• Title/Summary/Keyword: VIS Spectroscopy Analysis

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Silver (I)- Schiff-base complex intercalated layered double hydroxide with antimicrobial activity

  • Barnabas, Mary Jenisha;Parambadath, Surendran;Nagappan, Saravanan;Chung, Ildoo;Ha, Chang-Sik
    • Advances in nano research
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    • v.10 no.4
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    • pp.373-383
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    • 2021
  • In this work, silver nitrate complexes of sulfanilamide-5-methyl-2-thiophene carboxaldehyde (SMTCA) ligand intercalated Zn/Al-layered double hydroxide [Ag-SMTCA-LDH] were synthesized for the potential application as an antimicrobial system. The SMTCA ligand was synthesized by reacting sulfanilamide and 5-methyl-2-thiophene carboxaldehyde in methanol and further complexation with silver nitrate metal ions [Ag-SMTCA]. The structural analyses of synthesized compounds confirmed an intercalation of Ag-SMTCA into Zn/Al-NO3-LDH by flake/restacking method. SMTCA, Ag-SMTCA and Ag-SMTCA-LDH were characterized by 1H nuclear magnetic resonance (1H NMR) spectroscopy, Fourier-transform infrared (FTIR), ultraviolet-visible (UV-Vis) spectrophotometer, scanning electron microscopy (SEM) and transmission electron microscopy (TEM), X-ray diffraction (XRD), and thermogravimetric analysis (TGA). It was found that Ag-SMTCA-LDH exhibited good antimicrobial activity against both gram-positive (Bacillus subtilis, [B. subtilis], Staphylococcus aures, [S. aureus]) and gram-negative (Escherichia coli, [E. coli], Pseudomonas aeruginosa [P. aeroginosa]) bacteria as well as excellent antioxidant activity.

Synthesis and Characterization of the Layered Type $(C_nH_{2n+1}NH_3)_2PbCl_4$ System

  • Lee, Su Jong;Kim, Gye Ya;O, Eun Ju;Kim, Gyu Hong;Yeo, Cheol Hyeon
    • Bulletin of the Korean Chemical Society
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    • v.21 no.3
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    • pp.317-320
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    • 2000
  • Layered $K_2NiF_4$type ($C_nH_{2n+1}NH_3)_2PbCl_4$(n=6, 8 and 10) system, or alkylammonium tetrachloroplumbate compound, has been synthesized from $PbCl_2$ and $C_nH_{2n+1}NH_3Cl$ solutions under argon ambient pressure for 12hrs at $90^{\circ}C$. The crystal structure of the compound has been analyzed using X-ray powder diffaction in the range of $5^{\circ}{\leq}2{\theta}{\leq}55^{\circ}$, and all samples assigned to an orthorhombic system. Local distances of the Pb-Cl bond have been determined by Pb $L_{III}$-edge extended X-ray absorption fine structure (EXAFS) spectroscopy. The vibration modes of alkylammonium chains and the absorpton peaks of an excition have been examined by FT-IR and UV-Vis. reflectance spectra, respectively. The phase transition temperatures of the compounds have been studied by using DSC. According to the thermal analysis, two phase transition temperatures have been observed in the compositons of n=8 and 10.

IR Absorption Property in Nano-thick Ir-inserted Nickel Silicides (이리듐이 첨가된 니켈실리사이드의 적외선 흡수 특성)

  • Yoon, Kijeong;Song, Ohsung;Han, Jeungjo
    • Korean Journal of Metals and Materials
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    • v.46 no.11
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    • pp.755-761
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    • 2008
  • We fabricated thermally evaporated 10 nm-Ni/1 nm-Ir/(poly)Si films to investigate the energy saving property of silicides formed by rapid thermal annealing (RTA) at the temperature range of $300{\sim}1200^{\circ}C$ for 40 seconds. Moreover, we fabricated 100 nm-thick ITO/(poly)Si films with an rf-sputter as references. A transmission electron microscope (TEM) and an X-ray diffractometer were used to determine cross-sectional microstructure and phase changes. A UV-VIS-NIR and FT-IR (Fourier transform infrared spectroscopy) were employed for near-IR and middle-IR absorbance. Through TEM analysis, we confirmed 20~65 nm-thick silicide layers formed on the single and polycrystalline silicon substrates. Ir-inserted nickel silicide on single crystalline substrate showed almost the same absorbance in near IR region as well as ITO, but Ir-inserted nickel silicide on polycrystalline substrate, which had the uniform absorbance in specific region, showed better absorbance in near IR region than ITO. The Ir-inserted nickel silicide on polycrystalline substrate particularly showed better absorbance in middle IR region than ITO. The results imply that nano-thick Ir-inserted nickel silicides may have excellent absorbing capacity in near-IR and middle-IR region.

Analysis of Wafer Cleaning Solution Characteristics and Metal Dissolution Behavior according to the Addition of Chelating Agent (착화제 첨가에 따른 웨이퍼 세정 용액 특성 분석 및 금속 용해 거동)

  • Kim, Myungsuk;Ryu, Keunhyuk;Lee, Kun-Jae
    • Journal of Powder Materials
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    • v.28 no.1
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    • pp.25-30
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    • 2021
  • The surface of silicon dummy wafers is contaminated with metallic impurities owing to the reaction with and adhesion of chemicals during the oxidation process. These metallic impurities negatively affect the device performance, reliability, and yield. To solve this problem, a wafer-cleaning process that removes metallic impurities is essential. RCA (Radio Corporation of America) cleaning is commonly used, but there are problems such as increased surface roughness and formation of metal hydroxides. Herein, we attempt to use a chelating agent (EDTA) to reduce the surface roughness, improve the stability of cleaning solutions, and prevent the re-adsorption of impurities. The bonding between the cleaning solution and metal powder is analyzed by referring to the Pourbaix diagram. The changes in the ionic conductivity, H2O2 decomposition behavior, and degree of dissolution are checked with a conductivity meter, and the changes in the absorbance and particle size before and after the reaction are confirmed by ultraviolet-visible spectroscopy (UV-vis) and dynamic light scattering (DLS) analyses. Thus, the addition of a chelating agent prevents the decomposition of H2O2 and improves the life of the silicon wafer cleaning solution, allowing it to react smoothly with metallic impurities.

Properties of the White 5K Au-Ag-In Alloys with Indium Contents (백색 5K Au-Ag-In 합금재의 인듐 첨가량에 따른 물성 변화)

  • Song, Jeongho;Song, Ohsung
    • Korean Journal of Materials Research
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    • v.27 no.7
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    • pp.381-385
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    • 2017
  • In order to replace 14K white gold alloys, the properties of 5K white gold alloys (Au20-Ag80) were investigated by changing the contents of In (0.0-10.0 wt%). Energy dispersive X-ray spectroscopy (EDS) was used to determine the precise content of alloys. Properties of the alloys such as hardness, melting point, color difference, and corrosion resistance were determined using Vickers Hardness test, TGA-DTA, UV-VIS-NIR-colorimetry, and salt-spray tests, respectively. Wetting angle analysis was performed to determine the wettability of the alloys on plaster. The results of the EDS analysis confirmed that the Au-Ag-In alloys had been fabricated with the intended composition. The results of the Vickers hardness test revealed that each Au-Ag-In alloy had higher mechanical hardness than that of 14K white gold. TGA-DTA analysis showed that the melting point decreased with an increase in the In content. In particular, the alloy containing 10.0 wt% In showed a lower melting temperature (> $70^{\circ}C$) than the other alloys, which implied that alloys containing 10.0 wt% In can be used as soldering materials for Au-Ag-In alloys. Color difference analysis also revealed that all the Au-Ag-In alloys showed a color difference of less than 6.51 with respect to 14K white gold, which implied a white metallic color. A 72-h salt-spray test confirmed that the Au-AgIn alloys showed better corrosion resistance than 14K white gold alloys. All Au-Ag-In alloys showed wetting angle similar to that of 14K white gold alloys. It was observed that the 10.0 wt% In alloy had a very small wetting angle, further confirming it as a good soldering material for white metals. Our results show that white 5K Au-Ag-In alloys with appropriate properties might be successful substitutes for 14K white gold alloys.

Synthesis, Characterization, Thermal Stability and Conductivity of New Schiff Base Polymer Containing Sulfur and Oxygen Bridges (황과 산소를 함유하는 새로운 Schiff Base 고분자의 합성, 특성분석, 열적 안정성과 전도성)

  • Culhaoglu, Suleyman;Kaya, Ismet
    • Polymer(Korea)
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    • v.39 no.2
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    • pp.225-234
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    • 2015
  • In this study, we proposed to synthesize thermally stable, soluble and conjugated Schiff base polymer (SbP). For this reason, a specific molecule namely 4,4'-thiodiphenol which has sulfur and oxygen bridge in its structure was used to synthesize bi-functional monomers. Bi-functional amino and carbonyl monomers namely 4,4'-[thio-bis(4,1-phenyleneoxy)] dianiline (DIA) and 4,4'-[thiobis(4,1-phenyleneoxy)]dibenzaldehyde (DIB) were prepared from the elimination reaction of 4,4'-thiodiphenol with 4-iodonitrobenzene and 4-iodobenzaldehyde, respectively. The structures of products were confirmed by elemental analysis, FTIR, $^1H$ NMR and $^{13}C$ NMR techniques. The molecular weight distribution parameters of SbP were determined by size exclusion chromatography (SEC). The synthesized SbP was characterized by solubility tests, TG-DTA and DSC. Also, conductivity values of SbP and SbP-iodine complex were determined from their solid conductivity measurements. The conductivity measurements of doped and undoped SbP were carried out by Keithley 2400 electrometer at room temperature and atmospheric pressure, which were calculated via four-point probe technique. When iodine was used as a doping agent, the conductivity of SbP was observed to be increased. Optical band gap ($E_g$) of SbP was also calculated by using UV-Vis spectroscopy. It should be stressed that SbP was a semiconductor which had a potential in electronic and optoelectronic applications, with fairly low band gap. SbP was found to be thermally stable up to $300^{\circ}C$. The char of SbP was observed 29.86% at $1000^{\circ}C$.

Isolation and Characterization of Bacterial Cellulose-Producing Bacteria for Silver Nanoparticle Synthesis (은 나노입자 합성을 위한 Bacterial Cellulose 생산 세균의 분리 및 특성)

  • Yoo, Ji-Yeon;Jang, Eun-Young;Son, Yong-Jun;Park, Soo-Yeun;Son, Hong-Joo
    • Microbiology and Biotechnology Letters
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    • v.46 no.2
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    • pp.120-126
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    • 2018
  • As a basic study for environment-friendly production of bacterial cellulose (BC) dressing with antimicrobial activity, we isolated and identified acetic acid bacteria which are resistant to silver ions and can biosynthesize silver nanoparticles. Furthermore, conditions of BC production by selected strain were also investigated. Strain G7 isolated from decayed grape skin was able to grow in the presence of 0.1 mM $AgNO_3$ which was identified as Acetobacter intermedius based on 16S rRNA gene analysis. BC production was the highest in a medium containing 2% glucose as a carbon source, 2% yeast extract as a nitrogen source, and 0.115% acetic acid as a cosubstrate. Structural properties of BC produced in optimal medium were studied using Fourier-transform infrared spectroscopy and X-ray diffractometer, and it was found that BC produced was cellulose type I that was the same as a typical native cellulose. When strain G7 was cultured in an optimal medium containing 0.1 mM $AgNO_3$, the color of the culture broth turned into reddish brown, indicating that silver nanoparticles were formed. As a result of UV-Vis spectral analysis of the culture, it was found that a unique absorption spectrum of silver nanoparticles at 425 nm was also observed. Scanning electron microscopic observations showed that silver nanoparticles were formed on the surface and pores of BC membrane.

Syntheses and Characterization of Cr(III)-Hydrogensalicylato and -Hydroxonitrophenolato Tetraaza Macrocyclic Complexes

  • Byun, Jong-Chul;Yoon, Chang-Hoon;Mun, Dae-Hun;Kim, Ki-Ju;Park, Yu-Chul
    • Bulletin of the Korean Chemical Society
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    • v.27 no.5
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    • pp.687-693
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    • 2006
  • Chromium(III) complexes, cis-[Cr([14]-decane)$(HOC _6H _4COO) _2$]$ClO _4$ I and cis-[Cr([14]-decane)(OH) $(OC _6H _4NO _2)$]$ClO _4{\cdot}H _2O$ II ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) are synthesized and structurally characterized by a combination of elemental analysis, conductivity, IR and VIS spectroscopy, and X-ray crystallography. The complexes crystallizes in the monoclinic space groups, $C2 _1$/a in I and $P2 _1$/n in II. Analysis of the crystal structure of complex I reveals that central chromium(III) ion has a distorted octahedral coordination environment and two hydrogensalicylato ligands are unidentate to the chromium(III) ion via the carboxyl groups in the cis-position. For monomeric complex I the hydrogensalicylato coordination geometry is as follows: Cr-O(average) = 1.984(3) $\AA$;Cr-N range = 2.105(3)-2.141(4) $\AA$;C(24)-O(4) = 1.286(5) $\AA$;N(2)-Cr-N(4) (equatorial position) = 96.97(15)${^{\circ}}$; N(1)-Cr-N(3) (axial position) = 168.27(15)${^{\circ}}$; O(1)-Cr-O(4) = 85.70(13)${^{\circ}}$. The crystal structure of II has indicated that chromium(III) ion is six-coordinated by four secondary amines of the macrocycle, hydroxide anion and nitrophenolate anion.

Cr(III)-Tetraaza Macrocyclic Complexes Containing Auxiliary Ligands (Part IV); Synthesis and Characterization of Cr(III)-Acetylacetonato, -Malonato and -Oxalato Macrocyclic Complexes

  • Byun, Jong-Chul;Han, Chung-Hun
    • Bulletin of the Korean Chemical Society
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    • v.26 no.9
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    • pp.1395-1402
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    • 2005
  • The reaction of cis-[Cr([14]-decane)$(OH)_2]^+$ ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) with auxiliary ligands {$L_a$ = acetylacetonate (acac), oxalate (ox) or malonate (mal)} leads to a new cis-[Cr([14]-decane)(acac)]$(ClO_4)_2{\cdot}(1/2)H_2O\;(1),\;cis-[Cr([14]-decane)(ox)]ClO_4{\cdot}(1/2)H_2O\;(2)\;or\;cis-[Cr([14]-decane)(mal)]ClO_4{\cdot}(1/4)H_2O\;(3)$. These complexes have been characterized by a combination of elemental analysis, conductivity, IR and Vis spectroscopy, mass spectrometry, and X-ray crystallography. Analysis of the crystal structure of cis-[Cr([14]-decane)(acac)]$(ClO_4)_2{\cdot}(1/2)H_2O$ reveals that central chromium(III) has a distorted octahedral coordination environment and two acetylacetonate-oxygen atoms are bonded to the chromium(III) ion in the cis positions. The angle $N_{axial}-Cr-N_{axial}$ deviates by $11^{\circ}$ from the ideal value of $180^{\circ}$ for a perfect octahedron. The bond angle O-Cr-O between the chromium(III) ion and the two acetylacetonate-oxygen atoms is close to $90^{\circ}$. The bond lengths of Cr-O between the chromium and the acetylacetonate-oxygen atoms are 1.950(3) and 1.954(2) $\AA$. They are shorter than those between chromium and nitrogen atoms of the macrocycle. The IR spectra of 1, 2 and 3 display bands at 1560 {ν (C=O)}, 1710 {${\nu}_{as}$(OCO)} and 1660 $cm^{-1}$ {${\nu}_{as}$(OCO)} attributed to the acac, ox and mal auxiliary ligands stretching vibrations, respectively.

Cr(III)-Tetraaza Macrocyclic Complexes Containing Auxiliary Ligands (Part II); Synthesis and Characterization of Cr(III)-Citrato Macrocyclic Complex

  • Byun, Jong-Chul;Park, Yu-Chul;Youn, Jeung-Su;Han, Chung-Hun;Lee, Nam-Ho
    • Bulletin of the Korean Chemical Society
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    • v.26 no.4
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    • pp.634-640
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    • 2005
  • The reaction of cis-[Cr([14]-decane)(OH$_2)_2]^+$ ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) with auxiliary ligands {$L_a$ = citrate(cit)} leads to a new dimeric complex cis-[{Cr([14]-decane)($\mu$-cit)}$_2](ClO_4)_2$. This binuclear complex has been structurally characterized by a combination of elemental analysis, conductivity, IR and Vis spectroscopy, mass spectrometry, and X-ray crystallography. Analysis of the crystal structure of cis-[{Cr([14]-decane)($\mu$-cit)})($_2]^+$ reveals that each chromium has a distorted octahedral coordination environment and citrato ligands are monodentate to the two chromium atoms via the carboxyl groups. For dimeric complex the bridging geometry is as follows: Cr$\ldots$Cr = 7.361 $\AA$; Cr-O(average) = 1.958 (8) $\AA$; Cr-N range = 2.108 (9)-2.147(9) $\AA$; N(1)-Cr-N(3) (equatorial position) = 98.0(4)$^{\circ}$; N(2)-Cr-N(4) (axial position) = 166.4(4)$^{\circ}$; O(1)-Cr-N(2) = 98.1(4)$^{\circ}$; O(3)-Cr-N(4) = 96.6(3)$^{\circ}$; O(1)-Cr-O(3) = 90.4$^{\circ}$. The FAB mass spectrum of the dimeric complex displays peak due to the molecular ions cis-[{Cr([14]-decane)($\mu$-cit)})($_2]^+$ at m/z 1053.