skip to main content
US FlagAn official website of the United States government
dot gov icon
Official websites use .gov
A .gov website belongs to an official government organization in the United States.
https lock icon
Secure .gov websites use HTTPS
A lock ( lock ) or https:// means you've safely connected to the .gov website. Share sensitive information only on official, secure websites.


Title: In situ etching of β -Ga2O3 using tert -butyl chloride in an MOCVD system
In this study, we investigate in situ etching of β-Ga2O3 in a metalorganic chemical vapor deposition system using tert-butyl chloride (TBCl). We report etching of both heteroepitaxial 2¯01-oriented and homoepitaxial (010)-oriented β-Ga2O3 films over a wide range of substrate temperatures, TBCl molar flows, and reactor pressures. We infer that the likely etchant is HCl (g), formed by the pyrolysis of TBCl in the hydrodynamic boundary layer above the substrate. The temperature dependence of the etch rate reveals two distinct regimes characterized by markedly different apparent activation energies. The extracted apparent activation energies suggest that at temperatures below ∼800 °C, the etch rate is likely limited by desorption of etch products. The relative etch rates of heteroepitaxial 2¯01 and homoepitaxial (010) β-Ga2O3 were observed to scale by the ratio of the surface energies, indicating an anisotropic etch. Relatively smooth post-etch surface morphology was achieved by tuning the etching parameters for (010) homoepitaxial films.  more » « less
Award ID(s):
2039380
PAR ID:
10595137
Author(s) / Creator(s):
; ; ; ; ; ; ; ; ; ; ;
Publisher / Repository:
American Institute of Physics
Date Published:
Journal Name:
Applied Physics Letters
Volume:
125
Issue:
24
ISSN:
0003-6951
Format(s):
Medium: X
Sponsoring Org:
National Science Foundation
More Like this
  1. This work demonstrates an in situ etching technique for β-Ga2O3 using solid-source metallic gallium (Ga) in a low-pressure chemical vapor deposition (LPCVD) system, enabling clean, anisotropic, plasma damage-free etching. Etching behavior was systematically studied on (2¯01) β-Ga2O3 films and patterned (010) β-Ga2O3 substrates as a function of temperature (1000–1100 °C), Ar carrier gas flow (80–400 sccm) and Ga source-to-substrate distance (1–5 cm). The process exhibits vapor transport- and surface-reaction-limited behavior, with etch rates reaching a maximum of ∼2.25 µm/h on (010) substrates at 1050 °C and 2 cm spacing. Etch rates decrease sharply with increasing source-to-substrate distance due to reduced Ga vapor availability, while elevated temperatures enhance surface reaction kinetics through increased Ga reactivity and suboxide formation, leading to enhanced etch rates. In-plane anisotropy studies using radial trench patterns reveal that the (100) orientation produces the most stable etch front, characterized by smooth, vertical sidewalls and minimal lateral etching, consistent with its lowest surface free energy. In contrast, orientations such as (101), which possess higher surface energy, exhibit pronounced lateral etching and micro-faceting. As the trench orientation progressively deviates from (100), lateral etching increases. Facet evolution is observed between (100) and (1¯02), where stepped sidewalls composed of alternating (100) and (1¯02) segments progressively transition into a single inclined facet, which stabilizes along (100) or (1¯02) depending on the trench orientation. The (100)-aligned fins exhibit minimal bottom curvature, while (201)-aligned structures display increased under-etching and trench rounding. Collectively, these findings establish LPCVD-based in situ etching as a scalable, damage-free, and orientation-selective technique for fabricating high-aspect-ratio β-Ga2O3 3D structures in next-generation power devices. 
    more » « less
  2. This study presents a comprehensive analysis of the etching effects on β-Ga2O3 using two methods: H2_N2 (a mixture of hydrogen and nitrogen) etching and triethylgallium (TEGa) in situ etching performed in a metal-organic chemical vapor deposition system. By employing a mix of H2 and N2 gases at varying chamber pressures and maintaining a constant etching temperature of 750 °C, we investigated the etching dynamics across three different β-Ga2O3 orientations: (010), (001), and (2¯01). Field emission scanning electron microscopy analysis showed that the etching behavior of β-Ga2O3 depends on the crystal orientation, with the (010) orientation showing notably uniform and smooth surfaces, indicating its suitability for vertical device applications. High-aspect-ratio β-Ga2O3 fin arrays were fabricated on (010) substrates using H2_N2 etching, yielding fin structures with widths of 2 μm and depths of 3.1 μm, along with smooth and well-defined sidewalls. The etching process achieved exceptionally high etch rates (>18 μm/h) with a strong dependence on pressure and sidewall orientation, revealing the trade-off between etch depth and surface smoothness. Separately, TEGa in situ etching was investigated as an alternative etching technique for both β-Ga2O3 and β-(AlxGa1−x)2O3 films. The results revealed that the (010) orientation exhibited relatively high etching rates while maintaining smoother sidewalls and top surfaces, making it favorable for device processing. In contrast, the (001) orientation showed strong resistance to TEGa etching. Furthermore, Al-incorporated β-(AlxGa1−x)2O3 films showed substantially lower etch rates compared to pure β-Ga2O3, suggesting their potential use as an effective etch-stop layer in advanced device fabrication. 
    more » « less
  3. In this work, we report on the anisotropic etching characteristics of β-Ga2O3 using triethylgallium (TEGa) performed in situ within an MOCVD chamber. At sufficiently high substrate temperatures, TEGa can act as a strong etchant for β-Ga2O3 utilizing the suboxide reaction between Ga and Ga2O3 [4 Ga(s) + Ga2O3 (s) → 3Ga2O (g)]. We observe that due to the monoclinic crystal structure of β-Ga2O3, TEGa etching on both (010) and (001) substrates is highly anisotropic in nature, in terms of both sidewall roughness and lateral etch rate. Smooth sidewalls are only obtained along crystal orientations that minimize sidewall surface energy. Utilizing this technique, we also demonstrate deep sub-micrometer fins with smooth sidewalls and high aspect ratios. Furthermore, we also demonstrate the damage-free nature of TEGa etching by fabricating Schottky diodes on the etched surface, which display no change in the net donor concentration. 
    more » « less
  4. A new growth approach, based on the hot-wall metalorganic chemical vapor deposition concept, is developed for high-quality homoepitaxial growth of Si-doped single-crystalline β-Ga2O3 layers on (010)-oriented native substrates. Substrate annealing in argon atmosphere for 1 min at temperatures below 600 °C is proposed for the formation of epi-ready surfaces as a cost-effective alternative to the traditionally employed annealing process in oxygen-containing atmosphere with a time duration of 1 h at about 1000 °C. It is shown that the on-axis rocking curve widths exhibit anisotropic dependence on the azimuth angle with minima for in-plane direction parallel to the [001] and maximum for the [100] for both substrate and layer. The homoepitaxial layers are demonstrated to have excellent structural properties with a β-Ga2O3(020) rocking curve full-widths at half-maximum as low as 11 arc sec, which is lower than the corresponding one for the substrates (19 arc sec), even for highly Si-doped (low 1019 cm−3 range) layers. Furthermore, the structural anisotropy in the layer is substantially reduced with respect to the substrate. Very smooth surface morphology of the epilayers with a root mean square roughness value of 0.6 nm over a 5 × 5 μm2 area is achieved along with a high electron mobility of 69 cm2 V−1 s−1 at a free carrier concentration n=1.9×1019 cm−3. These values compare well with state-of-the-art parameters reported in the literature for β-Ga2O3(010) homoepitaxial layers with respective Si doping levels. Thermal conductivity of 17.4 Wm−1K−1 is determined along the [010] direction for the homoepitaxial layers at 300 K, which approaches the respective value of bulk crystal (20.6 Wm−1K−1). This result is explained by a weak boundary effect and a low dislocation density in the homoepitaxial layers. 
    more » « less
  5. Optimizing thermal anneals of Si-implanted β-Ga2O3 is critical for low resistance contacts and selective area doping. We report the impact of annealing ambient, temperature, and time on the activation of room temperature ion-implanted Si in β-Ga2O3 at concentrations from 5 × 1018 to 1 × 1020 cm−3, demonstrating full activation (>80% activation, mobilities >70 cm2/V s) with contact resistances below 0.29 Ω mm. Homoepitaxial β-Ga2O3 films, grown by plasma-assisted molecular beam epitaxy on Fe-doped (010) substrates, were implanted at multiple energies to yield 100 nm box profiles of 5 × 1018, 5 × 1019, and 1 × 1020 cm−3. Anneals were performed in an ultra-high vacuum-compatible quartz furnace at 1 bar with well-controlled gas compositions. To maintain β-Ga2O3 stability, pO2 must be greater than 10−9 bar. Anneals up to pO2 = 1 bar achieve full activation at 5 × 1018 cm−3, while 5 × 1019 cm−3 must be annealed with pO2 ≤ 10−4 bar, and 1 × 1020 cm−3 requires pO2 < 10−6 bar. Water vapor prevents activation and must be maintained below 10−8 bar. Activation is achieved for anneal temperatures as low as 850 °C with mobility increasing with anneal temperatures up to 1050 °C, though Si diffusion has been reported above 950 °C. At 950 °C, activation is maximized between 5 and 20 min with longer times resulting in decreased carrier activation (over-annealing). This over-annealing is significant for concentrations above 5 × 1019 cm−3 and occurs rapidly at 1 × 1020 cm−3. Rutherford backscattering spectrometry (channeling) suggests that damage recovery is seeded from remnant aligned β-Ga2O3 that remains after implantation; this conclusion is also supported by scanning transmission electron microscopy showing retention of the β-phase with inclusions that resemble the γ-phase. 
    more » « less