• Title/Summary/Keyword: XRD and FT-IR

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Synthesis and Characterization of Ruthenium Doped TiO2 Nanofibers

  • Park, Jung-Yeon;Lee, Deuk-Yong;Cho, Nam-Ihn;Oh, Young-Jei
    • Journal of Sensor Science and Technology
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    • v.20 no.2
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    • pp.82-89
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    • 2011
  • Ruthenium(Ru)-doped $TiO_2$ nanofibers were prepared using electrospun Ru-$TiO_2$/poly(vinyl acetate) (PVAc) fibers and subsequent annealing for 1 h at temperatures in the range of $500^{\circ}C$ to $1000^{\circ}C$ in air. The properties of the Ru-$TiO_2$ fibers were characterized as a function of the Ru content and calcination temperature using X-ray diffraction, thermal gravimetry with differential scanning calorimetry, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, and viscometer, pycnometer and dynamic tensiometer measurements. Although the diameter of the fiber decreased slightly with increasing calcination temperature, no dramatic changes were observed with respect to the ruthenium content. The XRD and FT-IR results revealed that anatase phase and ruthenium metal began to be formed after calcination at temperatures above $500^{\circ}C$. Anatase and rutile phases and ruthenium metal coexisted in the fibers calcined above $600^{\circ}C$. No anatase phase was detected in the fibers containing ruthenium when they were calcined at $1000^{\circ}C$. The morphology of the fibers changed from smooth and uniform to porous with increasing temperature. The experimental results suggest that the calcination temperature and Ru content were influential in determining the morphology and structure of the fibers.

Arsenic Contamination of Groundwater a Grave Concern: Novel Clay-based Materials for Decontamination of Arsenic (V)

  • Amrita Dwivedi;Diwakar Tiwari;Seung Mok Lee
    • Applied Chemistry for Engineering
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    • v.34 no.2
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    • pp.199-205
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    • 2023
  • Arsenic is a highly toxic element, and its contamination is widespread around the world. The natural materials with high selectivity and efficiency toward pollutants are important in wastewater treatment technology. In this study, the mesoporous synthetic hectorite was synthesized by facile hydrothermal crystallization of gels comprising silica, magnesium hydroxide, and lithium fluoride. Additionally, the naturally available clay was modified using zirconium at room temperature. Both synthetic and modified natural clays were employed in the removal of arsenate from aquatic environments. The materials were fully characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), and Fourier transform-infrared (FT-IR) analyses. The synthesized materials were used to remove arsenic (V) under varied physicochemical conditions. Both materials, i.e., Zr-bentonite and Zr-hectorite, showed high percentage removal of arsenic (V) at lower pH, and the efficiency decreased in an alkaline medium. The equilibrium-state sorption data agrees well with the Langmuir and Freundlich adsorption isotherms, and the maximum sorption capacity is found to be 4.608 and 2.207 mg/g for Zr-bentonite and Zr-hectorite, respectively. The kinetic data fits well with the pseudo-second order kinetic model. Furthermore, the effect of the background electrolytes study indicated that arsenic (V) is specifically sorbed at the surface of these two nanocomposites. This study demonstrated that zirconium intercalated synthetic hectorite as well as zirconium modified natural clays are effective and efficient materials for the selective removal of arsenic (V) from aqueous medium.

Syntheses and Characterizations of Serine and Threonine Capped Water-Dispersible ZnS:Mn Nanocrystals and Comparison Study of Toxicity Effects on the growth of E. coli by the Methionine, Serine, Threonine, and Valine Capped ZnS:Mn Nanocrystals

  • Lim, Eun-Ju;Park, Sang-Hyun;Byun, Jong-Hoe;Hwang, Cheong-Soo
    • Bulletin of the Korean Chemical Society
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    • v.33 no.5
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    • pp.1741-1747
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    • 2012
  • Water-dispersible ZnS:Mn nanocrystals were synthesized by capping the surface of the nanocrystals with conventional aminoacids ligands: serine and threonine. The aminoacids capped ZnS:Mn nanocrystal powders were characterized by XRD, HR-TEM, EDXS, ICP-AES and FT-IR spectroscopy. The optical properties were also measured by UV/Vis and solution photoluminescence (PL) spectroscopies in aqueous solvents. The solution PL spectra showed broad emission peaks around 600 nm with PL efficiencies of 9.7% (ZnS:Mn-Ser) and 15.4% (ZnS:Mn-Thr) respectively. The measured particle sizes for the aminoacid capped ZnS:Mn nanocrystals by HR-TEM images were about 3.0-4.0 nm, which were also supported by Debye-Scherrer calculations. In addition, cytotoxic effects of four aminoacids capped ZnS:Mn nanocrsystals over the growth of wild type E. coli were investigated. Although toxicity in the form of growth inhibition was observed with all the aminoacids capped ZnS:Mn nanocrystals at higher dose (1 mg/mL), ZnS:Mn-Met and ZnS:Mn-Thr appeared non-toxic at doses less than 100 ${\mu}g$/mL. Low biological toxicities were seen at doses less than 10 ${\mu}g$/ mL for all nanocrystals.

Synthesis of Porous TiO2-SiO2 Particles by Self-assembly of Nanoparticles (나노입자들의 자기조립에 의한 TiO2-SiO2 다공체 제조)

  • Oh, Kyoung Joon;Kim, Sun Kyung;Chang, Hankwon;Jang, Hee Dong
    • Particle and aerosol research
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    • v.7 no.3
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    • pp.79-85
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    • 2011
  • Porous $TiO_2-SiO_2$ particles were synthesized by co-assembly of nanoparticles of $TiO_2$ and $SiO_2$ in evaporating aerosol droplets. Poly styrene latex (PSL) particles were employed as a template of porous particles. Flowrate of dispersion gas, weight ratio of $TiO_2/SiO_2$ and $SiO_2$ concentration in the precursor, and PSL size were chosen as process variables. The morphology, crystal structure, chemical bonding, and pore size distribution were analyzed by FE-SEM, XRD, FT-IR, BET. The morphology of porous $TiO_2-SiO_2$ particles was spherical and the average particle size range were from 1 to $10{\mu}m$. The particles were composed of meso and macro pores. The average particle diameter and pore volume of the as prepared particles were dependant on process variables. It was found that UV-Vis absorption of the porous particles was comparable with pure $TiO_2$ nanoparticles even though $TiO_2/SiO_2$ ratio is low in the porous particles.

Synthesis of Activated Carbon from Rice Husk Using Microwave Heating Induced KOH Activation

  • Nguyen, Tuan Dung;Moon, Jung-In;Song, Jeong-Hwan;Kim, Taik-Nam
    • Korean Journal of Materials Research
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    • v.22 no.6
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    • pp.321-327
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    • 2012
  • The production of functional activated carbon materials starting from inexpensive natural precursors using environmentally friendly and economically effective processes has attracted much attention in the areas of material science and technology. In particular, the use of plant biomass to produce functional carbonaceous materials has attracted a great deal of attention in various aspects. In this study the preparation of activated carbon has been attempted from rice husks via a chemical activation-assisted microwave system. The rice husks were milled via attrition milling with aluminum balls, and then carbonized under purified $N_2$. The operational parameters including the activation agents, chemical impregnation weight ratio of the calcined rice husk to KOH (1:1, 1:2 and 1:4), microwave power heating within irradiation time (3-5 min), and the second activation process on the adsorption capability were investigated. Experimental results were investigated using XRD, FT-IR, and SEM. It was found that the BET surface area of activated carbons irrespective of the activation agent resulted in surface area. The activated carbons prepared by microwave heating with an activation process have higher surface area and larger average pore size than those prepared by activation without microwave heating when the ratio with KOH solution was the same. The activation time using microwave heating and the chemical impregnation ratio with KOH solution were varied to determine the optimal method for obtaining high surface area activated carbon (1505 $m^2$/g).

A Study of Surface Treatments of Titanium in Aqueous solutions Containing Phosphate and Calcium Ions (인산과 칼슘 이온을 함유한 수용액중에서의 타이타늄 표면처리)

  • Sin, Mi-Jeong;Kim, Do-Gyun;Kim, Gyo-Hwan
    • Korean Journal of Materials Research
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    • v.8 no.9
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    • pp.865-870
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    • 1998
  • The surfaces of titanium specimens were modified by immersion in calcium phosphate buffered solutions (pH 5.8, 7.0, 8.0) for 10 days and simulated body fluid(SBF) for 30 days by turns. The modified surfaces were characterized using scanning electron microscopy(SEM), X-ray diffractometery(XRD) and Fourier transform infrared spectrophotometer(FT-IR), and compared with specimen immersed in only SBF. The results indicated that the immersion in calcium phosphate buffered solutions accelerated the formation of the surface films. The formed layer showed granular shaped microstructure, and recognized as calcium phosphate such as a hydroxyapatite(HA) or a $\beta$-tri-calcium phosphate($\beta$-TCP). The thickness of the layer increased of the buffered solutions in order of pH 8.0, 7.0 and 5.8 and the density increased in order of pH 7.0, 8.0 and 5.8.

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Characterization and Synthesis of BN Fibers According to the Content of BN Nanopowder by Electrospinning Method (전기방사에 의한 질화붕소 나노분말의 함량에 따른 질화붕소 나노섬유 합성 및 특성 평가)

  • Lee, Jong Hyeok;Chun, Myoung Pyo;Hwang, Jin Ah;Jung, Young Geun;Chu, Jae Uk
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.31 no.7
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    • pp.455-461
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    • 2018
  • Boron nitride (BN) nanofibers were fabricated using BN nanoparticles (70 nm) by electrospinning. Morphologies such as the diameter and density of the BN nanofibers are strongly influenced by the viscosity and dispersion state of the precursor solution. In this study, the precursor solution was prepared by ball milling BN nanoparticles and polyvinylpyrrolidone (PVP, Mw~1,300,000) in ethanol, which was electrospun and then calcined to produce BN fibers. High-quality BN nanofibers were well fabricated at a BN concentration of 15 wt% with their diameters in the range of 500 nm to 800 nm; the viscosity of the precursor solution was $400mPa{\cdot}S$. The calcination of the as-electrospun BN fibers seemed to be completed by holding them at $350^{\circ}C$ for 2 h considering the TGA data. The morphologies and phases of the BN fibers were investigated by scanning electron microscopy (SEM) and X-ray diffractometry (XRD), respectively; Fourier transform infrared (FT-IR) was also used for structure analysis.

The Influence of Hydrotalcite Intercalated with Benzoate on UV Stability of Acrylic Coating

  • Nguyen, Thuy Duong;Nguyen, Anh Son;Thai, Thu Thuy;Pham, Gia Vu;To, Thi Xuan Hang;Olivier, Marie-Georges
    • Corrosion Science and Technology
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    • v.19 no.1
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    • pp.16-22
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    • 2020
  • It is important to realize that benzoate was intercalated into hydrotalcite (HTC-Bz) by the co-precipitation method. In this case, acrylic coating with 0.5 wt% HTC-Bz was deposited on carbon steel using the spin coating method. Next, the HTC-Bz structure was characterized by Field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR). In fact, an ultraviolet vision spectroscopy (UV-Vis) was used to determine the benzoate content in HTC-Bz, and the UV absorption ability of HTC-Bz. Using electrochemical techniques, water contact angle measurement, and thermal-gravimetric analysis, we compared the protective properties before and after QUV test, hydrophobicity and the thermal stability of acrylic coating containing HTC-Bz. The obtained results showed that HTC-Bz with a plate-like structure was successfully synthesized; benzoate was intercalated into the interlayer of hydrotalcite with a concentration of 28 wt%. Additionally, it was noted that HTC-Bz has an UV absorption peak at 225 nm. In conclusion, the addition of HTC-Bz enhanced the UV stability, hydrophobicity and the thermal stability of acrylic coating.

Preparation of AlN Powder Using Mesoporous Alumina and Its Characterization (메조포러스 알루미나를 이용한 AlN 분말 제조 및 특성분석)

  • Kim, Eun Bee;Lee, Yoon Joo;Shin, Dong Geun;Kwon, Woo Teck;Kim, Soo Ryong;Kang, Mi Sook;Kim, Young Hee
    • Journal of the Korean Ceramic Society
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    • v.51 no.6
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    • pp.544-548
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    • 2014
  • Aluminum nitride was synthesized using a carbothermal method from mesoporous alumina having a high surface area (> $1,000m^2/g$) as an aluminum source and CNTs (carbon nano tubes) as a carbon source. In this case the mesoporous alumina was used as the starting material instead of ${\alpha}-Al_2O_3$ with the expectation that the mesopores in mesoporous alumina act as channels for N2 gas and elimination of CO generated as by-product. It is also expected that the synthetic temperature should be lower compared to the use of ${\alpha}-Al_2O_3$ as a starting material due to its high surface area. The crystallinity of the produced aluminum nitride was studied by XRD and FT-IR, and the microstructure was investigated by FE-SEM. Also the purity of the aluminum nitride was analyzed through N/O determinator and ICP analysis.

Photocatalytic Generated Oxygen Species Properties by Fullerene Modified Two-Dimensional MoS2 and Degradation of Ammonia Under Visible Light

  • Zou, Cong-Yang;Meng, Ze-Da;Zhao, Wei;Oh, Won-Chun
    • Korean Journal of Materials Research
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    • v.31 no.6
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    • pp.353-366
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    • 2021
  • In this study, photocatalytic degradation of ammonia in petrochemical wastewater is investigated by solar light photocatalysis. Two-dimensional ultra-thin atomic layer structured MoS2 are synthesized via a simple hydrothermal method. We examine all prepared samples by means of physical techniques, such as SEM-EDX, HRTEM, FT-IR, BET, XRD, XPS, DRS and PL. And, we use fullerene modified MoS2 nanosheets to enhance the activity of photochemically generated oxygen (PGO) species. Surface area and pore volumes of the MoS2-fullerene samples significantly increase due to the existence of MoS2. And, PGO oxidation of MB, TBA and TMST, causing its concentration in aqueous solution to decrease, is confirmed by the results of PL. The generation of reactive oxygen species is detected through the oxidation reaction from 1,5-diphenyl carbazide (DPCI) to 1,5-diphenyl carbazone (DPCO). It is found that the photocurrent density and the PGO effect increase in the case with modified fullerene. The experimental results show that this heterogeneous catalyst has a degradation of 88.43% achieved through visible light irradiation. The product for the degradation of NH3 is identified as N2, but not NO2- or NO3-.