Mineral carbonation is a technology in which carbonates are synthesized from minerals including serpentine and olivine, and industrial wastes such as slag and cement, of which all contain calcium or magnesium when reacted with carbon dioxide. This study aims to develop the mineral carbonation technology for commercialization, which can reduce environmental burden and process cost through the reduction of carbon dioxide using steel slag and the slag reuse after calcium extraction. Calcium extraction was conducted using NH4Cl solution for air-cooled slag and convert slag, and ${\geq}98%$ purity calcium carbonate was synthesized by reaction with calcium-extracted solution and carbon dioxide. And we conducted experimentally to minimize the quantity of by-product, the slag residue after calcium extraction, which has occupied large amount of weight ratio (about 80-90%) at the point of mineral carbonation process using slag. The slag residue was used to replace silica sand in the manufacture of cement panel, and physical properties including compressive strength and flexible strength of panel using the slag residue and normal cement panel, respectively, were analyzed. The calcium concentration in extraction solution was analyzed by inductively coupled plasma optical emission spectrometer (ICP-OES). Field-emission scanning electron microscope (FE-SEM) was also used to identify the surface morphology of calcium carbonate, and XRD was used to analyze the crystallinity and the quantitative analysis of calcium carbonate. In addition, the cement panel evaluation was carried out according to KS L ISO 679, and the compressive strength and flexural strength of the panels were measured.
Park, Kwang-Min;Cho, Young-Keun;Ra, Jung-Min;Kim, Hyung-Suk
Journal of the Korea institute for structural maintenance and inspection
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v.21
no.1
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pp.109-116
/
2017
This paper describes the investigation into the durability alkali-activated materials(AAM) mortar and paste samples manufactured using fly-ash(FA) and ground granulated blast furnace slag(GGBFS) exposed to a sulfate environment with different GGBFS replace ratios(30, 50 and 100%), sodium silicate modules($Ms[SiO_2/Na_2O]$ 1.0, 1.5 and 2.0). The tests involved immersions into 10% sodium sulfate solution($Na_2SO_4$), 10% magnesium sulfate solution($MgSO_4$), 10% magnesium nitrate solution($Mg(NO_3)_2$) and 5% magnesium nitrate($Mg(NO_3)_2$+5% sodium sulfate solution+$Na_2SO_4$). The evolution of compressive strength, weight, length expansion and microstructural observation such as x-ray diffraction were studied. As a results, in case of immersed in $Na_2SO_4$, $Mg(NO_3)_2$ and $Mg(NO_3)_2+Na_2SO_4$ shows increase in long-term strength. However, for samples immersed in $MgSO_4$, the general observation was that the compressive strength decreased after immersion. The most drastic reduction of compressive strength and expansion of weight and length occurred when GGBFS or Ms ratios were higher. Also, the XRD analysis of samples immersed in magnesium sulfate indicated that expansion of AAM caused by gypsum($CaSO_4{\cdot}2H_2O$) and brucite(MgOH). The results showed that, an additional condition $Mg^{2+}$ in which ${SO_4}^{2-}$ is the presence of a certain concentration, sulfate erosion has to be accelerated.
Multi-anvil press (MAP) is one of the high pressure apparatuses and often generates the pressure-conditions ranging from 5 to 25 GPa and temperature-conditions up to $2,300^{\circ}C$. The MAP is, therefore, suitable to explore the pressure-induced structural changes in diverse earth materials from Earth's mantle and the bottom of the mantle transition zone (~660 km). In this study, we present the experimental results for pressure-load calibration of the 1,100-ton multi-anvil press equipped in the authors' laboratory. The pressure-load calibration experiments were performed for the 14/8 step, 14/8 G2, 14/8 HT, and 18/12 assembly sets. The high pressure experiments using ${\alpha}$-quartz, wollastonitestructure of $CaGeO_3$, and forsterite as starting materials were analyzed by powder X-ray diffraction spectroscopy. The phase transition of each mineral indicates the specific pressure that is loaded to a sample at $1,200^{\circ}C$: a transition of ${\alpha}$-quartz to coesite at 3.1 GPa, that of garnet-structure of $CaGeO_3$ to perovskite-structure at 5.9 GPa, that of coesite to stishovite at 9.2 GPa, and that of forsterite to wadsleyite at 13.6 GPa. While the estimated pressure-load calibration curve is generally consistent with those obtained in other laboratories, the deviation up to 50 tons is observed at high pressure above 10 GPa. This is partly because of the loss of oil pressure at high pressure resulting from the differences in a sample chamber, and the frictional force between pressure medium and second anvil. We also report the ${\sim}200^{\circ}C/mm$ of thermal gradient in the vertical direction of the sample chamber of 14/8 HT assembly. The pressure-load calibration curve and the observed thermal gradient within the sample chamber can be applied to explain the structural changes and the relevant macroscopic properties of diverse crystalline and amorphous earth materials in the mantle.
The Ag-Pd-Cu alloys containing a small amount of Au is commonly used for dental purposes, because this alloy cheaper than Au-base alloys for clinical use. However, the most important characteristic of this alloy is age-hardenability, which is not exhibited by other Ag-base dental alloys. The specimens used were Ag-30Pd-10Cu ternary alloy and Au addition alloy. These alloys were melted and casted by induction electric furnace and centrifugal casting machine in Ar atmosphere. These specimens were solution treated for 2hr at $800^{\circ}C$ and were then quenched into iced water, and aged at 350-$550^{\circ}C$ Age-hardening characteristic of the small Au-containing Ag-Pd-Cu dental alloys were investigated by means of hardness testing, X-ray diffraction and electron microscope observations, electrical resistance, differential scanning calorimetric, energy dispersed spectra and electron probe microanalysis. Principal results are as follows ; Maximum hardening occured in two co-phases of ${\alpha}_2$ + PdCu In stage II, decomposition of the $\alpha$ solid solution to a PdCu ordered phase($L1_o$ type) and an Ag-rich ${\alpha}_2$ phase occurred and a discontinuous precipitation occurred at the grain boundary. From the electron microscope study, it was concluded that the cause of age-hardening in this alloy is the precipitation of the PdCu redered phase, which has AuCu I type face-centered tetragonal structure. Precipitation procedure was ${\alpha}{\to}{\alpha}_1+PdCu{\to}{\alpha}_2+PdCu$ at Pd/Cu = 3 Pd element of Ag-Pd-Cu alloy is more effective dental alloy on anti-corrosion and is suitable to isothermal ageing at $450^{\circ}C$.
The Ag-Pd-Cu alloys containing a small amount of Au is commonly used for dental purposes, because this alloy is cheaper than Au-base alloys for clinical use. However, the most important characteristic of this alloy is age-hardenability, which is not exhibited by other Ag-base dental alloys. The specimens used were Ag-20Pd-20Cu ternary alloy and Au addition alloy. These alloys were melted and casted by induction electic furace and centrifugal casting machine in Ar atmoshpere. These specimens were solution treated for 2hr at $800^{\circ}C$ and were then quenched into iced water, and aged at $350{\sim}550^{\circ}C$ Age-hardening characteristics of the small Au-containing Ag-pPd-Cu dental alloys were investigated by means of hardness testing, X-ray diffraction and electron microscope observations, electrical resistance, differential scanning calorimetric, emergy dispersed spectra and electron probe microanalysis. Principal results are as follows : Hardening occured in two stages, I. e., stage I in low temperature and stage II in high temperature regions, during continuous aging. The case of hardening in stage I was due to the formation of the Llo type face centered tetragonal PdCu-ordered phase in the grain interior and hardening in stage I was affedted by the Cu concentration. In stage II, decomposition of the $\alpha$ solid solution to a PdCu ordered phase(L1o type) and an Agrich ${\alpha}2$ phase occurred and a discontiunous precipitation occurred at the grain boundary. Form the electron microscope study, it was concluded that the cause of age-hardening in this alloy is the precipitation of the PdCu ordered phase, which has AuCu I type face-centered tetragonal structure. Precipitation procedure was ${\alpha}\to{\alpha}+{\alpha}2+PdCu\to{\alpha}1+{\alpha}2+PdCu$ at Pd/Cu = 1 Ag-Pd-Cu alloy is more effective dental alloy as ageing treatment and is suitable to isothermal ageing at $450^{\circ}C$.
Seo, Sung-Man;Kim, Ghyung-Hwa;Lee, Seok-Hee;Bae, Jun-Seok;Lim, Woo-Taik
Bulletin of the Korean Chemical Society
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v.30
no.6
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pp.1285-1292
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2009
Large single crystals of zeolite, |$Na_{75}$|[$Si_{117}Al_{75}O_{384}$]-FAU (Na-Y, Si/Al = 1.56), were synthesized from gels with composition of 3.58Si$O_2$ : 2.08NaAl$O_2$ : 7.59NaOH : 455$H_2$O : 5.06TEA : 2.23TCl. One of these, a colorless single-crystal was ion exchanged by allowing aqueous 0.02 M CsOH to flow past the crystal at 293 K for 3 days, followed by dehydration at 673 K and 1 ${\times}\;10^{-6}$ Torr for 2 days. The crystal structure of fully dehydrated partially $Cs^+$-exchanged zeolite Y, |$Cs_{45}Na_{30}$|[$Si_{117}Al_{75}O_{384}$]-FAU per unit cell (a = 24.9080(10) $\AA$) was determined by single-crystal X-ray diffraction technique in the cubic space group Fd $\overline{3}$ m at 294(1) K. The structure was refined using all intensities to the final error indices (using only the 877 reflections with $F_o\;>\;4{\sigma}(F_o))\;R_1$ = 0.0966 (Based on F) and $R_2\;=\;0.2641\;(Based\;on\;F^2$). About forty-five $Cs^+$ ions per unit cell are found at six different crystallographic sites. The 2 $Cs^+$ ions occupied at site I, at the centers of double 6-ring (D6Rs, Cs-O = 2.774(10) $\AA$ and O-Cs-O = 88.9(3) and 91.1(3)$^o$). Two $Cs^+$ ions are found at site I’ in the sodalite cavity; the $Cs^+$ ions were recessed 2.05 $\AA$ into the sodalite cavity from their 3-oxygen plane (Cs-O = 3.05(3) $\AA$ and O-Cs-O = 77.4(13)$^o$). Site-II’ positions (opposite single 6-rings in the sodalite cage) are occupied by 7 $Cs^+$ ions, each of which extends 2.04 $\AA$ into the sodalite cage from its 3-oxygen plane (Cs-O = 3.067(11) $\AA$ and O-Cs-O = 80.1(3)$^o$). The 26 $Cs^+$ ions are nearly three-quarters filled at site II in the supercage, being recessed 2.34 $\AA$ into the supercage (Cs-O = 3.273(8) $\AA$ and O-Cs-O = 74.3(3)$^o$). The 4 $Cs^+$ ions are found at site III deep in the supercage (Cs-O = 3.321(19) and 3.08(3) $\AA$), and 4 $Cs^+$ ions at another site III’ (Cs-O = 2.87(4) and 3.38(4) $\AA$). About 30 $Na^+$ ions per unit cell are found at one crystallographic site; The $Na^+$ ions are located at site I’ in the sodalite cavity opposite double 6-rings (Na-O = 2.578(11) $\AA$ and O-Na-O = 97.8(4)$^o$).
Bang, Byoung Man;Park, No-Kuk;Han, Gi Bo;Yoon, Suk Hoon;Lee, Tae Jin
Korean Chemical Engineering Research
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v.45
no.6
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pp.566-572
/
2007
Two hybrid catalysts for the direct synthesis of DME were prepared and the catalytic activity of these catalysts were investigated. The hybrid catalyst for the direct synthesis of DME was composed as the catalytic active components of methanol synthesis and dehydration. The methanol synthesis catalyst was formed from the precursor contained Cu and Zn, the methanol dehydration catalyst was used ${\gamma}-Al_2O_3$. As PM-CZ+D and CP-CZA/D, Two hybrid catalysts were prepared by physical mixing method (PM-CZ+D) and precipitation method (CP-CZA/D), respectively. PM-CZ+D was prepared by physically mixing methanol synthesis catalyst and methanol dehydration catalyst, CP-CZA/D was prepared by depositing Cu-Zn or Cu-Zn-Al components on ${\gamma}-Al_2O_3$. The crystallinity and the surface morphology of synthesized catalyst were analyzed by X-ray diffraction (XRD) and scanning electron microscope (SEM) to investigate the physical property of prepared catalyst. And BET surface area by $N_2$ adsorption and the surface area of Cu by $N_2O$ chemisorption were investigated about the hybrid catalysts. In addition, catalytic activity of these hybrid catalysts was examined with varying reaction conditions. At that time, the reaction temperature of $250{\sim}290^{\circ}C$, the reaction pressure of 50~70 atm, the $[H_2]/[CO]$ mole ratio of 0.5~2.0 and the space velocity of $1,500{\sim}6,000h^{-1}$ were investigated the catalytic activity. From these results, it was confirmed that the reactivity of CP-CZA/D was higher than that of PM-CZ+D. When the conditions of reaction temperature, pressure, $[H_2]/[CO]$ ratio and space velocity were $260^{\circ}C$, 50 atm and 1.0, $3,000h^{-1}$ respectively, CO conversion using CP-CZA/D hybrid catalyst was 72% and the CO conversion of CP-CZA/D was more than 20% compared with the CO conversion of PM-CZ+D. It was known that Cu surface area of CP-CZA/D hybrid catalyst was higher than that of hybrid PM-CZ+D catalyst using $N_2O$ chemisorption. It was assumed that the catalytic activity was improved because Cu particle of hybrid catalyst prepared by precipitation method was well dispersed.
In this study, we investigated the structure and properties of a highly heat conductive metal-ceramic core-shell CoAl2O4@Al micro-composite for heterogeneous catalysts support. The CoAl2O4@Al was prepared by hydrothermal surface oxidation of Al metal powder, which resulted in the structure with a high heat conductive Al metal core encapsulated by a high surface area CoAl2O4 shell. For comparison, CoAl2O4 was also prepared by co-precipitation method and also utilized for a catalyst support. Rh catalysts supported on CoAl2O4@Al and CoAl2O4 were prepared by incipient wetness impregnation and characterized by N2 adsorption, X-ray diffraction (XRD), scanning electron microscopy (SEM), CO chemisorption, and temperature-programmed reduction (TPR). The properties of catalysts were investigated for glycerol steam reforming reaction for hydrogen production at 550 ℃. Rh/CoAl2O4@Al exhibited about 2.8 times higher glycerol conversion turnover frequency (TOF) than Rh/CoAl2O4 due to facilitated heat transport through the core-shell structure. The CoAl2O4@Al and CoAl2O4 also showed some catalytic activities due to a partial reduction of Co on the support, and a higher catalytic activity was also found on the CoAl2O4@Al core-shell than CoAl2O4. These catalysts, however, displayed deactivation on the reaction stream due to carbon deposition on the catalysts surface.
The samples were synthesized by using a solid state reaction. The X-ray diffraction pattern for $Ti_{0.96}Co_{0.02}Fe_{0.02}O_2$ showed a pure rutile phase with tetragonal structure, Mixtures of the proper proportions of the elements sealed in evacuated quartz ampoule were heated at $870{\sim}930^{\circ}C$ for one day and then slowly cooled down to room temperature at a rate of $10^{\circ}C$/h. In order to obtain single phase material, it was necessary to grind the sample after the first firing and to press the powders into pellets before annealing them for a second time in evacuated and sealed quartz ampoule. Magnetic properties have been investigated using the vibrating sample magnetometer (VSM). Room temperature magnetic hysteresis (M-H) curve showed an obvious ferromagnetic behavior and the magnetic moment per Fe atom under the applied of 0.8 T was estimated to be about $1.5\;{\mu}_B$/CoFe. But the magnetic moment per Fe atom under the applied of 0.8 T was estimated to be about $0.02\;{\mu}_B$/CoFe without Ti-getter. Size of particles is about $1\;{\mu}m$ using the transmission electron microscope (TEM). The ingredients of sample are distributed irregular in particles. Only Fe get shown on the surface of particles.
Kim, Joung-Ryul;Park, Jong-Sung;Choi, Young-Youn;Song, Oh-Sung
Journal of the Korean Vacuum Society
/
v.17
no.6
/
pp.528-537
/
2008
60 nm and 20 nm thick hydrogenated amorphous silicon(a-Si:H) layers were deposited on 200 nm $SiO_2$/single-Si substrates by inductively coupled plasma chemical vapor deposition(ICP-CVD). Subsequently, 30 nm-Ni layers were deposited by an e-beam evaporator. Finally, 30 nm-Ni/(60 nm and 20 nm) a-Si:H/200 nm-$SiO_2$/single-Si structures were prepared. The prepared samples were annealed by rapid thermal annealing(RTA) from $200^{\circ}C$ to $500^{\circ}C$ in $50^{\circ}C$ increments for 40 sec. A four-point tester, high resolution X-ray diffraction(HRXRD), field emission scanning electron microscopy(FE-SEM), transmission electron microscopy(TEM), and scanning probe microscopy(SPM) were used to examine the sheet resistance, phase transformation, in-plane microstructure, cross-sectional microstructure, and surface roughness, respectively. The nickel silicide from the 60 nm a-Si:H substrate showed low sheet resistance from $400^{\circ}C$ which is compatible for low temperature processing. The nickel silicide from 20 nm a-Si:H substrate showed low resistance from $300^{\circ}C$. Through HRXRD analysis, the phase transformation occurred with silicidation temperature without a-Si:H layer thickness dependence. With the result of FE-SEM and TEM, the nickel silicides from 60 nm a-Si:H substrate showed the microstructure of 60 nm-thick silicide layers with the residual silicon regime, while the ones from 20 nm a-Si:H formed 20 nm-thick uniform silicide layers. In case of SPM, the RMS value of nickel silicide layers increased as the silicidation temperature increased. Especially, the nickel silicide from 20 nm a-Si:H substrate showed the lowest RMS value of 0.75 at $300^{\circ}C$.
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