• Title/Summary/Keyword: 공정시험법

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열처리에 따른 Mo 박막의 잔류응력 완화에 관한 연구

  • Kim, Gang-Sam;Jo, Yong-Gi;Song, Yeong-Sik;Im, Tae-Hong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.02a
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    • pp.192-192
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    • 2011
  • Mo 박막은 열적 안전성과 전기 전도성이 우수한 소재로 CIGS 태양전지의 배면전극으로 사용되고 있다. 스퍼터링법에 의한 Mo 박막의 전도성은 공정압력에 민감하여 높은 압력과 낮은 압력에서 이중박막으로 제조되고 있다. 연구에서는 압력에 크게 영향을 받지 않으면서 전도성이 $10{\mu}{\Omega}-cm$ 이하로 우수한 Mo 박막을 얻을 수 있는 아크 이온플레이팅법으로 Mo 박막을 제조하였다. 그러나 Mo 박막 증착시에 나타나는 높은 압축응력은 기재(Soda lime Glass; SLG)와의 밀착성을 떨어뜨렸다. 기재(SLG)와의 밀착성을 확보하기 위해 Ti 중간층($0.3{\mu}m$, $0.9{\mu}m$)을 증착하고 그 위에 Mo 박막을 증착하여 전도성이 우수한 박막을 제조하였으나 여전히 압축잔류응력의 문제점을 보였다. 압축응력의 완화를 위해 CIGS 박막이 제조되는 $550^{\circ}C$의 온도에서 열처리를 1시간 수행하였다. 열처리를 통해 열처리 전과 후에 나타나는 전도성과 잔류응력의 변화를 공정압력(5 mTorr~30 mTorr)별로 알아보았다. 사용된 시험편은 Si wafer, SLG, SUS계 소재를 이용하였으며 공정압력별로 아크 타겟에 인가되는 전류는 100 A로 고정하였고, 바이어스 전압은 0V, -50V를 인가하였다. 열처리 전과 후에 전도성은 크게 변화가 관찰되지 않았으나 잔류응력에는 많은 변화가 관찰 되었다. 잔류응력은 공정압력(5mTorr~30mTorr)별로 응력 완화가 일어났으며, 바이어스 전압이 0V에서 공정압력이 5 mTorr일 때 열처리 전에 측정된 1346 MPa 압축응력이 열처리 후에는 188 MPa의 인장응력을 나타내었다. 이러한 응력 변화에 대해 XRD와 SEM으로 구조분석을 통해 Mo 박막의 결정성과 전도성 및 잔류응력의 상관관계에 대해 알아보았다.

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Establishment of an Analytical Method for Determination of Fungicide Oxathiapiprolin in Agricultural Commodities using HPLC-UV Detector (HPLC-UVD를 이용한 농산물 중 살균제 Oxathiapiprolin의 잔류분석법 확립)

  • Jang, Jin;Kim, Heejung;Do, Jung Ah;Ko, Ah-Young;Lee, Eun Hyang;Ju, Yunji;Kim, Eunju;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.31 no.3
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    • pp.186-193
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    • 2016
  • An analytical method was developed for the determination of oxathiapiprolin in agricultural commodities. Oxathiapiprolin is a new oomycide (fungicide of piperidinyl thiazole isoxazoline class) which controls downy mildew in cucurbits caused by Pseudoperonospora cubensis (oomycete plant pathogen). Agricultural commodities were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, adjusting pH between 9 and 10 by 1 N sodium hydroxide. After purification by silica SPE cartridge to clean up the interference of organic compounds, they were finally quantified by HPLC-UVD (high performance liquid chromatograph ultraviolet detector) using a wavelength at 260 nm and confirmed by LC-MS (liquid chromatograph mass spectrometer) in electro-spray ionization positive ion mode. The standard calibration curve was linear with coefficients of determination ($r^2$) 1.00 over the calibration ranges (0.025-2.5 mg/L). Recoveries were ranged between 86.7 to 112.7%, with relative standard deviations less than 10% at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates. The overall results were determined and estimated according to the CODEX guidelines (CAC/GL40). The proposed method for determination of oxathiapiprolin residues in agricultural commodities can be used as an official method.

Calibration: Theory and Practice (분석표준화와 검량선 작성의 국제적 동향)

  • Lee, Kyu-Seung;Kwon, Jin-Wook
    • Applied Biological Chemistry
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    • v.46 no.4
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    • pp.271-279
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    • 2003
  • Various definitions and terminology applied to measurement in analytical chemistry are not always consistent. But, internationally integrated terminology and interpretation of definitions play an essential role in analytical chemistry fields. The review in this paper focused on problems associated with terminology, definitions, statistical theories, and practical performance of calibration and validation.

Fabrication of MgO/NiCr bilayer coating via Plasma Electrolytic Oxidation and Radion Frequency Sputtering: Anti Corrosion Properties (플라즈마 전해 산화 및 고주파 스퍼터링을 통한 고내식성 MgO / NiCr 이중층 코팅 제조)

  • Gwon, Jeong-Hyeon;Na, Chan-Ung;Choe, Bo-Eun;Yun, Seong-Do
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2018.06a
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    • pp.63-63
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    • 2018
  • 본 연구는 플라즈마 전해 산화 (PEO) 및 RF (Radio Frequency) 스퍼터링을 이용한 2 단계 접근법에 의해 처리 된 MgO / Ni-Cr의 고내식성 이중층 코팅을 제조하기 위해 수행되었다. 이를 위해 $100mA/cm^2$ 교류 조건에서 180 s PEO를 한 후 150W 에서 900s RF 스퍼터링을 수행 하였다. 코팅의 형태는 주사전자현미경(SEM)을 사용하여 관찰되었으며 코팅의 상조성은 X-선 회절(XRD) 및 X-선 광전자 분광법(XPS)을 사용하여 분석하였다. SEM 이미지는 스퍼터링 된 Ni-Cr이 크랙의 대부분과 미세한 미세 공극을 덮어 코팅 결함이 감소함을 보여 주었다. 따라서, 코팅 된 샘플의 거칠기 값은 스퍼터링 공정 후에 감소되었다. 단면 이미지로부터, 스퍼터링된 코팅층은 낮은 두께 때문에 거의 검출되지 않았다. EDS, XRD 및 XPS를 사용한 조성 분석은 금속 상태의 형태로 Ni 및 Cr 존재를 나타내었고 XPS에서 NiCr2O4 부동태 피막이 검출되었다. MgO / Ni-Cr 이중층 코팅의 내부식성은 MgO / Ni-Cr 이중층을 가진 샘플의 금속 원소와 비교하여 우수한 부식 특성을 나타내는 전위 역학적 분극 시험 및 전기 화학적 임피던스 분광법으로 평가 하였다.

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Comparison and evaluation of methods for the measurement of total nitrogen in wastewater (고농도 질소함유 폐수의 총질소 분석법 비교·평가)

  • Choi, Sung-Deuk;Chang, Yoon-Seok
    • Analytical Science and Technology
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    • v.20 no.1
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    • pp.25-32
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    • 2007
  • The measurement methods for total nitrogen in wastewater containing a high concentration of nitrogen were evaluated. (1) The UV spectrophotometry, (2) reduction-distillation Kjeldahl, (3) total Kjeldahl nitrogen, and (4) ion chromatography methods were applied. The experimental procedure of the UV spectrophotometric method was simple, but it produced large errors deriving from the dilution of samples and calibration standards. While, the reduction-distillation Kjeldahl method didn't need dilution, but the amount of Devarda's alloy and NaOH lead to large errors up to 50 mg/L. The levels of total nitrogen measured by each method were as follows: reduction-distillation Kjeldahl ($568.6{\pm}38.7mg/L$) > UV spectrophotometry ($527.3{\pm}9.6mg/L$) > total Kjeldahl nitrogen method ($494.7{\pm}21.4mg/L$) > ion chromatography method ($417.9{\pm}7.3mg/L$). Therefore, the reduction-distillation Kjeldahl method is preferred for wastewater with the high concentration of nitrogen. Optimal conditions for each experimental procedure, however, are needed to be confirmed, and the Standard Operation Procedure (SOP) for total nitrogen is required for reliable measurements.

Establishment of an Analytical Method for Novobiocin in Livestock Products Using HPLC-UVD (HPLC-UVD를 이용한 축산식품 중 Novobiocin의 시험법 확립)

  • Park, Hee-Ra;Kwon, Chan-Hyeok;Lee, Jong-Goo;Kim, Hyung-Soo;Chae, Young-Sik;Oh, Jae-Ho;Kwon, Ki-Sung
    • Korean Journal of Food Science and Technology
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    • v.44 no.3
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    • pp.263-268
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    • 2012
  • Novobiocin is a coumarin-containing antibiotic, and has a longer half-life in various animals than other veterinary medicines. A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in chicken, beef and milk has been developed and validated. The separation condition for HPLC/UVD was optimized by a MG II $C_{18}$ (4.6 mm $ID{\times}250$ mm, 5 ${\mu}m$) column with 0.1% formic acid in $H_2O$/0.1% formic acid in Acetonitrile (40/60, v/v) as the mobile phase at a flow rate of 1.0 mL/min and the detection wavelength was set at 340 nm. Residues were extracted from tissue by blending with methanol. After liquid-liquid partitioning, lipid materials were removed with n-hexane and purification as Silica (1 g, 6 mL) cartridge with 10 mL acetone/dichloromethane (10/90, v/v). Limit of quantification and linearity performed by the analytical method were 0.02 mg/kg and 0.999 ($r^2$), and the recovery range was $88.8{\pm}5.6-100.3{\pm}4.4$, $88.8{\pm}7.2-97.0{\pm}3.2$ and $88.1{\pm}4.3-92.8{\pm}3.6%$. It is expected that this analytical method with regards to novobiocin in chicken, beef and milk could be applied as an official method to administer food safety on veterinary medicines.

Evaluation of Cryptosporidiurn Disinfection by Ozone and Ultraviolet Irradiation Using Viability and Infectivity Assays (크립토스포리디움의 활성/감염성 판별법을 이용한 오존 및 자외선 소독능 평가)

  • Park Sang-Jung;Cho Min;Yoon Je-Yong;Jun Yong-Sung;Rim Yeon-Taek;Jin Ing-Nyol;Chung Hyen-Mi
    • Journal of Life Science
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    • v.16 no.3 s.76
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    • pp.534-539
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    • 2006
  • In the ozone disinfection unit process of a piston type batch reactor with continuous ozone analysis using a flow injection analysis (FIA) system, the CT values for 1 log inactivation of Cryptosporidium parvum by viability assays of DAPI/PI and excystation were $1.8{\sim}2.2\;mg/L{\cdot}min$ at $25^{\circ}C$ and $9.1mg/L{\cdot}min$ at $5^{\circ}C$, respectively. At the low temperature, ozone requirement rises $4{\sim}5$ times higher in order to achieve the same level of disinfection at room temperature. In a 40 L scale pilot plant with continuous flow and constant 5 minutes retention time, disinfection effects were evaluated using excystation, DAPI/PI, and cell infection method at the same time. About 0.2 log inactivation of Cryptosporidium by DAPI/PI and excystation assay, and 1.2 log inactivation by cell infectivity assay were estimated, respectively, at the CT value of about $8mg/L{\cdot}min$. The difference between DAPI/PI and excystation assay was not significant in evaluating CT values of Cryptosporidium by ozone in both experiment of the piston and the pilot reactors. However, there was significant difference between viability assay based on the intact cell wall structure and function and infectivity assay based on the developing oocysts to sporozoites and merozoites in the pilot study. The stage of development should be more sensitive to ozone oxidation than cell wall intactness of oocysts. The difference of CT values estimated by viability assay between two studies may partly come from underestimation of the residual ozone concentration due to the manual monitoring in the pilot study, or the difference of the reactor scale (50 mL vs 40 L) and types (batch vs continuous). Adequate If value to disinfect 1 and 2 log scale of Cryptosporidium in UV irradiation process was 25 $mWs/cm^2$ and 50 $mWs/cm^2$, respectively, at $25^{\circ}C$ by DAPI/PI. At $5^{\circ}C$, 40 $mWs/cm^2$ was required for disinfecting 1 log Cryptosporidium, and 80 $mWs/cm^2$ for disinfecting 2 log Cryptosporidium. It was thought that about 60% increase of If value requirement to compensate for the $20^{\circ}C$ decrease in temperature was due to the low voltage low output lamp letting weaker UV rays occur at lower temperatures.

Bond Strength of Wafer Stack Including Inorganic and Organic Thin Films (무기 및 유기 박막을 포함하는 웨이퍼 적층 구조의 본딩 결합력)

  • Kwon, Yongchai;Seok, Jongwon
    • Korean Chemical Engineering Research
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    • v.46 no.3
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    • pp.619-625
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    • 2008
  • The effects of thermal cycling on residual stresses in both inorganic passivation/insulating layer that is deposited by plasma enhanced chemical vapor deposition (PECVD) and organic thin film that is used as a bonding adhesive are evaluated by 4 point bending method and wafer curvature method. $SiO_2/SiN_x$ and BCB (Benzocyclobutene) are used as inorganic and organic layers, respectively. A model about the effect of thermal cycling on residual stress and bond strength (Strain energy release rate), $G_c$, at the interface between inorganic thin film and organic adhesive is developed. In thermal cycling experiments conducted between $25^{\circ}C$ and either $350^{\circ}C$ or $400^{\circ}C$, $G_c$ at the interface between BCB and PECVD $ SiN_x $ decreases after the first cycle. This trend in $G_c$ agreed well with the prediction based on our model that the increase in residual tensile stress within the $SiN_x$ layer after thermal cycling leads to the decrease in $G_c$. This result is compared with that obtained for the interface between BCB and PECVD $SiO_2$, where the relaxation in residual compressive stress within the $SiO_2$ induces an increase in $G_c$. These opposite trends in $G_cs$ of the structures including either PECVD $ SiN_x $ or PECVD $SiO_2$ are caused by reactions in the hydrogen-bonded chemical structure of the PECVD layers, followed by desorption of water.

Measurement of EMC/PCB Interfacial Adhesion Energy of Chip Package Considering Warpage (휨을 고려한 칩 패키지의 EMC/PCB 계면 접합 에너지 측정)

  • Kim, Hyeong Jun;Ahn, Kwang Ho;Oh, Seung Jin;Kim, Do Han;Kim, Jae Sung;Kim, Eun Sook;Kim, Taek-Soo
    • Journal of the Microelectronics and Packaging Society
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    • v.26 no.4
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    • pp.101-105
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    • 2019
  • The adhesion reliability of the epoxy molding compound (EMC) and the printed circuit board (PCB) interface is critical to the quality and lifetime of the chip package since the EMC protects PCB from the external environment during the manufacturing, storage, and shipping processes. It is necessary to measure adhesion energy accurately to ensure product reliability by optimizing the manufacturing process during the development phase. This research deals with the measurement of EMC/PCB interfacial adhesion energy of chip package that has warpage induced by the coefficient of thermal expansion (CTE) mismatch. The double cantilever beam (DCB) test was conducted to measure adhesion energy, and the spring back force of specimens with warpage was compensated to calculate adhesion energy since the DCB test requires flat substrates. The result was verified by comparing the adhesion energy of flat chip packages come from the same manufacturing process.

Characterisrics of the Ag System Insert Metal Produced by Powder Mixing Process (분말 혼합 공정으로 만들어진 은계 삽입금속의 특성)

  • Kim, Gwang-Soo;Kim, Sang-Duck
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.9 no.2
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    • pp.311-316
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    • 2008
  • Powder type Ag system insert metals were manufactured by ball milling process. The variables of milling process were constant except the milling time. The milling times were selected for 24, 48 and 72 hours. The insert metals made by milling process were evaluated by performing scanning electron microscope, DSC(differential scanning calorimetry) analyses, spreading test and further in terms of wettability test. The selected insert metals that have the good characteristics compared to commercial insert metals were applied to make the brazed joints. The characterizations of those brazed joints were also conducted by microstructural observations. The results indicated that milling time of 48 hours for making powder type insert metals was the best condition showing the good spreadibility, low wetting angle. The brazed joints that applied the 48 hours milled insert metal were very sound condition indicating the stable microstructure in spite of containing small amount of porosity and the microhardness value of the joint was about 138VHN.