新型GaN与ZnO衬底ScAlMgO4晶体的研究进展

doi:10.15541/jim20220620

无机材料学报 ›› 2023, Vol. 38 ›› Issue (3): 228-242.DOI: 10.15541/jim20220620

新型GaN与ZnO衬底ScAlMgO₄晶体的研究进展

张超逸¹(), 唐慧丽¹(), 李宪珂¹, 王庆国¹, 罗平¹, 吴锋¹, 张晨波¹, 薛艳艳¹, 徐军¹(), 韩建峰², 逯占文²

1.同济大学物理科学与工程学院, 先进微结构材料教育部重点实验室, 上海 200092
2.连城凯克斯科技有限公司, 无锡 214000

收稿日期:2022-10-20 修回日期:2022-11-17 出版日期:2023-01-19 网络出版日期:2023-01-19
通讯作者: 唐慧丽, 副教授. E-mail: tanghl@tongji.edu.cn;
徐军, 教授. E-mail: 15503@tongji.edu.cn
作者简介:张超逸(1998-), 男, 博士研究生. E-mail: zcy99945111@163.com
基金资助:
国家自然科学基金(52032009);国家自然科学基金(61621001);国家自然科学基金(62075166)

Research Progress of ScAlMgO₄ Crystal: a Novel GaN and ZnO Substrate

ZHANG Chaoyi¹(), TANG Huili¹(), LI Xianke¹, WANG Qingguo¹, LUO Ping¹, WU Feng¹, ZHANG Chenbo¹, XUE Yanyan¹, XU Jun¹(), HAN Jianfeng², LU Zhanwen²

1. MOE Key Laboratory of Advanced Micro-Structured Materials, School of Physics Science and Engineering, Tongji University, Shanghai 200092, China
2. Linton Kayex Technology Co., Ltd., Wuxi 214000, China

Received:2022-10-20 Revised:2022-11-17 Published:2023-01-19 Online:2023-01-19
Contact: TANG Huili, associate professor. E-mail: tanghl@tongji.edu.cn;
XU Jun, professor. E-mail: 15503@tongji.edu.cn
About author:ZHANG Chaoyi (1998-), male, PhD candidate. E-mail: zcy99945111@163.com
Supported by:
National Natural Science Foundation of China(52032009);National Natural Science Foundation of China(61621001);National Natural Science Foundation of China(62075166)

摘要/Abstract

摘要：

二十一世纪以来, 以氮化镓(GaN)和氧化锌(ZnO)为代表的第三代宽禁带(E_g>2.3 eV)半导体材料正成为半导体产业发展的核心支撑材料。由于GaN与ZnO单晶生长难度较大, 成本较高, 常采用外延技术在衬底材料上生长薄膜, 因此寻找理想的衬底材料成为发展的关键。相比于传统的蓝宝石、6H-SiC、GaAs等衬底材料, 铝镁酸钪(ScAlMgO₄)晶体作为一种新型自剥离衬底材料, 因其与GaN、ZnO具有较小的晶格失配(失配率分别为~1.4%和~0.09%)以及合适的热膨胀系数而备受关注。本文从ScAlMgO₄晶体的结构出发, 详细介绍了其独特的三角双锥配位体结构与自然超晶格结构, 这是其热学性质与电学性质的结构基础。此外, ScAlMgO₄晶体沿着c轴的层状结构使其具有自剥离特性, 大大降低了生产成本, 在制备自支撑GaN薄膜方面具有良好的市场应用前景。然而ScAlMgO₄原料合成难度较大, 晶体生长方法单一, 主要为提拉法, 且与日本存在较大的差距, 亟需开发新的高质量、大尺寸ScAlMgO₄晶体的生长方法来打破技术壁垒。

关键词: ScAlMgO₄, 自剥离衬底, 晶格匹配, 晶体生长, 外延, 综述

Abstract:

Since the beginning of the 21st century, the third generation wide band gap (E_g>2.3 eV) semiconductor materials represented by gallium nitride (GaN) and zinc oxide (ZnO) are becoming the core supporting materials for development of semiconductor industry. Due to difficult growth and high cost of GaN and ZnO single crystal, epitaxial technology is always used as the substrate materials to grow GaN and ZnO films. Therefore, it is crucial to find an ideal substrate material for the development of third generation semiconductor. Compared with traditional substrate materials, such as sapphire, 6H-SiC and GaAs, scandium magnesium aluminate (ScAlMgO₄) crystal, as a new self-peeling substrate material, has attracted much attention because of its small lattice mismatch rate (~1.4% and ~0.09%, respectively) and suitable thermal expansion coefficient with GaN and ZnO. In this paper, based on structure of ScAlMgO₄ crystal, the unique trigonal bipyramid coordination and natural superlattice structure, the basis for its thermal and electrical properties, are introduced in detail. In addition, the layered structure of ScAlMgO₄ crystal along the c-axis makes it self-peeling, which greatly reduces its preparation cost and has a good application prospect in the preparation of self-supported GaN films. However, the raw material of ScAlMgO₄ is difficult to synthesize, and the crystal growth method is single, mainly through the Czochralski method (Cz), and growing techniques now in China lag far behind that in Japan. Therefore, it is urgent to develop a new growth method of growing high quality and large size ScAlMgO₄ crystals to break the technical barriers.

Key words: ScAlMgO₄, self-peeling substrate, lattice matching, crystal growth, epitaxy, review

中图分类号:

TQ174

张超逸, 唐慧丽, 李宪珂, 王庆国, 罗平, 吴锋, 张晨波, 薛艳艳, 徐军, 韩建峰, 逯占文. 新型GaN与ZnO衬底ScAlMgO₄晶体的研究进展[J]. 无机材料学报, 2023, 38(3): 228-242.

ZHANG Chaoyi, TANG Huili, LI Xianke, WANG Qingguo, LUO Ping, WU Feng, ZHANG Chenbo, XUE Yanyan, XU Jun, HAN Jianfeng, LU Zhanwen. Research Progress of ScAlMgO₄ Crystal: a Novel GaN and ZnO Substrate[J]. Journal of Inorganic Materials, 2023, 38(3): 228-242.

图/表 16

图1 SCAM晶体结构图(a)和[ScO6]八面体与[Al/MgO5]三角双锥体结构(b)

Fig. 1 Crystal structure of SCAM (a) and [ScO6] octahedran and [Al/MgO5] trigonal bipyramid (b)

图2 (RAO3)n(MO)m族结构中的两种三角双锥体[11]

Fig. 2 Two types of trigonal bipyramid coordination in (RAO3)n(MO)m compounds[11] (a) Type I with D3h symmetry environment; (b) Type II with C3v symmetry environment

图3 SCAM的电学性质[21]

Fig. 3 Electrical properties of SCAM[21] (a) Electronic energy band structure; (b) Density of states of cations

图4 SCAM的热学性质[37]

Fig. 4 Thermal properties of SCAM[37] (a) Cell parameters for SCAM as a function of temperature based on the high temperature XRD; (b, c) Length of a-axis (b) and the axial thermal expansion coefficient for a-axis (c) of SCAM in comparison to those of GaN, ZnO and Al2O3

图5 SCAM的光学性质[9]

Fig. 5 Optical properties of SCAM[9] (a) Transmittance spectrum; (b) PL spectrum under 200 nm excitation; (c) PLE spectrum monitoring at 300-500 nm emission bands of SCAM crystal; Inset in (c) focuses on ~250 nm band

图6 SCAM粉体1670 K下烧结168 h产物的XRD谱图[45]

Fig. 6 XRD patterns of products from SCAM powders sintered at 1670 K for 168 h[45]

图7 提拉法生长SCAM单晶[38]

Fig. 7 SCAM single crystal grown by Cz method[38] (a) SCAM single crystal with the dimension of ϕ30 mm×59 mm grown by Cz method; (b) Interference photograph of (0001) SCAM wafer under the polarizing microscopy

图8 提拉法生长各种直径的SCAM单晶[48]

Fig. 8 SCAM single crystal with various diameters grown by Cz method[48] 10 mm-3.5 inch; 1 inch=25.4 mm

图9 日本福田实验室生长的SCAM晶体的位错分析[50]

Fig. 9 Dislocation analysis of SCAM crystal grown by Fukuda laboratory[50] (a) Schematic diagram of the XRT test setup, and (b-d) reconstruct (b) maximum intensity map, (c) peak position map and (d) FWHM map using 201 XRT images

图10 GaN晶体结构示意图

Fig. 10 Crystal structural of GaN (a) Unit cell; (b) Distribution of [GaN4] tetrahedron

表1 GaN、ZnO外延层常用衬底

Table 1 Common substrates for GaN and ZnO epitaxial layers

Crystal		GaN	Sapphire	6H-SiC	Si	GaAs	SCAM
Space group		$\text{P}{{6}_{3}}\text{mc}$	$R 3 ¯ c$	$P 63 mc$	$Fd 3 ¯ m$	$F 4 ¯ 3 m$	$R 3 ¯ m$
Lattice parameters		a=b=0.319 nm c=0.519 nm α=β=90° γ=120°	a=b=0.476 nm c=1.299 nm α=β=90° γ=120°	a=b=0.307 nm c=1.508 nm α=β=90° γ=120°	a=b=c=0.543 nm α=β=γ=90°	a=b=c=0.565 nm α=β=γ=90°	a=b=0.324 nm c=2.515 nm α=β=90° γ=120°
Lattice mismatch, $Δ a / α$	GaN	0	16%^[61]	3.3%^[61]	16%^[62]	20%^[63]	1.4%^[5]
Lattice mismatch, $Δ a / α$	ZnO	2.2%^[64]	18%^[65]	5.8%^[66]	16.6%^[67]	22%^[64]	0.09%^[6]
Thermal expansion coefficient, α (~300 K)/(×10^-6, K^-1)		α_a=3.43 α_c=3.34^[36]	α_a=7.5 α_c=8.5^[68]	α_a=3.2 α_c=3.1^[69]	α=2.55^[70]	α=5.73^[71]	α_a=5.59 α_c=10.2^[37]
Melting point/K		2770^[54]	2326^[72]	3100^[69]	1680^[73]	1500^[74]	2220^[38]
Thermal conductivity, λ (~300 K)/(W·cm^-1·K^-1)		λ_c=2.2^[75]	λ_c=0.23^[68]	λ_c=4.3^[76]	λ=1.3^[77]	λ=0.55^[78]	λ_c=0.062^[50]
Growth methods		HVPE MOCVD	Cz, KY, EFG	PVT	Cz	LEC, VB	Cz
Cost		High	Medium	High	Low	Low	Low

表1 GaN、ZnO外延层常用衬底

Table 1 Common substrates for GaN and ZnO epitaxial layers

Crystal		GaN	Sapphire	6H-SiC	Si	GaAs	SCAM
Space group		$\text{P}{{6}_{3}}\text{mc}$	$R 3 ¯ c$	$P 63 mc$	$Fd 3 ¯ m$	$F 4 ¯ 3 m$	$R 3 ¯ m$
Lattice parameters		a=b=0.319 nm c=0.519 nm α=β=90° γ=120°	a=b=0.476 nm c=1.299 nm α=β=90° γ=120°	a=b=0.307 nm c=1.508 nm α=β=90° γ=120°	a=b=c=0.543 nm α=β=γ=90°	a=b=c=0.565 nm α=β=γ=90°	a=b=0.324 nm c=2.515 nm α=β=90° γ=120°
Lattice mismatch, $Δ a / α$	GaN	0	16%^[61]	3.3%^[61]	16%^[62]	20%^[63]	1.4%^[5]
Lattice mismatch, $Δ a / α$	ZnO	2.2%^[64]	18%^[65]	5.8%^[66]	16.6%^[67]	22%^[64]	0.09%^[6]
Thermal expansion coefficient, α (~300 K)/(×10^-6, K^-1)		α_a=3.43 α_c=3.34^[36]	α_a=7.5 α_c=8.5^[68]	α_a=3.2 α_c=3.1^[69]	α=2.55^[70]	α=5.73^[71]	α_a=5.59 α_c=10.2^[37]
Melting point/K		2770^[54]	2326^[72]	3100^[69]	1680^[73]	1500^[74]	2220^[38]
Thermal conductivity, λ (~300 K)/(W·cm^-1·K^-1)		λ_c=2.2^[75]	λ_c=0.23^[68]	λ_c=4.3^[76]	λ=1.3^[77]	λ=0.55^[78]	λ_c=0.062^[50]
Growth methods		HVPE MOCVD	Cz, KY, EFG	PVT	Cz	LEC, VB	Cz
Cost		High	Medium	High	Low	Low	Low

图11 SCAM衬底的再利用过程[58]

Fig. 11 SCAM substrate reuse process[58] (a) GaN film is naturally separated from SCAM substrate during the growth and cooling process of HVPE; (b) Separated SCAM substrate being cleaved with a razor blade to prepare the reusable SCAM substrate; (c) GaN film grown by MOVPE and HVPE being performed on the reusable SCAM substrate; (d, f) Photo and Nomarski microscope image of naturally separated SCAM substrate; (e, g) Photo and Nomarski microscope image of SCAM substrate cleaved with a razor blade; (h) AFM image of SCAM substrate cleaved with a razor blade

图12 不同激光重复频率在SCAM衬底上生长~300 nm GaN外延薄膜的AFM图像[85]

Fig. 12 AFM images of the ~300 nm-thick GaN epitaxial films grown on SCAM substrates with different laser repetition rates[85] (a) 10 Hz; (b) 20 Hz; (c) 30 Hz; (d) 40 Hz

图13 不同气氛下退火的SCAM衬底上生长的GaN外延薄膜[86]

Fig. 13 GaN epitaxial films grown on SCAM substrate annealed under different atmospheres[86] (a, b) RHEED patterns for as-grown GaN epitaxial films on SCAM annealed in (a) hydrogen and (b) ambient atmosphere. (c, d) SEM images for as-grown GaN epitaxial films on SCAM annealed in (c) hydrogen and (d) ambient atmosphere; (e, f) Surfaces of GaN epitaxial films after molten KOH etching for (c) and (d), respectively; (g, h) Schematic structures of SCAM annealed in (g) hydrogen and (h) ambient atmosphere; (i, j) HAADF-STEM images and schematic illustrations of (i) Ga-polarity and (j) N-polarity GaN, where the bright spots in the HAADF images indicates Ga atoms and the dark ones indicates N atoms with insets showing the simulated micrograph

图14 ZnO晶体结构示意图

Fig. 14 Crystal structural diagram of ZnO (a) Unit cell; (b) Distribution of [ZnO4] tetrahedron

图15 采用激光分子束外延技术在SCAM衬底上外延生长ZnO薄膜[65]

Fig. 15 ZnO films grown by laser-MBE on SCAM substrate[65] (a) Schematic illustration of the crystal structure of SCAM consisting of alternating layers of wurtzite AlMgO2.5 (0001) and rock salt ScO1.5 (111) layers; During epitaxy of ZnO, the wurtzite layer of SCAM is interconnected with the wurtzite layer of ZnO; (b, c) In-plane twisting (Δφ) and out-of-plane tilting (Δω) of epitaxial ZnO films on SCAM and sapphire substrates as a function of growth temperature; 1 Å=0.1 nm

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新型GaN与ZnO衬底ScAlMgO₄晶体的研究进展

Research Progress of ScAlMgO₄ Crystal: a Novel GaN and ZnO Substrate

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