• Title/Summary/Keyword: 사중극자 질량 분석기

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플라즈마 공정 모니터링용 사중극자 질량 분석기의 필라멘트 파손분석

  • Ha, Seong-Yong;Kim, Dong-Hun;Ju, Jeong-Hun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2015.08a
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    • pp.93.2-93.2
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    • 2015
  • 플라즈마를 포함한 반응성 가스 공정 분석용 사중극자 질량분석기의 필라멘트의 파손양상을 조사하였다. 또한 유전체 증착층이 이온원 성능에 미치는 영향을 분석하기 위하여 이온원의 일반적인 가동 전압 조건에서 Poisson방정식을 이용하여 전위를 수치 해석으로 구하였다. 사용중 파손된 필라멘트의 파단면을 주사전자현미경으로 관찰결과, 수직으로 절단되는 양상과 직경이 점차 작아지면서 erosion되는 두가지 양상을 보였다. 또한 파단면은 표면균열과 패시팅(faceting) 현상을 보였다. 필라멘트 사용시 가장 큰 문제는 패시팅(faceting)이다. 대부분의 결정에서는 다른 결정면보다 에너지 준위가 낮은 결정면이 존재한다. W 원자는 고온에서 확산 또는 증발하여 표면에서 다시 응축할 때 표면 에너지를 최소화하기 위한 독특한 평형 형상이 만들어 지는데 이것이 패시팅의 구동력이다. 이때 국부적으로 단면적이 감소하는 곳이 생기는데, 이 지점이 집중적으로 가열되고 증발이 가속화하여 파손된다. 파단면을 EDS 분석결과, 산화물을 포함한 F, Fe 및 C이 검출되었다. 이 F과 C는 공정중 사용된 CF4의 분해에 의한 것으로 생각되며, 파손된 필라멘트를 Ar 유도결합 플라즈마로 처리한 결과 이 F, Fe 및 C의 양이 감소하였다.

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QMS를 이용한 플라즈마 공정 진단

  • Ju, Jeong-Hun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.92-92
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    • 2016
  • 전기방전의 기본적인 특성을 가지고 있는 플라즈마를 이용하여 재료를 가공하는 증착, 식각, 표면처리 공정에 있어서 플라즈마 내의 전자 충돌 반응에 의한 이온, 라디칼의 생성과 재료 표면의 반응을 분석하는 도구로써 분압 측정은 일반적인 화학 조성 분석에 기원한 오랜 역사를 가지고 있다. 1 amu 정도의 분해능을 가지고 있고 크기가 30 cm 정도에 불과한 사중극자 질량 분석기는 적절한 질량 스캔 시간과 넓은 이온 전류 측정 범위를 가지므로 소형 차등 배기 시스템과 조합하면 1 mTorr 영역의 스퍼터링 시스템에서 1 Torr 영역의 PECVD/PEALD 시스템 진단에도 쉽게 적용이 가능하다. Inficon사의 CPM-300과 Pfeiffer사의 Prisma80을 이용한 플라즈마 식각 공정 분석 결과를 보면 동위원소까지 분석이 가능하다. 또한 전자충돌 이온화 에너지를 조절하여 m/q(질량전하비율)가 중첩되는 경우의 해석도 가능하다. 다중 오리피스를 갖는 compact design의 밸브 블록을 이용한 설계에서는 line-of-sight 입사가 불가능하여 이온 전류를 분석할 수 없다는 단점이 있으나 표준 가스를 이용한 정량화 등의 큰 장점들이 있다. 최근 이루어진 연구의 내용으로는 유도 결합 플라즈마 장치에서 전도성 메쉬를 이용한 라디칼 거동 관찰을 위해서 두 대의 CPM-300을 메쉬 전 후에 설치하여 라디칼의 양 변화를 전류 프로브와 같이 사용하여 조사하였다.

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Inductively Coupled $Ar/Cl_2$ Plasma Analysis with Quadrupole Mass Spectrometer (QMS) (사중극자 질량분석기(QMS)를 이용한 $Ar/Cl_2$ 유도결합 플라즈마 분석)

  • Kim, Jong-Gyu;Kim, Gwan-Ha;Lee, Cheol-In;Kim, Chang-Il
    • Proceedings of the KIEE Conference
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    • 2005.11a
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    • pp.41-43
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    • 2005
  • $Cl_2$ 플라즈마에 있어서 Ar 가스의 첨가에 의한 효과를 보기 위해 Ar 첨가 비율 rf 전력, 반응로 압력을 변화시켜가며 그 에너지와 질량을 분석하였다. Ar 첨가 비율에 따른 각 입자들의 질량 분석을 통해서, Ar의 비율이 80% 일 때 물리적, 화학적 반응이 최대가 되는 것을 확인하였다. 또한 Ar 첨가 비율에 따른 각 이온들의 에너지 분석을 통해, Ar 가스의 첨가에 의해 $Cl^+$$Cl_2^+$ 이온들의 이온 선속은 증가하나 그 에너지가 감소하는 것을 확인하였다. 반응로 압력과 rf 전력의 제어를 통해 이온 전류밀도, 이온 에너지와 전자온도를 제어 할 수 있음을 확인하였고, Ar 첨가 비율을 변화시키면서 전자 밀도 분포 함수의 변화를 관찰하여 이를 통해 Ar 비율에 따른 이온화 비율과 전자 온도, 밀도 등의 관계를 확인하였다.

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Development of a Prototype Mass Spectrometer (질량 분석기의 원형 모델 개발)

  • Jingeun Rhee;Nam-Seok Lee;Sung Won Kang;Seontae Kim;Kyu-Ha Jang;Yu Yi;Ik-Seon Hong;Cheong Rim Choi;Kyoung Wook Min;Jongil Jung
    • Journal of Space Technology and Applications
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    • v.3 no.1
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    • pp.86-99
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    • 2023
  • The mass spectrometer, being an essential scientific instrument for uncovering the origin of the solar system and life, has been used since the early 1970s on board spacecraft to obtain information of neutral and ionized elements in the atmosphere and surface of the moon, planets, asteroids, and comets. According to the 4th Basic Plan for the Promotion of Space Development (2023-2027), Korea plans to conduct lunar landing in 2032 and Mars landing in 2045 as the core goals of the plan and focuses on developing the technologies required for unmanned robotic exploration missions. In this regard, it is crucial to develop the technology of a mass spectrometer, which is the most fundamental payload for space exploration for maximized scientific achievements, however never tried before in any domestic space missions. We describe in this paper the principle of a domestically developed quadrupole mass spectrometer, its prototype model, and the test results of its performance. We conclude this paper with intended future improvements.

Diagnostics of Inductively Coupled $BCl_3/Ar$ Plasma Characteristics Using Quadrupole Mass Spectrometer (사중극자 질량 분석기를 이용한 $BCl_3/Ar$ 유도결합 플라즈마 특성 진단)

  • Kim, Gwan-Ha;Kim, Chang-Il
    • The Transactions of the Korean Institute of Electrical Engineers C
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    • v.55 no.4
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    • pp.204-208
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    • 2006
  • In this study, we investigated the ion energy distributions in a chlorine based inductively coupled plasma by quadrupole mass spectrometer with an electrostatic ion energy analyzer. Ion energy distributions are presented for various plasma parameters such as $BCl_3/Ar$ gas mixing ratio, RF power, and process pressure. As the $BCl_3/Ar$ gas mixing ratio and process pressure decreases, and RF power increases, the saddle-shaped structures is enhanced. The reason is that there are ionized energy difference between $BCl_3$ and Ar, change of plasma potential, alteration of mean free path. and variety of ion collision in the sheath.

Electrospray ionization tandem mass fragmentation pattern of camostat and its degradation product, 4-(4-guanidinobenzoyloxy)phenylacetic acid (Camostat 및 분해산물 4-(4-guanidinobenzoyloxy)phenylacetic acid의 전자분무 이온화 텐덤 질량 fragmentation 패턴)

  • Kwon, Soon-Ho;Shin, Hye-Jin;Park, Ji-Myeong;Lee, Kyoung-Ryul;Kim, Young-Jin;Lee, Sang-Hoo
    • Analytical Science and Technology
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    • v.24 no.2
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    • pp.78-84
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    • 2011
  • The fragmentation patterns of a serine protease inhibitor, camostat, and its degradation product, 4-(4-guanidinobenzoyloxy)phenylacetic acid (GBPA), were for the first time investigated by a triple quadrupole tandem mass spectrometry equipped with an electrospray source (ESI-MS/MS) in positive and/or negative ion mode under collision-induced dissociation (CID). The positive CID spectrum of camostat showed distinctly that the single bond (C-O) cleavage between carbonyl group and oxygen atom of the ester bonds of the compound favorably occurred and then the loss of N,N-dimethylcarbamoylmethyl group was more susceptible than that of guanidine moiety. In the positive ion CID spectrum of GBPA, the initial cleavage between the carbonyl group and oxygen atom of 4-guanidinobenzoyloxy group also occurred, yielding the most abundant fragment ion at m/z 145. On the other hand, the negative CID spectrum of GBPA characteristically showed the occurrence of the most abundant peak at m/z 226 resulting from the sequential neutral losses of $CO_2$ and HN=C=NH from the parent ion at m/z 312.

Development of a Noble Gas Isotope Dilution Mass Spectrometric System Combined with a Cryogenic Cold Trap (초저온 냉각 트랩을 결합한 비활성기체 동위원소 희석 질량분석 시스템의 제작)

  • HONG, BONGJAE;SHIN, DONGYOUB;PARK, KEYHONG;HAHM, DOSHIK
    • The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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    • v.27 no.3
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    • pp.144-157
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    • 2022
  • Noble gases, which are chemically inert and behave conservatively in marine environments, have been used as tracers of physical processes such as air-sea gas exchange, mixing of water masses, and distribution of glacial meltwater in the ocean. For precise measurements of Ne, Ar, and Kr, we developed a mass spectrometric system consisting of a quadrupole mass spectrometer (QMS), a high vacuum preparation line, an activated charcoal cryogenic trap (ACC), and a set of isotope standard gases. The high vacuum line consists of three sections: (1) a sample extraction section that extracts the dissolved gases in the sample and mixes them with the standard gases, (2) a gas preparation section that removes reactive gases using getters and separates the noble gases according to their evaporation points with the ACC, and (3) a gas analysis section that measures concentrations of each noble gas. The ACC attached to the gas preparation section markedly lowered the partial pressures of Ar and CO2 in the QMS, which resulted in a reduced uncertainty of Ne isotope analysis. The isotope standard gases were prepared by mixing 22Ne, 36Ar, and 86Kr. The amounts of each element in the mixed standard gases were determined by the reverse isotope dilution method with repeated measurements of the atmosphere. The analytical system achieved precisions for Ne, Ar, and Kr concentrations of 0.7%, 0.7%, and 0.4%, respectively. The accuracies confirmed by the analyses of air-equilibrated water were 0.5%, 1.0%, and 1.7% for Ne, Ar, and Kr, respectively.

Study of Simultaneous Analysis of Indicator Components of DTP(Digital Textile Printing) Textile Products Using HPLC-MS/MS - Focusing on Natural Dyes - (HPLC-MS/MS를 활용한 DTP(Digital Textile Printing) 제품의 지표성분 동시분석법 연구 - 천연염료를 중심으로 -)

  • Lee, Wonkyoung;Sung, Eunji;Moon, Joung Ryul;Kim, Miji;Kim, Jonghoon
    • Fashion & Textile Research Journal
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    • v.23 no.6
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    • pp.844-851
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    • 2021
  • Due to the increase in consumers' interest about well-being, interest in eco-friendly products has been increasing due to the harmful effects of various harmful substances contained in textile products and environmental issues. As a result, natural dyes of less potential risk than synthetic dyes and digital textile printing(DTP) textile products with less environmental pollution are drawing attention. However, due to the lack of evaluation criteria for DTP textile products with natural ink and the nature of many colors are stacked layer by layer for dying, the need for simultaneous analysis is emerging. To evaluate whether the natural dye is derived from natural ingredients, the biocarbon content is analyzed. However, in the case of ink made using natural dyes and DTP textile products using natural ink, it is difficult to analyze the biocarbon content due to the limitation of the presence of a small amount of dye contained therein. In this study, we were shown the possibility of natural derived verification by cross-checking the analytes of natural dyes (Persicaria tinctoria, an indigo dye; Dactylopius coccus, a light red; and Curcum longa L., i.e., turmeric) and natural ink with HPLC-MS/MS. The coefficient of determination was 0.999 or higher, the limit of quantification was 0.647-3.664 ㎍/L and a %RSD of each indicator material was less than 10. Then, the extraction amount of natural dyes for five patterned fabrics was analyzed.

Application of Dynamic Reaction Cell - Inductively Coupled Plasma Mass Spectrometry for the Determination of Calcium by Isotope Dilution Method (반응셀 유도결합플라스마 질량분석분석기를 이용한 칼슘 동위원소비율의 측정과 동위원소희석법의 적용)

  • Suh, Jungkee;Yim, Yonghyeon;Hwang, Euijin;Lee, Sanghak
    • Analytical Science and Technology
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    • v.15 no.5
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    • pp.417-426
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    • 2002
  • Inductively Coupled Plasma Dynamic Reaction Cell Quadrupole Mass Spectrometry (ICP-DRC-QMS) was characterized for the detection of the six naturally occurring calcium isotopes. The effect of the operating conditions of the DRC system was studied to get the best signal-to-noise ratio. This experiment shows that the potentially interfering ions such as $Ar^+$, ${CO_2}^+$, ${NO_2}^+$, $CNO^+$ at the calcium masses m/z 40, 42, 43, 44 and 48 were removed by flowing $NH_3$ gas at the rate of 0.7 mL/min $NH_3$ as reactive cell gas in the DRC with a RPq value (rejection parameter) of 0.6. The limits of detection for $^{40}Ca$, $^{42}Ca$, $^{43}Ca$, $^{44}Ca$, and $^{48}Ca$ were 1, 29, 169, 34, and 15 pg/mL, respectively. This method was applied to the determination of calcium in synthetic food digest samples (CCQM-P13) provided by LGC for international comparison. The isotope dilution method was used for the determination of calcium in the samples. The uncertainty evaluation was performed according to the ISO/GUM and EURACHEM guidelines. The determined mean concentration and its expanded uncertainty of calcium was ($66.4{\pm}1.2$) mg/kg. In order to assess our method, two reference samples, Riverine Water reference sample (NRCC SLRS-3) and Trace Elements in Water reference sample (NIST SRM 1643d), were analyzed.

A comparison study of 76Se, 77Se and 78Se isotope spikes in isotope dilution method for Se (셀레늄의 동위원소 희석분석법에서 첨가 스파이크 동위원소 76Se, 77Se 및 78Se들의 비교분석)

  • Kim, Leewon;Lee, Seoyoung;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.29 no.4
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    • pp.170-178
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    • 2016
  • Accuracy and precision of ID methods for different spike isotopes of 76Se, 77Se, and 78Se were compared for the analysis of Selenium using quadrupole ICP/MS equipped with Octopole reaction cell. From the analysis of Se inorganic standard solution, all of three spikes showed less than 1 % error and 1 % RSD for both short-term (a day) and long-term (several months) periods. They showed similar results with each other and 78Se showed was a bit better than 76Se and 77Se. However, different spikes showed different results when NIST SRM 1568a and SRM 2967 were analyzed because of the several interferences on the m/z measured and calculated. Interferences due to the generation of SeH from ORC was considered as well as As and Br in matrix. The results showed similar accuracy and precisions against SRM 1568a, which has a simple background matrix, for all three spikes and the recovery rate was about 80% with steadiness. The %RSD was a bit higher than inorganic standard (1.8 %, 8.6 %, and 6.3 % for 78Se, 76Se and 77Se, respectively) but low enough to conclude that this experiment is reliable. However, mussel tissue has a complex matrix showed inaccurate results in case of 78Se isotope spike (over 100 % RSD). 76Se and 77Se showd relatively good results of around 98.6 % and 104.2 % recovery rate. The errors were less than 5 % but the precision was a bit higher value of 15 % RSD. This clearly shows that Br interferences are so large that a simple mathematical calibration is not enough for a complex-matrixed sample. In conclusion, all three spikes show similar results when matrix is simple. However, 78Se should be avoided when large amount of Br exists in matrix. Either 76Se or 77Se would provide accurate results.