Crucible having an improved crystal growth base for manufacturing silicon carbide single crystal and method of use
11708646 · 2023-07-25
Assignee
Inventors
Cpc classification
H01L21/02271
ELECTRICITY
International classification
C30B35/00
CHEMISTRY; METALLURGY
C30B23/06
CHEMISTRY; METALLURGY
Abstract
A silicon carbide single crystal manufacturing apparatus includes a crucible constituted by a crucible body and a crucible lid and a base having a crucible lid side surface supported by the lower surface of the crucible lid, and a seed crystal mounting surface on which the seed crystal is mounted and which is a surface on the opposite side of the crucible lid side surface, wherein the base is made of graphite material, the area of the seed crystal mounting surface is larger than the area of the crucible lid side surface, and the base has at least of a portion in which the cross-sectional area orthogonal to the vertical direction connecting the crucible lid side surface and the seed crystal mounting surface is gradually reduced, and a portion that is getting smaller gradually, from the surface of the seed crystal mounting surface toward the crucible lid side surface.
Claims
1. A silicon carbide single crystal manufacturing apparatus, comprising: a crucible comprising a crucible body and a crucible lid; and a base comprising a crucible lid side surface supported by a lower surface of the crucible lid and a seed crystal mounting surface operable to have a seed crystal mounted thereon, wherein the seed crystal mounting surface is disposed on a side of the base opposite from the crucible lid side surface, wherein the base is made of graphite material, the area of the seed crystal mounting surface is larger than the area of the crucible lid side surface, and a cross-sectional area of the base orthogonal to a vertical direction connecting the crucible lid side surface and the seed crystal mounting surface is continuously reduced from the seed crystal mounting surface toward the crucible lid side surface.
2. The silicon carbide single crystal manufacturing apparatus according to claim 1, wherein the base has a truncated cone shape.
3. The silicon carbide single crystal manufacturing apparatus according to claim 1, wherein, assuming that the crucible lid side surface of the base is circular and has a radius r1, the seed crystal mounting surface is circular and has a radius r2, and a height of the base is h, (r2−r1)/h>0.15 is satisfied.
4. The silicon carbide single crystal manufacturing apparatus according to claim 3, wherein the radius r1, the radius r2, and the height h satisfy (r2−r1)/h>0.30.
5. The silicon carbide single crystal manufacturing apparatus according to claim 1, wherein the base is made of a graphite material with a Young's modulus of 5 GPa or more.
6. A method of manufacturing a silicon carbide single crystal, comprising: providing a crucible comprising a crucible body, a crucible lid and a base, the base comprising a crucible lid side surface supported by a lower surface of the crucible lid and a seed crystal mounting surface operable to have a seed crystal mounted thereon, wherein the seed crystal mounting surface is disposed on a side of the base opposite from the crucible lid side surface; mounting the seed crystal to the seed crystal mounting surface and placing a silicon carbide raw material in the crucibles; sublimating the silicon carbide raw material to form a sublimation gas; and precipitating the sublimation gas on the seed crystal to grow the silicon carbide single crystal, wherein the base is made of graphite material, an area of the seed crystal mounting surface is larger than an area of the crucible lid side surface, and a cross-sectional area of the base orthogonal to a vertical direction connecting the crucible lid side surface and the seed crystal mounting surface is continuously reduced from the seed crystal mounting surface toward the crucible lid side surface.
7. The method of manufacturing a silicon carbide single crystal according to claim 6, wherein a stress buffering member is arranged between the seed crystal and the base.
8. The method of manufacturing a silicon carbide single crystal according to claim 7, wherein the stress buffering member has a Young's modulus of less than 5 GPa.
9. The method of manufacturing a silicon carbide single crystal according to claim 6, wherein an outer diameter of the seed crystal is 150 mm or more.
10. The method of manufacturing a silicon carbide single crystal according to claim 9, wherein the outer diameter of the seed crystal is 200 mm or more.
11. A silicon carbide single crystal manufacturing apparatus, comprising: a crucible comprising a crucible body and a crucible lid; and a base consisting of a cross-sectional area reduction portion and a cross-sectional area invariant portion, wherein the cross-sectional area reduction portion comprises a crucible lid side surface of the base supported by a lower surface of the crucible lid and the cross-sectional area invariant portion comprises a seed crystal mounting surface operable to have a seed crystal mounted thereon, wherein the seed crystal mounting surface is disposed on a side of the base opposite from the crucible lid side surface, wherein the base is made of graphite material, the area of the seed crystal mounting surface is larger than the area of the crucible lid side surface, and a cross-sectional area of the base orthogonal to a vertical direction connecting the crucible lid side surface and the seed crystal mounting surface is invariant in the cross-sectional area invariant portion, and the cross-sectional area of the cross-sectional area reduction portion is continuously reduced from a boundary between the cross-sectional area invariant portion and the cross-sectional area reduction portion toward the crucible lid side surface.
Description
BRIEF DESCRIPTION OF DRAWINGS
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DESCRIPTION OF EMBODIMENTS
(16) Hereinafter, embodiments of the present disclosure will be described with reference to the drawings. In each of the following embodiments, the same or equal parts may be designated by the same reference numerals in the drawings. Further, in the drawings used in the following description, the featured portion may be enlarged for convenience in order to make the feature easy to understand, and the dimensional ratio of each component may not be the same as the actual one. Further, the materials, dimensions, etc. exemplified in the following description are examples, and the present disclosure is not limited thereto, and can be appropriately modified and carried out within the range in which the effects of the present disclosure are exhibited.
(17) (Silicon Carbide Single Crystal Manufacturing Apparatus)
(18)
(19) A silicon carbide single crystal manufacturing apparatus 100 shown in
(20) A heat insulating material (not shown) for keeping the crucible 10 warm and a heating means (not shown) are provided on the outer periphery of the crucible body 1. In
(21) In the production of the silicon carbide single crystal, the raw material powder G is filled in the bottom of the crucible 10 and the seed crystal S made of silicon carbide is placed on the base 20. The base 20 is located at a position facing the raw material powder G. Next, the crucible 10 is heated to about 2100 to 2400° C. in a reduced pressure atmosphere to sublimate the raw material powder G, whereby the sublimation gas (raw material gas) is supplied onto the seed crystal S. The raw material gas sublimated from the raw material powder G is recrystallized on the surface of the seed crystal S, so that the silicon carbide single crystal grows.
(22) <Crucible>
(23) The crucible 10 is a crucible for producing a silicon carbide single crystal by a sublimation method, and includes a crucible body 1 and a crucible lid 2. As long as the crucible body 1 and the crucible lid 2 can form a crystal growth space together, there is no limitation on the shape.
(24) As the crucible 10, for example, one made of graphite can be used. The crucible 10 becomes hot during crystal growth. Therefore, it needs to be made of a material that can withstand high temperatures. Graphite has an extremely high sublimation temperature of 3550° C. and can withstand high temperatures during growth.
(25) When the crucible 10 is made of graphite (graphite material), its surface may be coated with TaC or SiC.
(26) <Base>
(27) The base 20 shown in
(28) Like the crucible 10, the base 20 needs to be made of a material that can withstand a high temperature when growing a single crystal, and in this embodiment, it is made of graphite (graphite material).
(29) The base is preferably made of a graphite material having a Young's modulus of 5 GPa or more at room temperature. This is because it has rigidity that can stably support a silicon carbide single crystal.
(30) The surface of the base 20 made of a graphite material may be coated with TaC or SiC.
(31) In the base 20, the area Sb of the seed crystal mounting surface 20B is larger than the area Sa of the crucible lid side surface 20A, the cross-sectional area orthogonal to the straight line L extending in the vertical direction connecting the crucible lid side surface 20A and the seed crystal mounting surface 20B is gradually reduced from the surface of the seed crystal mounting surface 20B toward the crucible lid side surface 20A.
(32) Reference numerals CS1 and CS2 in
(33) The base 20 shown in
(34) In the base 20 shown in
(35) The thermal expansion coefficient of graphite (graphite material) constituting the base 20 does not match the thermal expansion coefficient of silicon carbide constituting the seed crystal in the entire wide temperature range from normal temperature to 2400° C. or higher where the sublimation method is used. Therefore, shear stress is generated at the joint surface (adhesive surface) between the graphite base and the silicon carbide seed crystal. In particular, the expansion difference becomes large in the outer peripheral portion of the seed crystal. When this shear stress becomes large, a gap is formed between the seed crystal and the base due to poor bonding, which leads to the occurrence of macro defects in the crystal.
(36) On the other hand, by making the shape of the base a truncated cone shape, it is possible to suppress such shear stress and reduce macro defects of silicon carbide seed crystals.
(37)
(38) In the base 21 shown in
(39) On the other hand, in the base 21 shown in
(40)
(41) The base 22 shown in
(42) On the other hand, a feature that the cross-sectional area of the base 22 shown in
(43) The base 22 shown in
(44) The side surface 22a of the base 22 is composed of side surfaces 22-1a, 22-2a, 22-3a, 22-4a extending in a direction orthogonal to the seed crystal mounting surface 22B (or the crucible lid side surface 22A), and side surfaces 22-1b, 22-2b, and 22-3b extending in a direction parallel to the seed crystal mounting surface 22B (or the crucible lid side surface 22A).
(45) The base 22 shown in
(46)
(47) The base 23 shown in
(48) On the other hand, in a base 23 shown in
(49) The portion where the cross-sectional area gradually decreases from the seed crystal mounting surface 23B toward the crucible lid side surface 23A and the portion where the cross-sectional area does not change may be integrally formed, or for example, may be bonded with a carbon adhesive or the like.
(50) The base 23 shown in
(51)
(52) The base 24 shown in
(53) On the other hand, in a base 24 shown in
(54) The portion where the cross-sectional area gradually decreases from the seed crystal mounting surface 24B toward the crucible lid side surface 24A and the portion where the cross-sectional area does not change may be integrally formed, or for example, may be bonded with a carbon adhesive or the like.
(55) The base 24 shown in
(56) (Method of Manufacturing Silicon Carbide Single Crystal)
(57) In a method of manufacturing a silicon carbide single crystal according to an embodiment of the present disclosure in which the silicon carbide seed crystal and a silicon carbide raw material are placed in the crucible and a sublimation gas sublimated from the silicon carbide raw material is precipitated on the seed crystal to grow a bulk silicon carbide single crystal, using a crucible constituted by a crucible body and a crucible lid, and a base that is placed on the underside of the crucible lid and holds a silicon carbide seed crystal, wherein the base is made of graphite material, the area of the seed crystal mounting surface is larger than the area of the crucible lid side surface, and the base has at least of a portion in which the cross-sectional area orthogonal to the vertical direction connecting the crucible lid side surface and the seed crystal mounting surface is gradually reduced, and a portion that is getting smaller gradually, from the surface of the seed crystal mounting surface toward the crucible lid side surface.
(58) The base and the seed crystal can be adhered (bonded) using a carbon adhesive or the like. The carbon adhesive is obtained by dispersing carbon powder in an organic solvent, and by volatilizing the solvent, it can be adhered (bonded) without impairing the characteristics of the carbon material.
(59)
(60) In this method for manufacturing a silicon carbide single crystal, a stress buffering member (stress buffering layer) arranged between the seed crystal and the base may be used for the purpose of reducing the stress applied to the seed crystal S during growth.
(61) As mentioned above, the thermal expansion coefficient of graphite (graphite material) constituting the base 20 does not match the thermal expansion coefficient of silicon carbide constituting the seed crystal in the entire wide temperature range from normal temperature to 2400° C. or higher where the sublimation method is used. Therefore, shear stress is generated at the joint surface (adhesive surface) between the graphite base and the silicon carbide seed crystal. In particular, the expansion difference becomes large in the outer peripheral portion of the seed crystal. When this shear stress becomes large, a gap is formed between the seed crystal and the base due to poor bonding, which leads to the occurrence of macro defects in the crystal.
(62) On the other hand, by providing the stress buffering member 30 between the seed crystal S and the base 20, such shear stress can be suppressed, and macro defects of the silicon carbide seed crystal can be reduced.
(63) The stress buffering member preferably has a Young's modulus of less than 5 GPa. As the stress buffering member having a Young's modulus of less than 5 GPa, a carbon sheet or the like can be exemplified.
(64) In this method for manufacturing a silicon carbide single crystal, a seed crystal S having an outer diameter of 150 mm or more can be used. Further, those having an outer diameter of 200 mm or more can also be used.
EXAMPLES
Example 1
(65) The configuration shown in
(66) General-purpose FEM analysis software ANSYS Mechanical (ANSYS, Inc.) was used for the simulation. In order to reduce the computational load, the simulation dealt with the structure of half of an arbitrary cross section passing through the central axis, and performed a two-dimensional simulation. The simulation conditions are as shown below.
(67) The thickness of silicon carbide seed crystal: 3 mm,
(68) The radius of silicon carbide seed crystal: 80 mm,
(69) r2 (Radius of seed crystal mounting surface (see
(70) In addition, as the physical property values of various materials, typical values were used as shown in Table 1.
(71) TABLE-US-00001 TABLE 1 STRESS SILICON GRAPHITE BUFFERING MEMBER CARBIDE BASE MEMBER DENSITY[kg/m.sup.3] 3210 1800 1000 YOUNG'S 500 10 1 MODULUS[Gpa] POISSON'S 0.3 0.3 0.3 RATIO[—] THERMAL EXPANSION 5.0e−6 5.5e−6 0 COEFFICIENT[1/K]
(72) In
(73) It can be seen that the shear stress generated between the silicon carbide seed crystal and the base is suppressed by 10% or more in the range of (r2−r1)/h>0.30.
(74) By reducing the shear stress generated between the silicon carbide seed crystal and the base by 10%, it is possible to suppress poor bonding (adhesion) at the bonding (adhesion) portion.
(75)
(76) Based on the results shown in
(77) When the height h was 20 mm to 40 mm, the relative value of the shear stress was 0.90 or less regardless of the radius r1 of 40 mm to 70 mm. That is, the shear stress generated between the silicon carbide seed crystal and the base is suppressed by 10% or more.
Example 2
(78) Example 2 is different from Example 1 in that it has a stress buffering member (stress buffering layer) between the silicon carbide seed crystal and the base, but other conditions are common. The thickness of the stress buffering member is 1 mm, and the physical property values used are as shown in Table 1.
(79)
(80)
(81) Similar to
(82) It can be seen that the shear stress generated at the evaluation position is suppressed by 10% or more in the range of (r2−r1)/h>0.15.
(83) By reducing the shear stress at the evaluation position by 10%, it is possible to suppress tearing (cracks) of the stress buffering member.
(84) In
(85) The strength of graphite varies depending on the material, but when a graphite sheet (carbon sheet) having a Young's modulus of less than 5 GPa is used as the stress buffering member, the tensile strength thereof is generally about several MPa. The shear strength is smaller than the tensile strength, and the shear strength is further reduced in a member such as a carbon sheet having anisotropy. Therefore, it is considered that stress suppression of several MPa or less has a sufficient effect on cracks in the stress buffering member.
(86)
(87) Based on the results shown in
(88) Further, when the radius r1 was 40 mm to 60 mm and the height h was 20 mm to 50 mm, the relative value of the shear stress was 0.70 or less. That is, the shear stress generated between the silicon carbide seed crystal and the base is suppressed by 30% or more.
Example 3
(89) Example 3 is different from Example 2 in that the radius r2 of the crystal mounting surface is changed to 100 mm, but other conditions are common.
(90)
(91) It can be seen that the shear stress generated at the evaluation position is suppressed by 10% or more in the range of (r2−r1)/h>0.15.
(92) By reducing the shear stress at the evaluation position by 10%, it is possible to suppress tearing (cracks) of the stress buffering member.
(93)
(94) Based on the results shown in
(95) Further, when the radius r1 was 40 mm to 80 mm and the height h was 20 mm to 50 mm, the relative value of the shear stress was 0.72 or less. That is, the shear stress generated between the silicon carbide seed crystal and the base is suppressed by about 30%.
REFERENCE SIGNS LIST
(96) 1: crucible body 2: crucible lid 10: crucible 20, 21, 22, 23, 24: base 20A, 21A, 22A, 23A, 24A: crucible lid side surface 20B, 21B, 22 B, 23B, 24 B: seed crystal mounting surface 30: stress buffering member 100: silicon carbide single crystal manufacturing apparatus