic steel production increased by about 3 percent in 2012, compared with production in 2011, increased use of magnesia for refractory products may account for the decrease in refractory-grade calcined bauxite imports. Guyana (55 percent) and China (45 percent) were the sources of U.S. refractory-grade calcined bauxite imports. Imports of nonrefractory-grade calcined bauxite in 2012 totaled 323 kt (356,000 st), 24 percent more than the quantity imported in 2011. This increase was attributed to increased use of bauxite in cement, as proppants for hydraulic fracturing by the petroleum industry and by steel makers. Guyana (32 percent), Australia (29 percent) and Greece (25 percent) were the leading sources.

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.

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.

The Influence of Alumina Properties on its Dissolution in Smelting Electrolyte

NASA Astrophysics Data System (ADS)

Bagshaw, A. N.; Welch, B. J.

The dissolution of a wide range of commercially produced aluminas in modified cryolite bath was studied on a laboratory scale. Most of the aluminas were products of conventional refineries and smelter dry scrubbing systems; a few were produced in laboratory and pilot calciners, enabling greater flexibility in the calcination process and the final properties. The mode of alumina feeding and the size of addition approximated to the point feeder situation. Alpha-alumina content, B.E.T. surface area and median particle size had little impact on dissolution behaviour. The volatiles content, expressed as L.O.I., the morphology of the original hydrate and the mode of calcination had the most influence. Discrete intermediate oxide phases were identified in all samples; delta-alumina content impacted most on dissolution. The flow properties of an alumina affected its overall dissolution.

[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.

Utilization of wasted cockle shell as a natural coagulant and a neutralizer of polluted water in Bangka Belitung islands, Indonesia

NASA Astrophysics Data System (ADS)

Tiandho, Y.; Aldila, H.; Mustari; Megiyo; Afriani, F.

2018-05-01

Bangka Belitung Islands is the largest tin producer in Indonesia. The high activity of tin mining caused the environmental damage which had an impact on the emergence of clean water crisis in some areas in this province. In this paper, a simple water quality improvement method based on wasted cockle shell was developed. Based on x-ray diffraction analysis it is known that calcination of cockle shell powder at 700°C will decompose the powder into calcium oxide compound. The addition of calcined cockle shell powder into acidic water from Merawang Sub-district will increase the pH of water through the process of forming hydroxide groups in the water. The calcined cockle shell powder can also coagulate pollutants in some polluted water from Koba Sub-district. The coagulation results were analyzed using SEM/EDS.

Aqueous Chloride Operations Overview: Plutonium and Americium Purification/Recovery

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

Gardner, Kyle Shelton; Kimball, David Bryan; Skidmore, Bradley Evan

These are a set of slides intended for an information session as part of recruiting activities at Brigham Young University. It gives an overview of aqueous chloride operations, specifically on plutonium and americium purification/recovery. This presentation details the steps taken perform these processes, from plutonium size reduction, dissolution, solvent extraction, oxalate precipitation, to calcination. For americium recovery, it details the CLEAR (chloride extraction and actinide recovery) Line, oxalate precipitation and calcination.

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.

Processing Studies for Optically Transparent La(2)O(3)-Doped Y(2)O(3).

DTIC Science & Technology

1986-07-31

sintering. EXPERIMENTAL PROCEDURE ’ "’ The control powder (A) used in this investigation was prepared by a standard oxalate coprecip- itation procedure...Possible sources of CO2 are the decomposition of any oxalate remaining after calcination and/or formation of ’.’ carbonates during exposure to air. The...all the volatiles are removed from oxalate -derived powders during calcining or prefiring to 15000C. C02 is the major species present and probably

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

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.

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

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.

Relationships Between Smelter Grade Alumina Characteristics and Strength Determined by Nanoindentation and Ultrasound-Mediated Particle Breakage

NASA Astrophysics Data System (ADS)

Wijayaratne, Hasini; McIntosh, Grant; Hyland, Margaret; Perander, Linus; Metson, James

2017-06-01

The mechanical strength of smelter grade alumina (SGA) is of considerable practical significance for the aluminum reduction process. Attrition of alumina during transportation and handling generates an increased level of fines. This results in generation of dust, poor flow properties, and silo segregation that interfere with alumina feeding systems. These lead to process instabilities which in turn result in current efficiency losses that are costly. Here we are concerned with developing a fundamental understanding of SGA strength in terms of its microstructure. Nanoindentation and ultrasound-mediated particle breakage tests have been conducted to study the strength. Strength of SGA samples both industry calcined and laboratory prepared, decrease with increasing α-alumina (corundum) content contrary to expectation. The reducing strength of alumina with increasing degree of calcination is attributed to the development of a macroporous and abrasion-prone microstructure resulting from the `pseudomorphic' transformation of precursor gibbsite during the calcination process.

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

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

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

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

M. L. Abbott; K. N. Keck; R. E. Schindler

This screening level risk assessment evaluates potential adverse human health and ecological impacts resulting from continued operations of the calciner at the New Waste Calcining Facility (NWCF) at the Idaho Nuclear Technology and Engineering Center (INTEC), Idaho National Engineering and Environmental Laboratory (INEEL). The assessment was conducted in accordance with the Environmental Protection Agency (EPA) report, Guidance for Performing Screening Level Risk Analyses at Combustion Facilities Burning Hazardous Waste. This screening guidance is intended to give a conservative estimate of the potential risks to determine whether a more refined assessment is warranted. The NWCF uses a fluidized-bed combustor to solidifymore » (calcine) liquid radioactive mixed waste from the INTEC Tank Farm facility. Calciner off volatilized metal species, trace organic compounds, and low-levels of radionuclides. Conservative stack emission rates were calculated based on maximum waste solution feed samples, conservative assumptions for off gas partitioning of metals and organics, stack gas sampling for mercury, and conservative measurements of contaminant removal (decontamination factors) in the off gas treatment system. Stack emissions were modeled using the ISC3 air dispersion model to predict maximum particulate and vapor air concentrations and ground deposition rates. Results demonstrate that NWCF emissions calculated from best-available process knowledge would result in maximum onsite and offsite health and ecological impacts that are less then EPA-established criteria for operation of a combustion facility.« less

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.

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

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

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.

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.

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

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.

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

Synthesis, Optical and Electrochemical Properties of Y2O3 Nanoparticles Prepared by Co-Precipitation Method.

PubMed

Saravanan, Thulasingam; Raj, Srinivasan Gokul; Chandar, Nagamuthu Raja Krishna; Jayavel, Ramasamy

2015-06-01

Y2O3 nanoparticles were synthesized by co-precipitation route using yttrium nitrate hexahydrate and ammonium hydroxide as precursors. The prepared sample was calcined at 500 degrees C and subjected to various characterization studies like thermal analysis (TG/DTA), X-ray diffraction (XRD), transmission electron microscope (TEM), UV-visible (UV-Vis) and photoluminescence (PL) spectroscopy. The XRD pattern showed the cubic fluorite structure of Y2O3 without any impurity peaks, revealing high purity of the prepared sample. TEM images revealed that the calcined Y2O3 nanoparticles consist of spherical-like morphology with an average particle size of 12 nm. The absorption spectrum of calcined samples shows blue-shift compared to the as-prepared sample, which was further confirmed by PL studies. The possible formation mechanism of Y2O3 nanoparticles has been discussed based on the experimental results. Electrochemical behavior of Y2O3 nanoparticles was studied by cyclic voltammetry to assess their suitability for supercapacitor applications.

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.

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.

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.

Synthesis of CaCu3Ti4O12 by modified Sol-gel method with Hydrothermal process

NASA Astrophysics Data System (ADS)

Masingboon, C.; Rungruang, S.

2017-09-01

CaCu3Ti4O12 powders were synthesized by modified Sol-gel method with Hydrothermal process using Ca(NO3)2· 4H2O, Cu(NO3)2·3H2O, Ti(OC3H7)4 and freshly extracted egg white (ovalbumin) in aqueous medium. The precursor was calcined at 800, 900 and 1000 °C in air for 8 h to obtain nanocrystalline powders of CaCu3Ti4O12. The calcined CaCu3Ti4O12 powders were characterized by XRD, TEM and EDX. The XRD results indicated that all calcined samples have a typical perovskite CaCu3Ti4O12 structure and a small amount of CaTiO3, CuO and TiO2. TEM micrographs showed particle size 100 - 500 nm and EDX results showed elements of CaCu3Ti4O12 powders have calcium, copper, titanium and oxygen.

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.

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.

Environmental geochemistry of abandoned mercury mines in West-Central Nevada, USA

USGS Publications Warehouse

Gray, J.E.; Crock, J.G.; Fey, D.L.

2002-01-01

The Humboldt River is a closed basin and is the longest river in Nevada. Numerous abandoned Hg mines are located within the basin, and because Hg is a toxic heavy metal, the potential transport of Hg from these mines into surrounding ecosystems, including the Humboldt River, is of environmental concern Samples of ore, sediment, water, calcines (roasted ore), and leachates of the calcines were analyzed for Hg and other heavy metals to evaluate geochemical dispersion from the mines. Cinnabar-bearing ore samples collected from the mines contain highly elevated Hg concentrations, up to 6.9 %, whereas calcines collected from the mines contain up to 2000 mg Hg/kg. Stream-sediment samples collected within 1 km of the mines contain as much as 170 mg Hg/kg, but those collected distal from the mines (> 5 km) contain 8 km from the Humboldt River, and Hg is transported and diluted through a large volume of pediment before it reaches the Humboldt River. ?? 2002 Elsevier Science Ltd. All rights reserved.

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.

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.

CALCINED CLAYS AS A LOW EMISSION CEMENT SUBSTITUTE

EPA Science Inventory

This study provides a better understanding of clay-cement materials including: (i) their associated energy demand and carbon dioxide emissions of their manufacturing and transport, (ii) their structural performance and properties, and (iii) their emission characteristics affe...

Fluidized-bed calciner with combustion nozzle and shroud

DOEpatents

Wielang, Joseph A.; Palmer, William B.; Kerr, William B.

1977-01-01

A nozzle employed as a burner within a fluidized bed is coaxially enclosed within a tubular shroud that extends beyond the nozzle length into the fluidized bed. The open-ended shroud portion beyond the nozzle end provides an antechamber for mixture and combustion of atomized fuel with an oxygen-containing gas. The arrangement provides improved combustion efficiency and excludes bed particles from the high-velocity, high-temperature portions of the flame to reduce particle attrition.

Bauxite and alumina

USGS Publications Warehouse

Bray, E.L.

2012-01-01

The United States is import-reliant for nearly all of the bauxite that it consumes. Small amounts of bauxite and bauxitic clays are produced in Alabama, Arkansas and Georgia for nonmetallurgical uses. Metallurgical-grade bauxite (crude dry) imports in 2011 totaled 9.54 Mt (10.5 million st), 18 percent more than the quantity imported in 2010. Jamaica (54 percent). Guinea (25 percent) and Brazil (18 percent) were the leading suppliers to the United States in 2011. In 2011,117 kt (129,000 st) of refractory-grade calcined bauxite was imported, a 69-percent decrease compared with imports in 2010. This decrease was partly attributed to an increase in net imports of refractory products such as bricks and crucibles, which were 39 percent higher than in the prior year. Imports of refractory-grade calcined bauxite from Brazil declined by 99 percent and by 75 percent from Greece. Restrictions on exports of raw materials from China also might have contributed a small amount to the decrease in imports. Imports from China declined by 45 percent. Guyana (42 percent), China (35 percent) and Greece (22 percent) were the leading sources of U.S. refractory-grade calcined bauxite imports. Imports of nonrefractory-grade calcined bauxite in 2011 totaled 236 kt (260,000 st), 23 percent less than the quantity imported in 2010. Guyana (51 percent), Australia (37 percent) and China (7 percent) were the leading sources

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.

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.

Luminescence properties of Lu2O3: Tb film prepared by Pechini sol-gel method

NASA Astrophysics Data System (ADS)

Shen, Siqing; Wang, Jian; Xu, Zhibin; Xie, Jianjun; Shi, Ying

2010-10-01

Uniform and crack free Tb3+ doped lutetium oxide (Lu2O3:Tb) films were prepared by Pechini sol-gel method combined with the spin-coating technique. The influence of the different substrate (monocrystalline silicon (111) and silica glass) and atmosphere (N2 and Air) on the luminescence properties of films was investigated. According to the emission spectra, we found that the luminous intensity was higher on silica glass substrate. Moreover, it was found that the luminous intensity calcined in N2 was higher almost twice as that calcined in air.

Luminescence properties of Lu2O3: Tb film prepared by Pechini sol-gel method

NASA Astrophysics Data System (ADS)

Shen, Siqing; Wang, Jian; Xu, Zhibin; Xie, Jianjun; Shi, Ying

2011-02-01

Uniform and crack free Tb3+ doped lutetium oxide (Lu2O3:Tb) films were prepared by Pechini sol-gel method combined with the spin-coating technique. The influence of the different substrate (monocrystalline silicon (111) and silica glass) and atmosphere (N2 and Air) on the luminescence properties of films was investigated. According to the emission spectra, we found that the luminous intensity was higher on silica glass substrate. Moreover, it was found that the luminous intensity calcined in N2 was higher almost twice as that calcined in air.

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.

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).

Method for storage of solid waste

DOEpatents

Mecham, William J.

1976-01-01

Metal canisters for long-term storage of calcined highlevel radioactive wastes can be made self-sealing against a breach in the canister wall by the addition of powdered cement to the canister with the calcine before it is sealed for storage. Any breach in the canister wall will permit entry of water which will mix with the cement and harden to form a concrete patch, thus sealing the opening in the wall of the canister and preventing the release of radioactive material to the cooling water or atmosphere.

Speciation of residual carbon contained in UO{sub 2}

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

Ziouane, Yannis; Arab-Chapelet, Bénédicte; Tamain, Christelle

2016-12-15

UO{sub 2} powders were synthesized thanks to oxalic precipitation (platelet morphology) and sol-gel route and completely characterized. A secondary phase was found depending on the calcination atmospheres. This phase has been identified by Raman spectroscopy as graphitic material (i.e. carbon-based secondary compound) and quantified by thermogravimetric analyses. Its amount varies with the calcination atmosphere. The presence of this secondary phase has no significant effect on the lattice parameter and its specific surface area. - Graphical abstract: Figure 2: Raman spectroscopy of the three UO{sub 2} powders and of the dissolution residues.

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

Small-scale studies of roasted ore waste reveal extreme ranges of stable mercury isotope signatures

NASA Astrophysics Data System (ADS)

Smith, Robin S.; Wiederhold, Jan G.; Jew, Adam D.; Brown, Gordon E.; Bourdon, Bernard; Kretzschmar, Ruben

2014-07-01

Active and closed Hg mines are significant sources of Hg contamination to the environment, mainly due to large volumes of mine waste material disposed of on-site. The application of Hg isotopes as source tracer from such contaminated sites requires knowledge of the Hg isotope signatures of different materials potentially released to the environment. Previous work has shown that calcine, the waste residue of the on-site ore roasting process, can exhibit distinct Hg isotope signatures compared with the primary ore. Here, we report results from a detailed small-scale study of Hg isotope variations in calcine collected from the closed New Idria Hg mine, San Benito County, CA, USA. The calcine samples exhibited different internal layering features which were investigated using optical microscopy, micro X-ray fluorescence, micro X-ray absorption spectroscopy (μ-XAS), and stable Hg isotope analysis. Significant Fe, S, and Hg concentration gradients were found across the different internal layers. Isotopic analyses revealed an extreme variation with pronounced isotopic gradients across the internal layered features. Overall, δ202Hg (±0.10‰, 2 SD) describing mass-dependent fractionation (MDF) ranged from -5.96 to 14.49‰, which is by far the largest range of δ202Hg values reported for any environmental sample. In addition, Δ199Hg (±0.06‰, 2 SD) describing mass-independent fractionation (MIF) ranged from -0.17 to 0.21‰. The μ-XAS analyses suggested that cinnabar and metacinnabar are the dominant Hg-bearing phases in the calcine. Our results demonstrate that the incomplete roasting of HgS ores in Hg mines can cause extreme mass-dependent Hg isotope fractionations at the scale of individual calcine pieces with enrichments in both light and heavy Hg isotopes relative to the primary ore signatures. This finding has important implications for the application of Hg isotopes as potential source tracers for Hg released to the environment from closed Hg mines and

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.

Biosynthesis of amorphous mesoporous aluminophosphates using yeast cells as templates

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

Sifontes, Ángela B., E-mail: asifonte@ivic.gob.ve; González, Gema; Tovar, Leidy M.

2013-02-15

Graphical abstract: Display Omitted Highlights: ► Amorphous aluminophosphates can take place using yeast as template. ► A mesoporous material was obtained. ► The specific surface area after calcinations ranged between 176 and 214 m{sup 2} g{sup −1}. -- Abstract: In this study aluminophosphates have been synthesized from aluminum isopropoxide and phosphoric acid solutions using yeast cells as template. The physicochemical characterization was carried out by thermogravimetric analysis; X-ray diffraction; Fourier transform infrared; N{sub 2} adsorption–desorption isotherms; scanning electron microscopy; transmission electron microscopy and potentiometric titration with N-butylamine for determination of: thermal stability; crystalline structure; textural properties; morphology and surface acidity,more » respectively. The calcined powders consisted of an intimate mixture of amorphous and crystallized AlPO particles with sizes between 23 and 30 nm. The average pore size observed is 13–16 nm and the specific surface area after calcinations (at 650 °C) ranged between 176 and 214 m{sup 2} g{sup −1}.« less

Fe K-Edge X-ray absorption near-edge spectroscopy (XANES) and X-ray diffraction (XRD) analyses of LiFePO4 and its base materials

NASA Astrophysics Data System (ADS)

Latif, C.; Negara, V. S. I.; Wongtepa, W.; Thamatkeng, P.; Zainuri, M.; Pratapa, S.

2018-03-01

XANES analysis has been performed with the aim of knowing the Fe oxidation state in a synthesized LiFePO4 and its base materials. XANES measurements were performed at SLRI on energy around Fe K-edge. An XRD analysis has also been performed with the aim of knowing the phase composition, lattice parameters and crystallite size of the LiFePO4 as well as the base materials. From the XRD analysis, it was found that the dominating phase in the iron sand sample was Fe3O4 and the only phase found after calcination was LiFePO4. The latter phase exhibited crystallite size of 100 nm and lattice parameters a = 10.169916 Å, b = 5.919674 Å, c = 4.627893 Å. Qualitative analysis of XANES data revealed that the oxidation number of Fe in the sample before calcination was greater than that after calcination and Fe in the natural iron sand, indicated by the E0 values of 7129.2 eV, 7120.6 eV and 7124.4 eV respectively.

Mercury in soil near a long-term air emission source in southeastern Idaho

USGS Publications Warehouse

Abbott, M.L.; Susong, D.D.; Olson, M.; Krabbenhoft, D.P.

2003-01-01

At the Idaho National Engineering and Environmental Laboratory in southeastern Idaho, a 500??C fluidized bed calciner was intermittently operated for 37 years, with measured Hg emission rates of 9-11 g/h. Surface soil was sampled at 57 locations around the facility to determine the spatial distribution of Hg fallout and surface Hg variability, and to predict the total residual Hg mass in the soil from historical emissions. Measured soil concentrations were slightly higher (p<0.05) within 5 km of the source but were overall very low (15-20 ng/g) compared to background Hg levels published for similar soils in the USA (50-70 ng/g). Concentrations decreased 4%/cm with depth and were found to be twice as high under shrubs and in depressions. Mass balance calculations accounted for only 2.5-20% of the estimated total Hg emitted over the 37-year calciner operating history. These results suggest that much of the Hg deposited from calciner operations may have been reduced in the soil and re-emitted as Hg(0) to the global atmospheric pool.

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.

Microwave-Assisted Synthesis of High Dielectric Constant CaCu3Ti4O12 from Sol-Gel Precursor

NASA Astrophysics Data System (ADS)

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

2015-07-01

CaCu3Ti4O12 (CCTO) powders derived from sol-gel precursors were calcined and sintered via microwave radiation. The obtained CCTO powders were compared with that obtained via a conventional heating method. For microwave heating, 89.1 wt.% CCTO was achieved from the sol-gel precursor, after only 17 min at 950°C. In contrast, the conventional calcination method required 3 h to generate 87.6 wt.% CCTO content at 1100°C. In addition, the CCTO powders prepared through 17 min of microwave calcination exhibited a small particle size distribution of D50 = 3.826 μm. It was found that a lengthy hold time of 1 h by microwave sintering is required to obtain a high dielectric constant (3.14 × 103 at 102 Hz) and a reasonably low dielectric loss (0.161) in the sintered CCTO ceramic. Based upon the distinct microstructures, the dielectric responses of the CCTO samples sintered by different methods are attributed to space charge polarization and internal barrier layer capacitor mechanism.

Hydrogen sulfide capture by limestone and dolomite at elevated pressure. 2: Sorbent particle conversion modeling

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

Zevenhoven, C.A.P.; Yrjas, K.P.; Hupa, M.M.

1996-03-01

The physical structure of a limestone or dolomite to be used in in-bed sulfur capture in fluidized bed gasifiers has a great impact on the efficiency of sulfur capture and sorbent use. In this study an unreacted shrinking core model with variable effective diffusivity is applied to sulfidation test data from a pressurized thermogravimetric apparatus (P-TGA) for a set of physically and chemically different limestone and dolomite samples. The particle size was 250--300 {micro}m for all sorbents, which were characterized by chemical composition analysis, particle density measurement, mercury porosimetry, and BET internal surface measurement. Tests were done under typical conditionsmore » for a pressurized fluidized-bed gasifier, i.e., 20% CO{sub 2}, 950 C, 20 bar. At these conditions the limestone remains uncalcined, while the dolomite is half-calcined. Additional tests were done at low CO{sub 2} partial pressures, yielding calcined limestone and fully calcined dolomite. The generalized model allows for determination of values for the initial reaction rate and product layer diffusivity.« less

MgCoAl and NiCoAl LDHs synthesized by the hydrothermal urea hydrolysis method: Structural characterization and thermal decomposition

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

Chagas, L.H., E-mail: lhchagas-prometro@inmetro.gov.br; Instituto Nacional de Metrologia Qualidade e Tecnologia, Divisão de Metrologia de Materiais, 25250-020 Duque de Caxias, RJ; De Carvalho, G.S.G.

Highlights: • We synthesized MgCoAl and NiCoAl LDHs by the urea hydrolysis method. • Aluminum rich and crystalline materials have been formed. • The calcination of the LDHs generated mixed oxides with high surface areas. - Abstract: Layered double hydroxides (LDHs) with Mg/Co/Al and Ni/Co/Al were synthesized for the first time by the urea hydrolysis method. The experimental conditions promoted aluminum rich and crystalline materials. The formation of LDHs was investigated by powder X-ray diffraction (XRD), chemical analysis, solid state nuclear magnetic resonance with magic angle spinning ({sup 27}Al-MAS-NMR), simultaneous thermogravimetric/differential thermal analysis (TGA/DTA), FTIR spectroscopy, scanning electron microscopy (SEM),more » and N{sub 2} adsorption–desorption experiments. A single phase corresponding to LDH could be obtained in all the investigated compositions. Thermal calcination of these LDHs at 500 °C resulted in the formation of solid solutions in which Al{sup 3+} was dissolved. All the calcined materials have rock-salt like structures and high surface areas.« less

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

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.

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.

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.

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.

Removing heavy metals from wastewaters with use of shales accompanying the coal beds.

PubMed

Jabłońska, Beata; Siedlecka, Ewa

2015-05-15

A possibility of using clay waste rocks (shales) from coal mines in the removal of heavy metals from industrial wastewaters is considered in this paper. Raw and calcined (600 °C) shales accompanying the coal beds in two Polish coal mines were examined with respect to their adsorptive capabilities for Pb, Ni and Cu ions. The mineralogical composition of the shales was determined and the TG/DTG analysis was carried out. The granulometric compositions of raw and calcined shales were compared. Tests of adsorption for various Pb(II), Ni(II) and Cu(II) concentrations were conducted and the pH before and after adsorption was analyzed. The results indicate that the shales from both coal mines differ in adsorptive capabilities for particular metal ions. The calcination improved the adsorptive capabilities for lead, but worsened them for nickel. The examined shales have good adsorptive capabilities, and could be used as inexpensive adsorbents of heavy metal ions, especially in the regions where resources of shale are easy accessible in the form of spoil tips. Copyright © 2015 Elsevier Ltd. All rights reserved.

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.

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.

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.

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.

Influence of thermally activated paper sludge on the behaviour of blended cements subjected to saline and non-saline environments.

PubMed

García, Rosario; Rubio, Virginia; Vegas, Iñigo; Frías, Moisés

2009-05-01

One of the problems to affect Portland cement matrices is low resistance to aggressive agents, due principally to the presence of a high content of portlandite in the hydrated cements. Pozzolanic materials have played an important role in the improving the durability of cement-based materials for decades. This work studies the behaviour of cement mortar matrices blended with 10% calcined paper sludge (source for metakaolinite) and exposed to different environmental conditions (saline and non-saline environments) after 6 and 12 months of exposure. Two cements were studied: an ordinary Portland cement (CEM 1, 42.5R), acting as reference cement, and a blended cement formulated by mixing 90% (by mass) of CEM 1, 42.5R with 10% (by mass) of paper sludge calcined at 700 degrees C for 2 h. The specimens were exposed 1 year to saline and non-saline environments. All the mineralogy samples were studied through X-ray diffraction and scanning electron microscopy (SEM) equipped with an energy dispersive X-ray analyser. The in-depth study on ionic mobility was performed on samples subjected to natural exposure (coast and tableland) for 6 and 12 months. Portland cement was composed of quartz, calcite, calcium hydroxide and tobermorite gels. The pozzolanic cement (10% calcined paper sludge) is of the same composition but a high calcite concentration and barium carbonate. SEM analysis from coastline show deposits of variable composition. The deposits are identified on the surface of different mineral components. The minerals from tableland are much fractured, i.e. calcite and feldspars. Inside the fractures, the deposits and the ions are located and trapped superficially. SEM analysis of control cement Portland and 10% calcined paper sludge shows deposits on quartz and calcite with a very high concentration of Pb, Zn, Cl and barium sulphate. A very porous aspect is due to the presence of the different aggregate types. This porous configuration permits retention of the ion

Stable mercury isotope ratios as tracers for Hg cycling at the inoperative New Idria Hg mine, California

NASA Astrophysics Data System (ADS)

Wiederhold, J. G.; Jew, A. D.; Brown, G. E.; Bourdon, B.; Kretzschmar, R.

2010-12-01

The seven stable isotopes of Hg are fractionated in the environment as a result of mass-dependent (MDF) and mass-independent (MIF) fractionation processes that can be studied in parallel by analyzing the ratios of even and odd mass Hg isotopes. MDF and MIF Hg isotope signatures of natural samples may provide a new tool to trace sources and transformations in environmental Hg cycling. However, the mechanisms controlling the extent of kinetic and equilibrium Hg isotope fractionations are still only partially understood. Thus, development of this promising tracer requires experimental calibration of relevant fractionation factors as well as assessment of natural variations of Hg isotope ratios under different environmental conditions. The inoperative Hg mine in New Idria (California, USA) represents an ideal case study to explore Hg isotope fractionation during Hg transformation and transport processes. More than a century of Hg mining and on-site thermal refining to obtain elemental Hg until 1972 produced large volumes of contaminated mine wastes which now represent sources of Hg pollution for the surrounding ecosystems. Here, we present Hg isotope data from various materials collected at New Idria using Cold-Vapor-MC-ICPMS with a long-term δ202Hg reproducibility of ±0.1‰ (2SD). Uncalcined mine waste samples were isotopically similar to NIST-3133 and did not exhibit any MIF signatures. In contrast, calcine samples, which represent the residue of the thermal ore processing at 700°C, had significantly heavier δ202Hg values of up to +1.5‰. In addition, we observed small negative MIF anomalies of the odd-mass Hg isotopes in the calcine samples, which could be caused either by nuclear volume fractionation or a magnetic isotope effect during or after the roasting process. The mass-dependent enrichment of heavy Hg isotopes in the calcine materials indicates that light Hg isotopes were preferentially removed during the roasting process, in agreement with a previous

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

High strength yttria-reinforced HA scaffolds fabricated via honeycomb ceramic extrusion.

PubMed

Elbadawi, M; Shbeh, M

2018-01-01

The present study investigated the effects of hydroxyapatite (HA) reinforced with yttria on porous scaffolds fabricated via honeycomb ceramic extrusion. Yttria was selected as it has been demonstrated to toughen other ceramics. Moreover, yttria has been surmised to suppress dehydroxylation in HA, a characteristic that prefigures decomposition thereof during sintering into mechanically weaker phases. However, the compressive strength of yttria-reinforced hydroxyapatite (Y-HA) porous scaffolds has hitherto not been reported. Y-HA was synthesised by calcining a commercially available HA with 10wt% yttria at 1000°C. Y-HA was then fabricated into porous scaffolds using an in-house honeycomb extruder, and subsequently sintered at 1200 and 1250°C. The results were compared to the uncalcined as-received commercial powder (AR-HA) and calcined pure HA powder at 1000°C (C-HA). It was discovered that calcination alone caused marked improvements to the stoichiometry, thermal stability, porosity and compressive strength of scaffolds. The improvements were ascribed to the calcined powders with less susceptibility to both agglomeration and enhanced densification. Still, differences were observed between C-HA and Y-HA at 1250°C. The compressive strength increased from 105.9 to 127.3MPa, a larger microporosity was descried and the HA matrix in Y-HA was more stoichiometric. The latter was confirmed by XRD and EDS analyses. Therefore, it was concluded that the reinforcing of hydroxyapatite with yttria improved the compressive strength and suppressed dehydroxylation of porous HA scaffolds. In addition, the compressive strength achieved demonstrated great potential for load-bearing application. Copyright © 2017 Elsevier Ltd. All rights reserved.

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).

[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.

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.

Gamma-radiolytic preparation of multi-component oxides

NASA Astrophysics Data System (ADS)

Procházková, Lenka; Bárta, Jan; Čuba, Václav; Ekberg, Christian; Tietze, Sabrina; Jakubec, Ivo

2016-07-01

The preparation of solid precursors to Zn1-xCdxO and (Lu,Y)3Al5O12:Ce induced by 60Co gamma-ray irradiation of aqueous solutions containing soluble metal salts and ammonium formate is presented. Due to the irradiation, crystalline zinc carbonate hydroxide Zn4(CO3)(OH)6·H2O or amorphous carbonates of Lu, Y and Al were formed in the solutions. After calcination at 500 °C, the agglomerated phase-pure Zn1-xCdxO with crystallite size about 50 nm was obtained if the Cd concentration in solutions remained below 16 M% (with respect to Zn) with x being up to 0.035. The solid precursors to garnets contained the intended concentration of all elements, according to X-ray fluorescence analysis. After calcination at 1200 °C in mild vacuum, the respective phase-pure garnets with crystallite size 100 nm or their solid solution were produced when the Ce dopation was kept below 2 M% (with respect to rare-earth metals). The Ce solubility in the garnet lattice was estimated as 1-2 M% at the calcination conditions used.

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.

Facile Synthesis of Platelike Hierarchical Li1.2Mn0.54Ni0.13Co0.13O2 with Exposed {010} Planes for High-Rate and Long Cycling-Stable Lithium Ion Batteries.

PubMed

Zeng, Jiong; Cui, Yanhui; Qu, Deyang; Zhang, Qian; Wu, Junwei; Zhu, Xiaomeng; Li, Zuohua; Zhang, Xinhe

2016-10-05

Lithium-rich layered oxides are promising cathode candidates for the production of high-energy and high-power electronic devices with high specific capacity and high discharge voltage. However, unstable cycling performance, especially at high charge-recharge rate, is the most challenge issue which needs to be solved to foster the diffusion of these materials. In this paper, hierarchical platelike Li 1.2 Mn 0.54 Ni 0.13 Co 0.13 O 2 cathode materials were synthesized by a facile solvothermal method followed by calcination. Calcination time was found to be a key parameter to obtain pure layered oxide phase and tailor its hierarchical morphology. The Li-rich material consists of primary nanoparticles with exposed {010} planes assembled to form platelike layers which exhibit low resistance to Li + diffusion. In detail, the product by calcination at 900 °C for 12 h exhibits specific capacity of 228, 218, and 204 mA h g -1 at 200, 400, and 1000 mA g -1 , respectively, whereas after 100 cycles at 1000 mA g -1 rate of charge and recharge the specific capacity was retained by about 91%.

Process for vitrification of contaminated sodium oxide

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

Blair, H.T.; Mellinger, G.B.

1983-03-01

A glass composition was developed to accommodate 30 wt % sodium oxide and resist devitrification and leaching. An in-can melting process that is compatible with a comtaminated sodium calciner developed by Argonne National Laboratory was tested both on a laboratory and on an engineering scale and found to be viable. The Liquid Metal Fast Breeder Reactor experimental program continues to produce elemental sodium contaminated with radionuclides. This material is presently in temporary storage facilities because the current criterion will not permit alkali metals to be disposed of in shallow land burials. As a first step in treatment, Argonne National Laboratorymore » (ANL) has developed a calciner that will convert the sodium metal to an oxide. In work supported by the U.S. Department of Energy, Pacific Northwest Laboratory (PNL) is developing and demonstrating a process that is compatible with the calciner and facilities at ANL-West for incorporating sodium oxide into a glass. Glass, which normally contains sodium oxide, was chosen as the waste form because it is chemically durable and nondispersible. It is simple to produce, and the technology for incorporating nuclear wastes into glass is well developed.« less

Synthesis, structure and magnetic properties of porous magnetic composite, based on MCM-41 molecular sieve with Fe{sub 3}O{sub 4} nanoparticles

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

Kolotilov, Sergey V.; Shvets, Oleksiy; Cador, Olivier

2006-08-15

Porous magnetic composites were prepared by the synthesis of molecular sieve MCM-41 in the presence of Fe{sub 3}O{sub 4} nanoparticles with average diameter of 15 nm. Nanoparticles were captured by porous silica matrix MCM-41, which resulted in their incorporation, as it was confirmed by TEM, SEM and X-ray diffraction. The materials possessed high surface area (392-666 m{sup 2} g{sup -1}), high pore volume (0.39-0.73 cm{sup 3} g{sup -1}) along with high magnetic response (M {sub S} up to 28.4 emu g{sup -1} at 300 K). Calcination of samples resulted in partial oxidation of Fe{sub 3}O{sub 4} to {alpha}-Fe{sub 2}O{sub 3}.more » The influence of nanoparticles content on sorption and magnetic properties of the composites was shown. No hysteresis was found for the samples at 300 K; at 5 K, H {sub C} was in the range 370-385 G for non-calcinated samples and 350-356 G for calcinated ones. - Graphical abstract: Schematic presentation of MCM-41/Fe{sub 3}O{sub 4} composite.« less

Exceptional capability of nanosized CeO(2) materials to "dissolve" lanthanide oxides established by time-gated excitation and emission spectroscopy.

PubMed

Tiseanu, Carmen; Parvulescu, Vasile; Avram, Daniel; Cojocaru, Bogdan; Sanchez-Dominguez, Margarita

2014-05-28

The atomic scale homogeneity of Ce and Zr oxygen bonds represents the main reason for enhanced total oxygen storage capability of CeO2-ZrO2 (Ce/Zr = 1) as compared to that of CeO2. Here, we demonstrate that the addition of 10% Eu(3+) by wet impregnation on preformed nanosized CeO2-ZrO2 (Ce/Zr = 1) followed by calcination induces a remarkable homogeneity of 10% Eu(3+)-CeO2-ZrO2 solid solution. By use of time-resolved emission and excitation spectroscopies, the improvement of the nanoscale chemical and structural homogeneity of 10% Eu(3+)-CeO2-ZrO2 calcined at 1000 as compared to sample calcined at 750 °C is demonstrated. Based on the comparison of luminescence properties of 10% Eu(3+) impregnated on preformed nanosized CeO2-ZrO2 and CeO2, we also show that the presence of zirconium does not only preserve the ability of cerium oxide to "dissolve" lanthanide oxide, but also determines an important stabilization of defects (oxygen vacancies) generated upon Eu(3+) doping.

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.

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.

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.

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.

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).

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.

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.

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.

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.

Application of silica-supported Fe-Cu nanoparticles in the selective hydrogenation of p-dinitrobenzene to p-phenylenediamine

NASA Astrophysics Data System (ADS)

Shesterkina, A. A.; Shuvalova, E. V.; Kirichenko, O. A.; Strelkova, A. A.; Nissenbaum, V. D.; Kapustin, G. I.; Kustov, L. M.

2017-02-01

Supported bimetallic Fe-Cu/SiO2 materials are synthesized, and their catalytic activity in hydrogenation of dinitrobenzene to phenylenediamine at 145-180°C and 1.3 MPa hydrogen pressure is studied for the first time. The best results (89% selectivity toward p-phenylenediamine at complete conversion of p-dinitrobenzene) are obtained for the sample synthesized via co-deposition with subsequent calcination at 300°C. The sample contains 7% iron and 3% copper. The formation of separate phases of metal oxides (for the catalysts prepared by impregnation) and mixed bimetallic oxide phases (in case of co-deposition procedure) in calcined samples is revealed via thermoprogrammed reduction with hydrogen.

Insights into the Formation and Properties of Templated Dual Mesoporous Titania with Enhanced Photocatalytic Activity.

PubMed

Naboulsi, Issam; Lebeau, Bénédicte; Michelin, Laure; Carteret, Cédric; Vidal, Loic; Bonne, Magali; Blin, Jean-Luc

2017-01-25

The one pot synthesis of dual mesoporous titania (2.3 and 7.7 nm) has been achieved from a mixture of fluorinated and Pluronic surfactants. The small and large mesopore networks are templated, respectively, by a fluorinated-rich liquid crystal and a Pluronic-rich liquid crystal, which are in equilibrium. After calcination at 350 °C, the amorphous walls are transformed into semicrystalline anatase preserving the mesoporous structure. Results concerning the photodegradation of methyl orange using the calcined photocatalysts highlight that the kinetic rate constant (k) determined for the dual mesoporous titania is 2.6 times higher than the k value obtained for the monomodal ones.

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.

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.

ICPP tank farm closure study. Volume 1

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

Spaulding, B.C.; Gavalya, R.A.; Dahlmeir, M.M.

1998-02-01

The disposition of INEEL radioactive wastes is now under a Settlement Agreement between the DOE and the State of Idaho. The Settlement Agreement requires that existing liquid sodium bearing waste (SBW), and other liquid waste inventories be treated by December 31, 2012. This agreement also requires that all HLW, including calcined waste, be disposed or made road ready to ship from the INEEL by 2035. Sodium bearing waste (SBW) is produced from decontamination operations and HLW from reprocessing of SNF. SBW and HLW are radioactive and hazardous mixed waste; the radioactive constituents are regulated by DOE and the hazardous constituentsmore » are regulated by the Resource Conservation and Recovery Act (RCRA). Calcined waste, a dry granular material, is produced in the New Waste Calcining Facility (NWCF). Two primary waste tank storage locations exist at the ICPP: Tank Farm Facility (TFF) and the Calcined Solids Storage Facility (CSSF). The TFF has the following underground storage tanks: four 18,400-gallon tanks (WM 100-102, WL 101); four 30,000-gallon tanks (WM 103-106); and eleven 300,000+ gallon tanks. This includes nine 300,000-gallon tanks (WM 182-190) and two 318,000 gallon tanks (WM 180-181). This study analyzes the closure and subsequent use of the eleven 300,000+ gallon tanks. The 18,400 and 30,000-gallon tanks were not included in the work scope and will be closed as a separate activity. This study was conducted to support the HLW Environmental Impact Statement (EIS) waste separations options and addresses closure of the 300,000-gallon liquid waste storage tanks and subsequent tank void uses. A figure provides a diagram estimating how the TFF could be used as part of the separations options. Other possible TFF uses are also discussed in this study.« less

Unraveling the Structure of Mn-Promoted Co/TiO2 Fischer-Tropsch Catalysts by In Situ X-Ray Absorption Spectroscopy

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

Grandjean, Didier; Morales, Fernando; Mens, Ad

2007-02-02

Combination of in situ X-ray absorption spectroscopy (XAFS) at the Co and Mn K-edges with electron microscopy (STEM-EELS) has allowed to unravel the complex structure of a series of unpromoted and Mn promoted TiO2-supported cobalt Fischer-Tropsch catalysts prepared by homogeneous deposition precipitation (HDP), both in their calcined and reduced states. After calcination the catalysts are generally composed of large Co3O4 aggregates (13-20 nm) and a MnO2-type phase that is either dispersed on the TiO2 surface or, for the major part, covering the Co3O4 particles. Additionally Mn is also forming a spinel-type Co3-xMnxO4 solid solution at the surface of the Co3O4more » particles. In pure Co or when small amount of this spinel-type phase are formed during calcination, reduction in H2 at 350 deg. C produces Co0 particles of variable sizes (3.5-15 nm) otherwise Co reduction is limited to the Co2+ state. Manganese that exists entirely in a Mn2+ state in the reduced catalysts is forming (1) a highly dispersed Ti2MnO4-type phase at the TiO2 surface, (2) a less dispersed MnO phase close to the cobalt particles that coexists with (3) a rock salt-type Mn1-xCoxO solid solution. Similarly, large amount of spinel solid solution in the calcined state favors the formation of Mn1-xCoxO-type solid solution during reduction showing that one of the main roles of the Mn promoter is to limit Co reducibility.« less

Performance of a novel synthetic Ca-based solid sorbent suitable for desulfurizing flue gases in a fluidized bed

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

Pacciani, R.; Muller, C.R.; Davidson, J.F.

2009-08-05

The extent and mechanism of sulfation and carbonation of limestone, dolomite, and chalk, were compared with a novel, synthetic sorbent (85 wt % CaO and 15 wt % Ca{sub 12}A{sub l14}O{sub 33}), by means of experiments undertaken in a small, electrically heated fluidized bed. The sorbent particles were used either (I) untreated, sieved to two particle sizes and reacted with two different concentrations of SO{sub 2}, or (ii) after being cycled 20 times between carbonation, in 15 vol % CO{sub 2} in N2, and calcination, in pure N2, at 750 degrees C. The uptake of untreated limestone and dolomite wasmore » generally low (<0.2 g(SO{sub 2})/g(sorbent)), confirming previous results, However, the untreated chalk and the synthetic sorbent were found to be substantially more reactive with SO{sub 2}, and their final uptake was significantly higher (>0.5 g(SO{sub 2})/g(sorbent)) and essentially independent of the particle size. Here, comparisons are made on the basis of the sorbents in the calcined state. The capacities for the uptake of SO{sub 2}, on a basis of unit mass of calcined sorbent, were comparable for the chalk and the synthetic sorbent. However, previous work has demonstrated the ability of the synthetic sorbent to retain its capacity for CO{sub 2} over many cycles of carbonation and calcination: much more so than natural sorbents such as chalk and limestone. Accordingly, the advantage of the synthetic sorbent is that it could be used to remove CO{sub 2} from flue gases and, at the end of its life, to remove SO{sub 2} on a once-through basis.« less

Mercury Methylation at Mercury Mines In The Humboldt River Basin, Nevada, USA

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

Gray, John E.; Crock, James G.; Lasorsa, Brenda K.

2002-12-01

Total Hg and methylmercury concentrations were measured in mine-waste calcines (retorted ore), sediment, and water samples collected in and around abandoned mercury mines in western Nevada to evaluate Hg methylation at the mines and in the Humboldt River basin. Mine-waste calcines contain total Hg concentrations as high as 14 000?g/g. Stream-sediment samples collected within 1 km of the mercury mines contain total Hg concentrations as high as 170?g/g, whereas stream sediments collected>5 km from the mines, and those collected from the Humboldt River and regional baseline sites, contain total Hg concentrations<0.5?g/g. Similarly, methylmercury concentrations in mine-waste calcines are locally asmore » high as 96 ng/g, but methylmercury contents in stream-sediments collected downstream from the mines and from the Humboldt River are lower, ranging from<0.05 to 0.95 ng/g. Stream-water samples collected below two mines studied contain total Hg concentrations ranging from 6 to 2000 ng/L, whereas total Hg in Humboldt River water was generally lower ranging from 2.1 to 9.0 ng/L. Methylmercury concentrations in the Humboldt River water were the lowest in this study (<0.02-0.27 ng/L). Although total Hg and methylmercury concentrations are locally high in mine-waste calcines, there is significant dilution of Hg and lower Hg methylation down gradient from the mines, especially in the sediments and water collected from the Humboldt River, which is> 8 km from any mercury mines. Our data indicate little transference of Hg and methylmercury from the sediment to the water column due to the lack of mine runoff in this desert climate.« 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

Efficacy assessment of acid mine drainage treatment with coal mining waste using Allium cepa L. as a bioindicator.

PubMed

Geremias, Reginaldo; Bortolotto, Tiago; Wilhelm-Filho, Danilo; Pedrosa, Rozangela Curi; de Fávere, Valfredo Tadeu

2012-05-01

The aim of this study was to evaluate the efficacy of the treatment of acid mine drainage (AMD) with calcinated coal mining waste using Allium cepa L. as a bioindicator. The pH values and the concentrations of aluminum, iron, manganese, zinc, copper, lead and sulfate were determined before and after the treatment of the AMD with calcinated coal mining waste. Allium cepa L. was exposed to untreated and treated AMD, as well as to mineral water as a negative control (NC). At the end of the exposure period, the inhibition of root growth was measured and the mean effective concentration (EC(50)) was determined. Oxidative stress biomarkers such as lipid peroxidation (TBARS), protein carbonyls (PC), catalase activity (CAT) and reduced glutathione levels (GSH) in the fleshy leaves of the bulb, as well as the DNA damage index (ID) in meristematic cells, were evaluated. The results indicated that the AMD treatment with calcinated coal mining waste resulted in an increase in the pH and an expressive removal of aluminum, iron, manganese and zinc. A high sub-chronic toxicity was observed when Allium cepa L. was exposed to the untreated AMD. However, after the treatment no toxicity was detected. Levels of TBARS and PC, CAT activity and the DNA damage index were significantly increased (P<0.05) in Allium cepa L. exposed to untreated AMD when compared to treated AMD and also to negative controls. No significant alteration in the GSH content was observed. In conclusion, the use of calcinated coal mining waste associated with toxicological tests on Allium cepa L. represents an alternative system for the treatment and biomonitoring of these types of environmental contaminants. Copyright © 2011 Elsevier Inc. All rights reserved.

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.

Characterization of the enhancement effect of Na2CO3 on the sulfur capture capacity of limestones.

PubMed

Laursen, Karin; Kern, Arnt A; Grace, John R; Lim, C Jim

2003-08-15

It has been known for a long time that certain additives (e.g., NaCl, CaCl2, Na2CO3, Fe2O3) can increase the sulfur dioxide capture-capacity of limestones. In a recent study we demonstrated that very small amounts of Na2CO3 can be very beneficial for producing sorbents of very high sorption capacities. This paper explores what contributes to these significant increases. Mercury porosimetry measurements of calcined limestone samples reveal a change in the pore-size from 0.04-0.2 microm in untreated samples to 2-10 microm in samples treated with Na2CO3--a pore-size more favorable for penetration of sulfur into the particles. The change in pore-size facilitates reaction with lime grains throughout the whole particle without rapid plugging of pores, avoiding premature change from a fast chemical reaction to a slow solid-state diffusion controlled process, as seen for untreated samples. Calcination in a thermogravimetric reactor showed that Na2CO3 increased the rate of calcination of CaCO3 to CaO, an effect which was slightly larger at 825 degrees C than at 900 degrees C. Peak broadening analysis of powder X-ray diffraction data of the raw, calcined, and sulfated samples revealed an unaffected calcite size (approximately 125-170 nm) but a significant increase in the crystallite size for lime (approximately 60-90 nm to approximately 250-300 nm) and less for anhydrite (approximately 125-150 nm to approximately 225-250 nm). The increase in the crystallite and pore-size of the treated limestones is attributed to an increase in ionic mobility in the crystal lattice due to formation of vacancies in the crystals when Ca is partly replaced by Na.

Recombinant expression of Intrepicalcin from the scorpion Vaejovis intrepidus and its effect on skeletal ryanodine receptors.

PubMed

Vargas-Jaimes, Leonel; Xiao, Liang; Zhang, Jing; Possani, Lourival D; Valdivia, Héctor H; Quintero-Hernández, Verónica

2017-04-01

Scorpion venoms contain toxins that modulate ionic channels, among which are the calcins, a small group of short, basic peptides with an Inhibitor Cystine Knot (ICK) motif that target calcium release channels/ryanodine receptors (RyRs) with high affinity and selectivity. Here we describe the heterologous expression of Intrepicalcin, identified by transcriptomic analysis of venomous glands from Vaejovis intrepidus. Recombinant Intrepicalcin was obtained in Escherichia coli BL21-DE3 (periplasm) by fusing the Intrepicalcin gene to sequences coding for signal-peptide, thioredoxin, His-tag and enterokinase cleavage site. [ 3 H]Ryanodine binding, used as a functional index of RyR activity, revealed that recombinant Intrepicalcin activates skeletal RyR (RyR1) dose-dependently with K d =17.4±4.0nM. Intrepicalcin significantly augments the bell-shaped [Ca 2+ ]-[ 3 H]ryanodine binding curve at all [Ca 2+ ] ranges, as is characteristic of the calcins. In single channel recordings, Intrepicalcin induces the appearance of a subconductance state in RyR1 with a fractional value ∼55% of the full conductance state, very close to that of Vejocalcin. Furthermore, Intrepicalcin stimulates Ca 2+ release at an initial dose=45.3±2.5nM, and depletes ~50% of Ca 2+ load from skeletal sarcoplasmic reticulum vesicles. We conclude that active recombinant Intrepicalcin was successfully obtained without the need of manual oxidation, enabling it to target RyR1s with high affinity. This is the first calcin heterologously expressed in the periplasma of Escherichia coli BL21-DE3, shown to be pharmacologically effective, thus paving the way for the generation of Intrepicalcin variants that are required for structure-function relationship studies of calcins and RyRs. Copyright © 2017 Elsevier B.V. All rights reserved.

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

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.

Investigation of optical properties of nickel oxide nanostructures using photoluminescence and diffuse reflectance spectroscopy

NASA Astrophysics Data System (ADS)

Siddique, M. Naseem; Ahmed, Ateeq; Ali, T.; Tripathi, P.

2018-05-01

Nickel oxide (NiO) nanoparticles with a crystal size of around 16.26 nm have been synthesized via sol-gel method. The synthesized precursor was calcined at 600 °C for 4 hours to obtain the nickel oxide nanoparticles. The XRD analysis result indicated that the calcined sample has a cubic structure without any impurity phases. The FTIR analysis result confirmed the formation of NiO. The NiO nanoparticle exhibited absorption band edge at 277.27 nm and the optical band gap have been estimated approximately 4.47 eV using diffuse reflectance spectroscopy and photoluminescence emission spectrum of our as-synthesized sample showed strong peak at 3.65 eV attributed to the band edge transition.

Nanometric study of nickel oxide prepared by sol gel process

NASA Astrophysics Data System (ADS)

Dessai, R. Raut; Desa, J. A. E.; Sen, D.; Babu, P. D.

2018-04-01

Nickel oxide nanopowder was synthesized by sol gel method using nickel nitrate as the starting material. Nickel oxide nanoparticles with a grain size of 15-90 nm have been studied by; small angle neutron scattering; scanning electron microscopy; and vibrating sample magnetometry. A combination of Ferro and paramagnetic behaviour of the particles after calcination at 800 °C is observed while for powder calcined at 400 °C, soft magnetic character with saturation is seen. The system of nanoparticles ofNiO embedded in a silica matrix is also studied for the structural change. Weak magnetic ordering is observed in this case with the likely-hood of particles being evenly distributed in the silica.

Environmental evaluation of alternatives for long-term management of Defense high-level radioactive wastes at the Idaho Chemical Processing Plant

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

Not Available

1982-09-01

The U.S. Department of Energy (DOE) is considering the selection of a strategy for the long-term management of the defense high-level wastes at the Idaho Chemical Processing Plant (ICPP). This report describes the environmental impacts of alternative strategies. These alternative strategies include leaving the calcine in its present form at the Idaho National Engineering Laboratory (INEL), or retrieving and modifying the calcine to a more durable waste form and disposing of it either at the INEL or in an offsite repository. This report addresses only the alternatives for a program to manage the high-level waste generated at the ICPP. 24more » figures, 60 tables.« less

Research on the Treatment of Wastewater by Waste Ceramic Adsorption

NASA Astrophysics Data System (ADS)

He, Lingfeng; Zhang, Yongli; Shi, Liang

2018-03-01

The process of preparing porous ceramic with waste porcelain powder as aggregate was researched. The affect of assimilate time on cuprum removal efficiency in wastewater containing copper was investigated. The results show the water copper removal rate increased along with the augment of assimilate time, and the assimilate time is suitable for 35 min; XRD characterizations show the porous ceramic catalyst before and after calcination in active components of X ray diffraction peak position almost had no changes, and the diffraction intensity slightly changed with calcination and absorption, and diffraction peaks became sharper, and its crystallinity was improved. Baking leads to the growth of crystal particles, and the performance of porous ceramics is stable before and after adsorption.

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.

Preparation of hydroxyapatite from animal bones.

PubMed

Sobczak, Agnieszka; Kowalski, Zygmunt; Wzorek, Zbigniew

2009-01-01

This paper presents the method of obtaining hydroxyapatite from animal bones. Bone sludge and calcined products were characterized by X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). Calcium concentration was determined with titration, and phosphorus--spectrophotometrically. Making use of the AAS and ICP methods the content of microelements was determined. In all the products, hydroxyapatite was the only crystalline phase indicated. The FT-IR spectra confirmed that calcination removed the total of organic substances. Calcium and phosphorus contents were 38% and 18%, respectively, which corresponded to the Ca/P molar ratio of nonstoichiometric hydroxyapatite. The specific surfaces of products were measured by BET method. The volume of micro- and mesopores was determined.

Treatment of petroleum cokes to inhibit coke puffing

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

Orac, T.H.; Quandt, H.C.; Ball, D.R.

1992-06-02

This patent describes apparatus for treating raw petroleum coke particles. It comprises an elongated, cylindrical, calcining kiln having an inlet end and an outlet end; and entrance chamber and a discharge chamber, an elongated, cylindrical, cooler having an inlet end and an outlet end; means defining a retention chamber communicating with the discharge chamber; means defining a hot zone communicating with the retention chamber and the inlet end of the cooler; means for introducing a dry, granulated, puffing inhibitor into the retention chamber in contact with the calcined coke particles; and a coke delivery chamber for collecting the cooled, calcinedmore » coke particles at the outlet end of the cooler.« less

24. CONSTRUCTION PROGRESS VIEW TO NORTHWEST, SHOWING BLOWER BUILDING. INEEL ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

24. CONSTRUCTION PROGRESS VIEW TO NORTHWEST, SHOWING BLOWER BUILDING. INEEL PHOTO NUMBER NRTS-60-4407. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

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.

Shape-Controlled Synthesis of NiCo2 O4 Microstructures and Their Application in Supercapacitors.

PubMed

Xiang, Nannan; Ni, Yonghong; Ma, Xiang

2015-09-01

The shape-controlled synthesis of NiCo2 O4 microstructures through a facile hydrothermal method and subsequent calcinations was explored. By employing CoSO4 , NiSO4 , and urea as the starting reactants, flower-like NiCo2 O4 microstructures were obtained at 100 °C after 5 h without the assistance of any additive and subsequent calcination at 300 °C for 2 h; dumbbell-like NiCo2 O4 microstructures were prepared at 150 °C after 5 h in the presence of trisodium citrate and subsequent calcination at 300 °C for 2 h. The as-prepared NiCo2 O4 microstructures were characterized by X-ray powder diffraction, field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, and (high-resolution) transmission electron microscopy. Both the flower-like and dumbbell-like NiCo2 O4 microstructures could be used as electrode materials for supercapacitors, and they exhibited excellent electrochemical performance, including high specific capacitance, good rate capability, and excellent long-term cycle stability. Simultaneously, the shape-dependent electrochemical properties of the product were investigated. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Morphology-modulation of SnO2 Hierarchical Architectures by Zn Doping for Glycol Gas Sensing and Photocatalytic Applications

NASA Astrophysics Data System (ADS)

Zhao, Qinqin; Ju, Dianxing; Deng, Xiaolong; Huang, Jinzhao; Cao, Bingqiang; Xu, Xijin

2015-01-01

The morphology of SnO2 nanospheres was transformed into ultrathin nanosheets assembled architectures after Zn doping by one-step hydrothermal route. The as-prepared samples were characterized in detail by various analytical techniques including scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and nitrogen adsorption-desorption technique. The Zn-doped SnO2 nanostructures proved to be the efficient gas sensing materials for a series of flammable and explosive gases detection, and photocatalysts for the degradation of methyl orange (MO) under UV irradiation. It was observed that both of the undoped and Zn-doped SnO2 after calcination exhibited tremendous gas sensing performance toward glycol. The response (S = Ra/Rg) of Zn-doped SnO2 can reach to 90 when the glycol concentration is 100 ppm, which is about 2 times and 3 times higher than that of undoped SnO2 sensor with and without calcinations, respectively. The result of photocatalytic activities demonstrated that MO dye was almost completely degraded (~92%) by Zn-doped SnO2 in 150 min, which is higher than that of others (MO without photocatalyst was 23%, undoped SnO2 without and with calcination were 55% and 75%, respectively).

Nonstoichiometric Zn Ferrite and ZnFe2O4/Fe2O3 Composite Spheres: Preparation, Magnetic Properties, and Chromium Removal

NASA Astrophysics Data System (ADS)

Hang, Chun-Liang; Yang, Li-Xia; Sun, Chang-Mei; Liang, Ying

2018-03-01

Monodisperse and porous nonstoichiometric Zn ferrite can be prepared by a solvothermal method. Such non-Zn ferrite was used to be the precursor for synthesis of ZnFe2O4/Fe2O3 composite via calcination at 600°C for 3 h in air. X-ray powder diffractometer (XRD) and Energy Dispersive Spectrometer (EDS) proved the nonstoichiometry of Zn ferrite synthesized by solvothermal method and the formation of ZnFe2O4/Fe2O3 composite via calcination. TEM image showed that non-Zn ferrite spheres with wormlike nanopore structure were made of primary nanocrystals. BET surface area of non-Zn ferrite was much higher than that of ZnFe2O4/Fe2O3 composite. Saturation magnetization of non-Zn ferrites was significantly higher than that of ZnFe2O4/Fe2O3 composites. Calcination of non-Zn ferrite resulted in the formation of large amount of non-magnetic Fe2O3,which caused a low magnetization of composite. Because of higher BET surface area and higher saturation magnetization, non-Zn ferrite presented better Cr6+ adsorption property than ZnFe2O4/Fe2O3 composites.

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).

Properties of carbonate rocks related to SO2 reactivity

USGS Publications Warehouse

Borgwardt, R.H.; Harvey, R.D.

1972-01-01

Petrographic examination and grain size-distribution measurements were made on 11 specimens representing a broad spectrum of limestones and dolomites. The SO2 reaction kinetics of calcines prepared from each rock type were determined at 980??C. Stones of various geological types yield calcines of distinctly different physical structures that show correspondingly large differences in both rate of reaction and capacity for SO2 sorption. Pore size and particle size together determine the extent to which the interiors of individual particles react. Particles smaller than 0.01 cm with pores larger than 0.1 ?? react throughout their internal pore structure at a rate directly proportional to the BET surface. The rate decays exponentially as sulfation proceeds until the pores are filled with reaction product. The ultimate capacity of small particles is determined by the pore volume available for product accumulation, which is generally equivalent to about 50% conversion of the CaO in limestones. Variations in effectiveness of carbonate rocks for flue gas desulfurization are explained by the physical properties of their calcines, which are related to the crystal structure of the original rock. The high reaction rates achieved in the limestone injection process apparently result from the large surface area existing for short periods immediately following the dissociation of CaCO3.

Morphology-modulation of SnO2 Hierarchical Architectures by Zn Doping for Glycol Gas Sensing and Photocatalytic Applications

PubMed Central

Zhao, Qinqin; Ju, Dianxing; Deng, Xiaolong; Huang, Jinzhao; Cao, Bingqiang; Xu, Xijin

2015-01-01

The morphology of SnO2 nanospheres was transformed into ultrathin nanosheets assembled architectures after Zn doping by one-step hydrothermal route. The as-prepared samples were characterized in detail by various analytical techniques including scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and nitrogen adsorption-desorption technique. The Zn-doped SnO2 nanostructures proved to be the efficient gas sensing materials for a series of flammable and explosive gases detection, and photocatalysts for the degradation of methyl orange (MO) under UV irradiation. It was observed that both of the undoped and Zn-doped SnO2 after calcination exhibited tremendous gas sensing performance toward glycol. The response (S = Ra/Rg) of Zn-doped SnO2 can reach to 90 when the glycol concentration is 100 ppm, which is about 2 times and 3 times higher than that of undoped SnO2 sensor with and without calcinations, respectively. The result of photocatalytic activities demonstrated that MO dye was almost completely degraded (~92%) by Zn-doped SnO2 in 150 min, which is higher than that of others (MO without photocatalyst was 23%, undoped SnO2 without and with calcination were 55% and 75%, respectively). PMID:25597269

Study of TiO2 anatase nano and microstructures with dominant {001} facets for NO oxidation.

PubMed

Sofianou, Maria-Veronica; Trapalis, Christos; Psycharis, Vassils; Boukos, Nikos; Vaimakis, Tiverios; Yu, Jiaguo; Wang, Wenguang

2012-11-01

TiO(2) anatase nanoplates and hollow microspheres were fabricated by a solvothermal-hydrothermal method using titanium isopropoxide as a titanium precursor and hydrofluoric acid as a capping agent in order to enhance the formation of the {001} crystal facets of the anatase nanocrystals. These different morphological structures of TiO(2) anatase can be achieved by only changing the solvent, keeping the amount of the precursor and of the capping agent identical during the solvothermal-hydrothermal process. After calcination of the samples, the adsorbed fluoride atoms on the {001} crystal facets of the TiO(2) anatase nanocrystals were completely removed from their surface according to XPS analysis. The calcined TiO(2) anatase structures were higher crystallized and the specific surface area of the catalysts increased, enhancing their photocatalytic activity in comparison to the non-calcined TiO(2) anatase structures. All TiO(2) anatase samples with adsorbed as well as non-adsorbed fluoride atoms on their {001} crystal facets, exhibited a higher photonic efficiency than Degussa P25, which was used as a reference. The fluoride free TiO(2) anatase nanoplates exhibited the best photocatalytic activity in oxidizing the NO gas to NO(2) and NO(3) (-).

Formation and characterization of high surface area thermally stabilized titania/silica composite materials via hydrolysis of titanium(IV) tetra-isopropoxide in sols of spherical silica particles.

PubMed

Khalil, Kamal M S; Elsamahy, Ahmed A; Elanany, Mohamed S

2002-05-15

A direct synthetic route leading to titania particles dispersed on nonporous spherical silica particles has been investigated; 5, 10, and 20% (w/w) titania/silica sols mixtures were achieved via hydrolyzation of titanium tetra-isopropxide solution in the mother liquor of a freshly prepared sol of spherical silica particles (Stöber particles). Titania/silica materials were produced by subsequent drying and calcination of the xerogels so obtained for 3 h at 400 and 600 degrees C. The materials were investigated by means of thermal analyses (TGA and DSC), FT-IR, N(2) gas adsorption-desorption, powder X-ray diffraction (XRD), and transmission electron microscopy (TEM). In spite of the low surface area (13.1 m(2)/g) of the pure spherical silica particles calcined at 400 degrees C, high surface area and mesoporous texture titania/silica materials were obtained (e.g., S(BET) ca. 293 m(2)/g for the 10% titania/silica calcined at 400 degrees C). Moreover, the materials were shown to be amorphous toward XRD up to 600 degrees C, while reasonable surface areas were preserved. It has been concluded that dispersion of titania particles onto the surface of the nonporous spherical silica particles increase their roughness, therefore leading to composite materials of less firm packing and mesoporosity.

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

The Preparation of TiO₂ Film by the Sol-Gel Method and Evaluation of Its Self-Cleaning Property.

PubMed

Liang, Yu; Sun, Sijia; Deng, Tongrong; Ding, Hao; Chen, Wanting; Chen, Ying

2018-03-19

TiO₂ sol was produced by the sol-gel method through the hydrolysis and the aging of tetrabutyl titanate and the TiO₂ film was obtained by dipping and uniform lifting of the acid-treated and ultrasound-treated clean glass slides into the TiO₂ sol followed by aging, drying, and calcination. The effect of the hydrolysis control agents to the formed sol was researched and the crystalline state, the morphology, and the photocatalytic properties of the products after calcination were characterized. The structural morphology, the contact angles before and after illumination, and the self-cleaning properties of the TiO₂ film were characterized as well. The results showed that by using acetylacetone as the hydrolysis control agent, the formed TiO₂ sol had relatively high stability. The product after the calcination of the TiO₂ sol was of single anatase type with crystalline size of 18-20 nm and it could degrade nearly 100% of methylene blue after 90 min illumination. The formed TiO₂ film is compact, continuous, smooth, and had the properties of super-hydrophilicity (after 30 min illumination due to its contact angle decreasing from 21° to nearly 0°) and anti-fogging capability, which indicated its excellent self-cleaning property.

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.

Hexagonal ZnO porous plates prepared from microwave synthesized layered zinc hydroxide sulphate via thermal decomposition

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

Machovsky, Michal, E-mail: machovsky@ft.utb.cz; Polymer Centre, Faculty of Technology, Tomas Bata University in Zlin, Nam. T.G. Masaryka 275, 762 72 Zlin; Kuritka, Ivo, E-mail: ivo@kuritka.net

2013-10-15

Graphical abstract: - Highlights: • Zinc hydroxy sulphate was synthesized in 3 min via microwave hydrothermal route. • Zinc hydroxy sulphate was converted into mesh like porous ZnO by calcining at 900°. • The process of transformation is topotactic. - Abstract: Layered zinc hydroxide sulphate (ZHS) was prepared by microwave-assisted hydrothermal precipitation of zinc sulphate monohydrate with hexamethylenetetramine. Under ambient conditions, the structure of ZHS determined by X-ray diffraction (XRD) was found to be a mixture of zinc hydroxide sulphate pentahydrate Zn{sub 4}SO{sub 4}(OH){sub 6}·5H{sub 2}O and tetrahydrate Zn{sub 4}SO{sub 4}(OH){sub 6}·4H{sub 2}O. Fourier transform infrared (FTIR) spectroscopy was usedmore » for characterization of the prepared materials. Based on the interpretation of ZHS's thermal decomposition profile obtained by thermogravimetric analysis, ZnO of high purity was prepared by calcination at 900 °C for 2 h. The structure of the resulting ZnO was confirmed by the XRD. The morphology examination by scanning electron microscopy revealed a porous mesh-like ZnO structure developed from the ZHS precursor at the expense of mass removal due to the release of water and sulphate during the calcination.« less

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

Application of atmospheric-pressure plasma jet processed carbon nanotubes to liquid and quasi-solid-state gel electrolyte supercapacitors

NASA Astrophysics Data System (ADS)

Kuok, Fei-Hong; Kan, Ken-Yuan; Yu, Ing-Song; Chen, Chieh-Wen; Hsu, Cheng-Che; Cheng, I.-Chun; Chen, Jian-Zhang

2017-12-01

We use a dc-pulse nitrogen atmospheric-pressure plasma jet (APPJ) to calcine carbon nanotubes (CNTs) pastes that are screen-printed on carbon cloth. 30-s APPJ treatment can efficiently oxidize and vaporize the organic binders, thereby forming porous structures. As indicated by X-ray photoelectron spectroscopy (XPS) and electron probe microanalysis (EPMA), the oxygen content decreases after APPJ treatment owing to the oxidation and vaporization of ethyl cellulose, terpineol, and ethanol. Nitrogen doping was introduced to the materials by the nitrogen APPJ. APPJ-calcination improves the wettability of the CNTs printed on carbon cloth, as evidenced by water contact angle measurement. Raman spectroscopy indicates that reactive species of nitrogen APPJ react violently with CNTs in only 30-s APPJ processing time and introduce defects and/or surface functional groups on CNTs. Carbon cloths with calcined CNT layers are used as electrodes for liquid and quasi-solid-state electrolyte supercapacitors. Under a cyclic voltammetry test with a 2 mV/s potential scan rate, the specific capacitance is 73.84 F/g (areal capacitance = 5.89 mF/cm2) with a 2 M KCl electrolyte and 66.47 F/g (areal capacitance = 6.10 mF/cm2) with a H2SO4/polyvinyl alcohol (PVA) gel electrolyte.

Balancing Sodium Impurities in Alumina for Improved Properties

NASA Astrophysics Data System (ADS)

Wijayaratne, Hasini; Hyland, Margaret; McIntosh, Grant; Perander, Linus; Metson, James

2018-06-01

As there are direct and indirect impacts of feed material purity on the aluminum production process and metal grade, there is a high demand on the so-called pure smelter grade alumina (SGA)—the main feedstock for aluminum production. In this work, impurities within the precursor gibbsite used for SGA production and SGA are studied using NanoSIMS and XPS with a focus on sodium—the most abundant impurity. Although the industry trend is towards minimizing sodium due to the well-known negative impacts on the process, high sodium is also correlated with relatively attrition-resistant calcined products. Here, we show that this relationship is indirect and arises from sodium's role in inhibiting α-alumina formation. Alpha alumina formation in SGA has previously been demonstrated to induce a macro-porous and therefore attrition-prone microstructure. Sodium distribution within the precursor gibbsite and its migration during the calcination process are proposed to be most likely responsible for the spatial distribution of α-alumina within the calcined product grain. This in turn determines the behavior of the product during its transportation and handling (i.e., attrition). Therefore, tolerance of a certain amount of sodium within the precursor material does demonstrate a net benefit while balancing its negative impacts on the process.

[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

23. CONSTRUCTION PROGRESS VIEW LOOKING TOWARD EAST SHOWING CONCRETE BLOCK ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

23. CONSTRUCTION PROGRESS VIEW LOOKING TOWARD EAST SHOWING CONCRETE BLOCK CONSTRUCTION. INEEL PHOTO NUMBER NRTS-59-4305. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

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.

19. CONSTRUCTION PROGRESS PHOTO SHOWING (TYPICALLY COMPLEX) WASTE HOLDING CELL ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

19. CONSTRUCTION PROGRESS PHOTO SHOWING (TYPICALLY COMPLEX) WASTE HOLDING CELL PIPING. INEEL PHOTO NUMBER NRTS-59-3212. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

15. CONSTRUCTION PROGRESS PHOTO SHOWING FORMS GOING UP ON ACCESS ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

15. CONSTRUCTION PROGRESS PHOTO SHOWING FORMS GOING UP ON ACCESS CORRIDOR. INEEL PHOTO NUMBER NRTS-59-336. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

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

20. CONSTRUCTION PROGRESS PHOTO OF INSTRUMENT PANEL IN PLACE IN ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

20. CONSTRUCTION PROGRESS PHOTO OF INSTRUMENT PANEL IN PLACE IN OPERATING CORRIDOR. INEEL PHOTO NUMBER NRTS-59-6091. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

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.

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.

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

Facile and scalable synthesis of magnetite/carbon adsorbents by recycling discarded fruit peels and their potential usage in water treatment.

PubMed

Ma, Ji; Sun, Shuangshuang; Chen, Kezheng

2017-06-01

In this study, apple, banana and orange peels were used as precursor compounds for the mass production of magnetite/carbon adsorbents. A so-called "soak-calcination" procedure was employed by firstly soaking these waste fruit peels in FeCl 3 aqueous solutions and secondly calcining these precursors in the nitrogen atmosphere to yield final magnetite/carbon composites. This approach is quite simple and effective to synthesize carbon-based adsorbents on an industrial scale. The as-produced adsorbents feature the merits of appropriate ferromagnetism (>4emug -1 ), high adsorption capacity (several hundreds of milligrams per gram for adsorption of methyl blue, Congo red, rhodamine B and Cr 6+ ions), and good regenerability (>85%). Copyright © 2017 Elsevier Ltd. All rights reserved.

[Amorphous silica. Types, health effects of exposure, NDS].

PubMed

Woźniak, H; Wiecek, E

1995-01-01

Maximum allowable concentration (MAC) values for amorphous silica dust have not been identified in the Polish legal regulations up-to-date. In this work the authors review values of allowable (recommended) amorphous silica dust concentrations in other countries. Data on other types of amorphous silica (natural and synthetic) used in industry as well as data on health effects of exposure to these types of dust are presented. The work encompasses 42 entries in the references and one Table which includes the following proposed MAC values: Non-calcinate diatomaceous earth (diatomite) and synthetic silica: Total dust--10 mg/m3 Respirable dust--2 mg/m3 Calcinate diatomaceous earth (diatomite) and fused silica (vitreous silica): Total dust--2 mg/m3 Respirable dust--1 mg/m3.

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

Catalyst and method for reduction of nitrogen oxides

DOEpatents

Ott, Kevin C [Los Alamos, NM

2008-05-27

A Selective Catalytic Reduction (SCR) catalyst was prepared by slurry coating ZSM-5 zeolite onto a cordierite monolith, then subliming an iron salt onto the zeolite, calcining the monolith, and then dipping the monolith either into an aqueous solution of manganese nitrate and cerium nitrate and then calcining, or by similar treatment with separate solutions of manganese nitrate and cerium nitrate. The supported catalyst containing iron, manganese, and cerium showed 80 percent conversion at 113 degrees Celsius of a feed gas containing nitrogen oxides having 4 parts NO to one part NO.sub.2, about one equivalent ammonia, and excess oxygen; conversion improved to 94 percent at 147 degrees Celsius. N.sub.2O was not detected (detection limit: 0.6 percent N.sub.2O).

Catalyst and method for reduction of nitrogen oxides

DOEpatents

Ott, Kevin C [Los Alamos, NM

2008-08-19

A Selective Catalytic Reduction (SCR) catalyst was prepared by slurry coating ZSM-5 zeolite onto a cordierite monolith, then subliming an iron salt onto the zeolite, calcining the monolith, and then dipping the monolith either into an aqueous solution of manganese nitrate and cerium nitrate and then calcining, or by similar treatment with separate solutions of manganese nitrate and cerium nitrate. The supported catalyst containing iron, manganese, and cerium showed 80 percent conversion at 113 degrees Celsius of a feed gas containing nitrogen oxides having 4 parts NO to one part NO.sub.2, about one equivalent ammonia, and excess oxygen; conversion improved to 94 percent at 147 degrees Celsius. N.sub.2O was not detected (detection limit: 0.6 percent N.sub.2O).

Catalyst for reduction of nitrogen oxides

DOEpatents

Ott, Kevin C.

2010-04-06

A Selective Catalytic Reduction (SCR) catalyst was prepared by slurry coating ZSM-5 zeolite onto a cordierite monolith, then subliming an iron salt onto the zeolite, calcining the monolith, and then dipping the monolith either into an aqueous solution of manganese nitrate and cerium nitrate and then calcining, or by similar treatment with separate solutions of manganese nitrate and cerium nitrate. The supported catalyst containing iron, manganese, and cerium showed 80 percent conversion at 113 degrees Celsius of a feed gas containing nitrogen oxides having 4 parts NO to one part NO.sub.2, about one equivalent ammonia, and excess oxygen; conversion improved to 94 percent at 147 degrees Celsius. N.sub.2O was not detected (detection limit: 0.6 percent N.sub.2O).

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.

Biodiesel production from waste frying oil using waste animal bone and solar heat.

PubMed

Corro, Grisel; Sánchez, Nallely; Pal, Umapada; Bañuelos, Fortino

2016-01-01

A two-step catalytic process for the production of biodiesel from waste frying oil (WFO) at low cost, utilizing waste animal-bone as catalyst and solar radiation as heat source is reported in this work. In the first step, the free fatty acids (FFA) in WFO were esterified with methanol by a catalytic process using calcined waste animal-bone as catalyst, which remains active even after 10 esterification runs. The trans-esterification step was catalyzed by NaOH through thermal activation process. Produced biodiesel fulfills all the international requirements for its utilization as a fuel. A probable reaction mechanism for the esterification process is proposed considering the presence of hydroxyapatite at the surface of calcined animal bones. Copyright © 2015 Elsevier Ltd. All rights reserved.

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.

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.

34. DOOR AND WINDOW DETAILS. INEEL DRAWING NUMBER 200063300287106358. FLUOR ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

34. DOOR AND WINDOW DETAILS. INEEL DRAWING NUMBER 200-0633-00-287-106358. FLUOR NUMBER 5775-CPP-633-A-8. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

33. ROOF PLAN AND DETAILS. INEEL DRAWING NUMBER 200063300287106357. FLUOR ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

33. ROOF PLAN AND DETAILS. INEEL DRAWING NUMBER 200-0633-00-287-106357. FLUOR NUMBER 5775-CPP-633-A-7. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

Lung-clearance classification of radionuclides in calcined phosphate rock dust

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

Kalkwarf, D.R.; Jackson, P.O.

1984-08-01

Lung-clearance classifications for /sup 210/Pb and /sup 210/Po in airborne dust from elemental phosphorus plants were estimated for use with the lung clearance model proposed by the ICRP Task Group on Lung Dynamics. Estimates were based on measurements of dissolution rates for these radionuclides from sized dust samples into simulated lung fluid at 37/sup 0/C. The estimates were expressed in the classification terms of the model, i.e., D, W and Y, indicating lung clearance half-times of 0 to 10 days, 11 to 100 days and more than 100 days. Dust samples were obtained from two plants in the western Unitedmore » States, and dissolution trials were conducted on fractions containing particles with aerodynamic equivalent diameters (AED) of 0 to 3 ..mu..m and of 3 to 10 ..mu..m. The /sup 210/Pb and /sup 210/Po in each of these fractions were classified 100% Class Y. The specific activities of both radionuclides increased with decreasing AED of the particles. 11 references, 1 figure, 4 tables.« less

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

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.

Preparation and optical properties of trivalent europium doped into cordierite using the sol-gel process

NASA Astrophysics Data System (ADS)

Thim, Gilmar P.; Brito, Hermi F.; Silva, Sandra A.; Oliveira, Maria A. S.; Felinto, Maria C. F. C.

2003-02-01

The photoluminescence properties of the Eu3+ ion doped into α-cordierite were studied based on the excitation and emission spectra and lifetime measurements. These samples were prepared by the sol-gel method and calcined by heating the xerogel at different temperatures: 873, 1133, 1223 and 1473 K. X-ray diffraction patterns were used to characterize the luminescent material. The 5D0→7F0 transition of the samples exhibits only one broad peak arising from the inhomogeneous linewidth of the amorphous phase, except for the ceramic material obtained at 1473 K that presents two peaks. Also, in the latter case the luminescence decay lifetime exhibits a bi-exponential fit when excited at 280 nm, corroborating that the Eu3+ ion exists in two sites of symmetry. The experimental intensity parameter Ω2 (10.0×10-20 cm2) indicates a moderately polarizable chemical environment around the Eu3+ ion. The emission spectra of the Mg2Al4Si5O18:Eu3+ samples calcined at 873, 1133 and 1223 K also presented inhomogeneous profiles for the 5D0→7FJ transitions suggesting disorder of the material. On the other hand, the sample calcined at 1473 K shows narrow bands indicating the crystalline form. The emission quantum efficiency (η) of the α-cordierite system is also discussed.

Improvement of the magnetic moment of NiZn ferrites induced by substitution of Nd3+ ions for Fe3+ ions

NASA Astrophysics Data System (ADS)

Wu, Xuehang; Chen, Wen; Wu, Wenwei; Wu, Juan; Wang, Qing

2018-05-01

Four types of Ni-Zn based ferrites materials having the general formula Ni0.5Zn0.5NdxFe2-xO4 (0.0 ≤ x ≤ 0.12) have been successfully synthesized by calcining oxalates in air and the influence of Nd content on the structure and magnetic properties of Ni0.5Zn0.5NdxFe2-xO4 is studied. X-ray diffraction examination confirms that a high-crystallized Ni0.5Zn0.5NdxFe2-xO4 with cubic spinel structure is obtained when the precursor is calcined at 1000 °C in air for 2 h. The substitutions of Nd3+ ions for partial Fe3+ ions do not change the spinel crystalline structure of MFe2O4. The incorporation of Nd3+ ions in place of Fe3+ ions in Ni-Zn ferrites increases the average crystallite size. Specific saturation magnetization decreases with increase in Nd content. This is because Nd3+ ions with smaller magnetic moment preferentially fill the octahedral sites. In addition, antiferromagnetic FeNdO3 increases with increase in Nd content. In this study, Ni0.5Zn0.5Nd0.08Fe1.92O4, calcined at 1000 °C, exhibits the highest magnetic moment (4.2954 μB) and the lowest coercivity (28.82 Oe).

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.

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.

Obtaining aluminas from the thermal decomposition of their different precursors: An {sup 27}Al MAS NMR and X-ray powder diffraction studies

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

Chagas, L.H.; De Carvalho, G.S.G.; San Gil, R.A.S.

2014-01-01

Graphical abstract: - Highlights: • We synthesized three precursors of alumina from different methods. • The calcination of the precursors generated several alumina polymorphs. • XRD and NMR were used for structural investigation of the polymorphs. • The synthesis route determines the structural and textural properties of the solids. - Abstract: A commercial sample of Boehmite was used as precursor of alumina polymorphs. For comparison, three other precursors were synthesized from different methods. Particularly, the use of excess of urea promoted a very crystalline form of basic aluminum carbonate. The characteristics of the four precursors were investigated by thermal, vibrationalmore » and X-ray powder diffraction (XRD) analysis. Additionally, the nuclear magnetic resonance, with magic angle spinning ({sup 27}Al MAS NMR), was used to verify the coordination of aluminum cations. Each precursor was calcined at various temperatures generating alumina polymorphs, which were structurally analyzed by XRD and {sup 27}Al MAS NMR. Due to interest in catalysis supports, special attention was given to the γ-Al{sub 2}O{sub 3} phase, which in addition to structural investigation was subjected to textural analysis. The results showed that, from different synthesis procedures and common route of calcination, one can obtain materials with the same composition but with different structural and textural properties, which in turn can significantly influence the performance of a supported catalyst.« less

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.

Soilless plant growth media influence the efficacy of phytohormones and phytohormone inhibitors.

PubMed

Best, Norman B; Hartwig, Thomas; Budka, Joshua S; Bishop, Brandon J; Brown, Elliot; Potluri, Devi P V; Cooper, Bruce R; Premachandra, Gnanasiri S; Johnston, Cliff T; Schulz, Burkhard

2014-01-01

Plant growth regulators, such as hormones and their respective biosynthesis inhibitors, are effective tools to elucidate the physiological function of phytohormones in plants. A problem of chemical treatments, however, is the potential for interaction of the active compound with the growth media substrate. We studied the interaction and efficacy of propiconazole, a potent and specific inhibitor of brassinosteroid biosynthesis, with common soilless greenhouse growth media for rice, sorghum, and maize. Many of the tested growth media interacted with propiconazole reducing its efficacy up to a hundred fold. To determine the molecular interaction of inhibitors with media substrates, Fourier Transform Infrared Spectroscopy and sorption isotherm analysis was applied. While mica clay substrates absorbed up to 1.3 mg of propiconazole per g substrate, calcined clays bound up to 12 mg of propiconazole per g substrate. The efficacy of the gibberellic acid biosynthesis inhibitor, uniconazole, and the most active brassinosteroid, brassinolide, was impacted similarly by the respective substrates. Conversely, gibberellic acid showed no distinct growth response in different media. Our results suggest that the reduction in efficacy of propiconazole, uniconazole, and brassinolide in bioassays when grown in calcined clay is caused by hydrophobic interactions between the plant growth regulators and the growth media. This was further confirmed by experiments using methanol-water solvent mixes with higher hydrophobicity values, which reduce the interaction of propiconazole and calcined clay.

Macroporous Calcium Phosphate/Chitosan Composites Prepared via Unidirectional Ice Segregation and Subsequent Freeze-Drying

PubMed Central

Aranaz, Inmaculada; Martínez-Campos, Enrique; Moreno-Vicente, Carolina; Civantos, Ana; García-Arguelles, Sara; del Monte, Francisco

2017-01-01

Calcium phosphate chitosan-based composites have gained much interest in recent years for biomedical purposes. In this paper, three-dimensional calcium phosphate chitosan-based composites with different mineral contents were produced using a green method called ice segregation induced self-assembly (ISISA). In this methodology, ice crystals were used as a template to produce porous structures from an aqueous solution of chitosan (CS) and hydroxyapatite (Hap) also containing acetic acid (pH = 4.5). For better characterization of the nature of the inorganic matter entrapped within the resulting composite, we performed either oxygen plasma or calcination processes to remove the organic matter. The nature of the phosphate salts was studied by XRD and NMR studies. Amorphous calcium phosphate (ACP) was identified as the mineral phase in the composites submitted to oxygen plasma, whereas crystalline Hap was obtained after calcination. SEM microscopy revealed the formation of porous structures (porosity around 80–85%) in the original composites, as well as in the inorganic matrices obtained after calcination, with porous channels of up to 50 µm in diameter in the former case and of up to 20 µm in the latter. The biocompatibility of the composites was assessed using two different cell lines: C2C12GFP premyoblastic cells and MC3T3 preosteoblastic cells. PMID:28772874

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.

Lead acetate trihydrate precursor route to synthesize novel ultrafine lead oxide from spent lead acid battery pastes

NASA Astrophysics Data System (ADS)

Sun, Xiaojuan; Yang, Jiakuan; Zhang, Wei; Zhu, Xinfeng; Hu, Yuchen; Yang, Danni; Yuan, Xiqing; Yu, Wenhao; Dong, Jinxin; Wang, Haifeng; Li, Lei; Vasant Kumar, R.; Liang, Sha

2014-12-01

A novel green recycling process is investigated to prepare lead acetate trihydrate precursors and novel ultrafine lead oxide from spent lead acid battery pastes. The route contains the following four processes. (1) The spent lead pastes are desulphurized by (NH4)2CO3. (2) The desulphurized pastes are converted into lead acetate solution by leaching with acetic acid solution and H2O2; (3) The Pb(CH3COO)2·3H2O precursor is crystallized and purified from the lead acetate solution with the addition of glacial acetic acid; (4) The novel ultrafine lead oxide is prepared by the calcination of lead acetate trihydrate precursor in N2 or air at 320-400 °C. Both the lead acetate trihydrate and lead oxide products are characterized by TG-DTA, XRD, and SEM techniques. The calcination products are mainly α-PbO, β-PbO, and a small amount of metallic Pb. The particle size of the calcination products in air is significantly larger than that in N2. Cyclic voltammetry measurements of the novel ultrafine lead oxide products show good reversibility and cycle stability. The assembled batteries using the lead oxide products as cathode active materials show a good cyclic stability in 80 charge/discharge cycles with the depth of discharge (DOD) of 100%.

Thermal hydrogen reduction for preservation of mesoporous silica film nanocomposites with a hexagonal structure containing amphiphilic triphenylene

NASA Astrophysics Data System (ADS)

Lintang, Hendrik O.; Jalani, Mohamad Azani; Yuliati, Leny

2017-11-01

We highlight that columnar assembly of self-assembled templates was successfully utilized using sol-gel technique of mesostructured silica for the quality improvement of transparent mesoporous film nanocomposites with a hexagonal structure through appropriate heat treatment methods and self-assembled templates in the removal of organic components. In contrast to the reported mesostructured silica film nanocomposites containing columnar assembly of trinuclear gold(I) pyrazolate complex ([Au3Pz3]C10TEG/silicahex) with calcination at 450 °C, mesostructured silica film nanocomposites from self-assembled template of triphenylene bearing amphiphilic decoxy triethylene glycol side chains (TPC10TEG/silicahex) can be completely collapsed upon calcination at 450 °C. This hexagonal structure can be only preserved with calcination at 250 °C although intensity of its main diffraction peak of d100 at 2θ of 3.70° was significantly decreased. On the other hands, thermal hydrogen reduction at the same temperature was found to be the best heat treatment to preserve the quality of mesoporous silica film nanocomposites with decreasing in intensity of diffraction peak up to 30%. Such phenomenon might be caused by slow decomposition of organic components with the presence of hydrogen gas upon heating to shrinkage the silica wall from interpenetration of ethylene glycol segments of the side chains and to open bonding of benzene ring from the core.

CaO-based CO2 sorbents: from fundamentals to the development of new, highly effective materials.

PubMed

Kierzkowska, Agnieszka M; Pacciani, Roberta; Müller, Christoph R

2013-07-01

The enormous anthropogenic emission of the greenhouse gas CO2 is most likely the main reason for climate change. Considering the continuing and indeed growing utilisation of fossil fuels for electricity generation and transportation purposes, development and implementation of processes that avoid the associated emissions of CO2 are urgently needed. CO2 capture and storage, commonly termed CCS, would be a possible mid-term solution to reduce the emissions of CO2 into the atmosphere. However, the costs associated with the currently available CO2 capture technology, that is, amine scrubbing, are prohibitively high, thus making the development of new CO2 sorbents a highly important research challenge. Indeed, CaO, readily obtained through the calcination of naturally occurring limestone, has been proposed as an alternative CO2 sorbent that could substantially reduce the costs of CO2 capture. However, one of the major drawbacks of using CaO derived from natural sources is its rapidly decreasing CO2 uptake capacity with repeated carbonation-calcination reactions. Here, we review the current understanding of fundamental aspects of the cyclic carbonation-calcination reactions of CaO such as its reversibility and kinetics. Subsequently, recent attempts to develop synthetic, CaO-based sorbents that possess high and cyclically stable CO2 uptakes are presented. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A comprehensive overview on the structure and comparison of magnetic properties of nanocrystalline synthesized by a thermal treatment method

NASA Astrophysics Data System (ADS)

Naseri, Mahmoud Goodarz; Halimah, M. K.; Dehzangi, Arash; Kamalianfar, Ahmad; Saion, Elias B.; Majlis, Burhanuddin Y.

2014-03-01

This study reports the simple synthesis of MFe2O4 (where M=Zn, Mn and Co) nanostructures by a thermal treatment method, followed by calcination at various temperatures from 723 to 873 K. Poly(vinyl pyrrolidon) (PVP) was used as a capping agent to stabilize the particles and prevent them from agglomeration. The pyrolytic behaviors of the polymeric precursor were analyzed by use of simultaneous thermo-gravimetry analyses (TGA) and derivative thermo-gravimetry (DTG) analyses. The characterization studies were conducted by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Fourier transform infrared spectroscopy (FT-IR) confirmed the presence of metal oxide bands for all the calcined samples. Magnetic properties were demonstrated by a vibrating sample magnetometer (VSM), which displayed that the calcined samples exhibited different types of magnetic behavior. The present study also substantiated that magnetic properties of ferrite nanoparticles prepared by the thermal treatment method, from viewing microstructures of them, can be explained as the results of the two important factors: cation distribution and impurity phase of α-Fe2O3. These two factors are subcategory of the preparation method which is related to macrostructure of ferrite. Electron paramagnetic resonance (EPR) spectroscopy showed the existence of unpaired electrons ZnFe2O4 and MnFe2O4 nanoparticles while it did not exhibit resonance signal for CoFe2O4 nanoparticles.

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

35. MISCELLANEOUS ARCHITECTURAL AND STRUCTURAL DETAILS. INEEL DRAWING NUMBER 200063300287106359. ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

35. MISCELLANEOUS ARCHITECTURAL AND STRUCTURAL DETAILS. INEEL DRAWING NUMBER 200-0633-00-287-106359. FLUOR NUMBER 5775-CPP-633-A-9. - Idaho National Engineering Laboratory, Old Waste Calcining Facility, Scoville, Butte County, ID

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...