• Journal of the Mineralogical Society of Korea
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• v.13 no.3
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• pp.164-170
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• 2000

Neutron single crystal and powder diffraction techniques have been applied to the structure analysis of yttria-stabilized zirconium, Z $r_{0.73}$ $Y_{0.27}$ $O_{1.87}$., prepared by the skull-melting method. The crystal structure has been determined to be cubic symmetry, space group Fm/equation omitted/ with a=5.155(2)$\AA$, V=136.99(5)$\AA$, Z=4, and R(F)=5.65%, $\omega$R(I)=10.57% for 70 integrated intensities of Bragg Peaks observed from single crystal of Z $r_{0.73}$ $Y_{0.27}$ $O_{1.87}$. The stabilizer atoms randomly occupy the zirconium sites and there are displacements of oxygen atoms with amplitudes of $\Delta$/a~0.033 and 0.11 along <110> and <100> directions from the ideal positions of the fluorite structure, respectively. There are no significant differences in crystallographic data between the single crystal and powder studies. Diffraction pattern after Rietveld refinement, using neutron powder data, has shown the evidence of a tetragonal impurity phase, or a slight tetragonal distortion.

• Korean Journal of Materials Research
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• v.5 no.7
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• pp.775-780
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• 1995

Thin films of titanium nitride are formed using the tetrakis-dimethyl-amino-titanium (TDMAT(Ti[N($CH_3$)$_2$]$_4$)) under various conditions. The formation of TiN films has been obtained from the thermal decomposition of the Ti-precursor and the gas phase reaction between TDMAT and ammonia(NH$_3$). The resistivity of the MOCVD film can be attributed to their impurity. Especially the curve fitting graph of XPS data is revealed that main impurities in the films as carbon and oxygen make various interstitial compounds which has influenced physical and electrical properties of the film. In the contact hole with the aspect ratio of 3:1 and the diameter of 0.5${\mu}{\textrm}{m}$, the SEM morphology shows that the step coverage is more decreased in the films formed y flowing ammonia additionally than the films formed by pyrolysis of TDMAT and the phenomenon is probably related with the activation energy.

• The Korean Journal of Nuclear Medicine
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• v.29 no.1
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• pp.110-117
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• 1995

Tc-99m Labeled hexamethylenepropyleneamineoxime ([$^{99m}Tc$]-HMPAO) is a famous amino-oxime compound and is widely used to construct SPECT images of cerebral blood flow. To investigate the relationship between chemical structure and radiolabeling in these kind of diamine-oxime compounds, we synthesized seven compounds by Schiff's base formation and successive reduction with sodium borohydride. They were (RR/SS )-4,8-diaza-3,6,6,9-tetramethylundecane-2,10-dione bisoxime (2), (RR/SS/meso)-4,8-diaza-3,9-dimethy-lundecane-2,10-dione bisoxime (4), (RR/SS/meso)-4,8-diaza-3,10-dimethyldodecane-2,11-dione bisoxime (5), (RR/SS/meso)-4,7-diaza-3,6,6,8-tetramethyldecane-2,9-dione bisoxime (8), (RR/SS/meso)-4,7-diaza-5,6-cyclohexyl-3,8-dimethyldecane-2,9-dione bisoxime (10), (RR/SS/meso)-3,4-bis(1-aza-2-methyl-3-oxime-1-butyl)-benzoic acid (12), and (RR/SS/ meso)-2,3-bis(1-aza-2-methyl-3-oxime-1-butyl) benzophenone (14). Chemical structures of all the synthesized compounds were identified by taking $^1H$ spectrum. Among them, 2 and 4 are propyleneamine oxime (PnAO), 6 is butyleneamine oxime (BnAO) and 8, 10, 12 and 14 are ethyleneamine oxime (EnAO). Each compound (0.5 mg) was incubated with stannous chloride (0.5 g - 8 g), carbonate-bicarbonate buffer (final concentration = 0.1 M, pH 7 - pH 10) and Tc-99m-pertechenate (1 ml). Tc-99m labeling of these compounds were checked by ITLC (acetone), ITLC (normal saline), reverse phase TLC (50 % acetonitrile) and ITLC (ethyl acetate). According to the results, EnAO's were not labeled by Tc-99m in any of above condition. About 11 % of maximum labeling efficiency was obtained with BnAO. However, 4 (PnAO) was labeled with Tc-99m to 85 % which is similar to the labeling efficiency of 2 (HMPAO). Hydrophilic impurity (9 % ) was the most significant problem with the labeling of 4, however, pertechnetate (3 % ) and colloid (3 %) were minor problem. In conclusion, we synthesized seven diamine blsoxlme compounds. Among them, four EnAO compounds were not labeled by Tc-99m. A BnAO was labeled poorly and two PnAO's were labeled well. These labeling can be explained by tertiary structure of their Tc-99m chelate.

• Korean Journal of Materials Research
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• v.8 no.5
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• pp.377-382
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• 1998

Atomic layer deposition(ALD) of amorphous TiN films on $SiO_2$ between 17$0^{\circ}C$ and 21O$^{\circ}C$ has been investigated by alternate supply of reactant sources, Ti[N($C_2,H_5,CH_3)_2]_4$ [tetrakis(ethylmethylamminoltitanium: TEMAT] and $NH_3$. Reactant sources were injected into the reactor in the order of TEMAT vapor pulse, Ar gas pulse, $NH_3$. gas pulse and Ar gas pulse. Film thickness per cycle was saturated at around 1.6 monolayer(MU per cycle with sufficient pulse times of reactant sources at 20$0^{\circ}C$. The results suggest that film thickness per cycle could be beyond 1 MLicycie in ALD, which were explained by rechemisorption mechanisms of reactant sources. The ideal linear relationship be¬tween number of cycles and film thickness is confirmed. As a results of surface limited reactions of ALD, step cover¬age was excellent. Particles caused by the gas phase reactions between TEMAT and NH3 were almost free because TEMAT was seperated from $NH_3$ by the Ar pulse. In spite of relatively low substrate temperature, carbon impurity was incorporated below 4 at%.

• Korean Chemical Engineering Research
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• v.51 no.5
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• pp.587-590
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• 2013

Solid-liquid equilibria for mixtures composed of n-vinyl-2-pyrrolidone (NVP) and 2-pyrrolidone were measured as a basic study for the melt crystallization process to remove 2-pyrrolidone as impurity included in NVP. A differential scanning calorimeter (DSC) and a crystallizer were used and the experimental results obtained from two methods were similar. The mixture showed a eutectic system which has a single composition at the minimum melting temperature. Calculation results from simple thermodynamic equations were found in general agreements with present data. To determine the growth rate of NVP crystal which is important for the design of crystallization process, thicknesses of the crystal were measured with the time using a layer melt crystallizer. The growth rates increased as cooling temperatures decreased. Heat transfer coefficient correlated from present data was found to successfully describe the crystal growth behavior.

• Journal of the Korean Magnetics Society
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• v.13 no.4
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• pp.171-175
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• 2003

Electron paramagnetic resonance (EPR) of Fe$^{3+}$ in LiTaO$_3$ single crystal, grown by Czochralski method, has been studied by employing an X-band spectrometer. Resonance spectra of Fe$^{3+}$ ion on the crystallographic principal axes were obtained with 9.447 ㎓ at room temperature. The spectroscopic splitting parameter g and zero-field splitting (ZFS) parameter D (= 3 B$_{2}$sup 0/) are calculated with effective spin Hamiltonian. Fe$^{3+}$ center in stoichometric single crystal turns out to be different with that in congruent single crystal reported previously. From the analysis of temperature dependence of resonance fields for Fe$^{3+}$ ion, there is no any phase transition at the temperature range (from -160 $^{\circ}C$ to 20 $^{\circ}C$).

• The Korean Journal of Nuclear Medicine Technology
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• v.16 no.1
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• pp.8-11
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• 2012

Purpose : Among quality control items, the radiochemical impurity must be below 10% of total radioactivity. In this regard, as the recently commercialized automatic synthesis module produces a large amount of 18F-FDG, radiolysis of radiopharmaceuticals is very likely to occur. Thus, this study compared the changes in radiochemical purity regarding radiolysis of $^{18}F$-FDG according to automatic synthesis module. Materials and methods : Cyclotron (PETtrace, GE Healthcare) was used to produce $^{18}F$ and automatic synthesis module (FASTlab, Tracerlab MX, GE Healthcare) was used to achieve synthesis into FDG. For radiochemical purity, Radio-TLC Scanner (AR 2000, Bioscan), GC (Gas Chromatograph, Agilent 7890A) was used to measure the content of ethanol included in $^{18}F$-FDG. Glass board applied with silica gel ($1{\times}10cm$) was used for stationary phase while a mixed liquid formed of acetonitrile and water (ratio 19:1) was used for mobile phase. High-concentration and low-concentration $^{18}F$-FDG were produced in each synthesis module and the radiochemical purity was measured every 2 hours. Results : The purity in low-concentration (below 2.59 GBq/mL) was measured as 99.26%, 98.69%, 98.25%, 98.09% in Tracerlab MX and as 99.09%, 97.83%, 96.89%, 96.62% in FASTlab according to 0, 2, 4, 6 hours changes, respectively. The purity in high-concentration (above 3.7 GBq/mL) was measured as 99.54%, 96.08%, 93.77%, 92.54% in Tracerlab MX and as 99.53%, 95.65%, 92.39%, 89.82% in FASTlab according to 0, 2, 4, 6 hours changes, respectively. Also, ethanol was not detected in GC of $^{18}F$-FDG produced in FASTlab, while 100~300 ppm ethanol was detected in Tracerlab MX. Conclusion : Whereas the change of radiochemical purity was only 3% in low-concentration $^{18}F$-FDG, the change was rapidly increased to 10% in high-concentration. Also, higher radiolysis were observed in $^{18}F$-FDG produced in FASTlab than Tracerlab MX. This is because ethanol is included in the synthesis stage of Tracerlab MX but not in the synthesis stage of FASTlab. Thus, radiolysis is influenced by radioactivity concentration than the inclusion of ethanol, which is the radioprotector. Therefore, after producing high-concentration $^{18}F$-FDG, the content must be diluted through saline to lower concentration.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.30 no.2
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• pp.47-54
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• 2020

To develop the bright-vivid red- and yellow-inorganic fluorescent pigments with high luminescence properties, A₃V₅O₁₄ (A = K and Rb) and Cs₂V₄O₁₁ inorganic pigments were synthesized by a water assisted solid state reaction (WASSR) method and a conventional solid state reaction method. Although impurity peaks corresponding to the AVO₃ and AV₃O₈ (A = K, Rb, and Cs) were observed in all samples prepared, the trigonal structure A₃V₅O₁₄ (A = K and Rb) and orthorhombic structure Cs₂V₄O₁₁ were successfully obtained as a main phase. These inorganic pigments showed the broad absorption band (under 550 nm) originated from CT transitions of VO₄ polyhedron, and the strong broad red- and green-emission bands due to ³T₂ → ¹A₁ and ³T₁ → ¹A₁ transitions of the [VO₄]^3- group. The A₃V₅O₁₄ (A = K and Rb) and Cs₂V₄O₁₁ pigments showed a bright-vivid red- and yellow-body color, where the a* values of the A₃V₅O₁₄ (A = K and Rb) were +35.5 and +45.9, respectively, and b* value of Cs₂V₄O₁₁ pigments was +50.3. The L* values of the A₃V₅O₁₄ (A = K and Rb) and Cs₂V₄O₁₁ inorganic pigments were over +45. These results indicate that the A₃V₅O₁₄ (A = K and Rb) and Cs₂V₄O₁₁ inorganic pigments could be an attractive candidate as a bright-vivid red- and yellow inorganic pigments.

• Applied Chemistry for Engineering
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• v.19 no.5
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• pp.477-483
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• 2008

$La_{0.7}Sr_{0.3}Co_{0.2}Fe_{0.8}O_{3-{\delta}$ oxide was synthesized by a citrate method and a typical dense membrane of perovskite oxide has been prepared using as-prepared powder by pressing and sintering at $1300^{\circ}C$. Precursor of $La_{0.7}Sr_{0.3}Co_{0.2}Fe_{0.8}O_{3-{\delta}$ prepared by citrate method was investigated by TGA and XRD. Metal-citrate complex in precursor was decomposed into perovskite oxide in the temperature range of $260{\sim}410^{\circ}C$ but XRD results showed $SrCO_3$ existed as impurity at less than $900^{\circ}C$. Electrical conductivity of membrane increased with increasing temperature but then decreased over $700^{\circ}C$ in air atmosphere ($Po_2=0.2atm$) and $600^{\circ}C$ in He atmosphere ($Po_2=0.01atm$) respectively due to oxygen loss from the crystal lattice. The oxygen permeation flux increased with increasing temperature and maximum oxygen permeation flux of $La_{0.7}Sr_{0.3}Co_{0.2}Fe_{0.8}O_{3-{\delta}$ membrane with 1.6 mm thickness was about $0.31cm^3/cm^2{\cdot}min$ at $950^{\circ}C$. The activation energy for oxygen permeation was 88.4 kJ/mol in the temperature range of $750{\sim}950^{\circ}C$. Perovskite structure of membrane was not changed after permeation test of 40 h and the membrane was stable without secondary phase change with 0.3 mol Sr addition.

• Economic and Environmental Geology
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• v.52 no.3
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• pp.223-230
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• 2019

The calcination of oyster shells have been studied as the possible substitute for the limestone used as an absorbent of $SO_2$ gas. However, since pure shells can not be used in calcination process, some impurities are contained and the changes in the characteristics of the calcination products are expected. In this study, the surface characteristics of the calcination products are investigated by mineralogical analysis according to the contents of NaCl, which can be derived from sea water, and sediments on the surface of the shell as impurities. The marine sediments on the shells were mainly composed of quartz, albite, calcite, small amounts of amphibole and clay minerals such as ilite, chlorite and smectite. After calcination of oyster shells mixed with 0.2-4.0 wt% sediments at $900^{\circ}C$ for 2 hours, regardless of the dehydration, dehydroxylation, and phase change of these minerals at the lower temperature than this experiment, no noticeable changes were observed on the specific surface area of the calcined product. However, when mixed with 0.1 to 2.0 wt% NaCl, the specific surface area generally increases as compared with the shell sample before calcination. The specific surface area increases with increasing amount of salt, and then decreases again. This is closely related to the changes of surface morphology. As the amount of NaCl increases, the morphology of the surface is similar to that of gel. It changes into a slightly angular, smaller particle and again looks like gel with increasing amount of NaCl. Our results show that NaCl affects morphological changes probably caused by melting of some oyster shells, but may have different effects on the specific surface area of calcination product depending on the NaCl contents.