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Development of Bulk Sic Single Crystal Grown by Physical Vapor Transport

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Development of Bulk Sic Single Crystal Grown by Physical Vapor Transport 中国科技论文在线 http://www.paper.edu.cn Optical Materials 23 (2003) 415–420 www.elsevier.com/locate/optmat Development of bulk SiC single crystal grown by physical vapor transport method Rongjiang Han a, Xiangang Xu a, Xiaobo Hu a,*, Naisen Yu a, Jiyang Wang a, Yulian Tian b, Wanxia Huang b a State Key Laboratory of Crystal Materials, Shandong University, Jinan 250100, PR China b Beijing Synchrotron Radiation Laboratory, Institute of High Energy Physics, Beijing 100039, PR China Abstract This paper reviews the development of bulk SiC single crystals grown by physical vapor transport method, including the polytype control, defects and doped consideration. In addition, defects in commercial 6H-SiC wafer, such as mic- ropipes, hexagonal voids and subgrain boundaries, are examined by transmission optical microscopy, X-ray syn- chrotron topography in back-reflection geometry and high-resolution X-ray diffraction methods. Ó 2003 Elsevier Science B.V. All rights reserved. PACS: 61.72.Dd; 81.05.Hd; 81.10.Bk Keywords: SiC; Crystal growth; Semiconductor; Defect 1. Introduction crystal is essential to realize the full potential ap- plication of this important semiconductor mate- The physical properties of silicon carbide (SiC) rial. In this paper, polytype control, defects and make this wide-band gap semiconductor well sui- doping for SiC crystals grown by physical vapor ted for high-temperature, high voltage, high- transport (PVT) method were reviewed. power, and high frequency electronic devices [1–3]. Furthermore, we examined micropipes, hexag- Many types of SiC-based electronic devices, in- onal voids and subgrain boundaries in commercial cluding power MESFETs, p–i–n diodes, Schottky 6H-SiC wafers using transmission optical micros- diodes, power MOSFETs, thyristor etc, are fabri- copy, X-ray synchrotron topography in back- cated. In addition, SiC will promote the realization reflection geometry and high-resolution X-ray of III-nitride-based optoelectronic devices because diffraction (HRXRD) methods. Optical micros- as a substrate it is considered superior to sapphire copy studies were carried out in the transmission for epitaxy of (Al, Ga, In)Ncompounds [4]. mode of the optical microscope (Opton, Germany). Therefore, the growth of high-quality SiC bulk X-ray back-reflection synchrotron topography ex- periments were performed at the 4W1A beam line of the topography station in Beijing synchrotron * Corresponding author. Fax: +86-531-8574135. radiation laboratory. HRXRD rocking curves E-mail address: [email protected] (X. Hu). were obtained using a D5005 X-ray diffractometer 0925-3467/03/$ - see front matter Ó 2003 Elsevier Science B.V. All rights reserved. doi:10.1016/S0925-3467(02)00330-0 转载 中国科技论文在线 http://www.paper.edu.cn 416 R. Han et al. / Optical Materials 23 (2003) 415–420 (Bruker-axs, Germany), in which a four-crystal 1800 °C, producing Si, SiC2 and Si2C vapors. monochromator was used for CuKa1 radiation. Based on this, SiC sublimation growth methods are developed. The Lely method [7], the first method of sublimation technique, is carried out in 2. Polytypism and basic properties of SiC argon ambient at about 2500 °C in a tight graphite container to prevent an escape of sublimation va- A striking structure property of SiC crystal is its pors from the growth chamber. As the SiC source polytypism [5]. SiC is the most prominent of a sublimes, the vapors penetrate a porous graph- family of close packed materials that exhibit a one- ite cylinder to produce lamellar crystals on its dimensional polymorphism called polytypism. So inner surface. The Lely platelets can exhibit far, over 250 SiC polytypes have been identified. good quality with micropipe densities of 1–3 cmÀ2 SiC polytypes are discriminated by the stacking and dislocation densities of 102–103 cmÀ2, respec- sequence of the tetrahedrally bonded Si–C bilay- tively. However, its primary drawback is uncon- ers, such that the individual bond lengths are trollable nucleation and dendrite-like growth. nearly identical, while the overall symmetry of the Also, the reliance on a porous graphite substrate crystal is determined by the stacking periodicity. limits the size of the SiC crystal (on the average, up SiC polytypes are divided into three basic crystal- to 3–5 mm). lographic categories: cubic (C), hexagonal (H) and Hence, a modified-Lely method [8] was devel- rhombohedral (R). 3C for cubic, 4H or 6H for oped in 1978. This method, also called physical hexagonal and 15R for rhombohedral are the vapor transport method or seeded sublimation common polytypes. An appreciation of potential method, has been further refined [6,9] for pro- of SiC for electronic applications can be obtained ducing larger SiC boules. The SiC seed crystal and from Table 1, which compares the relevant prop- the SiC source are placed in close proximity to erties of SiC with Si and GaAs. Despite numerical each other within a crucible. A temperature gra- values of some parameters being slightly different dient is established causing vapor phase transport in different literatures [1,3,6], the magnitude order of SiC species between the source and the seed, of them is consistent respectively. Due to the un- and the process is carried out at a low argon ique combination of high-saturated electron drift pressure. Now, it is successful to produce com- velocity, high breakdown electronic field, high mercial grade 4H- and 6H-SiC for wafer diameters thermal conductivity, wide band gap and excellent up to 100 mm. In addition, 15R-SiC [10] and 3C- stability, SiC is currently emerging as a very po- SiC [11] bulk single crystals had been successfully tential semiconductor material. grown by PVT method under appropriate growth conditions. Recently, Straubinger et al. [12] mod- ified the conventional PVT setup with an addi- 3. SiC bulk crystal grown by sublimation method tional gas pipe running through the lower isolation material and crucible wall into the growth cham- At atmospheric pressure, SiC does not melt but ber (M-PVT setup). High quality 6H- and 4H-SiC it undergoes sublimation at temperature above single crystals with an improved axial and lateral Table 1 Comparison of several important semiconductor material properties Properties Si GaAs 3C-SiC 6H-SiC 4H-SiC Band gap (eV) (T < 5 K) 1.12 1.43 2.40 3.02 3.26 Saturated electron drift velocity (107 cm/s) 1.0 2.0 2.5 2.0 2.0 Breakdown field (MV/cm) 0.25 0.3 2.12 2.5 2.2 Thermal conductivity (W cmÀ1 KÀ1) 1.5 0.5 3.2 4.9 3.7 Dielectric constant 11.8 12.8 9.7 9.7 9.7 Physical stability Good Fair Excellent Excellent Excellent 中国科技论文在线 http://www.paper.edu.cn R. Han et al. / Optical Materials 23 (2003) 415–420 417 Al-doping homogeneity were grown with the or 3C-SiC as seed crystal had been obtained by M-PVT setup. PVT with 1750 °C for seed crystal and 2250 °C for source materials [11]. A large temperature gradient (about 100 K cmÀ1) and a low pressure (<10À3 4. Polytype control of SiC bulk crystal growth mbar) were employed for 3C-SiC bulk crystal growth. SiC is a kind of polytypic material. Due to the Recent development of the crystal growth and low stacking fault energy [13], it is difficult to re- device fabrication for SiC crystals requires the strict syntaxy (parasitic polytype formation) dur- polytype identification. Raman scattering mea- ing the bulk crystal growth and thus to grow a surement [21], low temperature photoluminescence single polytype material. It is important to control [9] and infrared reflectivity [22] are all powerful the polytype for application to semiconductor tools to characterize SiC crystal non-destructively. devices because the band gap and electrical prop- erty of SiC varies with polytype. SiC crystal growth via sublimation is a complex 5. Defects in bulk SiC crystal process. The influences of growth parameters, such as growth temperature [14,15], supersaturation To meet the challenges of commercialization of [16,17] vapor phase composition and system pres- SiC semiconductors, specific efforts have been sure [16,18] and face polarity of seed crystal [19] on made towards larger diameter high quality SiC the polytype stability had been discussed. Among bulk crystals. Significant advances have been made them, the face polarity of seed crystals is one of in improving the quality of SiC crystals, especially most important growth parameters for controlling in the reduction of micropipe defects. However, the SiC polytype during PVT method. As well there are various defects in PVT-grown SiC crys- known, (0 0 0 1) faces of hexagonal and rhombo- tals, such as dislocations, micropipes, low-angle hedral SiC have different face polarity such as grain boundaries, stacking faults, hexagonal voids, (0 0 0 1)Si and (0 0 0 1)C face. The polytype of 6H- polytype inclusion, etc. The formation of these and 4H-SiC crystal, grown on [0 0 0 1] direction, is defects is related to the quality, the surface orien- mainly determined by the growth temperature as tation and the attachment of the seed [23] or the well as the polytype and face polarity of seed improper growth start conditions [24]. Further- crystal [14,19]. It was reported that 6H polytype more, the defects development depends on the crystal grew on (0 0 0 1)Si face and 4H polytype on growth orientation, possible stresses in the boule, (0 0 0 1)C face regardless of the seed polytype, growth front shape and temperature distribution which was attributed to the different surface free in the crucible. energy of the (0 0 0 1)Si and (0 0 0 1)C face. The Micropipes are hollow defects aligned along the polytype of PVT-grown SiC crystal depends upon c-axis in hexagonal or rhombohedral crystals, the growth direction.
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