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

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A Study on Cation Extraction and Impurity Separation in Slag (슬래그 내 양이온 추출 및 불순물 분리 연구)

  • Lee, Ye Hwan;Kang, Hyerin;Jang, Younghee;Lee, Si-Jin;Kim, Sung Su
    • Clean Technology
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    • v.25 no.4
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    • pp.311-315
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    • 2019
  • The cation extraction and impurity separation were studied in order to investigate the recyclability of a slag produced from the steel refinery industry. Two types of slag (Slag-A, B) were collected and characterized in this study. The initial characterization by X-ray diffraction (XRD) and X-ray fluorescence (XRF) confirmed the existence of various kinds of ions in the slag such as Ca2+ (30 ~ 40%), Fe3+ (20 ~ 30%), Si4+ (15%), Al3+ (10%), Mn2+ (7%), and Mg2+ (3 ~ 5%). Inductively coupled plasma atomic emission spectroscopy (ICP-AES) analysis on the extracted slag using 2 M HCl as a solvent indicated that a higher concentration of Ca2+ was extracted as the S/L ratio was increased. The Ca2+ extraction concentration were found to be 8,940 mg L-1 (Slag-A) and 10,690 (Slag-B) mg L-1 when the S/L ratio for Ca2+ extraction was 0.1. However, the extract was strongly acidic ( < pH 1) at 0.1 S/L. Also the other ions (impurities) were extracted simultaneously in addition to Ca2+. To increase the purity of Ca2+ in order to transform the slag to a high value resource, a pH-swing was conducted. The impurities tended to precipitate at higher rate as the pH was increased. Notably, the Ca2+ rapidly precipitated above a certain pH and at a pH of 10.5, while the selectivity of Ca2+ was over 99%. It is expected that the aqueous solution in which high contents of Ca2+ was selectively dissolved in this study would be suitable for the carbonation process for reducing CO2 and for the production of calcium carbonate.

A Study on the Replacement of a Light Burnt Dolomite with a Waste MgO-C Refractory Material for a Steel-Making Flux in Electric Arc Furnace (폐 MgO-C계 내화재의 전기로(EAF) 제강 Flux용 경소돌로마이트 대체 사용 연구)

  • Hyun-Jong Kim;Jong-Deok Lim;Hang-Goo Kim;Jei-Pil Wang
    • Resources Recycling
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    • v.31 no.6
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    • pp.44-51
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    • 2022
  • In the steelmaking process using an electric arc furnace (EAF), light-burnt dolomite, which is a flux containing MgO, is used to protect refractory materials and improve desulfurization ability. Furthermore, a recarburizing agent is added to reduce energy consumption via slag foaming and to induce the deoxidation effect. Herein, a waste MgO-C based refractory material was used to achieve the aforementioned effects economically. The waste MgO-C refractory materials contain a significant amount of MgO and graphite components; however, most of these materials are currently discarded instead of being recycled. The mass recycling of waste MgO-C refractory materials would be achievable if their applicability as a flux for steelmaking is proven. Therefore, experiments were performed using a target composition range similar to the commercial EAF slag composition. A pre-melted base slag was prepared by mixing SiO2, Al2O3, and FeO in an alumina crucible and heating at 1450℃ for 1 h or more. Subsequently, a mixed flux #2 (a mixture of light-burnt dolomite, waste MgO-C based refractory material, and limestone) was added to the prepared pre-melted base slag and a melting reaction test was performed. Injecting the pre-melted base slag with the flux facilitates the formation of the target EAF slag. These results were compared with that of mixed flux #1 (a mixture of light-burnt dolomite and limestone), which is a conventional steelmaking flux, and the possibility of replacement was evaluated. To obtain a reliable evaluation, characterization techniques like X-ray diffraction (XRD) analysis and X-ray fluorescence (XRF) spectrometry were used, and slag foam height, slag basicity, and Fe recovery were calculated.

Influence of a chemical additive on the reduction of highly concentrated ammonium nitrogen(NH4+-N) in pig wastewater (양돈 폐수로부터 고농도 암모니아성 질소의 감소를 위한 화학적 첨가제의 영향)

  • Su Ho Bae;Eun Kim;Keon Sang Ryoo
    • Korean Journal of Environmental Biology
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    • v.40 no.3
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    • pp.267-274
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    • 2022
  • Excess nitrogen (N) flowing from livestock manure to water systems poses a serious threat to the natural environment. Thus, livestock wastewater management has recently drawn attention to this related field. This study first attempted to obtain the optimal conditions for the further volatilization of NH3 gas generated from pig wastewater by adjusting the amount of injected magnesia (MgO). At 0.8 wt.% of MgO (by pig wastewater weight), the volatility rate of NH3 increased to 75.5% after a day of aeration compared to untreated samples (pig wastewater itself). This phenomenon was attributed to increases in the pH of pig wastewater as MgO dissolved in it, increasing the volatilization efficiency of NH3. The initial pH of pig wastewater was 8.4, and the pH was 9.2 when MgO was added up to 0.8 wt.%. Second, the residual ammonia nitrogen (NH4+-N) in pig wastewater was removed by precipitation in the form of struvite (NH4MgPO4·6H2O) by adjusting the pH after adding MgO and H3PO4. Struvite produced in the pig wastewater was identified by field emission scanning electron microscopy (FE-SEM) and X-ray diffraction (XRD) analysis. White precipitates began to form at pH 6, and the higher the pH, the lower the concentration of NH4+-N in pig wastewater. Of the total 86.1% of NH4+-N removed, 62.4% was achieved at pH 6, which was the highest removal rate. Furthermore, how struvite changes with pH was investigated. Under conditions of pH 11 or higher, the synthesized struvite was completely decomposed. The yield of struvite in the precipitate was determined to be between 68% and 84% through a variety of analyses.

Hydrothermal Synthesis of Kaolinite and Change of Its Properties (캐올리나이트의 수열합성 및 특성변화)

  • Jang, Young-Nam;Ryu, Gyoung-Won;Chae, Soo-Chun
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.3
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    • pp.241-248
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    • 2009
  • Kaolinite was synthesized from amorphous $SiO_2$ and $Al(OH)_3{\cdot}xH_{2}O$ as starting materials by hydrothermal reaction conducted at $250^{\circ}C$ and $30\;kg/cm^2$. The acidity of the solution was adjusted at pH 2. The synthesized kaolinite was characterized by XRD, IR, NMR, FE-SEM, TEM and EDS to clarify the formational process according to the reaction time from 2 to 36 hours. X-ray diffraction patterns showed after 2 h of reaction time, the starting material amorphous $Al(OH)_3{\cdot}xH_{2}O$ transformed to boehmite (AlOOH) and after the reaction time 5 h, the peaks of boehmite were observed to be absent thereby indicating the crystal structure is partially destructed. Kaolinite formation was identified in the product obtained after 10 h of reaction and the peak intensity of kaolinite increased further with reaction time. The results of TGA and DTA revealed that the principal feature of kaolinite trace are well resolved. TGA results showed 13 wt% amount of weight loss and DTA analysis showed that exothermic peak of boehmite observed at $258^{\circ}C$ was decreased gradually and after 10 h of reaction time, it was disappeared. After 5 h of the reaction time, the exothermicpeak of transformation to spinel phase was observed and the peak intensiy increased with reaction time. The results of FT-IR suggested a highly ordered kaolinite was obtained after 36 hours of reaction. It was identified by the characteristic hydroxide group bands positioned at 3,696, 3670, 3653 and $3620\;cm^{-1}$. The development of the hydroxyl stretching between 3696 and $3620\;cm^{-1}$, depends on the degree of order and crystalline perfection. TEM results showed that after 15 h reaction time, curved platy kaolinite was observed as growing of (001) plane and after 36 h, the morphology of synthetic kaolinite exhibited platy crystal with partial polygonal outlines.

A Study on Synthesis of Ca and Mg Compounds from Dolomite with Salt Additional React (MgCl2·6H2O) (염 첨가 반응(MgCl2·6H2O)을 이용하여 백운석으로부터 Ca 화합물과 Mg 화합물 합성에 관한 연구)

  • Hwang, Dae Ju;Yu, Young Hwan;Cho, Kye Hong;Lee, Jong Dae
    • Korean Chemical Engineering Research
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    • v.59 no.3
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    • pp.399-409
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    • 2021
  • In order to utilize dolomite as a calcium/magnesium compound material, it was prepared highly reactive calcined dolomite(CaO·MgO) using a microwave kiln (950 ℃, 60 min). The experiment was performed according to the standard of the hydration test (ASTM C 110) and hydration reactivity was analyzed as medium reactivity (max 74.1 ℃, 5 min). Experiments were performed with calcined dolomite and salt (MgCl2·6H2O) (a) 1:1, (b) 1:1.5, and (c) 1:2 wt% based on the hydration reaction of calcined dolomite. The result of X-ray diffraction analysis confirmed that MgO of calcined dolomite increased to Mg(OH)2 as the salt addition ratio increased. After the separating reaction, calcium was stirred at 80 ℃, 24 hr that produced CaCl2 of white crystal. XRD results, it was confirmed calcium chloride hydrate (CaCl2·(H2O)x) and CaO of calcined dolomite and salt additional reaction was separated into CaCl2. And it was synthesized with Ca(OH)2 99 wt% by NaOH adding reaction to the CaCl2 solution, and the synthesized Ca(OH)2 was manufactured CaO through the heat treatment process. In order to prepare calcium carbonate, CaCO3 was synthesized by adding Na2CO3 to CaCl2 solution, and the shape was analyzed in cubic form with a purity of 99 wt%.

Luminescence properties of $(Y,\;Zn)_2O_3$:$Eu^{3+}$ red phosphor as the effect of Zn ion (Zn ion의 영향에 따른 $(Y,\;Zn)_2O_3$:$Eu^{3+}$ 적색 형광체의 발광특성)

  • Song, Y.H.;Moon, J.W.;Park, W.J.;Yoon, D.H.
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.18 no.6
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    • pp.253-257
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    • 2008
  • To enhance the luminescence properties, the red phosphor composed of $(Y,\;Zn)_2O_3$:$Eu^{3+}$ as doping concentration of Zn ion is synthesized at $1200^{\circ}C$ for 6 hrs in air atmosphere by conventional solid reaction method. As a result of the red phosphor $(Y,\;Zn)_2O_3$:$Eu^{3+}$ is measured X-ray diffraction (XRD), The main peak is nearly corresponded to the same as JCPDS card (No. 41-1105). When the doping concentration of Zn ion is more than 5 mol%, However, the ZnO peak is showed by XRD analysis. Therefore, when the doping concentration of Zn ion is less than 5 mol%, the Zn ion is well mixed in $Y_2O_3$ structure without the impurity phases. The photoluminescence (PL) properties is shown as this phosphor is excited in 254 nm region and the highest emission spectra of $(Y,\;Zn)_2O_3$:$Eu^{3+}$ has shown in 612 nm region because of a typical energy transition ($^5D_0{\rightarrow}^7F_2$) of $Eu^{3+}$ ion. As the doping concentration of Zn ion is more than 10 mol%, the emission peak is suddenly decreased. when the highest emission peak as doping concentration of Zn ion is shown, the composition of this phosphor is $(Y_{0.95},\;Zn_{0.05})_2O_3$:$Eu^{3+}_{0.075}$ and the particle size analyzed by FE-SEM is confirmed from 0.4 to $3{\mu}m$.

Carbonate Biomineralization Using Speleothems and Sediments from Baekasan Acheon Cave (Limestone Cave) in Hwasun-gun, Jeollanam-do, South Korea (전남 화순군 백아산 아천동굴(석회동굴) 동굴생성물을 이용한 생광물화작용 연구)

  • Kim, Yumi;Seo, Hyunhee;Jo, Kyoung-nam;Jung, Dayae;Shin, Seungwon;Huh, Min;Roh, Yul
    • Journal of the Mineralogical Society of Korea
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    • v.31 no.2
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    • pp.113-121
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    • 2018
  • Baekasan Acheon cave located in Hwasun-gun, Jeollanam-do is a natural limestone cave only found in this province. In this study, the mineralogical and geochemical characteristics of speleothems collected from Baekasan Acheon cave were identified and the capability of carbonate mineral formation by aerobic microorganisms enriched from the cave and the mineralogical and geochemical characteristics of carbonate minerals formed by the microorganisms were investigated. The samples of sediments (clay) and speleothems (shelfstone and cave coral) were collected at three sites in the cave. The samples of shelfstone and cave coral were identified mainly as carbonate mineral, Mg-rich calcite, and clay minerals were composed of quartz, muscovite, and vermiculite by X-ray diffraction (XRD) analysis. To cultivate the carbonate forming microorganisms, parts of the sediment and speleothems were placed in D-1 medium containing urea, respectively, and the growth of microorganisms was observed under the aerobic condition at room temperature. The capability of carbonate mineralization of the cultured Baekasan Acheon cave microorganisms was examined through adding 1% (v/v) of the cultured microorganisms and calcium sources, Ca-acetate or Ca-lactate, into the D-1 medium. XRD analysis showed that the microorganisms cultured in cave deposits formed calcium carbonate ($CaCO_3$) under all conditions, and these microbial carbonate minerals included calcite and vaterite. The morphological characteristics and chemical composition of biologically formed minerals were observed by SEM-EDS showed various crystal forms such as rhomboid, spherical, perforated surface with Ca, C, and O of major chemical components. The existence of such microorganisms in the cave can contribute the formation of carbonate minerals, and it is likely to affect the geochemical cycles of carbon and calcium in the cave.

Mobility of Transition Metals by Change of Redox Condition in Dump Tailings from the Dukum Mine, Korea (덕음광산 광미의 산화${\cdot}$환원 조건에 따른 전이원소의 이동성)

  • 문용희;문희수;박영석;문지원;송윤구;이종천
    • Economic and Environmental Geology
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    • v.36 no.4
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    • pp.285-293
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    • 2003
  • Tailings of Dukum mine in the vadose and saturated zone were investigated to reveal the mobility of metal elements and the condition of mineralogical solubility according to redox environments throughout the geochemical analysis, thermodynamic modelling, and mineralogical study for solid-samples and water samples(vadose zone; distilled water: tailings=5 : 1 reacted, saturated zone; pore-water extracted). In the vadose zone, sulfide oxidation has generated low-pH(2.72∼6.91) condition and high concentration levels of S $O_4$$^{2-}$(561∼1430mg/L) and other metals(Zn : 0.12∼l57 mg/L, Pb : 0.06∼0.83 mg/L, Cd : 0.06∼l.35 mg/L). Jarosite$(KFe_3(SO_4)_2(OH)_6)$ and gypsum$(CaSO_4{\cdot}2H_2O$) were identified on XRD patterns and thermodynamics modelling. In the saturated zone, concentration of metal ions decreased because pH values were neutral(7.25∼8.10). But Fe and Mn susceptible to redox potential increased by low-pe values(7.40∼3.40) as the depth increased. Rhodochrosite$(MnCO_3)$ identified by XRD and thermodynamics modelling suggested that $Mn^{4+}$ or $Mn^{3+}$ was reduced to $Mn^{2+}$. Along pH conditions, concentrations of dissolved metal ions has been most abundant in vadose zone throughout borehole samples. It was observed that pH had more effect on metal solubilities than redox potential. How-ever, the release of co-precipitated heavy metals following the dissolution of Fe-Mn oxyhydroxides could be the mechanism by which reduced condition affected heavy metal solubility considering the decrease of pe as depth increased in tile saturated zone.

Mechanical Properties of Granulated Ground Blast Furnace Slag on Blended Activator of Sulfate and Alkali (황산염 및 알칼리계의 혼합 활성화제에 대한 고로슬래그미분말의 역학적 특성)

  • Kim, Tae-Wan;Jun, Yu-Bin;Eom, Jang-Sub
    • Journal of the Korea institute for structural maintenance and inspection
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    • v.19 no.5
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    • pp.104-111
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    • 2015
  • This study shows the mechanical properties of alkali-activated slag cement (AASC) synthesized using sulfate with NaOH solution. The used sulfates were calcium sulfate ($CaSO_4$, denoted CS) and sodium sulfate ($Na_2SO_4$, denoted SS). The replacement ratio of sulfates was 2.5, 5.0, 7.5 and 10.0% by weight of slag. NaOH solution of 2M and 4M concentration was used. A sample was activated with sulfate and activated with blended activator (blending NaOH solution with sulfate) respectively. 24 mix ratios were used and the water-binder weight ratio for the test was set 0.5. This research carried out the compressive strength, flexural strength, ultrasonic pulse velocity (UPV), absorption and X-ray diffraction (XRD). In the case of samples with CS, sample with 7.5% CS, sample with 2M NaOH+5.0% CS and sample with 4M NaOH+5.0% CS showed the good performance in the strength development. In the case of samples with SS, sample with 10.0% SS, sample with 2M NaOH+7.5% SS and sample with 4M NaOH+2.5% SS obtained good performance in strength. The results of UPV and water absorption showed a similar tendency to the strength properties. The XRD analysis of samples indicated that the hydration products formed in samples were ettringite, CSH and silicate phases. In this study, it is indicated that when compared to the use of sulfate only, the use of both sulfate and NaOH solution makes mechanical properties of AASC better.

Effects of Mn- and K-addition on Catalytic Activity of Calcium Oxide for Methane Activation (메탄 활성화반응에서 산화칼슘 촉매의 활성에 대한 망간과 칼륨의 첨가효과)

  • Park, Jong Sik;Kong, Jang Il;Jun, Jong Ho;Lee, Sung Han
    • Journal of the Korean Chemical Society
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    • v.42 no.6
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    • pp.618-628
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    • 1998
  • Pure CaO, Mn-doped CaO, Mn/CaO, and K/CaO catalysts were prepared and tested as catalysts for the oxidative coupling of methane in the temperature range of 600 to 800$^{\circ}C$ to investigate the effects of Mn- and K-addition on the catalytic activity of calcium oxide. To characterize the catalysts, X-ray powder diffraction(XRD), XPS, SEM, DSC, and TG analyses were performed. The catalytic reaction was carried out in a single-pass flow reactor using on-line gas chromatography system. Normalized reaction conditions were generally $p(CH_4)/p(O_2)=250$ Torr/50 Torr, total feed flow rate=30 mL/min, and 1 atm of total pressure with He being used as diluent gas. Among the catalysts tested, 6.3 mol% Mn-doped CaO catalyst showed the best $C_2$ yield of 8.0% with a selectivity of 43.2% at 775$^{\circ}C$. The $C_2$ selectivity increased on lightly doped CaO catalysts, while decreased on heavily doped CaO([Mn] > 6.3 mol%) catalysts. 6 wt.% Mn/CaO and 6 wt.% K/CaO catalysts showed the $C_2$ selectivities of 13.2% and 30.9%, respectively, for the reaction. Electrical conductivities of CaO and Mn-doped CaO were measured in the temperature range of 500 to 1000$^{\circ}C$ at Po2's of $10^{-3}\; to\;10^{-1}\;atm.$ The electrical conductivity was decreased with Mn-doping and increased with increasing $P0_2$in the range of $10^{-3}\;to\;10^{-1}\;atm,$ indicating the specimens to be p-type semiconductors. It was suggested that the interstitial oxygen ions formed near the surface can activate methane and the formation of interstitial oxygen ions was discussed on the basis of solid-state chemistry.

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