Practical interpretation of X-ray rocking curves from semiconductor heteroepitaxial layers

X-ray rocking curves are widely used to study semiconductor heteroepitaxial structures. Examples are given of the use of rocking curves to investigate crystal growth problems, determine layer growth rates, confirm layer thicknesses and to determine the state of relaxation in layers which are above the critical thickness. The application of dynamic simulation and Fourier transformation to the raw data as tools to interpret data from multilayer structures is discussed.     

X-ray rocking curves on inhomogeneous surface layers on Si single crystals

In this paper are studied the possibilities of investigating the structure of B⁺ -implanted Si single crystals by measuring X-ray rocking curves (the Bragg case). From the viewpoint of the dynamical diffraction of X-rays the structure of an implanted layer is described by a depth-profile of the statistical disorder of the layer structure and by a depth-profile of the relative change in the specific volume. These quantities take place in a modified form of the Takagi equations which are numerically computed for various values of the parameters of the layer, in order to trace their influence to the shape of the rocking curve. A great amount of free parameters and the complexity of their influence on the rocking curves make it impossible to fit the experimental and theoretical curves. On the basis of the theoretical study of the rocking curves the experimental curves measured on Si samples (dose 5×10¹⁵ cm^–2 of B⁺, energy 50–200 keV) are interpreted qualitatively.     

X-ray rocking curves on inhomogeneous surface layers on Si single crystals

Two cases of inhomogeneous surface layers are considered — diffusion layers as well as implanted layers. The parameters of the layers are investigated by means of an X-ray rocking curve analysis. In this paper the concentration profile of a diffusion layer in Si is determined from X-ray rocking curves, the rocking curves on implanted layers will be discussed in the next paper. A graph is constructed for determining approximate values of surface concentrationC ₀ and diffusion lengthL from subsidiary maxima on the X-ray rocking curve. The dependence of the shape of the rocking curves on the type of the concentration profile and on the values ofC ₀ andL was shown. The influence of crystal thickness and curvature is studied theoretically and experimentally. As an example of using this method a rocking curve of a crystal with a boron diffusion layer is measured and the parameters of the concentration profile are determined. The parameters found are proved by multiplied measurement of rocking curves after anodic oxidation and by comparing these rocking curves with theoretical ones.     

Structural perfection of GaN epitaxial layers according to x-ray diffraction measurements

Two-and three-crystal diffractometric study of the structural perfection of GaN epitaxial films grown on sapphire, GaAs, and SiC substrates is reported. The diffraction intensity distributions around the reciprocal-lattice points are shown to be extended in the direction parallel to the surface, which is connected with the anisotropy of the local strain fields in the layers. A comprehensive analysis is made of the broadening for several reflection orders measured in three geometries, namely, Bragg, symmetric Laue, and grazing-angle diffraction. The five independent components of the microdistorsion tensor δe _ij , as well as the average coherent-scattering lengths in two directions, τ _z and τ _x , have been obtained. It is shown that for most samples the components responsible for reflection broadening along the surface are noticeably larger, i.e. δe _xx >δe _zz , and δe _zx >δe _xz , as well as τ _z >τ _x . All tensor components are related to a specific dislocation type. Electron microscopy of the samples revealed a high density of pure edge and pure screw dislocations extending normal to the interface, and which provide a dominant contribution to e _xx and e _zx , respectively. Fiz. Tverd. Tela (St. Petersburg) 41, 30–37 (January 1999)     

Structural properties of GaN(0001) epitaxial layers revealed by high resolution X-ray diffraction

High-resolution X-ray diffraction has been used to analyze GaN(0001) epitaxial layers on sapphire substrates. Several structural properties of GaN, including the lattice constants, strains, and dislocation densities are revealed by the technique of X-ray dffraction (XRD). Lattice constants calculated from the omega/2theta scan are c=0.5185 nm and a=0.3157 nm. Also, the in-plane strain is -1.003%, while out of the plane, the epitaxial film is almost relaxed. Several methods are used to deduce the mosaicity a...     

Defect structure of epitaxial layers of III nitrides as determined by analyzing the shape of X-ray diffraction peaks

The shape of X-ray diffraction epitaxial layers with high dislocation densities has been studied experimentally. Measurements with an X-ray diffractometer were performed in double- and triple-crystal setups with both CuK _α and MoK _α radiation. Epitaxial layers (GaN, AlN, AlGaN, ZnO, etc.) with different degrees of structural perfection grown by various methods on sapphire, silicon, and silicon carbide substrates have been examined. The layer thickness varied in the range of 0.5–30 μm. It has been found that the center part of peaks is well approximated by the Voigt function with different Lorentz fractions, while the wing intensity drops faster and may be represented by a power function (with the index that varies from one structure to another). A well-marked dependence on the ordering of dislocations was observed. The drop in intensity in the majority of structures with a regular system and regular threading dislocations was close to the theoretically predicted law Δθ^–3; the intensity in films with a chaotic distribution decreased much faster. The dependence of the peak shape on the order of reflection, the diffraction geometry, and the epitaxial layer thickness was also examined.     

Formation of mismatched layers in pentagonal nanorods

A new mechanism is presented to model the relaxation phenomena in pentagonal nanorods (PNRs) – elongated multiple twinned crystals. It is demonstrated that a shell possessing crystal mismatch with respect to the PNR core region will reduce the internal energy of the PNR associated with wedge disclinations of strength 7°20′ lying along the PNR axis. We predict the existence of an optimal magnitude for core/shell crystal lattice mismatch and an optimal shell thickness providing maximum energy release for this mechanism of mechanical stress relaxation. The considered relaxation mechanism can be realized by the diffusion of impurities in the shell region without change of the PNR radius or by growth of a thin mismatched shell layer with the corresponding thickening of PNR. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Investigation of X-ray diffraction limitations upon the analysis of tellurium-atom injection into GaAs epitaxial layers

GaAs lattice “superdilation” caused by an introduced tellurium impurity, which is well known in publications, is experimentally studied. This phenomenon consists in the fact that the GaAs-lattice dilation can be more than 10 times greater than expansion that would appear upon the replacement of arsenic atoms with tellurium atoms if calculations are performed using the current-carrier concentration and Vegard’s law. The given phenomenon has already been observed at n _Te > 3 × 10¹⁸ cm^–3. A series of GaAs epitaxial layers heavily doped with tellurium and grown via metal-organic chemical vapor deposition are investigated using high-resolution X-ray diffractometry (HRXRD), secondary-ion mass spectrometry (SIMS), and the Hall effect. It is demonstrated that, despite a high Te concentration (10²⁰?10²¹ cm^–3) in the layer and variations in the growth conditions, the concentration estimates based on HRXRD data depend linearly on the results of elemental analysis performed by means of SIMS. The GaAs lattice expands even somewhat slighter as compared to the case where arsenic atoms are replaced with all Te atoms injected into the layer. At the same time, the Hall carrier concentration decreases sharply beginning at 2 × 10²⁰ cm^–3. In accordance with the obtained results, the examined phenomenon can be interpreted as the strong compensation of donor and acceptor carriers rather than as superdilation.     

Crystallite misorientation analysis in semiconductor wafers and ELO samples by rocking curve imaging

Rocking curve imaging is based on measuring a series of Bragg-reflection digital topographs by monochromatic parallel-beam synchrotron radiation in order to quantify local crystal lattice rotations within a large surface area with high angular and high spatial resolution. In this paper we apply the method to map local lattice tilts in two distinct semiconductor sample types with lattice misorientations up to 0.5° and with spatial resolution from 30  down to 1 . We analyse the measured surface-tilt data volumes for samples with almost smoothly varying specific misoriented defect formation in GaAs wafers and for an inherent subsurface grain structure of epitaxial lateral overgrowth wings in GaN. Back-projected tilt maps and histograms provide both local and global characteristics of the microcrystallinity.     

Characterization of oxide layers formed on electrochemically treated Ti by using soft X-ray absorption measurements

The oxide layers of electrolytic oxidized titanium (Ti) were characterized using Ti L_2,3 and O K edge X-ray absorption. The spectra show that the structure of the oxide layers that are formed during a 1 min treatment are dependent on the concentration of the electrolyte (H₂SO₄ or Na₂SO₄) with which the Ti surface was treated, and also on the magnitude of the potential that was applied during the anodic oxidation process (100 V or 150 V). It is found that a potential of 150 V and an electrolyte concentration of 0.5 M or 1.0 M produces a layer of TiO₂ having rutile crystal structure.     

Photoconductive response of GaAs epitaxial layers

In the present work the photoconductive response of low resistivity, n-type GaAs epitaxial layers is studied by experimentally monitoring the dependence of the photoconductive gain (PG) optoelectronic parameter upon incident photon flux and temperature. The characterized samples fall into three major categories: ion implanted (II) GaAs epilayers formed within undoped, semi-insulating GaAs substrates; GaAs epitaxial layers grown by liquid phase epitaxy (LPE) on Cr-doped, semi-insulating GaAs substrates; and ungated GaAs MESFETs.     

Elastic strain determination in semiconductor epitaxial layers by HREM

A new technique that is independent of image contrast and robust to the presence of experimental noise is presented to analyze strains from high resolution electron microscopy (HREM) lattice images. This approach involves the analysis of the cumulative sum of deviations (CUSUM) in lattice-fringe spacings from a target value. The effects of surface roughness at an interface, and surface relaxation due to transmission electron microscope (TEM) sample preparation are discussed. The CUSUM method was applied to two simulated and two experimental HREM images of semiconductor strained layer structures in [ ] zone axis projection. The CUSUM technique was able to accurately reproduce the strain profiles from the simulated and experimental images in all cases studied except for the component of the strain in the slip direction (e_xx) of an edge dislocation in a simulated image. In this case, the strain field near the core appeared hemispherical rather than lobed as expected.     

Investigation of 4H-SiC epitaxial layers implanted by Al ions

4H-SiC epitaxial layers 26 μm thick with N _d ?N _a = 1 × 10¹⁵ cm^?3 grown by the CVD method on 4H-SiC commercial wafers were implanted by Al ions with energy of 100 keV and a dose of 5 × 10¹⁶ cm^?2. To produce the p ⁺?n junction, a rapid thermal annealing for 15 s at 1700°C was used. The obtained samples were studied by the local cathodoluminescence, X-ray diffractometry, and transmission electron microscopy. It was established that under specified conditions of implantation, the width of a region with a high content of radiation defects exceeded by two orders of magnitude, the depth of the projective range of Al ions and was equal to 40 μm. This result is explained by the combined contribution of the radiation enhanced defect diffusion and long-range action effect. A short-term high-temperature annealing resulted in the recrystallization of the specimen surface layer and enhancement of CVD layer structure.     

EBIC investigations of GaN layers prepared by epitaxial lateral overgrowth

GaN films prepared by lateral overgrowth are investigated by scanning electron microscopy in the electron beam induced current (EBIC) mode. A comparison of experimental and simulated dependences of induced current on beam energy has allowed us to determine not only the diffusion length, but also the donor concentration in different areas of a film. It has been found that the donor distribution is inhomogeneous and this inhomogeneity increases under fast neutron irradiation. This is indicative of the significant influence of structural defects on the rate of radiation defect accumulation. An anomalously slow signal decay outside the Schottky barrier has been found, which can be determined by charged defects formed at the merger boundary.     

Growth of gallium nitride epitaxial layers and applications

The lack of appropriate substrates has delayed the realisation of devices based on IIInitrides. Currently, the heteroepitaxial growth of GaN by metal organic vapour phase epitaxy (MOVPE) produces GaN layers which, despite huge densities of dislocations, allow the fabrication of highly efficient optoelectronic devices. Henceforth, a new technology in heteroepitaxy of GaN, the epitaxial lateral overgrowth (ELO) has produced GaN layers in which the density of dislocations has been reduced by several orders of magnitude. With the ELO, nitride based laser diodes (LDs) working at room temperature in cw mode with a lifetime of 10,000 hours have been demonstrated by Nichia. In addition to LDs, IIInitrides presently offer a wide range of applications in optoelectronics (high brightness light emitting diodes (LEDs), from amber to UV, solar blind detectors); in electronics, high temperature/high power field effect transistors (FETs). The development of molecular beam epitaxy (MBE) of nitrides has been hindered during several years by the lack of an efficient nitrogen source. This problem being solved, MBE has recently demonstrated state-of-theart quantum well and quantum dot heterostructures, and 2D electron gas heterostructures.     

On the use of an external reference sample in the X-ray diffraction analysis of epitaxial layers

The differences in the high-resolution X-ray patterns for measurement of the crystal-lattice constant with and without the use of an external reference sample are discussed. The calculation procedures in the measurement of the lattice constant are compared. The results of the measurements of a Si(111) test crystal using a Bruker D8 Discover diffractometer are presented, and the examples of the use of this crystal as an external reference are described.     

Incorporation of hydrogen in CdTe and HgTe epitaxial layers grown by MOCVD

The incorporation of hydrogen into MOCVD-grown layers of CdTe, HgTe and CdHgTe using H₂ as the vector gas has been studied. Concentrations of incorporated H going from 6.5 × 10¹⁷ cm^-3 to 5 × 10¹⁸ cm^-3 have been found by SIMS in CdTe layers. This concentration decreases with increasing growth temperature and decreasing bond strength of the host material.     

Determination of elastic moduli of GaN epitaxial layers by microindentation technique

It is demonstrated that Young’s modulus of epitaxial gallium nitride layers can be determined by the microindentation of their growth surface. The technique is based on the solution of the Hertz problem for the elastic indentation of a steel sphere into the studied surface. It is established that the isotropic approximation applied in this case is justified and leads to the satisfactory results. The microhardness measurements of epitaxial layers are carried out.