• Bulletin of the Korean Chemical Society
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• v.26 no.12
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• pp.1991-1995
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• 2005

Sensitivity factors of elements by a glow discharge mass spectrometry (GD-MS) were intensively investigated and compared with a laser ablation inductively coupled plasma-mass spectrometry (ICP-MS). In case of copper matrix, the sensitivity factor by GD-MS generally decreases with the increase of the mass number of element. The details are a little different between each data measured by Faraday and multiplier detectors. The factor by a multiplier detector drastically decreases with the mass increase in the region of low mass as in Faraday detector’s case, but slowly in the high mass region. On the contrast, the sensitivity factor of solution standard by a conventional ICP-MS slowly increases with the increase of elemental mass number even though there are some exceptions such as gold and also the sensitivity factor by a laser ablation ICP MS generally increases with mass number of element in the specimen of glass type. In case of steel matrix, any definite trends could not be shown in the relationship between the GD-MS’s sensitivity factor and elemental mass.

• Bulletin of the Korean Chemical Society
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• v.10 no.6
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• pp.524-529
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• 1989

A glow discharge mass spectrometric(GDMS) analytical method was developed for direct analysis of impurities in solids. Ions extracted from a glow discharge ion source with a sample as a cathode were analyzed by a quadrupole mass filter. Ion extractions were carried out through differentially-pumped orifices biased to positive and negative potentials. Operating parameters of the glow discharge source such as discharge current, orifice-to-cathode distance, energy analyzer setting and bias voltages have been optimized. The developed GDMS was applied to the analysis of KSS copper-base alloy standards certified by Korea Standards Research Institute(KSRI). In the analysis, the reproducibility and the detection limits were estimated to be about 2.5% RSD, and in the low ppm range, respectively.

• Journal of the Korean Vacuum Society
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• v.13 no.2
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• pp.79-85
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• 2004

Secondary ion mass spectrometry(SIMS) and glow discharge mass spectrometry(GDMS) were used to determine the impurity concentrations of hydrogen, carbon, and oxygen elements in the Cu and Ta films, and the results of SIMS and GDMS analysis were carefully considered. The Cu and Ta films were deposited on Si (100) substrates at zero substrate bias voltage and a substrate bias voltage of -50 V(Cu films) or -125 V(Ta films) using a non-mass separated ion beam deposition method. As a result of SIMS with Cs+ ion beam, in the case of the Cu and Ta films deposited without the substrate bias voltage, many strong peaks were observed, which is considered to be detected as a the cluster state such as CxHx, OxHx, CxOxHx. All the peaks of SIMS results could be interpreted by the combination of these dominant impurities. Moreover, it was confirmed that the quantitative results of GDMS analysis were accordant to the SIMS results.

• Analytical Science and Technology
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• v.10 no.5
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• pp.357-361
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• 1997

A Griemm type Glow Discharge cell is attached to a commercial quadrapole based ICP-MS and used for the analysis of surface analysis. By employing 2.0mm diameter, mode and proper experimental conditions, several layers of few ${\mu}m$ thickness are analysed within 30 minutes. Multi-layers of Cu-Ni, Fe-Ni are analyzed with the resolution of 10nm by GDMS. Proper experimental conditions make a flat bottom crater shape and good resolution for multi-layer depth profile study.

• Journal of the Korean Vacuum Society
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• v.14 no.1
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• pp.17-23
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• 2005

Glow discharge mass spectrometry(GDMS) was used to determine the impurity concentrations of the deposited Cu films and the 6N Cu target. Cu films were deposited on Si (100) substrates at zero substrate bias voltage and a substrate bias voltage of -50 V using a non-mass separated ion beam deposition method. Since do GDMS has a little difficulty to apply to thin films because of the accompanying non-conducting substrate, we have used an aluminum foil to cover the edge of the Cu film in order to make an electrical contact of the Cu film deposited on the non-conducting substrate. As a result, the Cu film deposited at the substrate bias voltage of -50 V showed lower impurity contents than the Cu film deposited without the substrate bias voltage although both the Cu films were contaminated during the deposition. It was found that the concentration change of each impurity in the Cu films by applying the negative substrate bias voltage is related to the difference in their ionization potentials. The purification effect by applying the negative substrate bias voltage might result from the following reasons: 1) Penning ionization and an ionization mechanism proposed in the present study, 2) difference in the kinetic energy of accelerated Cu+ ions toward the substrate with/without the negative substrate bias voltage.

• Analytical Science and Technology
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• v.22 no.2
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• pp.152-158
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• 2009

In this study, we made a new discharge source improving previous SPI source to ionize softly organic compounds. The new SPI source consists of two electrodes as a hollow mesh cathode of half cylindrical shape and a hollow anode. We optimized the geometrical parameter of the SPI source by investigating the I-V curves at the various distance between the cathode and the anode. As the results, we found stable conditions of the soft plasma on broad range of the current and the voltage. The new SPI source attached to quadrupole mass spectrometer (QMS), and we obtained the mass spectra of dichloromethane (DCM). The fragment patterns of DCM appeared similarly with the pattern of electron ionization (EI).

• Resources Recycling
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• v.21 no.2
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• pp.59-65
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• 2012

The refining effect of tantalum by electron beam melting(EBM) process for recycling tantalum scraps was investigated in the study. The purity of the tantalum metals refined by EBM was evaluated using glow discharge mass spectrometry (GDMS). From the result of GDMS, most impurities in the tantalum metals were removed by EBM down to a few mass ppm levels. The purity of the refined tantalum scraps was improved up to 5N (99.9991%) from 4 N (99.996%) of the initial tantalum scraps. The amount of metallic impurities in the tantalum was decreased from 30 ppm to 8 ppm. In addition, the gaseous impurities in the tantalum were decreased from 470 ppm to 50 ppm. Therefore a possibility of refining method for recycling tantalum scraps by EBM process was confirmed in this study.

• Analytical Science and Technology
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• v.5 no.2
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• pp.169-176
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• 1992

Analytical detection limits and Relative Ion Yield (RIY) by a jet type ion source glow discharge mass spectrometer(GD/MS) have been measured. With a jet type ion source, the sample loss rate for a Cu sample is 0.23 mg/min with 0.1 L/min gas flow rate and 0.11 mg/min with no gas flow rate. However, the ion intensity of Cu does not change significantly with thee variation of the gas flow rate. The RIY values obtained from the calibration curves of the six copper based standards were between 0.57 of Fe and 3.5 of Cr. The detection limits of most elements were in the range of 0.9 and 2.0 ppm when the glow discharge was operated at 4 mA, 1000V.

• Bulletin of the Korean Chemical Society
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• v.13 no.6
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• pp.620-624
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• 1992

The analytical performance of glow discharge mass spectrometer (GD-MS), using a flat type ion source is discussed. The efficiency of ion extraction was maximized at the distance between anode and cathode of 6 mm. At the operation condition of 4 mA, -1000 volt, and 1 mbar for the source, the optimum voltages for sampler and skimmer were40 volt and -280 volt, respectively. The intensities of Cu, Zn, and Mn were increased as a function of square root of current approximately. Korea standard reference materials (KSRM) were tested for an application study. The detection limits of most elements were obtained in the range of several ppm at the optimized operating condition. The peaks of aluminum and chromium were interfered by those of residual gases. The depth profile of nickel coated copper specimens (3, 5, 10 ${\mu}m$ thickness) were obtained by plotting time versus intensities of Ni and Cr after checking the thickness of nickel coated using a scanning electron microscope (SEM). At this moment, the sputtering rate of 0.2 ${\mu}m/min$ at the optimum operating condition was determined from the slope of the plot of time to the coating thickness. The roughness spectra of specimen's crater after 16 min, discharge were obtained using a Talysuf5m-120 roughness tester as well.

• Resources Recycling
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• v.20 no.5
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• pp.40-45
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• 2011

We carried out to investigate the refining effect of molybdenum by Ar-H$_2$ vacuum arc melting(VAM) process for recycling Mo scrap. The purity of the Mo metals refined by VAM was evaluated using glow discharge mass spectromety(GDMS). From the result of GDMS, most impurities in the Mo metals except for W were removed by Ar-H$_2$ VAM down to a few mass ppm levels. The purity of the refined molybdenum scrap was improved up to 4N5(99.995%) from 3N(99.95%) of the initial Mo scrap. The amount of gaseous impurities such as C, N, and O in Mo scrap were decreased from 1290 ppm to 132 ppm. As a result, it is considered that a possibility of refining and cost-effective method for recycling Mo scrap by Ar-H$_2$ vacuum arc melting process was confirmed in this study.