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HIPIMS Arc-Free Reactive Deposition of Non-conductive Films Using the Applied Material ENDURA 200 mm Cluster Tool

  • Chistyakov, Roman
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.96-97
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    • 2012
  • In nitride and oxide film deposition, sputtered metals react with nitrogen or oxygen gas in a vacuum chamber to form metal nitride or oxide films on a substrate. The physical properties of sputtered films (metals, oxides, and nitrides) are strongly influenced by magnetron plasma density during the deposition process. Typical target power densities on the magnetron during the deposition process are ~ (5-30) W/cm2, which gives a relatively low plasma density. The main challenge in reactive sputtering is the ability to generate a stable, arc free discharge at high plasma densities. Arcs occur due to formation of an insulating layer on the target surface caused by the re-deposition effect. One current method of generating an arc free discharge is to use the commercially available Pinnacle Plus+ Pulsed DC plasma generator manufactured by Advanced Energy Inc. This plasma generator uses a positive voltage pulse between negative pulses to attract electrons and discharge the target surface, thus preventing arc formation. However, this method can only generate low density plasma and therefore cannot allow full control of film properties. Also, after long runs ~ (1-3) hours, depends on duty cycle the stability of the reactive process is reduced due to increased probability of arc formation. Between 1995 and 1999, a new way of magnetron sputtering called HIPIMS (highly ionized pulse impulse magnetron sputtering) was developed. The main idea of this approach is to apply short ${\sim}(50-100){\mu}s$ high power pulses with a target power densities during the pulse between ~ (1-3) kW/cm2. These high power pulses generate high-density magnetron plasma that can significantly improve and control film properties. From the beginning, HIPIMS method has been applied to reactive sputtering processes for deposition of conductive and nonconductive films. However, commercially available HIPIMS plasma generators have not been able to create a stable, arc-free discharge in most reactive magnetron sputtering processes. HIPIMS plasma generators have been successfully used in reactive sputtering of nitrides for hard coating applications and for Al2O3 films. But until now there has been no HIPIMS data presented on reactive sputtering in cluster tools for semiconductors and MEMs applications. In this presentation, a new method of generating an arc free discharge for reactive HIPIMS using the new Cyprium plasma generator from Zpulser LLC will be introduced. Data (or evidence) will be presented showing that arc formation in reactive HIPIMS can be controlled without applying a positive voltage pulse between high power pulses. Arc-free reactive HIPIMS processes for sputtering AlN, TiO2, TiN and Si3N4 on the Applied Materials ENDURA 200 mm cluster tool will be presented. A direct comparison of the properties of films sputtered with the Advanced Energy Pinnacle Plus + plasma generator and the Zpulser Cyprium plasma generator will be presented.

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Optical Diagnostics of Nanopowder Processed in Liquid Plasmas

  • Bratescu, M.A.;Saito, N.;Takai, O.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.02a
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    • pp.17-18
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    • 2011
  • Plasma in liquid phase has attracted great attention in the last few years by the wide domain of applications in material processing, decomposition of organic and inorganic chemical compounds and sterilization of water. The plasma in liquid is characterized by three main regions which interact each - other during the plasma operation: the liquid phase, which supply the plasma gas phase with various chemical compounds and ions, the plasma in the gas phase at atmospheric pressure and the interface between these two regions. The most complex region, but extremely interesting from the fundamental, chemical and physical processes which occur here, is the boundary between the liquid phase and the plasma gas phase. In our laboratory, plasma in liquid which behaves as a glow discharge type, is generated by using a bipolar pulsed power supply, with variable pulse width, in the range of 0.5~10 ${\mu}s$ and 10 to 30 kHz repetition rate. Plasma in water and other different solutions was characterized by electrical and optical measurements. Strong emissions of OH and H radicals dominate the optical spectra. Generally water with 500 ${\mu}S/cm$ conductivity has a breakdown voltage around 2 kV, depending on the pulse width and the repetition rate of the power supply. The characteristics of the plasma initiated in ultrapure water between pairs of different materials used for electrodes (W and Ta) were investigated by the time-resolved optical emission and the broad-band absorption spectroscopy. The deexcitation processes of the reactive species formed in the water plasma depend on the electrode material, but have been independent on the polarity of the applied voltage pulses. Recently, Coherent anti-Stokes Raman Spectroscopy method was employed to investigate the chemistry in the liquid phase and at the interface between the gas and the liquid phases of the solution plasma system. The use of the solution plasma allows rapid fabrication of the metal nanoparticles without being necessary the addition of different reducing agents, because plasma in the liquid phase provides a reaction field with a highly excited energy radicals. We successfully synthesized gold nanoparticles using a glow discharge in aqueous solution. Nanoparticles with an average size of less than 10 nm were obtained using chlorauric acid solutions as the metal source. Carbon/Pt hybrid nanostructures have been obtained by treating carbon balls, synthesized in a CVD chamber, with hexachloro- platinum acid in a solution plasma system. The solution plasma was successfully used to remove the template remained after the mesoporous silica synthesis. Surface functionalization of the carbon structures and the silica surface with different chemical groups and nanoparticles, was also performed by processing these materials in the liquid plasma.

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Molecular Characteristics of Extended-Spectrum β-Lactamase Genes in Clinical Isolates of Escherichia coli and Klebsiella pneumoniae (임상검체에서 분리된 Escherichia coli와 Klebsiella pneumoniae의 Extended-Spectrum β-Lactamase 유전자형 및 분자유전학적 특성)

  • Chung, Kyung-Suk
    • Korean Journal of Clinical Laboratory Science
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    • v.38 no.1
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    • pp.26-33
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    • 2006
  • Recently, the rapid increase in extended-spectrum ${\beta}$-lactamase (ESBL) producing clinical isolates has become a serious problem. In this study, the epidemiologic features and molecular characteristics of ESBL among clinical isolates of Escherichia coli and Klebsiella pneumoniae, antibiotic susceptibility testing, genotype of the ESBL and patterns of chromosomal DNA from PFGE (pulsed field gel electrophoresis) were observed. A total of 53 ESBL-producing clinical isolates (30 of E. coli and 23 of Klebsiella pneumoniae) were collected from two university hospitals in the period of June to July in 2002 and 2003 respectively. The antibiotic resistance frequency of those 53 strains was tested by the disk agar diffusion method with the result that all the strains were resistant to cephalothin. To other antibiotics, the resistance rates of E. coli (30 isolates) were in order of ceftazidime (90.0%), cefotaxime and aztreonam (respectively 83.3%). Also, the resistance rates of K. pneumoniae (23 isolates) were in order of aztreonam (78.3%), ceftazidime (73.9%) and cefotaxime (65.3%). Also the sensitivity of ceftazidime-clavulanic acid were 100% in E. coli and 95.7% in K. pneumoniae. And the sensitivity of cefotaxime-clavulanic acid was 96.7% in E. coli and 91.3% in K. pneumoniae. The types of the ESBL genes were determined by using polymerase chain reaction (PCR). Among the 30 isolates of ESBL-producing E. coli, 6 (20.0%) have SHV only, 5 (16.7%) have TEM only and, 18 (60.0%) have both of TEM and SHV. Among the 23 isolates of ESBL-producing K. pneumoniae, 7 (30.4%) have SHV only, 2 (8.7%) have TEM only, and 14 (60.9%) have both of TEM and SHV. These results show that 52 strains, with only one exception, were confirmed as either TEM or SHV. The patterns of Xba I-digested chromosomal DNA of ESBL-producing E. coli and K. pneumoniae isolates were analyzed by PFGE. PFGE patterns of E. coli and K. pneumoniae were multiclonal, but many strains were grouped into a few types. Therefore, it seems that there were clonal outbreaks or possible horizontal spread. In conclusion, the TEM and SHV ${\beta}$-lactamase are most widely spread in E. coli and K. pneumoniae in Korea. As these types are usually carried by plasmids, the spread of these ${\beta}$-lactamase genes could compromise the future usefulness of third generation cephalosporins for the treatment of infections caused by E. coli and K. pneumoniae.

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Silver nanowires and nanodendrites synthesized by plasma discharge in solution for the catalytic oxygen reduction in alkaline media

  • Kim, Hoe-Geun;Song, Myeon-Gyu;Kim, Dong-U;Lee, Sang-Yul
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2018.06a
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    • pp.62-62
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    • 2018
  • Pt is still considered as one of the most active electrocatalysts for ORR in alkaline fuel cells. However, the high cost and scarcity of Pt hamper the widespread commercialization of fuel cells. As a strong candidate for the replacement of Pt catalyst, silver (Ag) has been extensively studied due to its high activity, abundance, and low cost. Ag is more stable than Pt in the pH range of 8~14 as the equilibrium potential of Ag/Ag+ being ${\approx}200mV$ higher than that of Pt/PtO. However, Ag is the overall catalytic activity of Ag for oxygen reduction reaction(ORR) is still not comparable to Pt catalyst since the surface Ag atoms are approximately 10 times less active than Pt atoms. Therefore, further enhancement in the ORR activity of Ag catalysts is necessary to be competitive with current cutting-edge Pt-based catalysts. We demonstrate the architectural design of Ag catalysts, synthesized using plasma discharge in liquid phase, for enhanced ORR kinetics in alkaline media. An attractive feature of this work is that the plasma status controlled via electric-field could form the Ag nanowires or dendrites without any chemical agents. The plasma reactor was made of a Teflon vessel with an inner diameter of 80 mm and a height of 80 mm, where a pair of tungsten(W) electrodes with a diameter of 2 mm was placed horizontally. The stock solutions were made by dissolving the 5-mM AgNO3 in DI water. For the synthesis of Agnanowires, the electricfield of 3.6kVcm-1 in a 200-ml AgNO3 aqueous solution was applied across the electrodes using a bipolar pulsed power supply(Kurita, Seisakusyo Co. Ltd). The repetition rate and pulse width were fixed at 30kHz and 2.0 us, respectively. The plasma discharge was carried out for a fixed reaction time of 60 min. In case of Ag nanodendrites, the electric field of 32kVcm-1 in a 200-ml AgNO3 aqueous solution was applied and other conditions were identical to the plasma discharge in water in terms of electrode configuration, repetition rate and discharge time. Using SEM and STEM, morphology of Ag nanowires and dendrites were investigated. With 3.6 kV/cm, Ag nanowire was obtained, while Ag dendrite was constructed with 32 kV/cm. The average diameter and legth of Ag nanowireses were 50 nm and 3.5 um, and thoes values of Ag dendrites were 40 nm and 3.0 um. As a results of XPS analysis, the surface defects in the Ag nanowires facilitated O2 incorporation into the surface region via the interaction between the oxygen and the electron cloud of the adjacent Ag atoms. The catalytic activity of Ag for oxygen reduction reaction(ORR) showed that the catalytic ORR activity of Ag nanowires are much better than Ag nanodendrites, and electron transfer number of Ag nanowires is similar to that of Pt (${\approx}4$).

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Effect of $CeO_2$ buffer layer thickness on superconducting properties of $YBa_2Cu_3O_{7-{\delta}}$ films grown on $Al_2O_3$ substrates ($CeO_2$ 완충층의 두께가 $Al_2O_3$ 기판 위에 성장된 $YBa_2Cu_3O_{7-{\delta}}$ 박막의 초전도 특성에 미치는 영향)

  • Lim, Hae-Ryong;Kim, In-Seon;Kim, Dong-Ho;Park, Yong-Ki;Park, Jong-Chul
    • Journal of Sensor Science and Technology
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    • v.8 no.2
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    • pp.195-201
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    • 1999
  • C-axis oriented $YBa_2Cu_3O_{7-{\delta}}$ (YBCO) thin films were grown on $Al_2O_3$ (alumina and R-plane sapphire) substrates by a pulsed laser deposition method. The crystallinity of the $CeO_2$ buffer layer on sapphire substrate exhibit a strong dependence on the deposition temperature, resulting in the growth of a-axis orientation at $800^{\circ}C$. The superconducting properties of YBCO thin films on $Al_2O_3$ substrates showed strong dependence on both thickness and crystallinity of the $CeO_2$ buffer layer. Critical temperature of YBCO film on alumina substrate was ${\sim}83\;K$. In the case of R-plane sapphire substrate,

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Effects of Pretreatments and Storage Conditions on Quality and Vase Life of Cut 'Red Sandra' Rose (전처리와 저장조건이 절화장미 'Red Sandra'의 품질과 수명에 미치는 영향)

  • Bang, Chang-Seok;Song, Cheon-Young;Lee, Jong-Suk;Huh, Kun-Yang;Song, Jeong-Seob
    • Horticultural Science & Technology
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    • v.17 no.6
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    • pp.762-764
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    • 1999
  • This experiment was conducted to investigate the effect of pretreatments and storage conditions on quality and vase life of cut 'Red Sandra' rose (Rosa hybrida L.). 'Red Sandra' rose flowers were harvested and pulsed with distilled water, 0.2% RVB or 200ppm aluminum sulfate+3% sucrose+50ppm $AgNO_3$+0.1mM ethionine for 22 hours and then stored in wet or dry condition for 12, 24, 48 hours at low or room temperature. Pulsing with aluminum sulfate+sucrose+$AgNO_3$+ethionine delayed bent-neck, increased solution absorption and flower diameter, and prolonged vase life rather than pulsing with distilled water or RVB. Storage in wet condition or low temperature also delayed bent-neck, increased solution absorption and flower diameter, and prolonged vase life compared with storage in dry or room temperature condition. As the storage hours prolonged, solution absorption, flower diameter, and vase life were decreased especially pulsing with distilled water. Pulsing with aluminum sulfate+sucrose+$AgNO_3$+ethionine prolonged vase life compared to pulsing with distilled water or RVB regardless of storage conditions and shipping hours.

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Effects of Electrical Stimulation on the Mast Cell of Skin in Rats (전기자극이 흰쥐의 피부 비만세포에 미치는 영향)

  • Lee Jae-Hyoung;Jekal Seung-Joo;Park Seung-Teack
    • The Journal of Korean Physical Therapy
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    • v.11 no.3
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    • pp.81-87
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    • 1999
  • The purpose of this study was to determine the effect of electrical stimulation on the number of MCs and percent of degranulated MCs in rat skin. Twelve male Sprague-Dawley rats were divided into two group; electrical stimulation group (n=6) and control group (n=6). Each animals hair on the back was removed. The electrical stimulation group received an positive rectangular pulsed electrical stimulation, while the control group was given the same treatment without electricity. The biopsy specimens were fixed in formalin, embedded in paraffin and stained with toluidine blue-nuclear fast red and alcian blue-safranin O. respectively. The MCs were counted using a light microscope and computerized image analysis system and calculated as the density and the percent. A t-test showed a significantly higher density of MCs in the electrical stimulated rats than control rats(p<0.05), and the percent of degranulated MCs in the electrical stimulated rats was higher than in the control rats (p<0.05) in toluidine blue stained sections. The density of MCs was significantly higher in the electrical stimulated rats than the control rats in alcian blue-safranin O Stained sections (P<0.01). An analysis of variance showed that the densities of CTMCs was significantly lower than the densities of MMCs and mixed MCs in electrical stimulated rat in alcian blue-safranin O Stained sections (p<0.05). These results suggest that the electrical stimulation may have potential for increasing the number of MCs and lead to degranulate the MCs in rat skin.

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Use of the Color Doppler Ultrasonography for the Evaluation of the Hemodynamic Changes of the Cranial Pancreaticoduodenal Arterial Flow in Experimentally Induced Acute Pancreatitis Dogs (실험적으로 유발된 급성 췌장염 견에서 컬러도플러 초음파를 이용한 전방 십이지장 동맥 혈류의 혈역학적 변화에 대한 평가)

  • Lee, Hae-Woon;Um, Ki-Dong;Sung, Yoon-Sang;Lee, Jung-Min;Lee, Jong-Won;Lee, Geun-Woo;Kim, Myung-Chul;Kim, Doo;Park, Sun-Il
    • Journal of Veterinary Clinics
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    • v.20 no.3
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    • pp.334-340
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    • 2003
  • For the study of the hemodynamic changes of the cranial pancreaticoduodenal arterial flow(cPDAF) in the dog with acute pancreatitis, acute pancreatitis was experimentally induced in 10 dogs by the injection of oleic acid into the accessory pancreatic duct. The parameters of cPDAF were measured by transcutaneous pulsed-wave Doppler ultrasonography. The hemodynamic changes included resistive indexe(RI), pulsatility index(PI) and maximum velocity (Vmax). Ultrasonographic scans were performed before the induction of pancreatitis and once daily for five days after the induction. The RI, PI and Vmax were increased with day as follows; the RI prior to induction was 0.625$\pm$0.096 (mean$\pm$SD), the PI was 1.117$\pm$0.289 and the Vmax was 0.349$\pm$0.094 m/s. After five days, the RI was 0.727$\pm$0.051 (p<0.0l), the PI was 1.480$\pm$0.284 (p<0.0l) and the Vmax was 0.585:$\pm$0.114 m/s (p<0.00l). These results show that there is some relation between the increase of the RI, PI and Vmax of cPDAF and the progress of acute pancreatitis in dogs. Therefore, the measurements of the hemodynamic changes of cPDAF may be a valuable technique for the evaluation of acute pancreatitis in dogs.

플라즈마 표면 처리를 이용한 ZnO 습식성장 패터닝 기술 연구

  • Lee, Jeong-Hwan;Park, Jae-Seong;Park, Seong-Eun;Lee, Dong-Ik;Hwang, Do-Yeon;Kim, Seong-Jin;Sin, Han-Jae;Seo, Chang-Taek
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.330-332
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    • 2013
  • 소 분위기에서 플라즈마 표면 처리의 경우 기판 표면에 존재하는 수소와 탄소 유기물들이 산소와 반응하여 $H_2O$$CO_2$ 등으로 제거되며 표면에 오존 결합을 유도하여 표면 에너지를 증가시키는 것으로 알려져 있다. ZnO 나노구조물을 성장시키는 방법으로는 MOCVD (Metal-Organic Chemical Vapor Deposited), PLD (Pulsed Laser Deposition), VLS (Vapor-Liquid-Solid), Sputtering, 습식화학합성법(Wet Chemical Method) 방법 등이 있다. 그중에서도 습식화학합성법은 쉽게 구성요소를 제어할 수 있고, 저비용 공정과 낮은 온도에서 성장 가능하며 플렉서블 소자에도 적용이 가능하다. 그러므로 본 연구에서는 플라즈마 표면처리에 따라 표면에너지를 변화하여 습식화학합성법으로 성장시킨 ZnO nanorods의 밀도를 제어하고 photolithography 공정 없이 패터닝 가능성을 유 무를 판단하는 연구를 진행하였다. 기판은 Si wafer (100)를 사용하였으며 세척 후 표면에너지 증가를 위한 플라즈마 표면처리를 실시하였다. 분위기 가스는 Ar/$O_2$를 사용하였으며 입력전압 400 W에서 0, 5, 10, 15, 60초 동안 각각 실시하였다. ZnO nanorods의 seed layer를 도포하기 위하여 Zinc acetate dehydrate [Zn $(CH_3COO)_2{\cdot}2H_2O$, 0.03 M]를 ethanol 50 ml에 용해시킨 후 스핀코팅기를 이용하여 850 RPM, 15초로 5회 실시하였으며 $80^{\circ}C$에서 5분간 건조하였다. ZnO rods의 성장은 Zinc nitrate hexahydrate [$Zn(NO_3)_2{\cdot}6H_2O$, 0.025M], HMT [$C6H_{12}N_4$, 0.025M]를 deionized water 250 ml에 용해시켜 hotplate에 올리고 $300^{\circ}C$에서 녹인 후 $200^{\circ}C$에서 3시간 성장시켰다. ZnO nanorods의 성장 공정은(Fig. 1)과 같다. 먼저 플라즈마 처리한 시편의 표면에너지 측정을 위해 접촉각 측정 장치[KRUSS, DSA100]를 이용하였다. 그 결과 0, 5, 10, 15, 60 초로 플라즈마 표면 처리했던 시편이 각각 Fig. l, 2와 같이 $79^{\circ}$, $43^{\circ}$, $11^{\circ}$, $6^{\circ}$, $7.8^{\circ}$로 측정되었으며 이것을 각각 습식화학합성법으로 ZnO nanorods를 성장 시켰을 때 Fig. 3과 같이 밀도 차이를 확인할 수 있었다. 이러한 결과를 바탕으로 기판의 표면에너지를 제어하여 Fig. 4와 같이 나타나며 photolithography 공정없이 ZnO nanorods를 패터닝을 할 수 있었다. 본 연구에서는 플라즈마 표면 처리를 통하여 표면에너지의 변화를 제어함으로써 ZnO nanorods 성장의 밀도 차이를 나타냈었다. 이러한 저비용, 저온 공정으로 $O_2$, CO, $H_2$, $H_2O$와 같은 다양한 화학종에 반응하는 ZnO를 이용한 플렉시블 화학센서에 응용 및 사용될 수 있고, 플렉시블 디스플레이 및 3D 디스플레이 소자에 활용 가능하다.

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Prevalence and Genetic Characteristics of Meatborne Listeria monocytogenes Isolates from Livestock Farms in Korea

  • Oh, Hyemin;Kim, Sejeong;Lee, Soomin;Lee, Heeyoung;Ha, Jimyeong;Lee, Jeeyeon;Choi, Yukyung;Choi, Kyoung-Hee;Yoon, Yohan
    • Food Science of Animal Resources
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    • v.36 no.6
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    • pp.779-786
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    • 2016
  • This study aimed to evaluate the prevalence of Listeria monocytogenes on livestock farms in Korea and determine their serotypes and genetic correlations. Twenty-five livestock farms in Korea (central: 15, south west: 7, south east: 3) were visited 2-3 times, and 2,018 samples (feces: 677, soil: 680, silage: 647, sludge: 14) were collected. Samples were enriched in LEB (Listeria enrichment broth) and Fraser broth media, and then plated on Palcam agar. The isolates were identified by PCR and 16S rRNA gene sequencing. Then, the sero-types, presence of virulence genes (actA, inlA, inlB, plcB, and hlyA), and antibiotic resistance were determined. Genetic correlations among the isolates were evaluated by analyzing the restriction digest pattern with AscI. Of the 2,018 samples, only 3 (0.15%) soil samples (FI-1-FI-3) from 1 farm in the south east region were positive for L. monocytogenes. Based on biochemical tests and multiplex PCR, the serotype of the isolates were 4ab (FI-1 and FI-3) and 3a (FI-2), which are not common in foodborne L. monocytogenes. The 3a sero-type isolate was positive for all tested virulence genes, whereas the 4ab serotype isolates were only positive for hlyA, actA, and inlA. The isolates were resistant to all 12 tested antibiotics, especially FI-3. The genetic correlations among the isolates were 100% for those of the same serotype and 26.3% for those of different serotypes. These results indicate that the prevalence of L. monocytogenes on livestock farms in Korea is low; however, the isolates are pathogenic and antibiotic resistant.