X-ray photoelectron spectroscopic study on initial oxidation of hafnium hydride fractured in an ultra-high vacuum

The initial oxidation of hafnium hydride was studied by X-ray photoelectron spectroscopy (XPS). The clean surface of hafnium hydride was obtained by fracturing the specimen in an XPS measurement chamber under a background pressure of 2.7 × 10⁻⁶ Pa. The fractured surface was oxidized in situ with the exposure to high-purity oxygen and the residual gases in an ultra-high vacuum chamber. The XPS spectra for the oxidized surfaces had the shoulder due to the oxidation, and the shoulder grew up with increase in exposure time even in the ultra-high vacuum. The factor analysis for the XPS spectra of the oxidized surface showed that the oxide formed in the chamber consists of only the hafnium dioxide, and no suboxide states are contained. The result corresponded to the oxide observed on hafnium hydride fractured in air.     

The adsorption of water vapor on clean cleaved germanium: II. Electrical properties

Clean germanium surfaces obtained by cleavage in ultrahigh vacuum were exposed to water vapor in the range from 10^?9 up to 1 Torr min. Surface state properties have been derived from measurements of surface conductivity and field effect mobility. At coverages close to a monolayer a steplike change in surface state density indicates a change of the adsorption state similar to a phase transition. The results are described quantitatively by assuming that each structure has its characteristic surface state distribution.     

Effect of low-temperature annealing upon electrophysical parameters for germanium surfaces cleaved in liquid helium

The surface state localized charge on germanium surfaces cleaved in liquid helium is found to be low. He-vapour heating results in irreversible variations of SS characteristics, such as charge density, increase. These variations are believed to be due to rearrangements of the near surface crystalline structure induced by cleaving and subsequent heating of the samples. The temperature shock arised on cleaving might be responsible for the surface crystalline structure and defect formation. The surface obtained is heterogeneous. Nonuniform surface properties are caused by different energy release and relief geometry which results from different crack advancing conditions over the cleaved surface. The influence of adsorption of foreign atoms on the SS characteristics has been also investigated.     

Surface photovoltage spectroscopy of electronic surface states on cleaved germanium(111) surfaces

Surface photovoltage (SPV) measurements on UHV cleaved Ge(111) surfaces at 100 K are reported for photon energies 0.4 < ?ω < 1 eV. The SPV spectra are sensitive to surface treatment. Upon annealing to temperatures above 200°C, which is accompanied by a reconstruction change from the (2 × 1) to an (8) superstructure, the SPV spectrum shows 2 shoulders below band gap energy with threshold energies near 0.4 and 0.45 eV. These structures are interpreted in terms of electronic transitions from the valence band into empty surface state levels which are related to the (8) superstructure. Adsorbed oxygen and water vapor both cause new similar transitions from the valence band into empty surface states at 0.08 eV below the bottom of the conduction band.     

The adsorption of water vapor on clean cleaved germanium: I. Structural and kinetic properties

Germanium (111) faces cleaved in UHV have been exposed to water vapor in the pressure range 10^?8 to 1 torr. From LEED observations and Auger electron spectroscopy an adsorption up to one monolayer with two sites per molecule is derived. After adsorption each molecule precludes 3–4 surface atoms from further adsorption. From the disappearance of the superstructure of the clean surface with a fraction of a monolayer it is concluded that each adsorbed molecule converts a patch with about 50–80 surface atoms with respect to superstructure.     

Influence of adsorbates on UV-pulsed laser melting of Si in ultra-high vacuum

The dynamics of laser melting of atomically clean Si is investigated in ultra-high-vacuum (UHV) by transient reflectivity with single-pulse sensitivity in the presence of monitored amounts of chlorine, oxygen or propene. Adsorption of one monolayer (1 ML) leads to measurable variations of the melting dynamics, which are strongly adsorbate-dependent. The variations differ qualitatively and quantitatively from those observed with heavy exposures to gases. The melting dynamics returns to that of clean Si upon subsequent irradiation by laser pulses without readsorption. The required number of pulses for return to clean Si dynamics depends strongly on the type of adsorbate. Adsorbate-induced changes of absorption and reflectivity, and/or incorporation of adsorbates into the substrate, do not explain the results. By contrast, the variations of the melting dynamics are correlated to the photoemitted electron yield, suggesting that laser melting is sensitive to the presence of electrons in the conduction band. These results show that accurate modelling of laser melting of Si interacting with gases should take into account the presence of the gases. Received: 12 September 2000 / Accepted: 9 January 2001 / Published online: 27 June 2001     

Electrical breakdown properties of stainless steel and titanium electrodes in ultra-high vacuum

The breakdown voltage in ultra-high vacuum of stainless steel and titanium electrodes is measured as a function of the electrode separation in the range 0.05-0.80 mm. This relationship can be described by the simple equation V_b = Cd^a. Values for c and a are given for all electrode combinations. For titanium electrodes the current just before breakdown was about three times that for stainless steel electrodes. Comparative measurements with all combinations of stainless steel and titanium show that the cause of this difference must be sought in the anode. The microscopic breakdown field strength was a function of the emitting cathode area, as derived from Fowler-Nordheim plots. This dependence suggests that the breakdown was initiated by thermal instabilities at the anode due to field emission electrons. This is consistent with a theoretical analysis. Measurements of the pre-breakdown current allow an estimate of the number and dimensions of emitting sites.     

Simultaneous imaging of tunneling current and damping energy by noncontact-AFM in ultra-high vacuum

We have simultaneously observed the images of tunneling current and damping energy with the nc-AFM (noncontact atomic force microscopy) image of Si(111)7ǻ. When inverted contrast is observed in the constant frequency shift nc-AFM image, the current image is not inverted, and vice versa. On the other hand, the damping images show a contrast similar to that of the nc-AFM images; the damping decreases at a narrow separation between the tip and the sample. This possibly indicates that the damping decreases as the attractive interaction increases under a constant oscillation amplitude of the cantilever. To keep the oscillation amplitude constant under an attractive interaction between a tip and a sample, the total energy of the cantilever oscillation is reduced and the oscillation velocity of the cantilever decreases. An explanation is proposed that the change in energy dissipation occurs in the cantilever oscillation, depending on the oscillation velocity of the cantilever, and the value is estimated from a simple model.     

Chemical states of GeTe thin-film during structural phase-change by annealing in ultra-high vacuum

The chemical states of GeTe thin film are investigated using high-resolution X-ray photoelectron spectroscopy (HRXPS) with synchrotron radiation, during amorphous to crystalline structural phase transition. As the temperature increases from 250 to 400 °C, we observe the rock-salt crystalline structure and phase with X-ray diffraction (XRD) and transmission electron microscopy (TEM). Spin-orbit splitting of the Ge 3d core-level spectrum clearly appears after annealing at 400 °C for 5 min. However, the binding energy of the Ge 3d_5/2 core-level peak of 29.8 eV does not change in the amorphous to crystalline structural phase transition. In the case of the Te 4d core-level, change in binding energy and peak shapes is also negligible. We assume that the Te atom is fixed at a site between the amorphous and crystalline phases. Although the structural environment of the Ge atoms changes during the structural phase transition, the chemical environment does not.     

Surface chemistry study of Mn-doped germanium nanowires

Single crystal germanium nanowires have been grown by vapour-liquid-solid deposition onto silicon oxide substrates with Au catalyst nanoparticles. They have been doped by two different techniques: Ge and Mn co-evaporation during growth and post-growth Mn implantation. Scanning electron microscopy images show that Mn-implanted nanowires have a lower surface density and a smaller average diameter (18.8 nm) than the un-doped ones and those Mn doped by co-deposition. The effectiveness of Mn doping has been verified by X-ray photoemission spectroscopy and by energy-dispersive X-ray measurements, indicating in the two cases significant Mn atomic concentration in the nanowire. X-ray diffraction indicates that the nanowires are single crystals and that they do not contain precipitates of Mn extrinsic phases. Both SEM and XPS experimental evidences are in line to indicate that the Mn doping by ion implantation is preferable with respect to that one performed by co-evaporation as it reduces the thickness of the outer oxide sheath of the nanowires and their diameter.     

Titanium-induced germanium nanocones synthesized by vacuum electron-beam evaporation: growth mechanism and morphology evolution

High-vacuum electron-beam evaporation method is used for large area, metal-nucleated germanium (Ge) nanodots and nanocones on Si₃N₄/Si preparation. Nanodot and nanocone arrays with uniform size in bulk-quantity are synthesized using titanium (Ti) nanocrystals as nucleating center at 750 °C with different Ge deposition amount, respectively. The morphology evolution from nanodot to nanocone is studied by atomic force microscopy (AFM). The structure of the prepared sample is characterized by X-ray diffraction (XRD) and Raman scattering. Ge nanocones formed by this convenient fabrication process could have potential applications on nanoelectronics and vacuum electron field emission.     

AlN thin films fabricated by ultra-high vacuum electron-beam evaporation with ammonia for silicon-on-insulator application

The application of silicon-on-insulator (SOI) substrates to high-power integrated circuits is hampered by the self-heating effect due to the poor thermal conductivity of the buried SiO₂ layer. We introduce aluminum nitride (AlN) thin films formed by ultra-high vacuum electron-beam evaporation with ammonia as an alternative. The chemical composition, surface morphology, and electrical properties of these films were investigated. The film synthesized at 800 °C shows a high AlN content, low surface roughness with a root-mean-square value of 0.46 nm, and high electrical resistivity. Based on thermodynamic analysis and our experimental results, the mechanism of AlN formation is proposed.     

Auger and electron energy loss spectroscopic study of surfaces of iron-sulfur alloy,Fe7S8 and FeS2 cleaved in ultra high vacuum

The surfaces of an iron-210 at. ppm sulfur alloy, Fe₇S₈ and FeS₂ cleaved in an ultra high vacuum were studied by Auger (AES) and electron energy loss Spectroscopy (EELS). The S LVV Auger transition for the intergranular fracture plane of the alloy indicates that the sulfur is bonded to the surface as though it were adsorbed. The loss energies of the transition from valence to conduction bands for the surface are identical to those for the transgranular fracture planes. The trans- and intergranular fracture planes have very similar fine structure in the Fe MVV Auger transition profile. This indicates that the interaction between iron and sulfur is too weak to perturb the electronic structure at the fracture surface. The spectral features of the electron transitions having kinetic energies between approximately 40 and 50 eV are explained by a normal Fe MVV Auger transition and an autoionization process after excitation of Fe 3p electrons. The low spin ferrous ion in FeS₂ results in triplet peaks for the Fe MVV transition and doublet peaks for the autoionization event, but similar transitions for Fe₇S₈ exhibit singlet peak for each process.     

A PTIS study of quenched-in acceptors in germanium

The shallow acceptors produced in germanium crystals by quenching from 820–925 C have been studied for the first time using Photo-Thermal Ionization Spectroscopy (PTIS). We have found two acceptor-continua, which correspond to the E_v + 8.4 meV and E_v + 12 meV levels observed in earlier Hall measurements. With the lower energy continuum there are associated two previously unobserved hydrogenic acceptors. They are shallower than any known acceptor in germanium: their ionization energies are 8.69 ±0.01 meV and 9.48 ±0.01 meV. We attribute the acceptors to two different defects because of differences in their creation and annealing behaviour. No discrete lines were found to be associated with the higher energy continuum. We estimate the acceptor ionization energy to be about 14 meV. Finally, we have observed a number of as yet unexplained negative lines superimposed on both acceptor-continua.     

Size controlled deposition of Cu and Si nano-clusters by an ultra-high vacuum sputtering gas aggregation technique

In this paper we have reported the syntheses of copper and silicon nano-clusters by a sputtering-gas-aggregation type growth technique. The process involves typical magnetron sputtering vaporization of target materials followed by an inert gas condensation to form clusters of varying sizes. The size-distributions of the clusters typically follow a normal-distribution and the peak cluster sizes of the distributions depends on several factors, which include gas-flow rate, length of the growth region, deposition pressure etc. We have observed a variation in the peak cluster size with the variation of the gas (argon) flow rates. The experimental values are compared with the existing models and the results are found to be in good agreement. The results are significant since it demonstrates that proper optimization of operation conditions can lead to desired cluster sizes as well as desired cluster-size distributions. PACS 81.07.-b; 61.46.Bc; 39.10.+j; 81.20.-n; 36.40.-c     

X-ray topography study of the cleaved Si-(111)-face

Cleaved silicon (111) faces were studied with reflection x-ray topography using a high resolving double-crystal-diffractometer. Three types of defects due to cleavage process could be observed: long-range strain due to overlap cracks along macroscopic cleavage steps, a homogeneous decrease of intensity within the inclined portion of step mainly due to optical refraction of x-rays and point-like defects along some macroscopic cleavage steps, which develop only after heat treatment. The findings are important with respect to interpretation of electrical measurements, since all types of defects may influence the surfaces state density decisively.