• Economic and Environmental Geology
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• v.45 no.2
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• pp.79-88
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• 2012

The increased brightness and focused X-ray beams now available from laboratory X-ray sources facilitates a variety of powder diffraction experiments not practical using conventional in-house sources. Furthermore, the increased availability of 2-dimensional area detectors, along with implementation of improved software and customized sample environmental cells, makes possible new classes of in-situ and time-resolved diffraction experiments. These include phase transitions under variable pressure- and temperature conditions and ion-exchange reactions. Examples of in-situ and time-resolved studies which are presented here include: (1) time-resolved data to evaluate the kinetics and mechanism of ion exchange in mineral natrolite; (2) in-situ dehydration and thermal expansion behaviors of ion-exchanged natrolite; and (3) observations of the phases forming under controlled hydrostatic pressure conditions in ion-exchanged natrolite. Both the quantity and quality of the in-situ diffraction data are such to allow evaluation of the reaction pathway and Rietveld analysis on selected dataset. These laboratory-based in-situ studies will increase the predictability of the follow-up experiments at more specialized beamlines at the synchrotron.

• Economic and Environmental Geology
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• v.42 no.5
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• pp.509-512
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• 2009

Powder diffraction patterns of the zeolite mesolite ($Na_{5.33}Ca_{5.33}Al_{16}Si_{24}O_{80}{\cdot}21.33H_2O$), with a natrolite framework topology were measured as a function of pressure up to 5.0 GPa using a diamond-anvil cell and a $200{\mu}m$-focused monochromatic synchrotron X-ray. Under the hydrostatic conditions mediated by pore-penetrating alcohol and water mixture, the elastic behavior of mesolite is characterized by continuous volume expansion between ca. 0.5 and 1.5 GPa, which results from expansion in the ab-plane and contraction along the c-axis. Subsequent to this anomalous behavior, changes in the powder diffraction patterns suggest possible reentrant order-disorder transition. The ordered layers of sodium- and calcium-containing channels in a 1:2 ratio along the b-axis attribute to the $3b_{natrolite}$ cell below 1.5 GPa. When the volume expansion is completed above 1.5 GPa, such characteristic ordering reflections disappear and the $b_{natrolite}$ cell persists with marginal volume contraction up to ca. 2.5 GPa. Further increase in pressure leads to progressive volume contraction and appears to generate another set of superlattice reflections in the $3c_{natrolite}$ cell. This suggests that mesolite in the pressure-induced hydration state experiences order-disorder-order transition involving the motions of sodium and calcium cations either through cross-channel diffusion or within the respective channels.

• Journal of the Mineralogical Society of Korea
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• v.19 no.3 s.49
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• pp.189-195
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• 2006

Compression work on a pyrite powder has been carried out using energy dispersive X-ray diffraction (EDXRD) with Mao-Bell type diamond anvil cell (DAC) and synchrotron radiation(SR) at room temperature. It has been reported the bulk moduli of pyrite show the large variations depending on the experimental conditions as well as the apparatus used. Thus, two kinds of sample in different pressure transmitting media of both NaCl and MgO powder emerged in alcoholic fluids were subjected to measure their compressibilities. Bulk moduli thus obtained are 138.9 GPa and 198.2 GPa, respectively, and this result contradicts to the anticipated values according to the hydrostaticity conditions of the sample chamber. This might be due to the alcoholic fluids phase transition mainly with the side effects from the difference of both solid state detector (SSD) used and E*d value applied. All experiments were performed at the Beam Line 1B2 of Pohang Light Source (PLS).

• Economic and Environmental Geology
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• v.49 no.1
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• pp.23-30
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• 2016

Powder samples of natural lawsonite (Ca-lawsonite, $CaAl_2Si_2O_7(OH)_2{\cdot}H_2O$) was studied structurally up to 8 GPa at room temperature using monochromatic synchrotron X-ray powder diffraction and a diamond anvil cell (DAC) with a methanol : ethanol : water (16 : 3 : 1 by volume) mixture solution as a penetrating pressure transmitting medium (PTM). Upon pressure increase, lawsonite does not show any apparent pressure induced expansion (PIE) or phase transition. Pressure-volume data were fitted to a second-order Birch-Murnaghan equation of state using a fixed pressure derivative of 4 leading to a bulk modulus ($B_0$) of 146(6) GPa. This compression is further characterized to be isotropic with calculated linear compressibilities of ${\beta}^a=0.0022GPa^{-1}$, ${\beta}^b=0.0024GPa^{-1}$, and ${\beta}^c=0.0020GPa^{-1}$.

• Korean Journal of Mineralogy and Petrology
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• v.34 no.3
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• pp.169-176
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• 2021

This study aimed to fundamentally understand structural changes of zeolite under pressure and in the presence of different pressure-transmitting media (PTM) for application studies such as immobilization of heavy metal cation or CO₂ storage using pressure. High-pressure X-ray powder diffraction study was conducted on the zeolite-W (K_6.4Al_6.5Si_25.8O₆₄× 15.3H₂O, K-MER) to understand linear compressibility and the bulk moduli in different PTM conditions. Zeolite-w is a synthetic material having the same framework as natural zeolite merlinoite ((K, Ca_0.5, Ba_0.5, Na)₁₀ Al₁₀Si₂₂O₆₄× 22H₂O). The space group of the sample was identified as I4/mmm belonging to the tetragonal crystal system. Water, carbon dioxide, and silicone-oil were used as pressure-transmitting media. The mixture of sample and each PTM was mounted in a diamond anvil cell (DAC) and then pressurized up to 3 GPa with an increment of ca. 0.5 GPa. Pressure-induced changes of powder diffraction patterns were measured using a synchrotron X-ray light source. Lattice constants, and bulk moduli were calculated using the Le-Bail method and the Birch-Murnaghan equation. In all PTM conditions, linear compressibility of c-axis (𝛽^c) was 0.006(1) GPa^-1 or 0.007(1) GPa^-1. On the other hand, the linear compressibility of a(b)-axis (𝛽^a) was 0.013(1) GPa^-1 in silicone-oil run, which is twice more compressible than the a(b)-axis in water and carbon dioxide runs, 𝛽^a = 0.006(1) GPa^-1. The bulk moduli were measured as 50(3) GPa, 52(3) GPa, and 29(2) GPa in water, carbon dioxide, and silicone-oil run, respectively. The orthorhombicities of ac-plane in the water, and carbon dioxide runs were comparatively constant, near 0.350~0.353, whereas the value decreased abruptly in the silicone-oil run following formula, y = -0.005(1)x + 0.351(1) by non-penetrating pressure fluid condition.

• Korean Journal of Mineralogy and Petrology
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• v.33 no.1
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• pp.11-18
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• 2020

High-pressure synchrotron X-ray powder diffraction experiments were performed on natural illite (K_0.65Al₂(Al_0.65Si_3.35)O₁₀(OH)₂) using diamond anvil cell (DAC) under two different pressure transmitting media (PTM), i.e., water and ME41 (methanol:ethanol = 4:1 by volume). When using water as PTM, occasional heating was applied up to about 250℃ while reaching pressure up to 2.7 GPa in order to promote both hydrostatic conditions and intercalation of water molecules into the layer. When using ME41, pressure was reached up to 6.9 GPa at room temperature. Under these conditions, illite did not show any expansion of interlayer distance or phase transitions. Pressure-volume data were used to derive bulk moduli (K₀) of 45(3) GPa under water and 51(3) GPa under ME41 PTM. indicating no difference in compressibility within the analytical error. Linear compressibilities were then calculated to be β^a = 0.0025, β^b = 0.0029, β^c = 0.0144 under ME41 PTM showing the c-axis is ca. six times more compressible than a- and b-axes. These elastic behaviors of illite were compared to muscovite, one of its structural analogues.

• Korean Journal of Mineralogy and Petrology
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• v.35 no.4
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• pp.423-430
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• 2022

Pressure-dependent elastic behavior and chemical reaction of natural sepiolite (Mg₈Si₁₂O₃₀(OH)₄·12H₂O) was studied under two different pressure-transmitting medium (PTM) conditions using synchrotron X-ray powder diffraction. Under non pore-penetrating silicone oil PTM, we observed that the b-axis length increases up to ca. 3.6 GPa, marking an anisotropic compression region with negative linear compressibility of β^b= -0.0012 GPa^-1, which then decreases at 7.7 GPa. Under pore-penetrating water PTM, the anisotropic compression behavior is enhanced with doubled negative linear compressibility of β^b= -0.0025 GPa^-1 up to 3.2 GPa, where transformation into stevensite is observed upon ex-situ temperature treatment at 280 ℃ as confirmed via XRD and SEM. Derived bulk moduli (K₀) and linear compressibilities (β) were compared to other structurally and chemically related minerals.