Analysis of semiconducting materials by high-resolution radiofrequency glow discharge mass spectrometry

The analytical capabilities of a high-resolution mass spectrometer in combination with a 13.56 MHz glow discharge ion source for the analysis of semiconducting materials (silicon carbide and gallium arsenide) were studied. It was shown that single positively charged ions of sample material have about 10 eV higher average energy than the ions of the discharge and residual gas. Therefore effective energy separation of the ions of analyte from the ions of the discharge and residual gas was achieved by adjusting the ion transfer optics (breadth and position of energy slit), which improves the analytical capabilities of the developed method.Some analytical applications are presented to illustrate the performance of r.f. GDMS for the bulk analysis of semiconducting materials. The results of the trace element analysis of gallium arsenide and silicon carbide samples are compared with data of independent methods (LIMS, ICP-AES, SIMS).Dedicated to Professor Dr. rer. nat. Dr. h.c. Hubertus Nickel on the occasion of his 65th birthdayOn leave from the Institute of Inorganic Chemistry, 630090 Novosibirsk, Russia     

Analytical Potentials and Features of Atomic Emission Analysis Using Electron-Impact Excitation of Atoms in Helium under Atmospheric Pressure

A device is described for the atomic emission analysis of vaporous samples using electron-impact excitation in helium under atmospheric pressure. The device consists of a cathode atomizer with a test sample applied onto it and the anode located at 1–3 mm from the cathode. The electrons emitted by the cathode upon heating are accelerated by applying a constant voltage to the electrodes. The mechanism for the formation of a non-self-sustained gas discharge between the cathode and anode is considered and the properties of the discharge are compared to those of the known discharges used in atomic emission spectrometry. The influence of atomization temperature and helium pressure on the analytical and background signals was studied. It is shown that, under certain conditions, the analytical signal increases with helium pressure. The relative detection limits attained for a number of elements are from tenths to dozens of nanogram per liter; this is two or three orders of magnitude lower than those in inductively coupled plasma atomic emission spectrometry and of the same order of magnitude as detection limits in inductively coupled plasma mass spectrometry.     

Mass spectrometric analysis of ceramic components for solid oxide fuel cells

For the determination of trace impurities in ceramic components of solid oxide fuel cells (SOFCs), some mass spectrometric methods have been applied such as spark source mass spectrometry (SSMS), laser ionization mass spectrometry (LIMS), laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and inductively coupled plasma mass spectrometry (ICP-MS). Due to a lack of suitable standard reference materials for quantifying of analytical results on La _x Sr _y MnO₃ cathode material a matrix-matched synthetic standard-high purity initial compounds doped with trace elements-was prepared in order to determine the relative sensitivity coefficients in SSMS and LA-ICP-MS. Radiofrequency glow discharge mass spectrometry (rf-GDMS) was developed for trace analysis and depth profiling of thick non-conducting layers. Surface analytical techniques, such as secondary ion mass spectrometry (SIMS) and sputtered neutral mass spectrometry (SNMS), were used to determine the element distribution on surfaces (homogeneity) and the surface contaminants of SOFC ceramic layers.Dedicated to Professor Dr. rer. nat. Hubertus Nickel on the occasion of his 65th birthday     

Trace and surface analysis of ceramic layers of solid oxide fuel cells by mass spectrometry

For the trace analysis of impurities in thick ceramic layers of a solid oxide fuel cell (SOFC) sensitive solid-state mass spectrometric methods, such as laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and radiofrequency glow discharge mass spectrometry (rf-GDMS) have been developed and used. In order to quantify the analytical results of LA-ICP-MS, the relative sensitivity coefficients of elements in a La(0.6)Sr(0.35)MnO(3) matrix have been determined using synthetic standards. Secondary ion mass spectrometry (SIMS) - as a surface analytical method - has been used to characterize the element distribution and diffusion profiles of matrix elements on the interface of a perovskite/Y-stabilized ZrO(2) layer. The application of different mass spectrometric methods for process control in the preparation of ceramic layers for the SOFC is described.     

Optimization of an rf-powered magnetron glow discharge for the trace analysis of glasses and ceramics

A radiofrequency (rf) powered planar magnetron glow discharge ion source has been designed and coupled to a double-focusing mass spectrometer. Superposition of the electrical field of the plasma in the cathode dark space and the magnetic field obtained from a ring-shaped magnet located directly behind the sample (cathode) form the electron traps and enhance the sputtering and ionization efficiency of the ion source. In order to establish optimum conditions for the trace analysis of nonconducting materials, mass spectrometric studies have been carried out on the ion signal intensities and energy distributions of analyte and discharge gas ions depending on pressure.     

Adjusted multichannel frequency diplexer

Conclusion Relatively simple and practical way to construct multichannel diplexer using dielectric resonators placed on substrate with multiple microstrip have been developed. Band-passes less than 160 MGz at level –25 dB have been obtained using multimode structure. Further work must be done to use connected resonators.     

Depth profiling analysis of thick Ni- and Co-doped oxide layers on Cr-based alloys of the interconnector of a solid oxide fuel cell using rf GDMS

A radiofrequency glow discharge ion source designed in our laboratory was coupled to a commercial double-focusing mass spectrometer in the original mode with an inductively coupled plasma ion source. This modification of rf GDMS extends the analytical capability of the mass spectrometer with ICP for the analysis of liquids to the direct analysis of insulating, semiconducting and conducting solids in the whole range of conductivity.The analytical procedure of the depth profiling analysis of the oxide coating of chromium-based alloys used as interconnectors in SOFC technology was discussed. The investigation of the depth profiles of Ni and Co in the thick oxide layers on the surface of Ni- and Co-doped alloys showed that the incorporation of these elements into the oxide during oxidation at 950°C is uniform.     

Determination of gold and palladium in rocks and ores by atomic absorption spectrometry using two-stage probe atomization

The efficiency of two-stage probe atomization for the determination of gold and palladium in geological samples by electrothermal atomic absorption spectrometry is studied. The effects of temperature–time program and the position of the probe in an atomizer on the fractionation of sample components and the magnitude of the analytical signal are studied. It is demonstrated that gold and palladium can be quantitatively determined by atomic absorption spectrometry in rocks and ores, using a two-stage probe atomization with the limits of detection for gold and palladium 0.01 and 0.04 g/t, respectively.