• Title/Summary/Keyword: Sol-Gel process

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Failure Analysis of Ferroelectric $(Bi,La)_4Ti_3O_{12}$ Capacitor in Fabricating High Density FeRAM Device (고밀도 강유전체 메모리 소자 제작 시 발생하는 $(Bi,La)_4Ti_3O_{12}$ 커패시터의 불량 분석)

  • Kim, Young-Min;Jang, Gun-Eik;Kim, Nam-Kyeong;Yeom, Seung-Jin;Hong, Suk-Kyoung;Kweon, Soon-Yong
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2007.06a
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    • pp.257-257
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    • 2007
  • 고밀도 FeRAM (Ferroe!ectric Random Access Memory) 소자를 개발하기 위해서는 강유전체 물질을 이용한 안정적인 스텍형의 커패시터 개발이 필수적이다. 특히 $(Bi,La)_4Ti_3O_{12}$ (BLT) 강유전체 물질을 이용하는 경우에는 낮은 열처리 온도에서도 균질하고 높은 값의 잔류 분극 값을 확보하는 것이 가장 중요한 과제 중의 하나이다. 불행히도, BLT 물질은 a-축으로는 약 $50\;{\mu}C/cm^2$ 정도의 높은 잔류 분극 값을 갖지만, c-축 방향으로는 $4\;{\mu}C/cm^2$ 정도의 낮은 잔류 분극 값을 나타내는 동의 강한 비등방성 특성을 보인다. 따라서 BLT 박막에서 각각 입자들의 크기 및 결정 방향성을 세밀하게 제어하는 것은 무엇보다 중요하다. 본 연구에서는 16 Mb의 1T/1C (1-transistor/1-capacitor) 형의 FeRAM 소자를 BLT 박막을 적용하여 제작하였다. 솔-젤 (sol-gel) 용액을 이용하여 스핀코팅법으로 BLT 박막을 증착하고, 후속 열처리 공정을 RTP (rapid thermal process) 공정을 이용하여 수행하였다. 커패시터의 하부 전극 및 상부 전극은 각각 Pt/IrOx/lr 및 Pt을 적용하였다. 반응성 이온 에칭 (RIE: reactive ion etching) 공정을 이용하여 커패시터를 형성시킨 후, 32k-array (unit capacitor: $0.68\;{\mu}m$) 패턴에서 측정한 스위칭 분극 (dP=P*-P^) 값은 약 $16\;{\mu}C/cm^2$ 정도이고, 웨이퍼 내에서의 균일도도 2.8% 정도로 매우 우수한 특성을 보였다. 그러나 단위 셀들의 특성을 평가하기 위하여 bit-line의 전압을 측정한 결과, 약 10% 정도의 커패시터에서 불량이 발생하였다. 그리고 이러한 불량 젤들은 매우 불규칙적으로 분포함을 확인할 수 있었다. 이러한 불량 원인을 파악하기 위하여 양호한 젤과 불량이 발생한 셀에서의 BLT 박막의 미세구조를 분석하였다. 양호한 셀의 BLT 박막 입자들은 불량한 셀에 비하여 작고 비교적 균일한 크기를 갖고 있었다. 이에 비하여 불량한 셀에서의 BLT 박막에는 과대 성장한 입자들이 존재하고 이에 따라서 입자 크기가 매우 불균질한 것으로 확인되었다. 또 이러한 과대 성장한 입자들은 거의 모두 c-축 배향성을 나타내었다. 이상의 실험 결과들로부터, BLT 박막을 이용하여 제작한 FeRAM 소자에서 발생하는 불규칙한 셀 불량의 주된 원인은 c-축 배향성을 갖는 과대 성장한 입자의 생성임을 알 수 있었다. 즉 BLT 박막을 이용하여 FeRAM 소자를 제작하는 경우, 균일한 크기의 입자 및 c-축 배향성의 입자 억제가 매우 중요한 기술적 요소임을 알 수 있었다.

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Colossal Magnetoresistance and Mossbauer Studies of La-Ca-Mn-O Compound Doped with $^{57}Fe$ ($^{57}Fe$를 미량 치환한 La-Ca-Mn-O의 초거대자기저항과 Mossbauer분광학연구)

  • 박승일;김성철
    • Journal of the Korean Magnetics Society
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    • v.8 no.6
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    • pp.335-340
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    • 1998
  • Colossal magnetoresistance $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ material has been produced by a metal-salt routed sol-gel process method. Magnetic properties of $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ have been studied with x-ray diffraction, Rutherford back-scattering spectroscopy(RBS), vibrating sample magnetometer, and Mossbauer spectroscopy. Crystalline $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ was perovskite cubic structure with a lattice parameter $a_0=3.868$\AA$$. And there was no appreciable change in the value of the lattice parameter when a small amount (x=0.01) of iron was added. However, Mossbauer and VSM data indicate the Curie temperature of the $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ decreased from 282 to 270 k and also the saturation magnetization from 84 to 81 emu/g at 77 K. Mossbauer spectra of $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ have been taken at various temperatures ranging form 4.2 K to room temperature. Analysis of $^{57}Fe$ Mossbauer data in terms of the local configurations of Mn atoms has permitted the influence of the magnetic hyperfine interactions to be monitored. The isomer shifts show that the charge state of all Fe ions are ferric. The magnetoresistance of $La_{0.67}Ca_{0.33}Mn_{0.99}^{57}Fe_{0.01}O_3$ was about 33 % at semiconductor-metal transition temperature $T_{SC-M}=250K$.

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Synthesis and Electrochemical Properties of Porous Li4Ti5O12 Anode Materials (기공구조로 제조된 Li4Ti5O12 음극활물질의 전기화학적 특성)

  • Seo, Jin-Seong;Na, Byung-Ki
    • Korean Chemical Engineering Research
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    • v.57 no.6
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    • pp.861-867
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    • 2019
  • $Li_4Ti_5O_{12}$ is a promising next-generation anode material for lithium-ion batteries due to excellent cycle life, low irreversible capacity, and little volume expansion during charge-discharge process. However, it has poor charge capacity at high current density due to its low electrical conductivity. To improve this weakness, porous $Li_4Ti_5O_{12}$ was synthesized by sol-gel method with P123 as chelating agent. The physical characteristics of as-prepared sample was investigated by XRD, SEM, and BET analysis, and electrochemical properties were characterized by cycle performance test, cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS). $Li_4Ti_5O_{12}$ synthesized by 0.01mol ratio of P123/Ti showed most unified particle size, high specific surface area, and relatively high porosity. EIS analysis showed that depressed semicircle size was remarkably reduced, which suggested resistance value in electrode was decreased. Capacity in rate performance showed 178 mAh/g at 0.2C, 170 mAh/g at 0.5C, 110 mA/h at 5C, and 90 mAh/g at 10C. Capacity retention also showed 99% after rate performance.

Size Effect of Hollow Silica Nanoparticles as Paint Additives for Thermal Insulation (단열 페인트 첨가제로써 중공형 실리카 나노입자의 크기에 따른 효과)

  • Kim, Jisue;Kim, Younghun
    • Clean Technology
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    • v.28 no.1
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    • pp.18-23
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    • 2022
  • Using air as an insulator due to its low heat transfer coefficient has been studied and has been widely commercialized to save energy in the field of thermal insulation technology. In this study, we analyzed the heat insulating effect of hollow silica nanoparticles mixed in non-uniform size, and the maximum heat insulating efficiency of these particles given the limited number of particles that can be mixed with a medium such as paint. The hollow silica nanoparticles were synthesized via a sol-gel process using a polystyrene template in order to produce an air layer inside of the particles. After synthesis, the particles were analyzed for their insulation effect according to the size of the air layer by adding 5 wt % of the particles to paint and investigating the thermal insulation performance by a heat transfer experiment. When mixing the particles with white paint, the insulation efficiency was 15% or higher. Furthermore, the large particles, which had a large internal air layer, showed a 5% higher insulation performance than the small particles. By observing the difference in the insulation effect according to the internal air layer size of hollow silica nanoparticles, this research suggests that when using hollow particles as a paint additive, the particle size needs to be considered in order to maximize the air layer in the paint.

Core-shell TiO2/Ag Nanoparticle Synthesis and Characterization for Conductive Paste (전도성 페이스트용 코어-쉘 TiO2/Ag 나노입자의 합성 및 특성 연구)

  • Sang-Bo, Sim;Jong-Dae, Han
    • Applied Chemistry for Engineering
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    • v.34 no.1
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    • pp.36-44
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    • 2023
  • Core-shell TiO2/Ag nanoparticles were synthesized by a modified sol-gel process and the reverse micelle method using acetoxime as a reducing agent in water/dodecylbenzenesulfonic acid (DDBA)/cyclohexane. The structure, shape, and size of the TiO2/Ag nanoparticles were investigated using X-ray diffraction (XRD), UV-visible spectroscopy, scanning electron microscope (SEM), transmission electron microscope (TEM), and thermogravimetric analysis (TGA). The size of TiO2/Ag nanoparticles could be controlled by changing the [water]/[DDBA] molar ratio values. The size and the polydispersity of TiO2/Ag nanoparticles increased when the [water]/[DDBA] molar ratio rose. The resultant Ag nanoparticles over the anatase crystal TiO2 nanoparticles exhibited a strong surface plasmon resonance (SPR) peak at about 430 nm. The SPR peak shifted to the red side with the increase in nanoparticle size. Conductive pastes with 70 wt% TiO2/Ag nanoparticles were prepared, and the pastes were coated on the PET films using a screen-printing method. The printed paste films of the TiO2/Ag nanoparticles demonstrated greater surface resistance than conventional Ag paste in the range of 405~630 μΩ/sq.

Synthesis of Polyimide Crosslinked Silica-based Aerogel with Enhanced Mechanical Properties and Its Physico-chemical Properties (폴리이미드 가교로 기계적 강도가 향상된 실리카 기반 에어로겔의 합성 및 물리화학적 특성 분석)

  • Kim, Jiseung;Choi, Haryeong;Kim, Taehee;Lee, Wonjun;Lee, Hong-Sub
    • Journal of the Microelectronics and Packaging Society
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    • v.29 no.4
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    • pp.9-14
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    • 2022
  • Silica aerogel is a porous material with a very low density and high specific surface area. Still, its application is limited due to its weak mechanical properties due to structural features. To solve this problem, a method of complexing it with various polymers has been proposed. We synthesized polyimide cross-linked silica aerogel by the sol-gel process to obtain high mechanical properties. Tetraethyl orthosilicate (TEOS) was used as a precursor to make silica aerogel, and 3- aminopropyltriethoxysilane (APTES) was used as a coupling agent for cross-linking polyimide. Polyimide was synthesized using pyromellitic dianhydride and 3,5-diaminobenzoic acid, and mechanical properties were improved by crosslinking polyimide with 10 repeating units in the polyimide chain using the reaction formula ${\frac{n_1}{n_2}}={\frac{n}{n+1}}$ To realize silica aerogel, polyimide having various weight ratios was added before gelation, resulting in a 19-fold or greater increase in maximum compressive strength compared to pure silica aerogel. From this study, an enhancement of silica aerogel could be enhanced through polymer cross-linking bonds.

Stabilization/Solidification of Radioactive LiCl-KCl Waste Salt by Using SiO2-Al2O3-P2O5 (SAP) Inorganic Composite: Part 2. The Effect of SAP Composition on Stabilization/Solidification (SiO2-Al2O3-P2O5 (SAP) 무기복합체를 이용한 LiCl-KCl 방사성 폐기물의 안정화/고형화: Part 2. SAP조성에 따른 안정화/고형화특성 변화)

  • Ahn, Soo-Na;Park, Hwan-Seo;Cho, In-Hak;Kim, In-Tae;Cho, Yong-Zun
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.10 no.1
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    • pp.27-36
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    • 2012
  • Metal chloride waste is generated as a main waste streams in a series of electrolytic processes of a pyrochemical process. Different from carbonate or nitrate salt, metal chloride is not decomposed into oxide and chlorine but it is just vaporized. Also, it has low compatibility with conventional silicate glasses. Our research group adapted the dechlorination approach for the immobilization of waste salt. In this study, the composition of SAP ($SiO_2-Al_2O_3-P_2O_5$) was adjusted to enhance the reactivity and to simplify the solidification process as a subsequent research. The addition of $Fe_2O_3$ into the basic SAP decreased the SAP/Salt ratio in weight from 3 for SAP 1071 to 2.25 for M-SAP( Fe=0.1). The experimental results indicated that the addition of $Fe_2O_3$ increased the reactivity of M-SAP with LiCl-KCl but the reactivity gradually decreased above Fe=0.1. Also, introducing $B_2O_3$ into M-SAP requires no glass binder for the consolidation of reaction products. U-SAP ($SiO_2-Al_2O_3-Fe_2O_3-P_2O_5-B_2O_3$) could effectively dechlorinate the LiCl-KCl waste and its reaction product could be consolidated as a monolithic form without a glass binder. The leaching test result indicated that U-SAP 1071 was more durable than other SAPs wasteform. By using U-SAP, 1 g of waste salt could generated 3~4 g of wasteform for final disposal. The final volume would be about 3~4 times lower than the glass-bonded sodalite. From these results, it could be concluded that the dechlorination approach using U-SAP would be one of prospective methods to manage the volatile waste salt.

Heat Shield Property of Nanostructural-regulated Fe2O3/TiO2 Composites Filled with Polyacrylate Paint (나노구조 변화에 의한 Fe2O3/TiO2 복합재료를 충전한 Poly Acrylate 도료의 열차단 특성)

  • Kim, Dae Won;Ma, Young Kil;Kim, Jong Seok
    • Applied Chemistry for Engineering
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    • v.31 no.1
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    • pp.43-48
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    • 2020
  • Fe2O3 nanoparticles with the mixed structure of cubic and nanorod were synthesized by precipitation, hydrothermal, sol-gel method, etching process and heat treatment. Fe2O3/TiO2 core-shell (CS) of type Fe2O3@TiO2 composite was fabricated on a 20 nm nanolayer of TiO2 coated on the surface of Fe2O3 nanoparticles. Fe2O3/TiO2 yolk-shell (YS) composite was prepared by chemical etching and heat treatment of Fe2O3/TiO2 CS nanoparticles. Physical properties of Fe2O3, Fe2O3@TiO2 CS and Fe2O3@TiO2 YS nanoparticles were characterized by FE-SEM, HR-TEM and X-ray diffraction. The solar reflectance, commission internationale de l'Elcairage (CIE) color coordinate and heat shield temperatures of Fe2O3, CS and YS type Fe2O3@TiO2 pigments filled with poly acrylate (PA) paints were investigated by UV-Vis-NIR spectrometer and homemade heat shield temperature measuring device. The Fe2O3@TiO2 YS red pigment filled PA composite exhibited excellent near infrared light reflecting performance and also reduced the heat shield temperature of 13 ℃ than that of Fe2O3 filled counterparts.