• Journal of the Korean Ceramic Society
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• v.34 no.7
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• pp.685-692
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• 1997

Effects of sintering temperature and time on the phase formation, the characteristics of sintering and electrical behaviors of NASICON compounds with Na3Zr2Si2PO12 and Na3.2Zr1.3Si2.2P0.8O10.5 compositions synthesized by solid state reaction were investigated. Maximum relative densities of 96% and 91% were obtained for Na3Zr2Si2PO12 and Na3.2Zr1.3Si2.2P0.8O10.5 compounds, respectively. Complex impedance analysis in a frequency range below 4 MHz was performed to measure the ionic conductivity and migration barrier height of the compounds at RT-30$0^{\circ}C$. The maximum ionic conductivity and the minimum migration barrier height were 0.45 ohm-1cm-1 and 0.07 eV, respectively. The migration barrier height of the high temperature form (space group : R3c) is about 30-40% of that of the low temperature form (space group : C2/c) in two NASICON compounds. Ionic conductivity increases with increasing sinterability, and the presence of glass phase in Na3.2Zr1.3Si2.2P0.8O10.5 compounds lowers significantly ionic conductivity at temperatures above 14$0^{\circ}C$.

• The Korean Journal of Ceramics
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• v.1 no.4
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• pp.179-184
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• 1995

Sodium superionic conductor (NASICON) compounds were prepared. The effects of sintering temperature and cooling rate on the formation and the distribution of crystalline NASICON and $ZrO_3$ second phase were investigated. In the von Alpen-type composition, the $ZrO_2$ second phase is in thermal equilibrium with the crystalline NASICON above $1320^{\circ}C$, but when cooled through 1260-$1320^{\circ}C$ crystalline NASICON was formed by reaction between $ZrO_2$ and liquid phase. Very slow cooling ($1^{\circ}C$/hr) to $1260^{\circ}C$ from sintering temperature decreased the amount of sodium which prevents the formation of the crystalline NASICON resulted high number of $ZrO_2$ grains near the surface of some sintered bodies. Maximum electrical conductivity of 0.200 ohm-1cm-1 was obtained at $300^{\circ}C$ for well-sintered samples with little $ZrO_3$. On the other hand, low conductivities were obtained for rapid-cooled samples which have less dense microstructure.

• Nuclear Engineering and Technology
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• v.55 no.5
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• pp.1885-1891
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• 2023

The present work aims to fabricate Na_1+xZr₂Si_xP_3-xO₁₂ compound at various calcination temperatures based on the zircon mineral. The fabricated compound was calcinated at 250, 500, and 1000℃. The effect of calcination temperature on the structure, crystal phase, and radiation shielding properties was studied for the fabricated compound. The X-ray diffraction diffractometer demonstrates that, the monoclinic crystal phase appeared at a calcination temperature of 250℃ and 500℃ is totally transformed to a high-symmetry hexagonal crystal phase under a calcination temperature of 1000℃. The radiation shielding capacity was also qualified for the fabricated compounds using the Monte Carlo N-Particle transport code in the g-photons energy interval between 15keV and 122keV. The impacts of calcination temperature on the g-ray shielding behavior were clarified in the present study, where the linear attenuation coefficient was enhanced by 218% at energy of 122keV, when the calcination temperature increased from 250 to 1000℃, respectively.

• Bulletin of the Korean Chemical Society
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• v.19 no.1
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• pp.5-21
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• 1998

The purpose of this paper is to show that X-ray absorption spectroscopy (XANES and EXAFS) is a powerful technique for characterizing both crystalline and amorphous solids from structural (local order) and electronic point of view. The principle of this technique is briefly described by showing the main factors which must be considered for recording and fitting the experimental results. Some non-trivial examples have been selected for demonstrating that XAS spectroscopy is the only technique for bringing a definitive answer as for example: the determination of the local distortion of the $NiO_6$ octahedra in the $Li_{1-z}Ni_{1+z}O_2$ layered oxides and the evidence of the presence of copper pairs in the NASICON-type phosphate $CuZr_2 (PO_4)_3$. Are also reported some significant examples for which XAS spectroscopy is decisive with other characterization methods as (i) Raman spectroscopy for glasses (ii) Mossbauer spectroscopy for $LiNi_{1+z-t}Fe_To_2$ oxides (iii) magnetic measurements for Ce-based intermetallic compounds.

• Proceedings of the Materials Research Society of Korea Conference
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• 2003.11a
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• pp.26-26
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• 2003

Lithium storage electrodes for rechargeable batteries require mixed electronic-ionic conduction at the particle scale in order to deliver desired energy density and power density characteristics at the device level. Recently, lithium transition metal phosphates of olivine and Nasicon structure type have become of great interest as storage cathodes for rechargeable lithium batteries due to their high energy density, low raw materials cost, environmental friendliness, and safety. However, the transport properties of this family of compounds, and especially the electronic conductivity, have not generally been adequate for practical applications. Recent work in the model olivine LiFePO$_4$, showed that control of cation stoichiometry and aliovalent doping results in electronic conductivity exceeding 10$^{-2}$ S/cm, in contrast to ~10$^{-9}$ S/cm for high purity undoped LiFePO$_4$. The increase in conductivity combined with particle size refinement upon doping allows current rates of >6 A/g to be utilized while retaining a majority of the ion storage capacity. These properties are of much practical interest for high power applications such as hybrid electric vehicles. The defect mechanism controlling electronic conductivity, and understanding of the microscopic mechanism of lithiation and delithiation obtained from combined electrochemical and microanalytical techniques, will be discussed