Name: Sun Jiaqi

Abstract: Silicon carbide (SiC) devices have broad development prospects in high-power electronic devices, optoelectronic devices, and other high-temperature applications due to their advantages such as high frequency and efficiency, high pressure and high temperature resistance, strong radiation resistance, and stable chemical properties. The Physical Vapor Transmission (PVT) method, as the most widely used and industrialized technology in the preparation of single crystal silicon carbide, has been extensively studied by many predecessors. This article focuses on the preparation of single crystal silicon carbide by PVT method, combined with recent research progress, summarizes the process influencing factors of PVT method for preparing silicon carbide, including temperature distribution, atmosphere control, powder purity, working pressure, and growth time, and explains their influence mechanism on the growth of silicon carbide crystals. Finally, the difficulties and challenges faced by PVT method in preparing SiC were analyzed, such as crystal defect control, stress control, large-scale SiC growth, P-type substrate preparation, cost control, etc. With the increasing demand for silicon carbide in the field of electronic devices, how to further control crystal defects, improve crystal size, and reduce production costs will be the focus of future research.
Keywords: silicon carbide, SiC， Physical gas-phase transport, PVT， Temperature, crystal defects, large size

1、 Introduction
Currently, in order to alleviate the global energy security issues and achieve the “dual carbon” goal, power electronic devices are developing towards high-frequency, integrated, standardized modular, and intelligent directions. However, the physical limitations and bottlenecks of traditional silicon-based devices are becoming increasingly prominent, making it difficult to adapt to the more complex electronic and electrical architecture requirements of future terminal applications [1,2]. In contrast, third-generation compound semiconductor materials have the advantages of large bandgap, high breakdown field strength, high thermal conductivity, high electron mobility, and strong radiation resistance, which can effectively break through the limitations of key material performance indicators and significantly improve device efficiency. They have strategic and market-oriented dual characteristics and have become the forefront of wide bandgap semiconductor technology research and industry competition focus [3,4].
Devices such as Schottky diodes (SBDs) and metal oxide semiconductor field-effect transistors (MOSFETs) prepared by 4H SiC have been widely used in electric vehicles, photovoltaic inverters, and industrial power sources. Compared to traditional silicon devices, SiC devices have higher efficiency and stronger high-temperature resistance. SiC materials have excellent UV response characteristics and are widely used in optoelectronic devices such as UV detectors and light-emitting diodes (LEDs). Especially in the deep ultraviolet band, 4H SiC and 6H SiC have become ideal materials for ultraviolet detectors due to their large bandgap and radiation resistance. The thermal stability of SiC enables it to maintain good electronic properties even in high temperature environments, making it suitable for use in high-temperature sensors and electronic devices. It has been widely applied in sensor technology in extreme environments such as aerospace and automotive engine monitoring. Therefore, high-quality silicon carbide single crystals have a wide range of applications and broad development prospects in high-power electronic devices, optoelectronic devices, and other high-temperature applications.
2、 Introduction to Silicon Carbide
Silicon carbide (SiC) is a compound semiconductor composed of carbon and silicon elements, as shown in Figure 1, where carbon and silicon atoms form a covalent tetrahedral structure in the form of Si-C double atomic layers [5]. The actual crystal structure of SiC exceeds 200 types (different crystal structures are defined by the number of stacking layers and the symmetry type of crystals in the unit cell), among which the most widely used and studied are 3C SiC, 4H SiC, and 6H SiC (C represents cubic crystal system, H represents hexagonal crystal system), and the corresponding stacking sequence is shown in Figure 2 [6]. Due to their excellent properties such as wide bandgap, high thermal conductivity, high temperature resistance, and radiation resistance [7,8], 4H SiC and 6H SiC have important applications in high-power electronic devices, optoelectronic devices, and high-temperature structural materials [9,10].
Figure 1 SiC tetrahedral structure [5] Figure 2 Three different stacking sequences of SiC [6]
However, to fully realize the excellent performance of devices based on SiC, the growth of high-quality single crystal SiC and the processing technology of chips are key. There are various methods for preparing silicon carbide, mainly including physical vapor transfer (PVT), high-temperature chemical vapor deposition (HTCVD), and liquid phase deposition (LPE) [11]. Among them, the Physical Vapor Transport (PVT) method is one of the most commonly used techniques for preparing single crystal silicon carbide, particularly suitable for producing high-quality large-sized single crystal SiC [12]. The PVT method has the advantages of relatively simple process, low cost, and suitability for large-scale production, and has been widely applied in industrialization, occupying an important position in the research of SiC material preparation [13].
3、 The basic principle of PVT method for preparing silicon carbide
The PVT method for preparing SiC is based on the sublimation and recrystallization process of silicon carbide at high temperatures [14]. The main device structure is shown in Figure 3, consisting of a graphite crucible, SiC powder source, seed crystal, induction coil, and insulation layer [15].
Figure 3 Schematic diagram of the structure of SiC single crystal growth device using PVT method [15]
SiC powder is usually placed in a high-temperature graphite crucible, and under the eddy current heating effect of an induction coil, it is decomposed into gaseous silicon and carbon compounds (such as Si, Si ₂ C, SiC ₂, etc.) in a low-pressure high-temperature inert atmosphere at 2000-3000 ℃. The generated gas-phase substances flow towards the low-temperature seed crystal region under the combined action of concentration gradient and pressure gradient. During the flow process, as the temperature gradually decreases, the gas-phase substance gradually deviates from chemical equilibrium and becomes supersaturated, leading to recrystallization with the seed crystal fixed at the top of the crucible as the nucleation center, forming silicon carbide crystals [16]. This process can be summarized into three stages:
(1) Sublimation stage: SiC source material undergoes sublimation at high temperatures, forming gaseous Si and C compounds.
(2) Gas phase transport stage: sublimated gaseous molecules are transported from a high temperature zone to a lower temperature substrate surface through a carrier gas (usually argon).
(3) Deposition and crystal growth stage: Gaseous substances condense and react on the substrate surface, forming solid SiC crystals again.
At present, the maximum growth rate of silicon carbide crystals using PVT method can reach 1-2 mm/h [17]. The PVT method can control the growth rate, crystal quality, and size of SiC crystals by controlling conditions such as temperature gradient, atmosphere, and pressure.
4、 Process influencing factors of PVT method for preparing silicon carbide
(1) Temperature distribution
At present, the large-scale industrial physical gas transmission method uses intermediate frequency induction coils as heating power sources, and high-density graphite heating elements will be heated under the action of eddy currents. Fill the bottom of the graphite crucible with SiC powder, bond SiC seed crystals inside the graphite crucible cover at a certain distance from the raw material surface, and then place the graphite crucible as a whole in the graphite heating element. By adjusting the temperature of the external graphite felt, place the SiC raw material in the high temperature zone and the SiC seed crystals in the low temperature zone. At temperatures exceeding 2000 ℃, silicon carbide raw materials decompose into gas phase substances such as sublimated Si atoms, SiC2 molecules, and Si2C molecules. The gas phase substances are transported to the low-temperature region under the drive of temperature gradient and grow into SiC crystals on the C surface of SiC seed crystals. Usually, the temperature of SiC source material in the high-temperature region is above 2000 ℃, while the temperature in the substrate region is relatively low, forming a temperature gradient that drives gas-phase transport. A large temperature gradient may lead to defects or cracks within the crystal, while a small gradient can reduce the growth rate. As shown in Figure 4, SiC crystal forms have different relative proportions at different temperatures and can transform into each other at a certain temperature [18]. Therefore, the SiC crystal growth process of PVT method depends on the temperature distribution inside the furnace cavity. Li Pengcheng, Chen Yanyu, Jin Liyan, and others have all conducted optimization research on the temperature distribution in PVT equipment. By adjusting the coil position height, crucible rotation rate, heating power, cavity shape, and insulation layer design, the temperature distribution inside the cavity has been optimized [19-21], thereby reducing defects such as microtubes and dislocations and improving the size and quality of SiC.
Figure 4: Relationship between SiC crystal structure and temperature grown by PVT method [18]
(2) Atmosphere control
The atmosphere for gas-phase transmission usually uses inert gases such as argon. Appropriate gas flow rate and pressure can promote the transport and deposition of SiC molecules. Trace impurities in the atmosphere, such as oxygen or nitrogen, may react with SiC to form unexpected compounds, thereby affecting crystal quality [22]. Guo Jindi adjusted the hardness of the generated SiC by doping nitrogen gas [23]. When YANG YING used PVT method to grow SiC, he controlled the atmosphere more accurately, increased the growth gas flow rate, avoided N2 doping, and reduced the density of edge dislocations (TED) [24], thus improving the quality of single crystal SiC. Therefore, it is crucial to strictly control the purity of the atmosphere.
(3) Powder purity
SiC powder as a synthetic raw material directly affects the growth quality and electrical properties of SiC single crystals. Chen Zhizhan et al. studied the phase changes of SiC powder during the growth process and its effects on the uniformity and defects of single crystals. They found that when using β – SiC powder to grow SiC single crystals, there is a phase transition to α – SiC during the crystal growth process, which causes a significant change in the Si/C molar ratio in the gas phase composition and has adverse effects on crystal growth. In order to improve crystal uniformity and reduce defects such as microtubes, it is necessary to perform pre firing treatment on the raw materials. On the one hand, it promotes the transformation of crystal structure and increases the particle size of the powder, and on the other hand, it reduces the impurity content of the raw materials [25]. Shin et al. studied the effect of SiC powders with different particle sizes and impurity contents on the growth of SiC single crystals, and found that most of the impurities in the single crystals come from SiC powders. The quality of the single crystal is linearly related to the purity of the powder. High purity powder is beneficial for reducing the density of basal plane dislocations (BPD) in 4H SiC [26]. Wang Dian, Hu Zhichen, Gao Pan, Li Bin, Ma Kangfu and others have obtained high-purity silicon carbide powder by improving the process of preparing SiC powder and related parameters such as temperature and atmosphere [27-31], laying an important foundation for the subsequent growth of large-sized, low defect density high-quality single crystal SiC.
(4) Pressure inside the cavity
The working pressure of the system has a direct impact on the sublimation process and gas-phase transport process. High vacuum reduces impurities and lower pressure helps to increase the sublimation rate of SiC; However, excessively low pressure may result in the loss of sublimated substances during transport, affecting the rate of crystal growth. The general pressure range is 1-100 Torr, which needs to be optimized according to specific growth goals. Currently, there is limited research in this area.
(5) Growth time
The PVT method is usually a long-term crystal growth process, with growth times ranging from tens to hundreds of hours. Extending the growth time can increase the thickness of the crystal, but it also increases the risk of thermal stress and defect formation [32]. Therefore, reasonable growth time control is the key to ensuring crystal quality.
5、 Structure and Properties of Silicon Carbide Prepared by PVT Method
By optimizing the process parameters of PVT method, SiC single crystals of different crystal forms can be prepared, mainly including three crystal forms: 3C SiC, 4H SiC, and 6H SiC. The structural and performance differences of these crystal forms make them suitable for different application fields.
3C SiC is a cubic crystal structure in SiC with a small bandgap (about 2.3 eV) and high electron mobility, making it suitable for high-frequency electronic devices. However, the preparation of 3C SiC crystals is difficult and prone to defects, which limits their applications. 4H SiC is currently the most widely studied and applied SiC crystal form [33-36], with a large bandgap (about 3.3 eV) and high breakdown field strength, suitable for high-power, high-temperature electronic devices. Because 4H SiC crystal growth has good stability and fewer defects, it is the preferred material for power semiconductor devices. 6H SiC is also a common SiC polytope structure with a bandgap of approximately 3.0 eV and slightly lower electron mobility than 4H SiC. However, its growth technology is mature and the crystal quality is high, making it widely used in optoelectronic and electronic devices.
6、 Difficulties and challenges in preparing SiC by PVT method
Although significant progress has been made in the preparation of high-quality silicon carbide single crystals using PVT method, there are still some technical challenges that need to be overcome to further promote its application.
Firstly, crystal defect control. Although PVT method can prepare larger SiC single crystals, when the size is expanded to 8 inches, thermal stress increases and defect control becomes more difficult. Defects such as dislocations, stacking faults, and vacancies may still appear in the crystal [10,37]. These defects can affect the electrical performance and stability of the device [38-40]. At present, the TSD density of commercial 6-inch conductive 4H SiC substrates is controlled below 200 cm-2, while the TSD/BPD density of Youpin is less than 50 cm-2, the BPD density is below 800 cm-2, and the TSD/BPD density of Youpin is less than 500 cm-2 [41]. Therefore, how to reduce defect density by optimizing process conditions is currently the focus of research. In 2022, Shandong University and Nansha Wafer successfully prepared 8-inch conductive 4H SiC single crystal substrates with low micro tube density and high crystalline quality. Recently, significant breakthroughs have been made in controlling dislocation defects on 8-inch SiC substrates, and 8-inch conductive 4H SiC single crystal substrates with near zero screw dislocation (TSD) and low basal plane dislocation (BPD) densities have been prepared [32].

Next is stress control. During the growth process of PVT, SiC single crystals are prone to thermal stress due to temperature gradients and differences in thermal expansion coefficients, which can lead to crystal cracking or increased defects [42,43]. How to effectively control stress and avoid the formation of internal cracks in crystals is an important issue in improving the quality of SiC crystals.
Next is the preparation of large-sized single-crystal SiC. With the increasing demand for SiC in electronic devices, preparing larger sizes (such as 8 inches or even 12 inches) and high-quality SiC single crystals has become a major challenge. Expanding the size of SiC substrates is one of the important ways to increase production capacity and reduce costs. The current PVT method is mainly capable of stable preparation of 4-inch and 6-inch SiC chips, and further expansion of chip size still requires addressing material uniformity and growth rate issues. At present, the diameter of silicon carbide single crystals at home and abroad can generally reach 6 inches [44-46], but their thickness is usually between 20-30 mm, resulting in a limited number of silicon carbide substrate slices obtained from a silicon carbide ingot slice. The main challenge in increasing the thickness of silicon carbide single crystals is the increase in thickness during growth and the change in the internal thermal field of the growth chamber due to the consumption of source powder. The Advanced Semiconductor Research Institute Dry Crystal Semiconductor Joint Laboratory of Zhejiang University Hangzhou International Science and Technology Innovation Center (referred to as the Innovation Center) uses pulling seed crystals and already grown crystals to keep the crystal growth surface under a suitable radial temperature gradient, forming a surface morphology that is conducive to reducing crystal stress. By using the Czochralski physical vapor transmission method, the joint laboratory successfully grew a silicon carbide single crystal with a diameter of 6 inches (150 mm), and its thickness exceeded 100 mm. The results of the tested substrate showed that the ultra thick silicon carbide single crystal had a single 4H crystal structure [47]. The implementation of this thickness not only saves the amount of expensive silicon carbide seed crystals, but also doubles the number of silicon carbide substrate slices obtained from a silicon carbide single crystal ingot slice, which can significantly reduce the cost of silicon carbide substrates and is expected to strongly promote the development of the semiconductor silicon carbide industry.
In addition, among the current single crystal SiC substrates, there are more N-type substrates and the progress of P-type substrates is slower. P-type SiC is an ideal substrate for preparing high-power power electronic devices, but its resistivity is difficult to reduce, and its P-type doping technology is still in the research stage. Due to the difficulties of P-type doping, such as high acceptor ionization energy leading to high substrate resistivity; Lack of suitable gas doping sources leads to uneven doping; The high vapor pressure of the acceptor element causes a large number of defects in the crystal, making it relatively difficult to grow P-type bulk SiC [48].
Finally, although PVT method has relatively low cost, it still faces the problem of high production cost under high temperature and high energy consumption process conditions. The price of SiC substrate is still much higher than that of Si, sapphire and other substrates. Reducing costs requires more mature growth and processing technologies. On the one hand, it is necessary to improve the yield of substrate materials, and on the other hand, it is necessary to increase the area through diameter expansion research to reduce the cost of individual devices. Therefore, improving crystal growth rate, reducing production energy consumption, and ensuring crystal quality are key directions for future process improvement.
6、 Summary and Prospect
SiC devices are widely used in power electronics fields such as rail transit, wind power, photovoltaics, new energy vehicles, and uninterruptible power supplies due to their superior properties of high frequency efficiency, high voltage resistance, high temperature resistance, strong radiation resistance, and stable chemical properties. The Physical Vapor Transmission (PVT) method, as the core technology for the preparation of silicon carbide single crystals, has shown great potential in the material preparation of high-power electronic and optoelectronic devices. By optimizing process conditions, controlling crystal defects and stress, PVT method can prepare high-quality 4H SiC and 6H SiC single crystals, which have broad application prospects in high-temperature, high-pressure, and high-frequency devices. However, with the increasing demand for silicon carbide in the field of electronic devices, how to further improve crystal size, reduce costs, and control crystal defects will be the focus of future research.

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