• Title/Summary/Keyword: $St{\ddot{o}}ber$ method

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Preparation and characterization of nanosized hollow silica in the presence of aluminum isopropoxide

  • Nguyen, Ngoc Anh Thu;Kim, Hyun-Ik;Kim, Sang Hern
    • Journal of the Korean Applied Science and Technology
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    • v.33 no.3
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    • pp.421-427
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    • 2016
  • Nanosized hollow silica was prepared by $St{\ddot{o}}ber$ method in the presence of aluminum isopropoxide. The mixture of polyelectrolytes such as poly(sodium 4-styrene sulfonate)(PSS) and polyacrylic acid(PAA) were used as templates. Tetraethylorthosilicate(TEOS) and aluminum isopropoxide were used as precursors for silica and alumina, respectively. The function of aluminum isopropoxide is to increase the porosity of silica shell. The characterizations of hollow silica were examined by TEM(transmission electron microscopy), TGA(thermogravimetric analysis), BET(Brunauer Emmett Teller), Energy-dispersive X-ray spectroscopy(EDS), and FT-IR spectrum. It was found that the shell thickness of hollow silica was around 8 nm and the core diameter was around 20 nm by TEM.

A Study on the Blue Fluorescence Characteristics of Silica Nanoparticles with Different Particle Size (실리카 나노 입자의 크기에 따른 청색 형광 특성 연구)

  • Yoon, Ji-Hui;Kim, Ki-Chul
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.5
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    • pp.1-6
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    • 2019
  • Organic dye-doped silica nanoparticles are used as a promising nanomaterials for bio-labeling, bio-imaging and bio-sensing. Fluorescent silica nanoparticles(NPs) have been synthesized by the modified $St{\ddot{o}}ber$ method. In this study, dye-free fluorescent silica NPs of various sized were synthesized by Sol-Gel process as the modified $St{\ddot{o}}ber$ method. The functional material of APTES((3-aminopropyl)triethoxysilane) was added as an additive during the Sol-Gel process. The as-synthesized silica NPs were calcined at $400^{\circ}C$ for 2 hours. The surface morphology and particle size of the as-synthesized silica NPs were characterized by field-emission scanning electron microscopy. The fluorescent characteristics of the as-synthesized silica NPs was confirmed by UV lamp irradiation of 365 nm wavelength. The photoluminescence (PL) of the as-synthesized silica NPs with different size was analyzed by fluorometry. As the results, the as-synthesized silica NPs exhibits same blue fluorescent characteristics for different NPs size. Especially, as increased of the silica NPs size, the intensity of PL was decreased. The blue fluorescence of dye-free silica NPs was attributed to linkage of $NH_2$ groups of the APTES layer and oxygen-related defects in the silica matrix skeleton.

Electrochemical Performance of Hollow Silicon/Carbon Anode Materials for Lithium Ion Battery (리튬이차전지용 Hollow Silicon/Carbon 음극소재의 전기화학적 성능)

  • Jung, Min Ji;Lee, Jong Dae
    • Applied Chemistry for Engineering
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    • v.27 no.4
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    • pp.444-448
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    • 2016
  • Hollow silicon/carbon (H-Si/C) composites as anode materials for lithium ion batteries were investigated to overcome the large volume expansion. H-Si/C composites were prepared as follows; hollow $SiO_2\;(H-SiO_2)$ was prepared by adding $NaBH_4$ to $SiO_2$ synthesized using $st{\ddot{o}}ber$ method followed by magnesiothermic reduction and carbonization of phenolic resin. The H-Si/C composites were analyzed by XRD, SEM, BET and EDX. To improve the capacity and cycle performance, the electrochemical characteristics of H-Si/C composites synthesized with various $NaBH_4$ contents were investigated by charge/discharge, cycle, cyclic voltammetry and impedance tests. The coin cell using H-Si/C composite ($SiO_2:NaBH_4=1:1$ in weight) in the electrolyte of $LiPF_6$ dissolved in organic solvents (EC : DMC : EMC = 1 : 1 : 1 vol%) has better capacity (1459 mAh/g) than those of other composition coin cells. It is found that the coin cell ($SiO_2:NaBH_4=1:1$ in weight) has an excellent capacity retention from 2nd cycle to 40th cycle.

Ultrasound-Aided Monolayer Assembly of Spherical Silica Nanobeads (초음파 방법을 이용한 실리카 나노비드의 단층 정렬에 관한 연구)

  • Yoon, Sang-Hee;Yoon, Seo Young;Lee, Jin Seok
    • Journal of the Korean Vacuum Society
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    • v.22 no.6
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    • pp.298-305
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    • 2013
  • Uniform silica nanobeads were synthesized by St$\ddot{o}$ber method and assembled in the form of monolayer on glass substrate using sonication method. Before the assembly of silica nanobeads, glass substrates were treated with molecular linkers, such as CP-TMS and PEI, and nanobeads were dispersed in toluene. In attachment test, SO (sonication without stacking) method and SS (sonnication with stacking) method was used and sonication time was controled. After the experiment, microbalance was use to measure deviation between before and after the attachment experiment then calculate percent of coverage. Minutely observe with SEM (Scanning Electron Microscopy) then select the most close-packed and monolayer assembled cover glass and calculate DOC (Degree of Coverage). In SO method, DOC increased very sharply and reach over 140 percent point, also got lots of multi-layer region. On the other hand, in SS method DOC increased slower than SO method but more close-packed and monolayer assembled.

Electrochemical Characteristics of Porous Silicon/Carbon Composite Anode Using Spherical Nano Silica (구형 나노 실리카를 사용한 다공성 실리콘/탄소 음극소재의 전기화학적 특성)

  • Lee, Ho Yong;Lee, Jong Dae
    • Korean Chemical Engineering Research
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    • v.54 no.4
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    • pp.459-464
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    • 2016
  • In this study, the electrochemical characteristics of porous silicon/carbon composite anode were investigated to improve the cycle stability and rate performance in lithium ion batteries. In this study, the effect of TEOS and $NH_3$ concentration, mixing speed and temperature on particle size of nano silica was investigated using $St{\ddot{o}}ber$ method. Nano porous Si/C composites were prepared by the fabrication processes including the synthesis of nano $SiO_2$, magnesiothermic reduction of nano $SiO_2$ to obtain nano porous Si by HCl etching, and carbonization of phenolic resin. Also the electrochemical performances of nano porous Si/C composites as the anode were performed by constant current charge/discharge test, cyclic voltammetry and impedance tests in the electrolyte of $LiPF_6$ dissolved inorganic solvents (EC:DMC:EMC=1:1:1vol%). It is found that the coin cell using nano porous Si/C composite has the capacity of 2,006 mAh/g and the capacity retention ratio was 55.4% after 40 cycle.

The Distance-Dependent Fluorescence Enhancement Phenomena in Uniform Size Ag@SiO2@SiO2(dye) Nanocomposites

  • Arifin, Eric;Lee, Jin-Kyu
    • Bulletin of the Korean Chemical Society
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    • v.34 no.2
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    • pp.539-544
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    • 2013
  • $Ag@SiO_2@SiO_2$(FITC) nanocomposites were prepared by the simple polyol process and St$\ddot{o}$ber method. Fluorescence enhancement of fluorescein moiety (fluorescein isothiocyanate, FITC) was investigated in the presence of silver nanoparticles in $Ag@SiO_2@SiO_2$(FITC) system with varying thickness (X nm) of first silica shell. Maximum enhancement factor of 4.3 fold was achieved in $Ag@SiO_2@SiO_2$(FITC) structure with the first silica shell thickness of 8 nm and the average separation distance of 11 nm between the surface of silver nanoparticle and fluorescein moiety. The enhancement is believed to be originated from increased excitation rate of fluorescein moiety due to concentrated local electromagnetic field which was improved by interaction of light with silver nanoparticles.

Preparation of silica-coated gadolinium compound particle colloid solution and its application in imaging

  • Kobayashi, Yoshio;Morimoto, Hikaru;Nakagawa, Tomohiko;Gonda, Kohsuke;Ohuchi, Noriaki
    • Advances in nano research
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    • v.1 no.3
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    • pp.159-169
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    • 2013
  • A preparation method for gadolinium compound (GdC) nanoparticles coated with silica ($GdC/SiO_2$) is proposed. GdC nanoparticles were prepared with a homogeneous precipitation method at $80^{\circ}C$ using $1.0{\times}10^{-3}$ M $Gd(NO_3)_3$, 0.5 M urea and $0-3.0{\times}10^{-4}$ M ethylenediarinnetetraacetic acid disodium salt dihydrate (ETDA) in water. As a result of preparation at various EDTA concentrations, GdC nanoparticles with a size as small as $40.5{\pm}6.2$ nm, which were colloidally stable, were prepared at an EDTA concentration of $2.0{\times}10^{-4}$ M. Silica-coating of the GdC nanoparticles was performed by a St$\ddot{o}$ber method at $35^{\circ}C$ using $1.0-10.0{\times}10^{-3}$ M tetraethylorthosilicate (TEOS), 11 M $H_2O$ and $1.5{\times}10^{-3}$ M NaOH in ethanol in the presence of $1.0{\times}10^{-3}$ M GdC nanoparticles. Performance of preparation at various TEOS concentrations resulted in production of $GdC/SiO_2$ particles with an average size of $106.1{\pm}11.2$ nm at a TEOS concentration of $5.0{\times}10^{-3}$ M. The gadolinium (Gd) concentration of $1.0{\times}10^{-3}$ M in the as-prepared $GdC/SiO_2$ particle colloid solution was increased up to a Gd concentration of 0.2 M by concentrating with centrifugation. The core-shell structure of $GdC/SiO_2$ particles was undamaged, and the colloid solution was still colloidally stable, even after the concentrating process. The concentrated $GdC/SiO_2$ colloid solution showed images of X-ray and magnetic resonance with contrast as high as commercial Gd complex contrast agents.

Synthesis of Size Controlled Spherical Silica Nanoparticles via Sol-Gel Process within Hydrophilic Solvent

  • Kim, Tae Gyun;An, Gye Seok;Han, Jin Soon;Hur, Jae Uk;Park, Bong Geun;Choi, Sung-Churl
    • Journal of the Korean Ceramic Society
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    • v.54 no.1
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    • pp.49-54
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    • 2017
  • In this study, based on hydrolysis and condensation via $St{\ddot{o}}ber$ process of sol-gel method, synthesis of mono-dispersed silica nanoparticles was carried out with hydrophilic solvent. This operation was expected to be a more simplified process than that with organic solvent. Based on the sol-gel method, which involves simply controlling the particle size, the particle size of the synthesized silica specimens were ranged from 30 to 300 nm by controlling the composition of tetraethylorthosilicate (TEOS), DI water and ammonia solution, and by varying the stirring speeds while maintaining a fixed amount of ethanol. Increasing the content of DI water and decreasing the content of ammonia caused the particle size to decrease, while controlling the stirring speed at a high level of RPMs enabled a decrease of the particle size. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR) were utilized to investigate the success factors for synthesizing process; Field emission scanning electron microscopy (FE-SEM) was used to study the effects of the size and morphology of the synthesized particles. To analyze the dispersion properties, zeta potential and particle size distribution (PSD) analyses were utilized.

Electrochemical Characteristics of Silicon/Carbon Anode Materials using Petroleum Pitch (석유계 피치를 사용한 실리콘/탄소 음극소재의 전기화학적 특성)

  • Lee, Su Hyeon;Lee, Jong Dae
    • Korean Chemical Engineering Research
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    • v.56 no.4
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    • pp.561-567
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    • 2018
  • In this study, the electrochemical characteristics of Silicon/Carbon anode materials were analyzed to improve the cycle stability of silicon as an anode materials of lithium ion battery. Porous silicon was prepared from TEOS by the $st{\ddot{o}}ber$ method and the magnesiothermic reduction method. Silicon/Carbon anode materials were synthesized by varying the mass ratio between porous silicon and pitch. Physical properties of the prepared Silicon/Carbon anode materials were analyzed by XRD and TGA. Also the electrochemical performances of Silicon/Carbon anode materials were investigated by constant current charge/discharge, rate performance, cyclic voltammetry and electrochemical impedance tests in the electrolyte of $LiPF_6$ dissolved in organic solvents (EC : DEC = 1 : 1 vol%). The Silicon/Carbon anode composite (silicon : carbon = 5 : 95 in weight) has better capacity (453 mAh/g) than those of other composition cells. The cycle performance has an excellent capacity retention from 2nd cycle to 30th cycle.

Selective Pattern Growth of Silica Nanoparticles by Surface Functionalization of Substrates (기판 표면 기능화에 의한 실리카 나노입자의 선택적 패턴 성장)

  • Kim, Ki-Chul
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.21 no.4
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    • pp.20-25
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    • 2020
  • As nanoscience and nanotechnology advance, techniques for selective pattern growth have attracted significant attention. Silica nanoparticles (NPs) are used as a promising nanomaterials for bio-labeling, bio-imaging, and bio-sensing. In this study, silica NPs were synthesized by a sol-gel process using a modified Stöber method. In addition, the selective pattern growth of silica NPs was achieved by the surface functionalization of the substrate using a micro-contact printing technique of a hydrophobic treatment. The particle size of the as-synthesized silica NPs and morphology of selective pattern growth of silica NPs were characterized by FE-SEM. The contact angle by surface functionalization of the substrate was investigated using a contact angle analyzer. As a result, silica NPs were not observed on the hydrophobic surface of the OTS solution treatment, which was coated by spin coating. In contrast, the silica NPs were well coated on the hydrophilic surface after the KOH solution treatment. FE-SEM confirmed the selective pattern growth of silica NPs on a hydrophilic surface, which was functionalized using the micro-contact printing technique. If the characteristics of the selective pattern growth of silica NPs can be applied to dye-doped silica NPs, they will find applications in the bio imaging, and bio sensing fields.