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Electrical, structural, and optical properties of a free-standing 200 μm thick n-type GaN template grown by hydride vapor phase epitaxy have been investigated. Hall mobilities of 1100 and 6800 cm 2 /V s have been obtained at room temperature and 50 K, respectively. Quantitative analysis of acceptor concentration, donor concentration and donor activation energy has been conducted through simultaneous fitting of the temperature dependent Hall mobility and carrier concentration data which led to a donor concentration of 2.10×10 16 cm −3 and an acceptor concentration of 4.9×10 15 cm −3 . The resultant donor activation energy is 18 meV. The analysis indicates that the dominant scattering mechanism at low temperatures is by ionized impurities. The extended defect concentrations on Ga- and N-faces were about 5×10 5 cm −2 for the former and about 1×10 7 cm −2 for the latter, as revealed by a chemical etch. The full width at half maximum of the symmetric (0 0 0 2) X-ray diffraction peak was 69″ and 160″ for the Ga- and N-faces, respectively. That for the asymmetric (10–14) peak was 103″ and 140″ for Ga- and N-faces, respectively. The donor bound exciton linewidth as measured on the Ga- and N-face (after a chemical etch 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 2.45 eV.

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 potentials for Ga-face and N-face regions are 125610 and 230610 mV, respectively, with respect to the sapphire substrate, where the sign is consistent with Ga- and N-polarity GaN under compressive strain due to thermal mismatch with the sapphire substrate.

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.

A free-standing GaN template grown by hydride vapor phase epitaxy has been characterized by transmission electron microscopy ~TEM!. The TEM investigation was augmented by x-ray diffraction, defect delineation etching process followed by imaging with atomic force microscopy and variable temperature photoluminescence. The density of dislocations near the N face was determined to be, in order, 3613107, 4613107, and about 13107 cm22 by cross-sectional TEM, plan-view TEM, and a defect revealing etch, respectively. The same methods on the Ga face revealed the defect concentration to be, in order, less than 13107 cm22 by plan-view TEM, less than 53106 cm22 by cross-sectional TEM, and 53105 cm22 by defect revealing hot H3PO4 acid, respectively. 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 (101I4) peak was 103 and 140 arc sec for Ga and N faces, respectively. The donor bound exciton linewidth was about 1meV each at 10 K, and a green band centered at about 2.44 eV was observed.

We have fabricated GaN quantum dots (QDs) in AlN confined layer structures by molecular beam epitaxy. The size distribution and density of the QDs have been estimated from an atomic force microscopy study. Very high quantum efficiency of photoluminescence (PL) has been obtained in some samples with QDs. Compared to the GaN bulk samples, it increased by orders of magnitude. In some samples the quantum size effect dominated, resulting in the blue-shift of the QD related PL peak, whereas in the samples with larger dots a red-shift up to 0.8 eV has been observed, which is related to strong polarization effects. We have observed a blue-shift of the PL peak with excitation intensity in the samples with large dots due to screening effect. The temperature-induced quenching of PL occurs at higher temperatures compared to bulk GaN due to the confinement of nonequilibrium carriers in the QDs. An excited state has been observed in some samples.

Structural, electrical and optical properties of free-standing 200-µm thick GaN films grown by hydride vapor phase epitaxy (HVPE) have been investigated. After laser lift-off, the GaN substrates were mechanically polished on both Ga and N-sides and dry etched only on the Ga side to obtain a smooth epi-ready surface. Hot H3PO4 chemical etching on both surfaces was used to reveal the defect sites, which appeared as hexagonal pits. The etched surfaces were then examined by atomic force microscopy.

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.

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.

The availability of reliable and quick methods to investigate defects in GaN films is of great interest. Photo-electrochemical (PEC), and hot wet etching using both H3PO4 acid and molten KOH have been used to study structural defects in GaN layers grown by hydride vapor phase epitaxy and molecular beam epitaxy. The purpose of this work is to determine whether, and under what conditions, these different methods of investigation are consistent and to get to a more accurate estimation of the defect density. As-grown and etched surfaces were investigated by atomic force microscopy (AFM), and plan-view and cross-sectional transmission electron microscopy (TEM).

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.

Inversion domains (IDs) in III-nitride semiconductors degrade the performance of such devices, and so their identification and elimination is critical.An inversion domain on a Ga- polarity samples appears as an N-polarity domain, which has a polarization reversed with respect to the rest of the surface and therefore has a different surface potential. Surface-contact-potential electric force microscopy (SCP-EFM) is an extension of atomic force microscopy (AFM) that allows imaging of the surface electrostatic potential. Previously, we established the particular mode of operation necessary to identify inversion domains on III-nitrides using a control sample. We have now studied inversion domains in GaN films grown by metalorganic chemical vapor deposition (MOCVD) and molecular beam epitaxy (MBE). The existence of inversion domains was also verified by transmission electron microscopy (TEM) using multiple dark field imaging. In MOCVD grown GaN, we found predominant Ga-polarity with very low density of IDs, while in the MBE GaN, a mix polarity feature was identified.

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 3Å bi-layer steps. Hot H3PO4 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 (9×108 - 2 ×109 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.

Stress induced piezoelectric fields in III-nitride semiconductors induce charge at the surface that is comparable to the free carrier concentration intended by doping. These fields, coupled with mixed Ga-polarity and N-polarity within the film, are detrimental to device performance due to an additional scattering caused by a reversal of the electric field normal to the surface. Consequently, investigation of the polarization effects is important and timely as nitride semiconductor devices are being contemplated for system applications. By imaging the surface potential by electric force microscopy (EFM), both a qualitative and a quantitative measure of polarization induced charge distribution across the surface could be obtained. In this vein, we undertook an EFM study in a series of samples. EFM images of as-grown and progressively etched samples not only led to the identification and imaging of inversion domains, but also showed the evolution of different polarities. The polarization of the surface was calculated and was found to agree reasonably well with the values found experimentally. The role of polarization was addressed by extraction of the second harmonic term from EFM signal.

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)].

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.

Photoenhanced electro-chemical (PEC) wet etching has been shown to be suitable for dislocation-density estimation in n-GaN films as well as for GaN-based device fabrication. We report on PEC etching of n-GaN samples grown by MBE and HVPE methods in unstirred aqueous KOH solution under He-Cd laser illumination. Characterization of the etched samples was carried out using atomic force microscopy (AFM) in both cross-sectional and plan-view configurations and scanning electron microscopy (SEM). At moderate illumination densities, the SEM and AFM analyses reveal sub-100 nm scale threading vertical wires on the etched surfaces. The calculated density (∼1×10 9cm−2) is in agreement with dislocation density found by transmission electron microscopy. Using cross-sectional AFM, we find that these vertical wires are ∼1[.proportional]m high and are perpendicular to the sapphire surface. Applying a higher illumination density or an external voltage, we obtain a higher etch rate with a smooth free-feature etched surface. Some highly resistive samples that cannot be etched under normal conditions because the band bending is too small to confine the holes to the surface for them to participate in the PEC process, can be etched with the application of a voltage to the sample. In this case, the etch rate depends on both the polarity and the magnitude of the voltage applied. In an MBE-grown sample with an AlN/GaN superstructure inside, we report on high selectivity between AlN and GaN (AlN is an etch stop); the selectivity is due to the etching mechanism of the PEC process.