• 제목/요약/키워드: Hydrolysis-condensation reaction

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실란처리를 통한 안정화된 $TiO_2$졸의 합성 (Synthesis of stabilized $TiO_2$ sol by sillane treatment)

  • 한동희;강동준;김락희;강동필
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2007년도 하계학술대회 논문집 Vol.8
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    • pp.234-235
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    • 2007
  • Transparent nanosized $TiO_2$ sol has been made by sol-gel method, using Titanium(IV) isopropoxide precursor. To promote hydrolysis for titania is needed excess water, Oil bath and temperature about $80^{\circ}C$. $TiO_2$ sol is peptized ranging from pH 1 to 1.5 using hydrochloric acid for the stability of sol during a condensation reaction. The average particle size of $TiO_2$ sol was approximately 20nm. $TiO_2$-sillane sol was synthesized by surface treatment using MTMS to the $TiO_2$ sol. TEM analysis has been used to check the degree of dispersion and FT-IR analysis has been used to see if the sillane has been chemically bonded on the surface of $TiO_2$.

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Synthesis of Monodispersed and Spherical $SiO_2-coated Fe_2O_3$ Nanoparticle

  • 한양수;윤선미;김동국
    • Bulletin of the Korean Chemical Society
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    • 제21권12호
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    • pp.1193-1198
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    • 2000
  • The preparation of nanocrystalline hematite, ${\alpha}-Fe_2O_3$, paricles and their surface coating with silica layers are described. The hematite particles with the size of 30~60 nm are firstly prepared by thermal decomposition of trinuclear acetate-hydroxo iron (III) nitrate complex, $[Fe_3$(OCOCH_3)_7$OH${\cdot}$2H_2O]NO_3$, at $400^{\circ}C$. Subsequently the hematite surfaces are coated with siliva layers by a controlled hydrolysis and condensation reaction of TEOS with varying the TEOS concentration and pH. Monodispersed and spherical $SiO_2-coatedFe_2O_3$ particles with the average particle diameter of ~90 nm and extremely narrow size distribution can be obtained at the pH of 11 and the TEOS concentration of 0.68M, which are found to be the optimum conditions in the present study in achieving the homogeneous deposition of silica layers on hematite surfaces. Diffuse reflectance UV-Vis spectra reveal that the characteristic optical reflectance of ${\alpha}-Fe_2O_3$ particles is preserved almost constant even after coating the surfaces, suggesting that the $SiO_2$ layers can be regarded as protecting layers without degrading the optical properties of hematite particles.

Growth and Migration of BALB/3T3 Fibroblast Cells on Nano-engineered Silica Beads Surface

  • Kim, Jihee;Chandra, Prakash;Yang, Jiyoon;Rhee, Seog Woo
    • Bulletin of the Korean Chemical Society
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    • 제34권12호
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    • pp.3715-3721
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    • 2013
  • In this study, the behavior of cells on the modified surface, and the correlation between the modified substrates and the response of cells is described. A close-packed layer of nano-sized silica beads was prepared on a coverslip, and the adhesion, proliferation, and migration of BALB/3T3 fibroblast cells on the silica layer was monitered. The 550 nm silica beads were synthesized by the hydrolysis and condensation reaction of tetraethylorthosilicate in basic solution. The amine groups were introduced onto the surfaces of silica particles by treatment with 3-aminopropyltrimethoxysilane. The close-packed layer of silica beads on the coverslip was obtained by the reaction of the amine-functionalized silica beads and the (3-triethoxysilyl)propylsuccinic anhydride treated coverslip. BALB/3T3 fibroblast cells were loaded on bare glass, APTMS coated glass, and silica bead coated glass with the same initial cell density, and the migration and proliferation of cells on the substrates was investigated. The cells were fixed and stained with antibodies in order to analyze the changes in the actin filaments and nuclei after culture on the different surfaces. The motility of cells on the silica bead coated glass was greater than that of the cells cultured on the control substrate. The growth rate of cells on the silica bead coated glass was slower than that of the control. Because the close-packed layer of silica beads gave an embossed surface, the adhesion of cells was very weak compared to the smooth surfaces. These results indicate that the adhesion of cells on the substrates is very important, and the actin filaments might play key roles in the migration and proliferation of cells. The nuclei of the cells were shrunk on the weakly adhered surfaces, and the S1 stage in which DNA is duplicated in the cell dividing processes might be retarded. As a result, the rate of proliferation of cells was decreased compared to the smooth surface of the control. In conclusion, the results described here are very important in the understanding of the interaction between implanted materials and biosystems.

Photoaddition Reactions of Silyl Ketene Acetals with Aromatic Carbonyl Compounds: A New Procedure for β-Hydroxyester Synthesis

  • Yoon, Ung-Chan;Kim, Moon-Jung;Moon, Jae-Joon;Oh, Sun-Wha;Kim, Hyun-Jin;Mariano, Patrick S.
    • Bulletin of the Korean Chemical Society
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    • 제23권9호
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    • pp.1218-1242
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    • 2002
  • Photochemical reactions of aromatic carbonyl compounds with silyl ketene acetals have been explored. Irradiation of acetonitrile or benzene solutions containing aryl aldehydes or ketones in the presence of silyl ketene acetals is observed to promo te formation of ${\beta}-hydroxyester$, 2,2-dioxyoxetane and 3,3-dioxyoxetane products. The ratios of these photoproducts, which arise by competitive single electron transfer (SET) and classical Paterno-Buchi mechanistic pathways, is found to be dependent on the degree of methyl-substitution on the vinyl moieties of the ketene acetals in a manner which reflects expected alkyl substituent effects on the oxidation potentials of these electron rich donors. An analysis of the product distribution arising by irradiation of a solution containing butyrophenone (6) and the silyl ketene acetal 9, derived from methyl isobutyrate, provides an estimate of the rate constants for the competitive Norrish type Ⅱ, SET and Paterno-Buchi processes occuring. Finally, sequences involving silyl ketene acetal-aryl aldehyde or ketone photoaddition followed by 2,2-dioxyoxetane hydrolysis represent useful procedures for Claisen-condensation type, ${\beta}-hydroxyester$ synthesis.

고효율 소형 연료전지의 개발 : I.유기-무기 나노복합 전해질막의 합성 (Development of High-Efficient Small Euel Cells : I. Synthesis of Organic-Inorganic Nanocomposite Electrolyte Membranes)

  • 박용일;문주호;김혜경;김석환
    • 한국세라믹학회지
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    • 제42권1호
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    • pp.50-55
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    • 2005
  • (3-Mercaptopropyl) trimethoxysilane(MPTS)의 thoil기(-SH)의 적절한 산화 및 (3-glycidoxypropyl) trimethooxysilane(GHS)와의 수화/중축합 반응을 통하여 얻어진 고분자 기질을 사용하여 새로운 고 프로톤 전도성 유기-무기 나노복합막을 성공적으로 합성하였다. 합성된 나노복합막으로부터 얻어진 프로톤 전도도는 $25^{circ}C$에서 $10^{-2} S/cm$ 이상의 높은 값을 나타내었으며, 온도와 상대습도를 $70^{circ}C$$100RH\%$로 증가시킴에 따라 전도도는 $3.6{\times}10^{-1}$ S/cm까지 증가하였다. 복합체의 높은 프로톤 전도도는 MPTS 말단의 thiol의 산화에 의해 얻어지는 아황산기$(-SO_{3}^{-})$가 프로톤 donor로서 작용하고, GHS로부터 유도된 'pseudo polyethylene oxide' 네트워크가 프로톤의 전도 path로 작용하고 있음을 나타낸다.

EPD 방법을 이용한 알루미나-실리카 복합 코팅막의 제조와 전기절연 특성 (Preparation of Alumina-Silica Composite Coatings by Electrophoretic Deposition and their Electric Insulation Properties)

  • 지혜;김두환;박희정;임형미;이승호;김대성;김영희
    • 한국세라믹학회지
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    • 제51권3호
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    • pp.177-183
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    • 2014
  • Alumina-silica composite coating layers were prepared by electrophoretic deposition (EPD) of plate-shaped alumina particles dispersed in a sol-gel binder, which was prepared by hydrolysis and the condensation reaction of methyltrimethoxysilane in the presence of colloidal silica. The microstructure and the electrical and thermal properties of the coatings were compared according to the EPD process parameter: voltage, time and the content of the plate-shaped alumina particles. The electrical insulation property of the coatings was measured by a voltage test. The coatings were prepared by EPD of the sol-gel binder with 5-30 wt% plate alumina particles on parallel electrodes at a distance of 2 cm for 1-10 min under an applied voltage of 10-30 V. The coatings experienced increased breakdown voltage with increasing thickness. However, the higher the thickness was, the smaller the breakdown voltage strength was. A breakdown voltage as high as 4.6 kV was observed with a $400{\mu}m$ thickness, and a breakdown voltage strength as high as 27 kV/mm was achieved for the sample under a $100{\mu}m$ thickness.

재현성 있는 메조포러스 TiO2 박막의 제조에 대한 연구 (Reproducible Synthesis of Periodic Mesoporous TiO2 Thin Film)

  • 허재영;이형익;박영권;주오심;배귀남;김지만
    • Korean Chemical Engineering Research
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    • 제44권4호
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    • pp.399-403
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    • 2006
  • 현재 넓은 표면적과 메조기공 뿐만 아니라 $TiO_2$의 넓은 band gap과 그 광학 활성 등으로 인하여 크게 각광받고 있는 메조포러스 $TiO_2$ 박막을 합성하기 위해 여러 가지 합성방법이 제시되고 있으나, 그 합성이 습도나 온도 등의 여러조건에 따라 크게 영향을 받아 재현성이 떨어진다는 치명적인 문제점이 제기되어 왔다. 이는 합성 용액 내에서 $TiO_2$ 전구체가 가수분해 및 축합반응을 하면서 구조유도체와의 자기조립에 의한 나노구조물 형성하는 과정에서 $TiO_2$의 전구체가 온도나 습도 등 주변의 영향을 많이 받기 때문이다. 본 연구에서는 2차원 구조의 메조기공을 가진 $TiO_2$ 박막을 재현성 있게 얻을 수 있는 실험 조건을 찾고자 하였다. 이를 위해 촉매인 HCl과 $TiO_2$ 전구체의 몰비 그리고 $TiO_2$ 전구체와 P-123의 몰비 등의 합성 조건뿐 아니라 코팅과정 도중이나 이후의 습도와 온도가 미치는 영향에 대한 실험을 수행하였고 그 특성을 XRD와 TEM 등으로 분석하였다.

희토류 원소의 분리를 위한 표면 개질 된 메조 다공성 실리케이트의 개발에 관한 연구 (Study on CMPO (Carbamoylphosphate) derivative functionalized ordered mesoporous silicates for selective removal of lanthanide)

  • 권법진;정현;김종영
    • 한국결정성장학회지
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    • 제22권6호
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    • pp.291-298
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    • 2012
  • 자기 조립 분자 집합체 물질인 CMPO로 표면개질 된 메조 다공성 실리케이트를 가수분해와 축합반응을 이용하여 합성하였다. 손님 물질인 CMPO는 2-(diphenylphosphoryl) acetic acid와 3-(triethoxysilyl) propan-1-amine의 아마이드 결합반응을 이용하여 합성하였으며, MCM-41, SBA-15 그리고 실리카 나노입자와 같은 다양한 메조 다공성 실리케이트는 주인물질로 채택하였다. 메조 다공성 실리케이트의 비표면적은 680 $m^2/g$~1310 $m^2/g$의 넓이로 측정되었으며 BJH 방법을 이용해서 동공의 크기를 확인한 결과 2.3~9.1 nm 범위의 다양한 크기를 가지고 있었다. 메조 다공성 실리카 중에서는 SBA-15(II)가 가장 높은 약 35 wt%의 CMPO 함유량을 나타내었다. 메조 다공성 실리케이트의 표면에 개질된 CMPO 실란 작용기와 란탄족 이온과의 접근성에 관한 연구 결과, CMPO로 개질 된 모든 흡착제의 경우 상대적으로 이온 반경이 큰 La(III)보다는 크기가 작은 Nd(III)와 Eu(III) 이온을 더 선호하였다.

졸-겔 공정으로 합성된 코디어라이트를 이용하여 알루미나의 표면개질 (Surface Modification of Alumina Ceramic with Mg2Al4Si5O18 Glass by a Sol-Gel Process)

  • 최필규;추민철;배동식
    • 한국재료학회지
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    • 제24권1호
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    • pp.48-52
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    • 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.

Preparation and Characterization of Organic-inorganic Hybrid Composite Film with Plate-shaped Alumina by Electrophoretic Deposition as a Function of Aging Time of Sol-Gel Binder

  • Kim, Doo Hwan;Park, Hee Jeong;Choi, Jinsub;Lim, Hyung Mi
    • 한국세라믹학회지
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    • 제52권5호
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    • pp.366-373
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    • 2015
  • Sol-gel binder was prepared by hydrolysis and condensation reaction using boehmite sol and methyltrimethoxysilane as a function of aging-time. The coating slurry was composed of a plate-shape alumina in the sol-gel binder for the EPD process, in which particles dispersed in the slurry were deposited on the electrode under an electric field due to the surface charge. We studied the effects of three parameters: the content of boehmite, the aging time, and the applied voltage, on the physical, thermal, and electrical properties of the hybrid composite films by EPD. The amount of boehmite was 10 ~ 20 wt% and the aging time was 0.5 ~ 72, with a fixed amount of plate-shape alumina of 10 wt%. The condition of applied voltage was 5 ~ 30 V with a distance of 2 cm between the electrode during the EPD process. We confirmed that a structure of hybrid composite films of well-ordered plate alumina was deposited on the substrate when the film was prepared using a sol-gel binder composed of 15 wt% boehmite with 1 hr aging time and EPD at 10 V. The process shows a weight loss of 7% at $500^{\circ}C$ in TGA and a breakdown voltage of 8 kV at $87{\mu}m$.