A. D. Bulanov

The Highly Isotopic Enriched (99.9%), High-Pure 28Si Single Crystal

We report on the growth of 99,9 % enriched 28 Si, dislocation free monocrystals (111- and 100-orientated) with nearly 10 g weight and less than 10 15 foreign atoms/cm 3 .

Preparation and Fine Purification of SiF4 and 28SiH4

Silicon tetrafluoride was obtained by the thermal decomposition of pure-grade sodium hexafluorosilicate and purified by low-temperature distillation. Next, SiF4 was 28Si-enriched by centrifugation and converted to silane by calcium hydride reduction. To remove hydrocarbons, the silane was distilled.

Monoisotopic varieties of silicon and germanium with a high chemical and isotopic purity

We presented the results on the preparation of high-purity monoisotopic varieties of silicon and germanium. The process involves the separation of isotopes in the form of SiF4 and GeH4 by centrifugation, ultrapurification of volatile compounds, and preparation of poly and single crystals. The attained degree of isotopic and chemical purities of single crystals obtained was shown. The content of the main isotope in the single crystals of 28Si is >99.99% and those in the single crystals of 29Si and 30Si are >99.9%. The specific resistivity of the 28Si single crystals is ∼1 kOhm cm and those of 29Si and 30Si are about 100–150 Ohm cm. The samples of the 76Ge single crystals have the main isotope content of >88 at.% and the difference concentration of electrochemically active impurities of 5·1010 cm−3. The main isotope content in the 74Ge polycrystal is 99.93 at.%. The optical and thermophysical properties of the isotope-enriched silicon and germanium single crystals were measured, which suggest a significant effect of the isopotic composition on thermal capacity, thermal conductivity, luminiscence, and light absorption.

Ultrapurification of 76Ge-enriched GeH4 by distillation

Abstract76Ge-enriched germane has been ultrapurified by low-temperature distillation. The nature and concentration of molecular impurities in the germane samples were determined by gas chromatography/mass spectrometry, high-resolution Fourier transform IR spectroscopy, and gas chromatography. The distillate contains no more than 10−5 mol % hydrocarbons, 10−4 mol % carbon dioxide, 10−3 to 10−1 mol % digermane and trigermane, and <3 × 10−5 mol % other impurities. A distinctive feature of the impurity composition of the isotopically enriched germane samples is the presence of silicon tetrafluoride and sulfur hexafluoride impurities.

Synthesis of High-Purity Calcium Hydride

A procedure for synthesizing high-purity calcium hydride in high yield was suggested. The admixture composition of the resulting CaH2 was determined by laser mass spectrometry.

Fine Purification of Monoisotopic Silanes 28SiH4 , 29SiH4 , and 30SiH4 via Distillation

High-purity isotopically enriched (99.98% 28Si, 99.57% 29Si, and 99.83% 30Si) silane samples are prepared for the first time. The total hydrocarbon content of the samples is no higher than 0.1–0.3 ppm. The concentration of electroactive impurities in the silicon prepared from the purified monoisotopic silane is below 1015 cm–3.

Determination of low loss in isotopically pure single crystal 28Si at low temperatures and single microwave photon energy

The low dielectric losses of an isotopically pure single crystal 28Si sample were determined at a temperature of 20 mK and at powers equivalent to that of a single photon. Whispering Gallery Mode (WGM) analysis revealed large Quality Factors of order 2 × 106 (dielectric loss ~5 × 10−7) at high powers, degrading to 7 × 10−5 (dielectric loss ~1.4 × 10−6 at single photon energy. A very low-loss narrow line width paramagnetic spin flip transition was detected with extreme sensitivity in 28Si, with very small concentration below 1010 cm−3 (less than 10 parts per trillion) and g-factor of 1.995 ± 0.008. Such determination was only possible due to the low dielectric photonic losses combined with the long lifetime of the spin transition (low magnetic loss), which enhances the magnetic AC susceptibility. Such low photonic loss at single photon energy combined with the narrow line width of the spin ensemble, indicate that single crystal 28Si could be an important crystal for future cavity QED experiments.

Hydrocarbon impurities in SiF4 and SiH4 prepared from it

Using gas chromatography and high-resolution Fourier-transform IR spectroscopy, we have determined the concentrations of C1–C4 hydrocarbon impurities in isotopically unmodified silicon tetrafluoride before and after fine purification and in 28Si-enriched SiF4. The concentrations of C1–C4 hydrocarbon impurities in silicon tetrafluoride for SiH4 synthesis have been shown to correlate with those in the synthesized silane.

Impurity composition of high-purity isotopically enriched monosilane and monogermane

The impurity composition of 28SiH4, 29SiH4, and 30SiH4 silanes and 72GeH4, 73GeH4, 74GeH4, and 76GeH4 germanes isotopically enriched to above 99.9 at % has been studied by gas chromatography/mass spectrometry using capillary adsorption columns. Impurities have been identified by comparing their mass spectra with NIST data and information available in the literature, and by inferring their structure from fragment ions and retention times. We have identified 53 impurity substances in silanes and 42 in germanes: permanent gases; saturated, unsaturated, halogen-containing, and aromatic C1–C9 hydrocarbons; their homologues; alkyl derivatives of silane and germane; chlorogermane; siloxanes; fluorosiloxanes; sulfur compounds; and dioxane. The silicon- and germanium-containing impurities have been shown to be isotopically enriched, as the major component. The detection limits of the impurities are 5 × 10–8 to 3 × 10–5 vol %, comparing well with the best results in the literature.

Liquid-vapor equilibria in GeF4-A (A = C1-C4 alkane impurity) systems

The liquid–vapor separation factors in dilute solutions of methane, ethane, propane, n-butane, and isobutane in germanium tetrafluoride have been determined experimentally at 295 K by statically balancing phases. The measured temperature-dependent saturated vapor pressure over liquid germanium tetrafluoride in the range 260–300 K can be represented by the Antoine equation: log P (atm) = 5.2–1200/T. We have calculated the enthalpies of vaporization and fusion of germanium tetrafluoride:ΔHv0= 22.9 kJ/mol and ΔHm0(GeF4) = 8.0 kJ/mol.