• 한국재료학회지
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• 제25권8호
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• pp.423-428
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• 2015

Impedancemetric $NO_x$ (NO and $NO_2$) gas sensors were designed with a stacked-layer structure and fabricated using $LaCr_xCo_{1-x}O_3$ (x = 0, 0.2, 0.5, 0.8 and 1) as the receptor material and $Li_{1.3}Al_{0.3}Ti_{1.7}(PO_4)_3$ plates as the solid-electrolyte transducer material. The $LaCr_xCo_{1-x}O_3$ layers were prepared with a polymeric precursor method that used ethylene glycol as the solvent, acetyl acetone as the chelating agent, and polyvinylpyrrolidone as the polymer additive. The effects of the Co concentration on the structural, morphological, and $NO_x$ sensing properties of the $LaCr_xCo_{1-x}O_3$ powders were investigated with powder X-ray diffraction, field emission scanning electron microscopy, and its response to 20~250 ppm of $NO_x$ at $400^{\circ}C$ (for 1 kHz and 0.5 V), respectively. When the as-prepared precursors were calcined at $700^{\circ}C$, only a single phase was detected, which corresponded to a perovskite-type structure. The XRD results showed that as the Co concentration of the $LaCr_xCo_{1-x}O_3$powders increased, the crystal structure was transformed from an orthorhombic phase to a rhombohedral phase. Moreover, the $LaCr_xCo_{1-x}O_3$ powders with $0{\leq}x<0.8$ had a rhombohedral symmetry. The size of the particles in the $LaCr_xCo_{1-x}O_3$powders increased from 0.1 to $0.5{\mu}m$ as the Co concentration increased. The sensing performance of the stack-structured $LaCr_xCo_{1-x}O_3/Li_{1.3}Al_{0.3}Ti_{1.7}(PO_4)_3$ sensors was found to divide the impedance component between the resistance and capacitance. The response of these sensors to NO gas was more sensitive than that to $NO_2$ gas. Compared to other impedancemetric sensors, the $LaCr_{0.8}Co_{0.2}O_3/Li_{1.3}Al_{0.3}Ti_{1.7}(PO_4)_3$ sensor exhibited good reversibility and reliable sensingresponse properties for $NO_x$ gases.

• 자원리싸이클링
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• 제33권1호
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• pp.22-30
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• 2024

2차원 물질 MXene의 전구체로 사용되는 Ti₃AlC₂ MAX 상 합성을 위해, 출발물질로써 타이타늄 (Ti) 스크랩을 활용하는 것은 경제적인 접근이 될 수 있다. 본 연구는 Ti 스크랩을 활용하여 Ti₃AlC₂ MAX상의 상분율 향상을 위한 합성 조건의 최적화를 수행하였다. Ti 스크랩으로부터 수소화-탈수소화(hydrogenation-dehydrogenation, HDH) 공정에 의해 제조된 Ti 분말의 산소 함량은 고상탈산(Deoxidation in solid state, DOSS) 공정을 통하여 효과적으로 감소되었다. 최적 합성 조건은 25 ~ 32 ㎛의 DOSS-Ti, Al, graphite 분말을 3:1.1:2의 몰 비율로 혼합하여 합성되었다. 이 때의 Ti₃AlC₂, TiC 및 Al₃Ti의 상분율은 각각 97.25%, 0.93%, 1.82%로 나타났으며, 25 ~ 45 ㎛의 Ti₃AlC₂ MAX 분말의 산소 함량은 4,210 ppm으로 확인되었다.

• 한국재료학회지
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• 제34권4호
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• pp.185-193
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• 2024

In this study, NASICON-type Li_1+XGa_XTi_2-X(PO₄)₃ (x = 0.1, 0.3 and 0.4) solid-state electrolytes for all-solid-state batteries were synthesized through the sol-gel method. In addition, the influence on the ion conductivity of solid-state electrolytes when partially substituted for Ti⁴⁺ (0.61Å) site to Ga³⁺ (0.62Å) of trivalent cations was investigated. The obtained precursor was heat treated at 450 ℃, and a single crystalline phase of Li_1+XGa_XTi_2-X(PO₄)₃ systems was obtained at a calcination temperature above 650 ℃. Additionally, the calcinated powders were pelletized and sintered at temperatures from 800 ℃ to 1,000 ℃ at 100 ℃ intervals. The synthesized powder and sintered bodies of Li_1+XGa_XTi_2-X(PO₄)₃ were characterized using TG-DTA, XRD, XPS and FE-SEM. The ionic conduction properties as solid-state electrolytes were investigated by AC impedance. As a result, Li_1+XGa_XTi_2-X(PO₄)₃ was successfully produced in all cases. However, a GaPO₄ impurity was formed due to the high sintering temperatures and high Ga content. The crystallinity of Li_1+XGa_XTi_2-X(PO₄)₃ increased with the sintering temperature as evidenced by FE-SEM observations, which demonstrated that the edges of the larger cube-shaped grains become sharper with increases in the sintering temperature. In samples with high sintering temperatures at 1,000 ℃ and high Ga content above 0.3, coarsening of grains occurred. This resulted in the formation of many grain boundaries, leading to low sinterability. These two factors, the impurity and grain boundary, have an enormous impact on the properties of Li_1+XGa_XTi_2-X(PO₄)₃. The Li_1.3Ga_0.3Ti_1.7(PO₄)₃ pellet sintered at 900 ℃ was denser than those sintered at other conditions, showing the highest total ion conductivity of 7.66 × 10^-5 S/cm at room temperature. The total activation energy of Li-ion transport for the Li_1.3Ga_0.3Ti_1.7(PO₄)₃ solid-state electrolyte was estimated to be as low as 0.36 eV. Although the Li_1+XGa_XTi_2-X(PO₄)₃ sintered at 1,000 ℃ had a relatively high apparent density, it had less total ionic conductivity due to an increase in the grain-boundary resistance with coarse grains.

• 청정기술
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• 제24권4호
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• pp.371-379
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• 2018

본 연구의 목적은 친환경 액체 추진제 분해반응에 적용하기 위하여 백금이 담지된 헥사알루미네이트 펠렛 촉매를 개발하는 것이다. 초음파 분무 열분해법으로 제조한 hexaaluminate를 지지체로 사용하고 백금을 활성금속으로 사용한 펠렛 촉매를 두가지 방법으로 제조하였다. 백금 전구체를 헥사알루미네이트 분말에 담지한 후에 바인더를 첨가하여 성형한 펠렛 촉매의 경우(M1 method 촉매), $550^{\circ}C$에서 소성한 촉매는 메조기공이 잘 발달하였다. 그러나 이 촉매를 $1,200^{\circ}C$에서 소성하면 메조기공이 거의 무너지고 약간의 거대기공만 존재하였다. 반면에, 헥사알루미네이트를 성형하여 펠렛을 제조한 후, 펠렛 위에 백금을 담지한 촉매의 경우(M2 method 촉매), $1,200^{\circ}C$에서 소성한 후에도 표면적과 메조기공이 잘 유지되는 것으로 나타났다. 또한, 백금 분산도 측면에서도 M2 method로 제조한 촉매의 내열성이 더 우수하였다. 펠렛 촉매 제조 방법과 소성온도가 ammonium dinitramide (ADN) 또는 hydroxyl ammonium nitrate (HAN)을 주성분으로 하는 액상 추진제의 분해반응에 미치는 영향을 분석하였다. ADN 기반 액체 추진제 및 HAN 기반 액체추진제의 분해반응에서 Pt/hexaaluminate 펠렛 촉매를 사용하면 분해 개시 온도를 큰 폭으로 내릴 수 있음을 확인하였다. 특히, M2 method로 제조한 촉매의 경우, 소성온도를 $1,200^{\circ}C$로 올린 경우에도 분해 개시 온도가 큰 변화를 보이지 않았다. 따라서 M2 method로 제조한 Pt/hexaaluminate 펠렛 촉매가 내열성을 보유하고 있으며, 친환경 액상 추진제의 분해 반응용 촉매로서 잠재력이 있다는 것을 확인하였다.