WO2014034080A1 - Monocristal 3c-sic et son procédé de production - Google Patents

Monocristal 3c-sic et son procédé de production Download PDF

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Publication number
WO2014034080A1
WO2014034080A1 PCT/JP2013/005016 JP2013005016W WO2014034080A1 WO 2014034080 A1 WO2014034080 A1 WO 2014034080A1 JP 2013005016 W JP2013005016 W JP 2013005016W WO 2014034080 A1 WO2014034080 A1 WO 2014034080A1
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sic
crystal
single crystal
sic single
growth
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PCT/JP2013/005016
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English (en)
Japanese (ja)
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徹 宇治原
俊太 原田
和明 関
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国立大学法人名古屋大学
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Priority to JP2014532782A priority Critical patent/JP6296394B2/ja
Publication of WO2014034080A1 publication Critical patent/WO2014034080A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B19/00—Liquid-phase epitaxial-layer growth
    • C30B19/12—Liquid-phase epitaxial-layer growth characterised by the substrate
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/36—Carbides

Definitions

  • the present invention relates to a method of crystal growth of a SiC seed crystal to produce a 3C—SiC single crystal.
  • VLS vapor-liquid-solid
  • the present invention has been made in view of the above-described circumstances, and it is an object of the present invention to provide a method for producing a 3C-SiC single crystal while preferentially growing one of two types of 3C-SiC.
  • an off angle ⁇ is provided so that the normal line [0001] direction of the seed crystal surface is inclined by ⁇ °. It is particularly preferable to form the off angle ⁇ in the [1-100] direction on the surface of the seed crystal before forming the off angle, that is, the (0001) plane, but there is an acceptable range. In this range, the normal after the formation of the off angle is the rotation axis, and the direction rotated 90 ° from the normal direction toward the [1-100] direction (the [1-100] direction on the crystal surface after the formation of the off angle) Centering on a projection line of
  • 3C-SiC single crystal for solving the above problems is characterized in that 3C-SiC is formed on the (111) plane of the SiC seed crystal in a reaction atmosphere containing silicon (Si) and carbon (C). And a crystal growth process for step flow growth of a single crystal,
  • the SiC seed crystal is 3C—SiC in which an off angle is formed on the (111) plane,
  • the off-angle is a method of forming a range of ⁇ 15 ° in the [11-2] or [-1-12] direction from the (111) plane.
  • the formation direction of the off angle may be set as in the method shown in FIG.
  • the method for producing an SiC single crystal of the present invention preferably comprises any one of the following (1) to (4), and more preferably comprises a plurality of (1) to (4).
  • the seed crystal is step-flow grown by a liquid phase growth method in a raw material solution containing silicon (Si) and carbon (C).
  • Si silicon
  • C carbon
  • the off angle is formed so as to be in the range of ⁇ 10 ° in the [1-100] direction from the (0001) plane.
  • 3C—SiC is used as the SiC seed crystal, the off angle is formed so as to be in the range of ⁇ 10 ° in the [11-2] or [-1-12] direction from the (111) plane .
  • the 3C-SiC single crystal of the present invention which solves the above problems is manufactured by any of the above-mentioned manufacturing methods of the present invention, and one of two 3C-SiC crystals having different stacking order is compared with the other. Are included.
  • FIG. 5 is an explanatory view schematically showing the stacking order of atoms in 3C-SiC.
  • FIG. 5 is an explanatory view schematically showing the stacking order of atoms in 3C-SiC.
  • FIG. 5 is an explanatory view schematically showing an stacking order of atoms in 4H-SiC.
  • FIG. 6 is an explanatory view schematically showing the stacking order of atoms in 6H-SiC.
  • FIG. 3 is an explanatory view schematically showing a twin crystal of 3C—SiC. It is a microscope image by a Nomarski-type differential interference microscope of 3C-SiC single crystal in which a twin crystal is formed. It is an EBSD map image acquired based on the microscope image of FIG. FIG.
  • FIG. 5 is an explanatory view schematically showing the relationship between the crystal orientation of a 3C—SiC single crystal and the crystal growth rate.
  • FIG. 10 is an explanatory view schematically showing a step flow growth of 3C—SiC single crystal in [11-20] direction in a 6H—SiC seed crystal.
  • FIG. 6 is an explanatory view schematically showing a state in which 3C—SiC single crystal is step-flow grown in a [1-100] direction in a 6H—SiC seed crystal. It is explanatory drawing which represents typically the single-crystal growth apparatus used by embodiment.
  • FIG. 6 is an explanatory view showing a procedure of crystal growth in the method for producing 3C—SiC single crystal of Test 1.
  • 3C-SiC can be crystal-grown on a SiC seed crystal while suppressing generation of twins.
  • 3C-SiC (I) of lamination order ABCABCABC ... and ACBACBACB The 3C-SiC (II) of the lamination order of ... is simultaneously formed.
  • Such 3C-SiC (I) and 3C-SiC (II) are called twins because they have mirror symmetry. Crystal defects (DPB) are formed at twin boundaries.
  • FIG. 6 a microscope image obtained by imaging a 3C-SiC single crystal in which twins are formed with a Nomarski differential interference microscope (Olympus BH2-UMA) is shown in FIG.
  • 3C—SiC (I) and 3C—SiC (II) are confirmed on the surface of 3C—SiC single crystal in which twins are formed.
  • crystal defects are confirmed between 3C-SiC (I) and 3C-SiC (II).
  • An EBSD map image obtained based on this microscopic image is shown in FIG.
  • FIG. 7 on the surface of such a 3C-SiC single crystal, a region consisting of 3C-SiC (I) and a region consisting of 3C-SiC (II) are randomly arranged in a mosaic shape. There is.
  • the inventors of the present invention as a result of intensive research, have found that twin crystals can be suppressed by utilizing the orientation dependency at the time of crystal growth of 3C-SiC. That is, 3C—SiC has a fast direction of crystal growth and a slow direction. And, as shown in FIGS. 5 and 6, the crystal orientation of 3C—SiC (I) on the seed crystal and the crystal orientation of 3C—SiC (II) are different from each other.
  • 3C-SiC crystal is grown in the direction of high growth rate for 3C-SiC (I)
  • 3C-SiC (I) can be grown preferentially to 3C-SiC (II)
  • the growth of 3C-SiC (II) can be suppressed.
  • 3C-SiC (I) is covered with 3C-SiC (I)
  • the method of producing the 3C-SiC single crystal of the present invention will be more specifically described with reference to FIG. Due to the structure of the 3C-SiC single crystal, the step development rates of 3C-SiC oriented in the [1-10] direction along the step flow direction and 3C-SiC oriented in the [-110] direction are equivalent. On the other hand, for 3C-SiC oriented in the [11-2] direction along the step flow direction and 3C-SiC oriented in the [-1-12] direction, the [-1-12] direction is the step flow direction. The step evolution rate of SiC is higher. Therefore, in this case, it is expected that 3C-SiC in one stacking order will grow while covering 3C-SiC in the other stacking order, and finally 3C-SiC in one stacking order will be obtained. Ru.
  • the crystal structures of 3C-SiC are compared: [1-10] direction and [-110] direction of 3C-SiC Corresponds to the [11-20] direction of 6H-SiC, and the [11-2] direction and the [-1-12] direction of 3C-SiC correspond to the [1-100] direction of 6H-SiC.
  • the off substrate (SiC substrate) usually marketed is a crystal in which an off angle is provided in the [11-20] direction. When this off-substrate is used as a seed crystal, as shown in FIG.
  • a 3C—SiC single crystal is step-flow grown on a 6H—SiC substrate having an off angle in the [1-100] direction from the (0001) plane. Then, the step flow direction of this off-substrate, that is, 3C—SiC two-dimensionally nucleus-grown on the seed crystal is the [11-2] or [-1-12] direction.
  • the 3C—SiC single crystal due to the orientation dependency of the crystal growth rate described above, the 3C—SiC single crystal directs the high growth rate orientation in the step flow direction or the low growth rate orientation in the step flow direction. Therefore, a 3C-SiC single crystal (crystal on the left side in FIG. 10) with the slow growth direction oriented in the step flow direction is a 3C-SiC single crystal with the fast growth rate oriented in the step flow direction (FIG. 10 Covered by the right crystal).
  • 3C-SiC When 3C-SiC is used as a seed crystal, a step flow of 3C-SiC single crystal is performed on a 3C-SiC substrate with an off angle in the [-1-12] or [11-2] direction from the (111) plane. You can grow it.
  • the direction of the above-mentioned off-angle is [1-100] direction in 6H-SiC seed crystal and 4H-SiC seed crystal, and [11-2] direction and [11-2] direction in 3C-SiC seed crystal. Does not have to match.
  • the twin crystal growth rates become equivalent, that is, [11-20] direction in 6H-SiC crystal and 4H-SiC crystal, and [1-10] direction in 3C-SiC crystal. If a corner is provided and crystal growth is performed in the direction, it is difficult to suppress twins. However, it is possible to suppress at least a part of twins by crystal growth in directions other than this.
  • the off-angle is [1-100] direction in 6H-SiC crystal and 4H-SiC crystal, and [11-2] direction or [-1-12] direction in 3C-SiC crystal. It is preferable to provide at an angle close to.
  • the off angle in the range of [11-2] direction or [-1-12] ⁇ 15 ° from the (111) plane.
  • the [11-2] direction or the [-1-12] direction and the [1-10] direction appear alternately every 30 °. Therefore, if an off angle is provided in the range of ⁇ 15 ° that is the boundary with the [1-10] direction centering on the [11-2] direction or the [-1-12] direction, twin generation is suppressed it can.
  • the off angle is formed so as to be in the range of [1-100] direction ⁇ 10 ° from the (0001) plane. If the 3C-SiC single crystal is used as a seed crystal, form the off-angle so that it is within the range of ⁇ 10 ° in the [11-2] or [-1-12] direction from the (111) plane. Is good. Furthermore, in the case of using 6H-SiC single crystal or 4H-SiC single crystal as a seed crystal, it is preferable to form an off-angle so as to be within ⁇ 1 ° of [1-100] direction from the (0001) plane.
  • the 3C-SiC single crystal is used as the seed crystal, it is preferable to form the off-angle so as to be within the range of ⁇ 5 ° in the [11-2] or [-1-12] direction from the (111) plane. preferable. It is preferable to use 6H—SiC single crystal as the seed crystal.
  • the 3C—SiC single crystal growth method of the present invention may use liquid phase growth or vapor phase growth.
  • a general method such as a chemical vapor deposition (CVD) method or a physical vapor deposition (PVD) method can be used.
  • CVD chemical vapor deposition
  • PVD physical vapor deposition
  • 3C—SiC single crystal can be obtained by a CVD method using a silane gas and a hydrocarbon-based gas as a source gas.
  • SiC single crystal growth by the PVD method also called sublimation method
  • SiC powder is used as a raw material, the raw material is sublimed at a high temperature of 2000 ° C. or higher, and the seed crystal on which the vapor composed of Si and C is a low temperature Can be made supersaturated to precipitate the SiC single crystal.
  • a solution containing Si and C is used as a raw material solution.
  • a seed crystal is brought into contact with the raw material solution (SiC solution) to place the solution near at least the seed crystal in a supercooled state.
  • This causes the C concentration of the raw material solution to be in a supersaturated state in the vicinity of the seed crystal, and causes the SiC single crystal to grow (mainly epitaxial growth) on the seed crystal.
  • SiC solution raw material solution
  • the liquid phase growth method since crystal growth proceeds in an environment close to a thermal equilibrium state, it is possible to obtain a good quality 3C—SiC single crystal with a low density of defects such as stacking faults.
  • the off-angle is provided on the surface of the seed crystal in the direction according to the type of the seed crystal polymorphism, and the crystal is grown while controlling the step flow direction, twin crystals are reduced as described above.
  • the obtained 3C-SiC single crystal can be obtained.
  • the off angle can be formed by general cutting, but is not limited to this and can be formed by various methods.
  • the step width (terrace width) in the step flow direction is preferably larger.
  • the off angle provided to the seed crystal may be appropriately set within the above-described predetermined range in consideration of these.
  • the preferable range of the terrace width is 7 ⁇ m or more, more preferably 10 ⁇ m or more.
  • the seed crystal may be any single crystal of SiC, and various crystals represented by 3C—SiC, 4H—SiC, 6H—SiC can be used.
  • the single crystal growth apparatus 20 includes a crucible 21 made of carbon, a heating element 22 for heating the crucible 21, a holding element 23 capable of advancing and retracting to the inside of the crucible 21, and a crucible drive element 24 for rotating the crucible 21. And a chamber (not shown) for containing them.
  • the crucible 21 has a bottomed, substantially cylindrical shape that opens upward.
  • the inside diameter of the crucible 21 is 33 mm (or 45 mm), and the depth is 50 mm.
  • the heating element 22 is an induction heating heater.
  • the heating element 22 has a coiled lead 25 and a lead (not shown) for connecting the lead 25 to a power supply (not shown).
  • the conducting wire 25 is wound on the outside of the crucible 21 to form a coil coaxial with the crucible 21.
  • the holding element 23 has a rod-shaped dip shaft portion 26 and a dip shaft drive element 27 for advancing and retracting the dip shaft portion 26 in the longitudinal direction (vertical direction in FIG. 6) and rotating the dip shaft portion 26.
  • the diameter of the dip shaft 26 is 10 mm, and a holding portion 28 capable of holding the seed crystal 1 is formed at one end (lower end in FIG. 11) of the dip shaft 26 in the longitudinal direction.
  • the crucible 21 is formed.
  • the contained C was eluted into the Si melt in the crucible 21 to obtain a raw material solution 29.
  • the SiC seed crystal and the Si raw material were previously ultrasonic-cleaned in methanol, acetone and purified water (18 M ⁇ / cm), respectively.
  • the set temperature of the heating element 22 in the single crystal growth apparatus 20 was 1650 ° C. After the heating of the heating element 22 was started, the temperature was raised to 1450 ° C. in 27 minutes in the vicinity of the liquid surface of the raw material solution 29 in the crucible 21. Thereafter, the dip shaft 26 holding the SiC seed crystal 1 (hereinafter simply referred to as the seed crystal 1) was inserted into the crucible 1 (FIG. 11). Then, the temperature of the raw material solution 29 at the seed crystal holding position in the crucible 21 was raised to 1650 ° C. in 4 minutes. This is to clean the seed crystal 1 by melting the surface of the seed crystal 1. At this time, a temperature difference of 37 ° C.
  • seed crystal 1 6H—SiC single crystal (5 mm ⁇ 10 mm ⁇ 0.35 mm thickness) manufactured by vapor phase growth method (sublimation method) was used.
  • this 6H—SiC single crystal an off angle of 4 ° was provided in the [1-100] direction by cutting.
  • the seed crystal 1 is attached to the holder 28 so that the (0001) plane having the off angle faces the raw material solution 29 in the crucible 21 as shown in FIG.
  • the dip shaft 26 was advanced toward the inside of the crucible 21 to immerse the seed crystal 1 in the raw material solution 29. As described above, a temperature difference is formed in the raw material solution 29.
  • the SiC crystal grew on the surface of the seed crystal 1.
  • the dip shaft 26 is moved upward by the dip shaft driving element 27 and the seed crystal 1 (that is, SiC single crystal 10) which has been crystal grown is
  • the raw material solution 29 was pulled up.
  • the temperature in the crucible 21 was lowered to 700 ° C. by the heating element 22 in one hour while the seed crystals were in the chamber.
  • the seed crystal used in the method of producing the 3C—SiC single crystal of Test 1 has an off angle of 4 ° with respect to the (0001) plane. As described above, the short-time growth was performed, and the terrace width when 3C-SiC growth occurred was about 11 ⁇ m, and the height of the step calculated from this off angle was about 760 nm.
  • Test 2 The 3C-SiC of Test 1 is the method of producing 3C-SiC single crystal of Test 2 except that a 6H-SiC single crystal is provided with an off angle of 4 ° in the [11-20] direction as a seed crystal. It is the same method as the method of producing a single crystal.
  • a 3C-SiC single crystal of Test 2 was obtained by the method of producing a 3C-SiC single crystal of Test 2.
  • the size of the seed crystal 1 used in the test 2 was 5 mm ⁇ 10 mm ⁇ 0.25 mm in thickness.
  • Test 3 The method of producing the 3C-SiC single crystal of Test 3 is the 3C of Test 1 except that a 6H-SiC single crystal (so-called (0001) on-axis substrate) having no off angle is used as a seed crystal. The same method as the method of producing a SiC single crystal.
  • the 3C-SiC single crystal of Test 3 was obtained by the method of producing the 3C-SiC single crystal of Test 3.
  • the size of the seed crystal 1 used in Test 3 was 5 mm ⁇ 10 mm ⁇ 0.25 mm in thickness.
  • the SEM image of the 3C-SiC single crystal of Test 1 is shown in FIG. 13
  • the SEM image of the 3C-SiC single crystal of Test 2 is shown in FIG. 15
  • the SEM image of the 3C-SiC single crystal of Test 3 is shown in FIG. .
  • FIG. 14 shows the result of orientation mapping using EBSD for each of the regions shown in the SEM image of FIG.
  • the result of orientation mapping using EBSD is shown in FIG. 16 for each of the regions shown in the SEM image of FIG.
  • the result of orientation mapping using EBSD is shown in FIG. 18 for each of the regions shown in the SEM image of FIG.
  • the test was performed at intervals of 10 ⁇ m at an acceleration voltage of 10 kV using OIM (Orientation Imaging Microscopy) TM manufactured by EDAX.
  • OIM Orientation Imaging Microscopy
  • 3C—SiC crystals having different crystal orientations exist.
  • Test 3 in which the seed crystal was not provided with an off angle, twins were formed independently of the crystal orientation.
  • twin crystals are formed along the shape of the domain recognized by SEM.
  • 3C-SiC of Test 1 in which the off angle was provided in the [1-100] direction, only 3C-SiC of a single lamination cycle was observed.
  • 3C-SiC preferentially directed to the [-1-12] direction with respect to the step flow direction is grown. It is considered that the difference in the step development rate based on the crystal orientation of the two 3C-SiCs could reduce the 3C-SiC crystal of one lamination cycle and hence reduce the twins. Further, since no twin crystal was observed in the 3C-SiC single crystal of Test 1, it is understood that the twin crystal generation can be greatly reduced according to the method for producing 3C-SiC of the present invention.
  • the crystal surrounded by DPB had a size of about 100 ⁇ 100 ⁇ m 2 .
  • the manufacturing method of the present invention it has succeeded in obtaining a 3C—SiC single crystal substantially free of twins (that is, substantially free of crystal defects) in a large area of about 5 ⁇ 2 mm 2 .
  • the upper limit of the temperature difference is preferably 71 ° C. or less.
  • the temperature difference of the liquid phase is more preferably in the range of 23 ° C. to 71 ° C., and still more preferably in the range of 37 ° C. to 71 ° C.
  • the temperature difference of the liquid phase referred to here means the temperature of the raw material solution located in the vicinity of the highest temperature carbon-melted portion (in the embodiment, the inner bottom portion of the crucible 21) of the crucible 21 and the seed crystal It refers to the difference between the temperature of the raw material solution near the surface of 1.
  • This temperature difference can also be replaced by the difference between the temperature of the carbon melt in the crucible 21 and the surface temperature of the seed crystal 1.
  • the temperature difference may be a measured value or a calculated value.
  • the temperature gradient of the liquid phase refers to a value obtained by dividing the temperature difference between the two positions described above by the distance from the carbon melted portion of the crucible 21 to the surface of the seed crystal 1.
  • the direction of the temperature gradient with respect to the seed crystal is not particularly limited.
  • a temperature gradient may be provided in the direction perpendicular to the crystal growth plane, that is, the (0001) plane, or a temperature gradient may be provided in the parallel direction.
  • the degree of supersaturation can be calculated using the carbon solubility of the Si melt in the vicinity of the carbon melt and the carbon solubility of the Si melt in the vicinity of the crystal growth surface of the seed crystal. More specifically, the carbon solubility of the Si melt in the vicinity of the crystal growth surface of the seed crystal refers to the carbon solubility of the Si melt at a position adjacent to the crystal growth surface.
  • SiC seed crystal 10 SiC single crystal 20: single crystal growth apparatus 21: crucible 22: heating element 23: holding element 24: wedge driving element 25: lead 26: dip shaft 27: dip axis driving unit 28: holding unit 29: raw material solution

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Abstract

La présente invention concerne la fourniture d'un procédé de production d'un monocristal 3C-SiC, tout en établissant une priorité sur la croissance de l'un de deux types de 3C-SiC. Un 6H-SiC ou un 4H-SiC ayant un angle décalé, formé de manière à être compris dans une plage allant de la direction [1-100] ±15° depuis la surface (0001), est utilisé comme un germe de cristal et un monocristal 3C-SiC est amené à croître par écoulement sous forme de marches sur ce germe de cristal. De manière alternative, un 3C-SiC ayant un angle décalé, formé de manière à être compris dans une plage de la direction [11-2] ou [-1-12] ±15° depuis la surface (111) est utilisé comme un germe de cristal et un monocristal 3C-SiC est amené à croître par écoulement sous forme de marches sur ce germe de cristal.
PCT/JP2013/005016 2012-08-26 2013-08-26 Monocristal 3c-sic et son procédé de production WO2014034080A1 (fr)

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Cited By (7)

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JP2016056071A (ja) * 2014-09-11 2016-04-21 国立大学法人名古屋大学 炭化ケイ素の結晶の製造方法及び結晶製造装置
EP3260582A4 (fr) * 2015-02-18 2018-11-07 Showa Denko K.K. Procédé de production d'un lingot monocristallin de carbure de silicium et lingot monocristallin de carbure de silicium
EP3690085A4 (fr) * 2017-11-01 2021-07-07 Central Glass Co., Ltd. Procédé pour la production d'un monocristal de carbure de silicium
JP2021178762A (ja) * 2020-05-15 2021-11-18 株式会社Cusic ＳｉＣ積層体およびその製造方法ならびに半導体装置
JP2022021315A (ja) * 2020-07-21 2022-02-02 サイクリスタル ゲーエムベーハー 亀裂低減に最適な格子面配向を持つＳｉＣ結晶およびその製造方法
WO2023054264A1 (fr) 2021-09-30 2023-04-06 セントラル硝子株式会社 Tranche monocristalline de carbure de silicium et lingot monocristallin de carbure de silicium
WO2023054263A1 (fr) 2021-09-30 2023-04-06 セントラル硝子株式会社 Tranche de carbure de silicium monocristallin, lingot de carbure de silicium monocristallin et procédé de production de carbure de silicium monocristallin

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WO2023054264A1 (fr) 2021-09-30 2023-04-06 セントラル硝子株式会社 Tranche monocristalline de carbure de silicium et lingot monocristallin de carbure de silicium
WO2023054263A1 (fr) 2021-09-30 2023-04-06 セントラル硝子株式会社 Tranche de carbure de silicium monocristallin, lingot de carbure de silicium monocristallin et procédé de production de carbure de silicium monocristallin

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