Modeling growth rate of HfO2 thin films grown by metal-organic molecular beam epitaxy

HfO₂ dielectric layers were grown on the p-type Si (100) substrate by metal-organic molecular beam epitaxy (MOMBE). Hafnium-tetra-butoxide, Hf(O·t-C₄H₉)₄ was used as a Hf precursor and Argon gas was used as a carrier gas. The thickness of the HfO₂ film and intermediate SiO₂ layer were measured by scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM). The properties of the HfO₂ layers were evaluated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), high frequency (HF) capacitance-voltage (C-V) measurement, and current-voltage (I-V) measurement. C-V and I-V measurements have shown that HfO₂ layer grown by MOMBE has a high dielectric constant (k) of 20-22 and a low-level of leakage current density. The growth rate is affected by various process variables such as substrate temperature, bubbler temperature, Ar and O₂ gas flows and growth time. Since the ratio of O₂ and Ar gas flows are closely correlated, the effect of variations in O₂/Ar flow ratio on growth rate is also investigated using statistical modeling methodology.     

Growth and electronic properties of ZnO epilayers by plasma-assisted molecular beam epitaxy

ZnO thin films were grown on c-plane sapphire substrates by plasma-assisted molecular beam epitaxy (MBE). The crystalline properties of the layers as measured by x-ray diffraction were found to improve with lower growth temperatures, where the full-width at half-maximum (FWHM) of the x-ray rocking curves was shown to be in the range of 100 to 1,100 arcsec. The electronic properties were found to improve for higher growth temperatures, with n-type carrier concentration and electron mobility in the range of 1×10¹⁷ −5×10¹⁸ cm⁻³ and 80–36 cm²/Vs, respectively. Photoluminescence (PL) measurements indicated that growth at higher temperatures provided superior band edge radiative emission, while growth at lower temperatures resulted in significant deep level radiative emission centered at 2.35 eV. Photoconductive decay measurements exhibit a slow decay indicating the presence of hole traps, where Zn vacancies are believed to be the source of both the slow decay and the deep level emission observed in PL spectra.     

Growth of II-IV-V<Subscript>2</Subscript> chalcopyrite nitrides by molecular beam epitaxy

Synthesis of crystalline MgGeN₂ thin solid films is achieved using the technique of molecular beam epitaxy (MBE). The details of the epitaxial process are described. The microstructures of these films are investigated by both x-ray diffraction (XRD) and cross-sectional transmission electron microscopy (XTEM). Comparison of the lattice structure with powder diffraction standards suggests the lattice structure may be orthorhombic with a high degree of texture. Morphology is evaluated by atomic force microscopy, and a periodic pattern of growth mounds is observed. A formalism for dynamical roughening is applied to quantify the mounded surface features. Mounds are found to have an average spacing of 235 nm, and the surface exhibits a saturation value of 22 nm for the root mean correlated height difference. Diffusion bias is discussed as a mechanism for the formation of surface mounds.     

Electrical properties of low-temperature GaAs grown by molecular beam epitaxy and migration enhanced epitaxy

Measurements on low-temperature GaAs epitaxial layers (LT-GaAs) grown by molecular beam epitaxy and migration enhanced epitaxy showed that the excess arsenic incorporated during growth played a crucial role in determining their electrical properties. The electrical transport in LT-GaAs grown by a standard molecular beam epitaxy proceeded mainly via a hopping process, which showed a higher activation energy and onset temperature than those usually observed in lightly doped semiconductors. Using migration enhanced epitaxy to grow LT-GaAs, we were able to substantially reduce the density of As-rich defects and to achieve a good Hall mobility in Be-doped LT-GaAs. The study presented here indicates that, with controlled excess arsenic incorporation during growth, LT-GaAs can vary in a range of conduction properties and thus can be engineered for different device applications.     

InAs/GaSb超晶格中波焦平面材料的分子束外延技术

报道了InAs/GaSb超晶格中波材料的分子束外廷生长技术研究.通过改变GaSb衬底上分子束外延InAs/GaSb超晶格材料的衬底温度,以及界面的优化等,改善超晶格材料的表面形貌和晶格失配,获得了晶格失配△a/a=1.5×10-4,原子级平整表面的InAs/GaSb超晶格材料,材料77 K截止波长为4.87 μm.     

Structural characterization of DC magnetron-sputtered TiO2 thin films using XRD and Raman scattering studies

Titanium dioxide films have been deposited using DC magnetron sputtering technique onto well-cleaned p-silicon substrates at an oxygen partial pressure of 7×10^–5 mbar and at a sputtering pressure (Ar+O₂) of 1×10^–3 mbar. The deposited films were calcinated at 673 and 773 K. The composition of the films as analyzed using Auger electron spectroscopy reveals the stoichiometry with an O and Ti ratio 2.08. The influence of post-deposition annealing at 673 and 773 K on the structural properties of the titanium dioxide thin films have been studied using XRD and Raman scattering. The structure of the films deposited at the ambient was found to be amorphous and the films annealed at temperature 673 K and above were crystalline with anatase structure. The lattice constants, grain size, microstrain and the dislocation density of the film are calculated and correlated with annealing temperature. The Raman scattering study was performed on the as-deposited and annealed samples and the existence of Raman active modes A_1g, B_1g and E_g corresponding to the Raman shifts are studied and reported. The improvement of crystallinity of the TiO₂ films was also studied using Raman scattering studies.     

Crystal quality of InN thin films grown on ZnO substrate by radio-frequency molecular beam epitaxy

The growth of InN on {0001} ZnO substrates by radio-frequency, plasma-assisted, molecular-beam epitaxy (RF-MBE) has been experimentally investigated. The reflection high-energy electron diffraction (RHEED) pattern quickly recovered to a 1×1 streak pattern as the InN growth was started on nitridated ZnO substrates, whereas the RHEED pattern of the ZnO substrate was spotty because of plasma damage induced by nitridation. The full width at half maximum (FWHM) of the (0002) InN rocking curve was estimated to be around 150 arcsec from x-ray diffraction (XRD). Furthermore, we observed a remarkable feature from our experiments; namely, the crystal quality of InN does not seem to depend on the surface polarity of the ZnO substrate, while it is well known that InN growth on GaN has strong polarity dependence. To investigate this tendency, we have also investigated the surface stability of adatoms, In and N, on Zn- and O-face ZnO surfaces using a first-principles technique. From the theoretical study, N adsorption is more stable on ZnO surfaces of both polarities compared with In adsorption. Accordingly, the preferential initiation by N adatoms onto both ZnO surfaces can explain the unique style of InN growth on ZnO substrates.     

Optical characterization of anatase TiO2 films patterned by direct ultraviolet-assisted nanoimprint lithography

A direct ultraviolet (UV)-assisted nanoimprinting procedure using photosensitive titanium di-n-butoxide bis(2-ethylhexanoate) is employed in this study for the nanopatterning of anatase titanium dioxide (TiO₂) structure. Upon annealing at 400 °C for 1 h, the lateral shrinkage and thickness shrinkage of the TiO₂ nanostructure were 39.6% and 52.5%, respectively, which indicated an anisotropic volume loss. During UV irradiation and annealing treatment, the refractive index of UV-irradiated TiO₂ film is gradually increased by improvement in the packing density and crystallinity of the film. According to increasing UV exposure time and annealing temperature, the optical band gap (E_g) of UV-irradiated TiO₂ film is red-shifted from 3.73 to 3.33 eV due to the formation of lattice defects, vacancies and voids during the photochemical reaction and due to the effect of quantum confinement during annealing treatment. These results suggest that the refractive index and optical E_g of TiO₂ nanostructure could be controlled by tuning the UV exposure time and annealing treatment conditions. Nanopatterns of TiO₂ fabricated by direct UV-assisted nanoimprint lithography are potential candidates for use in protective coatings for optical mirrors and filters, high-reflectivity mirrors, broadband interference filters and active electro-optical devices where ordered surface nanostructures could be necessary.     

Lateral uniformity in HgCdTe layers grown by molecular beam epitaxy

The fabrication of high-quality focal plane arrays from HgCdTe layers grown by molecular beam epitaxy (MBE) requires a high degree of lateral uniformity in material properties such as the alloy composition, doping concentration, and defect density. While it is well known that MBE source flux nonuniformity can lead to radial compositional variation for rotating substrates, we have also found that composition can be affected significantly by lateral variations in substrate temperature during growth. In diagnostic experiments, we systematically varied the substrate temperature during MBE and quantified the dependence of HgCdTe alloy composition on substrate temperature. Based on these results, we developed a methodology to quickly and nondestructively characterize MBE-grown layers using postgrowth spatial mapping of the cutoff wavelength from the Fourier transform infrared (FTIR) transmission at 300 K, and we were able to obtain a quantitative relationship between the measured spatial variations in cutoff and the substrate temperature lateral distribution during growth. We refined this methodology by more directly inferring the substrate temperature distribution from secondary ion mass spectroscopy (SIMS) measurements of the As concentration across a wafer, using the fact that the As incorporation rate in MBE-grown p-type layers is highly sensitive to substrate temperature. Combining this multiple-point SIMS analysis with FTIR spatial mapping, we demonstrate how the relative contributions from flux nonuniformity and temperature variations on the lateral composition uniformity can be separated. This capability to accurately map the lateral variations in the substrate temperature has been valuable in optimizing the mounting and bonding of large substrates for MBE growth, and can also be valuable for other aspects of MBE process development.     

Structure of GaN films grown by molecular beam epitaxy on (0001) sapphire

GaN films grown by electron-cyclotron resonance plasma-assisted molecular beam epitaxy were studied by transmission electron microscopy and x-ray diffraction (XRD). Two sets of films were compared that were grown under identical conditions except for the ratio of the Ga to N flux. Films with a 30% higher Ga to N ratio (A films) were found to contain inversion domains (IDs). No IDs were found in films grown with a lower Ga to N ratio (B films), but instead the zinc-blende GaN was found near the film substrate interface. A narrower XRD rocking curve width along the (0002) direction and a broader rocking curve width along the asymmetric (1102) axis were found for A films compared to B films.     

Growth and properties of digitally-alloyed AlGaInP by solid source molecular beam epitaxy

Digital alloying using molecular beam epitaxy (MBE) was investigated to produce AlGaInP quaternary alloys for bandgap engineering useful in 600-nm band optoelectronic device applications. Alternating Ga_0.51In_0.49P/Al_0.51In_0.49P periodic layers ranging from 4.4 monolayers (ML) to 22.4 ML were used to generate 4,000-Å-thick (Al_0.5Ga_0.5)_0.51In_0.49P quaternary materials to understand material properties as a function of constituent superlattice layer thickness. High-resolution x-ray diffraction (XRD) analysis exhibited fine satellite peaks for all the samples confirming that digitally-alloyed (Al_0.5Ga_0.5)_0.51In_0.49P preserved high structural quality consistent with cross-sectional transmission electron microscopy (X-TEM) images. Low-temperature photoluminescence (PL) measurements showing a wide span of luminescence energies ～ 170 meV can be obtained from a set of identical composition digitally-alloyed (Al_0.5Ga_0.5)_0.51In_0.49P with different superlattice periods, indicating the bandgap tunability of this approach and its viability for III-P optoelectronic devices grown by MBE.     

Growth of HgSe and Hg1−xCdxSe thin films by molecular beam epitaxy

Thin epitaxial films of HgSe and Hg_1−xCd_xSe (x≤0.34) were successfully grown for the first time by molecular beam epitaxy. Film growth parameters are discussed, and results of structural, electrical, and optical studies are reported.     

Photoluminescence study of GaAs films on Si(100) grown by atomic hydrogen-assisted molecular beam epitaxy

Preliminary experimental results and analysis of photoluminescence (PL) measurements performed on GaAs heteroepitaxial films, which have been grown on Si(100) substrates by atomic hydrogen-assisted low-temperature molecular beam epitaxy technique have been presented and discussed. The results have also been compared with those obtained for GaAs homoepitaxial films. Furthermore, minority carrier lifetimes in n-GaAs on Si have been characterized by the PL decay method and an average lifetime of as high as 8.0 ns has been successfully obtained, which is the highest value ever reported to date.     

Characteristics and device applications of erbium doped III-V semiconductors grown by molecular beam epitaxy

We have studied the properties of molecular beam epitaxially (MBE)-grown Erdoped III-V semiconductors for optoelectronic applications. Optically excited Er³⁺ in insulating materials exhibits optical emission chiefly around 1.54 μm, in the range of minimum loss in silica fiber. It was thought, therefore, that an electrically pumped Er-doped semiconductor laser would find great applicability in fiber-optic communication systems. Exhaustive photoluminescence (PL) characterization was conducted on several of As-based III-V semiconductors doped with Er, on bulk as well as quantum-well structures. We did not observe any Errelated PL emission at 1.54 μm for any of the materials/structures studied, a phenomenon which renders impractical the realization of an Er-doped III-V semiconductor laser. Deep level transient spectroscopy studies were performed on GaAs and AlGaAs co-doped with Er and Si to investigate the presence of any Er-related deep levels. The lack of band-edge luminescence in the GaAs:Er films led us to perform carrier-lifetime measurements by electro-optic sampling of photoconductive transients generated in these films. We discovered lifetimes in the picosecond regime, tunable by varying the Er concentration in the films. We also found the films to be highly resistive, the resistivity increasing with increasing Er-concentration. Intensive structural characterization (double-crys-tal x-ray and transmission electron microscopy) performed by us on GaAs:Er epilayers indicates the presence of high-density nanometer-sized ErAs precipitates in MBE-grown GaAs:Er. These metallic nanoprecipitates probably form internal Schottky barriers within the GaAs matrix, which give rise to Shockley-Read-Hall recombination centers, thus accounting for both the high resistivities and the ultrashort carrier lifetimes. Optoelectronic devices fabricated included novel tunable (in terms of speed and responsivity) high-speed metal-semiconductor-metal (MSM) photodiodes made with GaAs:Er. Pseudomorphic AlGaAs/ InGaAs modulation doped field effect transistors (MODFETs) (for high-speed MSM-FET monolithically integrated optical photoreceivers) were also fabricated using a GaAs:Er buffer layer which substantially reduced backgating effects in these devices.     

Electrical properties and interfacial chemical environments of in situ atomic layer deposited Al2O3 on freshly molecular beam epitaxy grown GaAs

Interfacial chemical analyses and electrical characterization of in situ atomic layer deposited (ALD) Al₂O₃ on freshly molecular beam epitaxy (MBE) grown n- and p- GaAs (001) with a (4 × 6) surface reconstruction are performed. The capacitance-voltage (C-V) characteristics of as-deposited and 550 °C N₂ annealed samples are correlated with their corresponding X-ray photoelectron spectroscopy (XPS) interfacial analyses. The chemical bonding for the as-deposited ALD-Al₂O₃/n- and p-GaAs interface is similar, consisting of Ga₂O (Ga¹⁺) and As-As bonding (As⁰) without any detectable arsenic oxides or Ga₂O₃; the interfacial chemical environments remained unchanged after 550 °C N₂ annealing for 1hr. Both as-deposited and annealed p-GaAs metal-oxide-semiconductor capacitors (MOSCAPs) exhibit C-V characteristics with small frequency dispersion (<5%). In comparison, n-GaAs MOSCAPs shows much pronounced frequency dispersion than their p-counterparts.     

The influence of nitrogen ion energy on the quality of GaN films grown with molecular beam epitaxy

Since the growth of GaN using molecular beam epitaxy (MBE) occurs under metastable growth conditions, activated nitrogen is required to drive the forward synthesis reaction. In the process of exciting the nitrogen using a plasma or ion-beam source, species with large kinetic energies are generated. Impingement on the growth surface by these species can result in subsurface damage to the growing film, as well as an enhancement of the reverse decomposition reaction rate. In this study, we investigate the effect of the kinetic energy of the impinging nitrogen ions during growth on the resulting optical and structural properties of GaN films. Strong band-edge photoluminescence and cathodoluminescence are found when a kinetic energy of ∼10 eV are used, while luminescence is not detectable when the kinetic energies exceeds 18 eV. Also, we find that the use of conductive SiC substrates results in more homogeneous luminescence than the use of insulating sapphire substrates. This is attributed to sample surface charging in the case of sapphire substrates and subsequent variation in the incident ion flux and kinetic energy across the growth surface. This study clearly shows that the quality of GaN films grown by MBE are presently limited by damage from the impingement of high energy species on the growth surface.     

Origin of void defects in Hg1−xCdxTe grown by molecular beam epitaxy

Characterization of defects in Hg_1−xCd_xTe compound semiconductor is essential to reduce intrinsic and the growth-induced extended defects which adversely affect the performance of devices fabricated in this material system. It is shown here that particulates at the substrate surface act as sites where void defects nucleate during Hg_1−xCd_xTe epitaxial growth by molecular beam epitaxy. In this study, we have investigated the effect of substrate surface preparation on formation of void defects and established a one-to-one correlation. A wafer cleaning procedure was developed to reduce the density of such defects to values below 200 cm⁻². Focal plane arrays fabricated on low void density materials grown using this new substrate etching and cleaning procedure were found to have pixel operability above 98.0%.     

In situ control of gan growth by molecular beam epitaxy

Methods to determine GaN surface temperature, surface composition, and growth rates using in situ desorption mass spectroseopy (DMS) and reflection high energy electron diffraction (RHEED) are demonstrated for molecular beam epitaxial growth of GaN using NH₃. Using these methods, the GaN surface temperature, T_s, and GaN growth rates as a function of T_s, Ga flux, and NH₃ flux were obtained. Surface temperatures were determined from DMS and RHEED measurements of the temperature at which Ga condenses on GaN. NH₃-limited and Ga-limited growth regimes are identified and the transition between these regimes is shown to be abrupt. NH₃-limited samples have a weakly reconstructed (2 × 2) RHEED pattern, while Ga-limited samples reveal a transmission pattern. Atomic force microscopy showed that NH₃-limited samples exhibit atomic steps while Ga-limited samples exhibit faceting.     

利用全固态分子束外延方法在Ge(100)衬底上异质外延GaAs薄膜及相关特性表征

利用全固态分子束外延(MBE)方法在Ge(100)衬底上异质外延GaAs薄膜,并通过高能电子衍射(RHEED)、高分辨X射线衍射(XRD),原子力显微镜等手段研究了不同生长参数对外延层的影响.RHEED显示在较高的生长温度或较低的生长速率下,低温GaAs成核层呈现层状生长模式.同时降低生长温度和生长速率会使GaAs薄膜的XRD摇摆曲线半高宽(FWHM)减小,并降低外延层表面的粗糙度,这主要是由于衬底和外延薄膜之间的晶格失配度减小的结果.     

Microstructural and optical characterization of CdTe(211)B/ZnTe/Si(211) grown by molecular beam epitaxy

CdTe layers have been grown by molecular beam epitaxy on 3 inch nominal Si(211) under various conditions to study the effect of growth parameters on the structural quality. The microstructure of several samples was investigated by high resolution transmission electron microscopy (HRTEM). The orientation of the CdTe layers was affected strongly by the ZnTe buffer deposition temperature. Both single domain CdTe(133)B and CdTe(211)B were obtained by selective growth of ZnTe buffer layers at different temperatures. We demonstrated that thin ZnTe buffer layers (<2 nm) are sufficient to maintain the (211) orientation. CdTe deposited at ∼300°C grows with its normal lattice parameter from the onset of growth, demonstrating the effective strain accommodation of the buffer layer. The low tilt angle (<1°) between CdTe[211] and Si[211] indicates that high miscut Si(211) substrates are unnecessary. From low temperature photoluminescence, it is shown that Cd-substituted Li is the main residual impurity in the CdTe layer. In addition, deep emission bands are attributed to the presence of As_Te and Ag_Cd acceptors. There is no evidence that copper plays a role in the impurity contamination of the samples.