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S2. III-N Epitaxial Growth Techniques
S2. III-N Epitaxial Growth Techniques
Tuesday,
Nov. 11, 2025 15:00-17:15
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| Presider: |
Prof. Chun-Kai Wang (National Kaohsiung University of Science and Technology, Taiwan)
Prof. Hideto Miyake (Mie University, Japan) |
| Room: |
2nd Lecture Room |
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15:00 - 15:30
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Manuscript ID. 0129
Paper No. 2025-Tue-S0204-I001
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Invited Speaker: Prof. Hideto Miyake
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Polarity control of AlN via a combination of sputtering deposition and face-to-face annealing
Prof. Hideto Miyake, Professor, Mie University, Japan
We have successfully fabricated high-quality AlN templates by combining sputtering deposition of AlN (Sp-AlN) with high-temperature face-to-face annealing (FFA). These templates are hereafter referred to as FFA Sp-AlN. Additionally, we achieved Al-polar and N-polar FFA Sp-AlN by annealing Sp-AlN films sputtered using a sintered AlN target and an Al metal target, respectively. By controlling the polarity, we fabricated a bilayer polarity-inverted AlN structure, where the Al-polar FFA Sp-AlN serves as the lower layer and the N-polar FFA Sp-AlN as the upper layer. In this bilayer polarity-inverted FFA Sp-AlN, an inversion domain boundary (IDB) with an abrupt interface, consisting of several monolayers (ML), and an atomically smooth surface were observed. Various devices have been proposed using polarity inversion structures, such as second harmonic generation (SHG) devices based on quasi-phase matching, which exploits the nonlinear optical properties of nitride semiconductors. Leveraging the structural characteristics of the bilayer polarity-inverted FFA Sp-AlN, an SHG device with a transverse quasi-phase matched waveguide was fabricated. This device achieves a high nonlinear coupling coefficient by placing IDBs at the nodes of the second harmonic (SH) wave electric field distribution. The fabrication of a multi-layer polarity-inverted AlN structure with more than two layers is highly desirable. In this study, we demonstrate the fabrication of a four-layer polarity-inverted AlN structure using multiple sputtering of AlN and FFA with the polarity control method of FFA Sp-AlN. It was found that the IDB structures vary depending on the sequence of polarity inversion.
Preview abstract
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15:30 - 15:45
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Manuscript ID. 0108
Paper No. 2025-Tue-S0204-O001
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| Hiroki Yasunaga
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Structural Evaluation of AlGaN MQWs on Face-to-Face Annealed (11-22) AlN Templates
Hiroki Yasunaga, Kensei Oya, Ryota Akaike, Yongzhao Yao, Hideto Miyake, Mie University
(11-22) AlGaN multiple quantum wells (MQWs) grown by metalorganic vapor phase epitaxy (MOVPE) on sputter-deposited and face-to-face annealed AlN (FFA Sp-AlN) templates were structurally evaluated by transmission electron microscopy (TEM). Weak-beam dark-field TEM (WBDF-TEM) images revealed dislocation bending at the MOVPE-AlN/FFA Sp-AlN interface and the AlGaN/MOVPE-AlN interface, which is likely caused by compressive stress in FFA Sp-AlN. Most dislocations were identified as mixed a+c type, and the threading dislocation density was estimated to be 8.2 × 10⁹ cm⁻². High-angle annular dark-field scanning TEM (HAADF-STEM) images showed sharp MQW interfaces attributed to the small surface roughness.
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15:45 - 16:00
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Manuscript ID. 0073
Paper No. 2025-Tue-S0204-O002
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| Shinnosuke Mori
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Crystallographic Orientation Control of Nonpolar AlN via Thermal Treatment of r-Plane Sapphire Substrates
Shinnosuke Mori, Ryota Akaike, Hiroki Yasunaga, Takao Nakamura, Hideto Miyake, Mie University
AlGaN-based short-wavelength light-emitting devices with high Al content on polar planes suffer from reduced internal quantum efficiency due to the quantum-confined Stark effect and poor light extraction efficiency caused by preferential c-axis perpendicular emission. Nonpolar a-plane nitride semiconductor growth on r-plane sapphire substrates has attracted attention to solve these issues. This study investigates the effects of thermal treatment of r-plane sapphire substrates on crystallographic orientation and crystal quality of subsequently grown AlN films. Single-domain a-plane AlN growth was achieved on thermally treated substrates, while untreated substrates showed mixed a-plane and semipolar orientations.
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16:00 - 16:15
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Manuscript ID. 0027
Paper No. 2025-Tue-S0204-O003
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| Z.R. Zytkiewicz
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Calibration of Surface Temperature of Metallic Substrates in MBE – Unveiling the Impact of Thickness Dependent Emissivity of Thin Buffer Layers
Z.R. Zytkiewicz, K. Olszewski, A. Wierzbicka, M. Sobanska, Institute of Physics, Polish Academy of Sciences, Warsaw, Poland; M. Guziewicz, Łukasiewicz Research Network - Institute for Microelectronics and Photonics, Warsaw, Poland
Optical pyrometry-based substrate temperature calibration technique allowing reliable determination of emissivity of even nonstandard substrates such as thin metallic buffer on bulk wafer is presented. As example this approach is used to measure emissivity of metallic ZrN layers deposited on Si and Al2O3 wafers and reveals a strong dependence of substrate emissivity on thickness of the thin film. Accuracy of our technique is demonstrated by MBE growth of GaN nanowires on Si substrates with and without ZrN buffer and using nucleation kinetics of GaN nanowires as a sensitive probe of small changes in the surface temperature of the substrate.
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16:15 - 16:30
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Manuscript ID. 0074
Paper No. 2025-Tue-S0204-O004
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| Rennosuke Hara
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Estimation of Screw Dislocation Density in High-crystallinity AlN by X-ray Rocking Curves
Rennosuke Hara, Ryota Akaike, Hiroki Yasunaga, Takao Nakamura, Hideto Miyake, Mie University
We estimated the screw dislocation density in high-crystallinity AlN templates fabricated by sputtering and face-to-face annealing. Since the (0002) X-ray rocking curve (XRC) full widths at half maximum (FWHMs) were close to the instrumental resolution limit, estimating
the screw dislocation density solely from the (0002) XRC-FWHM was challenging. However, the (0002) XRC profiles exhibited both sharp and broad components. We found a positive correlation between the intensity of the broad component and the hillock density observed after AlGaN growth. These results indicate that screw dislocation densities can be estimated even when the (0002) XRC-FWHM approaches the instrumental resolution limit.
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16:30 - 16:45
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Manuscript ID. 0025
Paper No. 2025-Tue-S0204-O005
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| Makoto OHTSUKA
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Growth Behavior of AlN Crystals Using Type 304L Stainless Steel Flux
Makoto OHTSUKA, Masayoshi ADACHI, Hiroyuki FUKUYAMA, Institute of Multidisciplinary Research for Advanced Materials, Tohoku University
AlN is a key material for deep-UV LEDs and power devices. However, traditional sublimation growth is expensive due to the high temperatures required. This study focuses on low-temperature AlN crystal growth using type 304L stainless steel flux. AlN crystals were grown on sapphire substrates under different conditions. Substrate rotation improved surface smoothness and slightly increased thickness. Lower initial growth temperatures improved surface quality but reduced thickness. A slower cooling rate improved both thickness and smoothness. These results suggest that the solution growth method using stainless steel flux has the potential to produce AlN crystals efficiently and at a lower cost.
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16:45 - 17:00
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Manuscript ID. 0030
Paper No. 2025-Tue-S0204-O006
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| Shunya Nanri
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Effect of Nb Addition to Molten Fe on Solution Growth of AlN Crystals
Shunya Nanri, Makoto Ohtsuka, Masayoshi Adachi, Hiroyuki Fukuyama, Institute of Multidisciplinary Research for Advanced Materials, Tohoku University
AlN is a promising substrate material, but single crystal growth is difficult due to high-temperature constraints. This study explores AlN solution growth using Fe-Nb alloy fluxes, which offer improved nitrogen solubility. Thermodynamic calculations and growth experiments were conducted with Fe-Nb alloys of varying Nb content. Results showed that AlN solubility, N solubility and crystal thickness increased with Nb content up to 4 mass%, but declined at 5 mass%, suggesting an optimal Nb range. SEM analysis confirmed growth behavior, supporting the use of Fe-Nb alloys for improved AlN crystal fabrication.
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17:00 - 17:15
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Manuscript ID. 0138
Paper No. 2025-Tue-S0204-O007
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| Tomohiro Tamano
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Evaluation of Polarity-inverted AlN interface using oxidation processes
Tomohiro Tamano, Ryota Akaike, Hiroki Yasunaga, Hideto Miyake, Mie University; Zentaro Akase, Shigetaka Tomiya, Nara Institute of Science and Technology
Polarity-inverted AlN structures, which are promising for wavelength conversion devices, can be fabricated through oxidation processes. However, the effect of different oxidation methods on the atomic arrangement has not yet been fully clarified. In this study, polarity-inverted AlN structures were fabricated using several oxidation techniques, and polarity inversion was verified by KOH wet etching. For the oxygen plasma treatment, voids were observed at the position of the carbon spike, corresponding to the sputtering interface. Furthermore, secondary ion mass spectrometry (SIMS) analysis indicated that the position of the inversion domain boundaries (IDB) was influenced by the oxidation process employed.
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