• Title/Summary/Keyword: Silicate gel

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Multinuclear Solid-state NMR Investigation of Nanoporous Silica Prepared by Sol-gel Polymerization Using Sodium Silicate

  • Kim, Sun-Ha;Han, Oc-Hee;Kim, Jong-Kil;Lee, Kwang-Ho
    • Bulletin of the Korean Chemical Society
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    • v.32 no.10
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    • pp.3644-3649
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    • 2011
  • Multinuclear solid-state nuclear magnetic resonance (NMR) experiments were performed to investigate the local structure changes of nanoporous silica during hydrothermal treatment and surface modification with 3-aminopropyltriethoxysilane (3-APTES). The nanoporous silica was prepared by sol-gel polymerization using inexpensive sodium silicate as a silica precursor. Using $^1H$ magic angle spinning (MAS) NMR spectra, the hydroxyl groups, which play an important role in surface reactions, were probed. Various silicon sites such as $Q^2$, $Q^3$, $Q^4$, $T^2$, and $T^3$ were identified with $^{29}Si$ cross polarization (CP) MAS NMR spectra and quantified with $^{29}Si$ MAS NMR spectra. The results indicated that about 25% of the silica surface was modified. $^1H$ and $^{29}Si$ NMR data proved that the hydrothermal treatment induced dehydration and dehyroxylation. The $^{13}C$ CP MAS and $^1H$ MAS NMR spectra of 3-APTES attached on the surface of nanoporous silica revealed that the amines of the 3-aminopropyl groups were in the chemical state of ${NH_3}^+$ rather than $NH_2$.

Nanoporous Organo-functional Silica Synthesis Based on a Purely Inorganic Precursor

  • Oh, Chang-Sup;Koo, Kyung-Wan;Han, Chang-Suk;Kim, Jang-Woo;Kim, Heon-Chang;Lee, Yong-Sang;Choi, Young-Tai;Kim, Yong-Ha
    • Korean Journal of Metals and Materials
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    • v.47 no.8
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    • pp.516-521
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    • 2009
  • In this study we report a rapid synthesis of nanoporous organo-functional silica (OFS) with unimodal and bimodal pore structures encompassing pores ranging from meso-to macroscale. The problems of tediousness and high production cost in the conventional syntheses are overcome by co-condensation of an inexpensive inorganic precursor, sodium silicate with an organosilane containing trimethyl groups. The insitu covalent anchoring of the non-polar trimethyl groups to the inner pore walls prohibits irreversible shrinkage of the wet-gel during microwave drying at ambient pressure and thus larger size pores (from ca. 20 to ca. 100 nm) can be retained in the dried silica. The drying process of the silylated wet-gels at an ambient pressure can be greatly accelerated upon microwave exposure instead of drying in an oven or furnace. Using this approach, anoporous and superhydrophobic silicas showing a wide variation in texture and morphology can be readily synthesized in roughly two hours. The effects of various sol-gel parameters solely on the textural properties of the organo-functional silica (OFS) have been investigated and discussed.

Preparation of porous silica gel powders from sodium silicates

  • 장감용;전영관;임광일;이광희
    • Proceedings of the Korea Association of Crystal Growth Conference
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    • 1996.06b
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    • pp.29-53
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    • 1996
  • 다공성 실리카 게 분말은 저밀도, 고비표면적의 특성을 가지며 물리적, 화학적 성질이 우수하여 필름의 점착방지제, 페인트의 소광제, 맥주의 흡착제, 촉매의 담지체등 산업전반에 걸쳐 여러용도로 사용되고 있다. 이러한 다공성 실리카 겔 분말은 고상법, 기상법, 액상법등으로 제조할 수 있으며, 이 중에서 sodium silicate를 원료로 하는 액상공정은 다공성의 제어가 용이하고, 공정이 간단하며, 고순도의 균질한 실리카를 얻을 수 있는 방법으로 많이 사용되고 있다. 본 연구에서는 액상법(sol-gel method)를 사용하여 점착방지제, 소광제 등으로 사용되는 다공성 실리카 겔 미분말의 개발에 초점을 두어 연구하였다. 그리고, 겔 분말의 다공성 제어를 위하여 공정 각 단계에서의 겔 내부의 구조의 변화에 대한 연구와 함께 수화겔의 숙성이 기공특성에 미치는 영향, 건조조건의 기공특성에 대한 영향 등을 살펴보았다. 다공성 실리카 겔 미분말은 다음과 같은 공정에 의해 제조되었다. sodium silicate를 황산과 반응시켜 겔화하고 추가의 황산을 투입하여 미반응분의 Na를 제거한 후 pH 7이상의 알카리 영역에서 숙성하여 다공성을 지닌 실리카 수화겔을 제조하였다. 수화겔의 탈수, 세척, 건조 공정을 거쳐 건조겔을 제조하고, 1-20$\mu\textrm{m}$의 크기로 분쇄하여 최종 제품을 얻을 수 있었다. 최종 다공성 실리카 겔 분말은 비표면적 200-700$m^2$/g, 기공부피 0.5-2.5cc/g, 평균 입경 3-5$\mu\textrm{m}$, 백색도 95% 이상의 물성을 보였다. sodium silicate와 황산의 겔화 반응에 의해 생성된 수화겔은 수 nm크기의 일차입자들의 연속적인 network로이루어져 있으며, 일차입자크기가 너무 작기 때문에 내부의 기공들은 별로 존재하지 않는 상태이다. 2차 주가황산 투입에 의해 미반응의 알카리 이온들을 중화, 제거시킬 수 있으며, 겔의 다공성을 좌우하는 숙성단계에서 숙성 pH, 온도, 시간등의 인자에 의해 수화겔의 기공특성을 제어할 수 있다. pH 7이상에서 실리카의 용해도가 크고, 용해도의 입자크기 의존성이 크므로, 일자입자는 Ostwald-ripening에 의해 계속 성장할 수 있으며, 이때, 입자의 성장은 숙성 온도와 시간에 의존한다. 탈수, 세척공정에 의해 가용성 염인 Na2SO4를 제거하고, 건조조건을 변화시킴으로써 기공부피를 증가시키는 것이 가능하였으며, Fast drying을 사용하여 점착방지제에 적합한 기공부피를 갖는 실리카 건조겔을 제조할 수 있었다.

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Synthesis of Hollow Silica Particles from Sodium Silicate using Organic Template Particles (유기 주형 입자를 이용한 소디움 실리케이트로부터 중공형 실리카 입자 제조)

  • Lee, Chongmin;Kim, Jiwoong;Chang, Hankwon;Roh, Ki-Min;Jang, Hee Dong
    • Korean Chemical Engineering Research
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    • v.53 no.1
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    • pp.78-82
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    • 2015
  • Hollow silica particles were prepared using sodium silicate and organic templates. Polystyrene latex (PSL) particles produced by dispersion polymerization were used as organic templates. PSL particles ranged from $1{\mu}m$ to $3{\mu}m$ in diameter were synthesized by adjusting the amount of 2,2'-azobisisobutyronitrile (AIBN). The PSL/$SiO_2$ core-shell particles were prepared by coating of silica nanoparticles originated from sodium silicate using sol-gel method. The organic templates were removed by the organic solvent, tetrahydrofuran (THF). Morphology of hollow silica particles was investigated with respect to types of the reaction medium and pH during the process. By changing the solvent from ethanol to water, hollow silica particles were successfully formed. Hollow silica particles with the uniform shell thickness were produced at low pH as well. The reflectivity of the as-prepared silica particles was measured in the range of the wavelength of UV and visible light. Hollow silica particles showed much better reflective properties than the commercial light reflector, Insuladd.

Silica Glass Preparation by The Sol-Gel Process and The Effects of Glycerol as a DCCA (졸-겔법에 의한 실리카 유리의 제조와 DCCA로서의 Glycerol의 영향)

  • 이경희;이병하;이헌식;오부근
    • Journal of the Korean Ceramic Society
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    • v.25 no.5
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    • pp.479-487
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    • 1988
  • In this study we studied the function of Glycerol as a DCCA(Drying Control Chemical Additives) in the preparation of silica bulk glas through Sol-Gel method. We used TEOS(Tetra Ethyl Ortho Silicate) and maintained the mixing ratio of TEOS : H2O : EtOH : HCI as 1 : 4 : 4 : 0.0007(mol) and varied glycerol input quantity from 0.1vol% considering the ethnaol input quantity as 100vol%. We investigated the changes from Sol-Gel Synthetic solutions to the glass using DT-TG, FT-IR and other instruments. The results obtained from this experiment showed that the dried gels made from the synthetic solutions containing 0.1-1.0vol% of glycerol were easily heat-treated up to 85$0^{\circ}C$ so that transparant bulk silica glass was prepared.

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Optimum Synthesis and Characterization of Precursor Solution for a Hard Coating Silica Film Prepared by Sol-Gel Process

  • Kim, Seon Il;Kim, Gu Yeol;Im, Hyeong Mi;Lee, Bong U;Na, Jae Un
    • Bulletin of the Korean Chemical Society
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    • v.21 no.8
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    • pp.817-822
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    • 2000
  • Crack-free hard coating siIica films were prepared by sol-gel processfrom twokinds of silicon alkoxide (tetra-ethoxysilane and methyltrimethoxysilane) and two kinds of alcohol (methanol and isopropyl alcohol) with an acid catalyst,acetic acid. A silicate framework of the precursor solution was investigated by infrared spectros-copy (IR) in the process of hydrolysis and condensation. Theextent of the condensation in the intermediates was elucidated by gel permeation chromatography (GPC) and 29Si-NMR spectroscopy. The hard coating films werecharacterized by IR,scanning electron microscope (SEM), thermo gravimetric analyzer (TGA) and dif-ferential scanning calroimeter (DSC). The synthetic condition for the crack-free and transparent silica film for-mation was optimized interms of starting materials for the precursor solution as well as preparation method of the silica film.

Preparation and Characterization of Sol-Gel Derived $SiO_2-TiO_2$ -PDMS Composite Films

  • Hwang, Jin Myeong;Yeo, Chang Seon;Kim, Yu Hang
    • Bulletin of the Korean Chemical Society
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    • v.22 no.12
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    • pp.1366-1370
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    • 2001
  • Thin films of the SiO2-TiO2-PDMS composite material have been prepared by the sol-gel dip coating method. Acid catalyzed solutions of tetraethoxy silane (TEOS) and polydimethyl siloxane (PDMS) mixed with titanium isopropoxide Ti(OiPr) were used as precursors. The optical and structural properties of the organically modified 70SiO2-30TiO2 composite films have been investigated with Fourier Transform Infrared Spectroscopy (FT-IR), UV-Visible Spectroscopy (UV-Vis), Differential Thermal Analysis (DTA) and prism coupling technique. The films coated on the soda-lime-silicate glass exhibit 450-750 nm thickness, 1.56-1.68 refractive index and 88-94% transmittance depending on the experimental parameters such as amount of PDMS, thermal treatment and heating rate. The optical loss of prepared composite film was measured to be about 0.34 dB/cm.

Effect of annealing temperature on surface properties of chemical solution derived silicate fiber (화학적 용액법으로 제조한 실리케이트 섬유의 표면 특성에 미치는 열처리 온도의 영향)

  • 황규석;김상복;이영환;장승욱;오정선;안준형;김병훈
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.13 no.5
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    • pp.217-221
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    • 2003
  • In this work, chemical-solution derived silicate fibers were prepared by mixing tetraethyl orthosilicate, ethanol, distilled water, and hydrochloric acid in order to investigate surface roughness of fiber. Silicate fibers were drawn by using a viscous solution after evaporation at $80^{\circ}C$. The dried gel fibers were finally annealed at $1000^{\circ}C$, $1100^{\circ}C$, $1200^{\circ}C$ and $^1300{\circ}C$ for 60 min in dried air (flow rate = ∼200 ml/min). The crystallinity of the heat-treated silica fiber was analyzed by the X-ray diffraction $\theta$-2$\theta$ scan. A field emission-scanning electron microscope and an atomic force microscope were used to evaluate surface properties. The silicate fiber annealed at $1300^{\circ}C$ showed high value of root mean square roughness and had a relatively inhomogeneous surface structure.

Effect of Foliar and Root Application of Silicon Against Rice Blast Fungus in MR219 Rice Variety

  • Abed-Ashtiani, Farnaz;Kadir, Jugah-Bin;Selamat, Ahmad-Bin;Hanif, Ahmad Husni Bin-Mohd;Nasehi, Abbas
    • The Plant Pathology Journal
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    • v.28 no.2
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    • pp.164-171
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    • 2012
  • Rice blast disease caused by Magnaporthe grisea (Hebert) Barr [teleomorph] is one of the most devastating diseases in rice plantation areas. Silicon is considered as a useful element for a large variety of plants. Rice variety MR219 was grown in the glasshouse to investigate the function of silicon in conferring resistance against blast. Silica gel was applied to soil while sodium silicate was used as foliar spray at the rates of 0, 60, 120, 180 g/5 kg soil and 0, 1, 2, 3 ml/l respectively. The treatments were arranged in a completely randomized design. Disease severity and silicon content of leaves were compared between the non-amended controls and rice plants receiving the different rates and sources of silicon. Silicon at all rates of application significantly (${\alpha}$ = 0.05) reduced the severity of disease with highest reduction (75%) recorded in treatments receiving 120 g of silica gel. SEM/EDX observations demonstrated a significant difference in weight concentration of silicon in silica cells on the leaf epidermis between silicon treated (25.79%) and non treated plants (7.87%) indicating that Si-fertilization resulted in higher deposition of Si in silica cells in comparison with non-treated plants. Application of silicon also led to a significant increase in Si contents of leaves. Contrast procedures indicated higher efficiency of silica gel in comparison to sodium silicate in almost all parameters assessed. The results suggest that mitigated levels of disease were associated with silicification and fortification of leaf epidermal cells through silicon fertilization.

The Effect of Sodium Gluconic Acid on the Collapsability of $CO_2$ Mold (($CO_2$ 주형의 붕괴성에 미치는 글루콘산 소다의 영향)

  • Shin, Un-Yong;Kwon, Hae-Wook;Nam, Won-Sik
    • Journal of Korea Foundry Society
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    • v.14 no.6
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    • pp.499-507
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    • 1994
  • The effect of sodium gluconic acid on the collapsability of the sodium silicate type $CO_2$ mold was studied. The bending strength was saturated with gassing $CO_2$ for 60 sec. under $1kg/cm^2$ and with the flow rate of $10\;{\ell}\;/min$. It was decreased with aging after having been fully hardened. The retained strength was reduced in the heating temperature range of $100{\sim}1,100^{\circ}C$ and the retained strength peak near the heating temperature of $100^{\circ}C$ was removed by the effect of the sodium gluconic acid. Silica gel, $Na_2CO_3$ and dehydrated sodium silicates were formed from the binder of sodium silicate with the addition of sodium gluconic acid at the heating temperature of $100^{\circ}C$. $Na_4SiO_4$ was formed by the reaction of $Na_2O$, from decomposed $Na_2CO_3$, with the dehydrated sodium silicate at $500^{\circ}C$. The crystobalite type of $SiO_2$ was formed at $900^{\circ}C$. The sodium gluconic acid had no effect on the bending strength at around $1,100^{\circ}C$ due to the combustion loss of it.

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