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Crystal Structure of Dehydrated Partially Ag$^+$-Exchanged Zeolite A, Ag$_{4.6}Na_{7.4}$-A, Treated with Hydrogen at 350${^{\circ}C}$

  • Kim Yang;Seff Karl
    • Bulletin of the Korean Chemical Society
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    • v.6 no.4
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    • pp.202-206
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    • 1985
  • The crystal structure of The crystal structure of $Ag^+$-Exchanged Zeolite A, $Ag_{4.6}Na_{7.4}-A$, dehydrated, treated with $H_2$, and evacuated, all at $350^{\circ}C$, has been determined by single crystal x-ray diffraction methods in the cubic space group Pm3m at $24(1)^{\circ}C;$ a = $12.208(2)\AA.$ The structure was refined to the final error indices R1 = 0.088 and R2 (weighted) = 0.069 using 194 independent reflections for which II_0$ > $3{\sigma}(I_0)$. On threefold axes near the centers of 6-oxygen rings, $7.4 Na^+$ ions and $0.6 Ag^+$ ions are found. Two non-equivalent 8-ring $Ag^+$ ions are found off the 8-ring planes, each containing about $0.6 Ag^+$ ions. Three non-equivalent Ag atom positions are found in the large cavity, each containing about 0.6 Ag atoms. This crystallographic analysis may be interpreted to indicate that $0.6 (Ag_6)^{3+}$ clusters are present in each large cavity. This cluster may be viewed as a nearly linear trisilver molecule $(Ag_3)^0$ (bond lengths, 2.92 and 2.94 $\AA;$ angle, $153^{\circ})$ stabilized by the coordination of each atom to a Ag^+$ ion at 3.30, 3.33, and 3.43 $\AA$, respectively. In addition, one of the silver atoms approaches all of the 0(1) oxygens of a 4-ring at $2.76\AA.$ Altogether $7.4 Na^+$ ions, $1.8 Ag^+$ ions, and 1.8 Ag atoms are located per unit cell. The remaining $1.0 Ag^+$ ion has been reduced and has migrated out of the zeolite framework to form silver crystallites on the surface of the zeolite single crystal.

Crystal Structure of Dehydrated Partially Ag$^+$-Exchanged Zeolite A treated with Cesium Vapor at 250${^{\circ}C}$

  • Kim, Duk-Soo;Song, Seong-Hwan;Kim, Yang
    • Bulletin of the Korean Chemical Society
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    • v.10 no.3
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    • pp.234-238
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    • 1989
  • The crystal structure of partially $Ag^+$-exchanged zeolite A, $Ag_{3.2}Na_{8.8}$-A, vacuum dehydrated at $360^{\circ}C$ and then exposed to 0.1 torr of cesium vapor for 12 hours at $250^{\circ}C$ has been determined by single-crystal X-ray diffraction techniques in the cubic space group Pm3m (a = 12.262(2)${\AA})\;at\;21(1)^{\circ}C$. The structure was refined to the final error indexes $R_1=0.068\;and\;R_2=0.072$ by using 338 reflections for which $I_o\;>\;3{\sigma}(I_o)$ and the composition of unit cell is $Ag_{3.2}Cs_{8.8}-A.\;3\;Cs^+$ ions lie on the centers of the 8-rings at sites of D4h symmetry. Two crystallographycally different 6-ring $Cs^+$ ions were found: 1.5 $Cs^+$ ions at Cs(2) are located inside of sodalite cavity and 4.3 $Cs^+$ ions at Cs(3) are located in the large cavity. The fractional occupancies observed at Cs(2) and Cs(3) indicate that the existence of at least three types of unit cells with regard to the 6-ring $Cs^+$ ions. For example, 50% of unit cells may have two $Cs^+$ ions at Cs(2) and 4 $Cs^+$ ions at Cs(3). 30% of unit cells may have one Cs+ ion at Cs(2) and 5 $Cs^+$ ions at Cs(3). The remaining 20% would have one $Cs^+$ ion at Cs(2) and 4 $Cs^+$ ions at Cs(3). On threefold axes of the unit cell two non-equivalent Ag atom positions are found in the large cavity, each containing 0.64 and 1.92 Ag atoms, respectively. A crystallographic analysis may be interpreted to indicate that 0.64 $(Ag_5)^+$ clusters are present in each large cavity. This cluster may be viewed as a tetrasilver molecule $(Ag_4)^0$(bond length, 2.84${\AA}$) stabilized by the coordination of one $Ag^+$ ion.

Structure of a Copper(Ⅱ) Hexaazamacrotricyclic Complex : (1,3,6,9,11,14-Hexaazatricyclo[12.2.1.16,9]octadecane)-copper(Ⅱ) Perchlorate

  • Cheon Manseog;Suh Paik Myunghyun;Shin Whanchul
    • Bulletin of the Korean Chemical Society
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    • v.13 no.4
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    • pp.363-367
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    • 1992
  • The crystal structure of (1,3,6,9,11,14-hexaazatricycol[12.2.1.$1^{6,9}$]octadecane)copper(Ⅱ) perchlorate, Cu($C_{12}H_{26}N_6$)$(ClO_4)_2$, has been determined by the X-ray diffraction methods. The crystal data are as follows: Mr=516.9, triclinic, ${\alpha}=8.572\;(2)$, b=8.499 (3), c=15.204 (3) ${\AA}$, ${\alpha}=80.42\;(5),\;{\beta}=73.57\;(3),\;{\gamma}=69.82\;(4)^{\circ},\;V=994.2\;{\AA}^3,\;D_C=1.726\;gcm^{-3}$, space group $P{\tilde{1}},\;Z=2,\;{\mu}=21.27\;cm^{-1}&, F(000)=534 and T=297 K. The structure was solved by direct methods and refined by full-matrix least-squares methods to and R value of 0.081 for 1608 observed reflections measured with graphite-mono-chromated Mo Ka radiation on a diffractometer. There are two independent complexes in the unit cell. The two copper ions lie at the special positions (1/2, 0, 0) and (0, 1/2, 1/2)and each complex possesses crystallographic center of symmetry. Each Cu ion is coordinated to four nitrogen donors if the hexaazamacrotricyclic ligand and weakly interacts with two oxygen atoms of the perchlorate ions to form a tetragonally distorted octahedral coordination geometry. The Cu_N (sec), Cu_N(tert) and Cu_O coordination distances are 1.985 (14), 2.055 (14) and 2.757 (13) ${\AA}$ for the complex A and 1.996 (10), 2.040 (11) and 2.660 (13) ${\AA}$ for the complex B, respectively. The macrocycles in the two independent cations assume a similar conformation with the average r.m.s. deviation of 0.073 ${\AA}$. Two 1,3-diazacyclopentane ring moieties of the hexaazamacrotricyclic ligand are placed oppositely and almost perpendicularly to the square coordination plane of the ruffled 14-membered macrocycle. The secondary N atoms are hydrogen-bonded to the perchlorate O atoms with distances of 3.017 (23) and 3.025 (19) ${\AA}$ for the complexes A and B, respectively.

Crystal Structure and Magnetic Properties of Sodium-Iron Phosphates NaFe0.9Mn0.1PO4 Cathode Material

  • Seo, Jae Yeon;Choi, Hyunkyung;Kim, Chul Sung;Lee, Young Bae
    • Journal of the Korean Physical Society
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    • v.73 no.12
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    • pp.1863-1866
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    • 2018
  • The sodium-iron phosphate maricite-$NaFe_{0.9}Mn_{0.1}PO_4$ was synthesized using the ball mill method. The crystal structure and magnetic properties of the prepared materials were studied using X-ray diffraction (XRD), vibrating sample magnetometer (VSM), and $M{\ddot{o}}ssbauer$ spectroscopy. Structural refinement of maricite-$NaFe_{0.9}Mn_{0.1}PO_4$ was analyzed using the FullProf program. From the XRD patterns, the crystal structure of maricite-$NaFe_{0.9}Mn_{0.1}PO_4$ was found to be orthorhombic with the space group Pmnb. The lattice parameters of maricite-$NaFe_{0.9}Mn_{0.1}PO_4$ are as follows: $a_0=6.866{\AA}$, $b_0=8.988{\AA}$, $c_0=5.047{\AA}$, and $V=311.544{\AA}^3$. Maricite-$NaFePO_4$ has an edge-sharing structure that consists of $FeO_6$ octahedral. Under an applied field of 100 Oe, the temperature dependences of zero-field-cooled (ZFC) and field-cooled (FC) curves were measured from 4.2 to 295 K. $M{\ddot{o}}ssbauer$ spectra were also recorded at various temperatures ranging from 4.2 to 295 K. We thus confirmed that the $N{\acute{e}}el$ temperature of $NaFe_{0.9}Mn_{0.1}PO_4$ ($T_N=14K$) was lower than that of maricite-$NaFePO_4$ ($T_N=15K$).

Study on the Quadcopter for Person Search using PID Control and HSV (PID 제어 및 HSV를 활용한 인명 수색용 쿼드콥터에 관한 연구)

  • Ji, Min-Seok;Kim, Byeong-Kwan;Kim, Jun-Woo;Park, Nae-Hyeok;Park, Hyoung-keun
    • The Journal of the Korea institute of electronic communication sciences
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    • v.17 no.1
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    • pp.139-146
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    • 2022
  • Mountain accidents such as forest fires and missing people are increasing as hikers increase due to indoor activities restrictions caused by the prolonged COVID-19 incident. If a dangerous situation occurs at outside where rescue workers cannot reach, the search time for person can be reduced using a quadcopter. Considering this, in this paper, Multiwii is used to smoothly hover the quadcopter by setting optimized PID values of the x-axis, y-axis, and z-axis (Yaw) according to the change in the inclination of the gas. In addition, after installing Open CV on Raspberry Pie, the camera uses HSV color space to filter the color such as the description of the person, and uses a thermal imaging camera to receive thermal sensing images in real time in environments where color extraction is difficult. As a result, it was confirmed that hovering was possible at a height of 2 to 8 m, blue extraction was possible at a height of 5 m, and heat detection was possible at a distance of less than 10 cm.

Particle loading as a design parameter for composite radiation shielding

  • Baumann, N.;Diaz, K. Marquez;Simmons-Potter, K.;Potter, B.G. Jr.;Bucay, J.
    • Nuclear Engineering and Technology
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    • v.54 no.10
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    • pp.3855-3863
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    • 2022
  • An evaluation of the radiation shielding performance of high-Z-particle-loaded polylactic acid (PLA) composite materials was pursued. Specimens were produced via fused deposition modeling (FDM) using copper-PLA, steel-PLA, and BaSO4-PLA composite filaments containing 82.7, 75.2, and 44.6 wt% particulate phase contents, respectively, and were tested under broad-band flash x-ray conditions at the Sandia National Laboratories HERMES III facility. The experimental results for the mass attenuation coefficients of the composites were found to be in good agreement with GEANT4 simulations carried out using the same exposure conditions and an atomistic mixture as a model for the composite materials. Further simulation studies, focusing on the Cu-PLA composite system, were used to explore a shield design parameter space (in this case, defined by Cu-particle loading and shield areal density) to assess performance under both high-energy photon and electron fluxes over an incident energy range of 0.5-15 MeV. Based on these results, a method is proposed that can assist in the visualization and isolation of shield parameter coordinate sets that optimize performance under targeted radiation characteristics (type, energy). For electron flux shielding, an empirical relationship was found between areal density (AD), electron energy (E), composition and performance. In cases where ${\frac{E}{AD}}{\geq}2MeV{\bullet}cm{\bullet}g^{-1}$, a shield composed of >85 wt% Cu results in optimal performance. In contrast, a shield composed of <10 wt% Cu is anticipated to perform best against electron irradiation when ${\frac{E}{AD}}<2MeV{\bullet}cm{\bullet}g^{-1}$.

Influence of Co incorporation on morphological, structural, and optical properties of ZnO nanorods synthesized by chemical bath deposition

  • Iwan Sugihartono;Novan Purwanto;Desy Mekarsari;Isnaeni;Markus Diantoro;Riser Fahdiran;Yoga Divayana;Anggara Budi Susila
    • Advances in materials Research
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    • v.12 no.3
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    • pp.179-192
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    • 2023
  • We have studied the structural and optical properties of the non-doped and Co 0.08 at.%, Co 0.02 at.%, and Co 0.11 at.% doped ZnO nanorods (NRs) synthesized using the simple low-temperature chemical bath deposition (CBD) method at 95℃ for 2 hours. The scanning electron microscope (SEM) images confirmed the morphology of the ZnO NRs are affected by Co incorporation. As observed, the Co 0.08 at.% doped ZnO NRs have a larger dimension with an average diameter of 153.4 nm. According to the International Centre for Diffraction Data (ICDD) number #00-036-1451, the x-ray diffraction (XRD) pattern of non-doped and Co-doped ZnO NRs with the preferred orientation of ZnO NRs in the (002) plane possess polycrystalline hexagonal wurtzite structure with the space group P63mc. Optical absorbance indicates the Co 0.08 at.% doped ZnO NRs have stronger and blueshift bandgap energy (3.104 ev). The room temperature photoluminescence (PL) spectra of ZnO NRs exhibited excitonicrelates ultraviolet (UV) and defect-related green band (GB) emissions. By calculating the UV/GB intensity, the Co 0.08 at.% is the proper atomic percentage to have fewer intrinsic defects. We predict that Co-doped ZnO NRs induce a blueshift of near band edge (NBE) emission due to the Burstein-Moss effect. Meanwhile, the redshift of NBE emission is attributed to the modification of the lattice dimensions and exchange energy.

Measurement of S1 foramen depth for ultrasound-guided S1 transforaminal epidural injection

  • Ye Sull Kim;SeongOk Park;Chanhong Lee;Sang-Kyi Lee;A Ram Doo;Ji-Seon Son
    • The Korean Journal of Pain
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    • v.36 no.1
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    • pp.98-105
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    • 2023
  • Background: Ultrasound-guided first sacral transforaminal epidural steroid injection (S1 TFESI) is a useful and easily applicable alternative to fluoroscopy or computed tomography (CT) in lumbosacral radiculopathy. When a needle approach is used, poor visualization of the needle tip reduces the accuracy of the procedure, increasing its difficulty. This study aimed to improve ultrasound-guided S1 TFESI by evaluating radiological S1 posterior foramen data obtained using three-dimensional CT (3D-CT). Methods: Axial 3D-CT images of the pelvis were retrospectively analyzed. The radiological measurements obtained from the images included 1st posterior sacral foramen depth (S1D, mm), 1st posterior sacral foramen width (S1W, mm), the angle of the 1st posterior sacral foramen (S1A, °), and 1st posterior sacral foramen distance (S1ds, mm). The relationship between the demographic factors and measured values were then analyzed. Results: A total of 632 patients (287 male and 345 female) were examined. The mean S1D values for males and females were 11.9 ± 1.9 mm and 10.6 ± 1.8 mm, respectively (P < 0.001); the mean S1A 28.2 ± 4.8° and 30.1 ± 4.9°, respectively (P < 0.001); and the mean S1ds, 24.1 ± 2.9 mm and 22.9 ± 2.6 mm, respectively (P < 0.001); however, the mean S1W values were not significantly different. Height was the only significant predictor of S1D (β = 0.318, P = 0.004). Conclusions: Ultrasound-guided S1 TFESI performance and safety may be improved with adjustment of needle insertion depth congruent with the patient's height.

The comparison of the accuracy of temporary crowns fabricated with several 3D printers and a milling machine

  • Junsik Lee;Sungwon Ju;Jihyung Kim;Sion Hwang;Jinsoo Ahn
    • The Journal of Advanced Prosthodontics
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    • v.15 no.2
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    • pp.72-79
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    • 2023
  • PURPOSE. The purpose of this in vitro study was to compare the accuracy of various 3D printers and a milling machine. MATERIALS AND METHODS. The die model was designed using CAD (Autodesk Inventor 2018 sp3). The 30 ㎛ cement space was given to the die and the ideal crown of the mandibular left first molar was designed using CAD (ExoCAD). The crowns were produced using the milling machine (Imes-icore 250i) and the 3D printers (Zenith U, Zenith D, W11) and they were divided into four groups. In all groups, the interior of each crown was scanned (Identica blue) and superimposed (Geomagic Control X) with the previously designed die. The difference between the die and the actual crown was measured at specific points. The Kruskal-Wallis test, the Mann-Whitney test, and Bonferroni's method were performed with a statistical analysis software (P < .008 in inter-group comparison P < .001 in intra-group comparison). RESULTS. In all groups, the center of the occlusal area and the anti-rotational dimple area showed significantly greater difference and the marginal area showed the smallest difference comparatively. The mean value of the difference in each area and the sum of the differences were higher in order of W11, Imes-icore 250i, Zenith D, and Zenith U. CONCLUSION. The digital light processing (DLP) method shows higher accuracy compared to the sereolithography (SLA) method using the same resin material.

A novel method of objectively detecting tooth ankylosis using cone-beam computed tomography: A laboratory study

  • Luciano Augusto Cano Martins;Danieli Moura Brasil;Deborah Queiroz Freitas;Matheus L Oliveira
    • Imaging Science in Dentistry
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    • v.53 no.1
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    • pp.61-67
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    • 2023
  • Purpose: The aim of this study was to objectively detect simulated tooth ankylosis using a novel method involving cone-beam computed tomography (CBCT). Materials and Methods: Tooth ankylosis was simulated in single-rooted human permanent teeth, and CBCT scans were acquired at different current levels (5, 6.3, and 8 mA) and voxel sizes (0.08, 0.125, and 0.2). In axial reconstructions, a line of interest was perpendicularly placed over the periodontal ligament space of 21 ankylosed and 21 non-ankylosed regions, and the CBCT grey values of all voxels along the line of interest were plotted against their corresponding X-coordinates through a line graph to generate a profile. The image contrast was increased by 30% and 60% and the profile assessment was repeated. The internal area of the resulting parabolas was obtained from all images and compared between ankylosed and non-ankylosed regions under different contrast enhancement conditions, voxel sizes, and mA levels using multi-way analysis of variance with the Tukey post hoc test(α=0.05). Results: The internal area of the parabolas of all non-ankylosed regions was significantly higher than that of the ankylosed regions(P<0.05). Contrast enhancement led to a significantly greater internal area of the parabolas of non-ankylosed regions (P<0.05). Overall, voxel size and mA did not significantly influence the internal area of the parabolas(P>0.05). Conclusion: The proposed novel method revealed a relevant degree of applicability in the detection of simulated tooth ankylosis; increased image contrast led to greater detectability.