• Proceedings of the Korean Nuclear Society Conference
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• 1997.05b
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• pp.195-200
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• 1997

핵융합로 증식재용 r-LiAlO$_2$, Li$_2$ZrO$_3$, Li$_2$TiO$_3$ 분말을 자발착화 연소반응법으로 합성하였다. LiAlO$_2$와 달리 Li$_2$ZrO$_3$ 와 Li$_2$TiO$_3$는 가열하는 동안 침전물이 생겼지만 카르복실산기만을 지닌 구연산과 아민기만을 지닌 우레아를 화학정량의 조성으로 혼합한 연료로 쉽게 분말을 합성할 수 있었다. LiAlO$_2$나 Li$_2$TiO$_3$분말은 별도의 하소 공정이필요없이 원하는 결정상이 형성되었으며, Li$_2$ZrO$_3$분말은 Li이 과량인 상이 형성되므로 110$0^{\circ}C$에서 하소하여 원하는 상을 얻었다. 합성된 Li계 산화물 분말은 비표면적 10~17 $m^2$/g으로 약 150 nm정도의 입자크기를 갖는 미세한 입자이었다.

• Korean Chemical Engineering Research
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• v.46 no.1
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• pp.69-75
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• 2008

Discharge capacity of $LiCoO_2$ in preparation by mechanochemical process decreased remarkably over 4.3V. However, Zr coating of $LiCoO_2$ showed very stable electrochemical properties up to 4.5V. Zr coating of $LiCoO_2$ in this experiment showed the discharge capacity of 197 mAh/g at 3.0-4.5V, and it maintained 96% of the initial discharge capacity after 50 cycle of charge/discharge.

• Journal of the Korean Ceramic Society
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• v.44 no.4 s.299
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• pp.219-223
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• 2007

The ionic conductivity of $Li_2O-ZrO_2-SiO_2$ glasses has been designed and analyzed on the basis of a mixture design experiment with constraints. Fitted models for the activation energy and the ionic conductivity are as follows: $Q(kJ/moi)=54.8565x_1+144.825x_2+133.846x_3-170.908x_1x_3-334.338x_2x_3$ $log{\sigma}(300K)=-5.00245x_1-1.17876x_2-15.5173x_3+17.4522x_1x_3$. The electrical properties are very sensitive to the ratio of $Li_2O/SiO_2$. The effect of $ZrO_2$ is less than that of this ratio but $ZrO_2$ component attributes to the reduction of the activation energy. The optimal composition for best ionic conduction based on these fitted models is $55Li_2O{\cdot}10ZrO_2{\cdot}35SiO_2$. Its activation energy and ionic conductivity at 300 K are 46.98 kJ/mol and $1.08{\times}10^{-5}{\Omega}^{-1}{\cdot}cm^{-1}$, respectively.

• Journal of the Korean Ceramic Society
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• v.45 no.3
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• pp.167-171
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• 2008

Zirconium-doped $Li_{1.1}Co_{1-x}Zr_xO_2(0{\leq}x{\leq}0.05)$ powders as cathode materials for lithium ion batteries were synthesized using an ultrasonic spray pyrolysis method. Cyclic voltammetry and cyclic stability tests were performed, and the changes of microstructure were observed. The solubility limit of zirconium into $Li_{1.1}CoO_2$ was less than 5 mol%, and monoclinic $Li_2ZrO_3$ phase was formed above the limit. The Zr-doping suppressed the grain growth and increased the lattice parameters of the hexagonal $LiCoO_2$ phase. The Zr-dopiong of 1mol% resulted in the best cyclic performance in the range of $3.0{\sim}4.3V$ at 1C rate (140 mA/g); the initial discharge capacity decreased from 158 mAh/g to 60 mAh/g in the undoped powder, while from 154 mAh/g to 135 mAh/g in the Zr-doped powder of 1 mol% after 30 cycles. The excellent cycle stability of Zr-doped powder was due to the low polarization during chargedischarge processes which resulted from the delayed collapse of the crystal structure of the active materials with Zr-doping.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.19 no.2
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• pp.271-278
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• 2021

In this study, a chlorination technique for recycling Li₂ZrO₃, a reaction product of ZrO₂-assisted rinsing process, was investigated to minimize the generation of secondary radioactive pyroprocessing waste. It was found that the reaction temperature was a key parameter that determined the reaction rate and maximum conversion ratio. In the temperature range of 400-600℃, an increase in the reaction temperature resulted in a profound increase in the reaction rate. Hence, according to the experimental results, a reaction temperature of at least 450℃ was proposed to ensure a Li₂ZrO₃ conversion ratio that exceeded 80% within 8 h of the reaction time. The activation energy was found to be 102 ± 2 kJ·mol^-1·K^-1 between 450 and 500℃. The formation of LiCl and ZrO₂ as reaction products was confirmed by X-ray diffraction analysis. The experimental results obtained at various total flow rates revealed that the overall reaction rate depends on the Cl₂ mass transfer rate in the experimental condition. The results of this study prove that the chlorination technique provides a solution to minimize the amount of radioactive waste generated during the ZrO₂-assisted rinsing process.

• Journal of the Korean Ceramic Society
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• v.53 no.6
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• pp.712-718
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• 2016

In this study, we investigate the effect of the$Li_3BO_3$ additive on the densification and ionic conductivity of garnet-type $Li_7La_3Zr_2O_{12}$ solid electrolytes for all-solid-state lithium batteries. We analyze their densification behavior with the addition of $Li_3BO_3$ in the range of 2-10 wt.% by dilatometer measurements and isothermal sintering. Dilatometry analysis reveals that the sintering of $Li_7La_3Zr_2O_{12}-Li_3BO_3$ composites is characterized by two stages, resulting in two peaks, which show a significant dependence on the $Li_3BO_3$ additive content, in the shrinkage rate curves. Sintered density and total ion conductivity of the system increases with increasing $Li_3BO_3$ content. After sintering at $1100^{\circ}C$ for 8 h, the $Li_7La_3Zr_2O_{12}-8$ wt.% $Li_3BO_3$ composite shows a total ionic conductivity of $1.61{\times}10^{-5}Scm^{-1}$, while that of the pure $Li_7La_3Zr_2O_{12}$ is only $5.98{\times}10^{-6}Scm^{-1}$.

• Korean Journal of Materials Research
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• v.9 no.10
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• pp.1041-1046
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• 1999

(Zr(sub)0.8Sn(sub)0.2)$TiO_4$세라믹스와 소결조제로서 ($B_2$$O_3$.Li$_2$O)의 첨가에 따른 마이크로파 유전특성 및 미세구조에 미치는 영향에 대하여 연구하였다. 1.0 mol.% $Sb_2$O(sub)5를 첨가하고 130$0^{\circ}C$에서 5시간 소결한 (Zr(sub)0.8Sn(sub)0.2)$TiO_4$세라믹스의 경우 ($B_2$$O_3$.Li$_2$O)첨가량 증가에 따라 치밀화 및 결정립 성장에 의해 유전상수와 Q.f값은 증가하여 첨가량이 0.35wt.%에서 최대값인 38과 59,000을 각각 나타내었으며, 0.50wt.% 이상 첨가한 경우에서는 제 2상의 생성으로 인하여 감소하였다. 1.0 mol% Sb$_2$O(sub)5와 0.35wt.% ($B_2$$O_3$.$Li_2$O)를 첨가한 (Zr(sub)0.8Sn(sub)0.2)TiO$_4$세라믹스를 125$0^{\circ}C$와 135$0^{\circ}C$에서 5시간 소결한 경우에는 각각 미반응 TiO$_2$의 존재와 과대입자성장에 의한 결정립내기공의 생성으로 인하여 마이크로파 유전특성은 저하되었다.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.28 no.6
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• pp.229-234
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• 2018

The glass-ceramic of $Li_2O-Al_2O_3-SiO_2$ system was synthesized by using $ZrO_2$, $ZrSiO_4$, $ZrOCl_2$ and $Zr(SO_4)_2$, which is a raw material of Zr serving as a nucleation agent. It was confirmed that Avrami parameter of these four glasses is over 3 for bulk crystallization. The glass synthesized by $ZrOCl_2$, and $Zr(SO_4)_2$ showed high melting quality during the melting process. It is also observed that the Zr component is uniformly distributed in the glass. Various characterizations was evaluated, including composition analysis and bending strength.

• Journal of the Korean Ceramic Society
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• v.13 no.1
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• pp.30-34
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• 1976

In general the chemical composition of glass ceramics in Li2O-Al2O3-SiO2 system is similar to the composition of $\beta$-spodumene (Li2O-Al2O3-4SiO2). With the object to manufacture the glass ceramics which can be produced in the domestic pot the composition of glass was so settled at 1.0 Li2O.0.9Al2O3.6.0SiO2 in order to reduce the contents of Li2O, to prevent the corrosion of the pot and to decrease the cost of raw materials. 0.2 mole and 0.1 mole of the mixture of TiO2 and ZrO2 as nucleants were added to the basic composition of 1.0 Li2O-0.9Al2O3-6.0SiO2. Each sample was divided into two kinds with a TiO2/ZrO2 ratio of 2 to 1 and the other with a TiO2/ZrO2 ratio fo 1 to 1. Thermal expansion coefficient, the most important property of glass ceramics, was tested. The softening point and the melting point of the samples were observed by the use of a heating microscope. The results obtained were as follows. The manufacturing of glass ceramics seems to be possible in the industrial plant using the domestic pot. 1) The composition of the glass which can be melted in the domestic pot process was near 1.0 Li2O.0.9Al2O3.6.0SiO2. 2) The temperature range of crystal creation and crystal growth was between 850-94$0^{\circ}C$, and 5 hours holding the samples at the temperature range was enough to crystallize them. The major crystal was $\beta$-spdumene and there existed petalite partialy. 3) The thermal expansion coefficient fo the crystallized glass was negative. 4) The deforming point of the crystallized glass was 1435$^{\circ}C$.

• Journal of Powder Materials
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• v.25 no.2
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• pp.151-157
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• 2018

In this study, the compound $Li_3BO_3$ (LBO) is intended to be prepared by a polymeric complex method as a sintering aid for the densification of $Li_7La_3Zr_2O_{12}$ (LLZ) solid electrolyte. A polymeric precursor containing Li and B is heat-treated in an air atmosphere at a temperature range between $600^{\circ}C$ and $800^{\circ}C$. Instead of LBO, the compound $Li_{2+x}C_{1-x}B_xO_3$ (LCBO) is unexpectedly synthesized after a heat-treatment of $700^{\circ}C$. The effect of LCBO addition on sintering behavior and ion conductivity of LLZ is studied. It is found that the LCBO compound could lead to significant improvements in the densification and ionic conductivity of LLZ compared to pure LLZ. After sintering at $1100^{\circ}C$, the density of the LLZ-12wt%LBO composite is $3.72g/cm^3$, with a high Li-ion conductivity of $1.18{\times}10^{-4}Scm^{-1}$ at $28^{\circ}C$, while the pure LLZ specimen had a densify of $2.98g/cm^3$ and Li-ion conductivity of $5.98{\times}10^{-6}Scm^{-1}$.