Raman scattering and Rutherford backscattering studies on InN films grown by plasma-assisted molecular beam epitaxy

A series of InN thin films was grown on sapphire substrates via plasma-assisted molecular beam epitaxy (PA-MBE) with different nitrogen plasma power. Various characterization techniques, including Hall, photoluminescence, Raman scattering and Rutherford backscattering, have been employed to study these InN films. Good crystalline wurtzite structures have been identified for all PA-MBE grown InN films on sapphire substrate, which have narrower XRD wurtzite (0002) peaks, showed c-axis Raman scattering allowed longitudinal optical (LO) modes of A₁ and E₁ plus E₂ symmetry, and very weak backscattering forbidden transverse optical (TO) modes. The lower plasma power can lead to the lower carrier concentration, to have the InN film close to intrinsic material with the PL emission below 0.70 eV. With increasing the plasma power, high carrier concentration beyond 1 × 10²⁰ cm^− 3 can be obtained, keeping good crystalline perfection. Rutherford backscattering confirmed most of InN films keeping stoichiometrical In/N ratios and only with higher plasma power of 400 W leaded to obvious surface effect and interdiffusion between the substrate and InN film.     

A comparative study of InN growth on quartz,silicon, C-sapphire and bulk GaN substrates by RF magnetron sputtering

In this work, we investigate the growth of indium nitride (InN) films on quartz, bulk GaN, sapphire (001) and Si (111) substrates. An InN buffer layer was first deposited on all the substrates, then an InN film was grown on bare substrate and InN buffered substrates. The films were polycrystalline in nature with preferred orientation along (002) plane. Best structural quality was observed on InN buffered Si substrate. The structural properties were explained by calculating the full width at half maximum, crystallite size, micro-strain, and dislocation density. The morphology of the films revealed similar granular features except for bare sapphire substrate which showed cracks and more oxygen percentage. The application of buffer layer increased the surface roughness for quartz and reduced in other cases. The band gap of InN films was determined using UV–visible reflectance spectroscopy. The lowest band gap value was observed for InN buffered quartz substrate.     

Near-infrared photoluminescence of vertically aligned InN nanorods grown on Si(111) by plasma-assisted molecular-beam epitaxy

We demonstrate that vertically aligned InN nanorods have been grown on Si(111) substrates by plasma-assisted molecular-beam epitaxy (PA-MBE) at low and high growth temperatures (LT- and HT-InN nanorods). High-resolution scanning electron microscopy images clearly show that InN nanorods grown on Si(111) are hexagonal in shape, vertically aligned, well separated and densely distributed on the substrate. The size distribution of LT-InN nanorods is quite uniform, while the HT-InN nanorods exhibit a broad, bimodal distribution. The structural analysis performed by Raman scattering indicates that PA-MBE grown InN nanorods have the wurtzite-type InN single-crystal structure with the rod axis (growth direction) along the c-axis. In addition, both types of nanorods contain high concentrations of electrons (unintentionally doped). Compared to the HT-InN nanorods and the PA-MBE-grown InN epitaxial film, the LT-grown InN nanorods have a considerable number of structural defects. Near-infrared photoluminescence (PL) from LT- (∼ 0.77 eV) and HT-InN (∼ 0.70 eV) nanorods is clearly observed at room temperature. In comparison with the LT-InN nanorods, the PL efficiency of HT-InN nanorods is better and the PL peak energy is closer to that of InN-on-Si epitaxial films (∼ 0.66 eV). We also find that the PL band at low temperatures from nanorods is significantly weaker (compared to the InN film case) and exhibits anomalous temperature effects. We propose that these PL properties are results of considerable structural disorder (especially for the LT-InN nanorods) and strong surface electron accumulation effect (for both types of nanorods).     

Improvement of InN layers deposited on Si(111) by RF sputtering using a low-growth-rate InN buffer layer

We investigate the influence of a low-growth-rate InN buffer layer on structural and optical properties of wurtzite nanocrystalline InN films deposited on Si(111) substrates by reactive radio-frequency sputtering. The deposition conditions of the InN buffer layer were optimized in terms of morphological and structural quality, leading to films with surface root-mean-square roughness of ~ 1 nm under low-growth-rate conditions (60 nm/h). The use of the developed InN buffer layer improves the crystalline quality of the subsequent InN thick films deposited at high growth rate (180 nm/h), as confirmed by the narrowing of X-ray diffraction peaks and the increase of the average grain size of the layers. This improvement of the structural quality is further confirmed by Raman scattering spectroscopy measurements. Room temperature PL emission peaking at ~ 1.58 eV is observed for InN samples grown with the developed buffer layer. The crystal and optical quality obtained for InN films grown on Si(111) using the low-growth-rate InN buffer layer become comparable to high-quality InN films deposited directly on GaN templates by RF sputtering.     

Study of surface morphology control and investigation of hexagonal indium nitride nanorods grown on GaN/sapphire substrate

Heteroepitaxial growth of metal-catalyst-free indium nitride (InN) nanorods on GaN/sapphire substrates by radio-frequency metal-organic molecular beam epitaxy (RF-MOMBE) system was investigated. We found that different N/In flow ratios together with the growth temperatures greatly influenced the surface morphology of InN nanorods and their structural properties. The InN nanorods have been characterized in detail using X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM). Optical property was evaluated by photoluminescence (PL) measurements. At lower growth temperatures, InN nanorods were successfully grown. A pronounced two-dimensional growth mode was observed at higher growth temperature of 500 degrees C, and these films showed preferred orientation along the c-axis. XRD patterns and SEM images reveal that InN nanorods has high quality wurtzite structure with FWHM approaching 900 arcsec, and they have uniform diameters of about 150 nm and length of about 800 nm. Meanwhile, no metallic droplet was observed at the end of the nanostructured InN, and this is strong evidence that the nanorods are grown via the self-catalyst process. The PL peak at 0.8 eV is attributed to the quantum confinement and Moss-Burstein effects. These observations provide some valuable insights into the physical-chemical process for manufacturing InN nanorods devices.     

MOCVD growth of GaN layer on InN interlayer and relaxation of residual strain

100 nm InN layer was grown on sapphire c-plane using a metal-organic chemical vapor deposition (MOCVD) system. Low temperature (LT) GaN layer was grown on InN layer to protect InN layer from direct exposure to hydrogen flow during high temperature (HT) GaN growth and/or abrupt decomposition. Subsequently, thick HT GaN layer (2.5 μm thick) was grown at 1000 °C on LT GaN/InN/sapphire template. Microstructure of epilayer-substrate interface was investigated by transmission electron microscopy (TEM). From the high angle annular dark field TEM image, the growth of columnar structured LT GaN and HT GaN with good crystallinity was observed. Though thickness of InN interlayer is assumed to be about 100 nm based on growth rate, it was not clearly shown in TEM image due to the InN decomposition. The lattice parameters of GaN layers were measured by XRD measurement, which shows that InN interlayer reduces the compressive strain in GaN layer. The relaxation of compressive strain in GaN layer was also confirmed by photoluminescence (PL) measurement. As shown in the PL spectra, red shift of GaN band edge peak was observed, which indicates the reduction of compressive strain in GaN epilayer.     

Epitaxial growth of InN on c-plane sapphire by pulsed laser deposition with r.f. nitrogen radical source

We have grown InN films on c-plane sapphire substrates by pulsed laser deposition (PLD) with a radio frequency nitrogen radical source for the first time and investigated the effect of the substrate surface nitridation on the structural and electrical properties of InN films with reflection high energy electron diffraction (RHEED), atomic force microscope, the Hall effect measurements and high-resolution X-ray diffraction (HRXRD). RHEED and HRXRD characterizations revealed that high-quality InN grows epitaxially on sapphire by PLD and its epitaxial relationship is InN (0 0 0 1)∣∣sapphire (0 0 0 1) and InN [2 -1 -1 0]∣∣sapphire [1 0 -1 0]. The InN crystalline quality and the electron mobility are improved by the substrate nitridation process. The area of the pits at the InN surface is reduced by the substrate nitridation process probably due to the reduction in the interface energy between InN and the substrate. The full width at half maximum of the -1 -1 2 4 X-ray rocking curve for InN grown by the present technique without using any buffer layers was as small as 34.8 arcmin. These results indicate that the present technique is promising for the growth of the high-quality InN films.     

Depth dependence of structural quality in InN grown by metalorganic chemical vapor deposition

Rutherford backscattering and channeling is combined with X-ray diffraction to study the depth dependence of crystalline quality in InN layers grown by metalorganic chemical vapor deposition on sapphire substrate. The poorest crystalline quality in InN layer is produced at the intermediate region over 100 nm away from the InN/sapphire interface. With increasing layer thickness the crystalline quality improves to a certain degree dependent on the growth temperature. The InN sample grown at 450 °C is found to be more homogeneous than the sample grown at 550 °C. The difference in the defect profile is explained by the temperature-dependent growth modes. The inhomogeneity of structural quality and related properties such as carrier concentration and strain field is possibly the reason to observe a high energy wing in PL spectrum of the InN sample grown at 550 °C.     

Mn- and Cr-Doped InN: A Promising Diluted Magnetic Semiconductor Material

Cr- and Mn-doped InN films were successfully grown by plasma-assisted molecular beam epitaxy on c-plane sapphire substrates. Low temperature GaN buffer layers grown by metal-organic vapor-phase epitaxy were used to accommodate the large lattice mismatch between InN and sapphire. A high n-type carrier concentration of 1.5×10²⁰ cm^–3 was measured in InN films with 3% Cr-doping. Films of this type exhibit a well-defined in-plane magnetic hysteresis loop and remanence for temperatures varying from 5 to 300K. The Mn-doped films, however, turned out to exhibit less clear magnetic properties. Thus, ferromagnetism in Cr-doped InN can be concluded from our measurements.     

Oxidation study of polycrystalline InN film using in situ X-ray scattering and X-ray photoemission spectroscopy

Oxidation process of polycrystalline InN films were investigated using in situ X-ray diffraction (XRD) and X-ray photoemission spectroscopy (XPS). The films were grown by dc sputter on sapphire (0001) substrates and were oxidized in air at elevated temperatures. The XRD data showed that the structure of the films changed to the bixbyite In₂O₃ (a = 10.11 Å) above 450 °C. Chemical configurations of the sample surfaces were investigated using high-resolution XPS. For the non-intentionally oxidized InN film, XPS analysis on the In 3d peak and the N 1s main peak at 396.4 eV suggests that indium and nitrogen are bound dominantly in the form of InN. An additional peak observed at 397.4 eV in the N 1s photoelectrons and the O 1s peaks indicate that the InN film surface is partly oxidized to have InO_xN_y configuration. After oxidation of the InN film at elevated temperature, the O 1s spectrum is dominated by In₂O₃ peak, which indicates that the structure is stable chemically with In₂O₃ configuration at least within the XPS probing depth of a few nm.     

Initial stages of the cubic-InN growth with the technique of the pre-deposition of indium

The initial stages of the cubic indium nitride film growth at 350 °C were studied using low-pressure metal-organic chemical vapor deposition. The technique of the pre-deposition of indium was applied, that is, a layer of indium was first deposited on sapphire surface before the growth of InN. X-ray diffraction and X-ray photoelectron spectroscopy show that the pre-deposition of indium is able to promote the growth of InN films, and meanwhile, suppress the indium aggregation in the as-grown films. Atomic force microscopy images of InN films indicate that the pre-deposition of indium not only enhances the density of nucleate sites, but also facilitates the coalescence among the InN islands. The free energy calculations reveal that the pre-deposited indium atoms preferentially react with NH and N radicals after NH₃ introduction, which leads to the formation of InN on the sapphire surface. The preferentially formed InN is then supposed to be responsible for the above phenomena.     

Infrared spectra of the hydrogenated amorphous silicon layers on metallic substrates of solar absorbers

Infrared absorption spectra were investigated in hydrogenated amorphous silicon (a-Si(H)) films deposited both by d.c. reactive sputtering (RS) and by r.f. glow discharge (GD) of silane. The films were deposited onto polished niobium and tungsten solar test disks to form spectrally selective absorbers for comparative photothermal and photovoltaic studies. Spectra were observed from the normal spectral reflectance from 400 to 3900 cm^-1 with a Fourier transform spectrometer. Hydrogen, alloyed typically at 10–35 at.% in these a-Si films, significantly reduces the gap state density and produces IR spectra characteristic of Si-H bonding complexes depending on the deposition method and the substrate temperature T_D. Comparison between RS and GD films revealed significant differences in their IR spectra. RS films show a strong Si-O-Si bonding absorption from atmospheric oxygen. GD films have a marked Si-H wagging mode absorption resolved into three components. This band is very sensitive to the deposition conditions and decays with increasing T_D. The SiH₃ rocking mode was identified at 500 cm^-1 in the GD films. The hydrogen concentration from the IR stretching mode absorption was correlated with the H₂ evolution results of McMillan and Peterson on identical films. The transition with increasing T_D could be traced from the room temperature state with polymeric complexes of hydrogen to the high temperature state with the single monohydride complex.     

Hardness, elastic modulus and structure of indium nitride thin films on AlN-nucleated sapphire substrates

The structural properties of epitaxial indium nitride thin films were characterized and related to the mechanical properties as measured by nanoindentation. The seven epitaxial InN films examined were deposited over the temperature range 200–400°C by reactive magnetron sputtering on (0 0.1) sapphire substrates buffered with a thin AlN layer. The hardness, surface texture and crystal quality of the InN films were functions of the deposition temperature, with the maximum hardness (11.2 GPa), the smoothest surface, the minimum c-lattice constant (0.5708 nm), and the minimum (0 0.4) X-ray rocking curve width (0.6°) all occurring at the deposition temperature of 350°C. The crystal quality and the hardness of the InN films degraded at both higher and lower temperatures. This revised version was published online in July 2006 with corrections to the Cover Date.     

ZnO thin films deposited by a CVT technique in closed ampoules

ZnO thin films were prepared on quartz glass, Si (100), and sapphire (001) substrates by a chemical vapour transport (CVT) technique. During the growing processes, the source and substrate temperatures were maintained at 1000 °C and 600 °C, respectively. The scanning electron microscopy (SEM) and X-ray diffraction (XRD) measurements showed that the crystalline qualities of ZnO thin films were sensitively dependent on substrates. ZnO thin film deposited on sapphire substrate exhibited the best morphology with the largest crystallite size of more than 20 μm. Meanwhile, the XRD patterns showed that ZnO thin film deposited on sapphire substrate was strongly c-axis preferred-oriented with high crystalline quality. The optical properties of ZnO thin films were investigated by photoluminescence (PL) spectroscopy at room temperature (RT). The results suggested that the optical properties of ZnO thin films were highly influenced by their crystalline qualities and surface morphologies.     

Growth of InN layers on Si (111) using ultra thin silicon nitride buffer layer by NPA-MBE

Indium nitride (InN) epilayers have been successfully grown by nitrogen-plasma-assisted molecular beam epitaxy (NPA-MBE) on Si (111) substrates using different buffer layers. Growth of a (0001)-oriented single crystalline wurtzite-InN layer was confirmed by high resolution X-ray diffraction (HRXRD). The Raman studies show the high crystalline quality and the wurtzite lattice structure of InN films on the Si substrate using different buffer layers and the InN/β-Si₃N₄ double buffer layer achieves minimum FWHM of E₂ (high) mode. The energy gap of InN films was determined by optical absorption measurement and found to be in the range of ~ 0.73-0.78 eV with a direct band nature. It is found that a double-buffer technique (InN/β-Si₃N₄) insures improved crystallinity, smooth surface and good optical properties.     

Formation of a two-dimensional electron gas in ZnO/MgZnO single heterostructures and quantum wells

The properties of ZnO/MgZnO heterostructures grown by pulsed-laser deposition on sapphire (112?0) and ZnO (0001?) have been compared. Electron accumulation layers have been observed for ZnO/MgZnO heterostructures grown on sapphire by capacitance-voltage (C-V) spectroscopy. The formation of a two-dimensional electron gas (2DEG) in these structures has been confirmed by temperature dependent Hall effect measurements. From C-V measurements the sheet carrier density in a Zn_0.8 Mg_0.2O/ZnO/Zn_0.8 Mg_0.2O quantum well (QW) structure with a well width of about 5 nm is calculated to be only about 9.0 × 10¹⁰ cm^− 2. For the films deposited on sapphire 2D growth is observed in the Burton-Cabrera-Frank mode, as confirmed by atomic force microscopy. Step flow growth mode was achieved for the homoepitaxial thin films. Quantum confinement effects have been confirmed by photoluminescence (PL) measurements. Homoepitaxial QWs are more homogeneous (smaller inhomogeneous recombination broadening) than heteroepitaxial QWs.     

Effects of sapphire substrates surface treatment on epitaxial ZnO thin films grown by MOCVD

The surface treatment effects of sapphire substrate on the quality of epitaxial ZnO thin films grown by metal-organic chemical vapor deposition (MOCVD) were studied. The sapphire substrates have been investigated by means of atomic force microscopy (AFM) and X-ray diffraction rocking curves (XRCs). The results show that sapphire substrate surfaces have the best-quality by CMP with subsequent chemical etching. The surface treatment effects of sapphire substrate on the ZnO thin films were examined by X-ray diffraction (XRD), atomic force microscopy (AFM) and photoluminescence (PL) measurements. Results show that the intensity of (002) diffraction peak of ZnO thin films on sapphire substrates treated by CMP with subsequent chemical etching is strongest. FWHM of (002) diffraction peak is narrowest and the intensity of UV peak of PL spectrum is strongest, indicating surface treatment on sapphire substrate preparation may improve ZnO thin films crystal quality and photoluminescent property.     

Investigation on Mn doped ZnO thin films grown by RF magnetron sputtering

In this paper, we have investigated the Zn_1 − x Mn_xO (x = 0.05, 0.10 and 0.15) thin films grown by RF magnetron sputtering. The grown films on sapphire [Al₂O₃(0001)] substrates have been characterized using X-ray Diffraction (XRD), Photoluminescence (PL) and Vibrating Sample Magnetometer (VSM) in order to investigate the structural, optical and magnetic properties of the films respectively. It is observed from XRD that all the films are single crystalline with (002) preferential orientation along c-axis. PL spectra reveal that the addition of Mn marginally shifts the Near Band Edge (NBE) position towards the higher energy side. The magnetic measurements of the films using VSM clearly indicate the ferromagnetic nature.     

Low-temperature growth of highly c-oriented InN films on glass substrates with ECR-PEMOCVD

High quality InN films are deposited with an interlayer of high c-orientation (002) AZO (Aluminium-doped Zinc Oxide; ZnO:Al) films on glass substrates by electron cyclotron resonance plasma-enhanced metal organic chemical vapor deposition (ECR-PEMOCVD) at low temperature. AZO films used as a buffer layer are effective for the epitaxial growth of InN films. The influence of Trimethyl Indium (TMIn) flux on the properties of InN films is systematically investigated by reflection high energy electron diffraction (RHEED), X-ray diffraction analysis (XRD), atomic force microscopy (AFM) and optical transmittance spectra. The results indicate that high quality InN films with high c-orientation and small surface roughness are successfully achieved at an optimized Trimethyl Indium (TMIn) flux of 5.5 sccm. The InN/AZO structures have great potential for the development of full spectra solar cells.     

Annealing effects of sapphire substrate on the structure and properties of ZnO films grown via pulsed laser deposition

The structure, morphology, and properties of ZnO films were examined in relation to an annealed sapphire substrate prepared via pulsed laser deposition. The annealing effects of the sapphire substrate on the ZnO films were studied via X-ray diffraction (XRD), atomic-force microscopy (AFM), and photoluminescence (PL) measurements. The XRD patterns and PL spectra results showed that the optical quality of the ZnO films was significantly affected by the annealing temperature of the sapphire substrate. The optimum annealing temperature of the sapphire substrate was 1400 degrees C. Atomically-flat-surface and high-density atomic steps were formed after annealing treatment, which were qualified to be good nucleation sites for ZnO film growth.