Highly c-axis oriented AlN layers grown on c-plane sapphire substrates by radio-frequency sputter epitaxy at 1080 °C

Aluminum nitride (AlN) single-crystalline layers were grown on c-plane sapphire substrates by radio-frequency magnetron sputter epitaxy using N₂/Ar mixture ambient gas and 5-N grade Al target. The crystalline structures of the AlN layers depending on substrate temperature and N₂ composition ratio in ambient gas, were predominantly studied. The crystalline quality of the AlN layer was improved by elevating substrate temperature, and the full-widths at half-maximum (FWHMs) of X-ray rocking curves (XRC) for both symmetric and asymmetric planes of AlN layers grown at N₂ composition ratio of around 25%, became low. The FWHMs of XRC for (0002) diffraction of the AlN layers grown at 1080 °C, were less than 20 arcsec. The surface root-mean-square roughness of such highly c-axis oriented AlN layer was determined by atomic force microscopy, and was increased from 0.6 nm to 1.3 nm when AlN layer thickness was varied from 0.15 to 0.7 μm.     

Buffer effects on the mosaic structure of the HR-GaN grown on 6H-SiC substrate by MOCVD

High-resistive GaN (>10⁸ Ω cm) layers have been grown with different buffer structures on 6H-SiC substrate using metalorganic chemical vapor deposition reactor. Different combination of the GaN/AlN super lattice, low temperature AlN, high temperature AlN and Al_xGa_1?xN (x ≈ 0.67) layers were used in the buffer structures. The growth parameters of the buffer layers were optimized for obtaining a high-resistive GaN epilayer. The mosaic structure parameters, such as lateral and vertical coherence lengths, tilt and twist angle (and heterogeneous strain), and dislocation densities (edge and screw dislocations) of the high-resistive GaN epilayers have been investigated using x-ray diffraction measurements. In addition, the residual stress behaviors in the high-resistive GaN epilayers were determined using both x-ray diffraction and Raman measurements. It was found that the buffer structures between the HR-GaN and SiC substrate have been found to have significant effect on the surface morphology and the mosaic structures parameters. On the other hand, both XRD and Raman results confirmed that there is low residual stress in the high-resistive GaN epilayers grown on different buffer structures.     

Room-temperature growth of AlN/TiN epitaxial multi-layer by laser molecular beam epitaxy

We have fabricated epitaxial AlN thin films at room temperature on sapphire (0001) substrates with a TiN (111) epitaxial buffer layer by pulsed laser deposition in ultra-high vacuum (laser molecular beam epitaxy method). The TiN buffer layers were also fabricated at room temperature. Four-circle X-ray diffraction analysis and reflection high-energy electron diffraction results indicate the heteroepitaxial structure of AlN (0001)/TiN (111)/sapphire (0001) with the epitaxial relationship of AlN [10-10]||TiN [11-2]||sapphire [11-20]. The surface of the room-temperature grown AlN film was found to be atomically flat, reflecting the nano-stepped surface of ultrasmooth sapphire substrates. Then, we could achieve the room-temperature epitaxial growth of [AlN/TiN] multi-layer. The temperature dependence of resistivity of the AlN/TiN multi-layer film was also measured.     

Structural characterization of group III nitrides grown by pulsed laser deposition

We have grown thin GaN epitaxial films on Si(1 1 1) and sapphire (0 0 0 1) with AlN buffer layers using pulsed laser deposition and investigated the distortion of the films using synchrotron radiation grazing incidence-angle X-ray diffraction for the first time. We have found that the strains in the AlN films were almost fully relaxed at the growth temperature (800 °C) by the introduction of the misfit dislocations. However, we have also found that the introduction of misfit dislocations at the interfaces between the AlN buffer layers and the GaN films is not rigorous enough to release the stain fully at the growth temperature.     

Effect of buffer layer thickness on the growth properties of hydrothermally grown ZnO nanorods

We investigated the effect of ZnO buffer layer thickness on the growth of hydrothermally grown ZnO nanorods. A series of ZnO buffer layers with different thicknesses was deposited on a p-Si (111) substrate using a co-sputtering system. After annealing the ZnO buffer layer, ZnO nanorods grown were grown hydrothermally at 95 degrees C. Unlike ZnO nanorods grown on as-deposited ZnO buffer layer, the diameter and length of ZnO nanorods grown on annealed ZnO buffer layers can be controlled. The structural and optical properties of ZnO nanorods grown on annealed ZnO buffer layers were analyzed by field-emission scanning electron microscopy, X-ray diffraction, and photoluminescence. The influence of ZnO buffer layer thickness on ZnO nanorods growth is discussed.     

GaN films grown by vapor-phase epitaxy in a hydride-chloride system on Si(111) substrates with AlN buffer sublayers

Oriented GaN layers with a thickness of about 10 μm have been grown by hydride-chloride vaporphase epitaxy (HVPE) on Si(111) substrates with AlN buffer layers. The best samples are characterized by a halfwidth (FWHM) of the X-ray rocking curve of ω_θ = 3–4 mrad. The level of residual mechanical stresses in AlN buffer layers decreases with increasing temperature of epitaxial growth. The growth at 1080°C is accompanied by virtually complete relaxation of stresses caused by the lattice mismatch between AlN and Si.     

Growth and characterization of shape memory alloy thin films for Si microactuator technologies

NiTi thin film alloys have been grown on Si (1 0 0) substrates by sequential multilayer deposition of Ni and Ti layers followed by metal interdiffusion via annealing. Short-time (5 min) annealing of the deposited layers at 500 °C leads to alloying of Ni and Ti, provided that preferential oxidation of Ti is avoided. This has been achieved by capping the layers with AlN, which constitutes a very efficient barrier preventing oxygen contamination of the film. For uncapped films, annealing has to be performed under high vacuum conditions. The structure of the processed films strongly depends on the temperature and time of the thermal process, obtaining Ni- and Ti-rich phases when the films are annealed at higher temperatures and/or during longer times. As-grown and processed films are analyzed by X-ray diffraction, in-depth Auger electron spectroscopy and X-ray photoelectron spectroscopy techniques. Finally, resistivity measurements show the existence of a phase transition in the films annealed at 600 °C without the capping layers (vacuum furnace). This contrasts with the behavior observed for AlN capped films, where cracking of the film occurs during cooling, which has been attributed to generation of stress in the buried film during the phase transition.     

四步法制备高质量硅基砷化镓薄膜

为了提高在硅基上外延砷化镓薄膜的质量和实验的可重复性, 我们提出了一种叫做四步生长法的新方法, 该方法是通过在低温成核层和高温外延层中间先后插入低温缓冲层和高温缓冲层实现的。通过此方法, 可以制备出表面具有单畴结构、在强白光下依然光亮如镜、粗糙度低且缺陷少的高质量砷化镓薄膜, 而且此方法的重复性很好。即便没有任何生长后的退火处理, 外延出的1 μm厚砷化镓薄膜在5 μm×5 μm扫描区域内的表面粗糙度只有2.1 nm, 且由X射线双晶衍射测试出的砷化镓(004)峰的半高宽只有210.6 arcsec。     

Si(111)衬底上HVPE GaN厚膜生长

在Si(111)衬底上,以MOCVD方法高温外延生长的AIN为缓冲层,使用氮化物气相外延(HVPE)方法外延生长了15Km的c面GaN厚膜.并利用X射线衍射(XRD)、光致发光谱(PL)、拉曼光谱(Raman)等技术研究了GaN厚膜的结构和光学性质.分析结果表明,GaN厚膜具有六方纤锌矿结构,外延层中存在的张应力较小,...     

Study of the correlation between GaN material properties and the growth conditions of radio frequency plasma-assisted molecular beam epitaxy

The material properties of GaN thin films grown by radio frequency (RF) nitrogen plasma source molecular beam epitaxy (MBE) on (0001) Al₂O₃ substrates have been correlated to the V/III flux ratio during GaN growth and to the type and thickness of the buffer layer. The most remarkable observation is the change in the sign of the residual strain, from tensile to compressive as the V/III ratio alters from N-rich to stoichiometric (or slightly Ga-rich) conditions for GaN layers with a 17 nm AlN buffer layer. The residual strain was significantly reduced for a thinner 5 nm AlN buffer and it was zero for a 20 nm GaN buffer. A reduction of the rms surface roughness from 20 to 3 nm was achieved by decreasing the V/III ratio. Finally, stacking faults were observed only for significantly N-rich growth conditions.     

Sequential structural characterization of layers in the GaN/AlN/SiC/Si(111) system by X-ray diffraction upon every growth stage

X-ray diffraction and transmission electron microscopy techniques have been used to study the dynamics of variation of the structural characteristics and deformation state in SiC, AlN, and GaN epilayers sequentially grown on a Si(111) substrate. In this system, the SiC layer has been grown by solid-phase epitaxy, while the AlN and GaN layers have been deposited by chloride-hydride vapor-phase epitaxy (HVPE) using argon as a carrier gas.     

Effects of thermal annealing in oxygen plasma for buffer layers on properties of ZnO thin films

ZnO thin films with ZnO buffer layers were grown by plasma-assisted molecular beam epitaxy (PA-MBE) on p-type Si(100) substrates. Before the growth of the ZnO thin films, the ZnO buffer layers were deposited on the Si substrates for 20 minutes and then annealed at the different substrate temperature ranging from 600 to 800 degrees C in oxygen plasma. The structural and optical properties of the ZnO thin films have been investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), and room-temperature (RT) photoluminescence (PL). A narrower full width at half maximum (FWHM) of the XRD spectra for ZnO(002) and a larger grain are observed in the samples with the thermal annealed buffer layers in oxygen plasma, compared to those of the as-grown sample. The surface morphology of the samples is changed from rugged to flat surface. In the PL spectra, near-band edge emission (NBEE) at 3.2 eV (380 nm) and deep-level emission (DLE) around 1.77 to 2.75 eV (700 to 450 nm) are observed. By increasing the annealing temperatures up to 800 degrees C, the PL intensity of the NBEE peak is higher than that of the as-grown sample. These results imply that the structural and optical properties of ZnO thin films are improved by the annealing process.     

The thermal treatment effects of CrN buffer layer on crystal quality of Zn-polar ZnO films

We report on the annealing effects of CrN buffer layers on the crystal quality of Zn-polar ZnO films grown by plasma assisted molecular beam epitaxy. The high-temperature (HT) annealing of CrN buffer layer improved the crystallinity of ZnO films. The full width at half maximums of (0002) and (10-11) ZnO ω-scan X-ray diffraction show 574 and 1296 arcsec, respectively, which show the 3 and 2 times narrower values than those of ZnO films without the annealing process. Moreover, the HT annealing can be effective method to improve the surface smoothness of ZnO film and reduce the crystal tilting.     

Chloride vapor-phase epitaxy of gallium nitride on silicon: Structural and luminescent characteristics of epilayers

The structure and luminescent properties of gallium nitride (GaN) epilayers grown by hydride-chloride vapor-phase epitaxy (HVPE) in a hydrogen or argon atmosphere on 2-inch Si(111) substrates with AlN buffer layers have been studied. The replacement of hydrogen atmosphere by argon for the HVPE growth of GaN leads to a decrease in the epilayer surface roughness. The ratio of intensities of the donor-acceptor and exciton bands in the luminescence spectrum decreases with decreasing growth temperature. For the best samples of GaN epilayers, the halfwidth (FWHM) of the X-ray rocking curve for the (0002) reflection was 420 sec of arc, and the FWHM of the band of exciton emission at 77 K was 48 meV.     

High quality epitaxial ZnO films grown on solid-phase crystallized buffer layers

High quality epitaxial ZnO films on sapphire (110) plane have been fabricated on ZnO homo-buffer layers crystallized via solid-phase epitaxially (SPE). The SPE-ZnO films are fabricated by annealing of amorphous ZnON (a-ZnON) films deposited by RF magnetron sputtering. During annealing, the a-ZnON films are oxidized and converted to ZnO crystal. X-ray diffraction (XRD) analysis shows that the resultant films are epitaxially grown on the sapphire substrates. By using the SPE-ZnO films as homo-buffer layers, the ZnO films with high crystallinity, which are deposited by RF magnetron sputtering, are fabricated. The full width at half-maximum of XRD patterns for 2θ-ω and ω scan of (002) plane are 0.094° and 0.12°, respectively, being significantly small compared with 0.24° and 0.55° for the films without buffer layers. Thus utilizing SPE buffer layers is very promising to obtain epitaxial ZnO films with high crystallinity.     

Growth of thin Ag films produced by radio frequency magnetron sputtering

Thin Ag films in the thickness range D = 14–320 nm were deposited by radio frequency magnetron sputtering on glass substrates at room temperature inside a vacuum chamber with base pressure of about 5 × 10^− 6 Pa. The growth of the films was studied via X-ray diffraction and atomic force microscopy experiments. The two techniques are complementary and give us the opportunity to study the surface roughness, the statistical distribution and the average value of the grain size, as well as the texture of the samples. It is shown that the film roughness increases negligibly within the first 60 atomic layers of growth. The thicker films (D 300 nm) develop a nanocrystalline structure with a root mean square roughness of about 2.5 nm. The grain size evolves linearly with the thickness from 9.4 nm at D = 54 nm to 31.6 nm at D = 320 nm.     

Ion beam synthesis of aluminium nitride: characterisation of thin AIN layers formed in microelectronics aluminium

Abstract

Buried AlN thin layers have been formed by high dose N⁺ ion implantation into microelectronics grade Al films (containing 1 at.-%Si), which were deposited on Si wafers. The structures obtained have been characterised by spreading resistance measurements, transmission electron microscopy, secondary ion mass spectrometry, X-ray diffraction, and X-ray photoelectron spectroscopy. The results show the formation of buried dielectric precipitates of crystalline AlN at implantation doses below the threshold and a continuous polycrystalline AlN layer at doses above the threshold. The AlN grains have the wurtzite structure, sizes of about 10–15 nm, and a preferred orientation in relation to the Al matrix, namely, <110>_AIN parallel to <110>_Al. The data also show that, under certain conditions, the main impurities (Si and O) are gettered in the buried layer. Moreover, for thin Al films, the formation of a Si rich surface layer is observed. This surface layer is formed by Si diffusion from the substrate, probably due to the penetration of N⁺ ions into the Si substrate. The distribution and evolution of these impurities and the different phases formed are studied as a function of the thickness and grain size of the Al film, as well as of the annealing processes.

MST/3304     

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.     

A novel approach for codoping in ZnO by AlN

In the present work, we have illustrated a new idea of codoping in ZnO with AlN as codopant to achieve p-ZnO. ZnO films doped with different concentrations of AlN were grown by RF magnetron sputtering. The AlN doped ZnO (ANZO) films grown on sapphire substrate were subjected to X-ray diffraction (XRD), reflectance measurements, Hall measurements, atomic force microscopy (AFM) and energy dispersive spectroscopy (EDS) analysis. XRD analysis reveals that all films have grown in the form of hexagonal wurtzite structure with (002) preferential orientation. The FWHM of (002) peak decreases till 1 mol% of AlN and increases for further addition of AlN indicating the incorporation of more impurities (dopants). The reflectance measurements suggest that the reflectance decreases at lower concentration and increases above 1 mol% of AlN in the visible region ranging from 400 to 800 nm. Hall measurements show that all the films are n-type. The electron concentration increases initially and then decreases for further addition of AlN (>1 mol%) suggesting the incorporation of nitrogen into the film at higher concentrations of AlN. The presence of N in the films is further confirmed by EDS analysis. The rms surface roughness measured by AFM decreases exponentially with dopant concentration. The figure of merit increases upon codoping with AlN.     

Structural properties of GaN grown on AlGaN/AlN stress mitigating layers on 100-mm Si (111) by ammonia molecular beam epitaxy

The structural properties of GaN grown on AlGaN/AlN stress mitigating layers on 100-mm diameter Si (111) substrate by ammonia molecular beam epitaxy have been reported. High resolution X-ray diffraction, micro-Raman spectroscopy, transmission electron microscopy and secondary ion mass spectroscopy have been used to study the influence of AlN thickness and AlGaN growth temperature on the quality of GaN. GaN grown on thicker AlN showed reduced dislocation density and lesser tensile strain. Three-dimensional growth regime was observed for GaN grown at lower AlGaN growth temperature while higher AlGaN growth temperature resulted in two-dimensional growth mode. The dislocation bending and looping at the AlGaN/AlN interface was found to have significant influence on the dislocation density and strain in the GaN layer. The evolution and interaction of threading dislocations play a major role in determining the quality and the strain states of GaN.