Search results for: nanopowders

Authors: Otilia R. Vasile, Florina C. Ilie, Irina F. Nicoara, Cristina D. Ghitulica, Roxana Trusca, Ovidiu Oprea, Vasile A. Surdu, Bogdan S. Vasile, Ecaterina Adronescu

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In this work ZnO nanostructures (nanopowders and nanostars) have been synthesized via a simple sol-gel method. The used methods for synthesizing the nanostructures involve two steps as follows: (1) precipitation of zinc acetate precursor for the synthesis of ZnO nanopowders and zinc chloride precursor for the synthesis of ZnO nanostars and (2) addition of Eu2O3 in different concentrations (1%, 3%, and 5%) using europium acetate as precursor. Detailed crystalline parameters for each of the synthetized species were analysed using X-ray diffraction. Structural transitions were also discussed. The structure and morphology of the as-prepared ZnO nanopowders and nanostars were investigated by electron microscopy. TEM investigations have shown an average particle size range from 23 to 29 nm and polyhedral and spherical morphology with tendency to form aggregates for nanopowders. For nanostars structures, a star-like morphology could be observed. Cytotoxicity tests on MG-63 cell lines were also performed. Photocatalytic activity of ZnO nanopowders have reached higher values compared to ZnO nanostars.

Keywords: cytotoxicity, photocatalytic activity, TEM, ZnO

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Authors: Oral Lacin, Turan Calban, Fatih Sevim, Taner Celik

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In this study, Pb²⁺ uptake by the hydroxyapatite nanopowders (n-Hap) from aqueous solutions was investigated by using batch adsorption techniques. The adsorption equilibrium studies were carried out as a function of contact time, adsorbent dosage, pH, temperature, and initial Pb²⁺ concentration. The results showed that the equilibrium time of adsorption was achieved within 60 min, and the effective pH was selected to be 5 (natural pH). The maximum adsorption capacity of Pb²⁺ on n-Hap was found as 565 mg.g^-1. It is believed that the results obtained for adsorption may provide a background for the detailed mechanism investigations and the pilot and industrial scale applications.

Keywords: nanopowders, hydroxyapatite, heavy metals, adsorption

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Authors: S. Sharma, U. Batra, S. Kapoor, A. Dua

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In this study, the effects and interactions of reaction time and capping agent assistance during sol-gel synthesis of magnesium substituted hydroxyapatite nanopowder (MgHA) on hydroxyapatite (HA) to β-tricalcium phosphate (β-TCP) ratio, Ca/P ratio and mean crystallite size was examined experimentally as well as through statistical analysis. MgHA nanopowders were synthesized by sol-gel technique at room temperature using aqueous solution of calcium nitrate tetrahydrate, magnesium nitrate hexahydrate and potassium dihydrogen phosphate as starting materials. The reaction time for sol-gel synthesis was varied between 15 to 60 minutes. Two process routes were followed with and without addition of triethanolamine (TEA) in the solutions. The elemental compositions of as-synthesized powders were determined using X-ray fluorescence (XRF) spectroscopy. The functional groups present in the as-synthesized MgHA nanopowders were established through Fourier Transform Infrared Spectroscopy (FTIR). The amounts of phases present, Ca/P ratio and mean crystallite sizes of MgHA nanopowders were determined using X-ray diffraction (XRD). The HA content in biphasic mixture of HA and β-TCP and Ca/P ratio in as-synthesized MgHA nanopowders increased effectively with reaction time of sols (p < 0.0001, two way Anova), however, these were independent of TEA addition (p > 0.15, two way Anova). The MgHA nanopowders synthesized with TEA assistance exhibited 14 nm lower crystallite size (p < 0.018, 2 sample t-test) compared to the powder synthesized without TEA assistance.

Keywords: capping agent, hydroxyapatite, regression analysis, sol-gel, 2- sample t-test, two-way analysis of variance (ANOVA)

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Authors: Chundong Li, V. V. Neshchimenko, M. M. Mikhailov

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The effect of the modification of ZnO powders by ZrO2, Al2O3, TiO2, SiO2, CeO2 and Y2O3 nanoparticles with a concentration of 1-30 wt % is investigated by diffuse reflectance spectra within the wavelength range 200 to 2500 nm before and after 100 keV proton and electron irradiation. It has been established that the introduction of nanoparticles ZrO2, Al2O3 enhances the optical stability of the pigments under proton irradiation, but reduces it under electron irradiation. Modifying with TiO2, SiO2, CeO2, Y2O3 nanopowders leads to decrease radiation stability in both types of irradiation. Samples modified by 5 wt. % of ZrO2 nanoparticles have the highest stability of optical properties after proton exposure. The degradation of optical properties under electron irradiation is not high for this concentration of nanoparticles. A decrease in the absorption of pigments modified with nanoparticles proton exposure is determined by a decrease in the intensity of bands located in the UV and visible regions. After electron exposure the absorption bands have in the whole spectrum range.

Keywords: irradiation, nanopowders, radiation stability, zinc oxide

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Authors: N. Flores-Martinez, G. Franceschin, T. Gaudisson, J.-M. Greneche, R. Valenzuela-Monjaras, S. Ammar

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Tailoring bulk materials keeping their nanoscale properties is the daydream of material scientists. But especially in magnetism, this single desire can revolutionize our everyday life. Now, thanks to the methods of synthesis, based on the combination of colloidal chemistry (CC) to flash sintering (FS), customizing magnets becomes each time more 'easy', 'cheap' and 'clean'. Although by CC we can obtain straightway nanopowders with good magnetic featuring, like exchange bias (EB) phenomenon, it does not result so attractive for applications. Since a solid material is simple to manipulate and integrate in a device, many consolidation methods have been tested aiming to keep the nanopowders characteristics after consolidation. Unfortunately, the lack of structural crystalline arrangement and the grain growth worsen the magnetic properties. In this work, we exhibit, for the first-time author’s best knowledge, the EB in sintered ceramics, starting from CoFe₂O₄-core@CoO-shell NPs obtained by CC. Despite the fact that EB field is about 28 mT in ceramics and it is not yet considered for applications, this work opens an alternative in the permanent magnets fabrication through a FS method, the spark plasma sintering, starting from CC synthesized nanopowders.

Keywords: core-shell nanoparticles, exchange bias, nanostructured ceramics, spark plasma sintering

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Authors: Andrey V. Samokhin, Nikolay V. Alekseev, Mikhail A. Sinaiskii

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The report presents the results of R&D of plasma-chemical production of W, W-Cu, W-Ni-Fe nanopowders as well as spherical micropowders of these compounds for their use in modern 3D printing technologies. Plasma-chemical synthesis of nanopowdersis based on the reduction of tungsten oxide compounds powders in a stream of hydrogen-containing low-temperature thermal plasma generated in an electric arc plasma torch. The synthesis of W-Cu and W-Ni-Fe nanocompositesiscarried out using the reduction of a mixture of the metal oxides. Using the synthesized tungsten-based nanocomposites powders, spherical composite micropowders with a submicron structure canbe manufactured by spray dryinggranulation of nanopowder suspension and subsequent densification and spheroidization of granules by melting in a low-temperature thermal plasma flow. The DC arc plasma systems are usedfor the synthesis of nanopowdersas well as for the spheroidization of microgranuls. Plasma systems have a capacity of up to 1 kg/h for nanopowder and up to 5 kg/h for spheroidized powder. All synthesized nanopowders consist of aggregated particles with sizes less than 100 nm, and nanoparticles of W-Cu and W-Ni-Fe composites have core (W) –shell (Cu or Ni-Fe) structures. The resulting dense spherical microparticles with a size of 20-60 microns have a submicron structure with a uniform distribution of metals over the particle volume. The produced tungsten-based nano- and spherical micropowderscan be used to develop new materials and manufacture products using advanced modern technologies.

Keywords: plasma, powders, production, tungsten-based

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Authors: A. V. Samokhin, A. A. Fadeev, M. A. Sinaiskii, N. V. Alekseev, A. V. Kolesnikov

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Composite materials where metal matrix is reinforced by ceramic or metal particles are of great interest for use in the manufacturing of electrical contacts. Significant improvement of the composite physical and mechanical properties as well as increase of the performance parameters of composite-based products can be achieved if the nanoscale structure in the composite materials is obtained by using nanosized powders as starting components. The results of nanosized composite powders synthesis (Ag-SnO2, W-Cu and Cu-C) in the DC thermal plasma flows are presented in this paper. The investigations included the following processes: - Recondensation of micron powder mixture Ag + SnO2 in a nitrogen plasma; - The reduction of the oxide powders mixture (WO3 + CuO) in a hydrogen-nitrogen plasma; - Decomposition of the copper formate and copper acetate powders in nitrogen plasma. The calculations of equilibrium compositions of multicomponent systems Ag-Sn-O-N, W-Cu-O-H-N and Cu-O-C-H-N in the temperature range of 400-5000 K were carried to estimate basic process characteristics. Experimental studies of the processes were performed using a plasma reactor with a confined jet flow. The plasma jet net power was in the range of 2 - 13 kW, and the feedstock flow rate was up to 0.35 kg/h. The obtained powders were characterized by TEM, HR-TEM, SEM, EDS, ED-XRF, XRD, BET and QEA methods. Nanocomposite Ag-SnO2 (12 wt. %). Processing of the initial powder mixture (Ag-SnO2) in nitrogen thermal plasma stream allowed to produce nanopowders with a specific surface area up to 24 m2/g, consisting predominantly of particles with size less than 100 nm. According to XRD results, tin was present in the obtained products as SnO2 phase, and also as intermetallic phases AgxSn. Nanocomposite W-Cu (20 wt .%). Reduction of (WO3+CuO) mixture in the hydrogen-nitrogen plasma provides W-Cu nanopowder with particle sizes in the range of 10-150 nm. The particles have mainly spherical shape and structure tungsten core - copper shell. The thickness of the shell is about several nanometers, the shell is composed of copper and its oxides (Cu2O, CuO). The nanopowders had 1.5 wt. % oxygen impurity. Heat treatment in a hydrogen atmosphere allows to reduce the oxygen content to less than 0.1 wt. %. Nanocomposite Cu-C. Copper nanopowders were found as products of the starting copper compounds decomposition. The nanopowders primarily had a spherical shape with a particle size of less than 100 nm. The main phase was copper, with small amount of Cu2O and CuO oxides. Copper formate decomposition products had a specific surface area 2.5-7 m2/g and contained 0.15 - 4 wt. % carbon; and copper acetate decomposition products had the specific surface area 5-35 m2/g, and carbon content of 0.3 - 5 wt. %. Compacting of nanocomposites (sintering in hydrogen for Ag-SnO2 and electric spark sintering (SPS) for W-Cu) showed that the samples having a relative density of 97-98 % can be obtained with a submicron structure. The studies indicate the possibility of using high-intensity plasma processes to create new technologies to produce nanocomposite materials for electric contacts.

Keywords: electrical contact, material, nanocomposite, plasma, synthesis

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Authors: Anastasia Beketova, Emmanouil-George C. Tzanakakis, Ioannis G. Tzoutzas, Eleana Kontonasaki

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In restorative dentistry, yttria-stabilized zirconia (YSZ) nanoparticles can be applied as fillers to improve the mechanical properties of various resin-based materials. Using sol-gel based synthesis as simple and cost-effective method, nano-sized YSZ particles with high purity can be produced. The aim of this study was to synthesize YSZ nanoparticles by the Pechini sol-gel method at different temperatures and to investigate their composition, structure, and morphology. YSZ nanopowders were synthesized by the sol-gel method using zirconium oxychloride octahydrate (ZrOCl₂.8H₂O) and yttrium nitrate hexahydrate (Y(NO₃)₃.6H₂O) as precursors with the addition of acid chelating agents to control hydrolysis and gelation reactions. The obtained powders underwent TG_DTA analysis and were sintered at three different temperatures: 800, 1000, and 1200°C for 2 hours. Their composition and morphology were investigated by Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction Analysis (XRD), Scanning Electron Microscopy with associated with Energy Dispersive X-ray analyzer (SEM-EDX), Transmission Electron Microscopy (TEM) methods, and Dynamic Light Scattering (DLS). FTIR and XRD analysis showed the presence of pure tetragonal phase in the composition of nanopowders. By increasing the calcination temperature, the crystallinity of materials increased, reaching 47.2 nm for the YSZ1200 specimens. SEM analysis at high magnifications and DLS analysis showed submicron-sized particles with good dispersion and low agglomeration, which increased in size as the sintering temperature was elevated. From the TEM images of the YSZ1000 specimen, it can be seen that zirconia nanoparticles are uniform in size and shape and attain an average particle size of about 50 nm. The electron diffraction patterns clearly revealed ring patterns of polycrystalline tetragonal zirconia phase. Pure YSZ nanopowders have been successfully synthesized by the sol-gel method at different temperatures. Their size is small, and uniform, allowing their incorporation of dental luting resin cements to improve their mechanical properties and possibly enhance the bond strength of demanding dental ceramics such as zirconia to the tooth structure. This research is co-financed by Greece and the European Union (European Social Fund- ESF) through the Operational Programme 'Human Resources Development, Education and Lifelong Learning 2014- 2020' in the context of the project 'Development of zirconia adhesion cements with stabilized zirconia nanoparticles: physicochemical properties and bond strength under aging conditions' (MIS 5047876).

Keywords: dental cements, nanoparticles, sol-gel, yttria-stabilized zirconia, YSZ

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Authors: Adriana-Gabriela Plaiasu, Catalin Marian Ducu

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The interest in the unique properties associated with materials having structures on a nanometer scale has been increasing at an exponential rate in last decade. Among the functional mineral compounds such as perovskite (CaTiO3), rutile (TiO2), CaF2, spinel (MgAl2O4), wurtzite (ZnS), zincite (ZnO) and the cupric oxide (CuO) has been used in numerous applications such as catalysis, semiconductors, batteries, gas sensors, biosensors, field transistors and medicine. The Solar Physical Vapor Deposition (SPVD) presented in the paper as elaboration method is an original process to prepare nanopowders working under concentrated sunlight in 2kW solar furnaces. The influence of the synthesis parameters on the chemical and microstructural characteristics of zinc and manganese oxides synthesized nanophases has been systematically studied using XRD, TEM and SEM.

Keywords: characterization, morphological, nano-oxides, structural

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Authors: Gabouze Nourredine, Saloua Merazga

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Due to their exceptional durability, low-cost, high-power density, and reliability, cathodes based on titanium dioxide, and more specifically spinel LTO (Li4Ti5O12), present an attractive alternative to conventional lithium cathode materials for multiple applications. The aim of this work is to synthesize and characterize the nanopowders of titanium dioxide (TiO₂) and lithium titanate (Li₄Ti5O₁₂) by the hydrothermal method and to use them as a cathode in a lithium-ion battery. The structural and morphological characterizations of the synthesized powders were performed by XRD, SEM, EDS, and FTIR-ATR. Nevertheless, the study of the electrochemical performances of the elaborated electrode materials was carried out by: cyclic voltametry (CV) and galvanostatic charge/discharge (CDG). The prepared electrode by the powder annealed at 800 °C has a good specific capacity of about 173 mAh/g and a good cyclic stability

Keywords: lithuim-ion, battery, LTO, tio2, capacity

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Authors: S. Merazga, F. Boudeffar, A. Bouaoua, A. Cheriet, M. Berouaken, M. Mebarki, K. Ayouz, N. Gabouze

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Several anode materials as transition metal oxides (Fe3O4, SnO2 a, SnO2, LiCoO2, and Li₄Ti₅O₁₂) has been used. Although titanium oxide has attracted great attention as a; superior electrode for Li-ion batteries due tohis excellent characteristic such as: high capacity, low cost and non-toxicity. In this work, the Synthesis and Characterization of Si Doped Li₄Ti₅O₁₂ with hydrothermal Method was electrochemically evaluated. The SEM images shows that the morphology of LTO powders sizes in the range 70nm.The electrochemical properties of synthesizer nanopowders are investigated for use as an anode active material for lithium-ion batteries by galvanostatic techniques in Li-half cells, obtaining reversible discharge capacity of 173.8 mAh/g at 0.1C even upon 100 cycles.Though the doped powders exhibit an upgrade in The electrical conductivity , This is suitable for use as a high-power cathode material for lithium-ion batteries.

Keywords: LTO, li-ion, battteries, anode

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Authors: Nikoloz Jalabadze, Roin Chedia, Lili Nadaraia, Levan Khundadze

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Nanocrystalline materials in powder condition can be manufactured by a number of different methods, however manufacture of composite materials product in the same nanocrystalline state is still a problem because the processes of compaction and synthesis of nanocrystalline powders go with intensive growth of particles – the process which promotes formation of pieces in an ordinary crystalline state instead of being crystallized in the desirable nanocrystalline state. To date spark plasma sintering (SPS) has been considered as the most promising and energy efficient method for producing dense bodies of composite materials. An advantage of the SPS method in comparison with other methods is mainly low temperature and short time of the sintering procedure. That finally gives an opportunity to obtain dense material with nanocrystalline structure. Graphene has recently garnered significant interest as a reinforcing phase in composite materials because of its excellent electrical, thermal and mechanical properties. Graphene nanoplatelets (GNPs) in particular have attracted much interest as reinforcements for ceramic matrix composites (mostly in Al2O3, Si3N4, TiO2, ZrB2 a. c.). SPS has been shown to fully densify a variety of ceramic systems effectively including Al2O3 and often with improvements in mechanical and functional behavior. Alumina consolidated by SPS has been shown to have superior hardness, fracture toughness, plasticity and optical translucency compared to conventionally processed alumina. Knowledge of how GNPs influence sintering behavior is important to effectively process and manufacture process. In this study, the effects of GNPs on the SPS processing of Al2O3 are investigated by systematically varying sintering temperature, holding time and pressure. Our experiments showed that SPS process is also appropriate for the synthesis of nanocrystalline powders of alumina-graphene composites. Depending on the size of the molds, it is possible to obtain different amount of nanopowders. Investigation of the structure, physical-chemical, mechanical and performance properties of the elaborated composite materials was performed. The results of this study provide a fundamental understanding of the effects of GNP on sintering behavior, thereby providing a foundation for future optimization of the processing of these promising nanocomposite systems.

Keywords: alumina oxide, ceramic matrix composites, graphene nanoplatelets, spark-plasma sintering

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Authors: Nikolai A. Khlebnikov, Vladimir N. Krasilnikov, Evgenii V. Polyakov, Anastasia A. Maltceva

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Carbon materials with advanced surfaces are widely used both in modern industry and in environmental protection. The physical-chemical nature of these materials is determined by the morphology of primary atomic and molecular carbon structures, which are the basis for synthesizing the following materials: zero-dimensional (fullerenes), one-dimensional (fiber, tubes), two-dimensional (graphene) carbon nanostructures, three-dimensional (multi-layer graphene, graphite, foams) with unique physical-chemical and functional properties. Experience shows that the microscopic morphological level is the basis for the creation of the next mesoscopic morphological level. The dependence of the morphology on the chemical way and process prehistory (crystallization, colloids formation, liquid crystal state and other) is the peculiarity of the last called level. These factors determine the consumer properties of carbon materials, such as specific surface area, porosity, chemical resistance in corrosive environments, catalytic and adsorption activities. Based on the developed ideology of thin precursor synthesis, the authors discuss one of the approaches of the porosity control of carbon-containing materials with a given aggregates morphology. The low-temperature thermolysis of precursors in a gas environment of a given composition is the basis of the above-mentioned idea. The processes of carbothermic precursor synthesis of two different compounds: tungsten carbide WC:nC and zinc oxide ZnO:nC containing an impurity phase in the form of free carbon were selected as subjects of the research. In the first case, the transition metal (tungsten) forming carbides was the object of the synthesis. In the second case, there was selected zinc that does not form carbides. The synthesis of both kinds of transition metals compounds was conducted by the method of precursor carbothermic synthesis from the organic solution. ZnO:nC composites were obtained by thermolysis of succinate Zn(OO(CH2)2OO), formate glycolate Zn(HCOO)(OCH2CH2O)1/2, glycerolate Zn(OCH2CHOCH2OH), and tartrate Zn(OOCCH(OH)CH(OH)COO). WC:nC composite was synthesized from ammonium paratungstate and glycerol. In all cases, carbon structures that are specific for diamond- like carbon forms appeared on the surface of WC and ZnO particles after the heat treatment. Tungsten carbide and zinc oxide were removed from the composites by selective chemical dissolution preserving the amorphous carbon phase. This work presents the results of investigating WC:nC and ZnO:nC composites and carbon nanopowders with tubular, tape, plate and onion morphologies of aggregates that are separated by chemical dissolution of WC and ZnO from the composites by the following methods: SEM, TEM, XPA, Raman spectroscopy, and BET. The connection between the carbon morphology under the conditions of synthesis and chemical nature of the precursor and the possibility of regulation of the morphology with the specific surface area up to 1700-2000 m2/g of carbon-structured materials are discussed.

Keywords: carbon morphology, composite materials, precursor synthesis, tungsten carbide, zinc oxide

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Authors: Glauco M. M. M. Lustosa, João Paulo C. Costa, Leinig Antônio Perazolli, Maria Aparecida Zaghete

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SnO2 has electrical conductivity due to the excess of electrons and structural defects, being its electrical behavior highly dependent on sintering temperature and chemical composition. The addition of metals modifiers into the crystalline structure can improve and controlling the behavior of some semiconductor oxides that can therefore develop different applications such as varistors (ceramic with non-ohmic behavior between current and voltage, i.e. conductive during normal operation and resistive during overvoltage). The polymeric precursor method, based on the complexation reaction between metal ion and policarboxylic acid and then polymerized with ethylene glycol, was used to obtain nanopowders ceramic. The metal immobilization reduces its segregation during the decomposition of the polyester resulting in a crystalline oxide with high chemical homogeneity. The preparation of films from ceramics nanoparticles using electrophoretic deposition method (EPD) brings prospects for a new generation of smaller size devices with easy integration technology. EPD allows to control time and current and therefore it can have control of the thickness, surface roughness and the film density, quickly and with low production costs. The sintering process is key to control size and grain boundary density of the film. In this step, there is the diffusion of metals that promote densification and control of intrinsic defects or change these defects which will form and modify the potential barrier in the grain boundary. The use of microwave oven for sintering is an advantageous process due to the fast and homogeneous heating rate, promoting the diffusion and densification without irregular grain growth. This research was done a comparative study of sintering temperature by use of zinc as modifier agent to verify the influence on sintering step aiming to promote densification and grain growth, which influences the potential barrier formation and then changed the electrical behavior. SnO2-nanoparticles were obtained with 1 %mol of ZnO + 0.05 %mol of Nb2O5 (SZN), deposited as film through EPD (voltage 2 kV, time of 10 min) on Si/Pt substrate. Sintering was made in a microwave oven at 800, 900 and 1000 °C. For complete coverage of the substrate by nanoparticles with low surface roughness and uniform thickness was added 0.02 g of solid iodine in alcoholic suspension SnO2 to increase particle surface charge. They were also used magneto in EPD system that improved the deposition rate forming a compact film. Using a scanning electron microscope of high resolution (SEM_FEG) it was observed nanoparticles with average size between 10-20 nm, after sintering the average size was 150 to 200 nm and thickness of 5 µm. Also, it was verified that the temperature at 1000 °C was the most efficient in sintering. The best sintering time was also recorded and determined as 40 minutes. After sintering, the films were recovered with Cr3+ ions layer by EPD, then the films were again thermally treated. The electrical characterizations (nonlinear coefficient of 11.4, voltage rupture of ~60 V and leakage current = 4.8x10−6 A), allow considering the new methodology suitable for prepare SnO2-based varistor applied for development of electrical protection devices for low voltage.

Keywords: chemical synthesis, electrophoretic deposition, microwave sintering, tin dioxide

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