• 한국재료학회지
• /
• 제21권1호
• /
• pp.67-71
• /
• 2011

La doped CuO-ZnO-$Al_2O_3$ powders are prepared by sol-gel method with aluminum isopropoxide and primary distilled water as precursor and solvent. In this synthesized process, the obtained metal oxides caused the precursor such as copper (II) nitrate hydrate and zinc (II) nitrate hexahydrate were added. To improve the surface areas of La doped CuO-ZnO-$Al_2O_3$ powder, sorbitan (z)-mono-9-octadecenoate (Span 80) was added. The synthesized powder was calcined at various temperatures. The dopant was found to affect the surface area and particle size of the mixed oxide, in conjunction with the calcined temperature. The structural analysis and textual properties of the synthesized powder were measured with an X-ray Diffractometer (XRD), a Field-Emission Scanning Electron Microscope (FE-SEM), Bruner-Emmett-Teller surface analysis (BET), Thermogravimetry-Differential Thermal analysis (TG/DTA), $^{27}Al$ solid state Nuclear Magnetic Resonance (NMR) and transform infrared microspectroscopy (FT-IR). An increase of surface area with Span 80 was observed on La doped CuO-ZnO-$Al_2O_3$ powders from $25m^2$/g to $41m^2$/g.

• 한국지하수토양환경학회지:지하수토양환경
• /
• 제18권5호
• /
• pp.1-6
• /
• 2013

This study was performed to develop a method for quantitative analysis obtaining the amount of calcium carbonate minerals formed when Ca salts biomimetically reacted with carbon dioxide. There were two methods compared; 1) volumetric calcimeter method that determining the amount of released carbon dioxide after calcium carbonate minerals were acidified by 4N HCl and 2) Thermogravimetry-Differential Thermal Analysis (TG-DTA) adopting differential decomposition temperature breaking-up the structural link within calcium carbonate minerals. The comparisons were made by batch experiment (i.e., biocalcification process) along with control (i.e., nominal concentration of $CaCO_3$ prepared). For the control, TG-DTA took a minor root mean square deviation (RMSD) of 1.1~5.9 mg, whereas volumetric calcimeter exposed a greater RMSD of 28.3 mg. For the biocalcification, the amount of $CaCO_3$ was more precisely obtained for TG-DTA rather than that of volumetric calcimeter. It was decided that TG-DTA was more successfully used for quantitative analysis to observe the amount of calcium carbonate minerals derived from biocalcification.

• Nuclear Engineering and Technology
• /
• 제54권10호
• /
• pp.3641-3649
• /
• 2022

A simple solvothermal reaction was used to prepare a 3-aminopropyl-functionalized silica-gel-based adsorbent for adsorbing Pd(II) from the nitric acid solution. Scanning electron microscopy, fourier transform infrared spectroscopy, and thermogravimetry analysis were performed on the as-synthesized adsorbent to demonstrate the successful introduction of Schiff base groups. Batch experiments were used to investigate the effects of contact time, nitric acid concentration, solution temperature, and adsorption capacity. It is worth noting that the prepared adsorbent exhibited a higher affinity toward Pd(II) with the uptake approximately 100% even in a 2 M HNO₃ solution. At an equilibrium time of 5 h, the maximum adsorption capacity of Pd(II) was estimated to be 0.452 mmol/g. The adsorbed Pd(II) could be completely eluted by dissolving 0.2 M thiourea solution in 0.1 M HNO₃. Using a combination of particle-induced X-ray emission analysis and an X-ray photoelectron spectrometer, the adsorbed Pd was found to be uniformly distributed on the surface of the prepared adsorbent and the existing species were Pd(II) and zero-valent Pd(0). Due to the desirable performances, facile preparation method, and abundant raw material source, the prepared adsorbent demonstrated a high application potential in the recovery of Pd(II) from simulated high-level liquid waste treatment.

• Journal of Microbiology and Biotechnology
• /
• 제18권3호
• /
• pp.477-482
• /
• 2008

A variety of bacterial strains were isolated from waste disposal sites of Uttaranchal, India, and some from artificially developed soil beds containing maleic anhydride, glucose, and small pieces of polyethylene. Primary screening of isolates was done based on their ability to utilize high- and low-density polyethylenes (HDPE/LDPE) as a primary carbon source. Thereafter, a consortium was developed using potential strains. Furthermore, a biodegradation assay was carried out in 500-ml flasks containing minimal broth (250ml) and HDPE/LDPE at 5mg/ml concentration. After incubation for two weeks, degraded samples were recovered through filtration and subsequent evaporation. Fourier transform infrared spectroscopy (FTIR) and simultaneous thermogravimetric-differential thermogravimetry-differential thermal analysis (TG-DTG-DTA) were used to analyze these samples. Results showed that consortium-treated HDPE (considered to be more inert relative to LDPE) was degraded to a greater extent (22.41% weight loss) in comparison with LDPE (21.70% weight loss), whereas, in the case of untreated samples, weight loss was more for LDPE than HDPE (4.5% and 2.5%, respectively) at $400^{\circ}C$. Therefore, this study suggests that polyethylene could be degraded by utilizing microbial consortia in an eco-friendly manner.

• Applied Microscopy
• /
• 제47권3호
• /
• pp.110-120
• /
• 2017

Non-isothermal thermogravimetry (TG) measurements on melt-quenched $Bi_xSe_{100-x}$ specimens (x=0, 2.5, 7.5 at%) were made at a heating rate ${\beta}=10^{\circ}C/min$ in the range $T=35^{\circ}C{\sim}950^{\circ}C$. The as-measured TG curves confirm that $Bi_xSe_{100-x}$ samples were thermally stable with minor loss at $T{\leq}400^{\circ}C$ and mass loss starts to decrease up to $600^{\circ}C$, beyond which trivial mass loss was observed. These TG curves were used to estimate molar (Se/Bi)-ratios of $Bi_xSe_{100-x}$ samples, which were not in accordance with initial composition. Shaping features of conversion curves ${\alpha}(T)-T$ of $Bi_xSe_{100-x}$ samples combined with a reliable flow chart were used to reduce kinetic mechanisms that would have caused their thermal mass loss to few nth-order reaction models of the form $f[{\alpha}(T)]{\propto}[1-{\alpha}(T)]^n$ (n=1/2, 2/3, and 1). The constructed ${\alpha}(T)-T$ and $(d{\alpha}(T)/dT)-T$ curves were analyzed using Coats-Redfern (CR) and Achar-Brindley-Sharp (ABS) kinetic formulas on basis of these model functions, but the linearity of attained plots were good in a limited ${\alpha}(T)-region$. The applicability of CR and ABS methods, with model function of kinetic reaction mechanism R0 (n=0), was notable as they gave best linear fits over much broader ${\alpha}(T)-range$.

• 접착 및 계면
• /
• 제7권4호
• /
• pp.32-38
• /
• 2006

A series of organic-inorganic hybrids, PCL/EP/$SiO_2$, involving epoxy resin and triethoxysilane-terminated polycaprolactone elastomer (PCL-TESi) were prepared via polymerization of diglycidyl ether of bisphenol A (DGEBA) with amine curing agent KB-2 and sol-gel process of PCL-TESi. The curing reactions were started from the initially homogeneous mixture of DGEBA, KB-2 and the PCL-TESi. The organicinorganic hybrids containing up to 4.95% (wt) of $SiO_2$ were obtained and characterized by FT-IR, transmission electron microscopy (TEM), differential scanning calorimetry (DSC) and thermogravimetry analysis (TGA). It was experimentally shown that the swelling property in toluene, morphologies and thermal properties of the resulting hybrids were quite dependent on the contents of $SiO_2$. The crosslink network density decreases with increasing of the PCL-TESi. And in TEM, the phase separated morphology of these hybrids was found, which resulted from the coagulation of Si-O-Si networks resulting from $-Si(OC_2H_5)_3$ of PCL-TESi self-curing by hydrolytic silanol condensation, with the advancement of the curing reaction in the modified epoxy resin systems. Meanwhile, the change of the $SiO_2$ content made the morphologies changed from aggregated particles of Si-O-Si in the hybrid to nanocluster of interconnected Si-O-Si particles, then to aggregated Si-O-Si dispersing in the continuous cured epoxy phase again, and last to co-continuous interpenetrating network. The glass transition behavior of the hybrid material was cooperative motion of large chain segments, which were hindered by the inorganic Si-O-Si network. And in TG analysis, the characteristic temperature at 5% of weight loss was evidently increased from $120.5^{\circ}C$ of pure cured epoxy to $277.6^{\circ}C$ of 3.84% (wt) of $SiO_2$ modified epoxy due to the existence of Si-O-Si when PCL-TESi was added in the hybrid.

• 한국재료학회지
• /
• 제20권9호
• /
• pp.472-477
• /
• 2010

$Al_2O_3$ has received wide attention with established use as a catalyst and growing application in structural or functional ceramic materials. On the other hand, the boehmite (AlO(OH)) obtained by sol-gel process has exhibited a decrease in surface area during phase transformation due to a decline in surface active site at high temperature. In this work, $Al_2O_3$-CuO/ZnO (ACZ) and $Al_2O_3$-CuO/CeO (ACC) composite materials were synthesized with aluminum isopropoxide, copper (II) nitrate hemi (pentahydrate), and cerium (III) nitrate hexahydrate or zinc (II) nitrate hexahydrate. Moreover, the Span 80 as the template block copolymer was added to the ACZ/ACC composition to make nano size particles and to keep increasing the surface area. The ACZ/ACC synthesized powders were characterized by Thermogravimetry-Differential Thermal analysis (TG/DTA), X-ray Diffractometer (XRD), Field-Emmision Scanning Electron Microscope (FE-SEM), Bruner-Emmett-Teller (BET) surface analysis and thermal electrical conductivity (ZEM-2:M8/L). An enhancement of surface area with the addition to Span 80 surfactant was observed in the ACZ powders from 105 $m^2$/g to 142 $m^2$/g, and the ACC powders from 103 $m^2$/g to 140 $m^2$/g, respectively.

• Bulletin of the Korean Chemical Society
• /
• 제35권8호
• /
• pp.2257-2262
• /
• 2014

$C_{60}$ is widely investigated because of its unique structure. But its applications in solid propellant seem to be relatively neglected. $C_{60}$ has more outstanding features than carbon black which is widely used as a catalyst ingredient of solid propellant. To combine the advantages of fullerene and lead salts, another good composite in propellant catalysts, we synthesized a kind of fullerene phenylalanine lead salt (FPL) and explored its thermal performances by differential thermal analysis (DTA) and thermogravimetry analysis (TGA). The results show it undergoes four exothermic processes started from 408 K. Combined TGA and X-ray diffractometer (XRD), the decomposition mechanism of FPL was derived by TG-IR and comparing IR spectra of FPL and its residues after burned to $327^{\circ}C$, $376^{\circ}C$ and $424^{\circ}C$, respectively. Effect of FPL on the decomposition characteristic of hexogen (RDX), a type of explosive in propellant, has been investigated using DTA at different heating rate, which shows the decomposition temperatures of the explosive are all reduced by more than 20 K. The corresponding activation energy ($E_a$) is decreased by $30kJ{\cdot}mol^{-1}$. So FPL has potential application as a combustion catalyst in solid propellant.

• 한국재료학회지
• /
• 제23권1호
• /
• pp.31-34
• /
• 2013

Trivalent cerium-ion-doped $Y_3(Al,\;Ga)_5O_{12}$ nanoparticle phosphor nanoparticles were synthesized using the reverse micelle process. The Ce doped $Y_3(Al,\;Ga)_5O_{12}$ particles were obtained from nitrate solutions dispersed in the nanosized aqueous domains of a micro emulsion consisting of cyclohexane as the oil phase and poly(oxyethylene) nonylphenyl ether (Igepal CO-520) as the non-ionic surfactant. The crystallinity, morphology, and thermal properties of the synthesized $Y_3(Al,\;Ga)_5O_{12}:Ce^{3+}$ powders were characterized by thermogravimetry-differential thermal analysis (TGA-DTA), X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), and transmission electron microscopy. The crystallinity, morphology, and chemical states of the ions were characterized; the photo-physical properties were studied by taking absorption, excitation, and emission spectra for various concentrations of cerium. The photo physical properties of the synthesized $Y_3(Al,\;Ga)_5O_{12}:Ce^{3+}$ powders were studied by taking the excitation and emission spectra for various concentrations of cerium. The average particle size of the synthesized YAG powders was below $1{\mu}m$. Excitation spectra of the $Y_3Al_5O_{12}$ and $Y_3Al_{3.97}Ga_{1.03}O_{12}$ samples were 485 nm and 475 nm, respectively. The emission spectra of the $Y_3Al_5O_{12}$ and $Y_3Al_{3.97}Ga_{1.03}O_{12}$ were around 560 nm and 545 nm, respectively. $Y_3(Al,\;Ga)_5O_{12}:Ce^{3+}$ is a red-emitting phosphor; it has a high efficiency for operation under near UV excitation, and may be a promising candidate for photonic applications.

• Bulletin of the Korean Chemical Society
• /
• 제18권9호
• /
• pp.916-922
• /
• 1997

A superconducting phase La2CuO4+δ (Tc=44 K) has been prepared by electrochemical oxidation which allows the oxygen to intercalat into the La2O2 layers. According to the Cu K-edge X-ray absorption near edge structure spectroscopic analysis, the oxidized phase shows an overall spectra shift of about 0.5 eV to a higher energy region compared to the as sintered one with the occurrence of an additional peak corresponding to the transition to the |1s13dn+1L-14pσ1 > final state, indicating the oxidation of CuO2 layer. From the X-ray photoelectron spectroscopic studies, it is found that the binding energy of La 3d5/2 is significantly shifted from 834.3 eV (as sintered La2CuO4) to 833.6 eV (as electrochemically oxidized La2CuO4+δ), implying that the covalency of the (La-O) bond is decreased due to the oxygen intercalation. The O 1s spectra do not provide an evidence of the superoxide or peroxide, but the oxide (O2-) with the contaminated carbonate (CO32-) based on the peaks at 529 eV and 532 eV, respectively, which is clearly confirmed by the Auger spectroscopic analysis. Oxygen contents determined by iodometric titration (δ=0.07) and thermogravimetry (δ=0.09) show good coincidence each other, also giving an evidence for the "O2-" nature of excess oxygen. From the above results, it is concluded that "O2-" appeared as O 1s peak at 528.6 eV is responsible for superconductivity of La2CuO4+δ.