Determination of oxygen in gallium arsenide by3He activation analysis using substoichiometric precipitation

Distillation of fluoride as fluorosilicic acid and substoichiometric precipitation as lanthanum fluoride was studied for the determination of oxygen in gallium arsenide by³He activation analysis. Fluoride could be separated substoichiometrically with a good reproducibility by two distillations and successive precipitation with lanthanum. The oxygen concentration in gallium arsenide prepared by the horizontal Bridgman technique was 10 to 36 ppb and increased a little along the front, middle and tail portions in the crystal.     

Studies in the tetraarylborates : The preparation and reagent properties of sodium tetrakis(p-chlorophenyl)borate

Sodium tetrakis(p-chlorophenyl)borate was synthesized. It formed precipitates with K⁺, Rb⁺, Cs⁺, quarternary ammonium and protonated basic nitrogen compounds. The potassium salt was more soluble than potassium tetraphenylborate but flocculated more readily and filtered more easily. The salts formed with nitrogen compounds offer possibilities as derivatives suitable for qualitative analysis.     

Determination of nickel,gold and silver in gallium arsenide by radioactivation analysis based on the quantitative isotope dilution principle

A method of radioactivation analysis has been developed for the determination of Ni, Au and Ag impurities in gallium arsenide. The separation and substoichiometric extraction of these elements were studied and analytical procedures are suggested for their determination. All components are separated by suitable procedures and determined by substoichiometric methods. Ni is extracted as diethyldithiocarbamate into toluene, Au as a complex of rhodamine-B in chloroform, and Ag as dithizonate in carbon tetrachloride. The contents of Ni, Au and Ag in a gallium arsenide crystal with a carrier concentration of 1.8·10¹⁶/cm³ were 0.05–0.08, 0.006–0.008 and 0.002–0.005 ppm, respectively.     

Subtoichiometric determination of indium and tin by radioactivation analysis

A method of radioactivation analysis has been developed for the determination of indium and tin. It is based on substoichiometric extraction of indium diethyldithiocarbamate into carbon tetrachloride from a slightly ammoniacal solution in the presence of potassium cyanide. With this method, indium can be determined via^116m In (T=54 min) and tin via^113m In (T=104 min) which is formed by the reaction¹¹²Sn(n, ψ)¹¹³Sn. The method has been applied to the determination of indium in metallic zinc and of tin in tin-doped gallium arsenide, and 0.4 ppb of indium was analyzed in a zinc sample.     

A critical study on the determination of selenium in gallium arsenide by polarographic techniques

A simple voltammetric method is described for the determination of traces of selenium in gallium arsenide. Differential-pulse cathodic stripping voltammetry permits a direct determination of selenium without preliminary enrichment or separation processes. Selenium can be determined down to levels of 1–2 μg g^?1, with relative standard deviations of about 10%, in ? 100-mg samples of gallium arsenide. Results for gallium arsenide doped with 7–75 μg g^?1 selenium agree in most cases with those obtained by spectrophotometry based on 4-chloro-o-phenylenediamine.     

Determination of trace elements in gallium arsenide by graphite-furnace atomic absorption spectrometry after pretreatment in gas streams

Atomic absorption spectrometry (AAS) with a resistively-heated graphite furnace is used for the determination of chromium (0.3–1 atom/10⁶ atom) in chromium-doped gallium arsenide after pretreatment in a separate furnace in a stream of argon to remove arsenic, and of manganese and silver (0.03 and 0.04 atom/10⁶ atoms, respectively) by a similar procedure after pretreatment with argon and chlorine, the latter to remove both gallium and arsenic as volatile chlorides. Results for chromium were in agreement with those obtained by furnace AAS after dissolution and by spark-source mass spectrometry (SSMS) but AAS after dissolution is more precise. Results for manganese and silver obtained by both gas pretreatments were in good agreement, but were higher than those obtained for presparked material by SSMS, indicating that surface contamination of gallium arsenide was not completely removed by the etching methods used. The procedures established that the concentrations of bismuth, indium and lead in the gallium arsenide sample were below the limits of detection of 3 × 10^?3, 10 × 10^?3 and 1 × 10^?3 atom/10⁶ atoms, respectively. In all cases, calibration graphs were constructed from data obtained with aqueous solutions of appropriate salts.     

Spark Source Mass Spectrographic Analysis of Gallium Arsenide for Trace Oxygen and Carbon Using Liquid Helium Cryopumping

Abstract

A spark source mass spectrometric system has been developed for trace levels of oxygen and carbon in gallium arsenide using liquid helium cryopumping of the source chamber. Following bake-out, a collector positioned inside the source chamber is cooled using a controlled flow of liquid helium. Residual back-ground gases are more effectively removed than with liquid nitrogen and detectabilities of 0.02 ppma for oxygen and 0.05 ppma for carbon have been obtained. Routine analyses are carried out with a moderate consumption of liquid helium.     

Analysis of silicon carbonitride films by laser mass spectrometry

The possibilities of laser mass spectrometry in determining the main composition of silicon carbonitride films (SiC _x N _y ) deposited on a substrate made of germanium and gallium arsenide are considered. The conditions of laser sampling were selected and the instrument was adjusted to identify the major components of films synthesized by the plasma deposition. The instrument was calibrated by neat silicon compounds to obtain quantitative data on the concentrations of carbon, nitrogen, oxygen, and silicon. A calibration method was proposed, and the concentration of hydrogen in the layers of silicon carbonitride was estimated.     

The differential pulse polarographic determination of chromium in gallium arsenide

The method described for the determination of chromium in gallium arsenide is based on the catalytic current produced by nitrate in the electrolytic reduction of the chromium(VI)-diethylenetriaminepentaacetate complex. Matrix effects, primarily caused by gallium, are discussed in detail. The method is suitable for determinations of chromium at levels as low as about 1 μg g^?1 with about 50 mg of sample; the r.s.d. is better than 10%.     

Chemical Bonding and Electronic Localization in a GaI Amide

The electron density in a one‐coordinate [Ga^IN(SiMe₃)R] complex has been determined from ab initio calculations and multipole modeling of 90 K X‐ray data. The topologies of the Laplacian distribution and the ELI‐D match a situation having an sp³‐hybridized nitrogen with a tetrahedral arrangement of two single σ‐bonds (to carbon and silicon) and two lone pairs pointing towards gallium in a scissor‐grasping fashion. The analysis of the Laplacian distribution furthermore reveals a ligand‐induced charge concentration (LICC) in the outer core of gallium oriented directly towards the nitrogen atom, and thus in between the two lone pairs. These observations might suggest that the trigonal planar nitrogen geometry result from a dative Ga?N bond, in which the roles of the metal and the ligand have been reversed with respect to a “standard” metal–ligand interaction, that is, the metal is here electron‐donating. The ELI‐D reveals a diffuse and directional lone pair on gallium, suggesting that this complex could serve as a σ‐donor.     

Evaluation of departure from stoichiometry of gallium arsenide crystals

A method is described for determining arsenic in gallium arsenide. In order to avoid the conventional pre-reduction process, arsenic is directly titrated iodimetrically as As(V) in acidic solution. The determination is made with an automatic titrator and potentiometric detection of the equivalent point. Pure arsenic is used as a reference substance. Deviations from the stoichiometric composition of the order of 10^?3-10^?4% with a standard deviation of about 0.06% can be determined. The limits of chemical analysis for controlling the stoichiometry of the semiconductor are discussed.     

Neutral carrier potassium-selective electrodes with low resistances

Valinomycin-based electrodes for potassium are described which have resistances as low as 5 kΩ. Addition of a mixture of tetraphenylborate and a quaternary ammonium salt lowers the resistance to 1–3% of that without the additive. The electrode retains high selectivity for K⁺ over Na⁺ even in the presence of a large excess of the tetraphenylborate additive over the carrier.     

The epitaxial growth of gallium arsenide using triethylarsine

The thermal decomposition of triethylarsine (TEAs) has been studied. It decomposes at a lower temperature than arsine (AsH₃). The decomposition proceeds via a radical process at a temperature above 700°C. Epitaxial growth using TEAs has been investigated. A gallium arsenide (GaAs) layer with good morphology was obtained, but the layer was found to contain a considerable amount of carbon impurity originating from TEAs. The use of TEAs with 10% AsH₃ or with 20% ammonia (NH₃) apparently improves the quality of GaAs layer. A possible scheme for reducing carbon incorporation is discussed.     

The determination of carbon in aluminium by deuteron activation analysis

Carbon can be determined in aluminium by deuteron activation analysis via the ¹²C(d, n)¹³N reaction. ¹³N is separated from other activities by steam distillation. A carbon concentration of 0.25 μgg^-1 with a standard deviation of 0.05 μg g^-1 was obtained for aluminium of 99.5% purity.     

Atomabsorptionsspektralphotometrische bestimmung von zink in galliumarsenid und galliumaluminiumarsenid

The determination by atomic-absorption spectroscopy of zinc in gallium arsenide and gallium aluminium arsenide is described. In 5–20 mg of sample, 0·1–3 μg of zinc can be determined. The coefficient of variation is 4·5%. The influence of the matrix is described and discussed.     

Use of the ion microanalyzer for the characterization of bulk and epitaxial silicon and gallium arsenide

The ion microanalyzer permits a localized mass spectrometric analysis, i.e. the qualitative and quantitative analysis of the impurities contained in a small selected volume. This procedure makes possible the analysis of very thin epitaxial layers (for example silicon and gallium arsenide). As regards qualitative analysis, the apparatus is designed for the selection of ions. After the recording and analysis of the ion spectrum, a large number of the impurities present in the sample are determined qualitatively. Quantitative analysis can be performed with the equipment, but this requires the analysis of a homogeneous standard sample previously dosed by spark-source mass spectrometry. The quantitative analysis of bulk and epitaxial silicon and gallium arsenide is described and the limits of detection of the principal impurities are given. It is also shown how the possibility of localized analysis was exploited. A correlation was established between the existing impurities and the chemically revealed crystal imperfections. A comparative analysis of the distribution of the impurities in the epitaxial layers was also carried out. The periodic analysis of epitaxial layers makes it possible to follow the deterioration by contamination, if any, under the epitaxial conditions, and to improve the sample quality.     

Substoichiometric determination of trace impurities in high-purity materials by radioactivation analysis

The substoichiometric determination of some impurities in gallium arsenide and selenium supplied by OEC and IUPAC, respectively, as reference materials for radioactivation analysis is described.     

Properties of arsenic in molten potassium tetrachlorogallate at 300°C: Formation of gallium arsenide

Redox properties of As(III) species have been studied in molten KGaCl₄. The plot of equilibrium potential of As vs acidity is interpreted in terms of reaction AsCl⁴_? + 3 e = As + 4 Cl^?. X-Ray analysis of electrodeposits shows that only As is formed under potentiostatic conditions. Conversely, gallium arsenide is observed under galvanostatic conditions, for which the electrode potential becomes very negative.     

Radiofrequency spark source mass spectrometric analysis of oxygen in undoped silicon crystals and of carbon in undoped and carbon doped gallium arsenide crystals

Radiofrequency spark source mass spectrometry is a reliable and precise analytical method to measure the amount of oxygen in silicon grown by the Czochralski technique from SiO₂ crucibles in the common range from 2ppm(atomic) to 20ppm(atomic) and in silicon grown by the floating zone technique below 0.1ppm(atomic). The technique is also excellent for the measurement of the amount of carbon in semi-insulating gallium arsenide grown under low and high pressure N₂ ambient gas by the B₂O₃ encapsulated Czochralski technique from pyrolytic BN crucibles in the common range from 0.02ppm(atomic) to 0.4ppm(atomic). The results are in rather good agreement with concentrations measured by charged particle activation analysis and consistent with those obtained using other methods.     

Solubilization of arsenic from gallium arsenide using aqueous suspensions of organic halides

The solubilization of arsenic in solid gallium arsenide by aqueous solutions/suspensions of organic halides is described. Although arsenic is removed from gallium arsenide surfaces, excess quantities of gallium are not found in the solution. The abilities of the organic halide to solubilize arsenic decreases as follows: C₂H₅Br> CH₃I> 2-C₃H₇I> 1-C₃H₇I> 2-C₄H₉Br> CH₂?CHCH₂I> 2-C₃H₇Br? 1-C₄H₉Br. The results correlate with a combination of organic halide solubility, bond enthalpy and carbonium ion stability factors. Other parameters investigated using gallium arsenide and iodomethane include concentration, physical state of the arsenide, pH, role of oxygen and role of light.