Publications

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We developed a pyrometer that operates near the high-temperature bandgap of GaN, thus solving the transparency problem once a {approx} 1 {micro}m thick GaN epilayer has been established. The system collects radiation in the near-UV (380-415 nm) and has an effective detection wavelength of {approx}405 nm. By simultaneously measuring reflectance we also correct for emissivity changes when films of differing optical properties (e.g. AlGaN) are deposited on the GaN template. We recently modified the pyrometer hardware and software to enable measurements in a multiwafer Veeco D-125 OMVPE system. A method of synchronizing and indexing the detection system with the wafer platen was developed; so signals only from the desired wafer(s) could be measured, while rejecting thermal emission signals from the platen. Despite losses in optical throughput and duty cycle we are able to maintain adequate performance from 700 to 1100 C.

The AlGaInN material system is used for virtually all advanced solid state lighting and short wavelength optoelectronic devices. Although metal-organic chemical vapor deposition (MOCVD) has proven to be the workhorse deposition technique, several outstanding scientific and technical challenges remain, which hinder progress and keep RD&A costs high. The three most significant MOCVD challenges are: (1) Accurate temperature measurement; (2) Reliable and reproducible p-doping (Mg); and (3) Low dislocation density GaN material. To address challenge (1) we designed and tested (on reactor mockup) a multiwafer, dual wavelength, emissivity-correcting pyrometer (ECP) for AlGaInN MOCVD. This system simultaneously measures the reflectance (at 405 and 550 nm) and emissivity-corrected temperature for each individual wafer, with the platen signal entirely rejected. To address challenge (2) we measured the MgCp{sub 2} + NH{sub 3} adduct condensation phase diagram from 65-115 C, at typical MOCVD concentrations. Results indicate that it requires temperatures of 80-100 C in order to prevent MgCp{sub 2} + NH{sub 3} adduct condensation. Modification and testing of our research reactor will not be complete until FY2005. A new commercial Veeco reactor was installed in early FY2004, and after qualification growth experiments were conducted to improve the GaN quality using a delayed recovery technique, which addresses challenge (3). Using a delayed recovery technique, the dislocation densities determined from x-ray diffraction were reduced from 2 x 10{sup 9} cm{sup -2} to 4 x 10{sup 8} cm{sup -2}. We have also developed a model to simulate reflectance waveforms for GaN growth on sapphire.

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Optical reflectance and atomic force microscopy (AFM) are used to develop a detailed description of GaN nucleation layer (NL) evolution upon annealing in ammonia and hydrogen to 1050°C. For the experiments, the GaN NLs were grown to a thickness of 30nm at 540°C, and then heated to 1050°C, following by holding at 1050°C for additional time. As the temperature, T, is increased, the NL decomposes uniformly beginning at 850°C up to 980°C as observed by the decrease in the optical reflectance signal and the absence of change in the NL AFM images. Decomposition of the original NL material drives the formation of GaN nuclei on top of the NL, which begin to appear on the NL near 1000°C, increasing the NL roughness. The GaN nuclei are formed by gas-phase transport of Ga atoms generated during the NL decomposition that recombine with ambient NH3. The gas-phase mechanism responsible for forming the GaN nuclei is demonstrated in two ways. First, the NL decomposition kinetics has an activation energy, EA, of 2.7 eV and this EA is observed in the NL roughening as the GaN nuclei increase in size. Second, the power spectral density functions measured with atomic force microscopy reveal that the GaN nuclei grow via an evaporation and recondensation mechanism. Once the original NL material is fully decomposed, the GaN nuclei stop growing in size and begin to decompose. For 30 nm thick NLs used in this study, approximately 1/3 of the NL Ga atoms are reincorporated into GaN nuclei. A detailed description of the NL evolution as it is heated to high temperature is presented, along with recommendations on how to enhance or reduce the NL decomposition and nuclei formation before high T GaN growth. © 2004 Elsevier B.V. All rights reserved.

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This SAND report is the final report on Sandia's Grand Challenge LDRD Project 27328, 'A Revolution in Lighting -- Building the Science and Technology Base for Ultra-Efficient Solid-state Lighting.' This project, which for brevity we refer to as the SSL GCLDRD, is considered one of Sandia's most successful GCLDRDs. As a result, this report reviews not only technical highlights, but also the genesis of the idea for Solid-state Lighting (SSL), the initiation of the SSL GCLDRD, and the goals, scope, success metrics, and evolution of the SSL GCLDRD over the course of its life. One way in which the SSL GCLDRD was different from other GCLDRDs was that it coincided with a larger effort by the SSL community - primarily industrial companies investing in SSL, but also universities, trade organizations, and other Department of Energy (DOE) national laboratories - to support a national initiative in SSL R&D. Sandia was a major player in publicizing the tremendous energy savings potential of SSL, and in helping to develop, unify and support community consensus for such an initiative. Hence, our activities in this area, discussed in Chapter 6, were substantial: white papers; SSL technology workshops and roadmaps; support for the Optoelectronics Industry Development Association (OIDA), DOE and Senator Bingaman's office; extensive public relations and media activities; and a worldwide SSL community website. Many science and technology advances and breakthroughs were also enabled under this GCLDRD, resulting in: 55 publications; 124 presentations; 10 book chapters and reports; 5 U.S. patent applications including 1 already issued; and 14 patent disclosures not yet applied for. Twenty-six invited talks were given, at prestigious venues such as the American Physical Society Meeting, the Materials Research Society Meeting, the AVS International Symposium, and the Electrochemical Society Meeting. This report contains a summary of these science and technology advances and breakthroughs, with Chapters 1-5 devoted to the five technical task areas: 1 Fundamental Materials Physics; 2 111-Nitride Growth Chemistry and Substrate Physics; 3 111-Nitride MOCVD Reactor Design and In-Situ Monitoring; 4 Advanced Light-Emitting Devices; and 5 Phosphors and Encapsulants. Chapter 7 (Appendix A) contains a listing of publications, presentations, and patents. Finally, the SSL GCLDRD resulted in numerous actual and pending follow-on programs for Sandia, including multiple grants from DOE and the Defense Advanced Research Projects Agency (DARPA), and Cooperative Research and Development Agreements (CRADAs) with SSL companies. Many of these follow-on programs arose out of contacts developed through our External Advisory Committee (EAC). In h s and other ways, the EAC played a very important role. Chapter 8 (Appendix B) contains the full (unedited) text of the EAC reviews that were held periodically during the course of the project.

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Cantilever epitaxy (CE) has been developed to produce GaN on sapphire with low dislocation densities as needed for improved devices. The basic mechanism of seeding growth on sapphire mesas and lateral growth of cantilevers until they coalesce has been modified with an initial growth step at 950 C. This step produces a gable with (11{bar 2}2) facets over the mesas, which turns threading dislocations from vertical to horizontal in order to reduce the local density above mesas. This technique has produced material with densities as low as 2-3x10{sup 7}/cm{sup 2} averaged across extended areas of GaN on sapphire, as determined with AFM, TEM and cathodoluminescence (CL). This density is about two orders of magnitude below that of conventional planar growths; these improvements suggest that locating wide-area devices across both cantilever and mesa regions is possible. However, the first implementation of this technique also produced a new defect: cracks at cantilever coalescences with associated arrays of lateral dislocations. These defects have been labeled 'dark-block defects' because they are non-radiative and appear as dark rectangles in CL images. Material has been grown that does not have dark-block defects. Examination of the evolution of the cantilever films for many growths, both partial and complete, indicates that producing a film without these defects requires careful control of growth conditions and crystal morphology at multiple steps. Their elimination enhances optical emission and uniformity over large (mm) size areas.

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We demonstrate that when vertical threading dislocations in (0001) GaN are imaged in plan-view by transmission electron microscopy, a surface-relaxation contrast operates in addition to that due to the strain fields of dislocations passing through the specimen. We show that all three dislocation types (edge, screw, and mixed) can be detected in the same image using g = (11{bar 2}0) and 18{sup o} specimen tilt from [0001], allowing total densities to be assessed properly. The type of an individual dislocation can also be readily identified.

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This LDRD is aimed to place Sandia at the forefront of GaN-based technologies. Two important themes of this LDRD are: (1) The demonstration of novel GaN-based devices which have not yet been much explored and yet are coherent with Sandia's and DOE's mission objectives. UV optoelectronic and piezoelectric devices are just two examples. (2) To demonstrate front-end monolithic integration of GaN with Si-based microelectronics. Key issues pertinent to the successful completion of this LDRD have been identified to be (1) The growth and defect control of AlGaN and GaN, and (2) strain relief during/after the heteroepitaxy of GaN on Si and the separation/transfer of GaN layers to different wafer templates.

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The density of threading dislocations (TD) in GaN grown directly on flat sapphire substrates is typically greater than 10{sup 9}/cm{sup 2}. Such high dislocation densities degrade both the electronic and photonic properties of the material. The density of dislocations can be decreased by orders of magnitude using cantilever epitaxy (CE), which employs prepatterned sapphire substrates to provide reduced-dimension mesa regions for nucleation and etched trenches between them for suspended lateral growth of GaN or AlGaN. The substrate is prepatterned with narrow lines and etched to a depth that permits coalescence of laterally growing III-N nucleated on the mesa surfaces before vertical growth fills the etched trench. Low dislocation densities typical of epitaxial lateral overgrowth (ELO) are obtained in the cantilever regions and the TD density is also reduced up to 1 micrometer from the edge of the support regions.

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