• Korean Journal of Chemical Engineering
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• v.35 no.11
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• pp.2207-2219
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• 2018

Activated carbon (AC) was synthesized from Phoenix dactylifera stones and then modified by $CoFe_2O_4$ magnetic nanocomposite for use as a Cr(VI) adsorbent. Both $AC/CoFe_2O_4$ composite and AC were fully characterized by FTIR, SEM, XRD, TEM, TGA, and VSM techniques. Based on the surface analyses, the addition of $CoFe_2O_4$ nanoparticles had a significant effect on the thermal stability and crystalline structure of AC. Factors affecting chromium removal efficiency like pH, dosage, contact time, temperature, and initial Cr(VI) concentration were investigated. The best pH was found 2 and 3 for Cr adsorption by AC and $AC/CoFe_2O_4$ composite, respectively. The presence of ion sulfate had a greater effect on the chromium sorption efficiency than nitrate and chlorine ions. The results illustrated that both adsorbents can be used up to seven times to adsorb chromium. The adsorption process was examined by three isothermal models, and Freundlich was chosen as the best one. The experimental data were well fitted by pseudo-second-order kinetic model. The half-life ($t_{1/2}$) of hexavalent chromium using AC and $AC/CoFe_2O_4$ magnetic composite was obtained as 5.18 min and 1.52 min, respectively. Cr(VI) adsorption by AC and $AC/CoFe_2O_4$ magnetic composite was spontaneous and exothermic. In general, our study showed that the composition of $CoFe_2O_4$ magnetic nanoparticles with AC can increase the adsorption capacity of AC from 36 mg/L to 70 mg/L.

• Bulletin of the Korean Chemical Society
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• v.25 no.2
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• pp.182-184
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• 2004

Fine $La_{2/3}Ca_{1/3}MnO_3$ nanocrystalline powders have been successfully prepared by modified citrate pyrolysis process. The obtained LCMO nanoscale grains have a mean particle size of about 30 nm under optimal treatment conditions. The particle size can be controlled by adjusting processing parameters, such as treatment temperature and calcination time. X-ray diffraction, SEM and magnetoresistance effect were employed to study the crystal structure, morphology and magnetic property of these nanosized powders. A novel MR effect (MR > 45% (0 K < T < 340 K)) at room temperature has been found.

• Proceedings of the Korean Magnestics Society Conference
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• 2012.11a
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• pp.104-105
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• 2012

The temperature dependence of the effective magnetic anisotropy constant K(T) of ferrite nanoparticles is obtained based on the measurements of SQUID magnetometry. For this end, a very simple but intuitive and direct method for determining the temperature dependence of anisotropy constant K(T) in nanoparticles is introduced in this study. The anisotropy constant at a given temperature is determined by associating the particle size distribution f(r) with the anisotropy energy barrier distribution $f_A(T)$. In order to estimate the particle size distribution f(r), the first quadrant part of the hysteresis loop is fitted to the classical Langevin function weight-averaged with the log?normal distribution, slightly modified from the original Chantrell's distribution function. In order to get an anisotropy energy barrier distribution $f_A(T)$, the temperature dependence of magnetization decay $M_{TD}$ of the sample is measured. For this measurement, the sample is cooled from room temperature to 5 K in a magnetic field of 100 G. Then the applied field is turned off and the remanent magnetization is measured on stepwise increasing the temperature. And the energy barrier distribution $f_A(T)$ is obtained by differentiating the magnetization decay curve at any temperature. It decreases with increasing temperature and finally vanishes when all the particles in the sample are unblocked. As a next step, a relation between r and $T_B$ is determined from the particle size distribution f(r) and the anisotropy energy barrier distribution $f_A(T)$. Under the simple assumption that the superparamagnetic fraction of cumulative area in particle size distribution at a temperature is equal to the fraction of anisotropy energy barrier overcome at that temperature in the anisotropy energy barrier distribution, we can get a relation between r and $T_B$, from which the temperature dependence of the magnetic anisotropy constant was determined, as is represented in the inset of Fig. 1. Substituting the values of r and $T_B$ into the $N{\acute{e}}el$-Arrhenius equation with the attempt time fixed to $10^{-9}s$ and measuring time being 100 s which is suitable for conventional magnetic measurement, the anisotropy constant K(T) is estimated as a function of temperature (Fig. 1). As an example, the resultant effective magnetic anisotropy constant K(T) of manganese ferrite decreases with increasing temperature from $8.5{\times}10^4J/m^3$ at 5 K to $0.35{\times}10^4J/m^3$ at 125 K. The reported value for K in the literatures is $0.25{\times}10^4J/m^3$. The anisotropy constant at low temperature region is far more than one order of magnitude larger than that at 125 K, indicative of the effects of inter?particle interaction, which is more pronounced for smaller particles.

• Polymer(Korea)
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• v.36 no.3
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• pp.372-379
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• 2012

In this study, we treated silica nanoparticles with bis[3-(trimethoxysilyl)propyl]amine (BTMA) silane coupling agent to modify their surfaces. We investigated the effects of BTMA hydrolysis time, BTMA concentration and BTMA treatment time on the degree of silanization reaction of silica nanoparticles. We used Fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and solid state cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to obtain quantitative data. We found the decrease of isolated Si-OH peak intensity at 3747 $cm^{-1}$ and the increase of $-CH_2 $stretching and bending peaks with increasing hydrolysis time, concentration and treatment time of BTMA. EA analysis results also supported this trend. We found a strong effect of BTMA concentration on the degree of silanization of the silica particles, but weak effects of the hydrolysis time and the treatment time.

• Polymer(Korea)
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• v.36 no.5
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• pp.668-676
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• 2012

In this study, we modified silica nanoparticles with bis[3-(trimethoxysilyl)propyl]amine (BTMA) silane coupling agent to introduce secondary amino groups on the silica surface. After modification of silica, we investigated effects of different types of (meth)acrylate group containing monomers on the Michael addition reaction to introduce reactive (meth)acrylate groups on the BTMA modified silica surface. We used two kinds of (meth)acrylate monomers, trimethylolpropane ethoxylate triacrylate (TMPET) which has three identical acrylate groups, and 3-(acryloyloxy)-2-hydroxypropyl methacrylate (AHM) which has one acrylate and one methacrylate group. We used fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and solid state cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to understand reactions between NH groups on the silica surface with (meth)acrylate groups of TMPET and AHM monomers. We found almost complete Michael addition reaction between all three acrylate groups of TMPET with NH groups on the BTMA modified silica. But, for the AHM treatment of BTMA modified silica, we found Michael addition reaction occurred only between acrylate groups of AHM and NH groups of silica surface, not between methacrylate groups of AHM and NH groups of BTMA modified silica surface.

• Korean Chemical Engineering Research
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• v.49 no.2
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• pp.181-186
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• 2011

In this study, we used 3-(trimethoxysilyl)propylmethacrylate(MPS) silane coupling agent for surface modification of silica nanoparticles. We studied effects of reaction conditions such as solvent pH, MPS hydrolysis time, reaction time, and molar ratio of MPS to Si-OH groups on silica nanoparticle surfaces, on the surface modification reactions of silica nanoparticles. Fourier Transform Infrared Spectroscopy(FTIR), Elemental Analysis(EA) and solid state crosspolarization magic angle spinning(CP/MAS) Nuclear Magnetic Resonance Spectroscopy(NMR) techniques were used to determine the type and the degree of surface modification. We found MPS reacts preferentially with Si-OH groups of the silica nanoparticles as monomeric form at solvent pH = 4.5. But increasing hydrolysis time of MPS from 30 mins to 90 mins, and molar ratio of MPS to Si-OH groups on silica nanoparticle surfaces, we found that MPS reacts preferentially with Si-OH groups of the silica nanoparticles as oligomeric form.

• Journal of Microbiology and Biotechnology
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• v.29 no.6
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• pp.913-922
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• 2019

Magnetic $Ni_{0.7}Co_{0.3}Fe_2O_4$ nanoparticles that were prepared via the rapid combustion process were functionalized and modified to obtain magnetic $Ni_{0.7}Co_{0.3}Fe_2O_4@SiO_2-CHO$ nanocomposites, on which penicillin G acylase (PGA) was covalently immobilized. Selections of immobilization concentration and time of fixation were explored. Catalytic performance of immobilized PGA was characterized. The free PGA had greatest activity at pH 8.0 and $45^{\circ}C$ while immobilized PGA's activities peaked at pH 7.5 and $45^{\circ}C$. Immobilized PGA had better thermal stability than free PGA at the range of $30-50^{\circ}C$ for different time intervals. The activity of free PGA would be 0 and that of immobilized PGA still retained some activities at $60^{\circ}C$ after 2 h. $V_{max}$ and $K_m$ of immobilized PGA were 1.55 mol/min and 0.15 mol/l, respectively. Free PGA's $V_{max}$ and $K_m$ separately were 0.74 mol/min and 0.028 mol/l. Immobilized PGA displayed more than 50% activity after 10 successive cycles. We concluded that immobilized PGA with magnetic $Ni_{0.7}Co_{0.3}Fe_2O_4@SiO_2-CHO$ nanocomposites could become a novel example for the immobilization of other amidohydrolases.

• Polymer(Korea)
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• v.37 no.3
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• pp.308-315
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• 2013

In this study, we performed surface modification of silica nanoparticles with bis[3-(triethoxysilylpropyl)]tetrasulfide (TESPT) silane coupling agent to study the effects of treatment temperature, treatment time, and amount of TESPT used on the silanization degree with Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), elemental analysis (EA) and solid state $^{13}C$ and $^{29}Si$ cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR). We found peak area of isolated silanol groups at $3747cm^{-1}$ decreased, but peak area of $-CH_2$ asymmetric stretching of TESPT at $2938cm^{-1}$ increased with the amount of TESPT from FTIR measurements. We also used universal testing machine (UTM) to study mechanical properties of styrene butadiene rubber (SBR) nanocomposites with 20 phr (parts per hundred of rubber) of pristine and TESPT modified silicas, respectively. The tensile strength and 100% modulus of modified silica/SBR nanocomposite were enhanced from 5.65 to 9.38MPa, from 1.62 to 2.73 MPa, respectively, compared to those of pristine silica/SBR nanocomposite.

• Polymer(Korea)
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• v.38 no.2
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• pp.257-264
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• 2014

In this study, we modified silica nanoparticles with bis[3-(trimethoxysilyl)propyl]ethylenediamine (BTPED) silane coupling agent, which has two secondary amino groups in a molecule, to introduce amino groups on the silica surface. After modification of silica, we used acrylate group containing 3-(acryloyloxy)-2-hydroxypropyl methacrylate (AHM) to introduce polymerizable methacrylate groups by Michael addition reaction. We used Fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and liquid and solid state cross polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to understand the reactions between N-H groups of BTPED modified silica surface and acrylate groups of AHM monomer. We confirmed Michael addition reaction between BTPED modified silica and AHM completed in 2 hr reaction time. We also found increased methacrylate group introduction with increase of mol ratio of the acrylate group of AHM to N-H group of BTPED modified silica by increase of C=O peak area of measured FTIR spectra. These results were also supported by EA and solid state $^{13}C$ and $^{29}Si$ NMR results.

• Proceedings of the Materials Research Society of Korea Conference
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• 2009.11a
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• pp.6.2-6.2
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• 2009

Nanostructured materials arecurrently receiving much attention because of their unique structural andphysical properties. Research has been stimulated by the envisagedapplications for this new class of materials in electronics, optics, catalysisand magnetic storage since the properties derived from nanometer-scalematerials are not present in either isolated molecules or micrometer-scalesolids. This study presents the experimental results derived fromthe various functional materials processed in nano-scale using pulsed laserablation, since those materials exhibit new physical phenomena caused by thereduction dimensionality. This presentation consists of three mainparts to consider in pulsed laser ablation (PLA) technique; first nanocrystallinefilms, second, nanocolloidal particles in liquid, and third, nanocoating fororganic/inorganic hybridization. Firstly, nanocrystalline films weresynthesized by pulsed laser deposition at various Ar gas pressures withoutsubstrate heating and/or post annealing treatments. From the controlof processng parameters, nanocystalline films of complex oxides and non-oxidematerials have been successfully fabricated. The excellentcapability of pulsed laser ablation for reactive deposition and its ability totransfer the original stoichiometry of the bulk target to the deposited filmsmakes it suitable for the fabrication of various functionalmaterials. Then, pulsed laser ablation in liquid has attracted muchattention as a new technique to prepare nanocolloidal particles. Inthis work, we represent a novel synthetic approach to directly producehighly-dispersed fluorescent colloidal nanoparticles using the PLA from ceramicbulk target in liquid phase without any surfactant. Furthermore, novel methodbased on simultaneous motion tracking of several individual nanoparticles isproposed for the convenient determination of nanoparticle sizedistributions. Finally, we report that the GaAs nanocrystals issynthesized successfully on the surface of PMMA (polymethylmethacrylate)microspheres by modified PLD technique using a particle fluidizationunit. The characteristics of the laser deposited GaAs nanocrytalswere then investigated. It should be noted that this is the first successfultrial to apply the PLD process nanocrystals on spherical polymermatrices. The present process is found to be a promising method fororganic/inorganic hybridization.