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Nanosized Ni, NiCo-Y2O3 powders were successfully synthesized at low temperature via a simple polymer solution route. As an organic carrier, polyvinyl alcohol (PVA) afforded an atom-scale homogeneous precursor gel, which in turn gave fully crystallized nanosized Ni, NiCo-Y2O3 powder upon calcination at a low temperature under an Ar-4% H2 atmosphere. The PVA content, calcination temperature, heating time, and reduction conditions affected the microstructure and crystallization behavior of the as-synthesized powders. The PVA content also influenced the synthesis behavior and microstructure of the final powder. The particle size increased with an increase in the calcination temperature and decrease in the PVA content. At a PVA-metal ion ratio of 4:1, the measured particle size was about 20 nm. The results of TEM mapping on the NiCo-Y (0.6 wt%) powders revealed a well-dispersed Y2O3 phase in the NiCo crystalline matrix.
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Synroc (Synthetic Rock) consists of four main titanate phases: peroveskite (CaTiO3), zirconolite (CaZrTi2O7), hollandite (BaAl2Ti6O16) and rutile (TiO2). Nano-polycrystalline synroc powders were made by a synthesis combustion process. The combustion process, an externally initiated reaction is self-sustained owing to the exothermic reaction. A significant volume of gas is evolved during the combustion reaction and leads to loosely agglomerated powders. This exothermic reaction provides necessary heat to further carry the reaction in forward direction to produce nanocrystalline powders as the final product. Glycine is used as a fuel, being oxidized by nitrate ions. It is inexpensive, has high energy efficiency, fast heating rates, short reaction times and high compositional homogeneity. In this study, combustion synthesis of nano-sized synroc-B powder is introduced. The fabrication of synroc-B powder result of observation XRD were prepared for polycrystalline (perovskite, zirconolite, hollandite, rutile) structures. The characterization of the synthesized powders is conducted by using XRD, SEM/EDS and TEM.
Assuntos
Compostos de Cálcio/química , Cerâmica/química , Glicina/química , Nanopartículas/química , Óxidos/química , Resíduos Radioativos , Titânio/químicaRESUMO
A solution combustion process for the synthesis of perovskite (CaTiO3) powders is described. Perovskite is one of the crystalline host matrics for the disposal of high-level radioactive wastes (HLW) because it immobilizes Sr and Lns elements by forming solid solutions. Solution combustion synthesis, which is a self-sustaining oxi-reduction reaction between nitrate and organic fuel, the exothermic reaction, and the heat evolved convert the precursors into their corresponding oxide products above 1100 degrees C in air. To investigate the effects of amino acid on the combustion reaction, various types of fuels were used; a glycine, amine and carboxylic ligand mixture. Sr, La and Gd-nitrate with equivalent amounts of up to 20% of CaTiO3 were mixed with Ca and Ti nitrate and amino acid. X-ray diffraction analysis, SEM and TEM were conducted to confirm the formed phases and morphologies. While powders with an uncontrolled shape are obtained through a general oxide-route process, Ca(Sr, Lns)TiO3 powders with micro-sized soft agglomerates consisting of nano-sized primary particles can be prepared using this method.
Assuntos
Compostos de Cálcio , Cerâmica , Óxidos , Resíduos Radioativos , Estrôncio/química , Titânio , Compostos de Cálcio/síntese química , Compostos de Cálcio/química , Cerâmica/síntese química , Cerâmica/química , Óxidos/síntese química , Óxidos/química , Titânio/químicaRESUMO
Nano-sized nickel oxide powders were synthesized by an organic-inorganic solution route employing polyvinyl alcohol (PVA) as an organic carrier. In this study, it was possible to control the physical properties of the nickel oxide powders by change of the PVA content. The experimental factors, such as the PVA content, heating temperature and time, were studied for the synthesis of nano crystalline powders. Nickel nitrate, (Ni(NO3)2, reagent grade) was used as a source of nickel cation. Once the cation source was completely dissolved in de-ionized (DI) water, 5 wt% PVA solution was added to the sol solution. The resulting gel-type precursors were completely dried and then calcined or crystallized at various temperatures in an air atmosphere in a box furnace. In the high PVA content of 2:1 mixing ratio, nano crystallite nickel oxide powders of below 5 nm in size with a high specific surface area of 151.19 m2/g were obtained at low temperature of 400 degrees C for 1 h. The PVA polymer contributed to homogeneous nickel cations in atomic scale through the fabrication process of the sol precursor. In this paper, the PVA solution technique for the fabrication of nano-sized nickel oxide powders is introduced. The effects of PVA content and heating time on the powder crystallization, morphology and specific surface area are also studied. The characterization of the synthesized powders is examined by using XRD, DTA/TG, TEM and nitrogen gas adsorption.
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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).
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Cristalização/métodos , Nanoestruturas/química , Nanoestruturas/ultraestrutura , Álcool de Polivinil/química , Titânio/química , Temperatura Baixa , Substâncias Macromoleculares/química , Teste de Materiais , Conformação Molecular , Tamanho da Partícula , Pós , Propriedades de SuperfícieRESUMO
A cerium-doped YAG (Y3Al5O12) phosphor is used as a rare-earth element phosphor for blue light absorption and yellow light emission for a white light source. A solution combustion synthesis, which is a method for producing nano-powder, is a reaction that is spontaneous ignition by reaction heat released through oxidation/reduction reaction between metal nitrate and fuel. Since the reaction speed is fast and it does not go through a separate firing process, it is a method of easily synthesizing nano-powder by simple process. In this study, YAG:Ce nano-powders were prepared by using various fuels in the combustion synthesis method. Depending on the kind of the additive fuel, the reaction of the combustion synthesis process was different, and the shape of the powder particles according to the fuels was also different. The agglomerated particles of nanoparticles were observed and the characteristics of YAG:Ce powders synthesized under various conditions were analyzed.
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A Cu metal-ceramic filter composite with high thermal conductivity and a suitable thermal expansion coefficient was designed to be applied to high performance heat dissipation materials. The purpose of using the ceramic filler was to decrease the high coefficient of thermal expansion of Cu matrix utilizing the high thermal conductivity of Cu. In this study, a SiC ceramic filler powder was added to the Cu sol including Zn as a liquid phase sintering agent. The final complex was produced by applying a PVB polymer to prepare a homogeneous precursor followed by sintering in a reducing atmosphere. The pressureless sintered composite showed lower thermal conductivity than pure bulk Cu due to the some residual pores. In the case of the Cu-SiC composite in which 10 wt% of SiC filler was added, it showed a thermal conductivity of 100 W/m·°C and a thermal expansion coefficient of 13.3×10-6/°C. The thermal conductivity showed some difference from the theoretical calculated value due to the pores in the composite, but the thermal expansion coefficient did not show a significant difference.
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Various nanocrystalline metal alloy powders were synthesized by solution combustion synthesis in a reducing atmosphere in which a spray pyrolysis process was modified. Miscible Cu-Ni alloy powder and immiscible Ag-Ni alloy powder were synthesized, along with Cu-Y2O3 metal-ceramic composite powder. X-ray diffraction, SEM and TEM observations showed that the synthesized powders were nanocrystalline and well alloyed. Alloying occurred via the chemical routes of the decomposition of the metal salts, as well as the oxidation, reduction and sintering processes.
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Nano-sized SiO2 based powders were fabricated by a polymer solution technique. Nitrate metal sources and Ludox series silica sol were dissolved in D.I. water and then polyvinyl alcohol solution was added as a polymeric carrier. The metal cations were dispersed well in the solution and a homogeneous polymeric network was formed. The organic-inorganic precursor gels were turned to a porous powder with expanded volume through an explosive oxidation reaction during calcination process. The polymer molecular weight, polymer content and heating rate affected the particle agglomeration and size. The reaction between oxygen and unstable metal cations resulted in a vigorous exothermic reaction and simultaneously the reaction created extensive voids, which accompanied soft powders. The porous powders were crystallized at relatively lower temperature, and easily ground to a very fine powder having nano-sized particles. The crystalline development was also dependent on the polymer type, and the weak hydrogen bonding by optimum polymer content promoted homogeneous entrapment between the -(OH) hydroxyl groups and cations, which are solvates by water molecules.
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Cu nano particles were fabricated at a very low temperature via polymer solution and reduction firing processes using a polyvinyl alcohol (PVA) and Ar-4%H2 gas mixture. In the process, copper nitrate and 5 wt% PVA solution were dissolved in D.I. water and the organic-inorganic precursor sols were dried to porous gels. The precursor gels were calcined in an air atmosphere, and then refired at 250 degrees C-300 degrees C under an Ar-4%H2 atmosphere for the reduction of CuO. The morphology of precursor gels and CuO and Cu powders was strongly dependent on the PVA content, and the as- calcined CuO readily deoxidized to Cu with minimal residual carbon. The polymer also contributed to an atomic-scale copper cation distribution, which resulted in nano-sized CuO and Cu powders. The Cu powder synthesized with PVA content in a 4:1 ratio showed a crystallite size of about 20 nm or less. In this paper, the microstructure changes of Cu nano particles at each set of processing conditions were examined by SEM and TEM observations.
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Copper (Cu) nano particles were successfully fabricated at a significantly low temperature through a simple polymer solution route. In the process, the organic-inorganic precursor sols were turned to porous gels exhibiting volume expansion during the drying process. The PVA polymer, as an organic carrier, contributed to make an atom-scale homogeneous copper precursor gel, which resulted in fully crystallized, nano-sized copper powders through a low calcination temperature of 300 °C under Ar-4%H2 atmosphere. Variations in the processing technique, such as the content of PVA and calcination temperature, affected the microstructure and crystallization behavior of the synthesized powders. The copper powder synthesized with the PVA content of 4:1 ratio showed a crystallite size of about 10 nm or less with a high surface area. In this paper, the PVA solution technique for the fabrication of a nano-sized copper powder is introduced. The effects of the PVA content and calcination conditions on the powder morphology and crystallization are also studied. The characterization of the synthesized powders is conducted by using XRD, DTA/TG, SEM and TEM.