• Title/Summary/Keyword: Sample matrix

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Simultaneous Determination and Monitoring of Three Macrolide Antibiotics in Foods by HPLC (Macrolide계 항생물질 동시분석법 확립 및 모니터링)

  • Park, Sang-Ouk;Lee, Sang-Ho;Ahn, Jong-Hoon;Jung, Young-Ji;Kim, Seong-Cheol;Kim, Ji-Yeon;Keum, Eun-Hee;Sung, Ju-Hyun;Kim, Sang-Yub;Jang, Young-Mi;Kang, Chan-Soon
    • Korean Journal of Food Science and Technology
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    • v.42 no.3
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    • pp.287-291
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    • 2010
  • In this study, a simple and rapid pre-treatment method based on liquid extraction was applied for the simultaneous determination of three macrolides (spiramycin, tylosin, and tilmicosin) residues. In these studies, the stock farm products was used as a matrix sample. When the liquid extraction method was compared with the solid phase extraction (SPE) method, the former showed higher recovery percentages and simpler steps than the latter. The macrolids were separated using a reverse-phase C18 ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$) column and a gradient elution with mobile phases consisting of phosphate buffer (pH 2.5) and acetonitrile. Tylosin and tilmicosin were detected at 288 nm and spiramycin was detected at 232 nm. The average recovery percentage ranged between 83.0-90.2% for samples spiked with the three macrolids at 50 and 100 ng/g The validation results showed that the limit of detection (7 (spiramycin), 12 (tilmiconsin), 12 (tylosin) ng/g)) was under the regulatory tolerances and the linearity from calibration curves was satisfactory for determining the multi-residue of three macrolids in farm products. Monitoring samples were collected at the main cities in Korea as Seoul, Busan, Deajeon, Incheon, Deagu, and Gwangju. Microlide antibiotics were not detected in most samples.

Airborne Hyperspectral Imagery availability to estimate inland water quality parameter (수질 매개변수 추정에 있어서 항공 초분광영상의 가용성 고찰)

  • Kim, Tae-Woo;Shin, Han-Sup;Suh, Yong-Cheol
    • Korean Journal of Remote Sensing
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    • v.30 no.1
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    • pp.61-73
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    • 2014
  • This study reviewed an application of water quality estimation using an Airborne Hyperspectral Imagery (A-HSI) and tested a part of Han River water quality (especially suspended solid) estimation with available in-situ data. The estimation of water quality was processed two methods. One is using observation data as downwelling radiance to water surface and as scattering and reflectance into water body. Other is linear regression analysis with water quality in-situ measurement and upwelling data as at-sensor radiance (or reflectance). Both methods drive meaningful results of RS estimation. However it has more effects on the auxiliary dataset as water quality in-situ measurement and water body scattering measurement. The test processed a part of Han River located Paldang-dam downstream. We applied linear regression analysis with AISA eagle hyperspectral sensor data and water quality measurement in-situ data. The result of linear regression for a meaningful band combination shows $-24.847+0.013L_{560}$ as 560 nm in radiance (L) with 0.985 R-square. To comparison with Multispectral Imagery (MSI) case, we make simulated Landsat TM by spectral resampling. The regression using MSI shows -55.932 + 33.881 (TM1/TM3) as radiance with 0.968 R-square. Suspended Solid (SS) concentration was about 3.75 mg/l at in-situ data and estimated SS concentration by A-HIS was about 3.65 mg/l, and about 5.85mg/l with MSI with same location. It shows overestimation trends case of estimating using MSI. In order to upgrade value for practical use and to estimate more precisely, it needs that minimizing sun glint effect into whole image, constructing elaborate flight plan considering solar altitude angle, and making good pre-processing and calibration system. We found some limitations and restrictions such as precise atmospheric correction, sample count of water quality measurement, retrieve spectral bands into A-HSI, adequate linear regression model selection, and quantitative calibration/validation method through the literature review and test adopted general methods.

Study on the screening method for determination of heavy metals in cellular phone for the restrictions on the use of certain hazardous substances (RoHS) (유해물질 규제법(RoHS)에 따른 휴대폰 내의 중금속 함유량 측정을 위한 스크리닝법 연구)

  • Kim, Y.H.;Lee, J.S.;Lim, H.B.
    • Analytical Science and Technology
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    • v.23 no.1
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    • pp.1-14
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    • 2010
  • It is of importance that all countries in worldwide, including EU and China, have adopted the Restrictions on the use of certain Hazardous Substances (RoHS) for all electronics. IEC62321 document, which was published by the International Electronics Committee (IEC) can have conflicts with the standards in the market. On the contrary Publicly Accessible Specification (PAS) for sampling published by IEC TC111 can be adopted for complementary application. In this work, we tried to find a route to disassemble and disjoint cellular phone sample, based on PAS and compare the screening methods available in the market. For this work, the cellular phone produced in 2001, before the regulation was born, was chosen for better detection. Although X-ray Fluorescence (XRF) showed excellent performance for screening, fast and easy handling, it can give information on the surface, not the bulk, and have some limitations due to significant matrix interference and lack of variety of standards for quantification. It means that screening with XRF sometimes requires supplementary tool. There are several techniques available in the market of analytical instruments. Laser ablation (LA) ICP-MS, energy dispersive (ED) XRF and scanning electron microscope (SEM)-energy dispersive X-ray (EDX) were demonstrated for screening a cellular phone. For quantitative determination, graphite furnace atomic absorption spectrometry (GF-AAS) was employed. Experimental results for Pb in a battery showed large difference in analytical results in between XRF and GF-AAS, i.e., 0.92% and 5.67%, respectively. In addition, the standard deviation of XRF was extremely large in the range of 23-168%, compared with that in the range of 1.9-92.3% for LA-ICP-MS. In conclusion, GF-AAS was required for quantitative analysis although EDX was used for screening. In this work, it was proved that LA-ICP-MS can be used as a screening method for fast analysis to determine hazardous elements in electrical products.

Development of Simultaneous Analytical Method for Determination of Isoxaflutole and its Metabolite (Diketonitrile) residues in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Isoxaflutole과 대사산물(Diketonitrile)의 동시시험법 개발)

  • Ko, Ah-Young;Kim, Heejung;Do, Jung Ah;Jang, Jin;Lee, Eun-Hyang;Ju, Yunji;Kim, Ji Young;Chang, Moon-Ik;Rhee, Gyu-Seek
    • The Korean Journal of Pesticide Science
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    • v.20 no.2
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    • pp.93-103
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    • 2016
  • A simultaneous analytical method was developed for the determination of isoxaflutole and metabolite (diketonitrile) in agricultural commodities. Samples were extracted with 0.1% acetic acid in water/acetonitrile (2/8, v/v) and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2 by 1 N hydrochloric acid. The analytes were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive-ion mode using multiple reaction monitoring (MRM). Matrix matched calibration curves were linear over the calibration ranges ($0.02-2.0{\mu}g/mL$) for all the analytes into blank extract with $r^2$ > 0.997. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. The recoveries were ranged between 72.9 to 107.3%, with relative standard deviations (RSDs) less than 10% for all analytes. All values were consistent with the criteria ranges requested in the Codex guideline (CAC/GL40, 2003). Furthermore, inter-laboratory study was conducted to validate the method. The proposed analytical method was accurate, effective, and sensitive for isoxaflutole and diketonitrile determination in agricultural commodities.

The Ability of Cervus Elaphus Sibiricus Herbal Acupuncture to Inhibit the Generation of Inflammatory Enzymes on Collagen-induced Arthritis Mice (녹용약침(鹿茸藥鍼)이 CIA 모델 생쥐의 염증인자 생성억제에 미치는 영향)

  • Hwang, Jong-Soon;Hwang, Ji-Hye;Lee, Hyun-Jin;Lee, Dong-Gun;Kang, Min-Joo;Back, Song-Ook;Cho, Hyun-Seok;Kim, Kyung-Ho;Kim, Kap-Sung
    • Journal of Acupuncture Research
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    • v.24 no.6
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    • pp.1-14
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    • 2007
  • Backgrounds : Rheumatoid Arthritis(RA) is known as the chronic inflammatory diseasethat induces persistent inflammation in the joint cavity. The destruction of cartilage occurs as the result of bones destoyed by pannus, several influential cytokines induced by the synovial capsulitis, varieties of proteinases, $O_2$ radicals, and the secondary degenerative changes of articular cartilage. The type 2 collagen-induced arthritis model is used in recent experimental research on rheumatoid arthritis. Cervus elaphus sibiricus (Nockyong) has the effect of relieving pain by nourishing the muscles, joints, and bones. It is also known to be efficacious in promoting and enhancing the immune system. The objective of this study was to investigate the effect of Cervus elaphus sibiricus herbal acupuncture to inhibit the generation of proinflammatory enzyme on type 2 collagen-induced arthritis. I investigated the inhibition of mRNA transcription of MIF(macrophage migration inhibitory factor), $TNF-{\alpha}$(Tumor necrosis $factor-{\alpha}$) and MMP-9 (matrix metalloproteinase-9) of Cervus elaphus sibiricus herbal acupuncture using an in vitro test. Also investigated was the inhibition of differentiation of Th 1 cells and activation of cytokines(MIF, $TNF-{\alpha}$, IL-6, MMP-9), which are known to cause initial RA ,and are also related to the morphology of the synovial membranes of the joint capsule, by an in vivo test, using CIA(collagen induced arthritis) model mice. Materials & methods : The laboratory animals used in this experiment were 4 week-old DBA female mice, weighing approximately 20 grams, and adjusted to the laboratory environment. The experiment was divided into the normal group(NOR)-no treated group, control group(CON)-CIA induced group, and sample group(SAM)-Cervus elaphus sibiricus herbal acupuncture treated group. RA was induced in the mice via injection of $50{\mu}{\ell}$ C II mixed CFA. The Cervus elaphus sibiricus herbal acupuncture solution was applied on $GB_{35}$(陽陵泉) for 26 days from the 3rd day of RA inducement. The concentration of the solution was determined via a MTT assay. To research the effect on the expression of MIF, $TNF-{\alpha}$ and MMP-9 mRNA, RT-PCR was performed on synovial membrane cells from the knee joint of CIA mice. C II induced RA knee joint's histo-chemical synovial membrane was observed using a specimen model via the Hematoxilin and Eosin dying technique. Results : The expression of mRNA of RA-related cytokines such as MIF, $TNF-{\alpha}$, and MMP-9 dosedependently decreased in the cell from the synovial membranes of the joint, which is treated with Cervus elaphus sibiricus herbal acupuncture solution. In mice treated with Cervus elaphus sibiricusherbal acupuncture, the damage of synovial membranes of the joint was lessened, and differentiation of Th 1 cells was suppressed. The activation of RA-related cytokines such as MIF was suppressed, and the generation of $TNF-{\alpha}$ and MMP-9 showed a statistically significant decreas. Conclusions : It is speculated that Cervus elaphus sibiricus herbal acupuncture has the therapeutic effect of palliating the damage of the tissue impaired by RA by inhibition of the initial RA progression and by regulating excessive differentiation of Th 1 cell as it suppresses the generation of RA-related cytokines during the highest stage of RA by acting on pro-inflammatory enzymes.

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Usefulness of Flow Composite Image in Raynaud Scan ($^{201}Tl$) ($^{201}Tl$을 이용한 레이노 검사에서 동적 Composite 영상의 유용성)

  • Kim, Dae-Yeon;Shin, Gyoo-Seol;Oh, Eun-Jung;Kim, Gun-Jae
    • The Korean Journal of Nuclear Medicine Technology
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    • v.14 no.1
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    • pp.101-104
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    • 2010
  • Purpose: Raynaud scan is divided to flow, blood pool and local-delay image. Usually, we evaluate comparison through blood pool and local-delay image. We will evaluate about usability when comparative observe blood image and local-delay image in Raynaud scan that used $^{201}Tl$ as making flow image to one sheet of images. Materials and Methods: We have selected 29 Raynaud phenomenon patients aged 14~68 years who visited department of vascular surgery between Feb. 2008 and Aug. 2009. An intravenous injection $^{201}Tl$ of 111 MBq (3 mCi) to opposite side diagonal line limbs above an internal auditing department. Equipment used Philips gamma camera forte A-Z, and collimator used LEHR. Matrix size set up to each $64{\times}64$, $128{\times}128$, $256{\times}256$ and zoom factor used to full field. Protocol of dynamic is 2 second to 155 frames. Blood pool and delay count to 300 second. We set up ROI by a foundation to data acquired in PEGASYS processing program. Each results were analyzed with the SPSS 12.0 statistical software. Results: Each averages of count ratio (Rt / Lt) to have been given at composite image, a blood pool image, delay images analyzed at Raynaud phenomenon patients is $1.25{\pm}0.39$, $1.20{\pm}0.33$, $1.11{\pm}0.17$. The sample analysis results of blood pool image and delay image contented itself with p<0.029. Also, there don't have been each difference, and blood pool image, delay image regarding composite image was able to know. Conclusion: We were able to give help for comparison to evaluate a blood pool image and a local delay image at the Raynaud scan which used $^{201}Tl$ while making a flow image to one sheet image. Identification to be visual too was possible. If you are proceeded a researcher that there was further depth, you are more appropriate for, and you may get useful information.

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Stellite bearings for liquid Zn-/Al-Systems with advanced chemical and physical properties by Mechanical Alloying and Standard-PM-Route

  • Zoz, H.;Benz, H.U.;Huettebraeucker, K.;Furken, L.;Ren, H.;Reichardt, R.
    • Proceedings of the Korean Powder Metallurgy Institute Conference
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    • 2000.04a
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    • pp.9-10
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    • 2000
  • An important business-field of world-wide steel-industry is the coating of thin metal-sheets with zinc, zinc-aluminum and aluminum based materials. These products mostly go into automotive industry. in particular for the car-body. into building and construction industry as well as household appliances. Due to mass-production, the processing is done in large continuously operating plants where the mostly cold-rolled metal-strip as the substrate is handled in coils up to 40 tons unwind before and rolled up again after passing the processing plant which includes cleaning, annealing, hot-dip galvanizing / aluminizing and chemical treatment. In the liquid Zn, Zn-AI, AI-Zn and AI-Si bathes a combined action of corrosion and wear under high temperature and high stress onto the transfer components (rolls) accounts for major economic losses. Most critical here are the bearing systems of these rolls operating in the liquid system. Rolls in liquid system can not be avoided as they are needed to transfer the steel-strip into and out of the crucible. Since several years, ceramic roller bearings are tested here [1.2], however, in particular due to uncontrollable Slag-impurities within the hot bath [3], slide bearings are still expected to be of a higher potential [4]. The today's state of the art is the application of slide bearings based on Stellite\ulcorneragainst Stellite which is in general a 50-60 wt% Co-matrix with incorporated Cr- and W-carbides and other composites. Indeed Stellite is used as the bearing-material as of it's chemical properties (does not go into solution), the physical properties in particular with poor lubricating properties are not satisfying at all. To increase the Sliding behavior in the bearing system, about 0.15-0.2 wt% of lead has been added into the hot-bath in the past. Due to environmental regulations. this had to be reduced dramatically_ This together with the heavily increasing production rates expressed by increased velocity of the substrate-steel-band up to 200 m/min and increased tractate power up to 10 tons in modern plants. leads to life times of the bearings of a few up to several days only. To improve this situation. the Mechanical Alloying (MA) TeChnique [5.6.7.8] is used to prOduce advanced Stellite-based bearing materials. A lubricating phase is introduced into Stellite-powder-material by MA, the composite-powder-particles are coated by High Energy Milling (HEM) in order to produce bearing-bushes of approximately 12 kg by Sintering, Liquid Phase Sintering (LPS) and Hot Isostatic Pressing (HIP). The chemical and physical behavior of samples as well as the bearing systems in the hot galvanizing / aluminizing plant are discussed. DependenCies like lubricant material and composite, LPS-binder and composite, particle shape and PM-route with respect to achievable density. (temperature--) shock-reSistibility and corrosive-wear behavior will be described. The materials are characterized by particle size analysis (laser diffraction), scanning electron microscopy and X-ray diffraction. corrosive-wear behavior is determined using a special cylinder-in-bush apparatus (CIBA) as well as field-test in real production condition. Part I of this work describes the initial testing phase where different sample materials are produced, characterized, consolidated and tested in the CIBA under a common AI-Zn-system. The results are discussed and the material-system for the large components to be produced for the field test in real production condition is decided. Outlook: Part II of this work will describe the field test in a hot-dip-galvanizing/aluminizing plant of the mechanically alloyed bearing bushes under aluminum-rich liquid metal. Alter testing, the bushes will be characterized and obtained results with respect to wear. expected lifetime, surface roughness and infiltration will be discussed. Part III of this project will describe a second initial testing phase where the won results of part 1+11 will be transferred to the AI-Si system. Part IV of this project will describe the field test in a hot-dip-aluminizing plant of the mechanically alloyed bearing bushes under aluminum liquid metal. After testing. the bushes will be characterized and obtained results with respect to wear. expected lifetime, surface roughness and infiltration will be discussed.

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Development of Rapid Analytical Method of Forbidden Medicines in Dietary Supplements Using LC-ESI-Tandem MS (LC-ESI-tandem MS를 이용한 기능성표방식품 중 부정유해물질 신속검사체계 개발)

  • Kim, Hee-Yun;Jang, Young-Mi;Joo, Hyun-Jin;Jung, Young-Hyun;Lee, Myoung-Sook;Park, Jong-Seok;Lee, Kwang-Ho;Lee, Hwa-Mi
    • Korean Journal of Food Science and Technology
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    • v.39 no.4
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    • pp.372-379
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    • 2007
  • A high-performance liquid chromatography-electrospray ionization (HPLC-ESI) tandem MS was developed for the rapid and simultaneous determination of forbidden medicines in dietary supplements. Thirteen medicinal components such as PDE-5 inhibitors and their analogues, and the newly identified dimethylsildenafil and xanthoanthrafil, were included in this study. After tentative standardization of molecular ions in both polarities using thirteen references on the mass spectrometer, with ESI-continuous infusion via the syringe pump method, the relative intensity of the ions present in the resulting spectra was quantitatively compared. From the results, the ion mode was selected depending on each reference's characteristics. A HPLC method coupled with the ESI mode was developed considering the matrix effect and interference depending on the type of sample. The validation test of the developed method was followed by carrying out precision, accuracy, recovery, sensitivity and linearity, etc. The method showed sufficiently high sensitivity, reproducibility, and specificity, and produced 4 times faster results when compared with the existing HPLC/UV method for the determination of forbidden compounds in dietary supplements.

The Exposure Status and Biomarkers of Bisphenol A in Shipyard Workers (일부 조선업 근로자들의 bisphenol A 노출실태와 생물학적 지표)

  • Kim, Cheong-Sik;Park, Jun-Ho;Cha, Bong-Suk;Park, Jong-Ku;Kim, Heon;Chang, Soung-Hoon;Koh, Sang-Baek
    • Journal of Preventive Medicine and Public Health
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    • v.36 no.2
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    • pp.93-100
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    • 2003
  • Objectives : Because shipyard workers are involved with various manufacturing process, they are exposed to many kinds of hazardous materials. Welders especially, are exposed to bisphenol-A (BPA) during the welding and flame cutting of coated steel, This study was conducted to assess the exposure status of the endocrine disrupter based on the job-exposure matrix. The effects of the genetic polymorphism of xenobiotic enzyme metabolisms involved in the metabolism of BPA on the levels of urinary metabolite were investigated. Methods : The study population was recruited from a shipyard company in the f province. A total of 84 shipbuilding workers 47 and 37 in the exposed and control groups, respectively, were recruited for this study. The questionnaire variables included, age, sex, use of personal protective equipment, smoking, drinking and work duration. The urinary metabolite was collected in the afternoon and correction made for the urinary creatinine concentration. The of the CYP1A1, CYP2E1 and UGT1A6 genotypes were investigated using polymerase chain reaction-restriction fragment length polymorphism (PCR-RFLP) methods with the DNA extracted from venous blood. Results : The urinary BPA level in the welders group was significantly higher than in the control group (p<0.05). The urinary BPA concentration with the wild type UGT1A6 was higher than the other UGT1A6 genotypes, but with no statistical significant. From themultiple regression analysis of the urinary BPA, the regression coefficient for job grade was statistically significant (p<0.05). Conclusions : The grade of exposure to BPA affected the urinary BPA concentration was statistically significant. However, the genetic polymorphisms of xenobiotics enzyme metabolism were not statistically significant. Further investigation of the genetic polymorphisms with a larger sample size is needed.

Electrical properties of metal-oxide-semiconductor structures containing Si nanocrystals fabricated by rapid thermal oxidation process (급속열처리산화법으로 형성시킨 $SiO_2$/나노결정 Si의 전기적 특성 연구)

  • Kim, Yong;Park, Kyung-Hwa;Jung, Tae-Hoon;Park, Hong-Jun;Lee, Jae-Yeol;Choi, Won-Chul;Kim, Eun-Kyu
    • Journal of the Korean Vacuum Society
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    • v.10 no.1
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    • pp.44-50
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    • 2001
  • Metal oxide semiconductor (MOS) structures containing nanocrystals are fabricated by using rapid thermal oxidations of amorphous silicon films. The amorphous films are deposited either by electron beam deposition method or by electron beam deposition assisted by Ar ion beam during deposition. Post oxidation of e-beam deposited film results in relatively small hysteresis of capacitance-voltage (C-V) and the flat band voltage shift, $\DeltaV_{FB}$ is less than 1V indicative of the formation of low density nanocrystals in $SiO_2$ near $SiO_2$/Si interface. By contrast, we observe very large hysteresis in C-V characteristics for oxidized ion-beam assisted e-beam deposited sample. The flat band voltage shift is larger than 22V and the hysteresis becomes even broader as increasing injection times of holes at accumulation condition and electrons at inversion condition. The result indicates the formation of slow traps in $SiO_2$ near $SiO_2$/Si interface which might be related to large density nanocrystals. Roughly estimated trap density is $1{\times}10^{13}cm^{-2}$. Such a large hysteresis may be explained in terms of the activation of adatom migration by Ar ion during deposition. The activated migration may increase nucleation rate of Si nuclei in amorphous Si matrix. During post oxidation process, nuclei grow into nanocrystals. Therefore, ion beam assistance during deposition may be very feasible for MOS structure containing nanocrystals with large density which is a basic building block for single electron memory device.

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