• Title/Summary/Keyword: high pressure synthesis

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One-step Fabrication of a Tannic Acid-Transition Metal-Polymer Gel as a Pressure-Sensitive Adhesive (타닌산-전이 금속-고분자로 구성된 젤의 단일 단계 합성과 점착제로의 이용)

  • Lee, Jaehong;Lee, Kyoungmun;Choi, Siyoung Q.
    • Korean Chemical Engineering Research
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    • v.58 no.2
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    • pp.176-183
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    • 2020
  • In this study, synthesis of a hydrogel consisted of a coordination bond network between small organic molecules and transition metals had been carried out. By adding a tackifying material to the gel, the potential of the gel to be used as an adhesive material had been also confirmed. Synthesis of the adhesive had been done with simple mixing of 3 components: tannic acid, transition metal, and polymer. The tannic acid molecule possesses multiple hydroxyl groups that can form coordination bonds with the transition metals and hydrogen bonds with the hydrophilic polymers. Due to the morphology of the metal-organic complex and polymer dispersed in water, the fabricated material exhibited high adhesiveness and cohesiveness. Optimizing the rheological property had been conducted for use in adhesive by the synthesis with varying the transition metal (Fe3+, Ti4+), polymer, and treatment conditions. Rheological measurement results demonstrate the promising potential of the material as a bio-compatible and versatile pressure-sensitive adhesive with both high adhesiveness and cohesiveness.

High Pressure Synthesis and Physical Properties of the Solid Solution, $SrLaAl_{1-x}Ni_xO_4(0

  • 변송호
    • Bulletin of the Korean Chemical Society
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    • v.16 no.11
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    • pp.1084-1088
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    • 1995
  • A complete solid solution (SrLaAl1-xNixO4) between insulating SrLaAlO4 and metallic SrLaNi(Ⅲ)O4 oxides were prepared under high oxygen pressure (1.5 kbar, 800 ℃). They have tetragonal K2NiF4-type structure in all the solid solution range. Compared with lattice parameters of the same solid solution prepared under normal condition (1 bar, 1200 ℃), large decrease in the c-parameter was induced by high pressure treatment while no noticeable variation of the a-parameter was observed. Although marked changes of structural parameters, magnetic susceptibilities, and electron paramagnetic resonance spectra were consistently occurred before and after x=0.5, overall behaviors were essentially the same with those of solid solution prepared under normal condition. Such a phenomenon is explained by assuming the formation of partially filled narrow σ*x2-y2 band for x>0.5. Lattice contraction along the c-axis by high pressure treatment seems not to broaden this band. Particularly, the continuous absorption characteristic of a high free carrier concentration for x>0.5 and the absence of Ni-O in-plane stretching mode in the infrared absorption spectra supports this picture. However, the conductivities increasing with temperature for all solid solution suggest that some localization character, of probably Anderson type, remains for x>0.5.

Synthesis and Characterization of High Surface Area of Zirconia: Effect of pH (고비표면적 지르코니움 산화물의 제조 및 특성 분석: pH 영향)

  • Jeong, Ye-Seul;Shin, Chae-Ho
    • Korean Chemical Engineering Research
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    • v.57 no.1
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    • pp.133-141
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    • 2019
  • High specific surface area zirconia with acid-basic property was synthesized by precipitation using reflux method or hydrothermal synthesis method using ammonium hydroxide solution as precipitant in the range of pH of Zr solution from 2 to 10. The prepared zirconia was characterized by the nitrogen adsorption, X-ray diffraction (XRD), isopropanol temperature programmed desorption (IPA-TPD), scanning electron microscopy and X-ray photoelectron spectroscopy, and the catalytic activity in the IPA decomposition reaction was correlated with the acid-basic properties. When using reflux method, high pH of Zr solution was required to obtain high fraction of tetragonal zirconia, and pure tetragonal zirconia was possible at pH 9 or higher. High pH was required to obtain high specific surface area zirconia, and the hydrous zirconia synthesized at pH 10 had high specific surface area zirconia of $260m^2g^{-1}$ even after calcination at $600^{\circ}C$. However, hydrothermal synthesis with high pressure under the same conditions resulted in very low specific surface area below $40m^2g^{-1}$ and monoclinic phase zirconia was synthesized. High pH of the solution was required to obtain high specific surface area tetragonal phase zirconia. In hydrothermal synthesis requiring high pressure, monoclinic zirconia was produced irrespective of the pH of the solution, and the specific surface area was relatively low. Zirconia with high specific surface area and tetragonal phase was predominantly acidic compared to basicity and only propylene, which was observed as selective dehydration reaction in IPA decomposition reaction, was produced.

Thermodynamic Equilibrium Compositions for a $NH_3-AlCl_3-H_2$ Vapor-Phase Reacting System and Synthesis of High-Purity AlN ($NH_3-AlCl_3-H_2$ 기상반응계의 열역학적 평형조성 및 고순도 AIN 합성)

  • 현상훈;김준학
    • Journal of the Korean Ceramic Society
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    • v.23 no.1
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    • pp.33-43
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    • 1986
  • The synthesis of high-purity AlN by a vapor-phase reaction was investigated using the $NH_3-AlCl_3-H_2$ reacting system. The theoretical yields of AlN were determined from th thermodynamic equilibrium composi-tions. It was shown that the yields above 90% could by obtained even in the range of relatively low temper-ature of 600-1200K. The reaction temperature and the initial amounts/ratios of the reacting gases showed significant effects on the yields but the total pressure did not. The experimental results showed that a high-purity AlN having a needle shape was the only product as a solid phase and its amount produced increased with the reaction temperature. While the degree of agglmera-tion of the synthesized AlN increased with the reaction temperature the size of each particle consisting of the agglomerates was independent of the temperature but grew from 0.09 to 0.115${\mu}{\textrm}{m}$ with the flow rate of NH3. These experimental results were compared with the theoretical aspects for the synthesis of a high-purity AlN.

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Optimization of synthesis conditions and $CO_2$ capture capability of Cu-BTC Metal-Organic Framework (이산화탄소 흡착용 Cu-BTC MOF 합성 최적화)

  • Peng, Mei Mei;Hemalatha, Pushparaj;Ganesh, Mani;Jang, Hyun-Tae
    • Proceedings of the KAIS Fall Conference
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    • 2011.12a
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    • pp.200-203
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    • 2011
  • A copper-based metal organic framework (MOF) named Cu-BTC, also known as HKUST-1, was synthesized by using a solvothermal method at various synthesis temperature, time and pressure. The obtained samples were characterized with Powder X-ray diffraction (XRD) for phase structure, scanning electron microscopy (SEM) for crystal structure, and nitrogen adsorption-desorption for pore textural structure. The Cu-BTC sample was also studied for $CO_2$ adsorption. The analysis results displayed that the sample synthesized at the condition of temperature: $120^{\circ}C$, synthesis time: 12 hours, pressure: 1 bar exhibited a good crystal structure with uniform size of octahedral particles. The BET data revealed a high surface area of 1741.7 $m^2g^{-1}$ and a pore volume of 0.7137 $cm^3g^{-1}$and exhibiteda maximum $CO_2$ adsorption capacity of 170 mg/g of the sorbent at $25^{\circ}C$.

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A Study on the Synthesis of Titanium Hydride by SHS(Self-propagating High-temperature Synthesis) Method and the Preparation of Titanium Powder (SHS법에 의한 티타늄 수소화물 합성 및 티타늄 분말 제조에 관한 연구)

  • Ha, Ho;Park, Seung-Soo;Lee, Hee-Cheol
    • Applied Chemistry for Engineering
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    • v.5 no.2
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    • pp.263-273
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    • 1994
  • Titanium powder prepared by dehydrogenating the titanium hydride which is synthesized by reacting Ti-sponge (99.67%) with hydrogen using the self-propagating high-temperature synthesis method. In the synthesis of titanium hydride, the particle size of the product was found dependent on the amount of hydrogen incorporated into the titanium such that the particle size of titanium hydride decreased with increasing hydrogen pressure and after-burn time. In the dehydrogenation process, as the dehydrogenation time increase, the particle size of titanium powder increased due to partial melting and sintering of titanium particles.

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Synthesis of Nano-Sized Cu Powder by PVA Solution Method and Thermal Characteristics of Sintered Cu Powder Compacts (PVA 용액법을 통한 나노 Cu 분말합성 및 소결체의 열적 특성)

  • Oh, Bok-Hyun;Ma, Chung-Il;Lee, Sang-Jin
    • Korean Journal of Materials Research
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    • v.30 no.2
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    • pp.93-98
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    • 2020
  • Effective control of the heat generated from electronics and semiconductor devices requires a high thermal conductivity and a low thermal expansion coefficient appropriate for devices or modules. A method of reducing the thermal expansion coefficient of Cu has been suggested wherein a ceramic filler having a low thermal expansion coefficient is applied to Cu, which has high thermal conductivity. In this study, using pressureless sintering rather than costly pressure sintering, a polymer solution synthesis method was used to make nano-sized Cu powder for application to Cu matrix with an AlN filler. Due to the low sinterability, the sintered Cu prepared from commercial Cu powder included large pores inside the sintered bodies. A sintered Cu body with Zn, as a liquid phase sintering agent, was prepared by the polymer solution synthesis method for exclusion of pores, which affect thermal conductivity and thermal expansion. The pressureless sintered Cu bodies including Zn showed higher thermal conductivity (180 W/m·K) and lower thermal expansion coefficient (15.8×10-6/℃) than did the monolithic synthesized Cu sintered body.

High-Frequency Induction-Heated Combustion Synthesis and Consolidation of Nanostructured NbSi2 from Mechanically Activated Powders

  • Kim, Byung-Ryang;Yoon, Jin-Kook;Nam, Kee-Seok;Shon, In-Jin
    • Journal of Powder Materials
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    • v.15 no.4
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    • pp.279-284
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    • 2008
  • Dense nanostructured $NbSi_2$ was synthesized by high-frequency induction-heated combustion synthesis (HFIHCS) method within 1 minute in one step from mechanically activated Nb and Si powders. Highly dense $NbSi_2$ with relative density of up to 99% was simultaneously synthesized and consolidated under the combined effects of an induced current and mechanical pressure of 60 MPa. The average grain size and mechanical properties (hardness and fracture toughness) of the compound were investigated.

Synthesis of Intermetallics and Nanocomposites by High-Energy Milling

  • Bernd F. Kieback;H. Kubsch;Alexander Bohm;M. Zumdick;Thomas Weissgaerber
    • Journal of Powder Materials
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    • v.9 no.6
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    • pp.416-421
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    • 2002
  • Elemental powders are used in high energy milling processes for the synthesis of new compounds. The low temperature solid state reactions during milling in inert gas atmosphere may result in intermetallic phases, carbides, nitrides or silicides with a nanocrystalline structure. To obtain dense materials from the powders a pressure assisted densification is necessary. On the other side the defect-rich microstructure can be used for activated sintering of elemental powder mixtures to obtain dense bodies by pressureless sintering. Results are discussed for nanocrystalline cermet systems and for the sintering of aluminides and silicides.

Failure of Ammonia Synthesis Converter Due to Hydrogen Attack and Its On-Stream Assessment Using ToFD Method

  • Albiruni, Farabirazy;Lee, Joon-Hyun
    • Proceedings of the KSME Conference
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    • 2008.11a
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    • pp.132-137
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    • 2008
  • A failure analysis of ammonia converter which suffered hydrogen attack in two years since its initial operating time was presented. It is constructed from 2.25 Cr.1 Mo steel. Analysis showed that the failure on closing seam weld joint was due to local improper post weld heat treatment (PWHT). Improper PWHT can introduce high residual stresses in thick-walled pressure vessel. High residual stress level in weld joint is very prone to hydrogen attack for any components which are operating in hydrogen gas environment. The repair procedures based on the principle to decrease the residual stress then proposed. The repair was controlled very carefully by applying several nondestructive tests in the each stage of repair. To assure the successful of the proposed repair, after one year since repair time, high temperature ultrasonic and TOFD methods were applied on-stream to this equipment in order to evaluate its post repair condition. The two methods showed good results on the repaired area.

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