Thermal stability of SiGe films on an ultra thin Ge buffer layer on Si grown at low temperature

The thermal stability of SiGe films on an ultra thin Ge buffer layer on Si fabricated at low temperature has been studied. The microstructure and morphology of the samples were investigated by high-resolution X-ray diffraction, Raman spectra and atomic force microscopy, and using a diluted Secco etchant to reveal dislocation content. After thermal annealing processing, it is observed that undulated surface, threading dislocations (TDs) and stacking faults (SFs) appeared at the strained SiGe layer, which developed from the propagation of a misfit dislocation (MD) during thermal annealing, and no SFs but only TDs formed in strain-relaxed sample. And it is found that the SiGe films on the Ge layer grown at 300 °C has crosshatch-free surface and is more stable than others, with a root mean square surface roughness of less than 2 nm and the threading dislocation densities as low as ∼10⁵ cm⁻². The results show that the thermal stability of the SiGe films is associated with the Ge buffer layer, the relaxation extent and morphology of the SiGe layer.     

Strain relaxation of epitaxial SiGe layer and Ge diffusion during Ni silicidation on cap-Si/SiGe/Si(0 0 1)

Strain relaxation of the epitaxial SiGe layer and Ge diffusion during nickel silicidation by rapid thermal annealing the structure of Ni(≅14 nm)/cap-Si(≅26 nm)/Si_0.83Ge_0.17/Si(0 0 1) at the elevated annealing temperatures, T_A, were investigated by X-ray diffraction analyses of high-resolution ω-2θ scan and reciprocal space mapping. The analyses showed a much larger strain relaxation at a lower T_A and a reduction in Ge content in the SiGe layer of Ni/SiGe/Si(0 0 1) after thermal annealing compared to the case of cap-Si/SiGe/Si(0 0 1). The results indicate that the strain relaxation of the SiGe layers in NiSi/SiGe/Si(0 0 1) is related to the phenomena of NiSi agglomeration and penetration into the SiGe layer during silicidation at elevated anneal temperatures ≥750 °C. At elevated T_A ≥ 750 °C, Ge diffused into the intact cap-Si area during silicidation.     

Fabrication of high Ge content SiGe-on-insulator with low dislocation density by modified Ge condensation

A SiGe-on-insulator (SGOI) structure with high Ge content and low density of dislocations is fabricated by a modified Ge condensation technique. The formation and elimination of stacking faults during condensation process are analyzed by transmission electron microscopy. A Si_0.19Ge_0.81OI substrate is fabricated utilizing two steps of oxidation and intermittent annealing. The time of oxidation or annealing at 900 °C is essential for the elimination of stacking faults in high Ge content SGOI substrate. The surface morphology of SGOI is investigated by atomic force microscopy and the defect density is evaluated from wet etching method. After the final condensation, the surface root-mean-square roughness (rms) of SiGe layer is kept below 1 nm and the threading defect density is controlled around 10⁴ cm⁻². The smooth surface and integrated lattice structure of SiGe layer indicate that the SGOI is suitable for heteroepitaxial growth of strained Ge, GaAs and III-V compounds.     

Study of the surface cleaning of GOI and SGOI substrates for Ge epitaxial growth

An effective wet cleaning process, optimized for low temperature Ge epitaxial growth on thin Ge or SiGe structures with reduced surface roughening, is proposed. It is found that HF + HCl cleaning is the most effective wet cleaning method that is applicable to the low temperature thermal cleaning. It is also found that temperature of the thermal cleaning appropriate to 25-30 nm thick germanium on insulator (GOI) or silicon-germanium on insulator (SGOI) substrates is approximately 450 °C. Moreover, it is also found that the temperatures of Ge epitaxial growth even in lattice-matched systems must be reduced to around 400 °C to prevent surface roughening and those in lattice-mismatched systems also must be reduced sufficiently (300 °C for strained Ge growth on SGOI (X_eff = 0.6)) to prevent lattice relaxation as well as surface roughening. Finally, the successful formation of the compressively strained GOI structures is demonstrated by applying these wet cleaning and low temperature thermal cleaning processes and low temperature Ge epitaxy to thin SGOI substrates.     

Effect of annealing on structural, optical and electrical properties of nanostructured Ge thin films

Ge thin films with a thickness of about 110 nm have been deposited by electron beam evaporation of 99.999% pure Ge powder and annealed in air at 100-500 °C for 2 h. Their optical, electrical and structural properties were studied as a function of annealing temperature. The films are amorphous below an annealing temperature of 400 °C as confirmed by XRD, FESEM and AFM. The films annealed at 400 and 450 °C exhibit X-ray diffraction pattern of Ge with cubic-F structure. The Raman spectrum of the as-deposited film exhibits peak at 298 cm⁻¹, which is left-shifted as compared to that for bulk Ge (i.e. 302 cm⁻¹), indicating nanostructure and quantum confinement in the as-deposited film. The Raman peak shifts further towards lower wavenumbers with annealing temperature. Optical band gap energy of amorphous Ge films changes from 1.1 eV with a substantial increase to ∼1.35 eV on crystallization at 400 and 450 °C and with an abrupt rise to 4.14 eV due to oxidation. The oxidation of Ge has been confirmed by FTIR analysis. The quantum confinement effects cause tailoring of optical band gap energy of Ge thin films making them better absorber of photons for their applications in photo-detectors and solar cells. XRD, FESEM and AFM suggest that the deposited Ge films are composed of nanoparticles in the range of 8-20 nm. The initial surface RMS roughness measured with AFM is 9.56 nm which rises to 12.25 nm with the increase of annealing temperature in the amorphous phase, but reduces to 6.57 nm due to orderedness of the atoms at the surface when crystallization takes place. Electrical resistivity measured as a function of annealing temperature is found to reduce from 460 to 240 Ω-cm in the amorphous phase but drops suddenly to 250 Ω-cm with crystallization at 450 °C. The film shows a steep rise in resistivity to about 22.7 KΩ-cm at 500 °C due to oxidation. RMS roughness and resistivity show almost opposite trends with annealing in the amorphous phase.     

Solid phase epitaxy of Ge films on CaF2/Si(1 1 1)

At room temperature deposited Ge films (thickness < 3 nm) homogeneously wet CaF₂/Si(1 1 1). The films are crystalline but exhibit granular structure. The grain size decreases with increasing film thickness. The quality of the homogeneous films is improved by annealing up to 200 °C. Ge films break up into islands if higher annealing temperatures are used as demonstrated combining spot profile analysis low energy electron diffraction (SPA-LEED) with auger electron spectroscopy (AES). Annealing up to 600 °C reduces the lateral size of the Ge islands while the surface fraction covered by Ge islands is constant. The CaF₂ film is decomposed if higher annealing temperatures are used. This effect is probably due to the formation of GeF_x complexes which desorb at these temperatures.     

Luminescence properties of Ge implanted SiO2:Ge and GeO2:Ge films

We have investigated cathodeluminescence (CL) of Ge implanted SiO₂:Ge and GeO₂:Ge films. The GeO₂ films were grown by oxidation of Ge substrate at 550 °C for 3 h in O₂ gas flow. The GeO₂ films on Ge substrate and SiO₂ films on Si substrate were implanted with Ge-negative ions. The implanted Ge atom concentrations in the films were ranging from 0.1 to 6.0 at%. To produce Ge nanoparticles the SiO₂:Ge films were thermally annealed at various temperatures of 600-900 °C for 1 h in N₂ gas flow. An XPS analysis has shown that the implanted Ge atoms were partly oxidized. CL was observed at wavelengths around 400 nm from the GeO₂ films before and after Ge⁻-implantation as well as from SiO₂:Ge films. After Ge⁻-implantation of about 0.5 at% the CL intensity has increased by about four times. However, the CL intensity from the GeO₂:Ge films was several orders of magnitude smaller than the intensity from the 800 °C-annealed SiO₂:Ge films with 0.5 at% of Ge atomic concentration. These results suggested that the luminescence was generated due to oxidation of Ge nanoparticles in the SiO₂:Ge films.     

Nanoindentation analysis of the pop-in events on SiGe single layer

The growth of metastable silicon germanium (Si_0.8Ge_0.2) thin film on Si(1 0 0) by ultrahigh-vacuum chemical vapor deposition has been subjected to residual indentation studies. A nanoindentation system has been applied to analyze SiGe film after different annealing treatments. A number of phenomena have been found for the heteroepitaxial growth of SiGe film at the critical thickness of 350 nm, including single discontinuity (the so-called “pop-in” event) as well as the elastic/plastic contact translation. Atomic force microscopy is employed to investigate the surface impression. Pop-in events in the load-indentation depth curves of 400 and 500 °C and no nano-cracks in the vicinity regions are found. The values of H ranging from 13.13±0.9, 21.66±1.3, 18.52±1.1, 14.47±0.7 GPa and the values of E ranging from 221.8±5.3, 230.7±6.4, 223.5±4.6, 156.7±3.8 GPa, are obtained. The elastic/plastic contact translation of the SiGe film occurs at different annealing conditions, with h_f/h_max values in the range of 0.501, 0.392, 0.424, and 0.535 for samples are treated at RT, 400, 500, and 600 °C, respectively. The mechanism responsible for the pop-in event in such crystal structure is due to the interaction of the indenter tip with the pre-existing threading dislocations, since the release of the indentation load is bound to be reflected in the directly compressed volume.     

Infrared electroluminescence from a Si MOS structure with Ge in the oxide

We report on room-temperature infrared electroluminescence (EL) from metal-oxide-semiconductor devices made from Si. We compare the luminescence from RF sputtered oxide films containing SiO₂ with and without Ge by using a composite target and luminescence from a SiO₂ layer made by rapid thermal oxidation. The sputtered films were annealed in the temperature range 600-900 °C. This densifies the films and is likely to reduce the concentration of defects. A luminescence peak located around 1150-1170 nm is observed at current densities as low as 0.1 A/cm². The corresponding photon energy is close to that of the Si band gap. In addition, we observe several broad luminescence bands in the range 1000-1750 nm. These bands get stronger with Ge in the SiO₂ film. Some of these bands have previously been suggested and are directly associated with Ge. Since we observe that the intensity is correlated with the presence of Ge while the mere presence of the bands is not, we discuss the EL bands being due to defects which concentration is influenced by Ge in the oxide.     

Low-temperature oxidation of SiGe by liquid-phase deposition

Low-temperature silicon dioxide (SiO₂) films were grown on silicon germanium (SiGe) surfaces using the liquid-phase deposition (LPD) method. The growth solutions of LPD-SiO₂ are hydrofluorosilicic acid (H₂SiF₆) and boric acid (H₃BO₃). It was found that the growth rate increases with increasing temperature and concentration of H₃BO₃. The Auger electron spectroscopy profile shows that no pileup of Ge atoms occurs at the interface of SiO₂/SiGe after the LPD-SiO₂ growth. Al/LPD-SiO₂/p-SiGe MOS capacitors were prepared to determine capacitance-voltage (C-V) and current-voltage (I-V) characteristics. In our experiments, a low leakage current density of 8.69 × 10⁻⁹ A/cm² under a 2 MV/cm electric field was observed. Such a value is much smaller than those of plasma- and thermal-oxides as a result of no plasma damage and a lower growth temperature. Moreover, lower oxide charges and interface charge densities of 3.82 × 10¹⁰ cm⁻² and 1.12 × 10¹¹ eV⁻¹ cm⁻², respectively, were achieved in our LPD-SiO₂ compared to direct photochemical-vapor-deposition-SiO₂.     

Effect of oxidation temperature on microstructure, mechanical behaviors and surface morphology of nanocomposite Ti-Cx-Ny thin films

Two nanocomposite Ti-C_x-N_y thin films, TiC_0.95N_0.60 and TiC_2.35N_0.68, as well as one pure TiN, were deposited at 500 °C on Si(1 0 0) substrate by reactive unbalanced dc-magnetron sputtering. Oxidation experiments of these films were carried out in air at fixed temperatures in a regime of 250-600 °C with an interval of 50 °C. As-deposited and oxidized films were characterized and analyzed using X-ray diffraction (XRD), microindentation, Newton's ring methods and atomic force microscopy (AFM). It was found that the starting oxidation temperature of nanocomposite Ti-C_x-N_y thin films was 300 °C irrespective of the carbon content; however their oxidation rate strongly depended on their carbon content. Higher carbon content caused more serious oxidation. After oxidation, the film hardness value remained up to the starting oxidation temperature, followed by fast decrease with increasing heating temperature. The residual compressive stress did not show a similar trend with the hardness. Its value was first increased with increase of heating temperature, and got its maximum at the starting oxidation temperature. A decrease in residual stress was followed when heating temperature was further increased. The film surface roughness value was slightly increased with heating temperature till the starting oxidation temperature, a great decrease in surface roughness was followed with further increase of heating temperature.     

Nanoscratch studies of SiGe epitaxial layer damage on the Si substrate

The present study evaluates the wear performance of silicon-germanium (SiGe) epitaxial growth of thin films, in which the in situ scratch profile is followed by ex situ atomic force microscopy (AFM) examinations. The wear evaluation of SiGe films was carried out at different constant loads (2000, 4000, and 6000 μN) with the same sliding speeds. The microstructural morphology was observed by means of transmission electron microscopy (TEM)Findings show that annealing treatments of SiGe films exhibit the highest scratch resistance at 400 °C compared to that of the as-deposited sample. The main characteristic of SiGe film is its ability to withstand wear resistance; observations show that moderate compressive residual is beneficial to the film, since it can suppress crack initiation. The annealing treatments of SiGe films revealed the resultant adhesive and cohesive failure mechanism.     

Effect of nanostructured AlN coatings on the oxidation-resistant properties of optical diamond films

Diamond film is an ultra-durable optical material with high thermal conductivity and good transmission in near-infrared and far-IR (8-14 μm) wavebands. CVD diamond is subjected to oxidation at temperature higher than 780 °C bared in air for 3 min, while it can be protected from oxidation for extended exposure in air at temperature up to 900 °C by a coating of aluminum nitride. Highly oriented AlN coatings were prepared for infrared windows on diamond films by reactive sputtering method and the average surface roughness (R_a) of the coatings was about 10 nm. The deposited films were characterized by X-ray diffraction (XRD) and atom force microscope (AFM). XRD confirmed the preferential orientation nature and AFM showed nanostructures. Optical properties of diamond films coated AlN thin film was investigated using infrared spectrum (IR) compared with that for as-grown diamond films.     

Structural and surface properties of Si1−xGex thin films obtained by reduced pressure CVD

This paper investigates the structure and surface characteristics, and electrical properties of the polycrystalline silicon-germanium (poly-Si_1−xGe_x) alloy thin films, deposited by vertical reduced pressure CVD (RPCVD) in the temperature range between 500 and 750 °C and a total pressure of 5 or 10 Torr. The samples exhibited a very uniform good quality films formation, with smooth surface with rms roughness as low as 7 nm for all temperature range, Ge mole fraction up to 32% (at 600 °C), textures of 〈2 2 0〉 preferred orientation at lower temperatures and strong 〈1 1 1〉 at 750 °C, for both 5 and 10 Torr deposition pressures. The ³¹P⁺ and ¹¹B⁺ doped poly-Si_1−xGe_x films exhibited always lower electrical resistivity values in comparison to similar poly-Si films, regardless of the employed anneal temperature or implantat dose. The results indicated also that poly-Si_1−xGe_x films require much lower temperature and ion implant dose than poly-Si to achieve the same film resistivity. These characteristics indicate a high quality of obtained poly-Si_1−xGe_x films, suitable as a gate electrode material for submicron CMOS devices.     

Physico-chemical and electrical properties of rapid thermal oxides on Ge-rich SiGe heterolayers

Rapid thermal oxidation of high-Ge content (Ge-rich) Si_1−xGe_x (x = 0.85) layers in dry O₂ ambient has been investigated. High-resolution X-ray diffraction (HRXRD) and strain-sensitive two-dimensional reciprocal space mapping X-ray diffractometry (2D-RSM) are employed to investigate strain relaxation and composition of as-grown SiGe alloy layers. Characterizations of ultra thin oxides (∼6-8 nm) have been performed using Fourier transform infrared spectroscopy (FTIR) and high-resolution X-ray photoelectron spectroscopy (HRXPS). Formation of mixed oxide i.e., (SiO₂ + GeO₂) and pile-up of Ge at the oxide/Si_1−xGe_x interface have been observed. Enhancement in Ge segregation and reduction of oxide thickness with increasing oxidation temperature are reported. Interface properties and leakage current behavior of the rapid thermal oxides have been studied by capacitance-voltage (C-V) and current-voltage (J-V) techniques using metal-oxide-semiconductor capacitor (MOSCAP) structures and the results are reported.     

Formation of gold nanoparticles in heat-treated reactive co-sputtered Au-SiO2 thin films

In this work, formation of gold nanoparticles in radio frequency (RF) reactive magnetron co-sputtered Au-SiO₂ thin films post annealed at different temperatures in Ar + H₂ atmosphere has been investigated. Optical, surface topography, chemical state and crystalline properties of the prepared films were analyzed by using UV-visible spectrophotometry, atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and X-ray diffractometry (XRD) techniques, respectively. Optical absorption spectrum of the Au-SiO₂ thin films annealed at 800 °C showed one surface plasmon resonance (SPR) absorption peak located at 520 nm relating to gold nanoparticles. According to XPS analysis, it was found that the gold nanoparticles had a tendency to accumulate on surface of the heat-treated films in the metallic state. AFM images showed that the nanoparticles were uniformly distributed on the film surface with grain size of about 30 nm. Using XRD analysis average crystalline size of the Au particles was estimated to about 20 nm.     

Wet cleaning and surface characterization of Si1−xGex virtual substrates after a CMP step

New reactants such as ozone dissolved in ultra-pure water have been widely used the last few years instead of the original Radio Corporation of America (RCA) cleaning (which is a combination of the Standard Cleaning 1 (SC1) and the Standard Cleaning 2 (SC2)). In a first part of the study (Microelectron. Eng. 83 (2006) 1986), we had quantified the efficiency of a new cleaning sequence (that calls upon HF and H₂O/O₃ solutions) on polished Si_1−xGe_x virtual substrates (x = 0.2-0.5). We are discussing here the surface morphology and wetability together with the oxide thickness and structure typically obtained after this so-called “DDC-SiGe” wet cleaning. Flat surface morphologies are found after cleaning whatever the Ge content (from 20 to 50%). Typical root mean square roughness is around 0.4 nm. We have used X-ray Photoelectron Spectroscopy to determine the characteristics of the surface termination after this “DDC-SiGe” cleaning. An oxide mainly composed of SiO₂ is formed, with a low fraction of Ge sub-oxide and GeO₂. The distribution of chemical species is not that different from the one obtained after the use of a SC1 cleaning. However, the chemical oxide formed is slightly thicker. Such a HF/O₃ cleaning leads, when used on thick Ge layers grown on Si, to the formation of a really thin Ge sub-oxide. Our oxidation model assumes a competition in O₃ solutions between the oxidation rates of Si and Ge atoms (faster for Si) and the dissolution of the Ge oxide formed in solution. This mechanism, which implies the formation of a slightly porous oxide, is different from the one seeming to occur in SC1-based solutions. Indeed, the addition of surfactant in a SC1 solution modifies the oxidation rate compared to standard SC1 or O₃-based solutions, suggesting a diffusion of reactants towards the interface between the SiGe and the oxide in formation, assisted by the reactions of species within the cleaning solutions.     

Effect of H2 and O2 plasma etching treatment on the surface of diamond-like carbon thin film

In this study, we investigated the surface properties of diamond-like carbon (DLC) films for biomedical applications through plasma etching treatment using oxygen (O₂) and hydrogen (H₂) gas. The synthesis and post-plasma etching treatment of DLC films were carried out by 13.56 MHz RF plasma enhanced chemical vapor deposition (PECVD) system. In order to characterize the surface of DLC films, they were etched to a thickness of approximately 100 nm and were compared with an as-deposited DLC film. We obtained the optimum condition through power variation, at which the etching rate by H₂ and O₂ was 30 and 80 nm/min, respectively. The structural and chemical properties of these thin films after the plasma etching treatment were evaluated by Raman and Fourier transform infrared (FT-IR) spectroscopy. In the case of as-deposited and H₂ plasma etching-treated DLC film, the contact angle was 86.4° and 83.7°, respectively, whereas it was reduced to 35.5° in the etching-treated DLC film in O₂ plasma. The surface roughness of plasma etching-treated DLC with H₂ or O₂ was maintained smooth at 0.1 nm. These results indicated that the surface of the etching-treated DLC film in O₂ plasma was hydrophilic as well as smooth.     

Formation of periodic structures by the space-selective precipitation of Ge nanoparticles in channel waveguides

Thermally stabilized channel waveguides with Bragg gratings were fabricated by the space-selective precipitation technique of crystalline Ge nanoparticles using KrF excimer laser irradiation. The periodic structures consisting of Ge nanoparticles were formed in Ge-B-SiO₂ thin glass films after exposure to an interference pattern of the laser followed by annealing at 600 °C. The channel waveguides with the periodic structures were fabricated by the cladding of the patterned Cr layers on the films. The diffraction peak for the TE-like mode of 11.8 dB depth was observed clearly at a wavelength of 1526.4 nm, indicating that the periodic structure also served as the optical band-pass filter in optical communication wavelength. The spectral shape, diffraction efficiency, and diffraction wavelength remained unchanged even after annealing at 400 °C. Furthermore, a low temperature dependence of the diffraction wavelength - as low as 8.1 pm/°C - was achieved. The diffraction efficiency was further enhanced after subsequent annealing at 600 °C. The space-selective precipitation technique is expected to be useful for the fabrication of highly reliable optical filters or durable sensing devices operating at high temperature.     

In-plane magnetization with high coercivity in terbium iron garnet thin films deposited on Pt/Si substrate by PLD

We report on the growth of terbium iron garnet (TbIG, Tb₃Fe₅O₁₂) thin films having anomalously large coercivity and in-plane easy axis of magnetization. The TbIG thin films were prepared at room temperature (RT) on Pt/Si(1 0 0) substrates by pulsed laser deposition technique. The films deposited at RT were X-ray amorphous and do not show any magnetic order. Annealing of the RT deposited film at 900 °C resulted into fully textured (532) TbIG film. Atomic force microscopy and cross-sectional scanning electron microscopy studies of the TbIG films showed good surface quality with an average surface roughness of 5.0 nm and thickness of about 300 nm, respectively. The M-H loops measured at 20 K for TbIG films, exhibit about an order of magnitude enhancement in the coercivity value (H_c) than the single crystal. In-plane and out-of-plane M-H loops revealed that the easy axis of the magnetization lies within the film’s plane. In-plane magnetization combining with large H_c value of the TbIG thin film may be of scientific interest for the possible applications.