• Title/Summary/Keyword: x-ray diffractometry

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Uranyl Peroxide Compound Preparation from the Filtrate for Nuclear Fuel Powder Production Process (핵연료분말 제조공정 여액으로부터 Uranyl-peroxide 화합물의 제조)

  • Jeong, Kyung-Chai;Kim, Tae-Joon;Choi, Jong-Hyun;Park, Jin-Ho;Hwang, Seong-Tae
    • Applied Chemistry for Engineering
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    • v.8 no.3
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    • pp.430-437
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    • 1997
  • Uranyl-peroxide compound was prepared by the reaction of excess hydrogen peroxide solution and trace uranium in filtrate from nuclear fuel conversion plant. The $CO_3{^{2-}}$ in filtrate was removed first by heating more than $98^{\circ}C$, because uranyl-peroxide compound could not be precipitated by $CO_3{^{2-}}$ remaining in filtrate. The optimum condition for uranyl-peroxide compound was ageing for 1 hr after controling the pH with $NH_3$ gas and adding the excess $H_2O_2$ of 10ml/lit.-filtrate. Uranium concentration in the filtrate was appeared to 3 ppm after the precipitation of uranyl-peroxide compound, and the chemical composition of this compound was analyzed to $UO_4{\cdot}2NH_4F$ with FT-IR, X-ray diffractometry, TG and chemical analysis. Also, this fine particle, about $1{\sim}2{\mu}m$, could be grown up to $4{\mu}m$ at pH 9.5 and $60^{\circ}C$. The separation efficiency of precipitate from mother liquor was increased with increase of pH and reaction temperature. Otherwise, the crystal form of this particle showed octahedral by SEM and XRD, and $U_3O_8$ powder was obtained by thermal decomposition at $650^{\circ}C$ in air atmosphere.

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Porous silica ceramics prepared by sol-gel process-Effect of $H_2O/TEOS$ molar ratio- (솔-젤법에 의한 다공성 실리카 세라믹스의 제조-$H_2O/TEOS$ 몰비의 영향-)

  • Lee, Jin-Hui;Kim, Wha-Jung;Lee, Joon
    • Journal of the Korean Ceramic Society
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    • v.34 no.2
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    • pp.216-224
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    • 1997
  • Porous silica ceramics were prepared(with HCI catalyst) using H2O/TEOS molar ratios of 2.6~59.0, with the EtOH/TEOS ratio fixed. After preparing 9 kinds of sol, the followings were investigated; measurement of the gelation time, thermal analyses by TG/DTA, property analyses of the intermediates by FT-IR and X-ray diffractometry with dried samples, analyses of SiO2 polymer by FT-IR, the investigation of specific sur-face area and pore size distribution by N2-adsorption isotherm, and structural change of SiO2 polymer and pore morphology by TEM observation, with samples heat-treated to 50$0^{\circ}C$. In the concentrations of in-vestigated compositions and catalyst, gelation time showed a minimum at ca. 11 moles of water per one mole of TEOS, the highest degree of polymerization at ca. 8-18 moles, and the largest specific surface area at ca. 11 moles, which means that the polymerization proceeded fastest at ca. 11 moles of water. In con-clusion, the more water used, the faster the polymerization reaction up to ca. 11 moles, but more than ca. 11 moles of water caused retardation of gelation and resultant reduction of specific surface area.

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$M\"{o}ssbauer$ studies of $NdFe_{10.7}TiM{0.3}(M\;=\;B,\;Ti)$ ($NdFe_{10.7}TiM{0.3}(M\;=\;B,\;Ti)$$M\"{o}ssbauer$ 연구)

  • 김철성;이용종;김윤배;김창석
    • Journal of the Korean Magnetics Society
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    • v.5 no.1
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    • pp.64-70
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    • 1995
  • The authors have studied crystallographic and magrletic properties of $NdFe_{10.7}TiM_{0.3}(M=B,\;Ti)$ by X-ray diffraction, VSM magnetometer, and Mossbauer spectrometer. The Alloys were prepared by arc-melting under argon atmosphere. The $NdFe_{10.7}TiM_{0.3}$ has pure single phase, whereas the $NdFe_{10.7}Ti_{1.3}$ contains some $\alpha-Fe$, from powder X-ray diffractometry. The $NdFe_{10.7}TiM_{0.3}$ has the $ThMn_{12}$-type tetragonal structure with $a_{0}=8.587\;{\AA}\;and\;c_{0}=4.788\;{\AA}$. The Curie temperature ($T_c$) is $570{\pm}3\;K$ from $M\"{o}ssbauer$ spectroscopy performed at various temperatures ranging from 13 to 770 K. Each spectrum of below $T_c$ was fitted with five subspectra of Fe sites in the structure ($8i_{1},\;8i_{2},\;8j_{1},\;8j_{2}\;and\;8f$). The area fraction of the subspectra at room temperature are 16.4, 8.2, 14.8, 21.3 and 39.3 %, respectively. Magenetic hyperfine fields for the Fe sites decrease in the order, $H_{hf}(8i)>H_{hf}(8j)>H_{hf}(8f)$.

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Characterization of B-doped a-SiC:H Thin Films Grown by Plasma-Enhanced Chemical Vapor Deposition (플라즈마 화학증착법으로 제조된 B-doped a-SiC:H 박막의 물성)

  • Kim, Hyeon-Cheol;Sin, Hyeok-Jae;Lee, Jae-Shin
    • Korean Journal of Materials Research
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    • v.9 no.10
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    • pp.1006-1011
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    • 1999
  • B-doped hydrogenated amorphous silicon carbide (a-SiC:H) thin films were prepared by plasma-enhanced chemical-vapor deposition in a gas mixture of $SiH_4$, $CH_4$ and $B_2H_6$. Microstructures and chemical properties of a-SiC:H films grown with varing the volume ratio of $CH_4$ to $SiH_4$ were characterized with various analysis methods including scanning electron microscopy(SEM), X-ray diffractometry(XRD), Raman spectroscopy, Fourier-transform infrared (FTIR) spectroscopy. X-ray photoelectron spectroscopy(XPS), UV absorption spectroscopy and photoconductivity measurements. While Si:H films grown without $CH_4$ showed amorphous state, the addition of $CH_4$ during deposition enhanced the development of a microcrystalline phase. By introducing C atoms into the film, Si-Si and Si--$\textrm{H}_{n}$ bonds of a -Si:H films were gradually replaced by Si-C, C-C, and Si--$\textrm{C}_{n}\textrm{H}_{m}$ bonds. Consequently, the electrical resistivity and optical bandgap of a-SiC:H films were increased with the C concentration in the film.

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Enhanced Dissolution and Permeation of Biphenyl Dimethyl Dicarboxylate Using Solid Dispersions (고체분산체로부터 비페닐디메칠디카르복실레이트의 용출 및 투과 증전)

  • Moon, Jee-Hyun;Chun, In-Koo
    • Journal of Pharmaceutical Investigation
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    • v.29 no.3
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    • pp.227-234
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    • 1999
  • Solid dispersions were prepared to increase the dissolution rate of biphenyl dimethyl dicarboxylate (DDB) using water-soluble carriers such as povidone, copolyvidone, $2-hydroxypropyl-{\beta}-cyclodextrin (HPCD)$, sodium salicylate or sodium benzoate by solvent evaporation method. Solid dispersions were characterized by infrared spectrometry, differential scanning calorimetry (DSC) and powder X-ray diffractometry, dissolution and permeation studies. DDB tablets (7.5 mg) were prepared by compressing the powder mixtures composed of solid dispersions, lactose, com starch, crospovidone and magnesium stearate using a single-punch press. DDB capsules (7.5 mg) were also prepared by filling the mixtures in empty hard gelatin capsules (size No.1). From the DSC and powder x-ray diffractometric studies, it was found that DDB was amorphous in the HPCD or copolyvidone solid dispersions. Dissolution rates after 10 min of DDB alone and solid dispersions (1 : 10) in sodium benzoate, sodium salicylate and copolyvidone were 11.8, 23.5, 22.8 and 82.5%, respectively. Dissolution rates of DDB after 30 min from 1 : 10 and 1 : 20 copolyvidone solid dispersions were 80.5 and 95.0%, respectively. For the DDB tablets prepared using solid dispersions (1 : 20), the initial dissolution rate was dependent on carrier material, and was ranked in order, $Kollidon\;30\;{\ll}$ copolyvidone < HPCD. For the HPCD solid dispersion tablets, dissolution rate reached 97.4% after 15 min, but thereafter slowly decreased to 80.7% after 2 hr due to the precipitation of DDB. However, in the case of copolyvidone solid dispersion tablets, dissolution increased linearly and reached 93.4% after 2 hr. Reducing the volume of test medium from 900 to 300 ml markedly decreased the dissolution rate of the tablets containing 1 : 20 HPCD solid dispersions and 1 : 10 copolyvidone solid dispersion. For 1 : 20 copolyvidone solid dispersion tablets, there was no significant change in dissolution rate up to 1 hr with different volumes of test medium. Preparation of the copolyvidone solid dispersion (1 : 20) in capsules markedly delayed the dissolution (31.2 % after 2hr) due to the limited diffusion within capsules. The permeation rate $(13.4\;g/cm^2\;after\;8\;hr)$ of DDB through rabbit duodenal mucosa from copolyvidone solid dispersion (1 : 10) was markedly enhanced, when compared with drug alone or physical mixtures. From overall findings, DDB formulations containing copolyvidone solid dispersions (1 : 20) could be used to remarkably improve the dissolution rate in dosage form of powders and tablets.

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Properties of CaO added MgO Sintering at High Pressure and Low Temperatures (CaO 첨가된 MgO의 고압 저온 소결 조건에 따른 물성연구)

  • Song, Jeongho;Song, Ohsung
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.14 no.9
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    • pp.4185-4190
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    • 2013
  • We executed the property changes of the sintered MgO (99.9% purity, 300nm size) specimens with addition to CaO content of 0.00wt%, 0.25wt%, and 0.50wt%, processed at 7GPa, for 5min, 600~$800^{\circ}C$. To investigate the micro-structure and physical property changes of the sintered MgO(-CaO), we employed a scanning electron microscopy(SEM), X-ray diffractomerty(XRD), Vickers hardness, and density. The SEM result showed that MgO powder of 300nm size was changed into sintered structure of 520nm by high pressure and low temperature sintering, regardless of the CaO contents. According to the XRD analysis, no CaO phase observed, while MgO peaks shift indicated the existence of CaO in the MgO matrix. The Vickers hardness result showed that hardness of sintered MgO-CaO increased by 12% compared pure MgO under the same temperature conditions. It implied that we can obtain the same hardness with $100^{\circ}C$ lowered sintering temperatures by addition of CaO. The density results showed that it was possible to obtain density of 98%, which is 5% greater than that of pure MgO at low temperature of $600^{\circ}C$.

Biological Pretreatment of Softwood Pinus densiflora by Three White Rot Fungi

  • Lee, Jae-Won;Gwak, Ki-Seob;Park, Jun-Yeong;Park, Mi-Jin;Choi, Don-Ha;Kwon, Mi;Choi, In-Gyu
    • Journal of Microbiology
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    • v.45 no.6
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    • pp.485-491
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    • 2007
  • The effects of biological pretreatment on the Japanese red pine Pinus densiflora, was evaluated after exposure to three white rot fungi Ceriporia lacerata, Stereum hirsutum, and Polyporus brumalis. Change in chemical composition, structural modification, and their susceptibility to enzymatic saccharification in the degraded wood were analyzed. Of the three white rot fungi tested, S. hirsutum selectively degraded the lignin of this sortwood rather than the holocellulose component. After eight weeks of pretreatment with S. hirsutum, total weight loss was 10.7%, while lignin loss was the highest at 14.52% among the tested samples. However, holocellulose loss was lower at 7.81 % compared to those of C. lacerata and P. brumalis. Extracelluar enzymes from S. hirsutum showed higher activity of ligninase and lower activity of cellulase than those from other white rot fungi. Thus, total weight loss and changes in chemical composition of the Japanese red pine was well correlated with the enzyme activities related with lignin- and cellulose degradation in these fungi. Based on the data obtained from analysis of physical characterization of degraded wood by X-ray Diffractometry (XRD) and pore size distribution, S. hirsutum was considered as an effective potential fungus for biological pretreatment. In particular, the increase of available pore size of over 120 nm in pretreated wood powder with S. hirsutum made enzymes accessible for further enzymatic saccharification. When Japanese red pine chips treated with S. hirsutum were enzymatically saccharified using commercial enzymes (Cellulclast 1.5 L and Novozyme 188), sugar yield was greatly increased (21.01 %) compared to non-pre treated control samples, indicating that white rot fungus S. hirsutum provides an effective process in increasing sugar yield from woody biomass.

Effects of Eu3+ and Tb3+ Activator Ions on the Properties of SrSnO3 Phosphors (Eu3+와 Tb3+ 활성제 이온이 SrSnO3 형광체의 특성에 미치는 영향)

  • Kim, Jung Dae;Cho, Shinho
    • Korean Journal of Materials Research
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    • v.24 no.9
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    • pp.469-473
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    • 2014
  • $SrSnO_3$ phosphor powders were synthesized with two different contents of activator ions $Eu^{3+}$ and $Tb^{3+}$ using the solid-state reaction method. The structural, morphological, and optical properties of the phosphors were investigated using X-ray diffractometry, field-emission scanning electron microscopy, and fluorescence spectrophotometry, respectively. All the phosphors showed a cubic structure, irrespective of the type and the content ratio of activator ions. For $Eu^{3+}$-doped $SrSnO_3$ phosphors, the intensity of the 620 nm red emission spectrum resulting from the $^5D_0{\rightarrow}^7F_2$ transition of $Eu^{3+}$ was stronger than that of the 595 nm orange emission signal due to the $^5D_0{\rightarrow}^7F_1$ transition in the range 0.01-0.05 mol of $Eu^{3+}$, but the ratio of the intensity was reversed in the range 0.10-0.20 mol of $Eu^{3+}$. The variation in the emission intensity indicates that the site symmetry of the $Eu^{3+}$ ions around the host crystal was changed from non-inversion symmetry to inversion. For the $Tb^{3+}$-doped $SrSnO_3$ phosphors under excitation at 281 nm, one strong green emission band at 550 nm and several weak bands were observed. These results suggest that the optimum red and green emission signals can be realized when the activator ion content for $Eu^{3+}$- or $Tb^{3+}$-doped $SrSnO_3$ phosphors is 0.20 mol and 0.15 mol, respectively.

Effect of Defect Energy levels on the AC PDP Discharging Characteristics (MgO 보호막의 결함 전위 레벨이 AC-PDP 방전 특성에 미치는 효과)

  • Kwon, Sang-Jik;Kim, Yong-Jae;Cho, Eou-Sik
    • Journal of the Institute of Electronics Engineers of Korea SD
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    • v.44 no.12
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    • pp.12-17
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    • 2007
  • The effects of the evaporation rate of MgO films using an electron beam on the MgO properties and the discharge characteristics of a plasma display panel(PDP) were investigated and analyzed. Mgo films were deposited with the various MgO evaporation rates. The MgO properties such as the crystal orientation, the surface roughness, and the film structure, were inspected using XRD(X-ray diffractometry), AFM(atomic force microscopy). From the experiments and Paschen law, the maximum value of the secondary, electron emission coefficient $(\gamma)$ was obtained at the evaporation rate of $5\AA/sec$. The minimum firing voltage and the maximum luminous efficiency were obtained at an evaporation rate of $5\AA/sec$. In the MgO film deposited at $5\AA/sec$, the (200) orientation and $F^+$ center were most intensive. The XRD results and cathode-luminescence(CL) spectra show the $\gamma$ values are correlated with $F/F^+$ centers of the molecular structure of MgO films.

Size, Shape, and Crystal Structure of Silica Particles Generated as By-products in the Semiconductor Workplace (반도체 작업환경 내 부산물로 생성되는 실리카 입자의 크기, 형상 및 결정 구조)

  • Choi, Kwang-Min;Yeo, Jin-Hee;Jung, Myung-Koo;Kim, Kwan-Sick;Cho, Soo-Hun
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.25 no.1
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    • pp.36-44
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    • 2015
  • Objectives: This study aimed to elucidate the physicochemical properties of silica powder and airborne particles as by-products generated from fabrication processes to reduce unknown risk factors in the semiconductor manufacturing work environment. Materials and Methods: Sampling was conducted at 200 mm and 300 mm semiconductor wafer fabrication facilities. Thirty-two powder and airborne by-product samples, diffusion(10), chemical vapor deposition(10), chemical mechanical polishing(5), clean(5), etch process(2), were collected from inner chamber parts from process and 1st scrubber equipment during maintenance and process operation. The chemical composition, size, shape, and crystal structure of silica by-product particles were determined by using scanning electron microscopy and transmission electron microscopy techniques equipped with energy dispersive spectroscopy, and x-ray diffractometry. Results: All powder and airborne particle samples were composed of oxygen(O) and silicon(Si), which means silica particle. The by-product particles were nearly spherical $SiO_2$ and the particle size ranged 25 nm to $50{\mu}m$, and most of the particles were usually agglomerated within a particle size range from approximately 25 nm to 500 nm. In addition, the crystal structure of the silica powder particles was found to be an amorphous silica. Conclusions: The silica by-product particles generated from the semiconductor manufacturing processes are amorphous $SiO_2$, which is considered a less toxic form. These results should provide useful information for alternative strategies to improve the work environment and workers' health.