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8 -inch SIC wafer preparation and extension application
2024/09/23
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Silicon carbide is one of the ideal electronic materials for making high temperature, high -frequency, and high -power electronic devices
Silicon carbide is one of the ideal electronic materials for making high-temperature, high-frequency, and high-power electronic devices. In the past 20 years, with the continuous improvement of silicon carbide material processing technology, its application field has continued to expand. At present, the preparation of silicon carbide chips is still mainly based on 6-inch (1 inch = 25.4 mm) wafers, but leading companies in the industry have begun to develop next-generation devices and chips based on 8-inch wafers. This project unites leading upstream and downstream companies in the domestic silicon carbide industry chain to promote the domestic development of 8-inch silicon carbide chips, especially the key wafer preparation and epitaxial application links. In this paper, an 8-inch 4HSiC substrate was prepared by diameter expansion growth, with an average BPD density as low as 251 cm-2 and an average TSD density of less than 1 cm-2, achieving an 8-inch substrate with near "zero TSD" and low BPD density, which can meet production needs. Using domestic 8-inch epitaxial equipment and developed process packages, a rapid epitaxial growth rate of 68.66 μm/h was achieved, with a thickness non-uniformity of 0.89% and a doping non-uniformity of 2.05%. These two indicators have reached the excellent level of 6-inch epitaxial film and can fully meet production needs. Compared with the 8-inch results published abroad, the thickness and doping uniformity are better than the foreign data, while the defect density is only 1/4 of the foreign data. Multiple wafer repeatability tests were designed and implemented to verify its stability.

0 introduction 

Since the development of the first generation of semiconductors, silicon wafers have evolved from 8 inches (1 inch = 25.4 mm) to 12 inches. Larger wafer sizes mean that more chips can be manufactured on a single wafer. Due to reduced edge loss, the larger the size, the greater the utilization area and utilization rate of the wafer, and the lower the cost of a single chip. The third generation of semiconductors is no exception. The development of silicon carbide (SiC) materials from 2 inches, 3 inches, 4 inches to 6 inches has proved that increasing the size can significantly improve the economic efficiency of SiC chip and device production. Currently, the silicon carbide industry is already promoting the development of 8-inch wafers, with a 50 mm increase in wafer diameter, a 78% increase in wafer area, and a nearly 90% increase in the number of chips cut out.

As a typical representative of the third generation of wide bandgap semiconductor materials, SiC has the characteristics of high critical breakdown field strength, high thermal conductivity, high electron saturation drift velocity, large bandgap width, and strong radiation resistance. It can meet the requirements of the next generation of power electronic equipment for power devices to work under harsh conditions such as higher power, smaller volume, and high temperature and high radiation. It has the advantages of reducing size, reducing power loss, and reducing cooling requirements. Silicon carbide has become an indispensable material for high-end applications in power electronics, and has brought revolutionary changes in new energy vehicles, photovoltaics, energy storage, rail transportation, smart grids and other fields. In the past few years, the popularity of electric vehicles has driven the continuous supply and demand of SiC power devices. At present, SiC power devices are mainly produced by 6-inch diameter wafers. The factory standards of 6-inch epitaxial wafers of mainstream epitaxial manufacturers are: thickness non-uniformity is not more than 3%, doping non-uniformity is not more than 6%, and triangle and drop defect density is not more than 0.5cm-2.。 

Leading companies in the SiC industry have been researching and developing 8-inch SiC wafers. Cree (now renamed Wolfspeed) and II-VI Incorporated (now renamed Coherent) demonstrated 8-inch SiC wafers in 2015. In 2022, Wolfspeed opened the world's first integrated 8-inch SiC chip factory. In Europe, the European SiC 8-inch pilot production line project REACTION (euRopEAn siC eighT Inches pilOt-liNe), composed of 27 partners from industry and academia, developed an 8-inch SiC pilot production line for the production of power devices in 2022. The project adopted a step-by-step development strategy to promote 8-inch SiC wafers. Low-quality mechanical-grade wafers are used to support the development of production line equipment compatible with 8-inch wafer sizes, test and optimize the processing capabilities of different production tools in the production line; high-quality process-grade wafers are used to grow epitaxial films, develop and optimize epitaxial process parameters, and ultimately produce power devices. The project carried out epitaxial growth on a horizontal commercial 8-inch machine developed by LPE. The indicators of the grown epitaxial film are as follows: thickness non-uniformity is 2.1%, and concentration non-uniformity is 3.3%. It can be seen that the non-uniformity of the epitaxial film has reached the commercially available level, which is a good progress. However, the defect rate is as high as 3.05 cm-2, of which the killer defect density is as high as 1.35 cm-2, which cannot meet the needs of back-end chip commercial mass production.

In the development of domestic 8-inch SiC wafers, from 2021 to the end of 2023, more than 10 companies and research institutions including Shandong University, Beijing Tianke Heda Semiconductor Co., Ltd. (referred to as "Tianke Heda"), Shanxi Shuoke Crystal Co., Ltd. (referred to as "Shanxi Shuoke"), and Guangzhou Nansha Wafer Semiconductor Technology Co., Ltd. (referred to as "Nansha Wafer") have successively released 8-inch conductive 4H-SiC substrate wafers, and also conducted a partition simulation study on the thermal field of the 8-inch crystal growth furnace. From the comparison in Table 1, it can be seen that although the research and development time is relatively late compared to foreign countries, the number and speed of domestic companies in the research and development of 8-inch wafers are rapidly catching up with foreign countries.

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The 8-inch epitaxy link of SiC is also developing rapidly in China. Xiamen University released the results of 8-inch 4H-SiC epitaxy in March 2023. The thickness and doping concentration non-uniformity are 2.3% and <7.5% respectively, and the surface defect density is <0.5 cm-2. It can also be seen from the data in Table 2 (as of January 1, 2024) that the 8-inch SiC epitaxy link in China is also developing rapidly.

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However, China lacks upstream and downstream industrial collaboration similar to REACTION, and Guangdong Tianyu Semiconductor Co., Ltd. (hereinafter referred to as "Guangdong Tianyu") has made some efforts and attempts in this regard by uniting upstream and downstream companies of substrates, equipment and chip devices, striving to promote the faster industrialization of China's 8-inch SiC. This article summarizes the pioneering work done by Guangdong Tianyu in different links of the 8-inch SiC production line in cooperation with upstream and downstream companies such as Nansha Wafer, Core Third Generation Semiconductor Technology (Suzhou) Co., Ltd. (hereinafter referred to as "Core Third Generation") and Pure Semiconductor (Ningbo) Co., Ltd. (hereinafter referred to as "Pure Semiconductor"), and introduces the testing of 8-inch SiC from crystal growth, wafer slicing and polishing, epitaxial film deposition to chip manufacturing. The results show that China is rapidly catching up with the international advanced level in this field.

1 、8-inch 4H-SiC ingot growth 

One of the difficulties in manufacturing 8-inch SiC is the growth of ingots. When the diameter is expanded from 6 inches to 8 inches, the difficulty of ingot growth will increase exponentially. The quality requirements of 8-inch seed crystals are higher, and it is necessary to solve the problems of uneven temperature field, gas-phase raw material distribution and transportation efficiency caused by large size, and crystal cracking caused by increased stress. The 8-inch 4H-SiC substrate wafers in this article are manufactured by Nansha Wafer. SiC single crystal growth adopts the mainstream physical vapor transport (PVT) method. The growth system includes a heating system, a cooling system and a thermal field zone composed of graphite materials. The typical growth schematic diagram is shown in Figure 1. SiC powder is placed at the bottom of a graphite crucible with a higher temperature. In an inert gas environment, the growth pressure is less than 30 mbar (1 mbar=100 Pa). It is heated to above 2200 °C. The SiC powder sublimates and decomposes into gas phase components such as Si, SiC2 and Si2C. Driven by the temperature gradient, the gas phase components are transported to the seed crystal placed on the top of the crucible with a lower temperature. The gas phase components in the supersaturated state on the surface of the seed crystal recrystallize to form SiC crystals. Based on the new generation of 8-inch SiC crystal growth furnace independently developed by Nansha Wafer, through multiple iterative optimizations, the optimized design of the temperature field and flow field of the large-size growth system was achieved. Combined with the high-quality 8-inch 4H-SiC seed crystal obtained by independent diameter expansion, a suitable proportion of nitrogen was introduced during the crystal growth process to grow high-quality 8-inch conductive 4HSiC single crystals. The surface of the ingot is smooth and flat without polymorphic inclusions.

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2 、Preparation of SiC ingot to 8-inch substrate wafer 

Another difficulty in the manufacture of 8-inch SiC is the substrate cutting process. The cutting process plays a vital role in the final quality of the substrate. The larger the size, the more significant the cutting stress and warping problems. The key points of cutting include crystal orientation, maximum yield, minimum material loss and processing cost, and low defect surface. After the grown crystal is rounded and flattened, an 8-inch conductive 4H-SiC ingot with a standard diameter is obtained, and then sliced by a multi-wire saw to obtain the original wafer. Then it is mechanically polished and chemically mechanically polished to obtain a low-roughness 8-inch conductive 4H-SiC substrate with a thickness of 500 μm, as shown in Figure 2. Some of the processing tools must be redesigned, and all the tools used need to fine-tune the process parameters according to the 8-inch requirements to ensure the quality of the wafer. As can be seen from Figure 2, the 8-inch 4H-SiC substrate is uniform brown-yellow. Combined with Raman testing, it shows that there are no polymorphic inclusions such as 6H and 15R-SiC in the substrate wafer, and the proportion of 4H crystal type is 100%.

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Nansha Wafer has delivered multiple batches of 8-inch substrates to Guangdong Tianyu. The substrates were characterized from the perspective of surface morphology and electrical properties. The average thickness of the delivered wafers measured by FlatMaster 200 was 500.8 μm, indicating that the slicing process provided good wafer-to-wafer repeatability; the average value of the total thickness variance (TTV) within the wafer was about 2.4 μm; the average warpage of the delivered wafers was 7.1 μm, which can meet the basic requirements of subsequent production equipment. The wafer resistivity measured by the non-contact atlas system LEI 1510 showed an average value of 22.8 mΩ∙cm for the delivered wafers, and the intra-wafer deviation was less than 3% within the target range of 15~25 mΩ∙cm. Wet etching is a fast and effective method for measuring the distribution of dislocation defects in substrates and is widely used in the industry. The Nansha Wafer Research Team used molten KOH to selectively etch the prepared 8-inch conductive 4H-SiC single crystal substrate, with an etching temperature of 450 ℃ and an etching time of 40~50 min. Due to the anisotropy of the corrosion rate, regular-shaped corrosion pits will form at the defect position. The etching rate of threading screw dislocation (TSD) is higher than that of threading edge dislocation (TED), making the corrosion pits of TSD larger than TED, so the two can be easily distinguished based on the microscope image. Mixed screw dislocation (TMD) is counted as TSD, while base plane dislocation (BPD) is a typical shell shape that can be easily identified and calculated. Under appropriate corrosion conditions, the dislocation defect corrosion pits on the Si surface of the SiC wafer are clear in shape, moderate in size, fully exposed and without overlap. The etched wafers were repeatedly cleaned with boiling alcohol and distilled water, and tested after being wiped dry. The dislocation defect detector (model LFMSiC) is used to automatically identify and count the number of characteristic corrosion pits corresponding to different types of dislocations. The equipment can accurately identify various types of dislocations, and the results of the visual recognition system are manually reviewed and confirmed to ensure the reliability of the results of the current method, thereby obtaining the TSD and BPD density and distribution of the 8-inch 4H-SiC substrate wafer. As shown in Figure 3, the average BPD density is 251cm-2, and the average TSD density is less than 1cm-2. The preparation of 8-inch conductive 4H-SiC single crystal substrate wafers with near "zero TSD" and low BPD density is achieved.   

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3、Growth of 4H-SiC epitaxial layer on 8-inch wafer and study of its repeatability

Unlike Si devices, SiC devices cannot be made directly on wafers. Instead, epitaxial films need to be deposited and grown on SiC wafers to make devices. Therefore, SiC epitaxy plays an important role in the industry chain. The homogeneous epitaxial growth experiment on 8-inch wafers in this study was conducted by Tianyu Semiconductor in its laboratory in Dongguan. The equipment used was a 6/8-inch compatible SiC epitaxial CVD equipment developed by Core 3D, and the wafer used was an 8-inch n-type 4H-SiC wafer provided by Nansha Wafer. Before the implementation of this study, Tianyu had completed the commissioning and production of 6-inch epitaxy on this equipment. Previous research and production practices have proven the good performance of the equipment on 6-inch silicon carbide epitaxy. Core 3D assisted Tianyu Semiconductor in upgrading the equipment to 8 inches, updating and enlarging the temperature field and flow field consumables. The equipment is a vertical air intake hot wall type, and is also equipped with high-speed wafer rotation technology. Before epitaxy, H2 and HCl gases are used for etching and surface preparation. The epitaxial growth temperature is about 1600°C, the growth gases are trichlorosilane (SiHCl3) and ethylene (C2H4), and the doping gas is nitrogen.

In this study, epitaxial growth at a rate of 68.66 μm/h was achieved on an 8-inch wafer, and an epitaxial layer with a nominal thickness of 11.44 μm and a doping concentration of 10.50×1015 cm-3 was obtained. The thickness of the epitaxial layer was measured by infrared fast Fourier transform spectroscopy (FT-IR), the doping concentration was measured by mercury probe method, the surface roughness of the epitaxial film was detected by atomic force microscopy (AFM), and the surface defects were observed by Sica88 surface inspection system. Figures 4 and 5 show the radial distribution of the thickness and doping concentration of the epitaxial layer grown on an 8-inch SiC wafer, respectively. The average thickness of the epitaxial layer is 11.44 μm, the standard deviation is 0.10 μm, and the thickness non-uniformity evaluated by the ratio of standard deviation to average value is 0.89%. The average doping concentration of the epitaxial layer is 10.50×1015cm-3, the standard deviation is 0.22×1015cm-3, the doping non-uniformity is 2.05%, and the AFM characterization results show that the surface root mean square roughness is 0.162 nm, and the triangle + drop defect density is 0.11 cm-2. Compared with the factory standard of epitaxial wafers, it can be found that the non-uniformity and killer defect density of this experimental result are better than the 8-inch epitaxial wafer data published in Table 2, and also reach the level of 6-inch excellent epitaxial wafers, which fully meets the indicators required for mass shipments.

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In order to further investigate the repeatability and stability of epitaxial growth on 8-inch wafers, this study used the same menu and conducted repeatability tests under exactly the same epitaxial conditions. Two more repeatable epitaxial growths were performed, and the repeatability results are shown in Tables 3 and 4. As can be seen from Table 3, the film thickness and doping concentration inter-wafer non-uniformity are 4.25% and 4.11% respectively. At present, the industry has not established universal requirements for the inter-wafer non-uniformity of 8-inch epitaxial wafers. The inter-wafer non-uniformity requirements of 6-inch epitaxial wafers for reference are: thickness 4% and concentration 6%. Considering that 8-inch epitaxial wafers are in the research and development stage, the requirements for them are usually lower than the general production requirements for 6-inch epitaxial wafers. In contrast, it can be found that in the result data of this study, the non-uniformity of the doping concentration of 8-inch epitaxial wafers is 4.11%, which has reached the production requirement of 6 inches, while the non-uniformity of the film thickness is 4.25%, which exceeds the production requirement of 6 inches, and needs to be further improved, but the repeatability has reached a very good level. As can be seen from Table 4, the average value of the triangle + drop defect density of the three wafers is 0.12 cm-2, which fully meets the general shipping requirement of the triangle + drop defect density of 6-inch epitaxial wafers not exceeding 0.5 cm-2. Therefore, it can be preliminarily concluded that the 8-inch epitaxial wafer has good repeatability and good stability under this study, and can be used for large-scale trial production and further mass production research and optimization.。

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According to the analysis of Han Yuebin and others, the flow field of the vertical epitaxial equipment can easily achieve high uniformity due to the zoned spraying and uniform air intake, and the temperature field can easily achieve high uniformity due to the layered multi-zone compensation. After being enlarged to 8 inches, the advantages are well maintained, so the 8-inch epitaxy continues the high uniformity of the 6-inch; and the cooling system inside the shower head ensures that the top plate temperature is much lower than the growth temperature of the heterocrystalline SiC, thereby minimizing the generation of deposits. Combined with the high-speed rotation, the ejection effect of the small amount of particles generated makes it difficult for dropped defects and the "headed triangle defect" caused by dropped objects to form. Combined with this, the killer defect density is greatly reduced, and the maintenance cycle is greatly extended, which is more suitable for the needs of large-scale mass production.

3、Initial operation and device compatibility testing on chip product lines 

Some characteristics of the wafer, such as thickness and resistivity fluctuations, curvature, edge cracks and surface defects, may seriously affect or even damage some tools on the chip manufacturing production line, so advance compatibility testing is necessary. The 8-inch SiC epitaxial wafers were sent to Pure Semiconductor for operation and compatibility testing of the production tools of the 8-inch SiC chip production line. After testing and modification, it was finally verified that the main equipment required for the production of power devices can handle 8-inch SiC wafers, such as automatic inspection tools, lithography steppers, ion implanters, heat treatment machines and oxidation furnaces, reactors for depositing dielectric and metal films, wet etcher, etc. The success of these modifications and verifications is an important step towards achieving industrial mass production. Compatibility testing found alignment problems within the tool in the edge area, defects were found by automatic electron microscopy inspection, and some deficiencies in the slicing and polishing steps in the wafer manufacturing process were found by analyzing the type and location of the defects. The information was fed back to Nansha Wafer for further optimization.

5、in conclusion 

Achieving high-quality 8-inch SiC wafer manufacturing and epitaxial growth is a fundamental step in promoting the production of next-generation large-size power devices. This article outlines the establishment and progress of the 8-inch SiC wafer industrial test line under the coordination of Guangdong Tianyu. The ingot was grown by expanding the diameter using a new PVD crystal growth furnace, and the 8-inch SiC substrate wafer was obtained after cutting, grinding and polishing. The measurement results show that the average BPD density of the 8-inch SiC substrate wafer is as low as 251 cm-2, and the average TSD density is less than 1 cm-2, achieving an 8-inch substrate with near "zero TSD" and low BPD density, which can meet the requirements of epitaxy and chip processing production. Using vertical SiC domestic epitaxial equipment, epitaxial growth was carried out on domestic 8-inch wafers developed by Nansha Wafer Company in Tianyu Semiconductor Laboratory, achieving a rapid epitaxial growth rate of 68.66 μm/h, a thickness non-uniformity of 0.89%, and a doping non-uniformity of 2.05%. These two indicators and defect density have reached the excellent level of 6-inch epitaxial film, which can fully meet production needs. Compared with the results published abroad, the thickness and doping uniformity are better than the foreign data, while the defect density is only 1/4 of the foreign data. The results of the repeatability test found that the 8-inch epitaxy in this study has good repeatability and good stability, and can be used for large-scale trial production and further mass production research and optimization. The chip production line production tools were tested and improved using 8-inch wafers to achieve 8-inch compatibility. This research work has taken an important step in promoting large-scale chip manufacturing of 8-inch SiC wafers. This study proves that the localization of equipment and materials in the entire SiC industry chain has made great achievements. After several years of catching up with the 6-inch industrialization, domestic companies have caught up in the 8-inch SiC industrialization, and have done better than foreign countries in wafer preparation and epitaxy.

The core goal of the SiC industry's transition to 8-inch wafers is to reduce costs and expand applications. At present, the research on 8-inch SiC wafer preparation and epitaxial application has solved the problem of going from scratch. Looking forward to future research directions, the next step will focus on continued optimization to improve efficiency and reduce costs in mass production. At the same time, it is necessary to continue 8-inch batch testing and mass production in subsequent chip manufacturing links to discover improvements in materials and equipment, further improve stability and reduce defect rates, study equipment repeatability, continue process optimization, promote the rapid industrialization and localization of 8-inch SiC epitaxy, and promote the entire industry to leap to large sizes.



Source: Journal of Synthetic Crystals 

Source: China Industrial Ceramics






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