Authors: Kanita Srisurat, Anuson Niyompan, R. Tipakontitikul
Abstract: Na- β"-alumina solid electrolyte proposed for electric vehicle battery system application was prepared using liquid phase sintering method. Firstly, the Na- β"-alumina powder was prepared according to the formular Na1-xMg2xAl5-xO8 with x = 0.175, calcinations temperature was at 1200 C for 10 h. Calcined powder was milled and mixed with Bi2O3 or CuO in approximate concentration 1, 3 and 5 percent by mole respectively. The uniaxial dry-pressing was employed for green body forming. The green pellets were then sintered at different temperature and dwell time were kept constant for 4 h during the sintering process. Ionic conductivity measurement was performed by impedance analyzer. The XRD characterization on both powder and ceramic show that β"-alumina form as a major phase with tiny amount of the secondary phase β-alumina. The β"/β concentration proportion slightly decrease after sintering. Addition with Bi2O3 or CuO do not lead to phase change and high densification ceramic is obtained. Ionic conductivity of β"-alumina ceramic added with Bi2O3 is higher than that of ceramic with CuO addition. The relative calculated activation energy of the Na+ migration in the former composition is also lower. The highest ionic conductivity measured at 300 C is found in ceramic sample sintered at 1450 C and with 1 mol% of Bi2O3.
513
Authors: W. Prachamon, Anuson Niyompan, R. Tipakontitikul
Abstract: Na--alumina with MgO stabilized was produced through solid state reaction. High purity starting material, -Al2O3, -Al2O3, Na2CO3 and MgO were used. The desired amount of starting materials corresponding to the nominal formula Na(1+x)MgxAl(11-x)O17 were mixed and calcined at temperature 1200 for 10 h under atmospheric pressure. The effect of Al2O3 source on phase formation and averaged crystallite size of Na--alumina were investigated via X-ray diffraction (XRD), SEM and TGA/DTA. The XRD result show that formation of Na--alumina with high purity is obtained when -Al2O3 was used. The larger crystallite size is found for sample prepared form -Al2O3. For SEM study the Na--alumina microstructure is seen as randomly packing of several sheets. Calculated crystallite size of sample prepared from -Al2O3 show the larger value compared to that one prepared from -Al2O3.
272
Authors: Amporn Kamonlert, Anuson Niyompan, R. Tipakontitikul
Abstract: Powder of β-alumina solid electrolyte with general formula Na0.80Li0.20Al5O8 was prepared by solid state reaction according to the ternary systems Li2O-Na2O-Al2O3. All the calcined powders were heated at different temperatures for 1 h. The XRD results indicate that the β-alumina phase started to form at 1100 °C and these consistent with TG/DTA measurements. At constant calcined temperature of 1100 °C, When the dwell times was varied in range 5 h to 15 h, it was found that powder consists of β-alumina as a majority phase with a tiny amount of β-alumina and the β-alumina phase purity is about 82 wt% for dwell time of 10 h. The microstructures of β-alumina particles were seen as a layered structural arrangement with hexagonal shape and strong agglomeration between these particles are clearly seen.
157
Authors: R. Tipakontitikul, Amporn Kamonlert, Sukum Eitssayeam, Anuson Niyompan
Abstract: PZT-PMN ceramic system with presence of MnO2 contents were proposed and prepared using conventional sintering method as for piezoelectric transformer application. Phase formation and several dielectric and piezoelectric parameters were studied as a function of MnO2 concentration. The x-ray diffraction study revealed the tetragonal symmetry for all samples with MnO2 doping. To determine polarization, the P-E hysteresis loop were produced and the results indicated that entering of Mn4+ ions in the ceramic structure created large amount of oxygen vacancies and the consequent was observed as displacement of the loops to E axis. The obtained optimum parameter are d33 = 119 pC/N, kp = 0.207, Qm = 1669, tan = 0.0101, Pr = 20 μm/cm2 and Ec = 10 kV/cm.
381
Authors: Anuson Niyompan, Kanita Srisurat, R. Tipakontitikul
Abstract: The ferroelectric glass-ceramic of the composition Na2O-Nb2O5-Al2O3-SiO2 was prepared by controlling crystallization of the glass that added with small amount of TiO2. The effect of TiO2 content on crystallization behavior and the dielectric property were determined. X-ray diffraction studied indicated that NaNbO3, NaNbO8 and a compound of alkali alumino silicate composition were readily formed in the as-quenched glass as the product of phase separation. After treatment at 700oC for various times, NaNbO3 volume fraction was found to increase with time. Crystalline size of the NaNbO3 was lower than 300 nm and it was developed with treatment time. Presence of TiO2 had considerably effect on NaNbO3 volume fraction when treatment time shorter than 1.0 h. The dielectric response of the glass-ceramic samples was found to arise from all contributions of crystalline phases and glass matrix responds.
189
Authors: Anuson Niyompan, Kanita Srisurat, R. Tipakontitikul, Kamonpan Pengpat, Tawee Tunkasiri
Abstract: The β″-alumina solid electrolyte proposed for the application in the electric vehicle battery system was prepared via a liquid phase sintering method. The main aim of the study is to reduce sintering temperature which is normally required as high as 1700oC. The MgO-stabilized Naβ″-alumina with the composition Na1-xMg2xAl5-xO8 where x = 0.125 was prepared. The mixture of Na2CO3, MgO and γ -Al2O3 were produced and well-mixed by wet ball milling method. Then, calcination was performed at 1200oC for 10 h. Calcined β″-alumina was then added with a sintering aid, CuO, at several concentrations prior to forming by a dry pressing technique. The green pellets were then sintered at different temperatures with constant dwell time for 4 h. Phase identification on calcined powders indicate that β″-alumina present as a mojor phase co-existed with tiny proportion of β′-alumina. Co-existence of these two phases is commonly found for this particular system. Phase checking for sintered samples with CuO additive show no phase change but concentration ratio of the β′-alumina seem to increase with increasing sintering temperature and mol% of the CuO. Sintering at 1550oC, the higher densification is clearly observed for ceramic with higher CuO content, i.e. 5 and 10 mol%. Layered-structure of the β″-alumina can be clearly seen from the SEM micrographs. The SEM results also show that higher CuO content promoted a higher grain development and produced less porosity. Dc conductivity values of the samples with CuO adding are reasonable high comparing to that of without CuO adding. This study has been show that β″-alumina produced by liquid phase sintering here is considerably appropriate to the application in the battery of electric vehicles.
793
Authors: P. Pimsorn, R. Tipakontitikul, Anuson Niyompan, N. Kanchanarat, Tawee Tunkasiri
Abstract: Nano-crystalline boehmite (AlOOH) proposed as a precursor for g-Al2O3 production was prepared using precipitation process. The mixture of two starting solutions of AlN3O9.9H2O and Na2Al2O4 was formed and NaOH was used as pH adjustment. Various preparation conditions, starting pH and temperatures were applied. The results suggested that high purity AlOOH powder could be obtained at solution temperature above 60oC and starting pH was in range 7-11. Their crystalline size increased from 2.4 to 3.9 nm with increasing pH. According to the results, AlOOH from pH 8 and temperature 80oC was selected for producing the g-Al2O3 by calcination in the temperature range of 350oC-1100oC. Transformation from AlO(OH) to g-Al2O3 could be readily observed from the whole temperature range and g-Al2O3 crystalline size was increased with increasing calcination temperature. After the temperature reached 1100oC, transformation to a- and q- phases were also found. Morphology of g-Al2O3 powder shows a strong aggomeration.
653
Authors: S. Thongsaeng, Anuson Niyompan, R. Tipakontitikul, Kamonpan Pengpat
Abstract: Dielectric glass and glass-ceramics were derived from Na2O-Nb2O5-Al2O3-SiO2 system. Small amount of TiO2 were also introduced into glass compositions to study crystallization behavior of the glass with present of this nucleating agent. Conventional melt-quenching technique was employed for a glass production and the selected bulk glass samples were subjected to the heat-treatment process at appropriate temperature. After six different glass compositions were produced, and by observation with necked eyes, all obtained glass samples are in light brown color and some samples were opaque due to crystallization took place during quenching. Phase identification through XRD patterns show that there were 3 phases, NaNbO3, NaNbO8 and a sodium aluminum silicate compound, found in those opaque glass samples. NaNbO3 is a predominant phase in all samples. Fortunately, clear transparent glass was obtained from the composition with no TiO2 addition. Heat treatment of this glass did not induce phase change, three aforementioned phases still present. Increasing heat treatment time promoted a higher of observed intensity of NaNbO3. But the NaNbO3 crystalline size was not significantly developed with time. The dielectric response of the NaNbO3 crystals in the glass-ceramics samples are influenced by presence of other crystalline phases.
229
Authors: Y. Suwan, Anuson Niyompan, R. Tipakontitikul, Pitak Laoratanakul
Abstract: The PZT-PMN ceramics system was derived from Pb(Zr0.5Ti0.5)O3 and Pb(Mg2/3Nb1/3)O3 based compositions those obtained via the columbite method. The effect of MnO2 addition on microstructure, physical properties and piezoelectric properties were investigated. In this study, the composition with PZT/PMN ratio of 1:1 was selected. To observe the effect of MnO2 adding, its concentration was varied in range 0-10 mol%. Green pellets were sintered at temperature 1250oC for 4 hours. For piezoelectric investigation, the ceramics pellets were subjected to a poling process. The XRD results show that there is no phase transformation observed for all sintered PZT-PMN samples with presence of MnO2. The SEM micrographs reveal that MnO2 can enhance sinterability as evidenced by lowering of porosity and increasing of grain size with increasing of MnO2 content. Increasing of linear shrinkage and apparent densities also confirmed such effect. Improvement of d33 from 28 to 114 pC/N could only found for MnO2 in range 0 to 4 mol%. For higher MnO2 content, there is only slightly increased. However, increasing of kp with increasing of MnO2 is clearly observed. While dielectric constant measured at room temperature and at frequency 1 kHz is higher for ceramics without MnO2 doping and it decreases with increasing MnO2 concentration. The temperature dependence of relative dielectric constant go to peak of value about 6000 at temperature around 180oC and shifting of these peaks with frequency can only be observed for samples with higher MnO2 content. This indicates a normal ferroelectric behavior for sample with lower MnO2 and there are converted to relaxor after MnO2 increased.
189