• 한국세라믹학회지
• /
• 제27권8호
• /
• pp.991-1003
• /
• 1990

A precipitation method, one of the most effective liquid phase reaction methods, was adopted in order to prepare high-tech Al2O3/ZrO2 composite ceramics. Al2(SO4)3.18H2O, ZrOCl2.8H2O and YCl3.6H2O were used as starting materials and NH4OH as a precipitation agent, various types of metal hydroxides were obtained by single precipitation(series A) and co-precipitation(series B) method at the pH condition between 7 and 11. Fine Al2O3-ZrO2 powders were prepared at optimum calcination condition and the effects of ZrO2 on microstructures and mechanical properties of Al2O3 were investigated. The composition of Al2O3/ZrO2 composites wax fixed as Al2O3-15 v/o ZrO2(＋3m/o Y2O3). ZrO2 limited the grain growth of Al2O3 and increased grain size homogeneity of Al2O3 more effectively than MgO.Flexural strength values in Al2O3 and Al2O3/ZrO2 composites were 340-430 MPa and 540-820 MPa, respectively, and the effect of strength improvement showed 20-50% by adding ZrO2 to Al2O3. Fracture toughness of Al2O3/ZrO2 composites was improved by stress-induced phase transformation of tetragonal ZrO2 and toughening effect by microcrack was not observed. Also, ZrO2 particles located at Al2O3 grain junction contributed to toughening, while spherical ZrO2 particles located within Al2O3 grain did not contribute to toughening. Weibull moduli of Al2O3 ceramics and Al2O3/ZrO2 composites of series A and series B were 4.34, 5.17 and 9.06, respectively. Above 0.5 of failure probability, strength values in Al2O3 ceramics and Al2O3/ZrO3 composites of series A and series B were above 400 MPa, 700 MPa and 650 MPa, respectively.

• 대한화학회지
• /
• 제33권1호
• /
• pp.65-69
• /
• 1989

방사성 바륨 또는 방사성 란탄 추적자를 함유하고 있는 Ba(NO$_3)_2$ 와 TiO(NO$-3)_2$의 무기혼합용액을 옥살산의 에탄올 용액으로 적정하므로써 바륨티탄닐의 옥살산 염을 합성하였고, 이를 1000$^{\circ}$C에서 하소시켜 BaTiO$_3$를 만들었다. 옥살산염의 분석결과는 BaTiO(C$_2O_4)_2{\cdot}4H_2O$이며, 무기혼합용액중 Ba/Ti의 몰비가 0.950∼1.05 범위 내에서 화학양론적 결합으로 합성됨을 방사성 바륨 추적자의 도움으로 쉽게 확인하였고, Perovskite형의 구조임을 XRD로 확인하였다. 그리고 란탄 첨가제가 침전에 화학적으로 균일하게 혼입됨은 방사성 란탄의 추적자 실험으로 발견하였다. 이와 같은 실험적 사실로부터 침전물의 구성 성분의 결합이 분자준위에서 일어나고 또 티탄산바륨이 단일상의 결정임을 설명하였다.

• 한국재료학회지
• /
• 제24권1호
• /
• pp.48-52
• /
• 2014

The Mg-enriched magnesium aluminum silicate (MAS) glass is known for its higher mechanical strength and chemical resistance. Among such glasses, cordierite ($Mg_2Al_4Si_5O_{18}$) is well known to have a low thermal expansion and low melting point. Polycrystalline engineering ceramics such as alumina can be strengthened by a surface modification with low thermal expansion materials. The present study involves the synthesis of cordierite by a sol-gel process and investigates the effect of glass penetration on the surface of alumina. The cordierite powders were prepared from $Al(OC_3H_7)_3$, $Mg(OC_2H_5)_2$ and tetraethyl orthosilicate by hydrolysis and condensation reaction. The cordierite powders were characterized by X-ray diffraction (XRD, Rigaku), scanning electron microscope (SEM, JEOL: JSM-5610), energy dispersive spectroscopy (EDS, JEOL: JSM-5610), and universal testing machine (UTM, INSTRON). The X-ray diffraction patterns showed that the synthesized particles were ${\mu}$-cordierite calcined at $1100^{\circ}C$ for 1 h. The shape of synthesized cordierite was changed from ${\mu}$-cordierite to ${\alpha}$-cordierite with increasing calcination temperature. Synthesized cordierite was used for surface modification of alumina. Cordierite powders penetrated deeply into the alumina sample along grain boundaries with increasing temperature. The results of surface modification tests showed that the strength of the prepared alumina sample increased after surface modification. The strength of a surface modified with synthesized cordierite increased the most, to about 134.6MPa.

• 한국재료학회지
• /
• 제24권7호
• /
• pp.351-356
• /
• 2014

A spherical $Sr_4Al_{14}O_{25}:Eu^{2+}$ phosphor for use in white-light-emitting diodes was synthesized using a liquid-state reaction with two precipitation stages. For the formation of phosphor from a precursor, the calcination temperature was $1,100^{\circ}C$. The particle morphology of the phosphor was changed by controlling the processing conditions. The synthesized phosphor particles were spherical with a narrow size-distribution and had mono-dispersity. Upon excitation at 395 nm, the phosphor exhibited an emission band centered at 497 nm, corresponding to the $4f^65d{\rightarrow}4f^7$ electronic transitions of $Eu^{2+}$. The critical quenching-concentration of $Eu^{2+}$ in the synthesized $Sr_4Al_{14}O_{25}:Eu^{2+}$ phosphor was 5 mol%. A phosphor-converted LED was fabricated by the combination of the optimized spherical phosphor and a near-UV 390 nm LED chip. When this pc-LED was operated under various forward-bias currents at room temperature, the pc-LED exhibited a bright blue-green emission band, and high color-stability against changes in input power. Accordingly, the prepared spherical phosphor appears to be an excellent candidate for white LED applications.

• 한국세라믹학회지
• /
• 제53권5호
• /
• pp.529-534
• /
• 2016

Nanocrystalline powder of zirconia stabilized with 8 mol% yttria (YSZ) has been synthesized through oxalate process using $ZrOCl_2{\cdot}8H_2O$ and $Y(NO_3)_3{\cdot}6H_2O$ as starting materials. Understanding of the characteristic changes of YSZ powder as a function of processing conditions is crucial in developing dense and porous microstructures required for fuel cell applications. In this research, microstructure change, surface area, particle shape and particle size were measured as a function of different processing conditions such as calcination temperature, stirring speed and concentration of starting materials. The resultant crystallite sizes were calculated by XRD-LB (X-Ray Diffraction Line-Broadening) method, BET method, and morphology of the crystal was observed in TEM and FE-SEM. The TEM examination showed that the powder synthesized with 0.7 M of YSZ concentration had a spherical morphology with sizes ranging from 20 to 40 nm. However, the powder was gradually aggregated above 1.0 M of YSZ concentration with the aggregation being intensified as the YSZ concentration was increased.

• 자원리싸이클링
• /
• 제9권4호
• /
• pp.37-43
• /
• 2000

폐리륨이온전지의 재활용 일환으로 폐전지에서 분리한 양극활물질인 $LiCoO_2$로부터 Li과 Co룹 회수하기 위하여 침출거동올 조사하였다. 전 연구에서 얻은 최적조건에서 $LiCoO_2$를 1M 황산과 질산으료 침출하였을 때 Li과 Co의 침출율이 각각 70-80%, 40%로 Co의 침출율이 낮았다. 환원제를 첨가한 경우 Li과 Co의 침출율이 증가하였는데, 특히 $Na_2S_2O_3$ 및 $H_2O_2$ 와 같은 환원제에서 질산침출을 하는 경우 Li괴- Co의 용해가 거의 95% 이상 이루어졌다. 이는 환원제가 $Co^{3+}$를 $Co^{2+}$로 환원시켜 침출이 용이해졌기 때문으로 생각된다. 변수설험을 통하여 얻은 최적의 조건(광액농도 10g/l 반응온도 $75^{\circ}C$, 교반속도 400 rpm' 1.7 vol% $H_2O_2$)에서 폐리튬이온전지로부터 선별하고 열처리한 $LiCoO_2$ 분말을 침출 실험한 결과, Li과 Co의 침출율이 각각 99% 이상이었으며, 이는 충방전이 거듭되면서 양극활물질인 $LiCoO_2$이 화학적으로 활성화되었거나 Li의 탈착으로 겸정구조가 불안하기 때문으로 생각된다.

• 한국진공학회:학술대회논문집
• /
• 한국진공학회 2013년도 제45회 하계 정기학술대회 초록집
• /
• pp.317.2-317.2
• /
• 2013

Ultrathin oxide encapsulated metal-oxide hybrid nanocatalysts have been fabricated by a soft chemical and facile route. First, SiO2 nanoparticles of 25~30 nm size have been synthesized by modified Stobber's method followed by amine functionalization. Metal nanoparticles (Ru, Rh, Pt) capped with polymer/citrate have been deposited on functionalized SiO2 and finally an ultrathin layer of TiO2 coated on surface which prevents sintering and provides high thermal stability while maximizing the metal-oxide interface for higher catalytic activity. TEM studies confirmed that 2.5 nm sized metal nanoparticles are well dispersed and distributed throughout the surface of 25 nm SiO2 nanoparticles with a 3-4 nm TiO2 ultrathin layer. The metal nanoparticles are still well exposed to outer surface, being enabled for surface characterization and catalytic activity. Even after calcination at $600^{\circ}C$, the structure and morphology of hybrid nanocatalysts remain intact confirm the high thermal stability. XPS spectra of hybrid nanocatalyst suggest the metallic states as well as their corresponding oxide states. The catalytic activity has been evaluated for high temperature CO oxidation reaction as well as photocatalytic H2 generation under solar simulation. The design of hybrid structure, high thermal stability, and better exposure of metal active sites are the key parameters for the high catalytic activity. The maximization of metal-TiO2 interface interaction has the great role in photocatalytic H2 production.

• 공업화학
• /
• 제22권2호
• /
• pp.185-189
• /
• 2011

본 연구에서는 화학적 공침법을 적용하여 가스상 이산화탄소 분해를 위한 나노크기의 M-페라이트(M=Co, Ni, Cu, Zn)를 제조하였다. 열중량 분석 결과, 시험제조한 모든 시료의 최고 무게 감소율은 $350^{\circ}C$ 미만에서 발생하였다. 소성온도가 증가할수록 결정형은 우수하여 표면촉매활성화를 기대할 수 있지만, 입자결정의 크기가 크고, 비표면적이 낮은 페라이트가 합성됨을 알 수 있었다. FT-IR 분석으로부터 $375{\sim}406cm^{-1}$의 범위에서 octahedral site에 착화물이 존재함을 확인 할 수 있었으며, 이는 페라이트 내 스피넬 구조가 형성되어 있음을 보여주는 것이라고 믿는다. 본 연구로부터 얻은 이산화탄소 분해반응을 위한 금속페라이트의 최적 열처리 온도는 $500^{\circ}C$인 것으로 나타났다.

• 한국전기전자재료학회논문지
• /
• 제36권5호
• /
• pp.505-512
• /
• 2023

This study investigated crystal structures, microstructures, and electric-field-induced strain (EFIS) properties of Bi-based lead-free ferroelectric/relaxor composites. Bi_1/2Na_0.82K_0.18)_1/2TiO₃ (BNKT) as a ferroelectric material and 0.78Bi_1/2(Na_0.78K_0.22)_1/2TiO₃-0.02LaFeO₃ (BNKT2LF) as a relaxor material were synthesized using a conventional solid-state reaction method, and the resulting BNKT2LF powders were subjected to high-energy ball milling (HEBM) after calcination. As a result, HEBM proved a larger average grain size of sintered samples compared to conventional ball milling (CBM). In addition, the increased sintering time led to grain growth. Furthermore, HEBM treatment and sintering time demonstrated a significant effect on EFIS of BNKT/BNKT2LF composites. At 6 kV/mm, 0.35% of the maximum strain (S_max) was observed in the HEBM sample sintered for 12 h. The unipolar strain curves of CBM samples were almost linear, indicating almost no phase transitions, while HEBM samples displayed phase transitions at 5~6 kV/mm for all sintering time levels, showing the highest S_max/E_max value of 700 pm/V. These results indicated that HEBM treatment with a long sintering time might significantly enhance the electromechanical strain properties of BNT-based ceramics.

• Journal of Electrochemical Science and Technology
• /
• 제14권1호
• /
• pp.75-84
• /
• 2023

The accumulation of spent carbide (YG8), not only pollutes the environment but also causes waste of tungsten, cobalt and other rare metal resources. To better address this issue, we proposed a combined electrochemical separation process of low-temperature aqueous solution and high-temperature molten salt for tungsten and cobalt. H₂WO₄ was obtained from spent carbide in an aqueous solution, and we calcined it to obtain WO₃, which was used as a raw material to obtain tungsten by using molten salt electrodeposition. The influence of the current efficiency and the electrochemical behavior of the discharge precipitation of W(VI) were also studied. The calcination results showed that the morphology of WO₃ was regular and there were no other impurities. The maximum current efficiency of 82.91% was achieved in a series of electrodeposition experiments. According to XRD and SEM analysis, the recovered product was high purity tungsten, which belongs to the simple cubic crystal system. In the W(VI) reduction mechanism experiments, the electrochemical process of W(VI) in NaCl-Na₂WO₄-WO₃ molten salt was investigated using linear scanning voltammetry (LSV) and chronoamperometry in a three-electrode system. The LSV showed that W(VI) was reduced at the cathode in two steps and the electrode reaction was controlled by diffusion. The fitting results of chronoamperometry showed that the nucleation mechanism of W(VI) was an instantaneous nucleation mode, and the diffusion coefficient was 7.379×10^-10 cm²·s^-1.