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Freehang 방법을 이용한 DLC 필름의 탄성 특성 평가

  • 정진원;이광렬;은광용;고대홍
    • Proceedings of the Korean Vacuum Society Conference
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    • 2000.02a
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    • pp.128-128
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    • 2000
  • 박막의 탄성 특성을 평가하는 방법으로 nano-indentation, Brillouin light scattering measurement, ultrasonic surface wave measurement, bulge test, vibration membrane method 등 여러 가지가 제시되어 왔다. 이러한 방법들은 필름의 두께가 일정 두께 이상이 되어야 정확한 측정이 가능한 방법으로 매우 얇은 박막에서도 탄성특성을 평가할 수 있는 freehang, bridge 방법이 제시되었으며, 이 방법은 간단한 식각 공정을 통해 매우 얇은 박막에도 적용시킬 수 있다는 장점을 가지고 있다. 본 연구에서는 아주 얇은 박막에서도 탄성특성을 평가할 수 있는 freehang 방법을 이용하여 순수한 Diamond-like carbon (DLC) 필름과 Sidl 첨가된 DLC 필름의 탄성 특성을 평가하고자 한다. 실험에서 사용한 필름은 rf-PACVD 장비를 이용하여 증착하였다. 이때 전극과 플라즈마 사이의 바이어스 음전압은 -400 Vb로 합성압력은 10mTorr로 고정하였다. 사용한 반응 가스는 벤젠(C6H6), 그리고 벤젠과 희석된 실렌(SiH4 : H2 = 10 : 90)이며, 희석된 실렌의 첨가량을 조절하여 필름 내에 일정량의 Si을 함유시켰다. 각각의 조건에서 증착시간을 조절하여 필름의 두께를 변화시켰으며, KOH(5.6mol) 용액을 이용하여 습식 식각을 함으로써 freehang을 제작하였다. 이때 식각액에 의한 DLC 필름의 손상은 관찰되지 않았다. 필름의 잔류 응력을 측정하기 위해 200$\pm$10 혹은 100$\pm$5$\mu\textrm{m}$ 두께의 얇은 (100) Si wafer를 5$\times$50 mm2의 strip 형태로 절단하여 사용하였다. 필름의 압축 잔류 응력에 의해 발생한 필름/기판 복합체의 곡률은 laser 반사법과 $\alpha$-step profiler를 이용하여 측정하였으며, 이 결과를 Brenner 등에 유도된 식을 이용하여 잔류 응력을 계산하였다. 또한 제작된 frddhang은 광학 현미경과 전자주사현미경에 의해 관찰되었다. 이렇게 제작된 freehang을 이용하여 필름이 기판에 부착되기 위해 필요한 변형률을 측정하고, 독립적으로 측정된 필름의 잔류 응력을 박막의 응력-변형률 관계식에 적용하여 biaxial elastic modulus, E/(1-v)를 구할 수 있었다. 측정 결과 필름의 잔류 응력과 biaxial elastic modulus는 필름의 두께가 감소함에 따라 감소하는 경향을 나타냈으며, 같은 두께의 필름인 경우, 식각 깊이에 따른 biaxial elastic modulus 의 변화를 통해 최적의 식각 깊이를 알 수 있었다.

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Effects of Processing Parameters on the Fabrication of in-situ Al/TiC Composites by Thermally Activated Combustion Reaction Process in an Aluminium Melt using Al-TiO2-C Powder Mixtures (알루미늄 용탕에서 Al-TiO2-C의 연소합성반응에 의한 in-situ Al/TiC 복합재료의 제조에 미치는 공정변수의 영향)

  • Kim, Hwa-Jung;Lee, Jung-Moo;Cho, Young-Hee;Kim, Jong-Jin;Kim, Su-Hyeon;Lee, Jae-Chul
    • Korean Journal of Metals and Materials
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    • v.50 no.9
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    • pp.677-684
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    • 2012
  • A feasible way to fabricate in-situ Al/TiC composites was investigated. An elemental mixture of $Al-TiO_2-C$ pellet was directly added into an Al melt at $800-920^{\circ}C$ to form TiC by self-combustion reaction. The addition of CuO initiates the self-combustion reaction to form TiC in $1-2{\mu}m$ at the melt temperature above $850^{\circ}C$. Besides the CuO addition, a diluent element of excess Al plays a significant role in the TiC formation by forming a precursor phase, $Al_3Ti$. Processing parameters such as CuO content, the amount of excess Al and the melt temperature, have affected the combustion reaction and formation of TiC, and their influences on the microstructures of in-situ Al/TiC composites are examined.

6-(1-Hydroxy or Acyloxyalkyl)-5,8-Dialkoxy-1,4-Naphthoquinones: Synthesis, Evaluation of Cytotoxic Activity; Antitumor Activity and Inhibitory effect on DNA Topoisomerase-I (6-(1-하이드록시 또는 아실옥시알킬)-5,8-디알콕시-1,4-나프토퀴논 유도체의 합성, DNA Topoisomerase-I에 대한 억제, 세포독성 및 항암활성)

  • Kim, Yong;Choi, Su-La;Myung, Pyung-Keun;Ahn, Byung-Zun
    • YAKHAK HOEJI
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    • v.44 no.2
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    • pp.141-148
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    • 2000
  • A new synthetic method of 6-(1-oxyalkyl)-5,8-dimethoxy-1,4-naphthoquinones was developed, 2-formyl-1,4,5,8-tetramethoxynaphthalene was oxidized to form 6-formyl-5,8-dimethoxy-1,4-naphthoquinone(DMNQ). This was selectively reduced and benzylated to produce 6-formyl-5,8-dimethoxy-1,4-dibenzyloxynaphthalene, to which various alkylmagnesium halide were added, followed by debenzylation and oxidation in sequence, yielding 6-(1-hydroxyalkyl)-DMNQ derivatives. 6-(1-hydroxyalkyl)-5,8-diethoxy-1,4-naphthalene (DENQ) derivatives were synthesized by similar procedure. 1'-OH of the naphthoquinone derivatives was acylated with various alkanoic acids to give 6-(1-acyloxyalkyl)-DMNQ or DENQ derivatives. TOPO-I inhibitory activity and cytotoxicity of DENQs were less potent than that of DMNQs. Among the DMNQ and DENQ analogues, the ones with alkyl group being heptyl were most potent in TOPO-I inhibition $IC_{50}$/; 30.1, 36.4 $\mu$M). DUNQ derivatives with a longer side chain exhibited a weaker cytotoxicity. A correlation between size of the alkyl side chain and cytotoxicity was not observed for DENQ derivatives. Acylation of 1'-hydroxyl group, in general, decreased both TOPO-I inhibitory activity and cytotoxicity T/C (%) values of the DENQ derivatives on S-180 intraperitoneal tumor were larger than those of DMNQ derivatives. Among the compounds synthesized,6-(1-hydroxyheptyl)-DENQ and 6-(1-hex-anoyloxyoctyl)-DMNQ showed the highest T/C values of 183% and 182%, respectively.

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Effects of the Mixing Method and Sintering Temperature on the Characteristics of PZNN-PZT Piezoelectric Ceramic Materials (합성방법과 소결 온도가 PZNN-PZT 압전 세라믹스 소재특성에 미치는 영향)

  • Kim, So Won;Jeong, Yong Jeong;Lee, Hee Chul
    • Journal of Powder Materials
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    • v.25 no.6
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    • pp.487-493
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    • 2018
  • The impact of different mixing methods and sintering temperatures on the microstructure and piezoelectric properties of PZNN-PZT ceramics is investigated. To improve the sinterability and piezoelectric properties of these ceramics, the composition of $0.13Pb((Zn_{0.8}Ni_{0.2})_{1/3}Nb_{2/3})O_3-0.87Pb(Zr_{0.5}Ti_{0.5})O_3$ (PZNN-PZT) containing a Pb-based relaxor component is selected. Two methods are used to create the powder for the PZNN-PZT ceramics. The first involves blending all source powders at once, followed by calcination. The second involves the preferential creation of columbite as a precursor, by reacting NiO with $Nb_2O_5$ powder. Subsequently, PZNN-PZT powder can be prepared by mixing the columbite powder, PbO, and other components, followed by an additional calcination step. All the PZNN-PZT powder samples in this study show a nearly-pure perovskite phase. High-density PZNN-PZT ceramics can be fabricated using powders prepared by a two-step calcination process, with the addition of 0.3 wt% MnO2 at even relatively low sintering temperatures from $800^{\circ}C$ to $1000^{\circ}C$. The grain size of the ceramics at sintering temperatures above $900^{\circ}C$ is increased to approximately $3{\mu}m$. The optimized PZNN-PZT piezoelectric ceramics show a piezoelectric constant ($d_{33}$) of 360 pC/N, an electromechanical coupling factor ($k_p$) of 0.61, and a quality factor ($Q_m$) of 275.

Adsorption and Desorption Characteristics of Sr, Cs, and Na Ions with Na-A Zeolite Synthesized from Coal Fly Ash in Low-Alkali Condition (석탄 비산재로부터 저알칼리 조건에서 합성된 Na-A 제올라이트의 Sr, Cs 및 Na 이온의 흡탈착 특성)

  • Choi, Jeong-Hak;Lee, Chang-Han
    • Journal of Environmental Science International
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    • v.28 no.6
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    • pp.561-570
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    • 2019
  • A zeolitic material (Z-Y2) was synthesized from Coal Fly Ash (CFA) using a fusion/hydrothermal method under low-alkali condition (NaOH/CFA = 0.6). The adsorption performance of the prepared zeolite was evaluated by monitoring its removal efficiencies for Sr and Cs ions, which are well-known as significant radionuclides in liquid radioactive waste. The XRD (X-ray diffraction) patterns of the synthesized Z-Y2 indicated that a Na-A type zeolite was formed from raw coal fly ash. The SEM (scanning electron microscope) images also showed that a cubic crystal structure of size $1{\sim}3{\mu}m$ was formed on its surface. In the adsorption kinetic analysis, the adsorption of Sr and Cs ions on Z-Y2 fitted the pseudo-second-order kinetic model well, instead of the pseudo-first-order kinetic model. The second-order kinetic rate constant ($k_2$) was determined to be $0.0614g/mmol{\cdot}min$ for Sr and $1.8172g/mmol{\cdot}min$ for Cs. The adsorption equilibria of Sr and Cs ions on Z-Y2 were fitted successfully by Langmuir model. The maximum adsorption capacity ($q_m$) of Sr and Cs was calculated as 1.6846 mmol/g and 1.2055 mmol/g, respectively. The maximum desorption capacity ($q_{dm}$) of the Na ions estimated via the Langmuir desorption model was 2.4196 mmol/g for Sr and 2.1870 mmol/g for Cs. The molar ratio of the desorption/adsorption capacity ($q_{dm}/q_m$) was determined to be 1.44 for Na/Sr and 1.81 for Na/Cs, indicating that the amounts of desorbed Na ions and adsorbed Sr and Cs ions did not yield an equimolar ratio when using Z-Y2.

Research on Afterglow Brightness of Sr4-(x+y+z)Al14O25 : Eux, Dyy, Agz by Solid State Synthesis (고상법으로 합성한 Sr4-(x+y+z)Al14O25 : Eux, Dyy, Agz계 축광성 형광체 장잔광의 연구)

  • Kim, Seung-woo;Kim, Jung-sik
    • Korean Journal of Metals and Materials
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    • v.49 no.4
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    • pp.348-354
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    • 2011
  • Long-lasting brightness $Sr_{4}Al_{14}O_{25}$ : $Eu^{2+}$, $Dy^{3+}$, $Ag^{+}$ phosphor was synthesized by modified solid state reaction and its photoluminescence was investigated. $Sr(NO_3)_{2}$ and $Al(NO_3)_3{\cdot}9H_{2}O$ as starting materials, and $B_{2}O_{3}$ as a flux were mixed with $Eu_{2}O_{3}$ as an activator, $Dy_{2}O_{3}$ as a coactivator, and $AgNO_{3}$ as a charge compensator. The crystalline of target powder showed a single-phase $Sr_{4}Al_{14}O_{25}$ by the XRD characterization and the average particle size was about 20-30 ${\mu}m$ from the FE-SEM observation. $Ag^{+}$ ion doping effects (0-0.06 mol) on $Sr_{4}Al_{14}O_{25}:Eu^{2+},\;Dy^{3+},\;Ag^{+}$ phosphor were measured by photoluminescence spectrometer and luminescence meter. The of photoluminescence intensity of the $Sr_{3.64}Al_{14}O_{25}:Eu_{0.11},\;Dy_{0.22},\;Ag_{0.03}$ phosphor was higher than other compositions and afterglow brightness was 0.186 $cd/m^{2}$.

Adsorption of Arsenate on the Synthesized Layered Double Hydroxide Materials (층상이중 수산화물을 이용한 5가 비소 흡착 특성)

  • Choi, Young-Mu;Choi, Won-Ho;Kim, Jung-Hwan;Park, Joo-Yang
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.29 no.1B
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    • pp.91-96
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    • 2009
  • Layered double hydroxide is synthesized and used in the arsenate adsorption experiments. The shapes of two materials analyzed by TEM showed that unheated material is amorphous in shape, micro-sized while heat treated material showed more crystallized in shape and nano-sized. X-ray diffraction showed this result more obvious. $N_2$ adsorption-desorption results showed that the materials are mesoporous and the specific surface area of the heated material is more than two times larger than the unheated material. Adsorption of As(V) is expected to be more in the heated material than the unheated material. Kinetic test of arsenate adsorption showed very fast reaction. The reactivity of Fe with As(V) might be the main factor for this result. The reaction kinetic of the heated and the unheated materials were similar and even the adsorption isotherms showed similar results for both materials. Both materials are found to be useful in remediation of soil and groundwater polluted by waste mine tailings consist of high concentration of As(V).

A Study on Optimal Packing Volume of Media in Swirl Flow Biological Fluidized Bed (선회류 생물학적 유동상의 최적 메디아 충전량에 관한 연구)

  • Choi, Doo-Hyoung;Kim, Hwan-Gi
    • Journal of Korean Society of Environmental Engineers
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    • v.22 no.2
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    • pp.331-340
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    • 2000
  • The existing two-phase biological fluidized bed has some problems such as limit of oxygen transfer and blockade of fluidized distributor. In this study, three-phase swirl flow biological fluidized bed has designed to solve the problems and to investigate its running characteristics. TOC of influent synthetic wastewater was approximately $70mg/{\ell}$. HRT of reactor was 1.6 hours. Mean particle size of sand, as packing media, was 0.397mm and packing volume was varied from $200m{\ell}/{\ell}$ to $600m{\ell}/{\ell}$ by stages in the bed. The amount of biomass and effluent water quality was throughly investigated in the bed. Showing experiment results from the above conditions, it was possible to solve the problems of existing fluidized bed and to keep DO of $3mg/{\ell}$ or more. And it was also TOC removal rate of 91 to 94 %, MLVSS of 2,360 to $3,860mg/{\ell}$, MLVSS per g-media of 8.4 to 17.3 mg/g, F/M ratio of 0.59 to $1.04kg-TOC/kg-MLVSS{\cdot}day$, biofilm thickness of $35{\sim}71{\mu}m$ and sludge productivity of 1.03 to $2.35kg-SS/m^3{\cdot}day$. Optimal conditions in this experimental were as follows.; those were biofilm thickness of approximately $54{\mu}m$. MLVSS per g-media of 13 mg and media packing volume of 350 to $400m{\ell}/{\ell}$ when F/M ratio was low, treatment efficiency was high and sludge productivity was low. Showing the media with optics microscope in this optimal condition, attached microbes such as Epistylis sp. were observed. From SEM photographs, it showed that Coccus adhere to and grow on the media surface.

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Determination of methamphetamine, 4-hydroxymethamphetamine, amphetamine and 4-hydroxyamphetamine in urine using dilute-and-shoot liquid chromatography-tandem mass spectrometry (시료 희석 주입 LC-MS/MS를 이용한 소변 중 메스암페타민, 4-하이드록시메스암페타민, 암페타민 및 4-하이드록시암페타민 동시 분석)

  • Heo, Bo-Reum;Kwon, NamHee;Kim, Jin Young
    • Analytical Science and Technology
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    • v.31 no.4
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    • pp.161-170
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    • 2018
  • The epidemic of disorders associated with synthetic stimulants, such as methamphetamine (MA) and amphetamine (AP), is a health, social, legal, and financial problem. Owing to the high potential of their abuse and addiction, reliable analytical methods are required to detect and identify MA, AP, and their metabolites in biological samples. Thus, a dilute-and-shoot liquid chromatography-tandem mass spectrophotometry (LC-MS/MS) was developed for simultaneous determination of MA, 4-hydroxymethamphetamine (4HMA), AP, and 4-hydroxyamphetamine (4HA) in urine. Urine sample ($100{\mu}L$) was mixed with $50{\mu}L$ of mobile phase consisting of 0.4 % formic acid and methanol and $50{\mu}L$ of working internal-standard solution. Aliquots of $8{\mu}L$ diluted urine was injected into the LC-MS/MS system. For all analytes, chromatographic separation was performed using a C18 reversed-phase column with gradient elution and a total run time of 5 min. The identification and quantification were performed by multiple reaction monitoring (MRM). Linear least-squares regression was conducted to generate a calibration curve, with $1/x^2$ as the weighting factor. The linear ranges were 2.0-200, 1.0-800, and 10-2500 ng/mL for 4HA and 4HMA, AP, and MA, respectively. The inter- and intraday precisions were within 6.6 %, whereas the inter- and intraday accuracies ranged from -14.9 to 11.3 %. The low limits of quantification were 2.0 ng/mL (4HA and 4HMA), 1.0 ng/mL (AP), and 10 ng/mL (MA). The proposed method exhibited satisfactory selectivity, dilution integrity, matrix effect, and stability, which are required for validation. Moreover, the purification efficiency of high-speed centrifugation was clearly higher than 6-15 % for QC samples (n=5), which was higher than that of the membrane-filtration method. The applicability of the proposed method was tested by forensic analysis of urine samples from drug abusers.

Characterization of a Psychrophilic Metagenome Esterase EM2L8 and Production of a Chiral Intermediate for Hyperlipemia Drug (메타게놈유래의 저온성 에스터라제 EM2L8의 효소적 특성과 이를 활용한 고지혈증 치료제 키랄소재의 생산)

  • Jung, Ji-Hye;Choi, Yun-Hee;Lee, Jung-Hyun;Kim, Hyung-Kwoun
    • Microbiology and Biotechnology Letters
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    • v.37 no.2
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    • pp.118-124
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    • 2009
  • Esterase EM2L8 gene isolated from deep sea sediment was expressed in Escherichia coli BL21 (DE3) and the esterase activity of the cell-free extract was assayed using p-nitrophenyl butyrate-spectrophotometric method. Its optimum temperature was $40-45^{\circ}C$ and 45% activity of the maximum activity was retained at $15^{\circ}C$. The activation energy at $15-45^{\circ}C$ was calculated to be 4.9 kcal/mol showing that esterase EM2L8 was a typical cold-adapted enzyme. Enzyme activity was maintained for 6 h and 4 weeks at $30^{\circ}C$ and $4^{\circ}C$, respectively. When each ethanol, methanol, and acetone was added to the reaction mixture to 15% concentration, enzyme activity was maintained. In the case of DMSO, enzyme activity was kept up to 40% concentration. (S)-4-Chloro-3-hydroxy butyric acid is a chiral intermediate for the synthesis of Atorvastatin, a hyperlipemia drug. When esterase EM2L8 (40 U) was added to buffer solution (1.2 mL, pH 9.0) containing ethyl-(R,S)-4-chloro-3-hydroxybutyrate (38 mM), it was hydrolyzed into 4-chloro-3-hydroxy butyric acid with a rate of $6.8\;{\mu}mole/h$. The enzyme hydrolyzed (S)-substrate more rapidly than (R)-substrate. When conversion yield was 80%, e.e.s value was 40%. When DMSO was added, hydrolysis rate increased to $10.4\;{\mu}mole/h$. The plots of conversion yield vs e.e.s in the presence or absence of DMSO were almost same, implying that the reaction enantioselectivity was not changed by the addition of DMSO. Taken together, esterase EM2L8 had high activity and stability at low temperatures as well as in various organic solvents/aqueous solutions. These properties suggested that it could be used as a biocatalyst in the synthesis of useful pharmaceuticals.