• 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.

• Bulletin of the Korean Chemical Society
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• v.14 no.2
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• pp.266-271
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• 1993

The reaction of $(CO_5$)M=C(OMe)Tol (M=Cr, Mo, W and $Tol=p-C_6H_4Me)$ and $BBr_3$ followed by treatment with tetramethylethylenediamine (TMEDA) yields a mixture of two diastereomers, trans, $cis-Br(CO)_2(tmeda)M{\equiv}$CTol [M=Cr(1a), Mo(2a), W(3a)] and cis, $trans-Br(CO)_2(tmeda)M{\equiv}$CTol [M=Cr(1b), Mo(2b), W(3b)], respectively. These compounds have been isolated as crystalline solids and characterized by spectroscopic (infrared, mass, $^1H$ and $^{13}C-NMR)$ data. The trans, cis-Br(CO)2(tmeda)Cr${\equiv}$CTol (1a), has been examine via a single crystal X-ray diffraction study : $BrCrO_2N_2C_{16}H_{23}$, Mr=407.27, triclinic, $P{\bar{1}},\;a=12.792(2),\;b=13.400(5),\;c= 11.645(4)\;{\AA},\;{\alpha}=101.26(2)^{\circ},\;{\beta}=103.04(2)^{\circ},\;{\gamma}=91.88(2)^{\circ},\;{\nu}=1907(1){\AA}^3,\;Z=2,\;{\rho}(calcd)=1.418\;gcm^{-3},\;{\lambda}(MoK{\alpha})=0.71069\;{\AA},\;{\mu}=26.25 cm^{-1},\;F(000)=831.97,\;T=295K,\;R=0.0977$ for 1332 significant reflections $[F_0>5{\sigma}(F_0)]$. There are two essentially equivalent molecules in the crystallographic asymmetric unit. Each molecule is octahedral with the bromide ligand trans to the alkylidyne carbon, the two cis-carbonyl ligands, and the bidentate TMEDA ligand.

• 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.

• Korean Journal of Metals and Materials
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• v.49 no.2
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• pp.93-103
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• 2011

Precipitation behavior of high-nitrogen duplex Fe-24Cr-7Mn-4Ni-4Mo-0.43N stainless steel aged at $850^{\circ}C$ was investigated using scanning transmission electron microscopy. Based on the analyses of selected area diffraction patterns, four kinds of precipitates (intermetallic sigma (${\sigma}$) and chi (${\chi}$), $Cr_2N$ and secondary austenite) were identified. At the ferrite/austenite phase boundary, the ${\sigma}$ phase and secondary austenite were formed via ${\alpha}{\rightarrow}{\gamma}+{\sigma}$ eutectoid reaction. The precipitation of $Cr_2N$ occurred at the austenite grain boundary as well as the interior of the ferrite. The intermetallic ${\chi}$ phase also formed within the ferrite and showed a cube-cube orientation relationship with the ferrite. Further aging produced a lamellar structure composed of $Cr_2N$ and austenite along the ferrite/austenite boundary and enhanced the precipitation of the ${\chi}$ phase. The crystallographic features of the precipitates were also examined in terms of the orientation relationship with the austenite or ferrite matrix.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.35 no.3
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• pp.223-231
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• 2022

Spectroscopies are the most widely used for understanding the crystallographic, chemical, and physical aspects of materials; therefore, numerous commercial and non-commercial software have been introduced to help researchers better handling their spectroscopic data. However, not many researchers, especially early-stage ones, have a proper background knowledge on the choice of fitting functions and a technique for actual fitting, although the essence of such data analysis is peak fitting. In this regard, we present a practical guide for peak fitting for data analysis. We start with a basic-level theoretical background why and how a certain protocol for peak fitting works, followed by a step-by-step visualized demonstration how an actual fitting is performed. We expect that this contribution is sure to help many active researchers in the discipline of materials science better handle their spectroscopic data.

• Nuclear Engineering and Technology
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• v.54 no.6
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• pp.1947-1953
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• 2022

As the plasma facing material in the nuclear fusion reactor, tungsten has to bear the irradiation impact of high energy particles. The surface quality of tungsten may affect its irradiation resistance, and even affect the service life of fusion reactor. In this paper, tungsten samples with different surface quality were polished by mechanical processing, subsequently conducted by D₂⁺ implantation and thermal desorption. D₂⁺ implantation was performed at room temperature (RT) with the irradiation dose of 1 × 10²¹ D₂⁺/m² by 5 keV D₂⁺ ions, and thermal desorption spectroscopy measurements were done from RT to 900 K. In addition, He irradiation was also performed by 50 eV He⁺ ions energy with the fluxes of 5.5 × 10²¹ m^-2s^-1 and 1.5 × 10²² m^-2s^-1, respectively. Results reveal that the hydrogen/helium irradiation behavior are both related to surface quality. Samples with high surface quality has superior D₂⁺ retention behavior with less D₂ retained after implantation. However, such samples are more likely to generate fuzzes on the surface after helium irradiation. Different morphologies (smooth, wavy, pyramids) after helium irradiation also demonstrates that the surface morphology is related to tungsten crystallographic orientation.

• Journal of Sensor Science and Technology
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• v.32 no.1
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• pp.10-15
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• 2023

It is well known that polycrystalline ceramics fabricated via the templated grain growth method along a desired crystallographic direction, generally along [001], exhibits enhanced piezoelectric response. Generally, the piezoelectric properties of textured ceramics depend on the degree of texture, as piezoelectric properties peak in single crystals. Therefore, understanding the relationship between the degree of texture and piezoelectric properties is fundamental. Here, we present state-of-the-art textured piezoceramics by focusing on critical issues such as the quality of templates used for texturing and proper evaluation of the degree of texture analysis. The relationship between the degree of texture and its impact on the properties of textured materials is exclusively defined by the Lotgering factor (L.F.) calculated from the X-ray diffraction profiles. Additionally, we show that L.F. is not a suitable indicator of the degree of texture, contrary to previous interpretations. This statement was further supported by the fact that the true degree of texture can be better quantified by the multiples of random distribution. This argument was justified by comparing the quantitative values of the degree of texture obtained from both methods to those of the piezoelectric charge coefficient of textured and random ceramics.

• Journal of the Korean Magnetics Society
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• v.4 no.3
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• pp.214-218
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• 1994

$Y_{3}Fe_{5}O_{12}$ based garnet films(thin or thick) offer a great promise for the application of microwave communication components. We investigated the magnetic and crystallographic preperties of $Y_{3}Fe_{5}O_{12}$ thick films prepared by KrF eximer laser ablation of a stoichiometric garnet target. It was possible to obtain almost epitaxially oriented films on $Al_{2}O_{3}$(1102) plane. Although the crystalline quality depends on substrate temperature and $O_{2}$ partial pressure used($Po_{2}$), 4.1m thick films of $4{\pi}M_{s}=1300$ Gauss and $H_{c}=37.5$ Oe were obtained at the substrate temperature of $700^{\circ}C$ with the $Po_{2}$ of 100 mTorr after annealing the as-deposited films at $700^{\circ}C$ for 2 hours. These films are expected to be used for magnetostatic spin wave filters at narrow bandwidth frequency.

• Analytical Science and Technology
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• v.21 no.6
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• pp.562-568
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• 2008

A novel two-dimensional cadmium(II)-nickel(II) bimetallic host clathrate, $[Cd{NH_2CH_2CH_2OH}_2Ni(CN)_4]{\cdot}3C_6H_5NH_2{\cdot}H_2O$, 1, has been synthesized and structurally characterized by X-ray single crystallographic method. The clathrate 1 crystallizes in the monoclinic system, space group $P2_1/c$ with a = 14.370(3), b = 7.728(1), c = 28.172(4) ${\AA}$, ${\beta}=97.58(1)^{\circ}$, V = 3101.1(9) ${\AA}^3$, Z = 4. The host framework of the clathrate 1 is built of the cyanide bridges between octahedral Cd(II) atom and square planar Ni(II) atom. The octahedral Cd atoms ligated by two 2-aminoethanol molecules and four cyanide ligands bridged with square planar Ni atoms. The Ni atoms bridges to four Cd atoms via cyanides is made up of puckered quadrangles of composition $\{CdNi(CN)_2\}_2$, all edges are shared. This cyanide bridges form an infinite two-dimensional host networks stacking along b axis. 2-Aminoethanol ligands bond to Cd atom through N atom as a monodentate ligand in the axial position and four cyanides take an equatorial plane with all in trans-configurations. The aniline guest molecules and water molecules are located in between the host layer sheets, respectively.

• Journal of Electrochemical Science and Technology
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• v.13 no.2
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• pp.279-291
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• 2022

In this report the thermochemical conversion of Sm₂O₃ to SmCl₃ using AlCl₃ in LiCl-KCl melt at 773 K is discussed. The final product was a mixture of SmCl₃, Al₂O₃, unreacted Sm₂O₃ and AlCl₃ in the chloride melt. The electrochemical attributes of the mixture was analyzed with cyclic voltammetry (CV) and square wave voltammetry (SWV). The crystallographic phases of the mixture were studied with X-ray diffraction (XRD) technique. The major chemical conversion was optimized by varying the effective parameters, such as concentrations of AlCl₃, duration of reaction and the amount of LiCl-KCl salt. The extent of conversion and qualitative assessment of efficiency of the present protocol were evaluated with fluorescence spectroscopy, UV-Vis spectrophotometry and inductively coupled plasma atomic emission spectroscopy (ICP-AES) studies of the mixture. Thus, a critical assessment of the thermochemical conversion efficiency was accomplished by analysing the amount of SmCl₃ in LiCl-KCl melt. In the process, a conversion efficiency of 95% was achieved by doubling the stoichiometric requirement of AlCl₃ in 50 g of LiCl-KCl salt. The conversion reaction was found to be very fast as the reaction reached equilibrium in 15 min.