• Title/Summary/Keyword: XRD (X-ray diffraction)

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Optimization of Calcium Acetate Preparation from Littleneck Clam (Ruditapes philippinarum) Shell Powder and Its Properties (바지락(Ruditapes philippinarum) 패각분말로부터 초산칼슘 제조 및 특성)

  • Park, Sung Hwan;Jang, Soo Jeong;Lee, Hyun Ji;Lee, Gyoon-Woo;Lee, Jun Kyu;Kim, Yong Jung;Kim, Jin-Soo;Heu, Min Soo
    • Korean Journal of Food Science and Technology
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    • v.47 no.3
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    • pp.321-327
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    • 2015
  • The optimal condition for preparation of powdered calcium acetate (LCCA) which has high solubility, from calcined powder (LCCP) of the littleneck clam shell by response surface methodology (RSM) was examined. Increased molar ratio of LCCP led to reduced solubility, yield, color values, and overall quality. The critical values of multiple response optimization of independent variables were 2.57 M of acetic acid and 1.57 M of LCCP. The actual values (pH 7.0, 96.1% for solubility, and 220.9% for yield) under the optimized condition were similar to the predicted values. LCCA showed strong buffering capacity between pH 4.89 and 4.92 on addition of ~2 mL of 1 N HCl. The calcium content and solubility of LCCA were 21.9-23.0 g/100 g and 96.1-100.1%, respectively. The FT-IR and XRD patterns of LCCA were identified as calcium acetate monohydrate, and FESEM images revealed an irregular and rod-like microstructure.

Synthesis of Chromium Nitride and Evaluation of its Catalytic Property (크롬 질화물(CrN)의 합성 및 촉매특성에 관한 연구)

  • Lee, Yong-Jin;Kwon, Heock-Hoi
    • Applied Chemistry for Engineering
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    • v.17 no.5
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    • pp.451-457
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    • 2006
  • We synthesized phase pure CrN having surface areas up to $47m^2/g$ starting from $CrCl_{3}$ with $NH_{3}$. Thermal Gravimetric Analysis coupled with X-ray diffraction was carried out to identify solid state transition temperatures and the phase after each transition. In addition, the BET surface areas, pore size distributions, and crystalline diameters for the synthesized materials were analyzed. Space velocity influenced a little to the surface areas of the prepared materials, while heating rate did not. We believe it is due to the fast removal of reaction by-products from the system. Temperature programmed reduction results revealed that the CrN was hardly passivated by 1% $O_{2}$. Molecular nitrogen was detected from CrN at 700 and $950^{\circ}C$, which may be from lattice nitrogen. In temperature programmed oxidation with heating rate of 10 K/min in flowing air, oxidation started at or higher than $300^{\circ}C$ and resulting $Cr_{2}O_{3}$ phase was observed with XRD at around $800^{\circ}C$. However the oxidation was not completed even at $900^{\circ}C$. CrN catalysts were highly active for n-butane dehydrogenation reaction. Their activity is even higher than that of a commercial $Pt-Sn/Al_{2}O_{3}$ dehydrogenation catalyst in terms of volumetric reaction rate. However, CrN was not active in pyridine hydrodenitrogenation.

The Characterization of Controlled Low Strength Material (CLSM) Using High CaO Fly Ash without Chemical Alkaline Activator (고칼슘 플라이애쉬를 이용한 알칼리 활성화제 무첨가 저강도 유동화 채움재 특성 평가)

  • Lim, Sanghyeong;Choo, Hyunwook;Lee, Woojin;Lee, Changho
    • Journal of the Korean GEO-environmental Society
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    • v.17 no.12
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    • pp.17-26
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    • 2016
  • The experimental investigation aims at developing controlled low strength materials (CLSM) using a self-cementitious fly ash (FA) as a binder and a bottom ash (BA) as a aggregate. The fly ash and bottom ash used in this study were obtained from a circulating fluidized bed combustion boiler (CFBC) which produces relatively high CaO containing fly ash. To find the optimum mixing condition satisfying flow consistency and unconfined compression strength (UCS), the CLSM specimens were prepared under various mixing conditions, including two types of aggregate and different weight fractions between fly ash and aggregate. Additionally, the prepared specimens were evaluated using a scanning electron microscope (SEM) and X-ray diffraction (XRD). The results of this study demonstrate that the water content satisfying flow consistency ranges from 42% to 85% and the flowability is improved with increasing the fraction of aggregate in whole mixture. The USC ranges from 0.3 MPa to 1.9 MPa. The results of UCS increases with increasing the fraction of aggregate in FA-sand mixtures, but decreases with increasing the fraction of aggregate in FA-BA mixtures. SEM images and XRD patterns reveal that the occurrence of both geopolymerization and hydration. The results of this study demonstrate that CFBC fly ash could be used as an alternative binder of CLSM mixtures.

Preparation and Electrochemical Properties of PANI/TiO2 Composites for Supercapacitor Electrodes (수퍼커패시터 전극을 위한 폴리아닐린/TiO2 복합체의 제조 및 전기화학적 성질)

  • Park, Sukeun;Kim, Kwang Man;Lee, Young-Gi;Jung, Yongju;Kim, Seok
    • Korean Chemical Engineering Research
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    • v.50 no.1
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    • pp.50-54
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    • 2012
  • In this study, PANI and PANI/$TiO_2$ composites were prepared as electrode materials for a supercapacitor application. Cyclic voltammetry (CV) was performed to investigate the supercapacity properties of these electrodes in an electrolyte solution of 6 M KOH. The PANI/$TiO_2$ composites were polymerized by amount of various ratios through a simple in-situ method. The morphological properties of composites were analyzed by SEM and TEM method. The crystallinity of the composite and $TiO_2$ particle size were identified using X-ray diffraction (XRD). In the electrochemical test, The electrode containing 10 wt% $TiO_2$ content against aniline units showed the highest specific capacitance (626 $Fg^{-1}$) and delivered a capacitance of 286 $Fg^{-1}$ reversibly at a 100 $mVs^{-1}$ rate. According to the surface morphology, the increased capacitance was related to the fact that nano-sized $TiO_2$ particles (~6.5 nm) were uniformly connected for easy charge transfer and an enhanced surface area for capacitance reaction of $TiO_2$ itself.

Selective Oxidation of Hydrogen Over Palladium Catalysts in the Presence of Carbon Monoxide: Effect of Supports (Pd 촉매상에서 일산화탄소 존재 하 수소의 선택적 산화반응: 담체 효과)

  • Kim, Eun-Jeong;Kang, Dong-Chang;Shin, Chae-Ho
    • Korean Chemical Engineering Research
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    • v.55 no.1
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    • pp.121-129
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    • 2017
  • Pd based catalysts were prepared by impregnating palladium precursor using incipient wetness method on $TiO_2$, $Al_2O_3$, $ZrO_2$, and $SiO_2$ and were applied for the selective oxidation of $H_2$ in the presence of CO. Their physicochemical properties were studied by X-ray diffraction (XRD), $N_2$-sorption, temperature programmed desorption of CO (CO-TPD) and (CO+$H_2O$)-TPD, temperature programmed reduction of CO (CO-TPR) and XPS a. The results of CO- and (CO+$H_2O$)-TPD showed the correlation between peak temperature of TPD and catalytic activities for $H_2$ and CO conversion. The $Pd/ZrO_2$ catalyst exhibited the highest conversion of $H_2$. The addition of $H_2O$ vapor promotes the conversion of $H_2$ and CO by inducing easy desorption of CO and $H_2$ in the competitive adsorption of $H_2O$, CO and $H_2$.

Effect of Temperature on the Formation of Vaterite in Ca(OH)2-CH3OH-H2O-CO2 System (Ca(OH)2-CH3OH-H2O-CO2계에서 바테라트의 생성에 미치는 반응온도의 영향)

  • Park, Jong-Lyuck;Choi, Sang-Kuen;Kim, Byoung-Gon;Lee, Jae-Jang
    • Journal of the Korean Ceramic Society
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    • v.39 no.12
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    • pp.1143-1148
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    • 2002
  • Precipitated calcium carbonate is one of the most versatile mineral fillers and is consumed in an wide range of products including paper, paint, plastics, rubber, textiles, sealants, adhesives and printing ink and can be produced by several methods. Calcium carbonate has three isomorphism; vaterite, aragonite and calcite, with numerous variations of morphology in the natural mineral or organism. Formation process of vaterite in the reaction of system $Ca(OH)_2-CH_3OH-H_2O-CO_2$ were investigated by measuring the electrical conductivity, $Ca^{2+}$ ion concentration, pH in the slurries and by means of X-ray diffraction and electron microscopic observation. It was clearly established that the reaction temperature is important variable in the carbonation process; in general over 50${\circ}C$, the vaterite was precipitated with the calcite and aragonite. SEM and XRD observations revealed that the vaterite formation could be prepared the temperature range of 40 to 50${\circ}C$ and mean size of particles in this range is controlled from 0.5 to 0.8 ${\mu}m$.

Physiochemical Characteristics of Calcium Supplement Manufactured using Starfish (불가사리를 이용하여 제조한 칼슘보충제의 이화학적 특성)

  • Park, Hee-Yeon;Lee, Jung Im;Nam, Ki-Ho;Jang, Mi-Soon
    • Food Science and Preservation
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    • v.19 no.5
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    • pp.727-734
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    • 2012
  • For developing calcium supplement from the harmful marine organism starfish, the physiochemical property of the powdered starfish skeletal plate and the hydrolysis condition of the starfish digestive enzyme were studied. The optimal hydrolysis condition of the starfish digestive enzymes was at $55^{\circ}C$ for 12 h. The bulk densities of the powdered starfish skeletal plates of Asterias amurensis and Asterina pectinifera were $1.1{\pm}0.0$ and $1.2{\pm}0.0g/cm^3$, respectively. As for the median size, the values were 10.738 and $11.799{\mu}m$, respectively. According to the added concentration of sodium polyacrylate, the dispersibility rate of the powdered starfish skeletal plate was shown to be 6h at 0.0%, 3 days at 0.1%, 20 days at 0.2%, and until 30 days at 0.4%. The elementary composition of the powdered starfish skeletal plates from A. amurensis and A. pectinifera mainly consisted of calcium, and it formed 98.95 and 98.52% of the powdered starfish skeletal plates, respectively. The results of the X-ray diffraction (XRD) analysis showed that they were present in the form of $CaCO_3$. Based on these results, it is suggested that starfish skeletal plate can be utilized as a functional material for a calcium supplement.

Development of Biomass-Derived Anode Material for Lithium-Ion Battery (리튬이온 전지용 바이오매스 기반 음극재 개발)

  • Jeong, Jae Yoon;Lee, Dong Jun;Heo, Jungwon;Lim, Du-Hyun;Seo, Yang-Gon;Ahn, Jou-Hyeon;Choi, Chang-Ho
    • Clean Technology
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    • v.26 no.2
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    • pp.131-136
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    • 2020
  • Biomass bamboo charcoal is utilized as anode for lithium-ion battery in an effort to find an alternative to conventional resources such as cokes and petroleum pitches. The amorphous phase of the bamboo charcoal is partially converted to graphite through a low temperature graphitization process with iron oxide nanoparticle catalyst impregnated into the bamboo charcoal. An optimum catalysis amount for the graphitization is determined based on the characterization results of TEM, Raman spectroscopy, and XRD. It is found that the graphitization occurs surrounding the surface of the catalysis, and large pores are formed after the removal of the catalysis. The formation of the large pores increases the pore volume and, as a result, reduces the surface area of the graphitized bamboo charcoal. The partial graphitization of the pristine bamboo charcoal improves the discharge capacity and coulombic efficiency compared to the pristine counterpart. However, the discharge capacity of the graphitized charcoal at elevated current density is decreased due to the reduced surface area. These results indicate that the size of the catalysis formed in in-situ graphitization is a critical parameter to determine the battery performance and thus should be tuned as small as one of the pristine charcoal to retain the surface area and eventually improve the discharge capacity at high current density.

Effect of Reaction Conditions for n-Butane Dehydrogenation over Pt-Sn/θ-Al2O3 Catalyst (Pt-Sn/θ-Al2O3 촉매상에서 반응조건에 따른 n-부탄의 탈수소화 반응)

  • Cho, Kyung-Ho;Kang, Seong-Eun;Park, Jung-Hyun;Cho, Jun-Hee;Shin, Chae-Ho
    • Clean Technology
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    • v.18 no.2
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    • pp.162-169
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    • 2012
  • Pt-Sn/${\theta}-Al_2O_3$ catalyst for n-butane dehydrogenation reaction was prepared by incipient wetness method. To confirm the physicochemical properties of Pt-Sn/${\theta}-Al_2O_3$ catalyst, the characterization was performed using X-ray diffraction (XRD), $N_2$ sorption analysis, temperature programmed desorption of $NH_3$ ($NH_3$-TPD), temperature programmed reduction of $H_2$ ($H_2$-TPR) techniques. Also, the catalytic activities of Pt-Sn/${\theta}-Al_2O_3$ for n-butane dehydrogenation was tested as a function of pretreatment temperature, pretreatment time, reaction temperature, and the partial pressure of n-butane and hydrogen. The sum of selectivities to n-butenes consisting of 1-butene, cis-2-butene, and trans-2-butene was almost constant 95% in the range of conversion of n-butane 5-55%. The activation energy calculated from Arrhenius equation was $82.4kJ\;mol^{-1}$ and the reaction orders of n-butane and hydrogen from Power's law were 0.70 and -0.20, respectively.

Improvement of Hydrogen Storage Properties of Mg by Addition of NbF5 via Mechanical Milling under H2

  • Kwak, Young Jun;Song, Jiyoung;Mumm, Daniel R.
    • Korean Journal of Materials Research
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    • v.23 no.10
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    • pp.562-567
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    • 2013
  • A 90 wt% Mg-10 wt% $NbF_5$ sample was prepared by mechanical milling under $H_2$ (reactive mechanical grinding). Its hydriding and dehydriding properties were then examined. Activation of the 90 wt% Mg-10 wt% $NbF_5$ sample was not required. At n=1, the sample absorbed 3.11 wt% H for 2.5 min, 3.55 wt% H for 5 min, 3.86 wt% H for 10 min, and 4.23 wt% H for 30 min at 593K under 12 bar $H_2$. At n=1, the sample desorbed 0.17 wt% H for 5 min, 0.74 wt% H for 10 min, 2.03 wt% H for 30 min, and 2.81 wt% H for 60 min at 593K under 1.0 bar $H_2$. The XRD pattern of the 90 wt% Mg-10 wt% $NbF_5$ after reactive mechanical grinding showed Mg, ${\beta}-MgH_2$ and small amounts of ${\gamma}-MgH_2$, $NbH_2$, $MgF_2$ and $NbF_3$. The XRD pattern of the 90 wt% Mg-10 wt% $NbF_5$ dehydrided at n=3 revealed Mg, ${\beta}-MgH_2$, a small amount of MgO and very small amounts of $MgH_2$ and $NbH_2$. The 90 wt% Mg-10 wt% $NbF_5$ had a higher initial hydriding rate and a larger quantity of hydrogen absorbed for 60 min than the 90 wt% Mg-10 wt% MnO and the 90 wt% Mg-10 wt% $Fe_2O_3$, which were reported to have quite high hydriding rates and/or dehydriding rates. The 90 wt% Mg-10 wt% $NbF_5$ had a higher initial dehydriding rate (after an incubation period) and a larger quantity of hydrogen desorbed for 60 min than the 90 wt% Mg-10 wt% MnO and the 90 wt% Mg-10 wt% $Fe_2O_3$.