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1.
ACS Omega ; 9(17): 19057-19062, 2024 Apr 30.
Artigo em Inglês | MEDLINE | ID: mdl-38708201

RESUMO

The dramatic increase in plastics production, coupled with a low recycling and recovery rate, has been a major challenge for sustainable practices and combating climate change. Hydrotreatment processing to upgrade fuel oils is a well-known process in the petroleum industry. In this work, we aim to investigate the catalyst properties before and after the hydrotreatment of pyrolysis oil derived from plastics, namely, linear low-density polyethylene, as no such report is available in the literature. Granular and powder forms of the Pt/Al2O3 catalyst were used in this study with characterization methods executed as such: transmission electron microscopy, X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), thermogravimetric analysis (TGA), and IR-RIS. XRD data show that the crystallinity of the catalyst support was unaffected by the hydrotreatment without any residues left, as the characteristic diffraction peaks were indicated for the crystalline phase of the support as 37.4, 39.8, 46.3, and 67.3°. In addition, the TGA experiments revealed that the carbon deposition on the spent catalyst was higher, as indicated by the higher weight loss (15.359%) compared to the fresh catalyst sample (11.43%). XPS analysis showed that the carbon deposition is more intense on the granular spent catalyst, as the intensity of the peaks is some 15 times greater than the peaks from the fresh catalyst. Also, compared to the observed peaks of the powder catalyst, less coke is formed. The band at 1624.05 cm-1 from the IR-RIS spectra was attributed to a shifted C=O band from the coke formation. The extension of these investigations using different catalysts to improve their characteristics and performance and to inhibit coke deposition will contribute to the incorporation of such processes in industry as well as the cost of fuels.

2.
Sci Rep ; 13(1): 7453, 2023 May 08.
Artigo em Inglês | MEDLINE | ID: mdl-37156861

RESUMO

In the present investigation, two sets of pure and substituted ferrite- and manganite-based mixed oxides were prepared within the stoichiometric formula[Formula: see text], where A = Bi or La, A' = Sr, B = Fe or Mn, B' = Co, x = 0 or 0.2, by calcination at 700 °C (for 1 h) of corresponding metal citrate xerogels. Materials thus obtained were examined for bulk and surface characteristics using X-ray diffractometry, ex situ Fourier transform infrared spectroscopy, UV-Vis diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy, and N2 sorptiometry. Their redox catalytic activity was evaluated towards a 2-propanol dehydrogenation reaction in the gas phase by employing in situ Fourier transform infrared spectroscopy. The results obtained could help reveal that (1) the presence of Bi (versus La) and Mn (versus Fe) facilitated the formation of polymeric crystalline phases assuming lattice-charge imbalance (due to excess positive charge), (2) the surface exposure of the excess positive charge was manifested in the generation of Mn sites having various oxidation states ≥ 3+, (3) the consequent development of visible light absorptions at 498-555 nm suggested occurrence of electron double-exchange facilitated by the formation of Mnn+-O2--Mn(n+1)+ Zener-type linkages, and (4) the exposure of such linkages at the surface warrants the establishment of the electron-mobile environment necessitated by the redox catalytic activity. Moreover, the relationship between the alcohol dehydrogenation activity and the magnitude of the lattice-charge imbalance (i.e., the net excess positive charge) of the catalysts was highlighted.

3.
J Chromatogr A ; 1671: 462991, 2022 May 24.
Artigo em Inglês | MEDLINE | ID: mdl-35378321

RESUMO

Developing of new core@shell particles (CSPs) bearing metal oxides on their outer surfaces is of a great interest. Such hybrid systems have many benefits, i.e., low cost, operation simplicity, chemical stability and tunability along with simple recoverability and reusability that make them suitable as dispersive solid phase extraction (DSPE) sorbents for selecting/extracting different types of molecular structures. Accordingly, herein, novel chromia-based CSPs were successfully prepared and utilized as efficient DSPE for selective enrichment toward phosphotyrosine (pTyr). A modified version of Stöber method was used to prepare highly dispersed core particles that were further coated with the chromium oxide. The outer shell surface morphology and thickness of SiO2@Cr2O3-CSP system were characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), whereas the surface functionalities were determined using X-ray photoelectron spectroscopy (XPS), FT-IR spectroscopy and zeta potential. The prepared chromia sorbent showed a significant improvement in extracting a probe-analyte (pTyr) compared to the results obtained by titania-based counterparts. As well to this, a noticeable stability of the SiO2@Cr2O3-CSP sorbent was remarkably achieved which upon simple solvent-wash cycles, the studied sorbent can be regenerated/reused. Noticeably low-levels of LOD and LOQ (3.0 and 15 pg mL-1) were attained with good linearity (R2 of 0.9995), batch-to-batch reproducibility (RSD% ≤ 10) and run-to-run repeatability (RSD% ≤ 5.5).


Assuntos
Dióxido de Silício , Extração em Fase Sólida , Fosfotirosina , Reprodutibilidade dos Testes , Dióxido de Silício/química , Extração em Fase Sólida/métodos , Espectroscopia de Infravermelho com Transformada de Fourier
4.
Nanomaterials (Basel) ; 11(8)2021 Jul 24.
Artigo em Inglês | MEDLINE | ID: mdl-34443737

RESUMO

Optimizing the physicochemical properties of the chitosan-based activated carbon (Ch-ACs) can greatly enhance its performance toward heavy metal removal from contaminated water. Herein, Ch was converted into a high surface area (1556 m2/g) and porous (0.69 cm3/g) ACs with large content of nitrogen (~16 wt%) using K2CO3 activator and urea as nitrogen-enrichment agents. The prepared Ch-ACs were tested for the removal of Cr(VI) and Pb(II) at different pH, initial metal ions concentration, time, activated carbon dosage, and temperature. For Cr(VI), the best removal was at pH = 2, while for Pb(II) the best pH for its removal was in the range of 4-6. At 25 °C, the Temkin model gives the best fit for the adsorption of Cr(VI), while the Langmuir model was found to be better for Pb(II) ions. The kinetics of adsorption of both heavy metal ions were found to be well-fitted by a pseudo-second-order model. The findings show that the efficiency and the green properties (availability, recyclability, and cost effectiveness) of the developed adsorbent made it a good candidate for wastewaters treatment. As preliminary work, the prepared sorbent was also tested regarding the removal of heavy metals and other contaminations from real wastewater and the obtained results were found to be promising.

5.
Front Chem ; 9: 633877, 2021.
Artigo em Inglês | MEDLINE | ID: mdl-33692986

RESUMO

The test alumina (the so-called ι-Al2O3) was thermally recovered at 1,100°C from chitosan-AlOx hybrid films and found to contain Na and Ca impurity ions inherited from the parent chitosan. Two different modifications of pure alumina, namely, γ- and α-Al2O3, were adopted as control samples. The test and control aluminas were examined for 1) the bulk elemental constitution by atomic absorption spectroscopy (AAS), 2) the surface chemical composition by X-ray photoelectron spectroscopy (XPS), 3) the bulk phase composition by X-ray powder diffractometry (XRD), ex-situ Fourier-transform infrared spectroscopy (IR), and Laser Raman (LRa) spectroscopy, 4) the surface area, topography, and morphology by N2 sorptiometry, and atomic force (AFM) and scanning electron microscopy (SEM), 5) the surface adsorptive interactions with pyridine and 2-propanol gas-phase molecules by in-situ IR spectroscopy of the adsorbed species, and 6) the surface catalytic interactions with 2-propanol gas-phase molecules by in-situ IR spectroscopy of the gas phase. Results obtained could clearly show that the test alumina (ι-Al2O3) is only hypothetically pure alumina since in reality its bulk structure is majored by mullite-type Na-aluminate (Na0.67Al6O9.33/NaAlO2) and minored by Na-ß-alumina (Na1.71Al11O17) and ß-alumina (NaAl11O17). Consistently, observed Na-influenced modifications of the surface chemistry, topology, and morphology, as well as adsorptive and catalytic interactions with pyridine and 2-propanol gas-phase molecules, showed significant deviations from those exhibited by the control pure aluminas (γ- and α-Al2O3).

6.
Front Chem ; 8: 391, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-32509727

RESUMO

Resistance to stainless steel corrosion in marine-based industries requires more research into materials with an improved surface and enhanced protection by utilizing surface coatings. Herein, a thermally stable aramid-zirconia nanocomposite has been successfully prepared using the sol-gel method to produce a zirconia network-structure bonded to the polymer chain. Using thermal gravimetric analysis (TGA), the residue mass of zirconia retained after the thermal degradation of aramid-zirconia film was determined and found to be 10% by mass. The investigated nanocomposite (using 10% zirconia) was coated on the stainless-steel surface through a facile and effective spin coating method and its protection was examined in saline solution (3.5% NaCl). The aramid-zirconia nanocomposite coating (Ar-Zr10) was found to provide an outstanding corrosion resistance to steel surfaces which led to protecting it against the corrosive marine environment. The electrochemical impedance (EIS) measurements were carried out to evaluate steel resistance against dissolution in chloride solution in the absence and presence of the investigated coatings showed a corrosion protection efficiency of 99.3% using Ar-Zr10 compared to 92.1% using pure aramid. Moreover, the potentiodynamic polarization (PDP) plots showed a pronounced decrease in the corrosion current values which confirmed the formation of a passive layer which mitigated the corrosion reaction and ions diffusion. The water contact angle of stainless-steel coated with pure aramid and the aramid-zirconia was found to be 84.2° and 125°, respectively, confirming the hydrophobic nature of the hybrid coating Ar-Zr10. On the other hand, the results achieved through the electrochemical and surface techniques were used to clarify the protection mechanism. The aramid-zirconia nanocomposite coating showed a remarkable protection performance by controlling the charge transfer at the interface between the steel alloy and the electrolyte which prevented the alloy dissolution.

7.
ChemistryOpen ; 9(1): 87-92, 2020 01.
Artigo em Inglês | MEDLINE | ID: mdl-31988844

RESUMO

We report the successful direct synthesis of an ultrastable mesoporous silicon dioxide framework containing silver nanoclusters using a modified true liquid crystal templating method. Our modification produced an extraordinary material with a high average Brunauer-Emmett-Teller specific surface area of 1785 m2 g-1 - the highest reported surface area to date - and an ultrastable mesoporous structure, which has been stable for nine years so far. This method eliminates the need for reduction of silver oxide into metallic silver and restricts the growth of silver clusters. The silver nanoclusters, with an average size of 1 nm, occupy the pores and walls of the framework. Analysis of the material using nitrogen adsorption/desorption method, high-resolution transmission electron microscopy, X-ray diffractometry, energy-dispersive X-ray diffractometry, X-ray photoelectron spectroscopy, and scanning electron microscopy is discussed herein.

8.
Adv Colloid Interface Sci ; 270: 38-53, 2019 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-31174003

RESUMO

Colloidal synthesis of nanoparticles using polymeric stabilizers as a template of a structure directing agent provided a plethora of opportunities in fabricating nanoparticles (NPs) with controlled size, shape, composition and structural characteristics. To understand the complete potency of polymeric stabilizers during the synthesis of nanoparticles, the relationship between polymer characteristics such as structure, molecular weight and concentration and nanoparticles characteristics is discussed in depth. This review portrays the use of polymers to attain nanostructured materials via covalent and non-covalent approaches. These polymers can also serve as surfaces modifier as well as the growth regulators during the synthesis of nanomaterials. The effect provided by polymers that directs the formation of nanomaterials into desired forms is otherwise hard to achieve. We especially spotlight on the approaches for tuning the characteristic properties of nanoparticles via cautious choice of the polymer system with special focus to stimuli-responsive polymers. This review mainly focusses on answering the main challenging question; what is the ideal polymeric stabilizer system to obtain specific morphology, size and phase structure of nanoparticles? Such vital information will enable rational design of nanoparticles to meet specific needs for different applications.

9.
Nanomaterials (Basel) ; 8(5)2018 May 07.
Artigo em Inglês | MEDLINE | ID: mdl-29735952

RESUMO

In this work in-situ polymerization technique has been used to chemically link the functionalized multiwalled carbon nanotubes (CNTs) with aramid matrix chains. Phenylene diamine monomers were reacted in the first stage with the carboxylic acid functionalized CNTs and then amidized in-situ using terephthaloyl chloride generating chemically bonded CNTs with the matrix. Various proportions of the CNTs were used to prepare the hybrid materials. The functionalization procedure was studied by Fourier transform infrared (FTIR) spectroscopy and composite morphology investigated by scanning electron microscopy (SEM). Thermal mechanical properties of these hybrids, together with those where pristine CNTs with similar loadings were used, are compared using tensile and dynamic mechanical analysis (DMA). The tensile strength and temperature involving α-relaxations on CNT loading increased with CNT loading in both systems, but much higher values, i.e., 267 MPa and 353 °C, respectively, were obtained in the chemically bonded system, which are related to the nature of the interface developed as observed in SE micrographs. The water absorption capacity of the films was significantly reduced from 6.2 to 1.45% in the presence pristine CNTs. The inclusion of pristine CNTs increased the electric conductivity of the aramid films with a minimum threshold value at the loading of 3.5 wt % of CNTs. Such mechanically strong and thermally stable aramid and easily processable composites can be suitable for various applications including high performance films, electromagnetic shielding and radar absorption.

10.
Sci Rep ; 8(1): 3695, 2018 Feb 27.
Artigo em Inglês | MEDLINE | ID: mdl-29487379

RESUMO

In this investigation, well defined mesoporous zirconia nanoparticles (ZrO2 NPs) with cubic, tetragonal or monoclinic pure phase were synthesized via thermal recovery (in air) from chitosan (CS)- or polyvinyl alcohol (PVA)-ZrOx hybrid films, prepared using sol-gel processing. This facile preparative method was found to lead to an almost quantitative recovery of the ZrOx content of the film in the form of ZrO2 NPs. Impacts of the thermal recovery temperature (450, 800 and 1100 °C) and polymer type (natural bio-waste CS or synthetic PVA) used in fabricating the organic/inorganic hybrid films on bulk and surface characteristics of the recovered NPs were probed by means of X-ray diffractometry and photoelectron spectroscopy, FT-IR and Laser Raman spectroscopy, transmission electron and atomic force microscopy, and N2 sorptiometry. Results obtained showed that the method applied facilates control over the size (6-30 nm) and shape (from loose cubes to agglomerates) of the recovered NPs and, hence, the bulk crystalline phase composition and the surface area (144-52 m2/g) and mesopore size (23-10 nm) and volume (0.31-0.11 cm3/g) of the resulting zirconias.

11.
Sci Rep ; 7(1): 14788, 2017 11 01.
Artigo em Inglês | MEDLINE | ID: mdl-29093548

RESUMO

Herein, we report the synthesis of chromium oxide nanoparticles, α -Cr2O3 NPs, followed by full characterization via XRD, SEM, XPS, and N2 sorptiometry. The synthesized nanoparticles were tested as catalysts toward the oxidation of CO. The impact of calcination temperature on the catalytic activity was also investigated. CO conversion (%), light-off temperature, T50, data were determined. The results revealed that chromia obtained at low calcination temperature (400 °C) is more active than those obtained at high calcination temperatures (600° or 800 °C) and this is ascribed to the smaller particle size and higher surface area of this sample. The results revealed a superior catalytic activity of Cr2O3 NPs at lower temperature as we reached a complete conversion at 200 °C which is high value in the forefront of the published results of other non-noble catalysts. The high activity of Cr2O3 nanoparticles (T50 as low as 98 °C) where found to be dependent on a careful selection of the calcination temperature. These results may provide effective and economic solutions to overcome one of the major environmental threats.

13.
Nanoscale Res Lett ; 10: 19, 2015.
Artigo em Inglês | MEDLINE | ID: mdl-25852317

RESUMO

Zinc oxide (ZnO) nanostructures of uniform shapes and sizes (spherical, needle-like, and acicular) were directly synthesized using a relatively precursor-insensitive water-in-n-heptane microemulsion system stabilized by a mixture of cationic and non-ionic surfactants. With this colloidal system, the synthesized ZnO possesses the highest reported surface area (76 m(2) g(-1)) among the published reports utilizing other microemulsion systems. Such precursor insensitivity allowed studying the effect of Zn precursor:precipitating agent molar ratio (as high as 1:8) on the particle size, specific surface area, porosity, and morphology of the synthesized nanoparticles. The interaction of the cationic surfactant head groups and their Br(-) counter ions with Zn(2+) and OH(-) ions is believed to play a major role in controlling the ZnO characteristics. Due to such interactions, it is believed that the nucleation processes are retarded while the growth is more dominating if compared with other microemulsion systems.

14.
Photochem Photobiol ; 91(2): 265-71, 2015.
Artigo em Inglês | MEDLINE | ID: mdl-25400159

RESUMO

Methyl tert-butyl ether is a commonly used fuel oxygenate that is present in gasoline. It was introduced to eliminate the use of leaded gasoline and to improve the octane quality because it aids in the complete combustion of fuel by supplying oxygen during the combustion process. Over the past decade, the use of MTBE has increased tremendously worldwide. For obvious reasons relating to accidental spillage, MTBE started to appear as an environmental and human health threat because of its nonbiodegradable nature and carcinogenic potential, respectively. In this work, MTBE was degraded with the help of an advanced oxidation process through the use of zinc oxide as a photocatalyst in the presence of visible light. A mixture of 200 mg of zinc oxide in 350 mL of 50 ppm MTBE aqueous solution was irradiated with visible light for a given time. The complete degradation of MTBE was recorded, and approximately 99% photocatalytic degradation of 100 ppm MTBE solution was observed. Additionally, the photoactivity of 1% Pd-doped ZnO was tested under similar conditions to understand the effect of Pd doping on ZnO. Our results obtained under visible light irradiation are very promising, and they could be further explored for the degradation of several nondegradable environmental pollutants.


Assuntos
Elétrons , Poluentes Ambientais/química , Éteres Metílicos/química , Paládio/química , Fotólise , Óxido de Zinco/química , Catálise , Cinética , Luz , Nanopartículas/química , Nanopartículas/ultraestrutura , Oxirredução , Soluções , Termodinâmica , Água
15.
Phys Chem Chem Phys ; 16(16): 7146-58, 2014 Apr 28.
Artigo em Inglês | MEDLINE | ID: mdl-24554000

RESUMO

Although TiO2 is one of the most efficient photocatalysts, with the highest stability and the lowest cost, there are drawbacks that hinder its practical applications like its wide band gap and high recombination rate of the charge carriers. Consequently, many efforts were directed toward enhancing the photocatalytic activity of TiO2 and extending its response to the visible region. To head off these attempts, modification of TiO2 with noble metal nanoparticles (NMNPs) received considerable attention due to their role in accelerating the transfer of photoexcited electrons from TiO2 and also due to the surface plasmon resonance which induces the photocatalytic activity of TiO2 under visible light irradiation. This insightful perspective is devoted to the vital role of TiO2 photocatalysis and its drawbacks that urged researchers to find solutions such as modification with NMNPs. In a coherent context, we discussed here the characteristics which qualify NMNPs to possess a great enhancement effect for TiO2 photocatalysis. Also we tried to understand the reasons behind this effect by means of photoluminescence (PL) and electron paramagnetic resonance (EPR) spectra, and Density Functional Theory (DFT) calculations. Then the mechanism of action of NMNPs upon deposition on TiO2 is presented. Finally we introduced a survey of the behaviour of these noble metal NPs on TiO2 based on the particle size and the loading amount.

16.
J Hazard Mater ; 264: 71-8, 2014 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-24275473

RESUMO

A series of binary oxide catalysts (ceria-ZnO) were prepared and doped with different amounts of palladium in the range of 0.5%-1.5%. The prepared catalysts were characterized by SEM, TEM, XRD and XPS, as well as by N2 sorptiometry study. The XPS results confirmed the structure of the Pd CeO2-x-ZnO. The photocatalytic activity of these catalysts was evaluated for degradation of MTBE in water. These photocatalyst efficiently degrade a 100ppm aqueous solution of MTBE upon UV irradiation for 5h in the presence of 100mg of each of these photocatalysts. The removal of 99.6% of the MTBE was achieved with the ceria-ZnO catalyst doped with 1% Pd. In addition to the Pd loading, the N2 sorptiometry study introduced other factors that might affect the catalytic efficiency is the catalyst average pore sizes. The photoreaction was determined to be a first order reaction.


Assuntos
Poluentes Ambientais/química , Éteres Metílicos/química , Nanocompostos/química , Paládio/química , Óxido de Zinco/química , Poluentes Ambientais/efeitos da radiação , Éteres Metílicos/efeitos da radiação , Microscopia Eletrônica , Nitrogênio , Espectroscopia Fotoeletrônica , Fotólise , Difração de Raios X
17.
J Colloid Interface Sci ; 393: 210-8, 2013 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-23200348

RESUMO

The structure of solubilized water in water-in-n-heptane aggregates stabilized by mixtures of single- and double-tail quaternary ammonium surfactants, namely didodecyldimethylammonium chloride/dodecyltrimethylammonium chloride (DDAC/DTAC) or didodecyldimethylammonium bromide/dodecyltrimethylammonium bromide (DDAB/DTAB) was studied by two noninvasive techniques, (1)H NMR and FT-IR. In the former, the chemical shift data, δ(obs), were used to calculate the so-called deuterium/protium fractionation factor, φ(M), of the aggregate-solubilized water and were found to be unity. In the FT-IR study, upon increasing water/surfactant molar ratio, W, the frequency, ν(OD), of the HOD species decreases, while its full width at half height and its area increase. The results obtained from both techniques indicate that the water appears to be present as a single nano-phase and the structure varies continuously as a result of increasing W. In addition, the effect of changing the counter-ion (Br(-) or Cl(-)) on (1)H NMR and FT-IR results was investigated. In spite of the known difference in the dissociation of these counter-ions from micellar aggregates, this was found not to affect the state of solubilized water. This report gives further insight into the contradictory scientific debates on the structure of water in the polar nano-cores of microemulsions.


Assuntos
Óleos/química , Tensoativos/química , Água/química , Cátions/química , Emulsões/química , Espectroscopia de Ressonância Magnética , Prótons , Solubilidade , Espectroscopia de Infravermelho com Transformada de Fourier
18.
Inorg Chem ; 51(2): 844-50, 2012 Jan 16.
Artigo em Inglês | MEDLINE | ID: mdl-22220745

RESUMO

A sonochemical method was employed to prepare reactive nanoparticles of FeSbO(4) at 300 °C, which is the lowest calcination temperature reported so far for preparing FeSbO(4). A systematic evolution of the FeSbO(4) phase formation as a function of temperature was monitored by in situ synchrotron X-ray measurements. The 300 and 450 °C calcined powders exhibited specific surface areas of 116 and 75 m(2)/g, respectively. The X-ray photoelectron spectra analysis confirmed the presence of mainly Fe(3+) and Sb(5+) in the calcined powder. The response of the fabricated sensors (using both 300 and 450 °C calcined powders) toward 1000 ppm and 1, 2, 4, and 8% hydrogen, respectively, has been monitored at various operating temperatures. The sensors fabricated using 300 °C calcined powder exhibited a response of 76% toward 4% H(2) gas at an operating temperature of 300 °C, while those fabricated using 450 °C calcined powder exhibited a higher response of 91% with a quick recovery toward 4% H(2) gas at 300 °C. The results confirmed that a higher calcination temperature was preferred to achieve better sensitivity and selectivity toward hydrogen in comparison to other reducing gases such as butane and methane. The experimental results confirmed that the sonochemical process can be easily used to prepare FeSbO(4) nanoparticles for various catalytic applications as demonstrated. Here, we project FeSbO(4) as a new class of material exhibiting high sensitivity toward a wide range of hydrogen gas. Such sensors that could detect high concentrations of hydrogen may find application in nuclear reactors where there will be a leakage of hydrogen.

19.
Nanotechnology ; 22(27): 275506, 2011 Jul 08.
Artigo em Inglês | MEDLINE | ID: mdl-21613735

RESUMO

The gas sensitivity exhibited by nanoparticles of 1 wt% Pd catalysed antimony doped tin dioxide (ATO) prepared by a citrate-nitrate process is reported here. The reduction of particle size to <3 nm, a dimension smaller than double the thickness of the charge depletion layer, has resulted in an exceptionally high butane sensitivity and selectivity. The sensitivity and selectivity of ATO particles of different sizes unequivocally proved that reducing the size of particles to below twice the Debye length dimension produces materials with exceptionally high sensitivity and selectivity for sensor applications. The sensitivity of the samples towards 1000 ppm butane varied in the order 98%>55%>47%, for CNP>SP>CP samples having crystallite sizes of the order of 2.4 nm to 18 nm to 25 nm, respectively. The ATO nanoparticles exhibited not only a remarkable increase in gas sensitivity of around 98% towards 1000 ppm butane at 350 °C, but also a preferential selectivity to butane compared to other gases such as CO, CO2, SO2, CH4 and H2. In addition to the exceptionally high sensitivity and selectivity, the developed sensors also exhibited an improved response time and long term stability, which are of paramount importance for practical device development.

20.
J Colloid Interface Sci ; 355(2): 282-92, 2011 Mar 15.
Artigo em Inglês | MEDLINE | ID: mdl-21232750

RESUMO

Iron oxide-hydroxide (α-Fe(2)O(3); Fe(OH)(3)) nanoparticles have been prepared by a microemulsion route using ammonia (NH(3)) solution or tetrabutylammonium hydroxide (TBAH) as precipitants. The iron oxide-hydroxide nanoparticles obtained were characterized by TGA, N(2) sorptiometry, XRD, IR, SEM, HR-TEM, and DLS techniques. Properties such as specific surface area (S(BET)), pore sizes and shapes, average particle size and distribution, crystallite structure, and thermal stability were determined. The properties of nanoparticles prepared using NH(3) and TBAH were compared after drying at 100°C and after being calcined in the temperature range 250-1100°C. It was found that the suspensions prepared using TBAH suffered immediate separation while those prepared using NH(3) resulted in very stable suspensions. Also, it was found that TBAH did not offer any advantage over NH(3) either in terms of specific surface area or in particle size of the prepared nanoparticles. Hence, the later part of the study was concentrated on the NH(3)-precipitated nanoparticles with particular emphasis on finding the most favorable, W (water-to-surfactant ratio) and/or surfactant concentration, S, to obtain the best conditions in terms of higher surface areas and narrower particle size distribution. It was found that the prepared suspension consisted of monodisperse nanoparticles (standard deviations <10%) and after separation and drying, high surface area powders were obtained. The highest surface area (315 m(2) g(-1)) was obtained when the smallest W (=20) and highest S (=0.20 mol L(-1)) were employed.

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