• Title/Summary/Keyword: Infrared microscopy

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A Deep Investigation of the Thermal Decomposition Process of Supported Silver Catalysts

  • Jiang, Jun;Xu, Tianhao;Li, Yaping;Lei, Xiaodong;Zhang, Hui;Evans, D.G.;Sun, Xiaoming;Duan, Xue
    • Bulletin of the Korean Chemical Society
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    • v.35 no.6
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    • pp.1832-1836
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    • 2014
  • A deep understanding of the metallic silver catalysts formation process on oxide support and the formation mechanism is of great scientific and practical meaning for exploring better catalyst preparing procedures. Herein the thermal decomposition process of supported silver catalyst with silver oxalate as the silver precursor in the presence of ethylenediamine and ethanolamine is carefully investigated by employing a variety of characterization techniques including thermal analysis, in situ diffuse reflectance infrared Fourier transform spectroscopy, scanning electron microscopy, and X-ray diffraction. The formation mechanism of supported silver particles was revealed. Results showed that formation of metallic silver begins at about $100^{\circ}C$ and activation process is essentially complete below $145^{\circ}C$. Formation of silver was accompanied by decomposition of oxalate group and removal of organic amines. Catalytic performance tests using the epoxidation of ethylene as a probe reaction showed that rapid activation (for 5 minutes) at a relatively low temperature ($170^{\circ}C$) afforded materials with optimum catalytic performance, since higher activation temperatures and/or longer activation times resulted in sintering of the silver particles.

Hydrothermal Synthesis of LaCO3OH and Ln3+-doped LaCO3OH Powders under Ambient Pressure and Their Transformation to La2O2CO3 and La2O3

  • Lee, Min-Ho;Jung, Woo-Sik
    • Bulletin of the Korean Chemical Society
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    • v.34 no.12
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    • pp.3609-3614
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    • 2013
  • Orthorhombic and hexagonal lanthanum(III) hydroxycarbonate ($LaCO_3OH$) and $Ln^{3+}$-doped $LaCO_3OH$ ($LaCO_3OH:Ln^{3+}$, where Ln = Ce, Eu, Tb, and Ho) powders were prepared by a hydrothermal reaction under ambient pressure and characterized by thermogravimetry, powder X-ray diffraction, infrared and luminescence spectroscopy, and field-emission scanning electron microscopy. The polymorph of $LaCO_3OH$ depended on the reaction temperature, inorganic salt additive, species of $Ln^{3+}$ dopant, and solvent. The calcination of orthorhombic $LaCO_3OH:Ln^{3+}$ (2 mol %) powers at $600^{\circ}C$ yielded a mixture of hexagonal and monoclinic $La_2O_2CO_3:Ln^{3+}$ powders. The relative quantity of the latter increased with decreasing ionic radius of the $Ln^{3+}$ dopant ion and increasing doping concentrations. On the other hand, the calcination of hexagonal $LaCO_3OH:Ln^{3+}$ (2 mol %) powders at $600^{\circ}C$ resulted in a pure hexagonal $La_2O_2CO_3:Ln^{3+}$ powder, regardless of the species of $Ln^{3+}$ ions (Ln = Ce, Eu, and Tb). The luminescence spectra of $LaCO_3OH:Ln^{3+}$ and $La_2O_2CO_3:Ln^{3+}$ were measured to examine the effect of their polymorph on the spectra.

Bioactivity of $CaO-P_2O_5-SiO_2$ Glasses ($CaO-P_2O_5-SiO_2$계 유리의 생체활성)

  • 조정식;김철영
    • Journal of the Korean Ceramic Society
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    • v.30 no.6
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    • pp.433-440
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    • 1993
  • The bioactivity of glasses in the CaO-SiO2 system and CaO-P2O5-SiO2 system with less than 10mol% of P2O5 was investigated by in vitro test in simulated body flood(SBF). The formation of Ca.P film and hydroxyapatite on the surface of glasses after in vitro test was analysed by X-ray photoelectron spectoscopy (XPS), fourier transform infrared reflection spectroscopy (FT-IRRS), energy dispersive X-ray spectroscopy (EDS), and scanning electron microscopy (SEM) observation. In the early stage of Ca.P film formation after in vitro test for CaO-SiO2 and CaO-P2O5-SiO2 glasses, the rate of Ca.P film formation on the surface of the glasses was dependent of structural parameter (Y) evaluated from the glass composition. First, in the case of the glasses having Y value below 2, Ca.P film and SiO2-rich layer were formed simultaneously, and there were no differences of the rate of Ca.P film formation in terms of the Y values. Second, in the case of the glasses having Y value above 2, the SiO2-rich layer was formed, and then Ca.P.Si mixed layer was formed in the silica gel structure of the SiO2-rich layer, and finally the Ca.P film on the surface of SiO2-rich layer. The rate of Ca.P film formation delayed as the Y values increased. The rate of hydroxyapatite formation of glasses (the rate of transformation from Ca.P film to hydroxyapatite) seems to be propotional to the rate of Ca.P film formation and Y value. The rate of hydroxyapatite formation of glasses belonging to the second group was delayed as structural parameter increased, and the hydroxyapatite crystal showed spherical growth in the early reaction stage, and then showed silkworm-like linear growth as the reaction time increased.

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A Study of Upgrading Real Biogas via CO2 Precipitation Route Under Indian Scenario

  • Gehlaut, Avneesh Kumar;Gaur, Ankur;Hasan, Shabih Ul;Park, Jin-Won
    • Korean Chemical Engineering Research
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    • v.56 no.3
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    • pp.381-387
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    • 2018
  • Our study focuses on upgrading real biogas obtained under Indian scenario using carbon capture and utilization (CCU) technology to remove carbon dioxide ($CO_2$) and utilize it by forming metal carbonate. Amines such as monoethanolamine (MEA), diethanolamine (DEA), and sodium hydroxide (NaOH) were used to rapidly convert gaseous $CO_2$ to aqueous $CO_2$, and $BaCl_2$ was used as an additive to react with the aqueous $CO_2$ and rapidly precipitating the aqueous $CO_2$. All experiments were conducted at $25^{\circ}C$ and 1 atm. We analyzed the characteristics of the $BaCO_3$ precipitates using X-ray diffractometry (XRD), scanning electron microscopy - Energy dispersive spectroscopy (SEM-EDS) and Fourier-transform infrared spectroscopy (FT-IR) analyses. The precipitates exhibited witherite morphology confirmed by the XRD results, and FT-IR confirmed that the metal salt formed was $BaCO_3$, and EDS showed that there were no traces of impurities present in it. The quantity of the $BaCO_3$ was larger when formed with DEA. Also, a comparison was done with a previous study of ours conducted in Korean conditions. Finally, we observed that the carbonate obtained using real biogas showed similar properties to carbonates available in the market. An economic analysis was done to show the cost effectiveness of the method employed by us.

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.

A Review of SERS for Biomaterials Analysis Using Metal Nanoparticles (바이오 물질 분석을 위한 금속 나노입자를 이용한 SERS 분석 연구동향)

  • Jang, Eue-Soon
    • Ceramist
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    • v.22 no.3
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    • pp.281-300
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    • 2019
  • Surface enhanced Raman scattering (SERS) was first discovered in 1974 by an unexpected Raman signal increase from Pyridine adsorbed on rough Ag electrode surfaces by the M. Fleishmann group. M. Moskovits group suggested that this phenomenon could be caused by surface plasmon resonance (SPR), which is a collective oscillation of free electrons at the surface of metal nanostructures by an external light source. After about 40 years, the SERS study has attracted great attention as a biomolecule analysis technology, and more than 2500 new papers and 500 review papers related to SERS topic have been published each year in recently. The advantages of biomaterials analysis using SERS are as follows; ① Molecular level analysis is possible based on unique fingerprint information of biomolecule, ② There is no photo-bleaching effect of the Raman reporters, allowing long-term monitoring of biomaterials compared to fluorescence microscopy, ③ SERS peak bandwidth is approximately 10 to 100 times narrower than fluorescence emission from organic phosphor or quantum dot, resulting in higher analysis accuracy, ④ Single excitation wavelength allows analysis of various biomaterials, ⑤ By utilizing near-infrared (NIR) SERS-activated nanostructures and NIR excitation lasers, auto-fluorescence noise in the visible wavelength range can be avoided from in vivo experiment and light damage in living cells can be minimized compared to visible lasers, ⑥ The weak Raman signal of the water molecule makes it easy to analyze biomaterials in aqueous solutions. For this reason, SERS is attracting attention as a next-generation non-invasive medical diagnostic device as well as substance analysis. In this review, the principles of SERS and various biomaterial analysis principles using SERS analysis will be introduced through recent research papers.

Synthesis and Characterization of Phosphoric Acid-doped Poly (2,5-benzimidazole) Membrane for High Temperature Polymer Electrolyte Membrane Fuel Cells (고온 고분자 연료전지용 인산 도핑 폴리(2,5-벤지이미다졸) 막의 제조 및 특성)

  • Nguyen, Thi Xuan Hien;Mishra, Ananta Kumar;Choi, Ji-Sun;Kim, Nam-Hoon;Lee, Joong-Hee
    • Transactions of the Korean hydrogen and new energy society
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    • v.23 no.1
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    • pp.26-33
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    • 2012
  • Phosphoric acid-doped poly (2,5-benzimidazole) (DABPBI) was prepared by condensation polymerization of 3,4-diaminobenzoic acid for high temperature proton electrolyte membrane fuel cells. The membranes were casted directly using a hot-press unit and characterized by fourier transform infrared spectroscopy, thermogravimetric analysis, conductivity measurement, scanning electron microscopy and tensile test. The proton conductivities of DABPBI are observed to be 0.062 and 0.018 $S{\cdot}cm^{-1}$ under 30 and 1% relative humidity, respectively at a temperature of $120^{\circ}C$ which is appreciably higher than that of Nafion 115 under similar conditions. The DABPBI membrane has demonstrated excellent thermo- mechanical properties and proton conductivity suggesting its suitability as a high temperature membrane.

Enhanced electrocapacitive performance and high power density of polypyrrole/graphene oxide nanocomposites prepared at reduced temperature

  • Mudila, Harish;Joshi, Varsha;Rana, Sweta;Zaidi, Mohmd. Ghulam Haider;Alam, Sarfaraz
    • Carbon letters
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    • v.15 no.3
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    • pp.171-179
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    • 2014
  • An attempt was made to investigate the effect of the preparation temperature on the electrocapacitive performance of polypyrrole (PPY)/graphene oxide (GO) nanocomposites (PNCs). For this purpose, a series of PNCs were prepared at various temperatures by the cetyltrimethylammonium bromide-assisted dilute-solution polymerization of pyrrole in presence of GO (wt%) ranging from 1.0 to 4.0 with ferric chloride as an oxidant. The formation of the PNCs was ascertained through Fourier-transform infrared spectrometry, X-ray diffraction spectra, scanning electron microscopy and simultaneous thermogravimetric-differential scanning calorimetry. The electrocapacitive performance of the electrodes derived from sulphonated polysulphone-bound PNCs was evaluated through cyclic voltammetry with reference to Ag/AgCl at a scan rate (V/s) ranging from 0.2 and 0.001 in potassium hydroxide (1.0 M). The incorporation of GO into the PPY matrix at a reduced temperature has a pronounced effect on the electrocapacitive performance of PNCs. Under identical scan rates (0.001 V/s), PNCs prepared at $10{\pm}1^{\circ}C$ render improved specific conductivity (526.33 F/g) and power density (731.19 W/Kg) values compared to those prepared at $30{\pm}1^{\circ}C$ (217.69 F/g, 279.43 W/Kg). PNCs prepared at $10{\pm}1^{\circ}C$ rendered a capacitive retention rate of ~96% during the first 500 cycles. This indicates the excellent cyclic stability of the PNCs prepared at reduced temperatures for supercapacitor applications.

Development of Cobalt Sulfide-graphene Composite for Supercapacitor Applications

  • Jana, Milan;Samanta, Pranab;Murmu, Naresh Chandra;Kim, Nam Hoon;Kuila, Tapas;Lee, Joong Hee
    • Composites Research
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    • v.29 no.4
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    • pp.167-172
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    • 2016
  • $Co_9S_8/reduced$ graphene (CSRG) has been prepared by a facile two step hydrothermal method and used as a supercapacitor electrode material. It is anticipated that the $Co_9S_8$ and reduced graphene oxide (RGO) would serve as a spacer material to each other to stop the agglomeration and simultaneous contribution of electrical double layer capacitance (RGO) and pseudocapacitance ($Co_9S_8$) would provide high electrochemical properties. The chemical analysis has been done by Fourier transform infrared spectroscopy and the morphology is characterised by field emission scanning electron microscopy. CSRG shows a high electrical conductivity of $98S\;m^{-1}$. The symmetric supercapacitor shows a specific capacitance of ${\sim}728F\;g^{-1}$ with a current density of $2A\;g^{-1}$. CSRG also showed an energy density of $25.2Wh\;kg^{-1}$ with a power density of $1000W\;kg^{-1}$.

Characteristics of the Shells and Calcined Powders from the Butter Clam Saxidomus purpuratus and Littleneck Clam Ruditapes philippinarum as a Natural Calcium Resource (천연칼슘소재로서 개조개(Saxidomus purpuratus)와 바지락(Ruditapes philippinarum) 패각 및 소성분말의 특성)

  • Kim, Jin-Soo;Jung, Nam Young;Soo Jang, Jeong;Lee, Hyun Ji;Park, Sung Hwan;Kim, Min Joo;Heu, Min Soo
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.48 no.2
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    • pp.168-177
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    • 2015
  • Shell waste from the butter clam Saxidomus purpuratus and littleneck clam Ruditapes philippinarum is a large by-product of shellfish aquaculture, and it is desirable to convert it into value-added products for industrial applications. In this study, calcium carbonate (CaC) polymorphs from butter clam (BCSP) and littleneck clam (LCSP) shell powders and commercial CaC were characterized using Fourier transmission infrared spectroscopy (FT-IR), X-ray diffraction (XRD), and scanning electron microscopy (SEM). The results revealed that the optimal calcination conditions to eliminate organic substances and improve solubility for both BCSP and LCSP were $800^{\circ}C$ for 8 h in an electrical furnace. Calcination improved the white index of the butter clam (BCCP) and littleneck clam (LCCP) calcined powder compared with shell powders. The calcium content in BCCP (51.1%) was higher than that of LCCP (44.9%) or commercial calcium oxide (CaO, 44.7%). The XRD patterns of BCCP and LCCP were similar to that of CaO. Cubic-like crystals of CaC and irregular crystals of BCCP and LCCP were observed by SEM. The FT-IR and XRD analyses revealed the presence of calcite and aragonite in the BCSP and aragonite in the LCSP, whereas the CaC contained calcite. These results indicate that butter and littleneck clam shells are potential biomass resources for calcium carbonate and calcium oxide.