2-inch diameter (010) principal-face β-Ga2O3 single crystals grown by EFG method

Xuyang Dong; Wenxiang Mu; Pei Wang; Yue Dong; Hao Zhao; Boyang Chen; Zhitai Jia; Xutang Tao

doi:10.1088/1674-4926/24110029

J. Semicond. > In Press

ARTICLES

2-inch diameter (010) principal-face β-Ga₂O₃ single crystals grown by EFG method

Xuyang Dong¹, Wenxiang Mu^1,, Pei Wang¹, Yue Dong¹, Hao Zhao¹, Boyang Chen¹, Zhitai Jia^{1, 2,} and Xutang Tao¹

+ Author Affiliations

Corresponding author: Wenxiang Mu, mwx@sdu.edu.cn; Zhitai Jia, z.jia@sdu.edu.cn

DOI: 10.1088/1674-4926/24110029CSTR: 32376.14.1674-4926.24110029

Abstract: The (010)-oriented substrates of β-Ga₂O₃ are endowed with the maximum thermal conductivity and fastest homoepitaxial rate, which is the preferred substrate direction for high-power devices. However, the size of (010) plane wafer is critically limited by die in the commercial edge-defined film-fed growth (EFG) method. It is difficult to grow the β-Ga₂O₃ crystal with (010) principal face due to the (100) and (001) are cleavage planes. Here, the 2-inch diameter (010) principal-face β-Ga₂O₃ single crystal is successfully designed and grown by improved EFG method. Unlike previous reported techniques, the single crystals are pulled with [001] direction, and in this way the (010) wafers can be obtained from the principal face. In our experiments, tree-like defects (TLDs) in (010) principal-face bulk crystals are easy to generate. The relationship between stability of growth interface and origin of TLDs are thoroughly discussed. The TLDs are successfully eliminated by optimizing growth conditions. The high crystalline quality of (010)-oriented substrates are comprehensive demonstrated by full width at half maximum (FWHM) with 50.4 arcsec, consistent orientation arrangement of (010) plane, respectively. This work shows that the (010)-oriented substrates can be obtained by EFG method, predicting the commercial prospects of large-scale (010)-oriented β-Ga₂O₃ substrates.

Key words: β-Ga₂O₃, EFG, (010) principal-face single crystal

References

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Fig. 1. (Color online) (a) Schematic diagram of (010) principal-face β-Ga₂O₃ bulk crystals grown by EFG method. (b) (010) principal-face macro-morphology image of TLDs, showing obvious branching tendency of evolution process with (001) pulling direction from right to left. (c) Enlarged-morphology image of red rectangular block from (b). (d) Micro-morphology image of TLDs of yellow rectangular block in (b). (e) 2-inch diameter (010) principal-face non-TLDs β-Ga₂O₃ single crystal.

DownLoad: Full-Size Img PowerPoint

Fig. 2. (Color online) (a) SEM image of (010) principal-face β-Ga₂O₃ bulk crystals growth cross section at early pulling stage, the bright region with branches is cross-sectional TLDs, enlarged images of (b)−(f) are different location in (a) marked by yellow rectangular block, and the location of (b) is termination point of TLDs, exhibiting destructive effect for crystalline structure of β-Ga₂O₃ bulk crystals. (g) SEM image of growth cross section at later growth stage of the same bulk crystal, the bright region is cross-sectional TLDs, showing the worse surface morphology than early stage in (a), enlarged images of (h) and (i) are also marked in (g), indicating severe deteriorating scene of TLDs.

DownLoad: Full-Size Img PowerPoint

Fig. 3. (Color online) (a) XRD pattern and (b) X-ray rocking curve of (010)-oriented substrate from (010) principal-face β-Ga₂O₃ single crystal. (c) Laue diffraction image, (d) indexation of Laue spots, and (e) identification of (010)-oriented crystallographic plane, manifesting great symmetry and consistency.

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Fig. 4. (Color online) (a) UV−VIS−NIR transmittance spectra of (010)-oriented β-Ga₂O₃, the inset is optical bandgap with 4.4 eV of (010) plane. (b) MWIR transmittance spectra of (010)-oriented β-Ga₂O₃, showing wide transmission range from UV to MWIR band. (c) Temperature-dependent resistivity of (010)-oriented β-Ga₂O₃. (d) Fe acceptor activation energy with 0.78 eV was fitted with Arrhenius equation.

DownLoad: Full-Size Img PowerPoint

[1]	Zhang J C, Dong P F, Dang K, et al. Ultra-wide bandgap semiconductor Ga₂O₃ power diodes. Nat Commun, 2022, 13, 3900 doi: 10.1038/s41467-022-31664-y
[2]	Tsao J Y, Chowdhury S, Hollis M A, et al. Ultrawide-bandgap semiconductors: Research opportunities and challenges. Adv Elect Materials, 2018, 4(1), 1600501 doi: 10.1002/aelm.201600501
[3]	Pearton S J, Yang J C, Cary P H, et al. A review of Ga₂O₃ materials, processing, and devices. Appl Phys Rev, 2018, 5(1), 011301 doi: 10.1063/1.5006941
[4]	Heinselman K N, Haven D, Zakutayev A, et al. Projected cost of gallium oxide wafers from edge-defined film-fed crystal growth. Cryst Growth Des, 2022, 22(8), 4854 doi: 10.1021/acs.cgd.2c00340
[5]	Lu X, Deng Y X, Pei Y L, et al. Recent advances in NiO/Ga₂O₃ heterojunctions for power electronics. J Semicond, 2023, 44(6), 061802 doi: 10.1088/1674-4926/44/6/061802
[6]	Xu G W, Wu F H, Liu Q, et al. Vertical β-Ga₂O₃ power electronics. J Semicond, 2023, 44(7), 070301 doi: 10.1088/1674-4926/44/7/070301
[7]	Wei J S, Bu Y Z, Sai Q L, et al. Effect of high-temperature remelting on the properties of Sn-doped β-Ga₂O₃ crystal grown using the EFG method. CrystEngComm, 2023, 25(30), 4317 doi: 10.1039/D3CE00415E
[8]	Mastro M A, Kuramata A, Calkins J, et al. Perspective: Opportunities and future directions for Ga₂O₃. ECS J Solid State Sci Technol, 2017, 6(5), P356 doi: 10.1149/2.0031707jss
[9]	Aida H, Nishiguchi K, Takeda H, et al. Growth of β-Ga₂O₃ single crystals by the edge-defined, film fed growth method. Jjap, 2008, 47(11R), 8506 doi: 10.1143/JJAP.47.8506
[10]	Ohba E, Kobayashi T, Taishi T, et al. Growth of (100), (010) and (001) β-Ga₂O₃ single crystals by vertical Bridgman method. J Cryst Growth, 2021, 556, 125990 doi: 10.1016/j.jcrysgro.2020.125990
[11]	Hoshikawa K, Ohba E, Kobayashi T, et al. Growth of β-Ga₂O₃ single crystals using vertical Bridgman method in ambient air. J Cryst Growth, 2016, 447, 36 doi: 10.1016/j.jcrysgro.2016.04.022
[12]	Galazka Z. Growth of bulk β-Ga₂O₃ single crystals by the Czochralski method. 2022, 131(3), 0311, 03
[13]	Chen B Y, Mu W X, Liu Y Y, et al. Growth and characterization of the β-Ga₂O₃ (011) plane without line-shaped defects. CrystEngComm, 2023, 25(16), 2404 doi: 10.1039/D3CE00052D
[14]	Li P K, Han X L, Chen D Y, et al. Controllability of β-Ga₂O₃ single crystal conductivity by V doping. CrystEngComm, 2022, 24(31), 5588 doi: 10.1039/D2CE00418F
[15]	Zhang Q Y, Li N, Zhang T, et al. Enhanced gain and detectivity of unipolar barrier solar blind avalanche photodetector via lattice and band engineering. Nat Commun, 2023, 14(1), 418 doi: 10.1038/s41467-023-36117-8
[16]	Guo D, Guo Q, Chen Z, et al. Review of Ga₂O₃-based optoelectronic devices. Mater Today Phys, 2019, 11, 100157 doi: 10.1016/j.mtphys.2019.100157
[17]	Song Y W, Bhattacharyya A, Karim A, et al. Ultra-wide band gap Ga₂O₃-on-SiC MOSFETs. ACS Appl Mater Interfaces, 2023, 15(5), 7137 doi: 10.1021/acsami.2c21048
[18]	Singh M, Casbon M A, Uren M J, et al. Pulsed large signal RF performance of field-plated Ga₂O₃ MOSFETs. IEEE Electron Device Lett, 2018, 39(10), 1572 doi: 10.1109/LED.2018.2865832
[19]	Moser N, Liddy K, Islam A, et al. Toward high voltage radio frequency devices in β-Ga₂O₃. Appl Phys Lett, 2020, 117(24), 242101 doi: 10.1063/5.0031482
[20]	Mu W X, Jia Z T, Cittadino G, et al. Ti-doped β-Ga₂O₃: A promising material for ultrafast and tunable lasers. Cryst Growth Des, 2018, 18(5), 3037 doi: 10.1021/acs.cgd.8b00182
[21]	Zhang Y H, Xing F. Anisotropic optical and electric properties of β-gallium oxide. J Semicond, 2023, 44(7), 071801 doi: 10.1088/1674-4926/44/7/071801
[22]	Lovejoy T C, Yitamben E N, Shamir N, et al. Surface morphology and electronic structure of bulk single crystal β-Ga₂O₃ (100). Appl Phys Lett, 2009, 94(8), 1906
[23]	Bermudez V M. The structure of low-index surfaces of β-Ga₂O₃. Chem Phys, 2006, 323(2/3), 193
[24]	Meng L Y, Yu D S, Huang H L, et al. MOCVD Growth of β-Ga₂O₃ on (001) Ga₂O₃ Substrates. Cryst Growth Des, 2024, 24(9), 3737 doi: 10.1021/acs.cgd.4c00060
[25]	Nandi A, Cherns D, Sanyal I, et al. Epitaxial growth of (-201) β-Ga₂O₃ on (001) diamond substrates. Cryst Growth Des, 2023, 23(11), 8290 doi: 10.1021/acs.cgd.3c00972
[26]	Bu Y Z, Sai Q L, Qi H J. Stability of interfacial thermal balance in thick β-Ga₂O₃ crystal growth by EFG. J Cryst Growth, 2023, 612, 127194 doi: 10.1016/j.jcrysgro.2023.127194
[27]	Mu W X, Jia Z T, Yin Y R, et al. Solid-liquid interface optimization and properties of ultra-wide bandgap β-Ga₂O₃ grown by Czochralski and EFG methods. CrystEngComm, 2019, 21(17), 2762 doi: 10.1039/C8CE02189A
[28]	Tang X, Liu B T, Yu Y, et al. Numerical analysis of difficulties of growing large-size bulk β-Ga₂O₃ single crystals with the czochralski method. Crystals, 2021, 11(1), 25
[29]	Kuramata A, Koshi K, Watanabe S, et al. High-quality β-Ga₂O₃ single crystals grown by edge-defined film-fed growth. Jpn J Appl Phys, 2016, 55(12), 1202A2 doi: 10.7567/JJAP.55.1202A2
[30]	Hou T, Zhang W Y, Mu W X, et al. The anisotropy dependence of deformation mechanism of cleavage planes in β-Ga₂O₃ single crystal. Mater Sci Semicond Process, 2023, 158, 107357 doi: 10.1016/j.mssp.2023.107357
[31]	Ge M, Li Y, Zhu Y H, et al. An improved design for e-mode AlGaN/GaN HEMT with gate stack β-Ga₂O₃/p-GaN structure. J Appl Phys, 2021, 130(3), 035703 doi: 10.1063/5.0051274
[32]	Yao Y Z, Hirano K, Sugawara Y, et al. Observation of dislocations in thick β-Ga₂O₃ single-crystal substrates using Borrmann effect synchrotron X-ray topography. Apl Materials, 2022, 10(5), 051101 doi: 10.1063/5.0088701
[33]	Ueda O, Kasu M, Yamaguchi H. Structural characterization of defects in EFG- and HVPE-grown β-Ga₂O₃ crystals. Jpn J Appl Phys, 2022, 61(5), 050101 doi: 10.35848/1347-4065/ac4b6b
[34]	Yao Y Z, Tsusaka Y, Hirano K, et al. Three-dimensional distribution and propagation of dislocations in β-Ga₂O₃ revealed by Borrmann effect X-ray topography. J Appl Phys, 2023, 134(15), 155104 doi: 10.1063/5.0169526
[35]	Ma X C, Xu R, Xu J F, et al. In-plane crystalline anisotropy of bulk β-Ga₂O₃. J Appl Cryst, 2021, 54(4), 1153 doi: 10.1107/S1600576721006427
[36]	Wang M G, Mu S, Speck J S, et al. First-principles study of twin boundaries and stacking faults in β-Ga₂O₃. Adv Materials Inter, 2025, 12(2), 2300318 doi: 10.1002/admi.202300318
[37]	Haven D, Moutinho H, Mangum J S, et al. Multimodal microscopy of extended defects in β-Ga₂O₃ (010) EFG crystals. AIP Advances, 2023, 13(7), 075122 doi: 10.1063/5.0158904
[38]	Gu Y, Wang W W, Li Y J, et al. Designable ultra-smooth ultra-thin solid-electrolyte interphases of three alkali metal anodes. Nat Commun, 2018, 9(1), 1339 doi: 10.1038/s41467-018-03466-8
[39]	Lee B, Paek E, Mitlin D, et al. Sodium metal anodes: emerging solutions to dendrite growth. Chem Rev, 2019, 119(8), 5416 doi: 10.1021/acs.chemrev.8b00642
[40]	Li C Z, Yuan Q, Ni B, et al. Dendritic defect-rich palladium-copper-cobalt nanoalloys as robust multifunctional non-platinum electrocatalysts for fuel cells. Nat Commun, 2018, 9(1), 3702 doi: 10.1038/s41467-018-06043-1
[41]	Liu Y J, Li S J, Wang H L, et al. Microstructure, defects and mechanical behavior of beta-type titanium porous structures manufactured by electron beam melting and selective laser melting. Acta Mater, 2016, 113, 56 doi: 10.1016/j.actamat.2016.04.029
[42]	Glicksman M E, Lupulescu A O. Dendritic crystal growth in pure materials. J Cryst Growth, 2004, 264(4), 541 doi: 10.1016/j.jcrysgro.2003.12.034
[43]	Gránásy L, Pusztai T, Börzsönyi T, et al. A general mechanism of polycrystalline growth. Nature Mater, 2004, 3(9), 645 doi: 10.1038/nmat1190
[44]	Dong X Y, Yu S J, Mu W X, et al. Solar-blind photodetectors prepared using semi-insulating Co: β-Ga₂O₃ single crystals that are stable over a wide temperature range. J Mater Chem C, 2023, 11(26), 8919 doi: 10.1039/D3TC00906H

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Received: 21 December 2024 Revised: 23 January 2025 Online: Accepted Manuscript: 18 February 2025Uncorrected proof: 21 March 2025

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Xuyang Dong, Wenxiang Mu, Pei Wang, Yue Dong, Hao Zhao, Boyang Chen, Zhitai Jia, Xutang Tao. 2-inch diameter (010) principal-face β-Ga2O3 single crystals grown by EFG method[J]. Journal of Semiconductors, 2025, In Press. doi: 10.1088/1674-4926/24110029 ****X Y Dong, W X Mu, P Wang, Y Dong, H Zhao, B Y Chen, Z T Jia, and X T Tao, 2-inch diameter (010) principal-face β-Ga2O3 single crystals grown by EFG method[J]. J. Semicond., 2025, 46(6), 062501 doi: 10.1088/1674-4926/24110029

Citation:

Xuyang Dong, Wenxiang Mu, Pei Wang, Yue Dong, Hao Zhao, Boyang Chen, Zhitai Jia, Xutang Tao. 2-inch diameter (010) principal-face β-Ga₂O₃ single crystals grown by EFG method[J]. Journal of Semiconductors, 2025, In Press. doi: 10.1088/1674-4926/24110029 ****

X Y Dong, W X Mu, P Wang, Y Dong, H Zhao, B Y Chen, Z T Jia, and X T Tao, 2-inch diameter (010) principal-face β-Ga₂O₃ single crystals grown by EFG method[J]. J. Semicond., 2025, 46(6), 062501 doi: 10.1088/1674-4926/24110029

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2-inch diameter (010) principal-face β-Ga₂O₃ single crystals grown by EFG method

DOI: 10.1088/1674-4926/24110029

CSTR: 32376.14.1674-4926.24110029

1.
State Key Laboratory of Crystal Materials, Institute of novel semiconductors, Shandong University, Institute of Crystal materials, Jinan 250100, China
2.
Shandong Research Institute of Industrial Technology, Jinan 250100, China

More Information

Xuyang Dong got his BS degree from Nanjing Tech University in 2019. Now he is a PhD student at Shandong University under the supervision of Prof. Zhitai Jia. His research focuses on the crystal growth and investigation of properties of ultrawide-bandgap semiconductor material of β-Ga₂O₃
Wenxiang Mu got his BS degree in 2013 and PhD degree in 2018 at Shandong University. Now he is an associate professor at institute of novel semiconductors of Shandong University. His research interests include crystal growth, substrate processing, performance optimization and device design based on ultrawide-bandgap semiconductor material of β-Ga₂O₃
Zhitai Jia got his BS degree in 2003 and PhD degree in 2008 at Shandong University. Now he is a full professor at institute of novel semiconductors of Shandong University. His research focuses on the crystal growth, performance optimization and device design of oxide semiconductor and magneto-optic functional crystal
Corresponding author: mwx@sdu.edu.cn; z.jia@sdu.edu.cn
Received Date: 2024-12-21
Revised Date: 2025-01-23

Available Online: 2025-02-18

Abstract

Abstract

The (010)-oriented substrates of β-Ga₂O₃ are endowed with the maximum thermal conductivity and fastest homoepitaxial rate, which is the preferred substrate direction for high-power devices. However, the size of (010) plane wafer is critically limited by die in the commercial edge-defined film-fed growth (EFG) method. It is difficult to grow the β-Ga₂O₃ crystal with (010) principal face due to the (100) and (001) are cleavage planes. Here, the 2-inch diameter (010) principal-face β-Ga₂O₃ single crystal is successfully designed and grown by improved EFG method. Unlike previous reported techniques, the single crystals are pulled with [001] direction, and in this way the (010) wafers can be obtained from the principal face. In our experiments, tree-like defects (TLDs) in (010) principal-face bulk crystals are easy to generate. The relationship between stability of growth interface and origin of TLDs are thoroughly discussed. The TLDs are successfully eliminated by optimizing growth conditions. The high crystalline quality of (010)-oriented substrates are comprehensive demonstrated by full width at half maximum (FWHM) with 50.4 arcsec, consistent orientation arrangement of (010) plane, respectively. This work shows that the (010)-oriented substrates can be obtained by EFG method, predicting the commercial prospects of large-scale (010)-oriented β-Ga₂O₃ substrates.
- β-Ga₂O₃,
- EFG,
- (010) principal-face single crystal

Supplementary materials to this article can be found online at https://doi.org/10.1088/1674-4926/24110029.

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