• Title/Summary/Keyword: 건조겔법

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Effects of Drying Agents on the Drying and Calcination in Synthesis of Mullite by Sol-Gel Process (졸-겔법에 의한 mullite합성시 건조 첨가제가 건조 및 소성에 미치는 영향)

  • Hahm, Yeong-Min;Hong, Young-Ho;Choi, Seung-Il
    • Applied Chemistry for Engineering
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    • v.4 no.3
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    • pp.497-504
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    • 1993
  • The effect of DCCA (Drying Control Chemical Additives) on the drying of gel was investigated in order to determine an optimum drying condition of mullite precursor through sol-gel process. Aluminium sec-butoxide was synthesized from aluminium foil and then mullite powders were synthesized from Tetra-ethyl-ortho-silicate (TEOS) and the aluminium sec-butoxide. N, N-dimethyl formamide (DMF), Glycerol, 1, 4-Dioxane, and Oxalic acid were used as DCCA. Mullite powders that were calcined at 200, 900, 1100, and $1250^{\circ}C$ for 2hr were analysed by XRD, TG-DTA, FT-IR, and SEM in order to investigate structural change and characteristics of calcined powders. The results of this work showed that the drying time of gel was reduced to about half in the presence of 0.1mol DMF compared with the absence of DCCA and also calcined powders were obtained without remarkable structural change despite of the addition of DCCA.

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Chemical solution derived hydroxyapatite films on Si substrates (화학 용액법으로 Si 기판 위에 제조한 하이드록시아파타이트 박막에 관한 연구)

  • 송종은;류현욱;신종윤;김병훈;김윤호;임용무
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.9 no.6
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    • pp.570-573
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    • 1999
  • Hydroxyapatite films were prepared on Si(100) substrates by using a sol-gel method with calcium nitrate and phosphoric acid as starting materials. Precursor sols were spin-coated onto the substrates and prefired at $500^{\circ}C$ for 10 min in air. Formation of the hydroxypatite structure was confirmed in the sample annealed at $500^{\circ}C$ by the X-ray diffraction $\theta$-2$\theta$ scans and a tricalcium phosphate phase was observed in the samples annealed at both temperature regions of $500^{\circ}C$~$700^{\circ}C$ and $900^{\circ}C$. From the results of Fourier transform infrared spectroscopy, the change of a carbon content and improvement of crystallinity have been discussed as a function of increase of annealing temperature.

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Synthesis and Physical Properties of MO·Fe12O18 (M/Ba and Sr) Nanoparticles Prepared by Sol-Gel Method Using Propylene Oxide (Propylene Oxide를 이용한 졸-겔법에 의한 MO·Fe12O18 (M/Ba, Sr) 나노 분말의 합성과 물리적 특성)

  • Lee, Su Jin;Choe, Seok Burm;Gwak, Hyung Sub;Paik, Seunguk
    • Applied Chemistry for Engineering
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    • v.17 no.4
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    • pp.420-425
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    • 2006
  • Nano sized mixed metal hexagonal ferrite powders with improved magnetic properties have been prepared by sol-gel method using propylene oxide as a gelation agent. To obtain the desired ferrite, two different metal ions were used. One of the ions has only +2 formal charge. The key step in the processes is that hydrated $Ba^{2+}$ or $Sr^{2+}$ ions are hydrolyzed and condensed at the surface of the previously formed $Fe_{2}O_{3}$ gel. In this processes, all the reaction can be finished within a few minutes. The magnetic properties of the produced powder were improved by heat treatment. The highest values of the magnetic properties were achieved at temperature $150^{\circ}C$ lower than those of the previously published values. The highest observed values of coercivity and the saturation magnetization of Sr-ferrite and Ba-ferrite powder were 6198 Oe, 5155 Oe and 74.4 emu/g, 68.1 emu/g, respectively. The ferrite powder annealed at $700^{\circ}C$ showed spherical particle shapes. The resulting spheres which were formed by the aggregation of nanoparticles with size 3~5 nm have diameter around 50 nm. The powder treated at $800^{\circ}C$ showed hexagonal-shaped grains with crystallite size above 500 nm.

Synthesis and Magnetic Properties of Nanosized Ce-substituted Yttrium Iron Garnet Powder Prepared by Sol-gel Method (졸-겔법에 의한 Cerium 치환 Nanosize YIG 분말의 합성 및 자기적 특성)

  • 장학진;김광석;윤석영;김태옥
    • Journal of the Korean Ceramic Society
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    • v.38 no.11
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    • pp.1008-1014
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    • 2001
  • Nanosize YIG powders added by Cerium which is exellent element in magneto-optical effect were synthesized by Sol-Gel method using Ethylene Glycol solvent. In 120 to 150 minute reaction time, stable sol solution which showed no change in viscosity, pH, and aging time was obtained. Monolithic YIG was synthesized at 80$0^{\circ}C$ with DTA and XRD measurement and its lattice parameter had a tendency to increase from 12.3921 $\AA$. Increasing annealing temperature from 80$0^{\circ}C$ to 105$0^{\circ}C$, average particle size was in the range of 40 nm to 330 nm. Saturation magnetization (M$_{s}$) value was increased from 18.37 to 21.25 emu/g due to enhancement of YIG crystallity and decreasing of orthoferrite phase. On the other hand, coercivity (H$_{c}$) value increased up to 90$0^{\circ}C$ and then decreased above 90$0^{\circ}C$. With increasing Ce addition, coercivity was almost not changed but saturation magnetization value was maximum at Ce 0.1 mol% and then decreased because of increasing a orthoferrite amount. Also, curie temperature (T$_{c}$) of YIG were not changed with Ce addition.ion.

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Annealing Temperature Dependence on Anodizing Properties of ZrO2/Al Films Prepared by Sol-gel Method (졸-겔법으로 제조된 ZrO2/Al막의 열처리 온도에 따른 양극산화 특성)

  • 박상식;이병택
    • Journal of the Korean Ceramic Society
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    • v.40 no.9
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    • pp.909-915
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    • 2003
  • Anodic oxide films on aluminum play an important role as a dielectrics in aluminum electrolytic capacitor. In order to obtain the high capacitance, ZrO$_2$ films were coated on aluminum foils by sol-gel method and then, the properties of anodized films were studied. The coating and drying of the films were repeated 4-10 times and annealed at 300~$600^{\circ}C$ and the triple layer of ZrO$_2$/Al-ZrO$_{x}$ /Al$_2$O$_3$ was formed onto aluminum substrates after anodizing of ZrO$_2$/Al film. The thickness of $Al_2$O$_3$ layer was decreased with increasing the annealing temperature due to the densification of ZrO$_2$ film. The ZrO$_2$ films were crystallized even at 30$0^{\circ}C$ and showed nanocrystalline structure. The. capacitance of aluminum foil annealed at low temperature was higher than that at high temperature. The increase of capacitance was due to the high capacitance of ZrO$_2$ film annealed at low temperature. The capacitance of ZrO$_2$ coated aluminum increased about 3 times compared to that without a ZrO$_2$ layer after anodizing to 400 V. From these results, the aluminum foils with composite oxide layers are found to be applicable to the aluminum electrolytic capacitor.

A study on the preparation and analysis of cordierite by sol-gel method (졸-겔법에 의한 코디어라이트 제조와 분석에 관한 연구)

  • Chun, Kyung Soo;Lee, Young Hwan
    • Analytical Science and Technology
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    • v.21 no.2
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    • pp.123-128
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    • 2008
  • The golden turbid solution of cordierite precursor was obtained by using magnesium ethoxide in sol-gel method, while the clear solution of cordierite precursor was obtained when 5%-$Zr(OC_3H_7)_4$ solution was used in the sol-gel reaction. $SiO_2$ component was confirmed by infrared spectra showing $1045cm^{-1}$ and the stretching vibration of gelish $SiO_4$ showed $1140cm^{-1}$ and $940cm^{-1}$. The component of $Al_2O_3$ showed at $580cm^{-1}$ and network structure of $Al_2O_6$ showed at $680cm^{-1}$. The component of MgO was confirmed at $575cm^{-1}$ as the stretching vibration. X-ray diffraction analysis showed ${\mu}$-cordierite crystal was showed up at temperature above $1000^{\circ}C$ at the mole ratio of cordierite precursor and water (1:5). ${\mu}$-Cordierite and ${\alpha}$-cordierite were coexisted at $1050^{\circ}C$ for the mole ratio of cordierite precursor and ammonia (1:5) while ${\alpha}$-cordierite was only existed at $1100^{\circ}C$ for the same mole ratio as mentioned above.

Synthesis of Borosilicate Zeotypes by Steam-assisted Conversion Method (수증기 쪼임법에 의한 제올라이트형 보로실리케이트 제조방법)

  • Mansour, R.;Lafjah, M.;Djafri, F.;Bengueddach, A.
    • Journal of the Korean Chemical Society
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    • v.51 no.2
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    • pp.178-185
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    • 2007
  • Intermediate pentasil borosilicate zeolite-like materials have been crystallized by a novel method named steam-assisted conversion, which involves vapor-phase transport of water. Indeed, amorphous powders obtained by drying Na2O.SiO2.B2O3.TBA2O gels of various compositions using different boron sources are transformed into crystalline borosilicate zeolite belonging to pentasil family structure by contact with vapors of water under hydrothermal conditions. Using a variant of this method, a new material which has an intermediate structure of MFI/MEL in the ratio 90:10 was crystallized. The results show that steam and sufficiently high pH in the reacting hydrous solid are necessary for the crystallization to proceed. Characterization of the products shows some specific structural aspects which may have its unique catalytic properties. X-ray diffraction patterns of these microporous crystalline borosilicates are subjected to investigation, then, it is shown that the product structure has good crystallinity and is interpreted in terms of regular stacking of pentasil layers correlated by inversion centers (MFI structure) but interrupted by faults consisting of mirror-related layers (MEL structure). The products are also characterized by nitrogen adsorption at 77 K that shows higher microporous volume (0.160 cc/g) than that of pure MFI phase (0.119 cc/g). The obtained materials revealed high surface area (~600 m2/g). The infrared spectrum reveals the presence of an absorption band at 900.75 cm-1 indicating the incorporation of boron in tetrahedral sites in the silicate matrix of the crystalline phase.

Magnetic Characteristics of BaFe12-2xCoxTixO19 Particles Prepared by Sol-gel Synthesis (졸-겔 합성에 의한 BaFe12-2xCoxTixO19 미립자의 자기적 특성)

  • 최현승;정지형;박효열;김태옥
    • Journal of the Korean Ceramic Society
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    • v.40 no.1
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    • pp.62-68
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    • 2003
  • Ba-ferrite particles added with Co and Ti, which were known well the additives for the control in coercivity, were synthesized by sol-gel method. In the range 90 to 120 minute reaction time, a stable sol solution which showed no change with temperature, pH, viscosity and aging time. After dried and heat treatment of sol solution, Ba-ferrite phase formed at $700^{\circ}C$ with Differential Thermal Analysis(DTA) and X-Ray Diffractometer(XRD) measurement. The crystallinity became to be better with increasing the temperature. It were showed by Scanning Electron Microscopy(SEM) that Ba-ferrite increased to particle sizes as increasing heating temperature and obtained of narrow particles size distribution. Also, magnetic characteristics of Ba-ferrite powders Co and Ti added were observed by a Vibrating Sample Magnetometer(VSM). Saturation magnetization$(M_s)$ was not much changed, however. the coercivity$(H_c)$dramatically dropped with addition of Co and Ti.

Particle Size Control by the Addition of PVA and HNO3 in γ-Al2O3 Synthesis Using by Sol-Gel Method (졸-겔법을 이용한 γ-Al2O3 합성 시 PVA와 HNO3 첨가에 따른 입자크기 제어)

  • Um, Myeong-Heon;Kim, Na-Eun;Ha, Beom-Yong
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.11
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    • pp.537-543
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    • 2019
  • Alumina(Al2O3) is a ceramic material used in industry with a range of particle sizes and characteristics. In this study, a boehmite sol was prepared by a hydrolysis and peptizing process using the Sol-Gel method from aluminum isopropoxide (AIP). γ-Al2O3 was prepared by drying and calcining. To prevent particle agglomeration during the manufacturing process, four kinds of polyvinyl alcohol (PVA) with molecular weights of 9,000~10,000, 31,000~50,000, 89,000~98,000, and 130,000 were added and three concentrations of HNO3 (0.1, 0.3, 0.5 molar ratio) were added to determine their effects on the particles. The crystal structure, composition, particle size and shape of the prepared γ-Al2O3 were confirmed through x-ray diffraction (XRD), x-ray fluorescence analyzer (XRF), particle size analyzer (PSA), and field emission scanning electron microscopy (FE-SEM). As a result, γ-Al2O3 with a purity of approximately 98.2% was synthesized, and the particle size decreased and the uniformity increased with increasing ratio of HNO3 addition and PVA molecular weight. From these results, the particle size can be controlled during the manufacturing process of γ-Al2O3 by controlling the addition ratio of PVA and HNO3.

The Optimum of $CO_2$ Decomposition using Spinel Phase $Li{Mn_2}{O_4}$ (스피넬상 $Li{Mn_2}{O_4}$를 이용한 $CO_2$ 분해의 최적조건)

  • Lee, Dong-Suek;Rim, Byung-O;Yang, Chun-Hoe;Lee, Poong-Hun
    • Journal of the Korean Ceramic Society
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    • v.38 no.10
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    • pp.894-900
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    • 2001
  • The spinel $Li{Mn_2}{O_4}$ catalysts for $CO_2$ decomposition were synthesized by a sol-gel method using manganese acetate and lithium hydroxide as starting materials through drying at $150^{\circ}C$ for 12 hrs under oxygen atmosphere followed by heat treatment at $480^{\circ}C$ for 12 hrs. The synthesized $Li{Mn_2}{O_4}$ were reduced by hydrogen for 3 hrs at various temperatures and the decomposition rate of carbon dioxide was investigated at 300, 325, 350, 375 and $400^{\circ}C$ using the $Li{Mn_2}{O_4}$ reduced by hydrogen gases. As a result of experiment, the optimum temperature of hydrogen reduction and $CO_2$ decomposition was shown $350^{\circ}C$. The physicochemical properties of the spinel $Li{Mn_2}{O_4}$ the reduced $Li{Mn_2}{O_4}$ and the $Li{Mn_2}{O_4}$ after $CO_2$ decomposition were examined with XRD, SEM and TGA.

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