K. M. Jones

Dislocation density in GaN determined by photoelectrochemical and hot-wet etching

Defects in GaN layers grown by hydride vapor-phase epitaxy have been investigated by photoelectrochemical (PEC) etching, and by wet etching in hot H3PO4 acid and molten potassium hydroxide (KOH). Threading vertical wires (i.e., whiskers) and hexagonal-shaped etch pits are formed on the etched sample surfaces by PEC and wet etching, respectively. Using atomic-force microscopy, we find the density of “whisker-like” features to be 2×109 cm−2, the same value found for the etch-pit density on samples etched with both H3PO4 and molten KOH. This value is comparable to the dislocation density obtained in similar samples with tunneling electron microscopy, and is also consistent with the results of Youtsey and co-workers [Appl. Phys. Lett. 73, 797 (1998); 74, 3537 (1999)].

Dependence of GaN polarity on the parameters of the buffer layer grown by molecular beam epitaxy

The polarity of GaN films grown using GaN and AlN buffer layers on sapphire substrates by molecular beam epitaxy were investigated by atomic force microscopy, hot wet chemical etching, and reflection high-energy electron diffraction. We found that the GaN films grown on high temperature AlN (>890 °C) and GaN (770–900 °C) buffer layers invariably show Ga and N polarity, respectively. However, the films grown using low temperature (∼500 °C) buffer layers, either GaN or AlN, could have either Ga or N polarity, depending on the growth rate of the buffer layer.

Investigation of inversion domains in GaN by electric-force microscopy

Inversion domains in III-nitride semiconductors degrade the performance of devices fabricated in them. Consequently, it is imperative that we understand their electrostatic manifestation, the growth conditions under which such domains form, and an effective means of their identification. In what is nominally referred to as Ga-polarity samples, N-polarity domains have a polarization that is reversed with respect to the remainder of the surface, and therefore, have a different potential under strain. We have used surface-potential electric-force microscopy (SP-EFM) to image the electrostatic surface potential of GaN grown on sapphire, which is strained due to the thermal mismatch between the substrate and GaN. Employing a control sample with side-by-side Ga- and N-polarity regions, we have established the EFM mode necessary to identify inversion domains on GaN samples grown by molecular-beam epitaxy. This method is not sensitive to topology and has a spatial resolution of under 100 nm. The measured surface ...

Characteristics of free-standing hydride-vapor-phase-epitaxy-grown GaN with very low defect concentration

A free-standing 300-μm-thick GaN template grown by hydride vapor phase epitaxy has been characterized for its structural and optical properties using x-ray diffraction, defect delineation etch followed by imaging with atomic force microscopy, and variable temperature photoluminescence. The Ga face and the N face of the c-plane GaN exhibited a wide variation in terms of the defect density. The defect concentrations on Ga and N faces were about 5×105 cm−2 for the former and about 1×107 cm−2 for the latter. The full width at half maximum of the symmetric (0002) x-ray diffraction peak was 69 and 160 arc sec for the Ga and N faces, respectively. That for the asymmetric (10–14) peak was 103 and 140 arc sec for Ga and N faces, respectively. The donor bound exciton linewidth as measured on the Ga and N faces (after a chemical etching to remove the damage) is about 1 meV each at 10 K. Instead of the commonly observed yellow band, this sample displayed a green band, which is centered at about 2.44 eV.

Growth of Ag rows on Si(5 5 12)

Our scanning tunneling microscopy studies show that Ag deposited onto Si(5 5 12) and annealed to moderate temperatures (400–450 °C) forms well-ordered overlayer rows. These rows have aspect ratios up to 150:1 and therefore are possible candidates as “nanowires.” As the Ag coverage is increased, the rows grow in length and number until the surface forms a periodic array of such structures at ∼0.25 monolayer (ML). A statistical analysis of these rows reveals a linear increase in median row length as a function of coverage with a median length of 67 nm at full coverage (∼0.25 ML). At higher annealing temperatures (>500 °C), Ag continues to form row-like structures, but the rows are wider and cause local faceting of the underlying Si substrate. We can therefore conclude that the lower temperature Ag rows are actually a metastable arrangement of the surface.

STM studies of 1-D noble metal growth on silicon

Our scanning tunneling microscopy (STM) studies show that noble metals (Ag, Au) form a wide variety of 1-D structures on the high-index Si(5 5 12) surface. At coverages below 0.25 monolayer (ML), both metals grow as overlayer rows with an inter-row spacing of approximately 5 nm. At higher coverages and annealing temperatures, the underlying Si reconstruction is removed, but periodic row structures persist. Au can also induce faceting to nearby planes, e.g. (7 7 15) and (2 2 5), at temperatures above 500 degrees C. For all coverages and annealing temperatures studied here (0.02-1 ML, 450-800 degrees C), the Si(5 5 12) template initiates 1-D growth of the deposited noble metals.

Highly selective photoelectrochemical etching of nitride materials for defect investigation and device fabrication

Photoenhanced electrochemical (PEC) etching in an unstirred KOH solution under He–Cd laser illumination was used for delineating extended defects in GaN films. When a low-excitation intensity was employed, the process yielded threading vertical features at dislocation sites. Application of an external voltage or a higher-illumination intensity led to high-etch rates with smooth surfaces. Some highly resistive samples, for which no etching was obtained under normal etching conditions, could be etched with the application of a single-polarity external voltage. Finally, in a GaN sample with an AlN/GaN superstructure inside, high selectivity between AlN and GaN was achieved; in this case, the PEC process stopped at the thin AlN stop layer.

Investigation of Buffer Layers for GaN Grown by MBE

The structural quality of the buffer layer juxtaposed to the substrate is pivotal in attaining high quality GaN layers. In MBE deposition, low temperature, medium temperature and high temperature AlN buffer layers are at the disposal of the grower. There are quite a few reports, some discussing the benefits of high temperature buffer layers and others doing the same for low temperature buffer layers. The reports emanate from different laboratories; and due to stringent parameter control required, it is difficult to compare one type of buffer with another. To gain some insight, we undertook an investigation wherein these varieties of buffer layers were grown on nitridated sapphire substrate under similar conditions for a comparative analysis. In addition to the single buffer layers of both GaN and AlN varieties, some combinations of stacked buffer layers, including cases where these buffer layers were separated by GaN layers, were employed. Structural analysis by high resolution X-ray diffractometry and topological analysis by AFM were carried out to assess the quality of the epilayers grown on these buffers. Hall measurements at room temperature were carried out to characterize the electrical transport properties.

Recombination at surface states in GaN

We have studied radiative and nonradiative recombination at surface states in GaN, including as-grown samples and those treated with acids or bases. The surface states manifested themselves in two ways: (i) a reversible increase of the photoluminescence (PL) intensity after ultraviolet (UV) illumination in vacuum and (ii) appearance of new PL bands after treatment with acid or base and subsequent exposure to air. It has been established that the GaN surface physi-sorbs species from air (presumably oxygen) which induce surface states acting as nonradiative recombination centers. It has been found that nonradiative recombination of photogenerated carriers via surface states comprises more than 70% of the recombination in some GaN samples. Another type of the surface state, which participates in radiative recombination, has been found in GaN samples with Ga polarity after brief etching of the surface with hot acid or base and subsequent exposure to air. In such samples, a broad PL band emerges in the blue region of the spectrum at low temperatures. The blue band has been attributed to transitions of photogenerated electrons from donors in the near-surface depletion region to the surface states introduced by the above-mentioned procedure. The changes in the GaN surface caused by etching were examined by atomic force microscopy. In some samples the blue band appeared even when no evidence of the layer etching was found except for quite shallow etch pits formed at dislocation sites. The emerging blue band can be related to the surface states formed on the a -planes of etch pits.

Structural, optical and electrical properties of GaN films grown by metalorganic chemical vapor deposition on sapphire.

Properties of GaN layers grown by metalorganic chemical vapor deposition (MOCVD) on c-plane of sapphire have been investigated using atomic force microscopy (AFM), wet etching for defect investigation, transmission electron microscopy (TEM), high-resolution X-ray diffraction, Hall effect measurements and low-temperature photoluminescence (PL). Tapping-mode AFM images of the as-grown samples showed atomically smooth surfaces (rms roughness ≍ 0.2 nm) consisting of terraces separated by about 3A bi-layer steps. Hot H 3 PO 4 chemical etching was used to produce hexagonal-shaped etch pits at the surface defect sites as revealed by AFM imaging. The obtained etch pit densities (9×10 8 - 2 ×10 9 cm −2 ) were in agreement with the dislocation density found by plan-view and cross-sectional TEM observations. The full-width at half-maximum (FWHM) of the X-ray diffraction rocking curve was about 4.8 and 3.9 arcmin for the symmetric (002) and asymmetric (104) directions, respectively. PL spectrum at 15 K demonstrated sharp peaks (FWHM ≍ 4 meV) in the excitonic region, which were attributed to free and bound excitons. The spectrum contained also weak PL bands with maxima at about 2.2, 2.9 and 3.27 eV, which have been attributed to three different acceptors.