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Synthesis of Single Crystalline Analcime and Its Single-crystal Structure, |Na0.94(H2O)|[Si2.06Al0.94O6]-ANA: Determination of Cation Sites, Water Positions, and Si/Al Ratios (결정성 아날심(|Na0.94(H2O)|[Si2.06Al0.94O6]-ANA)의 합성 및 단결정구조: 양이온 및 물 분자의 위치, Si/Al 비의 결정)

  • Seo, Sung-Man;Suh, Jeong-Min;Ko, Seong-Oon;Lim, Woo-Taik
    • Journal of the Korean Chemical Society
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    • v.55 no.4
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    • pp.570-574
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    • 2011
  • Large colorless single crystals of analcime with diameters up to 0.20 mm have been synthesized from gels with the composition of $3.00SiO_2$ : $1.50NaAlO_2$ : 8.02NaOH : $454H_2O$ : 5.00TEA. The fully $Na^+$-exchanged analcime have been prepared with aqueous 0.1 M NaCl (pH adjusted from 6 to 11 by dropwise addition of NaOH). The single-crystal structure of hydrated $|Na_{0.94}(H_2O)|[Si_{2.06}Al_{0.94}O_6]$-ANA per unit cell, a=13.703(3) ${\AA}$, has been determined by single-crystal X-ray diffraction technique in the orthorhombic space group Ibca at 294 K. The structure was refined using all intenties to the final error indices (using only the 1,446 reflections for which $F_o$ > $4{\sigma}(F_o))R_1/wR_2$ = 0.054/0.143. About 15 $Na^+$ ions are located at three nonequivalent positions and octahedrally coordinated. The chemical composition is $Na_{0.94}(H_2O)Si_{2.06}Al_{0.94}O_6$. The Si/Al ratio of synthetic analcime is 2.19 determined by the occupations of cations, 14.79, in the single-crystal determination work.

Crystal Structure of Probenecid, $C_{13}H_{19}NO_4S$ (Probenecid, $C_{13}H_{19}NO_4S$의 結晶構造)

  • Kim, Eui-Sung;Shin, Hyun-So
    • Journal of the Korean Chemical Society
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    • v.35 no.6
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    • pp.603-606
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    • 1991
  • The crystal structure of Probenecid has been determined from 2574 independent reflections collected on an automatic ENRAF-NONIUS CAD-4 diffractometer using graphite-monochromated $Mo-K{\alpa}$ radiation. The crystal is triclinic, space group P$\bar{1}$ with unit cell dimensions a = 7.535(2)${\AA}$, b = 18.473 (5)${\AA}$, c = 5.317(9)${\AA}$, ${\alpha} = 92.00(5)^{\circ}$, ${\beta} = 99.02(5)^{\circ}$, ${\gamma} = 94.89(2)^{\circ}$, V = 727.4(2)${\AA}^3$, Z = 2, $D_m$ = 1.310, $D_x$ = $1.302 gcm^{-3}$, ${\mu}$ = $1.88 cm^{-1}$, F(000) = 304, and T = 298 K. Final R = 0.0676 and $R_w$ = O.0630 for 1209 reflections > 5${\sigma}(F_o)$. In the spacial arrangement about N(13), the sum of bond angles about nitrogen is 350.9° and the nitrogen lies only 0.268(6)${\AA}$ out of S(1)-C(14)-C(17) plane. The S(1)-C(4) distance is 1.792(6)${\AA}$ and the C(4)-S(1)-N(13) angle is $106.5(3)^{\circ}$. The overall conformation of the molecule is folded with respect to sulfur.

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A Study on the Use of Active Protocol Using the Change of Pitch and Rotation Time in PET/CT (PET/CT에서 Pitch와 Rotation Time의 변화를 이용한 능동적인 프로토콜 사용에 대한 연구)

  • Jang, Eui Sun;Kwak, In Suk;Park, Sun Myung;Choi, Choon Ki;Lee, Hyuk;Kim, Soo Young;Choi, Sung Wook
    • The Korean Journal of Nuclear Medicine Technology
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    • v.17 no.2
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    • pp.67-71
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    • 2013
  • Purpose: The Change of CT exposure condition have a effect on image quality and patient exposure dose. In this study, we evaluated effect CT image quality and SUV when CT parameters (Pitch, Rotation time) were changed. Materials and Methods: Discovery Ste (GE, USA) was used as a PET/CT scanner. Using GE QA Phantom and AAPM CT Performance Phantom for evaluate Noise of CT image. Images are acquired by using 24 combinations that four stages pitch (0.562, 0.938, 1.375, 1.75:1) and six stages X-ray tube rotation time (0.5s-1.0s). PET images are acquired using 1994 NEMA PET Phantom ($^{18}F-FDG$ 5.3 kBq/mL, 2.5 min/frame). For noise test, noise are evaluated by standard deviation of each image's CT numbers. And then we used expectation noise according to change of DLP (Dose Length Product) to experimental noise ratio for index of effectiveness. For spatial resolution test, we confirmed that it is possible to identify to 1.0 mm size of the holes at the AAPM CT Performance Phantom. Finally we evaluated each 24 image's SUV. Results: Noise efficiency were 1.00, 1.03, 1.01, 0.96 and 1.00, 1.04, 1.02, 0.97 when pitch changes at the QA Phantom and AAPM Phantom. In case of X-ray tube rotation time changes, 0.99, 1.02, 1.00, 1.00, 0.99, 0.99 and 1.01, 1.01, 0.99, 1.01, 1.01, 1.01 at the QA Phantom and AAPM Phantom. We could identify 1.0 mm size of the holes all 24 images. Also, there were no significant change of SUV and all image's average SUV were 1.1. Conclusion: 1.75:1 pitch is the most effective value at the CT image evaluation according to pitch change and It doesn't affect to the spatial resolution and SUV. However, the change of rotation time doesn't affect anything. So, we recommend to use the effective pitch like 1.75:1 and adequate X-ray tube rotation time according to patient size.

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The Crystal Structure of Bis(N-Methylphenazinium) Bis(Oxalato)Palladate(Ⅱ) (Bis(N-Methylphenazinium) Bis(Oxalato)Palladate(Ⅱ)의 결정구조)

  • Kim, Se Hwan;NamGung, Hae;Lee, Hyeon Mi
    • Journal of the Korean Chemical Society
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    • v.38 no.11
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    • pp.827-832
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    • 1994
  • The crystal structure of bis(N-methylphenazinium) bis(oxalato)palladate(II) has been determined by X-ray crystallography. Crystal data: ((C_{13}H_{11}N_2)_2[Pd(C_2O_4)_2]) $M_w$ = 672.93, Triclinic, Space Group P1 (No = 2), a = 7.616(8), b = 9.842(3), c = $20.335(7)\AA$, $\alpha$ = 103.53(3), $\beta$ = 90.00(5), $\gamma$ = $112.38(5)^{\circ}$, Z = 2, $V = 1363(2){\AA}^3\;D_c = 1.639\;gcm^{-3},\;{\mu} = 7.3\;cm^{-1},\;F(000) = 680.0$. The intensity data were collected with $Mo-K\alpha$ radiation (${\lambda}$= 0.7107\;\AA)$ on an automatic four-circle diffractometer with a graphite monochromater. The structure was solved by Patterson method and refined by full matrix least-square methods using Killean & Lawrence weights. The final R and S values were $R = 0.069,\;R_w = 0.050,\;R_{all} = 0.069$ and S = 5.45 for 3120 observed reflections. Both cation and anion complexes are essentially planar and have dihedral angles of 6.3(6) and $57.06(6)^{\circ}$ between their planes. The planar complex anions are sandwiched between slightly bent cations. The interplanar separations of two triads are 3.328 and 3.463 $\AA$, respectively. The triads are stacked along b-axis, but their orientations are different based on dihedral angle $59.08(9)^{\circ}$ of two complex anions.

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Synthesis and Characterization of the Large Single Crystal of Fully K+-exchanged Zeolite X (FAU), |K80|[Si112Al80O384]-FAU (Si/Al=1.41)

  • Lim, Woo-Taik;Jeong, Gyo-Cheol;Park, Chang-Kun;Park, Jong-Sam;Kim, Young-Hun
    • Bulletin of the Korean Chemical Society
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    • v.28 no.1
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    • pp.41-48
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    • 2007
  • Large colorless single crystals of sodium zeolite X, stoichiometry |Na80 |[Si112Al80O384]-FAU, with diameters up to 200 μm and Si/Al = 1.41 have been synthesized from gels with the composition of 2.40SiO2 : 2.00NaAlO2 : 7.52NaOH : 454H2O : 5.00TEA. One of these, a colorless octahedron about 200 μm in cross-section has been treated with aqueous 0.1 M KNO3 for the preparation of K+-exchanged zeolite X. The crystal structure of |K80|[Si112Al80O384]-FAU per unit cell, a = 24.838(4) A, dehydrated at 673 K and 1 × 10-6 Torr, has been determined by single-crystal X-ray diffraction techniques in the cubic space group Fd at 294 K. The structure was refined using all intensities to the final error indices (using only the 707 reflections for which Fo > 4σ (Fo)) R1 = 0.075 (based on F) and R2 = 0.236 (based on F2). About 80 K+ ions per unit cell are found at an unusually large number of crystallographically distinct positions, eight. Eleven K+ ions are at the centers of double 6-rings (D6Rs, site I; K-O = 2.492(6) A and O-K-O (octahedral) = 88.45(22)o and 91.55(22)o). Site-I' position (in the sodalite cavities opposite D6Rs) is occupied by five K+ ions per unit cell; these K+ ions are recessed 1.92 A into the sodalite cavities from their 3-oxygen planes (K-O = 2.820(19) A, and O-K-O = 78.6(6)o). Twety-three K+ ions are found at three nonequivalent site II (in the supercage) with occupancies of 5, 9, and 9 ions; these K+ ions are recessed 0.43 A, 0.75 A, and 1.55 A, respectively, into the supercage from the three oxygens to which it is bound (K-O = 2.36(13) A, 2.45(13) A, and 2.710(13) A, O-K-O = 116.5(20)o, 110.1(17)o, and 90.4(6)o, respectively). The remaining sixteen, thirteen, and twelve K+ ions occupy three sites III' near triple 4-rings in the supercage (K-O = 2.64(3) A, 2.94(3) A, 2.73(5) A, 2.96(6) A, 3.06(4) A, and 3.08(3) A).

Protection Effect of Undariia pinnatifida sporophylls-derived Fucoidan in Rat Lung Injury from X-ray Irradiation (미역포자엽추출 푸코이단의 X-선 조사 흰쥐 폐장상해에 대한 방오기능 평가)

  • Kim, Hong-Tae;Jeong, Eui-Sook;Chung, Duck-Soo;Kim, Ki-Hong;Kim, Jong-Ki
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.42 no.2
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    • pp.131-138
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    • 2009
  • The radioprotect effects of fractinated fucoidan, derived from Undaria pinnatifida sporophylls, were examined in lung injured rats treated with partial body irradiation. The right lung of Sprague-Dawley rats, eight separately grouped by including radiation only control group (ROG) and fucoidan+radiation treated group (FRG), were treated with various fraction of Undaria-derived fucoidan every other day by intraperitoneal injection 6 days prior to irradiation and during monitoring at 24 hours, 48 hours, 2 weeks, 4 weeks and 12-weeks post-irradiation of 6 Mev/2 Gy. The rats were euthanized at completion of the treatment. Tissue samples from the injured lung, fixed in formaldehyde using lung perfusion prior to extraction, were H/E stained for histological analysis using optical microscopy. Interstitial congestion (IC), hemorrhage in alveolar sac (HM), number of macrophage (MP) and alveolar wall thickness (AWT) as a measure of early indication of fibrosis were measured. AWTs in 24 hrs post-irradiation rats increased in comparison with $2.49{\pm}0.06{\mu}m$ of control group by $3.67{\pm}0.09{\mu}m$, $3.21{\pm}0.08{\mu}m$ (p=0.013), $2.98{\pm}0.08{\mu}m$ (p=0.00) in ROG, F1-fucoidan+radiation, and F3-fucoidan+radiation group, respectively. AWT of the ROG was further increased by $4.30{\pm}0.13{\mu}m$ in the 12 weeks post-irradiation group, but AWT on average was $2.56{\pm}0.05{\mu}m$ in the FRG. MP in the 24 hrs post-irradiation group markedly increased in comparison with $2.6{\pm}0.34/0.14\;mm^2$ of the control group by $8.0{\pm}1.48/0.14\;mm^2$ in the ROG, but it was only $3.6{\pm}0.48/0.14\;mm^2$ in F3-FRG. MP in the 12 weeks post-irradiation group was $7.2{\pm}1.28/0.14\;mm^2$ in ROG, but it was $2.8{\pm}0.37/0.14\;mm^2$ or $2.4{\pm}0.4/0.14\;mm^2$ (p<0.05) in the FRG. In addition, increased IC and HM in ROG were relatively smaller in FRG of the 24 hr and 12 weeks post-irradiation rats. In conclusion, Undaria pinnatifida sporophylls-derived fucoidan fractions exhibited radioprotectant activity on injured rat lung subjected to X-ray irradiation. However, success was variable according to the fractions and also time of injection post injury.

Crystallographic and Magnetic Properties of Li0.5Fe2.5-χRhχO4 by Using Applied Field Mossbauer Spectrometer (외부자기장 뫼스바우어 분광기를 이용한 Li0.5Fe2.5-χRhχO4의 자기적 성질과 결정학적 구조에 관한 연구)

  • Kang, Kun-Uk;Kim, Chul-Sung
    • Journal of the Korean Magnetics Society
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    • v.14 no.6
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    • pp.219-223
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    • 2004
  • L $i_{0.5}$F $e_{2.5-{\chi}}$R $h_{\chi}$ $O_4$ ($\chi$ = 0.25, 0.50, 0.75, 1.00) has been prepared by solid state reaction. Crystallographic and magnetic properties were investigated by Mossbauer spectroscopy, SQUID magnetometry, and x-ray diffraction. The crystal structure is found to be a cubic spinel structure with space group Fd3m for all the samples. The lattice constant $a_{0}$ increases from 8.3365 $\AA$ to 8.3932 $\AA$ with increasing Rh concentration $\chi$. The migration of Li ion has been confirmed by x-ray patterns and the results of applied field Mossbauer analysis. The temperature dependence of the absorption area of each site was analyzed with the Debye model for the recoil-free fraction. The Debye temperature for the octahedral sites is almost as large as for the tetrahedral sites, thereby suggesting similar inter-atomic binding forces for the octahedral and the tetrahedral sites. The saturated magnetic moment and the Mossbauer spectra taken at 4.2 K under the applied field (6 T) show that the spin structure of L $i_{0.5}$F $e_{2.5-{\chi}}$R $h_{\chi}$ $O_4$ is compatible with the collinear Neel Model.

The Evaluation of Reconstruction Method Using Attenuation Correction Position Shifting in 3D PET/CT (PET/CT 3D 영상에서 감쇠보정 위치 변화 방법을 이용한 영상 재구성법의 평가)

  • Hong, Gun-Chul;Park, Sun-Myung;Jung, Eun-Kyung;Choi, Choon-Ki;Seok, Jae-Dong
    • The Korean Journal of Nuclear Medicine Technology
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    • v.14 no.2
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    • pp.172-176
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    • 2010
  • Purpose: The patients' moves occurred at PET/CT scan will cause the decline of correctness in results by resulting in inconsistency of Attenuation Correction (AC) and effecting on quantitative evaluation. This study has evaluated the utility of reconstruction method using AC position changing method when having inconsistency of AC depending on the position change of emission scan after transmission scan in obtaining PET/CT 3D image. Materials and Methods: We created 1 mL syringe injection space up to ${\pm}2$, 6, 10 cm toward x and y axis based on central point of polystyrene ($20{\times}20110$ cm) into GE Discovery STE16 equipment. After projection of syringe with $^{18}F$-FDG 5 kBq/mL, made an emission by changing the position and obtained the image by using AC depending on the position change. Reconstruction method is an iteration reconstruction method and is applied two times of iteration and 20 of subset, and for every emission data, decay correction depending on time pass is applied. Also, after setting ROI to the position of syringe, compared %Difference (%D) at each position to radioactivity concentrations (kBq/mL) and central point. Results: Radioactivity concentrations of central point of emission scan is 2.30 kBq/mL and is indicated as 1.95, 1.82 and 1.75 kBq/mL, relatively for +x axis, as 2.07, 1.75 and 1.65 kBq/mL for -x axis, as 2.07, 1.87 and 1.90 kBq/mL for +y axis and as 2.17, 1.85 and 1.67 kBq/mL for -y axis. Also, %D is yield as 15, 20, 23% for +x axis, as 9, 23, 28% for -x axis, as 12, 21, 20% for +y axis and as 8, 22, 29% for -y axis. When using AC position changing method, it is indicated as 2.00, 1.95 and 1.80 kBq/mL, relatively for +x axis, as 2.25, 2.15 and 1.90 kBq/mL for -x axis, as 2.07, 1.90 and 1.90 kBq/mL for +y axis, and as 2.10, 2.02, and 1.72 kBq/mL for -y axis. Also, %D is yield as 13, 15, 21% for +x axis, as 2, 6, 17% for -x axis, as 9, 17, 17% for +y axis, and as 8, 12, 25% for -y axis. Conclusion: When in inconsistency of AC, radioactivity concentrations for using AC position changing method increased average of 0.14, 0.03 kBq/mL at x, y axis and %D was improved 6.1, 4.2%. Also, it is indicated that the more far from the central point and the further position from the central point under the features that spatial resolution is lowered, the higher in lowering of radioactivity concentrations. However, since in actual clinic, attenuation degree increases more, it is considered that when in inconsistency, such tolerance will be increased. Therefore, at the lesion of the part where AC is not inconsistent, the tolerance of radioactivity concentrations will be reduced by applying AC position changing method.

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Synthesis and Single-crystal Structure of Fully Dehydrated Fully Ca2+exchanged Zeolite Y (FAU), |Ca35.5|[Si121Al71O384]-FAU

  • Seo, Sung-Man;Choi, Sik-Young;Suh, Jeong-Min;Jung, Ki-Jin;Heo, Nam-Ho;Lim, Woo-Taik
    • Bulletin of the Korean Chemical Society
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    • v.30 no.8
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    • pp.1703-1710
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    • 2009
  • The single-crystal structure of |$Ca_{35.5}$|[$Si_{121}Al_{71}O_{384}$]-FAU, $Ca_{35.5}Si_{121}Al_{71}O_{384}$ per unit cell, a = 24.9020(10) $\AA$, dehydrated at 673 K and 2 ${\times}\;10^{-6}$Torr, has been determined by single-crystal X-ray diffraction techniques in the cubic space group Fd$\overline{3}$m at 294 K. The large single crystals of zeolite Y (Si/Al = 1.70) were synthesized up to diameters of ${\mu}m\;and\;Ca^{2+}$-exchanged zeolite Y were prepared by ion exchange in a batch method of 0.05 M aqueous Ca($NO_3)_2$ for 4 hrs at 294 K. The structure was refined using all intensities to the final error indices (using only the 971 reflections for which $F_o\;>\;4{\sigma}(F_o))\;R_1$ = 0.038 (based on F) and $R_2$ = 0.172 (based on $F^2$). About 35.5 $Ca^{2+}$ ions per unit cell are found at an unusually large number of crystallographically distinct positions, four. Nearly filling site I (at the centers of the double 6-rings), 14.5 octahedrally coordinated $Ca^{2+}$ ions (Ca-O = 2.4194(24) $\AA$ and O-Ca-O = 87.00(8) and 93.00($8^o$) are found per unit cell. One $Ca^{2+}$ ion per unit cell is located at site II’ in the sodalite cavity and extends 0.50 $\AA$ into the sodalite cavity from its 3-oxygen plane (Ca-O = 2.324(13) $\AA$ and O-Ca-O = 115.5(10)o). The remaining twenty $Ca^{2+}$ ions are found at two nonequivalent sites II (in the supercages) with occupancies of 10 and 10 ions, respectively. Each of these $Ca^{2+}$ ions coordinates to three framework oxygens, either at 2.283(3) or 2.333(5) $\AA$, respectively, and extends either 0.24 or 0.54 $\AA$, respectively, into the supercage from the three oxygens to which it is bound. In this crystal, site I is the most populated; sites II’ and II are only sparsely occupied.$Ca^{2+}$+ appears to fit the octahedral site I best. No cations are found at sites III or III’, which are clearly less favorable for $Ca^{2+}$ ions in dehydrated zeolite Y.

Formation and Characteristics of the Fluorocarbonated SiOF Film by $O_2$/FTES-Helicon Plasma CVD Method

  • Kyoung-Suk Oh;Min-Sung Kang;Chi-Kyu Choi;Seok-Min Yun
    • Proceedings of the Korean Vacuum Society Conference
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    • 1998.02a
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    • pp.77-77
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    • 1998
  • Present silicon dioxide (SiOz) 떠m as intennetal dielectridIMD) layers will result in high parasitic c capacitance and crosstalk interference in 비gh density devices. Low dielectric materials such as f f1uorina뼈 silicon oxide(SiOF) and f1uoropolymer IMD layers have been tried to s이ve this problem. I In the SiOF ftlm, as fluorine concentration increases the dielectric constant of t뼈 film decreases but i it becomes unstable and wa않r absorptivity increases. The dielectric constant above 3.0 is obtain어 i in these ftlms. Fluoropolymers such as polyte$\sigma$따luoroethylene(PTFE) are known as low dielectric c constant (>2.0) materials. However, their $\alpha$)Or thermal stability and low adhesive fa$\pi$e have h hindered 야1리ru뚱 as IMD ma따"ials. 1 The concept of a plasma processing a찌Jaratus with 비gh density plasma at low pressure has r received much attention for deposition because films made in these plasma reactors have many a advantages such as go여 film quality and gap filling profile. High ion flux with low ion energy in m the high density plasma make the low contamination and go어 $\sigma$'Oss피lked ftlm. Especially the h helicon plasma reactor have attractive features for ftlm deposition 야~au똥 of i앙 high density plasma p production compared with other conventional type plasma soun:es. I In this pa야Jr, we present the results on the low dielectric constant fluorocarbonated-SiOF film d밑JOsited on p-Si(loo) 5 inch silicon substrates with 00% of 0dFTES gas mixture and 20% of Ar g gas in a helicon plasma reactor. High density 띠asma is generated in the conventional helicon p plasma soun:e with Nagoya type ill antenna, 5-15 MHz and 1 kW RF power, 700 Gauss of m magnetic field, and 1.5 mTorr of pressure. The electron density and temperature of the 0dFTES d discharge are measUI벼 by Langmuir probe. The relative density of radicals are measured by optic허 e emission spe따'Oscopy(OES). Chemical bonding structure 3I피 atomic concentration 따'C characterized u using fourier transform infrared(FTIR) s야3띠"Oscopy and X -ray photonelectron spl:’따'Oscopy (XPS). D Dielectric constant is measured using a metal insulator semiconductor (MIS;AVO.4 $\mu$ m thick f fIlmlp-SD s$\sigma$ucture. A chemical stoichiome$\sigma$y of 야Ie fluorocarbina$textsc{k}$영-SiOF film 따~si야영 at room temperature, which t the flow rate of Oz and FTES gas is Isccm and 6sccm, res야~tvely, is form려 야Ie SiouFo.36Co.14. A d dielec$\sigma$ic constant of this fIlm is 2.8, but the s$\alpha$'!Cimen at annealed 5OOt: is obtain려 3.24, and the s stepcoverage in the 0.4 $\mu$ m and 0.5 $\mu$ m pattern 킹'C above 92% and 91% without void, res야~tively. res야~tively.

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